# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2005



data_global
_journal_name_full               Org.Biomol.Chem.

_journal_coden_Cambridge         0177

_publ_contact_author_name        'ProfD Harry Gibson'
_publ_contact_author_address     
;
Department of Chemistry
Virginia Polytechnic Institute and State University
Blacksburg
VA
24061
UNITED STATES OF AMERICA
;

_publ_contact_author_email       HWGIBSON@VT.EDU

_publ_section_title              
;
Regioselective Routes to Disubstituted Dibenzo Crown
Ethers and Their Complexations (2/28)
;
loop_
_publ_author_name
'Harry Gibson'
'Klaus Bonrad'
'Bradley Habenicht'
'Jason W. Jones'
'Peter Lobue'
'Amy E. Ratliff'
;
C.Slebodnick
;
'Hong Wang'

data_cs539
_database_code_depnum_ccdc_archive 'CCDC 265204'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C28 H36 O12, C14 H16 N, P F6, C0.265 H1.060 O0.265'
_chemical_formula_sum            'C42.26 H53.06 F6 N O12.27 P'
_chemical_formula_weight         916.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.324(6)
_cell_length_b                   22.806(6)
_cell_length_c                   26.470(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.20(3)
_cell_angle_gamma                90.00
_cell_volume                     8579(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    967
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      18.97

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.028
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3846
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <2%
_diffrn_reflns_number            32751
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0770
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.73
_diffrn_reflns_theta_max         30.07
_reflns_number_total             12526
_reflns_number_gt                7038
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction)'
_computing_cell_refinement       'CrysAlis (Oxford Diffraction)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12526
_refine_ls_number_parameters     571
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0578
_refine_ls_wR_factor_ref         0.1901
_refine_ls_wR_factor_gt          0.1477
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_restrained_S_all      0.962
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
F2 F 0.67071(19) 0.07557(11) 0.17432(8) 0.0856(8) Uani 1 1 d . . .
P1 P 0.61254(5) 0.12710(3) 0.14655(3) 0.03787(19) Uani 1 1 d . . .
F1 F 0.53202(16) 0.08356(11) 0.12640(9) 0.0875(8) Uani 1 1 d . . .
F3 F 0.69477(14) 0.17045(10) 0.16920(8) 0.0725(6) Uani 1 1 d . . .
F4 F 0.56184(13) 0.13944(9) 0.19567(7) 0.0577(5) Uani 1 1 d . . .
F5 F 0.66423(12) 0.11560(8) 0.09768(6) 0.0466(4) Uani 1 1 d . . .
F6 F 0.55716(17) 0.18051(10) 0.12025(8) 0.0807(7) Uani 1 1 d . . .
O1 O 0.32266(10) 0.39491(7) 0.18452(6) 0.0210(3) Uani 1 1 d . . .
O2 O 0.17459(10) 0.44178(7) 0.11222(5) 0.0203(3) Uani 1 1 d . . .
O3 O 0.00862(10) 0.39003(7) 0.04869(6) 0.0221(3) Uani 1 1 d . . .
O4 O -0.08564(11) 0.27231(7) 0.03652(6) 0.0233(3) Uani 1 1 d . . .
O5 O -0.08372(11) 0.18412(7) 0.09829(6) 0.0251(3) Uani 1 1 d . . .
O6 O 0.04930(11) 0.17128(7) 0.18887(6) 0.0250(4) Uani 1 1 d . . .
O7 O 0.23528(10) 0.17971(7) 0.16114(6) 0.0234(3) Uani 1 1 d . . .
O8 O 0.34184(10) 0.28396(6) 0.20436(5) 0.0201(3) Uani 1 1 d . . .
O9 O 0.48642(10) 0.42617(7) 0.40254(6) 0.0217(3) Uani 1 1 d . . .
O10 O 0.45502(15) 0.49967(8) 0.34854(7) 0.0418(5) Uani 1 1 d . . .
O11 O -0.23201(12) 0.04771(7) -0.08788(6) 0.0261(4) Uani 1 1 d . . .
O12 O -0.21308(11) 0.01091(7) -0.00910(6) 0.0276(4) Uani 1 1 d . . .
C1 C 0.35971(14) 0.38127(9) 0.23309(8) 0.0186(4) Uani 1 1 d . . .
C2 C 0.38779(15) 0.42139(10) 0.27054(8) 0.0209(4) Uani 1 1 d . . .
H2 H 0.3816 0.4621 0.2634 0.025 Uiso 1 1 calc R . .
C3 C 0.42528(14) 0.40275(9) 0.31883(8) 0.0195(4) Uani 1 1 d . . .
C4 C 0.43417(15) 0.34384(9) 0.32953(8) 0.0195(4) Uani 1 1 d . . .
H4 H 0.4596 0.3312 0.3626 0.023 Uiso 1 1 calc R . .
C5 C 0.40605(14) 0.30304(10) 0.29207(8) 0.0207(4) Uani 1 1 d . . .
H5 H 0.4121 0.2624 0.2996 0.025 Uiso 1 1 calc R . .
C6 C 0.36934(14) 0.32095(9) 0.24402(8) 0.0178(4) Uani 1 1 d . . .
C7 C 0.30951(16) 0.45596(10) 0.17349(9) 0.0236(5) Uani 1 1 d . . .
H7A H 0.3704 0.4768 0.1799 0.028 Uiso 1 1 calc R . .
H7B H 0.2660 0.4732 0.1957 0.028 Uiso 1 1 calc R . .
C8 C 0.26970(15) 0.46218(10) 0.11909(8) 0.0226(5) Uani 1 1 d . . .
H8A H 0.2717 0.5038 0.1088 0.027 Uiso 1 1 calc R . .
H8B H 0.3077 0.4391 0.0974 0.027 Uiso 1 1 calc R . .
C9 C 0.12278(15) 0.46576(10) 0.06761(8) 0.0219(4) Uani 1 1 d . . .
H9A H 0.1485 0.4509 0.0370 0.026 Uiso 1 1 calc R . .
H9B H 0.1286 0.5090 0.0681 0.026 Uiso 1 1 calc R . .
C10 C 0.02174(15) 0.44878(9) 0.06540(9) 0.0225(5) Uani 1 1 d . . .
H10A H 0.0013 0.4530 0.0996 0.027 Uiso 1 1 calc R . .
H10B H -0.0173 0.4752 0.0417 0.027 Uiso 1 1 calc R . .
C11 C -0.08867(14) 0.37712(10) 0.03589(9) 0.0217(4) Uani 1 1 d . . .
H11A H -0.1201 0.4104 0.0166 0.026 Uiso 1 1 calc R . .
H11B H -0.1182 0.3721 0.0675 0.026 Uiso 1 1 calc R . .
C12 C -0.10239(15) 0.32252(9) 0.00455(9) 0.0220(4) Uani 1 1 d . . .
H12A H -0.1674 0.3213 -0.0132 0.026 Uiso 1 1 calc R . .
H12B H -0.0585 0.3224 -0.0215 0.026 Uiso 1 1 calc R . .
C13 C 0.45599(15) 0.44816(10) 0.35686(8) 0.0221(5) Uani 1 1 d . . .
C14 C 0.51339(17) 0.46856(11) 0.44165(9) 0.0263(5) Uani 1 1 d . . .
H14A H 0.5706 0.4888 0.4344 0.039 Uiso 1 1 calc R . .
H14B H 0.5254 0.4487 0.4747 0.039 Uiso 1 1 calc R . .
H14C H 0.4626 0.4972 0.4426 0.039 Uiso 1 1 calc R . .
C15 C -0.11478(15) 0.17295(10) 0.04876(8) 0.0203(4) Uani 1 1 d . . .
C16 C -0.14649(14) 0.11901(10) 0.03033(8) 0.0210(4) Uani 1 1 d . . .
H16 H -0.1484 0.0870 0.0532 0.025 Uiso 1 1 calc R . .
C17 C -0.17563(14) 0.11092(9) -0.02121(8) 0.0192(4) Uani 1 1 d . . .
C18 C -0.17393(15) 0.15750(10) -0.05433(8) 0.0209(4) Uani 1 1 d . . .
H18 H -0.1932 0.1521 -0.0897 0.025 Uiso 1 1 calc R . .
C19 C -0.14421(14) 0.21216(10) -0.03609(8) 0.0206(4) Uani 1 1 d . . .
H19 H -0.1439 0.2442 -0.0590 0.025 Uiso 1 1 calc R . .
C20 C -0.11495(14) 0.22052(9) 0.01517(8) 0.0200(4) Uani 1 1 d . . .
C21 C -0.08933(17) 0.13675(11) 0.13298(8) 0.0262(5) Uani 1 1 d . . .
H21A H -0.0540 0.1025 0.1224 0.031 Uiso 1 1 calc R . .
H21B H -0.1558 0.1250 0.1334 0.031 Uiso 1 1 calc R . .
C22 C -0.04801(17) 0.15695(11) 0.18470(9) 0.0279(5) Uani 1 1 d . . .
H22A H -0.0832 0.1919 0.1940 0.033 Uiso 1 1 calc R . .
H22B H -0.0569 0.1257 0.2096 0.033 Uiso 1 1 calc R . .
C23 C 0.10686(17) 0.12231(10) 0.18174(9) 0.0268(5) Uani 1 1 d . . .
H23A H 0.0974 0.1101 0.1456 0.032 Uiso 1 1 calc R . .
H23B H 0.0897 0.0890 0.2028 0.032 Uiso 1 1 calc R . .
C24 C 0.20742(17) 0.13857(10) 0.19681(9) 0.0261(5) Uani 1 1 d . . .
H24A H 0.2152 0.1560 0.2313 0.031 Uiso 1 1 calc R . .
H24B H 0.2475 0.1031 0.1975 0.031 Uiso 1 1 calc R . .
C25 C 0.33432(15) 0.18849(10) 0.16713(9) 0.0250(5) Uani 1 1 d . . .
H25A H 0.3517 0.2084 0.1364 0.030 Uiso 1 1 calc R . .
H25B H 0.3659 0.1498 0.1696 0.030 Uiso 1 1 calc R . .
C26 C 0.36959(16) 0.22373(10) 0.21263(9) 0.0247(5) Uani 1 1 d . . .
H26A H 0.3435 0.2082 0.2429 0.030 Uiso 1 1 calc R . .
H26B H 0.4390 0.2210 0.2191 0.030 Uiso 1 1 calc R . .
C27 C -0.20810(14) 0.05168(10) -0.03735(8) 0.0203(4) Uani 1 1 d . . .
C28 C -0.26432(19) -0.00908(11) -0.10618(10) 0.0321(6) Uani 1 1 d . . .
H28A H -0.2155 -0.0384 -0.0960 0.048 Uiso 1 1 calc R . .
H28B H -0.2777 -0.0082 -0.1434 0.048 Uiso 1 1 calc R . .
H28C H -0.3217 -0.0194 -0.0916 0.048 Uiso 1 1 calc R . .
N1 N 0.16726(12) 0.32052(8) 0.13212(6) 0.0178(4) Uani 1 1 d . . .
H1A H 0.1700 0.3600 0.1251 0.021 Uiso 1 1 calc R . .
H1B H 0.2225 0.3104 0.1518 0.021 Uiso 1 1 calc R . .
C29 C 0.15975(15) 0.28723(9) 0.08338(8) 0.0193(4) Uani 1 1 d . . .
H29A H 0.0948 0.2905 0.0658 0.023 Uiso 1 1 calc R . .
H29B H 0.1728 0.2453 0.0908 0.023 Uiso 1 1 calc R . .
C30 C 0.22761(15) 0.30984(9) 0.04895(8) 0.0199(4) Uani 1 1 d . . .
C31 C 0.32392(16) 0.31204(11) 0.06419(9) 0.0253(5) Uani 1 1 d . . .
H31 H 0.3478 0.3008 0.0979 0.030 Uiso 1 1 calc R . .
C32 C 0.38536(17) 0.33015(11) 0.03134(10) 0.0284(5) Uani 1 1 d . . .
H32 H 0.4511 0.3310 0.0423 0.034 Uiso 1 1 calc R . .
C33 C 0.35159(17) 0.34683(11) -0.01710(9) 0.0295(5) Uani 1 1 d . . .
H33 H 0.3939 0.3589 -0.0400 0.035 Uiso 1 1 calc R . .
C34 C 0.25617(18) 0.34608(10) -0.03270(9) 0.0284(5) Uani 1 1 d . . .
H34 H 0.2327 0.3582 -0.0662 0.034 Uiso 1 1 calc R . .
C35 C 0.19447(16) 0.32769(10) 0.00023(8) 0.0227(5) Uani 1 1 d . . .
H35 H 0.1287 0.3274 -0.0108 0.027 Uiso 1 1 calc R . .
C36 C 0.08648(15) 0.30946(10) 0.16198(8) 0.0222(5) Uani 1 1 d . . .
H36A H 0.0291 0.3288 0.1450 0.027 Uiso 1 1 calc R . .
H36B H 0.0741 0.2668 0.1633 0.027 Uiso 1 1 calc R . .
C37 C 0.10893(15) 0.33278(10) 0.21466(8) 0.0230(5) Uani 1 1 d . . .
C38 C 0.13582(17) 0.29494(12) 0.25463(9) 0.0295(5) Uani 1 1 d . . .
H38 H 0.1381 0.2540 0.2484 0.035 Uiso 1 1 calc R . .
C39 C 0.15935(18) 0.31586(14) 0.30326(9) 0.0362(6) Uani 1 1 d . . .
H39 H 0.1769 0.2893 0.3305 0.043 Uiso 1 1 calc R . .
C40 C 0.15754(18) 0.37501(14) 0.31258(9) 0.0359(6) Uani 1 1 d . . .
H40 H 0.1747 0.3894 0.3461 0.043 Uiso 1 1 calc R . .
C41 C 0.13093(18) 0.41348(13) 0.27342(10) 0.0357(6) Uani 1 1 d . . .
H41 H 0.1295 0.4544 0.2799 0.043 Uiso 1 1 calc R . .
C42 C 0.10619(16) 0.39243(11) 0.22435(9) 0.0277(5) Uani 1 1 d . . .
H42 H 0.0873 0.4190 0.1973 0.033 Uiso 1 1 calc R . .
O13 O 0.0873(9) 0.5511(6) 0.2845(5) 0.090(5) Uiso 0.265(7) 1 d P . .
C43 C -0.0301(19) 0.5415(11) 0.2385(11) 0.143(12) Uiso 0.265(7) 1 d P . .
H43A H -0.0157 0.5371 0.2034 0.214 Uiso 0.265(7) 1 calc PR . .
H43B H -0.0699 0.5761 0.2407 0.214 Uiso 0.265(7) 1 calc PR . .
H43C H -0.0633 0.5066 0.2483 0.214 Uiso 0.265(7) 1 calc PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
F2 0.126(2) 0.0825(17) 0.0528(13) 0.0139(11) 0.0292(13) 0.0579(15)
P1 0.0424(4) 0.0352(4) 0.0374(4) -0.0098(3) 0.0104(3) 0.0040(3)
F1 0.0755(15) 0.0954(18) 0.0985(18) -0.0679(15) 0.0384(13) -0.0406(13)
F3 0.0555(12) 0.0861(16) 0.0792(15) -0.0422(12) 0.0204(10) -0.0138(11)
F4 0.0568(11) 0.0693(13) 0.0506(11) -0.0286(9) 0.0209(9) -0.0022(9)
F5 0.0566(11) 0.0511(10) 0.0345(9) -0.0019(8) 0.0146(8) 0.0125(8)
F6 0.0980(17) 0.0821(16) 0.0640(14) 0.0090(12) 0.0174(12) 0.0523(14)
O1 0.0242(8) 0.0196(8) 0.0178(8) 0.0017(6) -0.0028(6) 0.0000(6)
O2 0.0201(8) 0.0218(8) 0.0181(8) 0.0038(6) -0.0014(6) -0.0028(6)
O3 0.0180(7) 0.0184(8) 0.0289(9) -0.0027(6) -0.0013(6) 0.0007(6)
O4 0.0263(8) 0.0191(8) 0.0234(8) -0.0022(6) -0.0016(6) -0.0009(6)
O5 0.0320(9) 0.0260(8) 0.0155(8) -0.0003(6) -0.0042(6) -0.0017(7)
O6 0.0291(9) 0.0234(8) 0.0215(8) -0.0032(6) -0.0013(6) -0.0030(6)
O7 0.0241(8) 0.0246(8) 0.0200(8) -0.0006(6) -0.0026(6) -0.0010(6)
O8 0.0234(8) 0.0185(8) 0.0170(7) -0.0025(6) -0.0027(6) 0.0016(6)
O9 0.0253(8) 0.0205(8) 0.0179(8) -0.0043(6) -0.0025(6) -0.0022(6)
O10 0.0700(14) 0.0203(9) 0.0301(10) -0.0011(7) -0.0127(9) -0.0045(8)
O11 0.0352(9) 0.0216(8) 0.0197(8) -0.0030(6) -0.0035(7) 0.0005(7)
O12 0.0301(9) 0.0245(9) 0.0270(9) 0.0011(7) -0.0008(7) -0.0029(7)
C1 0.0165(10) 0.0221(11) 0.0169(10) 0.0013(8) 0.0008(8) 0.0009(8)
C2 0.0220(11) 0.0173(10) 0.0224(11) 0.0009(8) -0.0014(8) -0.0018(8)
C3 0.0191(10) 0.0202(10) 0.0190(11) -0.0015(8) 0.0021(8) -0.0017(8)
C4 0.0206(10) 0.0226(11) 0.0150(10) 0.0011(8) 0.0005(8) 0.0003(8)
C5 0.0214(10) 0.0194(10) 0.0209(11) 0.0017(8) 0.0013(8) -0.0002(8)
C6 0.0140(9) 0.0226(11) 0.0170(10) -0.0024(8) 0.0022(7) 0.0003(8)
C7 0.0252(11) 0.0196(11) 0.0243(12) 0.0028(9) -0.0030(9) -0.0021(9)
C8 0.0205(11) 0.0249(11) 0.0219(11) 0.0047(9) -0.0002(9) -0.0050(8)
C9 0.0249(11) 0.0207(11) 0.0189(11) 0.0021(8) -0.0022(9) -0.0022(8)
C10 0.0250(11) 0.0183(11) 0.0227(11) -0.0013(9) -0.0032(9) 0.0025(8)
C11 0.0162(10) 0.0219(11) 0.0263(12) -0.0010(9) -0.0001(8) 0.0020(8)
C12 0.0211(11) 0.0211(11) 0.0229(11) 0.0005(9) -0.0009(8) 0.0003(8)
C13 0.0224(11) 0.0213(11) 0.0223(11) -0.0016(9) 0.0016(9) 0.0005(8)
C14 0.0275(12) 0.0280(12) 0.0218(12) -0.0085(9) -0.0029(9) -0.0016(9)
C15 0.0187(10) 0.0246(11) 0.0168(10) -0.0006(8) -0.0004(8) 0.0027(8)
C16 0.0185(10) 0.0235(11) 0.0203(11) 0.0024(9) 0.0002(8) 0.0015(8)
C17 0.0151(10) 0.0221(11) 0.0201(11) -0.0027(8) 0.0006(8) 0.0021(8)
C18 0.0173(10) 0.0286(12) 0.0163(10) -0.0015(9) 0.0005(8) 0.0013(8)
C19 0.0205(10) 0.0226(11) 0.0183(11) 0.0017(8) 0.0007(8) 0.0006(8)
C20 0.0162(10) 0.0211(11) 0.0224(11) -0.0017(8) 0.0013(8) 0.0005(8)
C21 0.0281(12) 0.0310(13) 0.0183(11) 0.0021(9) -0.0015(9) -0.0053(9)
C22 0.0324(13) 0.0337(13) 0.0169(11) -0.0012(10) 0.0012(9) -0.0043(10)
C23 0.0339(13) 0.0206(11) 0.0254(12) -0.0027(9) 0.0022(10) -0.0017(9)
C24 0.0321(13) 0.0217(11) 0.0231(12) 0.0011(9) -0.0022(9) 0.0002(9)
C25 0.0254(12) 0.0236(11) 0.0257(12) -0.0054(9) 0.0019(9) 0.0016(9)
C26 0.0248(11) 0.0196(11) 0.0279(12) -0.0035(9) -0.0044(9) 0.0041(9)
C27 0.0163(10) 0.0242(11) 0.0199(11) -0.0018(9) -0.0003(8) 0.0020(8)
C28 0.0425(15) 0.0234(12) 0.0278(13) -0.0061(10) -0.0061(11) -0.0046(10)
N1 0.0196(9) 0.0189(9) 0.0147(8) -0.0018(7) 0.0009(7) 0.0001(7)
C29 0.0229(10) 0.0201(10) 0.0145(10) -0.0025(8) 0.0005(8) 0.0005(8)
C30 0.0250(11) 0.0173(10) 0.0174(10) -0.0044(8) 0.0029(8) 0.0009(8)
C31 0.0270(12) 0.0286(12) 0.0199(11) -0.0004(9) 0.0008(9) 0.0022(9)
C32 0.0232(12) 0.0295(13) 0.0332(14) -0.0070(10) 0.0066(10) -0.0026(9)
C33 0.0351(13) 0.0281(12) 0.0277(13) -0.0074(10) 0.0135(10) -0.0090(10)
C34 0.0422(14) 0.0263(12) 0.0170(11) -0.0031(9) 0.0053(10) -0.0036(10)
C35 0.0262(11) 0.0220(11) 0.0194(11) -0.0036(9) 0.0006(9) 0.0011(9)
C36 0.0200(10) 0.0296(12) 0.0173(10) 0.0005(9) 0.0034(8) -0.0048(9)
C37 0.0184(11) 0.0328(13) 0.0182(11) -0.0031(9) 0.0040(8) -0.0044(9)
C38 0.0326(13) 0.0341(13) 0.0220(12) 0.0015(10) 0.0045(10) -0.0035(10)
C39 0.0350(14) 0.0549(18) 0.0184(12) 0.0028(12) 0.0019(10) -0.0061(12)
C40 0.0282(13) 0.0603(19) 0.0194(12) -0.0120(12) 0.0038(10) -0.0123(12)
C41 0.0364(14) 0.0424(15) 0.0293(14) -0.0152(12) 0.0086(11) -0.0080(11)
C42 0.0264(12) 0.0334(13) 0.0238(12) -0.0037(10) 0.0053(9) -0.0024(10)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F2 P1 1.569(2) . ?
P1 F1 1.564(2) . ?
P1 F6 1.568(2) . ?
P1 F5 1.5907(18) . ?
P1 F4 1.5919(19) . ?
P1 F3 1.596(2) . ?
O1 C1 1.364(3) . ?
O1 C7 1.430(3) . ?
O2 C9 1.423(3) . ?
O2 C8 1.430(3) . ?
O3 C10 1.416(3) . ?
O3 C11 1.423(3) . ?
O4 C20 1.353(3) . ?
O4 C12 1.426(3) . ?
O5 C15 1.355(3) . ?
O5 C21 1.427(3) . ?
O6 C23 1.415(3) . ?
O6 C22 1.422(3) . ?
O7 C25 1.422(3) . ?
O7 C24 1.423(3) . ?
O8 C6 1.366(3) . ?
O8 C26 1.439(3) . ?
O9 C13 1.331(3) . ?
O9 C14 1.434(3) . ?
O10 C13 1.195(3) . ?
O11 C27 1.342(3) . ?
O11 C28 1.439(3) . ?
O12 C27 1.201(3) . ?
C1 C2 1.372(3) . ?
C1 C6 1.409(3) . ?
C2 C3 1.390(3) . ?
C3 C4 1.376(3) . ?
C3 C13 1.473(3) . ?
C4 C5 1.382(3) . ?
C5 C6 1.376(3) . ?
C7 C8 1.488(3) . ?
C9 C10 1.492(3) . ?
C11 C12 1.495(3) . ?
C15 C16 1.379(3) . ?
C15 C20 1.403(3) . ?
C16 C17 1.388(3) . ?
C17 C18 1.380(3) . ?
C17 C27 1.475(3) . ?
C18 C19 1.385(3) . ?
C19 C20 1.382(3) . ?
C21 C22 1.494(3) . ?
C23 C24 1.492(3) . ?
C25 C26 1.483(3) . ?
N1 C29 1.489(3) . ?
N1 C36 1.502(3) . ?
C29 C30 1.504(3) . ?
C30 C35 1.379(3) . ?
C30 C31 1.389(3) . ?
C31 C32 1.376(3) . ?
C32 C33 1.366(4) . ?
C33 C34 1.377(4) . ?
C34 C35 1.382(3) . ?
C36 C37 1.489(3) . ?
C37 C38 1.382(3) . ?
C37 C42 1.386(3) . ?
C38 C39 1.375(3) . ?
C39 C40 1.372(4) . ?
C40 C41 1.375(4) . ?
C41 C42 1.388(3) . ?
O13 C43 0.98(2) 2 ?
O13 C43 1.96(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 P1 F6 91.80(15) . . ?
F1 P1 F2 90.56(16) . . ?
F6 P1 F2 177.53(15) . . ?
F1 P1 F5 90.94(11) . . ?
F6 P1 F5 91.62(11) . . ?
F2 P1 F5 89.05(11) . . ?
F1 P1 F4 89.91(11) . . ?
F6 P1 F4 88.17(12) . . ?
F2 P1 F4 91.12(12) . . ?
F5 P1 F4 179.13(12) . . ?
F1 P1 F3 177.83(15) . . ?
F6 P1 F3 89.66(14) . . ?
F2 P1 F3 87.96(15) . . ?
F5 P1 F3 90.62(11) . . ?
F4 P1 F3 88.54(11) . . ?
C1 O1 C7 116.11(17) . . ?
C9 O2 C8 111.71(16) . . ?
C10 O3 C11 110.95(16) . . ?
C20 O4 C12 115.65(16) . . ?
C15 O5 C21 116.25(17) . . ?
C23 O6 C22 112.96(18) . . ?
C25 O7 C24 112.19(17) . . ?
C6 O8 C26 115.16(16) . . ?
C13 O9 C14 115.46(18) . . ?
C27 O11 C28 115.30(18) . . ?
O1 C1 C2 125.0(2) . . ?
O1 C1 C6 115.64(18) . . ?
C2 C1 C6 119.38(19) . . ?
C1 C2 C3 120.3(2) . . ?
C4 C3 C2 120.2(2) . . ?
C4 C3 C13 122.3(2) . . ?
C2 C3 C13 117.49(19) . . ?
C3 C4 C5 119.9(2) . . ?
C6 C5 C4 120.4(2) . . ?
O8 C6 C5 124.6(2) . . ?
O8 C6 C1 115.72(18) . . ?
C5 C6 C1 119.71(19) . . ?
O1 C7 C8 108.36(18) . . ?
O2 C8 C7 109.61(18) . . ?
O2 C9 C10 109.58(18) . . ?
O3 C10 C9 110.35(18) . . ?
O3 C11 C12 111.15(17) . . ?
O4 C12 C11 109.81(18) . . ?
O10 C13 O9 122.2(2) . . ?
O10 C13 C3 124.7(2) . . ?
O9 C13 C3 113.07(19) . . ?
O5 C15 C16 124.3(2) . . ?
O5 C15 C20 116.25(19) . . ?
C16 C15 C20 119.4(2) . . ?
C15 C16 C17 120.8(2) . . ?
C18 C17 C16 119.7(2) . . ?
C18 C17 C27 123.5(2) . . ?
C16 C17 C27 116.9(2) . . ?
C17 C18 C19 120.1(2) . . ?
C20 C19 C18 120.6(2) . . ?
O4 C20 C19 124.8(2) . . ?
O4 C20 C15 115.77(19) . . ?
C19 C20 C15 119.5(2) . . ?
O5 C21 C22 107.96(19) . . ?
O6 C22 C21 114.43(19) . . ?
O6 C23 C24 109.10(19) . . ?
O7 C24 C23 109.14(18) . . ?
O7 C25 C26 113.60(19) . . ?
O8 C26 C25 109.53(18) . . ?
O12 C27 O11 122.8(2) . . ?
O12 C27 C17 124.8(2) . . ?
O11 C27 C17 112.48(19) . . ?
C29 N1 C36 113.17(16) . . ?
N1 C29 C30 111.59(17) . . ?
C35 C30 C31 118.3(2) . . ?
C35 C30 C29 119.67(19) . . ?
C31 C30 C29 122.0(2) . . ?
C32 C31 C30 121.2(2) . . ?
C33 C32 C31 119.8(2) . . ?
C32 C33 C34 119.9(2) . . ?
C33 C34 C35 120.2(2) . . ?
C30 C35 C34 120.5(2) . . ?
C37 C36 N1 110.03(17) . . ?
C38 C37 C42 118.9(2) . . ?
C38 C37 C36 120.0(2) . . ?
C42 C37 C36 121.1(2) . . ?
C39 C38 C37 120.8(3) . . ?
C40 C39 C38 120.1(3) . . ?
C39 C40 C41 120.1(2) . . ?
C40 C41 C42 119.9(3) . . ?
C37 C42 C41 120.2(2) . . ?
C43 O13 C43 6.5(10) 2 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 O1 C1 C2 -2.6(3) . . . . ?
C7 O1 C1 C6 177.89(18) . . . . ?
O1 C1 C2 C3 -179.6(2) . . . . ?
C6 C1 C2 C3 -0.1(3) . . . . ?
C1 C2 C3 C4 -0.3(3) . . . . ?
C1 C2 C3 C13 178.6(2) . . . . ?
C2 C3 C4 C5 0.2(3) . . . . ?
C13 C3 C4 C5 -178.6(2) . . . . ?
C3 C4 C5 C6 0.2(3) . . . . ?
C26 O8 C6 C5 -11.2(3) . . . . ?
C26 O8 C6 C1 167.70(18) . . . . ?
C4 C5 C6 O8 178.36(19) . . . . ?
C4 C5 C6 C1 -0.5(3) . . . . ?
O1 C1 C6 O8 1.1(3) . . . . ?
C2 C1 C6 O8 -178.50(18) . . . . ?
O1 C1 C6 C5 -179.97(18) . . . . ?
C2 C1 C6 C5 0.5(3) . . . . ?
C1 O1 C7 C8 179.47(17) . . . . ?
C9 O2 C8 C7 158.21(18) . . . . ?
O1 C7 C8 O2 70.6(2) . . . . ?
C8 O2 C9 C10 -173.46(18) . . . . ?
C11 O3 C10 C9 -167.45(18) . . . . ?
O2 C9 C10 O3 -77.8(2) . . . . ?
C10 O3 C11 C12 163.50(18) . . . . ?
C20 O4 C12 C11 166.31(18) . . . . ?
O3 C11 C12 O4 77.9(2) . . . . ?
C14 O9 C13 O10 3.1(3) . . . . ?
C14 O9 C13 C3 -177.39(18) . . . . ?
C4 C3 C13 O10 175.2(2) . . . . ?
C2 C3 C13 O10 -3.6(3) . . . . ?
C4 C3 C13 O9 -4.3(3) . . . . ?
C2 C3 C13 O9 176.84(19) . . . . ?
C21 O5 C15 C16 -3.1(3) . . . . ?
C21 O5 C15 C20 176.02(19) . . . . ?
O5 C15 C16 C17 -178.9(2) . . . . ?
C20 C15 C16 C17 2.1(3) . . . . ?
C15 C16 C17 C18 -0.8(3) . . . . ?
C15 C16 C17 C27 179.81(19) . . . . ?
C16 C17 C18 C19 -0.7(3) . . . . ?
C27 C17 C18 C19 178.71(19) . . . . ?
C17 C18 C19 C20 0.8(3) . . . . ?
C12 O4 C20 C19 11.3(3) . . . . ?
C12 O4 C20 C15 -168.62(18) . . . . ?
C18 C19 C20 O4 -179.35(19) . . . . ?
C18 C19 C20 C15 0.5(3) . . . . ?
O5 C15 C20 O4 -1.2(3) . . . . ?
C16 C15 C20 O4 177.95(19) . . . . ?
O5 C15 C20 C19 178.90(18) . . . . ?
C16 C15 C20 C19 -1.9(3) . . . . ?
C15 O5 C21 C22 177.46(18) . . . . ?
C23 O6 C22 C21 -64.8(3) . . . . ?
O5 C21 C22 O6 -63.6(3) . . . . ?
C22 O6 C23 C24 -168.86(18) . . . . ?
C25 O7 C24 C23 -168.46(18) . . . . ?
O6 C23 C24 O7 -68.8(2) . . . . ?
C24 O7 C25 C26 -73.7(2) . . . . ?
C6 O8 C26 C25 179.27(18) . . . . ?
O7 C25 C26 O8 -71.8(2) . . . . ?
C28 O11 C27 O12 0.0(3) . . . . ?
C28 O11 C27 C17 179.97(19) . . . . ?
C18 C17 C27 O12 -177.5(2) . . . . ?
C16 C17 C27 O12 1.9(3) . . . . ?
C18 C17 C27 O11 2.5(3) . . . . ?
C16 C17 C27 O11 -178.07(18) . . . . ?
C36 N1 C29 C30 166.24(18) . . . . ?
N1 C29 C30 C35 -124.4(2) . . . . ?
N1 C29 C30 C31 57.3(3) . . . . ?
C35 C30 C31 C32 -1.6(3) . . . . ?
C29 C30 C31 C32 176.8(2) . . . . ?
C30 C31 C32 C33 0.6(4) . . . . ?
C31 C32 C33 C34 0.7(4) . . . . ?
C32 C33 C34 C35 -0.9(4) . . . . ?
C31 C30 C35 C34 1.3(3) . . . . ?
C29 C30 C35 C34 -177.1(2) . . . . ?
C33 C34 C35 C30 -0.1(3) . . . . ?
C29 N1 C36 C37 167.14(18) . . . . ?
N1 C36 C37 C38 -102.6(2) . . . . ?
N1 C36 C37 C42 75.4(3) . . . . ?
C42 C37 C38 C39 0.1(3) . . . . ?
C36 C37 C38 C39 178.2(2) . . . . ?
C37 C38 C39 C40 -0.9(4) . . . . ?
C38 C39 C40 C41 0.9(4) . . . . ?
C39 C40 C41 C42 -0.2(4) . . . . ?
C38 C37 C42 C41 0.5(3) . . . . ?
C36 C37 C42 C41 -177.5(2) . . . . ?
C40 C41 C42 C37 -0.5(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        30.07
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.162


data_gib64
_database_code_depnum_ccdc_archive 'CCDC 265205'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H36 F6 K O12 P'
_chemical_formula_weight         748.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3429(7)
_cell_length_b                   12.6823(9)
_cell_length_c                   13.1381(9)
_cell_angle_alpha                83.7740(10)
_cell_angle_beta                 72.7110(10)
_cell_angle_gamma                77.9380(10)
_cell_volume                     1607.17(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8841
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.51

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.779
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13450
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         27.51
_reflns_number_total             6911
_reflns_number_gt                5996
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.9282P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6911
_refine_ls_number_parameters     577
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.0988
_refine_ls_wR_factor_gt          0.0950
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.65205(4) 0.24404(3) 0.32469(3) 0.01790(9) Uani 1 1 d . . .
O1 O 0.50580(12) 0.39843(10) 0.19241(10) 0.0206(3) Uani 1 1 d . . .
O2 O 0.37346(13) 0.26613(10) 0.36303(10) 0.0201(3) Uani 1 1 d . . .
O3 O 0.47808(12) 0.38293(9) 0.48667(10) 0.0190(3) Uani 1 1 d . . .
O4 O 0.61307(13) 0.19968(9) 0.55752(10) 0.0210(3) Uani 1 1 d . . .
O5 O 0.65849(13) 0.03569(9) 0.44573(10) 0.0192(3) Uani 1 1 d . . .
O6 O 0.64791(13) 0.05892(10) 0.22687(10) 0.0219(3) Uani 1 1 d . . .
O7 O 0.81552(14) 0.20514(10) 0.12042(10) 0.0238(3) Uani 1 1 d . . .
O8 O 0.75635(13) 0.42369(10) 0.18521(10) 0.0213(3) Uani 1 1 d . . .
O9 O 0.80535(17) 0.79299(13) -0.00942(15) 0.0447(4) Uani 1 1 d . . .
O10 O 0.59627(15) 0.85273(11) -0.03239(11) 0.0294(3) Uani 1 1 d . . .
O11 O 1.08837(13) -0.16403(11) 0.66965(11) 0.0260(3) Uani 1 1 d . . .
O12 O 0.98367(13) -0.24987(10) 0.58555(11) 0.0222(3) Uani 1 1 d . . .
C1 C 0.53979(18) 0.49520(14) 0.15096(14) 0.0188(3) Uani 1 1 d . . .
C2 C 0.67459(18) 0.50689(14) 0.14324(14) 0.0191(3) Uani 1 1 d . . .
C3 C 0.71982(19) 0.60130(15) 0.09947(14) 0.0208(4) Uani 1 1 d . . .
C4 C 0.63199(19) 0.68553(14) 0.06105(14) 0.0212(4) Uani 1 1 d . . .
C5 C 0.4973(2) 0.67483(15) 0.07209(15) 0.0227(4) Uani 1 1 d . . .
C6 C 0.45097(19) 0.58061(15) 0.11692(15) 0.0216(4) Uani 1 1 d . . .
C7 C 0.36610(18) 0.38651(15) 0.20475(15) 0.0211(4) Uani 1 1 d . . .
C8 C 0.34914(19) 0.27797(15) 0.26103(15) 0.0219(4) Uani 1 1 d . . .
C9 C 0.28348(18) 0.34122(14) 0.43905(15) 0.0202(4) Uani 1 1 d . . .
C10 C 0.35726(18) 0.42807(13) 0.45382(15) 0.0195(4) Uani 1 1 d . . .
C11 C 0.44686(19) 0.35757(15) 0.59845(15) 0.0213(4) Uani 1 1 d . . .
C12 C 0.5736(2) 0.29155(14) 0.62269(15) 0.0210(4) Uani 1 1 d . . .
C13 C 0.71131(18) 0.11648(13) 0.57750(14) 0.0184(3) Uani 1 1 d . . .
C14 C 0.73313(17) 0.02482(13) 0.51821(14) 0.0172(3) Uani 1 1 d . . .
C15 C 0.82381(17) -0.06667(13) 0.53601(14) 0.0174(3) Uani 1 1 d . . .
C16 C 0.89857(17) -0.06578(13) 0.60901(14) 0.0177(3) Uani 1 1 d . . .
C17 C 0.88221(18) 0.02618(14) 0.66333(14) 0.0197(3) Uani 1 1 d . . .
C18 C 0.78648(19) 0.11733(14) 0.64883(14) 0.0203(4) Uani 1 1 d . . .
C19 C 0.6783(2) -0.05659(14) 0.38438(15) 0.0209(4) Uani 1 1 d . . .
C20 C 0.6000(2) -0.02375(15) 0.30230(16) 0.0233(4) Uani 1 1 d . . .
C21 C 0.7791(2) 0.02510(16) 0.15242(16) 0.0275(4) Uani 1 1 d . . .
C22 C 0.8060(2) 0.11533(16) 0.06933(16) 0.0281(4) Uani 1 1 d . . .
C23 C 0.8561(2) 0.29192(16) 0.04772(16) 0.0251(4) Uani 1 1 d . . .
C24 C 0.88186(19) 0.37419(16) 0.10909(16) 0.0239(4) Uani 1 1 d . . .
C25 C 0.6890(2) 0.78109(15) 0.00490(15) 0.0254(4) Uani 1 1 d . . .
C26 C 0.6482(3) 0.94263(17) -0.09760(19) 0.0340(5) Uani 1 1 d . . .
C27 C 1.00053(17) -0.16251(14) 0.62566(14) 0.0192(3) Uani 1 1 d . . .
C28 C 1.0819(2) -0.34764(16) 0.59098(19) 0.0284(4) Uani 1 1 d . . .
P1 P 0.02122(5) 0.65970(4) 0.26683(4) 0.02260(12) Uani 1 1 d . . .
F1 F -0.08851(16) 0.58951(10) 0.33580(11) 0.0529(4) Uani 1 1 d . . .
F2 F -0.03380(12) 0.74773(9) 0.35565(9) 0.0309(3) Uani 1 1 d . . .
F3 F 0.13164(13) 0.72953(11) 0.19751(10) 0.0397(3) Uani 1 1 d . . .
F4 F 0.07801(14) 0.57093(10) 0.17796(10) 0.0372(3) Uani 1 1 d . . .
F5 F 0.13123(16) 0.59815(13) 0.32740(11) 0.0589(5) Uani 1 1 d . . .
F6 F -0.08699(13) 0.72179(11) 0.20659(11) 0.0405(3) Uani 1 1 d . . .
H3 H 0.810(2) 0.6078(16) 0.0954(17) 0.022(5) Uiso 1 1 d . . .
H5 H 0.437(2) 0.7308(18) 0.0474(18) 0.028(6) Uiso 1 1 d . . .
H6 H 0.362(2) 0.5750(18) 0.1204(18) 0.029(6) Uiso 1 1 d . . .
H7A H 0.349(2) 0.3891(17) 0.1347(18) 0.025(5) Uiso 1 1 d . . .
H7B H 0.303(2) 0.4449(18) 0.2436(17) 0.023(5) Uiso 1 1 d . . .
H8A H 0.415(2) 0.2246(17) 0.2181(17) 0.021(5) Uiso 1 1 d . . .
H8B H 0.255(2) 0.2689(16) 0.2666(16) 0.019(5) Uiso 1 1 d . . .
H9A H 0.256(2) 0.3001(16) 0.5049(17) 0.017(5) Uiso 1 1 d . . .
H9B H 0.202(2) 0.3769(15) 0.4208(15) 0.013(5) Uiso 1 1 d . . .
H10A H 0.292(2) 0.4782(16) 0.5054(16) 0.017(5) Uiso 1 1 d . . .
H10B H 0.389(2) 0.4682(15) 0.3845(16) 0.014(5) Uiso 1 1 d . . .
H11A H 0.417(2) 0.4233(17) 0.6376(17) 0.021(5) Uiso 1 1 d . . .
H11B H 0.376(2) 0.3171(16) 0.6209(16) 0.017(5) Uiso 1 1 d . . .
H12A H 0.5516(19) 0.2712(15) 0.6994(16) 0.013(5) Uiso 1 1 d . . .
H12B H 0.649(2) 0.3328(15) 0.6068(15) 0.015(5) Uiso 1 1 d . . .
H15 H 0.842(2) -0.1309(17) 0.4951(17) 0.021(5) Uiso 1 1 d . . .
H17 H 0.936(2) 0.0271(17) 0.7123(17) 0.025(5) Uiso 1 1 d . . .
H18 H 0.773(2) 0.1792(17) 0.6859(17) 0.024(5) Uiso 1 1 d . . .
H19A H 0.775(2) -0.0817(16) 0.3515(16) 0.018(5) Uiso 1 1 d . . .
H19B H 0.6421(19) -0.1166(15) 0.4331(15) 0.014(5) Uiso 1 1 d . . .
H20A H 0.606(2) -0.0855(18) 0.2639(18) 0.027(6) Uiso 1 1 d . . .
H20B H 0.503(2) 0.0046(17) 0.3356(18) 0.026(5) Uiso 1 1 d . . .
H21A H 0.779(3) -0.038(2) 0.118(2) 0.040(7) Uiso 1 1 d . . .
H21B H 0.851(2) 0.0107(17) 0.1872(18) 0.025(5) Uiso 1 1 d . . .
H22A H 0.894(3) 0.0932(19) 0.014(2) 0.038(6) Uiso 1 1 d . . .
H22B H 0.731(2) 0.1334(18) 0.0378(18) 0.028(6) Uiso 1 1 d . . .
H23A H 0.937(2) 0.2676(17) -0.0067(18) 0.024(5) Uiso 1 1 d . . .
H23B H 0.787(2) 0.3238(17) 0.0119(18) 0.026(6) Uiso 1 1 d . . .
H24A H 0.923(2) 0.4270(16) 0.0602(17) 0.020(5) Uiso 1 1 d . . .
H24B H 0.942(2) 0.3411(16) 0.1517(16) 0.015(5) Uiso 1 1 d . . .
H26A H 0.666(3) 0.993(2) -0.056(2) 0.056(8) Uiso 1 1 d . . .
H26B H 0.573(3) 0.982(2) -0.127(2) 0.055(8) Uiso 1 1 d . . .
H26C H 0.725(3) 0.914(2) -0.155(2) 0.042(7) Uiso 1 1 d . . .
H28A H 1.069(2) -0.3740(19) 0.663(2) 0.036(6) Uiso 1 1 d . . .
H28B H 1.063(3) -0.394(2) 0.546(2) 0.040(7) Uiso 1 1 d . . .
H28C H 1.172(3) -0.335(2) 0.559(2) 0.038(7) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
K1 0.01642(18) 0.01745(17) 0.01847(19) -0.00179(13) -0.00367(14) -0.00152(13)
O1 0.0151(6) 0.0221(6) 0.0238(7) 0.0004(5) -0.0036(5) -0.0053(5)
O2 0.0196(6) 0.0180(6) 0.0218(6) -0.0051(5) -0.0030(5) -0.0033(5)
O3 0.0191(6) 0.0169(6) 0.0199(6) -0.0024(5) -0.0039(5) -0.0022(5)
O4 0.0263(7) 0.0144(6) 0.0237(7) -0.0053(5) -0.0110(5) 0.0008(5)
O5 0.0234(6) 0.0144(5) 0.0220(6) -0.0037(5) -0.0100(5) -0.0017(5)
O6 0.0241(7) 0.0195(6) 0.0214(7) -0.0017(5) -0.0066(5) -0.0020(5)
O7 0.0285(7) 0.0243(6) 0.0172(6) -0.0014(5) -0.0031(5) -0.0067(5)
O8 0.0181(6) 0.0238(6) 0.0208(6) 0.0019(5) -0.0050(5) -0.0032(5)
O9 0.0361(9) 0.0368(9) 0.0666(12) 0.0195(8) -0.0219(8) -0.0191(7)
O10 0.0332(8) 0.0223(7) 0.0297(8) 0.0050(6) -0.0064(6) -0.0055(6)
O11 0.0210(7) 0.0288(7) 0.0299(7) -0.0024(6) -0.0119(6) -0.0009(5)
O12 0.0197(6) 0.0168(6) 0.0300(7) -0.0016(5) -0.0091(5) 0.0002(5)
C1 0.0211(9) 0.0200(8) 0.0136(8) -0.0030(6) -0.0009(6) -0.0044(7)
C2 0.0184(8) 0.0215(8) 0.0167(8) -0.0035(7) -0.0043(6) -0.0022(7)
C3 0.0198(9) 0.0246(9) 0.0189(9) -0.0034(7) -0.0046(7) -0.0065(7)
C4 0.0255(9) 0.0199(8) 0.0181(9) -0.0042(7) -0.0048(7) -0.0046(7)
C5 0.0240(9) 0.0216(9) 0.0204(9) -0.0019(7) -0.0058(7) 0.0002(7)
C6 0.0174(9) 0.0257(9) 0.0207(9) -0.0025(7) -0.0036(7) -0.0036(7)
C7 0.0152(8) 0.0272(9) 0.0215(9) -0.0028(7) -0.0040(7) -0.0059(7)
C8 0.0193(9) 0.0248(9) 0.0228(9) -0.0066(7) -0.0042(7) -0.0066(7)
C9 0.0163(8) 0.0201(8) 0.0219(9) -0.0032(7) -0.0019(7) -0.0028(7)
C10 0.0197(9) 0.0139(8) 0.0227(9) -0.0020(7) -0.0044(7) 0.0000(7)
C11 0.0246(9) 0.0188(8) 0.0192(9) -0.0056(7) -0.0034(7) -0.0031(7)
C12 0.0275(10) 0.0155(8) 0.0206(9) -0.0057(7) -0.0062(7) -0.0034(7)
C13 0.0197(8) 0.0147(8) 0.0197(9) 0.0010(6) -0.0043(7) -0.0039(6)
C14 0.0172(8) 0.0177(8) 0.0172(8) 0.0000(6) -0.0043(6) -0.0057(6)
C15 0.0177(8) 0.0156(8) 0.0181(8) -0.0007(6) -0.0032(6) -0.0046(6)
C16 0.0152(8) 0.0185(8) 0.0181(8) 0.0021(6) -0.0025(6) -0.0047(6)
C17 0.0192(8) 0.0233(9) 0.0186(9) 0.0009(7) -0.0066(7) -0.0077(7)
C18 0.0248(9) 0.0182(8) 0.0197(9) -0.0025(7) -0.0056(7) -0.0077(7)
C19 0.0268(10) 0.0139(8) 0.0234(9) -0.0042(7) -0.0089(8) -0.0024(7)
C20 0.0278(10) 0.0192(9) 0.0262(10) -0.0023(7) -0.0106(8) -0.0065(7)
C21 0.0311(11) 0.0225(9) 0.0248(10) -0.0067(8) -0.0044(8) 0.0017(8)
C22 0.0340(11) 0.0269(10) 0.0208(10) -0.0053(8) -0.0037(8) -0.0032(8)
C23 0.0220(9) 0.0281(10) 0.0211(9) 0.0020(8) -0.0024(8) -0.0026(8)
C24 0.0149(8) 0.0262(9) 0.0279(10) 0.0025(8) -0.0033(7) -0.0034(7)
C25 0.0313(10) 0.0225(9) 0.0232(10) -0.0026(7) -0.0075(8) -0.0065(8)
C26 0.0466(14) 0.0226(10) 0.0317(12) 0.0042(9) -0.0092(10) -0.0099(9)
C27 0.0157(8) 0.0220(8) 0.0173(8) 0.0009(7) -0.0006(6) -0.0044(7)
C28 0.0266(11) 0.0232(9) 0.0334(12) -0.0044(8) -0.0105(9) 0.0041(8)
P1 0.0224(2) 0.0221(2) 0.0195(2) -0.00299(18) -0.00133(18) -0.00148(18)
F1 0.0656(10) 0.0299(7) 0.0451(8) -0.0066(6) 0.0221(7) -0.0214(7)
F2 0.0309(6) 0.0302(6) 0.0270(6) -0.0104(5) -0.0008(5) -0.0020(5)
F3 0.0378(7) 0.0559(8) 0.0284(7) -0.0123(6) 0.0024(5) -0.0276(6)
F4 0.0432(7) 0.0328(6) 0.0295(7) -0.0128(5) 0.0027(5) -0.0065(5)
F5 0.0583(10) 0.0699(10) 0.0338(8) -0.0135(7) -0.0200(7) 0.0360(8)
F6 0.0336(7) 0.0457(7) 0.0460(8) -0.0054(6) -0.0204(6) -0.0009(6)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O11 2.6845(13) 2_756 ?
K1 O2 2.7323(13) . ?
K1 O7 2.7470(13) . ?
K1 O6 2.8097(13) . ?
K1 O3 2.8429(12) . ?
K1 O5 2.9314(12) . ?
K1 O8 2.9427(13) . ?
K1 O1 2.9545(13) . ?
K1 O4 2.9707(13) . ?
K1 C8 3.4083(19) . ?
K1 C10 3.5259(18) . ?
O1 C1 1.359(2) . ?
O1 C7 1.443(2) . ?
O2 C8 1.422(2) . ?
O2 C9 1.433(2) . ?
O3 C11 1.422(2) . ?
O3 C10 1.430(2) . ?
O4 C13 1.366(2) . ?
O4 C12 1.438(2) . ?
O5 C14 1.373(2) . ?
O5 C19 1.438(2) . ?
O6 C20 1.424(2) . ?
O6 C21 1.428(2) . ?
O7 C22 1.418(2) . ?
O7 C23 1.424(2) . ?
O8 C2 1.382(2) . ?
O8 C24 1.450(2) . ?
O9 C25 1.200(2) . ?
O10 C25 1.343(2) . ?
O10 C26 1.447(2) . ?
O11 C27 1.209(2) . ?
O11 K1 2.6845(13) 2_756 ?
O12 C27 1.341(2) . ?
O12 C28 1.439(2) . ?
C1 C6 1.393(3) . ?
C1 C2 1.405(2) . ?
C2 C3 1.381(2) . ?
C3 C4 1.404(3) . ?
C3 H3 0.94(2) . ?
C4 C5 1.391(3) . ?
C4 C25 1.486(3) . ?
C5 C6 1.387(3) . ?
C5 H5 0.94(2) . ?
C6 H6 0.92(2) . ?
C7 C8 1.508(3) . ?
C7 H7A 0.98(2) . ?
C7 H7B 0.96(2) . ?
C8 H8A 0.95(2) . ?
C8 H8B 0.98(2) . ?
C9 C10 1.523(2) . ?
C9 H9A 0.96(2) . ?
C9 H9B 0.954(19) . ?
C10 H10A 0.98(2) . ?
C10 H10B 0.99(2) . ?
C11 C12 1.501(3) . ?
C11 H11A 0.97(2) . ?
C11 H11B 0.94(2) . ?
C12 H12A 0.98(2) . ?
C12 H12B 0.99(2) . ?
C13 C18 1.386(2) . ?
C13 C14 1.411(2) . ?
C14 C15 1.377(2) . ?
C15 C16 1.402(2) . ?
C15 H15 0.98(2) . ?
C16 C17 1.387(2) . ?
C16 C27 1.484(2) . ?
C17 C18 1.392(3) . ?
C17 H17 0.97(2) . ?
C18 H18 0.93(2) . ?
C19 C20 1.508(3) . ?
C19 H19A 0.96(2) . ?
C19 H19B 1.000(19) . ?
C20 H20A 0.96(2) . ?
C20 H20B 0.98(2) . ?
C21 C22 1.503(3) . ?
C21 H21A 0.96(3) . ?
C21 H21B 0.96(2) . ?
C22 H22A 0.99(3) . ?
C22 H22B 0.96(2) . ?
C23 C24 1.495(3) . ?
C23 H23A 0.95(2) . ?
C23 H23B 0.97(2) . ?
C24 H24A 0.95(2) . ?
C24 H24B 0.96(2) . ?
C26 H26A 0.96(3) . ?
C26 H26B 0.99(3) . ?
C26 H26C 0.96(3) . ?
C28 H28A 0.95(3) . ?
C28 H28B 0.96(3) . ?
C28 H28C 0.94(3) . ?
P1 F6 1.5881(13) . ?
P1 F1 1.5930(13) . ?
P1 F3 1.5961(13) . ?
P1 F2 1.5982(12) . ?
P1 F5 1.6029(14) . ?
P1 F4 1.6053(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 K1 O2 160.86(4) 2_756 . ?
O11 K1 O7 71.07(4) 2_756 . ?
O2 K1 O7 117.99(4) . . ?
O11 K1 O6 90.31(4) 2_756 . ?
O2 K1 O6 81.34(4) . . ?
O7 K1 O6 60.08(4) . . ?
O11 K1 O3 118.59(4) 2_756 . ?
O2 K1 O3 61.94(4) . . ?
O7 K1 O3 152.66(4) . . ?
O6 K1 O3 139.28(4) . . ?
O11 K1 O5 71.05(4) 2_756 . ?
O2 K1 O5 89.89(4) . . ?
O7 K1 O5 107.06(4) . . ?
O6 K1 O5 60.42(4) . . ?
O3 K1 O5 100.27(4) . . ?
O11 K1 O8 87.97(4) 2_756 . ?
O2 K1 O8 111.16(4) . . ?
O7 K1 O8 60.62(4) . . ?
O6 K1 O8 117.59(4) . . ?
O3 K1 O8 93.08(4) . . ?
O5 K1 O8 158.66(4) . . ?
O11 K1 O1 138.84(4) 2_756 . ?
O2 K1 O1 59.64(4) . . ?
O7 K1 O1 76.86(4) . . ?
O6 K1 O1 95.56(4) . . ?
O3 K1 O1 81.29(4) . . ?
O5 K1 O1 144.94(4) . . ?
O8 K1 O1 53.40(3) . . ?
O11 K1 O4 78.60(4) 2_756 . ?
O2 K1 O4 88.29(4) . . ?
O7 K1 O4 147.89(4) . . ?
O6 K1 O4 110.89(4) . . ?
O3 K1 O4 54.77(3) . . ?
O5 K1 O4 51.38(3) . . ?
O8 K1 O4 129.61(4) . . ?
O1 K1 O4 135.00(4) . . ?
O11 K1 C8 160.89(4) 2_756 . ?
O2 K1 C8 23.66(4) . . ?
O7 K1 C8 94.85(4) . . ?
O6 K1 C8 71.16(4) . . ?
O3 K1 C8 79.86(4) . . ?
O5 K1 C8 102.27(4) . . ?
O8 K1 C8 96.39(4) . . ?
O1 K1 C8 43.10(4) . . ?
O4 K1 C8 111.80(4) . . ?
O11 K1 C10 140.97(4) 2_756 . ?
O2 K1 C10 43.57(4) . . ?
O7 K1 C10 138.08(4) . . ?
O6 K1 C10 124.90(4) . . ?
O3 K1 C10 22.88(4) . . ?
O5 K1 C10 109.48(4) . . ?
O8 K1 C10 89.15(4) . . ?
O1 K1 C10 61.44(4) . . ?
O4 K1 C10 73.56(4) . . ?
C8 K1 C10 57.93(4) . . ?
C1 O1 C7 116.72(14) . . ?
C1 O1 K1 124.76(10) . . ?
C7 O1 K1 114.98(10) . . ?
C8 O2 C9 115.17(14) . . ?
C8 O2 K1 105.90(10) . . ?
C9 O2 K1 119.22(10) . . ?
C11 O3 C10 112.15(13) . . ?
C11 O3 K1 125.68(10) . . ?
C10 O3 K1 106.49(10) . . ?
C13 O4 C12 117.95(13) . . ?
C13 O4 K1 111.43(10) . . ?
C12 O4 K1 116.99(10) . . ?
C14 O5 C19 116.40(13) . . ?
C14 O5 K1 113.24(9) . . ?
C19 O5 K1 115.36(10) . . ?
C20 O6 C21 114.26(14) . . ?
C20 O6 K1 112.52(10) . . ?
C21 O6 K1 109.62(11) . . ?
C22 O7 C23 113.18(14) . . ?
C22 O7 K1 119.42(11) . . ?
C23 O7 K1 120.62(11) . . ?
C2 O8 C24 115.08(14) . . ?
C2 O8 K1 124.02(10) . . ?
C24 O8 K1 105.34(10) . . ?
C25 O10 C26 115.42(17) . . ?
C27 O11 K1 146.78(12) . 2_756 ?
C27 O12 C28 116.76(14) . . ?
O1 C1 C6 124.49(16) . . ?
O1 C1 C2 115.99(15) . . ?
C6 C1 C2 119.51(16) . . ?
C3 C2 O8 121.83(16) . . ?
C3 C2 C1 120.20(16) . . ?
O8 C2 C1 117.89(15) . . ?
C2 C3 C4 120.16(17) . . ?
C2 C3 H3 119.0(13) . . ?
C4 C3 H3 120.8(13) . . ?
C5 C4 C3 119.31(17) . . ?
C5 C4 C25 122.23(17) . . ?
C3 C4 C25 118.38(17) . . ?
C6 C5 C4 120.70(17) . . ?
C6 C5 H5 119.2(14) . . ?
C4 C5 H5 120.0(14) . . ?
C5 C6 C1 120.02(17) . . ?
C5 C6 H6 118.5(14) . . ?
C1 C6 H6 121.4(14) . . ?
O1 C7 C8 107.10(15) . . ?
O1 C7 H7A 110.4(13) . . ?
C8 C7 H7A 109.6(13) . . ?
O1 C7 H7B 109.6(13) . . ?
C8 C7 H7B 112.6(13) . . ?
H7A C7 H7B 107.6(18) . . ?
O2 C8 C7 113.63(14) . . ?
O2 C8 K1 50.44(8) . . ?
C7 C8 K1 92.91(10) . . ?
O2 C8 H8A 107.1(13) . . ?
C7 C8 H8A 107.5(13) . . ?
K1 C8 H8A 70.7(12) . . ?
O2 C8 H8B 111.1(12) . . ?
C7 C8 H8B 106.8(12) . . ?
K1 C8 H8B 158.2(12) . . ?
H8A C8 H8B 110.6(17) . . ?
O2 C9 C10 111.00(14) . . ?
O2 C9 H9A 106.4(12) . . ?
C10 C9 H9A 110.2(12) . . ?
O2 C9 H9B 114.2(12) . . ?
C10 C9 H9B 107.5(11) . . ?
H9A C9 H9B 107.6(16) . . ?
O3 C10 C9 111.92(14) . . ?
O3 C10 K1 50.64(8) . . ?
C9 C10 K1 82.46(9) . . ?
O3 C10 H10A 111.4(11) . . ?
C9 C10 H10A 108.6(12) . . ?
K1 C10 H10A 162.0(11) . . ?
O3 C10 H10B 106.3(11) . . ?
C9 C10 H10B 109.4(11) . . ?
K1 C10 H10B 79.1(11) . . ?
H10A C10 H10B 109.2(16) . . ?
O3 C11 C12 108.55(15) . . ?
O3 C11 H11A 110.4(12) . . ?
C12 C11 H11A 110.2(12) . . ?
O3 C11 H11B 111.0(12) . . ?
C12 C11 H11B 108.5(12) . . ?
H11A C11 H11B 108.2(17) . . ?
O4 C12 C11 105.87(14) . . ?
O4 C12 H12A 112.7(11) . . ?
C11 C12 H12A 108.9(11) . . ?
O4 C12 H12B 110.7(11) . . ?
C11 C12 H12B 112.0(11) . . ?
H12A C12 H12B 106.7(16) . . ?
O4 C13 C18 125.23(15) . . ?
O4 C13 C14 114.31(15) . . ?
C18 C13 C14 120.46(16) . . ?
O5 C14 C15 125.12(15) . . ?
O5 C14 C13 115.18(15) . . ?
C15 C14 C13 119.69(16) . . ?
C14 C15 C16 119.54(16) . . ?
C14 C15 H15 121.3(12) . . ?
C16 C15 H15 119.0(12) . . ?
C17 C16 C15 120.70(16) . . ?
C17 C16 C27 119.29(16) . . ?
C15 C16 C27 119.97(16) . . ?
C16 C17 C18 119.89(16) . . ?
C16 C17 H17 120.5(13) . . ?
C18 C17 H17 119.6(13) . . ?
C13 C18 C17 119.58(16) . . ?
C13 C18 H18 119.7(13) . . ?
C17 C18 H18 120.8(13) . . ?
O5 C19 C20 107.73(14) . . ?
O5 C19 H19A 110.6(12) . . ?
C20 C19 H19A 111.5(12) . . ?
O5 C19 H19B 109.1(11) . . ?
C20 C19 H19B 110.3(11) . . ?
H19A C19 H19B 107.5(16) . . ?
O6 C20 C19 114.29(15) . . ?
O6 C20 H20A 108.0(13) . . ?
C19 C20 H20A 109.1(13) . . ?
O6 C20 H20B 105.3(13) . . ?
C19 C20 H20B 111.4(13) . . ?
H20A C20 H20B 108.5(18) . . ?
O6 C21 C22 107.96(16) . . ?
O6 C21 H21A 110.2(15) . . ?
C22 C21 H21A 109.2(15) . . ?
O6 C21 H21B 110.9(13) . . ?
C22 C21 H21B 108.5(13) . . ?
H21A C21 H21B 110.1(19) . . ?
O7 C22 C21 108.04(16) . . ?
O7 C22 H22A 109.0(14) . . ?
C21 C22 H22A 110.3(14) . . ?
O7 C22 H22B 110.4(13) . . ?
C21 C22 H22B 108.7(13) . . ?
H22A C22 H22B 110.4(19) . . ?
O7 C23 C24 107.95(16) . . ?
O7 C23 H23A 110.9(13) . . ?
C24 C23 H23A 109.5(13) . . ?
O7 C23 H23B 111.9(13) . . ?
C24 C23 H23B 110.5(13) . . ?
H23A C23 H23B 106.1(18) . . ?
O8 C24 C23 111.75(15) . . ?
O8 C24 H24A 111.1(12) . . ?
C23 C24 H24A 108.9(12) . . ?
O8 C24 H24B 104.8(12) . . ?
C23 C24 H24B 110.9(12) . . ?
H24A C24 H24B 109.3(17) . . ?
O9 C25 O10 122.86(18) . . ?
O9 C25 C4 124.93(18) . . ?
O10 C25 C4 112.17(16) . . ?
O10 C26 H26A 111.7(18) . . ?
O10 C26 H26B 105.7(17) . . ?
H26A C26 H26B 106(2) . . ?
O10 C26 H26C 108.2(15) . . ?
H26A C26 H26C 115(2) . . ?
H26B C26 H26C 109(2) . . ?
O11 C27 O12 123.37(16) . . ?
O11 C27 C16 125.17(16) . . ?
O12 C27 C16 111.46(15) . . ?
O12 C28 H28A 109.8(14) . . ?
O12 C28 H28B 103.1(15) . . ?
H28A C28 H28B 114(2) . . ?
O12 C28 H28C 110.1(15) . . ?
H28A C28 H28C 112(2) . . ?
H28B C28 H28C 107(2) . . ?
F6 P1 F1 90.15(9) . . ?
F6 P1 F3 89.97(8) . . ?
F1 P1 F3 179.73(8) . . ?
F6 P1 F2 90.29(7) . . ?
F1 P1 F2 89.98(7) . . ?
F3 P1 F2 90.25(7) . . ?
F6 P1 F5 179.39(9) . . ?
F1 P1 F5 90.39(10) . . ?
F3 P1 F5 89.48(9) . . ?
F2 P1 F5 89.43(7) . . ?
F6 P1 F4 90.28(7) . . ?
F1 P1 F4 90.23(7) . . ?
F3 P1 F4 89.53(7) . . ?
F2 P1 F4 179.39(8) . . ?
F5 P1 F4 90.00(8) . . ?

_diffrn_measured_fraction_theta_max 0.934
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.934
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.055

data_cs525
_database_code_depnum_ccdc_archive 'CCDC 265206'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            HW-trans-24C8
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H36 O12'
_chemical_formula_sum            'C28 H36 O12'
_chemical_formula_weight         564.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.8926(14)
_cell_length_b                   12.4235(11)
_cell_length_c                   8.2043(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.243(9)
_cell_angle_gamma                90.00
_cell_volume                     1366.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2865
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      23.3

_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.066
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             600
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2'
_diffrn_detector                 CCD
_diffrn_detector_type            'Oxford Diffraction Sapphire 2 CCD'
_diffrn_source_voltage           50
_diffrn_source_current           40
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <2%
_diffrn_reflns_number            8078
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         27.57
_reflns_number_total             3162
_reflns_number_gt                2411
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.10 beta (release 25.09.2003 CrysAlis171 VC++)
(compiled Sep 25 2003,17:01:25)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.10 beta (release 25.09.2003 CrysAlis171 VC++)
(compiled Sep 25 2003,17:01:25)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.10 beta (release 25.09.2003 CrysAlis171 VC++)
(compiled Sep 25 2003,17:01:25)
;

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1313P)^2^+0.2020P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3162
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.2109
_refine_ls_wR_factor_gt          0.1886
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.73535(11) 0.79696(12) 0.16967(18) 0.0214(4) Uani 1 1 d . . .
O2 O 0.52104(12) 0.73255(15) 0.1453(2) 0.0324(4) Uani 1 1 d . . .
O3 O 0.33518(11) 0.85119(12) 0.06535(19) 0.0241(4) Uani 1 1 d . . .
O4 O 0.20214(11) 1.02772(12) -0.06483(19) 0.0218(4) Uani 1 1 d . . .
O5 O 1.18478(12) 0.87043(13) 0.5775(2) 0.0263(4) Uani 1 1 d . . .
O6 O 1.16237(12) 1.00899(14) 0.3960(2) 0.0285(4) Uani 1 1 d . . .
C1 C 0.83105(16) 0.82313(17) 0.2463(3) 0.0186(4) Uani 1 1 d . . .
C2 C 0.89459(17) 0.76288(18) 0.3725(3) 0.0228(5) Uani 1 1 d . . .
H2 H 0.8715 0.6980 0.4106 0.027 Uiso 1 1 calc R . .
C3 C 0.99194(16) 0.79735(17) 0.4431(3) 0.0224(5) Uani 1 1 d . . .
H3 H 1.0348 0.7566 0.5307 0.027 Uiso 1 1 calc R . .
C4 C 1.02673(16) 0.89141(17) 0.3857(2) 0.0204(5) Uani 1 1 d . . .
C5 C 0.96295(15) 0.95223(17) 0.2586(3) 0.0191(4) Uani 1 1 d . . .
H5 H 0.9864 1.0164 0.2190 0.023 Uiso 1 1 calc R . .
C6 C 0.86587(15) 0.91864(16) 0.1907(2) 0.0171(4) Uani 1 1 d . . .
C7 C 0.69985(16) 0.69358(16) 0.2086(3) 0.0207(5) Uani 1 1 d . . .
H7A H 0.6980 0.6918 0.3284 0.025 Uiso 1 1 calc R . .
H7B H 0.7455 0.6361 0.1909 0.025 Uiso 1 1 calc R . .
C8 C 0.59711(17) 0.67502(18) 0.0957(3) 0.0248(5) Uani 1 1 d . . .
H8A H 0.5963 0.6964 -0.0209 0.030 Uiso 1 1 calc R . .
H8B H 0.5819 0.5971 0.0944 0.030 Uiso 1 1 calc R . .
C9 C 0.50960(19) 0.8401(2) 0.0853(4) 0.0341(6) Uani 1 1 d . . .
H9A H 0.4910 0.8409 -0.0398 0.041 Uiso 1 1 calc R . .
H9B H 0.5731 0.8800 0.1266 0.041 Uiso 1 1 calc R . .
C10 C 0.42952(19) 0.8917(2) 0.1490(4) 0.0435(7) Uani 1 1 d . . .
H10A H 0.4424 0.8783 0.2718 0.052 Uiso 1 1 calc R . .
H10B H 0.4306 0.9705 0.1314 0.052 Uiso 1 1 calc R . .
C11 C 0.25639(17) 0.88797(18) 0.1329(3) 0.0230(5) Uani 1 1 d . . .
H11A H 0.2813 0.9462 0.2155 0.028 Uiso 1 1 calc R . .
H11B H 0.2333 0.8281 0.1927 0.028 Uiso 1 1 calc R . .
C12 C 0.17084(16) 0.92903(17) -0.0054(3) 0.0217(5) Uani 1 1 d . . .
H12A H 0.1528 0.8760 -0.0984 0.026 Uiso 1 1 calc R . .
H12B H 0.1118 0.9414 0.0384 0.026 Uiso 1 1 calc R . .
C13 C 1.13002(16) 0.93066(17) 0.4522(3) 0.0209(5) Uani 1 1 d . . .
C14 C 1.28889(16) 0.9045(2) 0.6413(3) 0.0280(5) Uani 1 1 d . . .
H14A H 1.3243 0.8923 0.5542 0.042 Uiso 1 1 calc R . .
H14B H 1.3208 0.8628 0.7424 0.042 Uiso 1 1 calc R . .
H14C H 1.2912 0.9812 0.6698 0.042 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0201(8) 0.0200(8) 0.0226(8) 0.0025(6) 0.0031(6) 0.0017(6)
O2 0.0219(8) 0.0436(10) 0.0325(9) 0.0133(8) 0.0086(7) 0.0105(7)
O3 0.0197(8) 0.0270(9) 0.0253(8) -0.0032(6) 0.0051(6) 0.0011(6)
O4 0.0209(8) 0.0195(8) 0.0231(8) 0.0033(6) 0.0025(6) 0.0000(6)
O5 0.0192(8) 0.0298(9) 0.0264(8) 0.0034(7) -0.0002(6) 0.0004(6)
O6 0.0237(8) 0.0323(9) 0.0305(9) 0.0039(7) 0.0087(7) -0.0025(7)
C1 0.0206(10) 0.0181(10) 0.0180(9) -0.0016(8) 0.0065(8) 0.0013(8)
C2 0.0251(11) 0.0230(11) 0.0210(10) 0.0043(8) 0.0075(9) 0.0023(9)
C3 0.0215(10) 0.0246(11) 0.0198(10) 0.0031(8) 0.0035(8) 0.0029(8)
C4 0.0206(11) 0.0249(11) 0.0151(9) -0.0018(8) 0.0035(8) 0.0052(8)
C5 0.0216(10) 0.0178(10) 0.0193(10) 0.0007(8) 0.0079(8) 0.0023(8)
C6 0.0189(10) 0.0166(10) 0.0160(9) -0.0020(7) 0.0052(8) 0.0044(8)
C7 0.0227(11) 0.0162(10) 0.0236(10) 0.0036(8) 0.0067(8) 0.0005(8)
C8 0.0224(11) 0.0210(11) 0.0295(11) 0.0039(9) 0.0042(9) 0.0003(9)
C9 0.0244(12) 0.0275(13) 0.0475(15) -0.0019(11) 0.0043(11) -0.0020(10)
C10 0.0241(13) 0.0395(15) 0.0599(18) -0.0198(13) -0.0015(12) 0.0004(11)
C11 0.0244(11) 0.0221(11) 0.0238(10) 0.0026(8) 0.0086(9) 0.0050(8)
C12 0.0226(11) 0.0186(10) 0.0246(10) 0.0027(8) 0.0075(9) 0.0021(8)
C13 0.0195(10) 0.0256(11) 0.0184(9) -0.0026(8) 0.0063(8) 0.0036(8)
C14 0.0177(11) 0.0372(13) 0.0262(11) -0.0012(10) 0.0006(9) 0.0002(9)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.352(3) . ?
O1 C7 1.441(2) . ?
O2 C9 1.419(3) . ?
O2 C8 1.421(3) . ?
O3 C10 1.403(3) . ?
O3 C11 1.426(3) . ?
O4 C6 1.375(2) 3_675 ?
O4 C12 1.429(3) . ?
O5 C13 1.336(3) . ?
O5 C14 1.465(3) . ?
O6 C13 1.213(3) . ?
C1 C2 1.390(3) . ?
C1 C6 1.402(3) . ?
C2 C3 1.391(3) . ?
C3 C4 1.393(3) . ?
C4 C5 1.399(3) . ?
C4 C13 1.477(3) . ?
C5 C6 1.381(3) . ?
C6 O4 1.375(2) 3_675 ?
C7 C8 1.501(3) . ?
C9 C10 1.492(4) . ?
C11 C12 1.500(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C7 117.59(16) . . ?
C9 O2 C8 113.46(18) . . ?
C10 O3 C11 114.13(18) . . ?
C6 O4 C12 117.49(16) 3_675 . ?
C13 O5 C14 114.94(18) . . ?
O1 C1 C2 124.82(19) . . ?
O1 C1 C6 115.69(18) . . ?
C2 C1 C6 119.5(2) . . ?
C1 C2 C3 120.1(2) . . ?
C2 C3 C4 120.2(2) . . ?
C3 C4 C5 119.8(2) . . ?
C3 C4 C13 122.81(19) . . ?
C5 C4 C13 117.4(2) . . ?
C6 C5 C4 119.8(2) . . ?
O4 C6 C5 124.18(19) 3_675 . ?
O4 C6 C1 115.26(18) 3_675 . ?
C5 C6 C1 120.55(19) . . ?
O1 C7 C8 108.99(17) . . ?
O2 C8 C7 113.83(19) . . ?
O2 C9 C10 108.0(2) . . ?
O3 C10 C9 111.2(2) . . ?
O3 C11 C12 110.60(17) . . ?
O4 C12 C11 107.35(17) . . ?
O6 C13 O5 123.3(2) . . ?
O6 C13 C4 123.1(2) . . ?
O5 C13 C4 113.60(19) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 O1 C1 C2 -7.0(3) . . . . ?
C7 O1 C1 C6 173.04(17) . . . . ?
O1 C1 C2 C3 -179.90(19) . . . . ?
C6 C1 C2 C3 0.1(3) . . . . ?
C1 C2 C3 C4 -1.1(3) . . . . ?
C2 C3 C4 C5 1.0(3) . . . . ?
C2 C3 C4 C13 -178.26(19) . . . . ?
C3 C4 C5 C6 0.0(3) . . . . ?
C13 C4 C5 C6 179.34(18) . . . . ?
C4 C5 C6 O4 -179.53(18) . . . 3_675 ?
C4 C5 C6 C1 -1.0(3) . . . . ?
O1 C1 C6 O4 -0.4(3) . . . 3_675 ?
C2 C1 C6 O4 179.60(17) . . . 3_675 ?
O1 C1 C6 C5 -179.05(17) . . . . ?
C2 C1 C6 C5 1.0(3) . . . . ?
C1 O1 C7 C8 -173.17(17) . . . . ?
C9 O2 C8 C7 83.9(2) . . . . ?
O1 C7 C8 O2 -77.1(2) . . . . ?
C8 O2 C9 C10 -178.8(2) . . . . ?
C11 O3 C10 C9 173.3(2) . . . . ?
O2 C9 C10 O3 -72.0(3) . . . . ?
C10 O3 C11 C12 130.6(2) . . . . ?
C6 O4 C12 C11 -178.68(16) 3_675 . . . ?
O3 C11 C12 O4 -70.6(2) . . . . ?
C14 O5 C13 O6 -1.3(3) . . . . ?
C14 O5 C13 C4 177.47(17) . . . . ?
C3 C4 C13 O6 175.6(2) . . . . ?
C5 C4 C13 O6 -3.7(3) . . . . ?
C3 C4 C13 O5 -3.2(3) . . . . ?
C5 C4 C13 O5 177.54(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.57
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.141

data_cs535
_database_code_depnum_ccdc_archive 'CCDC 265207'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            '[K-trans24c8][PF6]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H36 F6 K O12 P'
_chemical_formula_sum            'C28 H36 F6 K O12 P'
_chemical_formula_weight         748.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.840(2)
_cell_length_b                   19.447(3)
_cell_length_c                   19.410(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.429(11)
_cell_angle_gamma                90.00
_cell_volume                     6354.4(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3209
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      22.64

_exptl_crystal_description       trapezoid
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3104
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <2%
_diffrn_reflns_number            22885
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         30.12
_reflns_number_total             9339
_reflns_number_gt                7305
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction)'
_computing_cell_refinement       'CrysAlis (Oxford Diffraction)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+3.3164P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9339
_refine_ls_number_parameters     436
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.1926
_refine_ls_wR_factor_gt          0.1704
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K K 0.69587(2) 0.08281(2) 0.07548(2) 0.01506(12) Uani 1 1 d . . .
P1 P 0.5000 0.36079(4) 0.2500 0.01860(17) Uani 1 2 d S . .
P2 P 0.5000 0.21136(5) 0.7500 0.02501(19) Uani 1 2 d S . .
F1 F 0.44360(9) 0.36046(11) 0.18293(8) 0.0440(5) Uani 1 1 d . . .
F2 F 0.5513(2) 0.41744(17) 0.21578(10) 0.1148(15) Uani 1 1 d . . .
F3 F 0.4492(2) 0.30441(17) 0.28467(12) 0.1129(14) Uani 1 1 d . . .
F4 F 0.48322(14) 0.20963(11) 0.83031(9) 0.0547(5) Uani 1 1 d . . .
F5 F 0.4362(2) 0.2664(2) 0.73926(18) 0.1320(18) Uani 1 1 d . . .
F6 F 0.5628(2) 0.15162(19) 0.75899(13) 0.1142(14) Uani 1 1 d . . .
O1 O 0.86577(8) 0.07997(8) 0.12113(7) 0.0168(3) Uani 1 1 d . . .
O2 O 0.75299(8) -0.00160(8) 0.18032(7) 0.0170(3) Uani 1 1 d . . .
O3 O 0.68068(9) -0.06122(8) 0.06368(8) 0.0175(3) Uani 1 1 d . . .
O4 O 0.54140(8) 0.01613(7) 0.08448(8) 0.0161(3) Uani 1 1 d . . .
O5 O 1.19035(9) 0.16808(9) 0.03806(8) 0.0209(3) Uani 1 1 d . . .
O6 O 1.16516(10) 0.12971(10) 0.14454(8) 0.0267(4) Uani 1 1 d . . .
O7 O 0.53692(8) 0.14537(7) 0.06613(7) 0.0156(3) Uani 1 1 d . . .
O8 O 0.66159(9) 0.20052(8) -0.00365(7) 0.0182(3) Uani 1 1 d . . .
O9 O 0.68300(9) 0.07024(8) -0.06509(8) 0.0169(3) Uani 1 1 d . . .
O10 O 0.83926(8) 0.06140(8) -0.01024(7) 0.0169(3) Uani 1 1 d . . .
O11 O 0.32002(9) 0.22948(8) 0.22293(8) 0.0198(3) Uani 1 1 d . . .
O12 O 0.32808(10) 0.15615(9) 0.31158(8) 0.0225(3) Uani 1 1 d . . .
C1 C 0.92904(12) 0.09023(10) 0.07967(10) 0.0144(4) Uani 1 1 d . . .
C2 C 1.00369(12) 0.10904(11) 0.10354(10) 0.0163(4) Uani 1 1 d . . .
H2 H 1.0140 0.1138 0.1516 0.020 Uiso 1 1 calc R . .
C3 C 1.06423(12) 0.12115(10) 0.05699(10) 0.0155(4) Uani 1 1 d . . .
C4 C 1.04898(12) 0.11436(10) -0.01330(10) 0.0168(4) Uani 1 1 d . . .
H4 H 1.0897 0.1240 -0.0449 0.020 Uiso 1 1 calc R . .
C5 C 0.97447(12) 0.09361(11) -0.03768(10) 0.0162(4) Uani 1 1 d . . .
H5 H 0.9647 0.0878 -0.0858 0.019 Uiso 1 1 calc R . .
C6 C 0.91448(11) 0.08141(10) 0.00824(10) 0.0146(4) Uani 1 1 d . . .
C7 C 0.88565(12) 0.05260(12) 0.18847(10) 0.0192(4) Uani 1 1 d . . .
H7A H 0.9153 0.0873 0.2161 0.023 Uiso 1 1 calc R . .
H7B H 0.9195 0.0113 0.1841 0.023 Uiso 1 1 calc R . .
C8 C 0.80928(12) 0.03401(12) 0.22349(10) 0.0196(4) Uani 1 1 d . . .
H8A H 0.8223 0.0049 0.2641 0.024 Uiso 1 1 calc R . .
H8B H 0.7844 0.0767 0.2404 0.024 Uiso 1 1 calc R . .
C9 C 0.78273(13) -0.06291(12) 0.15031(12) 0.0217(4) Uani 1 1 d . . .
H9A H 0.8100 -0.0914 0.1859 0.026 Uiso 1 1 calc R . .
H9B H 0.8212 -0.0515 0.1143 0.026 Uiso 1 1 calc R . .
C10 C 0.71322(14) -0.10140(11) 0.11919(12) 0.0220(4) Uani 1 1 d . . .
H10A H 0.7307 -0.1467 0.1019 0.026 Uiso 1 1 calc R . .
H10B H 0.6726 -0.1091 0.1543 0.026 Uiso 1 1 calc R . .
C11 C 0.60359(13) -0.08273(11) 0.04107(11) 0.0185(4) Uani 1 1 d . . .
H11A H 0.6020 -0.1336 0.0395 0.022 Uiso 1 1 calc R . .
H11B H 0.5931 -0.0654 -0.0063 0.022 Uiso 1 1 calc R . .
C12 C 0.53946(12) -0.05729(10) 0.08734(11) 0.0184(4) Uani 1 1 d . . .
H12A H 0.4869 -0.0746 0.0712 0.022 Uiso 1 1 calc R . .
H12B H 0.5494 -0.0734 0.1352 0.022 Uiso 1 1 calc R . .
C13 C 1.14358(12) 0.13961(11) 0.08559(10) 0.0172(4) Uani 1 1 d . . .
C14 C 1.26937(12) 0.18401(12) 0.06311(12) 0.0218(4) Uani 1 1 d . . .
H14A H 1.2665 0.2157 0.1022 0.033 Uiso 1 1 calc R . .
H14B H 1.2993 0.2055 0.0262 0.033 Uiso 1 1 calc R . .
H14C H 1.2962 0.1416 0.0780 0.033 Uiso 1 1 calc R . .
C15 C 0.49051(11) 0.12219(10) 0.11799(10) 0.0134(3) Uani 1 1 d . . .
C16 C 0.44373(11) 0.16278(10) 0.15876(10) 0.0145(4) Uani 1 1 d . . .
H16 H 0.4421 0.2112 0.1524 0.017 Uiso 1 1 calc R . .
C17 C 0.39864(11) 0.13148(10) 0.20963(10) 0.0144(4) Uani 1 1 d . . .
C18 C 0.39955(12) 0.06109(11) 0.21837(10) 0.0160(4) Uani 1 1 d . . .
H18 H 0.3689 0.0407 0.2533 0.019 Uiso 1 1 calc R . .
C19 C 0.44526(12) 0.01990(10) 0.17614(10) 0.0156(4) Uani 1 1 d . . .
H19 H 0.4448 -0.0287 0.1812 0.019 Uiso 1 1 calc R . .
C20 C 0.49151(11) 0.05041(10) 0.12660(10) 0.0138(3) Uani 1 1 d . . .
C21 C 0.54105(13) 0.21797(10) 0.05514(11) 0.0187(4) Uani 1 1 d . . .
H21A H 0.5709 0.2405 0.0935 0.022 Uiso 1 1 calc R . .
H21B H 0.4871 0.2380 0.0519 0.022 Uiso 1 1 calc R . .
C22 C 0.58328(14) 0.22743(11) -0.01157(11) 0.0204(4) Uani 1 1 d . . .
H22A H 0.5543 0.2030 -0.0492 0.024 Uiso 1 1 calc R . .
H22B H 0.5855 0.2769 -0.0235 0.024 Uiso 1 1 calc R . .
C23 C 0.70074(13) 0.19367(11) -0.06786(11) 0.0199(4) Uani 1 1 d . . .
H23A H 0.7588 0.1910 -0.0591 0.024 Uiso 1 1 calc R . .
H23B H 0.6898 0.2349 -0.0965 0.024 Uiso 1 1 calc R . .
C24 C 0.67331(12) 0.13029(11) -0.10675(10) 0.0173(4) Uani 1 1 d . . .
H24A H 0.6167 0.1355 -0.1207 0.021 Uiso 1 1 calc R . .
H24B H 0.7044 0.1253 -0.1491 0.021 Uiso 1 1 calc R . .
C25 C 0.74019(12) 0.02242(11) -0.08875(11) 0.0178(4) Uani 1 1 d . . .
H25A H 0.7281 0.0117 -0.1378 0.021 Uiso 1 1 calc R . .
H25B H 0.7355 -0.0208 -0.0622 0.021 Uiso 1 1 calc R . .
C26 C 0.82446(12) 0.04812(11) -0.08199(10) 0.0175(4) Uani 1 1 d . . .
H26A H 0.8619 0.0130 -0.0988 0.021 Uiso 1 1 calc R . .
H26B H 0.8311 0.0907 -0.1092 0.021 Uiso 1 1 calc R . .
C27 C 0.34656(12) 0.17263(11) 0.25404(10) 0.0161(4) Uani 1 1 d . . .
C28 C 0.26692(16) 0.27008(14) 0.26282(13) 0.0316(6) Uani 1 1 d . . .
H28A H 0.2199 0.2427 0.2735 0.047 Uiso 1 1 calc R . .
H28B H 0.2507 0.3109 0.2364 0.047 Uiso 1 1 calc R . .
H28C H 0.2939 0.2843 0.3058 0.047 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
K 0.0166(2) 0.0173(2) 0.01131(19) 0.00018(13) 0.00095(14) 0.00003(14)
P1 0.0158(3) 0.0202(4) 0.0198(4) 0.000 0.0007(3) 0.000
P2 0.0261(4) 0.0247(4) 0.0239(4) 0.000 -0.0069(3) 0.000
F1 0.0248(7) 0.0840(14) 0.0230(7) 0.0198(8) -0.0048(6) 0.0074(8)
F2 0.182(3) 0.141(3) 0.0219(9) -0.0121(12) 0.0223(14) -0.139(3)
F3 0.145(3) 0.140(3) 0.0511(13) 0.0589(15) -0.0551(15) -0.120(2)
F4 0.0821(15) 0.0531(12) 0.0289(9) -0.0104(8) 0.0049(9) -0.0116(11)
F5 0.122(3) 0.165(3) 0.111(3) 0.081(2) 0.052(2) 0.113(3)
F6 0.168(3) 0.130(3) 0.0438(13) 0.0130(15) -0.0049(17) 0.111(2)
O1 0.0132(6) 0.0266(8) 0.0106(6) 0.0039(5) 0.0009(5) -0.0002(5)
O2 0.0141(6) 0.0228(7) 0.0141(6) -0.0010(5) 0.0000(5) 0.0005(5)
O3 0.0161(7) 0.0185(7) 0.0178(7) 0.0020(5) -0.0014(5) 0.0004(5)
O4 0.0171(7) 0.0139(6) 0.0176(7) 0.0002(5) 0.0048(5) 0.0008(5)
O5 0.0141(7) 0.0305(8) 0.0179(7) 0.0037(6) -0.0017(5) -0.0063(6)
O6 0.0213(8) 0.0391(10) 0.0194(8) 0.0079(7) -0.0048(6) -0.0053(7)
O7 0.0183(7) 0.0128(6) 0.0159(7) 0.0020(5) 0.0052(5) -0.0002(5)
O8 0.0204(7) 0.0211(7) 0.0134(6) -0.0008(5) 0.0048(5) -0.0029(6)
O9 0.0165(7) 0.0198(7) 0.0146(6) 0.0001(5) 0.0025(5) 0.0006(5)
O10 0.0133(6) 0.0251(7) 0.0122(6) -0.0015(5) 0.0000(5) -0.0035(5)
O11 0.0233(7) 0.0221(7) 0.0141(7) 0.0011(5) 0.0056(5) 0.0057(6)
O12 0.0267(8) 0.0269(8) 0.0142(7) 0.0029(6) 0.0059(6) 0.0011(6)
C1 0.0150(9) 0.0159(9) 0.0124(8) 0.0020(6) 0.0011(7) 0.0006(7)
C2 0.0178(9) 0.0201(9) 0.0110(8) 0.0029(7) -0.0014(7) -0.0005(7)
C3 0.0143(9) 0.0172(9) 0.0150(9) 0.0022(7) -0.0005(7) 0.0004(7)
C4 0.0152(9) 0.0190(9) 0.0162(9) 0.0008(7) 0.0021(7) -0.0002(7)
C5 0.0167(9) 0.0202(9) 0.0118(8) -0.0007(7) 0.0011(7) -0.0013(7)
C6 0.0132(8) 0.0164(9) 0.0141(8) 0.0002(6) -0.0010(7) -0.0003(7)
C7 0.0167(9) 0.0290(11) 0.0117(8) 0.0038(7) -0.0023(7) -0.0024(8)
C8 0.0167(9) 0.0305(11) 0.0117(8) 0.0001(8) -0.0004(7) -0.0027(8)
C9 0.0193(10) 0.0218(10) 0.0240(10) 0.0007(8) -0.0008(8) 0.0046(8)
C10 0.0239(10) 0.0186(9) 0.0232(10) 0.0040(8) -0.0040(8) 0.0020(8)
C11 0.0185(9) 0.0183(9) 0.0187(9) -0.0046(7) -0.0002(7) 0.0002(7)
C12 0.0178(9) 0.0137(9) 0.0238(10) -0.0011(7) 0.0026(7) -0.0014(7)
C13 0.0150(9) 0.0209(10) 0.0156(9) 0.0014(7) 0.0001(7) -0.0014(7)
C14 0.0147(9) 0.0279(11) 0.0229(10) 0.0003(8) -0.0011(7) -0.0054(8)
C15 0.0118(8) 0.0161(8) 0.0124(8) 0.0011(6) 0.0002(6) -0.0013(6)
C16 0.0139(8) 0.0172(9) 0.0123(8) -0.0003(7) 0.0000(6) -0.0012(7)
C17 0.0129(8) 0.0190(9) 0.0113(8) -0.0002(7) 0.0001(6) -0.0003(7)
C18 0.0149(9) 0.0193(9) 0.0138(8) 0.0018(7) -0.0002(7) -0.0017(7)
C19 0.0156(9) 0.0160(9) 0.0151(8) 0.0008(7) -0.0009(7) -0.0010(7)
C20 0.0122(8) 0.0175(9) 0.0118(8) -0.0008(6) -0.0003(6) 0.0000(7)
C21 0.0239(10) 0.0130(9) 0.0194(9) 0.0001(7) 0.0064(8) 0.0003(7)
C22 0.0287(11) 0.0160(9) 0.0169(9) 0.0026(7) 0.0065(8) 0.0029(8)
C23 0.0214(10) 0.0223(10) 0.0163(9) -0.0008(7) 0.0067(7) -0.0056(8)
C24 0.0184(9) 0.0210(9) 0.0124(8) -0.0001(7) -0.0002(7) -0.0008(7)
C25 0.0167(9) 0.0210(9) 0.0157(9) -0.0049(7) 0.0010(7) -0.0018(7)
C26 0.0161(9) 0.0227(10) 0.0136(8) -0.0044(7) 0.0003(7) 0.0003(7)
C27 0.0137(8) 0.0205(9) 0.0140(8) -0.0003(7) 0.0008(7) -0.0010(7)
C28 0.0384(14) 0.0322(13) 0.0248(11) 0.0050(9) 0.0154(10) 0.0177(10)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K O12 2.6546(16) 2_655 ?
K O9 2.7427(15) . ?
K O2 2.7683(15) . ?
K O8 2.8084(16) . ?
K O3 2.8214(16) . ?
K O4 2.9156(15) . ?
K O7 2.9416(15) . ?
K O1 2.9745(15) . ?
K O10 2.9955(15) . ?
P1 F3 1.555(2) . ?
P1 F3 1.555(2) 2_655 ?
P1 F2 1.559(2) 2_655 ?
P1 F2 1.559(2) . ?
P1 F1 1.5923(16) 2_655 ?
P1 F1 1.5923(16) . ?
P2 F5 1.527(2) 2_656 ?
P2 F5 1.527(2) . ?
P2 F6 1.578(2) . ?
P2 F6 1.578(2) 2_656 ?
P2 F4 1.5915(18) 2_656 ?
P2 F4 1.5915(18) . ?
O1 C1 1.366(2) . ?
O1 C7 1.443(2) . ?
O2 C9 1.424(3) . ?
O2 C8 1.428(2) . ?
O3 C11 1.423(3) . ?
O3 C10 1.429(3) . ?
O4 C20 1.361(2) . ?
O4 C12 1.429(2) . ?
O5 C13 1.347(2) . ?
O5 C14 1.439(2) . ?
O6 C13 1.207(3) . ?
O7 C15 1.366(2) . ?
O7 C21 1.430(2) . ?
O8 C22 1.424(3) . ?
O8 C23 1.431(2) . ?
O9 C25 1.423(2) . ?
O9 C24 1.427(2) . ?
O10 C6 1.365(2) . ?
O10 C26 1.432(2) . ?
O11 C27 1.332(2) . ?
O11 C28 1.434(3) . ?
O12 C27 1.210(2) . ?
O12 K 2.6546(16) 2_655 ?
C1 C2 1.378(3) . ?
C1 C6 1.412(3) . ?
C2 C3 1.399(3) . ?
C3 C4 1.388(3) . ?
C3 C13 1.478(3) . ?
C4 C5 1.390(3) . ?
C5 C6 1.384(3) . ?
C7 C8 1.513(3) . ?
C9 C10 1.503(3) . ?
C11 C12 1.505(3) . ?
C15 C16 1.379(3) . ?
C15 C20 1.406(3) . ?
C16 C17 1.400(3) . ?
C17 C18 1.379(3) . ?
C17 C27 1.480(3) . ?
C18 C19 1.392(3) . ?
C19 C20 1.386(3) . ?
C21 C22 1.504(3) . ?
C23 C24 1.512(3) . ?
C25 C26 1.507(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O12 K O9 149.28(5) 2_655 . ?
O12 K O2 76.62(5) 2_655 . ?
O9 K O2 134.10(5) . . ?
O12 K O8 88.88(5) 2_655 . ?
O9 K O8 61.22(4) . . ?
O2 K O8 161.48(5) . . ?
O12 K O3 125.81(5) 2_655 . ?
O9 K O3 79.98(4) . . ?
O2 K O3 60.01(4) . . ?
O8 K O3 138.39(5) . . ?
O12 K O4 92.02(5) 2_655 . ?
O9 K O4 88.36(4) . . ?
O2 K O4 89.22(4) . . ?
O8 K O4 102.93(4) . . ?
O3 K O4 58.94(4) . . ?
O12 K O7 70.85(5) 2_655 . ?
O9 K O7 85.77(4) . . ?
O2 K O7 126.12(4) . . ?
O8 K O7 56.97(4) . . ?
O3 K O7 108.97(4) . . ?
O4 K O7 51.38(4) . . ?
O12 K O1 85.92(5) 2_655 . ?
O9 K O1 110.26(4) . . ?
O2 K O1 57.04(4) . . ?
O8 K O1 111.17(4) . . ?
O3 K O1 95.18(4) . . ?
O4 K O1 145.78(4) . . ?
O7 K O1 153.26(4) . . ?
O12 K O10 132.42(5) 2_655 . ?
O9 K O10 58.66(4) . . ?
O2 K O10 93.19(4) . . ?
O8 K O10 88.11(4) . . ?
O3 K O10 83.66(4) . . ?
O4 K O10 134.76(4) . . ?
O7 K O10 140.18(4) . . ?
O1 K O10 51.69(4) . . ?
F3 P1 F3 90.3(3) . 2_655 ?
F3 P1 F2 89.8(2) . 2_655 ?
F3 P1 F2 179.56(13) 2_655 2_655 ?
F3 P1 F2 179.56(13) . . ?
F3 P1 F2 89.8(2) 2_655 . ?
F2 P1 F2 90.1(3) 2_655 . ?
F3 P1 F1 88.10(11) . 2_655 ?
F3 P1 F1 91.57(10) 2_655 2_655 ?
F2 P1 F1 88.86(13) 2_655 2_655 ?
F2 P1 F1 91.47(13) . 2_655 ?
F3 P1 F1 91.57(10) . . ?
F3 P1 F1 88.10(11) 2_655 . ?
F2 P1 F1 91.47(13) 2_655 . ?
F2 P1 F1 88.86(13) . . ?
F1 P1 F1 179.53(16) 2_655 . ?
F5 P2 F5 91.1(4) 2_656 . ?
F5 P2 F6 91.9(3) 2_656 . ?
F5 P2 F6 176.8(3) . . ?
F5 P2 F6 176.8(3) 2_656 2_656 ?
F5 P2 F6 91.9(3) . 2_656 ?
F6 P2 F6 85.2(3) . 2_656 ?
F5 P2 F4 90.39(15) 2_656 2_656 ?
F5 P2 F4 91.31(15) . 2_656 ?
F6 P2 F4 87.58(12) . 2_656 ?
F6 P2 F4 90.63(13) 2_656 2_656 ?
F5 P2 F4 91.31(15) 2_656 . ?
F5 P2 F4 90.39(15) . . ?
F6 P2 F4 90.63(13) . . ?
F6 P2 F4 87.58(13) 2_656 . ?
F4 P2 F4 177.57(17) 2_656 . ?
C1 O1 C7 114.89(15) . . ?
C1 O1 K 125.48(11) . . ?
C7 O1 K 118.45(11) . . ?
C9 O2 C8 114.27(16) . . ?
C9 O2 K 108.37(12) . . ?
C8 O2 K 110.92(12) . . ?
C11 O3 C10 113.67(17) . . ?
C11 O3 K 113.40(11) . . ?
C10 O3 K 116.70(12) . . ?
C20 O4 C12 116.79(15) . . ?
C20 O4 K 112.52(11) . . ?
C12 O4 K 117.90(11) . . ?
C13 O5 C14 114.12(16) . . ?
C15 O7 C21 117.82(15) . . ?
C15 O7 K 110.76(11) . . ?
C21 O7 K 111.72(11) . . ?
C22 O8 C23 112.70(16) . . ?
C22 O8 K 122.40(11) . . ?
C23 O8 K 107.93(12) . . ?
C25 O9 C24 114.86(16) . . ?
C25 O9 K 110.00(11) . . ?
C24 O9 K 119.72(11) . . ?
C6 O10 C26 116.42(15) . . ?
C6 O10 K 124.77(11) . . ?
C26 O10 K 116.24(11) . . ?
C27 O11 C28 114.76(17) . . ?
C27 O12 K 162.26(15) . 2_655 ?
O1 C1 C2 123.99(17) . . ?
O1 C1 C6 116.22(17) . . ?
C2 C1 C6 119.78(18) . . ?
C1 C2 C3 120.05(18) . . ?
C4 C3 C2 119.92(18) . . ?
C4 C3 C13 122.37(18) . . ?
C2 C3 C13 117.69(18) . . ?
C3 C4 C5 120.37(18) . . ?
C6 C5 C4 119.84(18) . . ?
O10 C6 C5 124.56(18) . . ?
O10 C6 C1 115.46(17) . . ?
C5 C6 C1 119.98(18) . . ?
O1 C7 C8 108.33(16) . . ?
O2 C8 C7 114.29(17) . . ?
O2 C9 C10 107.64(17) . . ?
O3 C10 C9 108.10(18) . . ?
O3 C11 C12 112.45(17) . . ?
O4 C12 C11 106.71(16) . . ?
O6 C13 O5 123.18(19) . . ?
O6 C13 C3 124.41(19) . . ?
O5 C13 C3 112.40(17) . . ?
O7 C15 C16 125.41(17) . . ?
O7 C15 C20 114.20(16) . . ?
C16 C15 C20 120.36(17) . . ?
C15 C16 C17 118.93(18) . . ?
C18 C17 C16 120.91(18) . . ?
C18 C17 C27 118.03(17) . . ?
C16 C17 C27 121.03(18) . . ?
C17 C18 C19 120.21(18) . . ?
C20 C19 C18 119.40(19) . . ?
O4 C20 C19 124.96(18) . . ?
O4 C20 C15 114.87(16) . . ?
C19 C20 C15 120.16(17) . . ?
O7 C21 C22 105.97(16) . . ?
O8 C22 C21 108.59(17) . . ?
O8 C23 C24 111.67(16) . . ?
O9 C24 C23 110.80(16) . . ?
O9 C25 C26 113.49(17) . . ?
O10 C26 C25 106.57(16) . . ?
O12 C27 O11 123.19(19) . . ?
O12 C27 C17 124.34(19) . . ?
O11 C27 C17 112.45(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12 K O1 C1 -136.20(15) 2_655 . . . ?
O9 K O1 C1 16.96(16) . . . . ?
O2 K O1 C1 147.11(16) . . . . ?
O8 K O1 C1 -48.99(15) . . . . ?
O3 K O1 C1 98.18(15) . . . . ?
O4 K O1 C1 136.20(14) . . . . ?
O7 K O1 C1 -106.95(16) . . . . ?
O10 K O1 C1 20.47(14) . . . . ?
O12 K O1 C7 56.86(14) 2_655 . . . ?
O9 K O1 C7 -149.98(14) . . . . ?
O2 K O1 C7 -19.84(13) . . . . ?
O8 K O1 C7 144.07(14) . . . . ?
O3 K O1 C7 -68.77(14) . . . . ?
O4 K O1 C7 -30.74(17) . . . . ?
O7 K O1 C7 86.10(16) . . . . ?
O10 K O1 C7 -146.48(15) . . . . ?
O12 K O2 C9 -178.96(13) 2_655 . . . ?
O9 K O2 C9 1.81(15) . . . . ?
O8 K O2 C9 -139.61(16) . . . . ?
O3 K O2 C9 34.78(12) . . . . ?
O4 K O2 C9 88.78(12) . . . . ?
O7 K O2 C9 127.27(12) . . . . ?
O1 K O2 C9 -85.11(13) . . . . ?
O10 K O2 C9 -46.02(12) . . . . ?
O12 K O2 C8 -52.76(12) 2_655 . . . ?
O9 K O2 C8 128.01(12) . . . . ?
O8 K O2 C8 -13.4(2) . . . . ?
O3 K O2 C8 160.98(13) . . . . ?
O4 K O2 C8 -145.02(12) . . . . ?
O7 K O2 C8 -106.53(12) . . . . ?
O1 K O2 C8 41.08(11) . . . . ?
O10 K O2 C8 80.18(12) . . . . ?
O12 K O3 C11 91.86(13) 2_655 . . . ?
O9 K O3 C11 -69.75(13) . . . . ?
O2 K O3 C11 133.63(14) . . . . ?
O8 K O3 C11 -49.04(15) . . . . ?
O4 K O3 C11 24.41(12) . . . . ?
O7 K O3 C11 12.21(13) . . . . ?
O1 K O3 C11 -179.45(12) . . . . ?
O10 K O3 C11 -128.96(13) . . . . ?
O12 K O3 C10 -43.16(15) 2_655 . . . ?
O9 K O3 C10 155.23(14) . . . . ?
O2 K O3 C10 -1.38(13) . . . . ?
O8 K O3 C10 175.94(13) . . . . ?
O4 K O3 C10 -110.61(14) . . . . ?
O7 K O3 C10 -122.81(14) . . . . ?
O1 K O3 C10 45.53(14) . . . . ?
O10 K O3 C10 96.02(14) . . . . ?
O12 K O4 C20 17.29(12) 2_655 . . . ?
O9 K O4 C20 -131.97(12) . . . . ?
O2 K O4 C20 93.88(12) . . . . ?
O8 K O4 C20 -72.02(12) . . . . ?
O3 K O4 C20 148.75(13) . . . . ?
O7 K O4 C20 -46.07(11) . . . . ?
O1 K O4 C20 103.01(13) . . . . ?
O10 K O4 C20 -172.40(11) . . . . ?
O12 K O4 C12 -123.22(13) 2_655 . . . ?
O9 K O4 C12 87.52(13) . . . . ?
O2 K O4 C12 -46.64(13) . . . . ?
O8 K O4 C12 147.47(13) . . . . ?
O3 K O4 C12 8.24(12) . . . . ?
O7 K O4 C12 173.41(15) . . . . ?
O1 K O4 C12 -37.50(16) . . . . ?
O10 K O4 C12 47.09(15) . . . . ?
O12 K O7 C15 -61.88(12) 2_655 . . . ?
O9 K O7 C15 138.39(12) . . . . ?
O2 K O7 C15 -5.70(14) . . . . ?
O8 K O7 C15 -163.47(13) . . . . ?
O3 K O7 C15 60.50(12) . . . . ?
O4 K O7 C15 47.10(11) . . . . ?
O1 K O7 C15 -92.93(14) . . . . ?
O10 K O7 C15 163.80(11) . . . . ?
O12 K O7 C21 71.61(12) 2_655 . . . ?
O9 K O7 C21 -88.12(12) . . . . ?
O2 K O7 C21 127.79(12) . . . . ?
O8 K O7 C21 -29.98(11) . . . . ?
O3 K O7 C21 -166.01(12) . . . . ?
O4 K O7 C21 -179.41(14) . . . . ?
O1 K O7 C21 40.56(16) . . . . ?
O10 K O7 C21 -62.71(14) . . . . ?
O12 K O8 C22 -72.26(14) 2_655 . . . ?
O9 K O8 C22 100.38(15) . . . . ?
O2 K O8 C22 -110.35(18) . . . . ?
O3 K O8 C22 76.97(15) . . . . ?
O4 K O8 C22 19.56(15) . . . . ?
O7 K O8 C22 -4.50(13) . . . . ?
O1 K O8 C22 -157.44(13) . . . . ?
O10 K O8 C22 155.23(14) . . . . ?
O12 K O8 C23 154.46(12) 2_655 . . . ?
O9 K O8 C23 -32.90(12) . . . . ?
O2 K O8 C23 116.37(16) . . . . ?
O3 K O8 C23 -56.31(14) . . . . ?
O4 K O8 C23 -113.72(12) . . . . ?
O7 K O8 C23 -137.79(13) . . . . ?
O1 K O8 C23 69.27(13) . . . . ?
O10 K O8 C23 21.95(12) . . . . ?
O12 K O9 C25 156.88(12) 2_655 . . . ?
O2 K O9 C25 -24.58(14) . . . . ?
O8 K O9 C25 142.36(13) . . . . ?
O3 K O9 C25 -53.17(12) . . . . ?
O4 K O9 C25 -111.91(12) . . . . ?
O7 K O9 C25 -163.30(12) . . . . ?
O1 K O9 C25 38.69(13) . . . . ?
O10 K O9 C25 35.47(11) . . . . ?
O12 K O9 C24 20.59(18) 2_655 . . . ?
O2 K O9 C24 -160.87(12) . . . . ?
O8 K O9 C24 6.07(12) . . . . ?
O3 K O9 C24 170.54(14) . . . . ?
O4 K O9 C24 111.80(13) . . . . ?
O7 K O9 C24 60.41(13) . . . . ?
O1 K O9 C24 -97.60(13) . . . . ?
O10 K O9 C24 -100.82(14) . . . . ?
O12 K O10 C6 10.73(17) 2_655 . . . ?
O9 K O10 C6 154.52(16) . . . . ?
O2 K O10 C6 -64.03(15) . . . . ?
O8 K O10 C6 97.48(15) . . . . ?
O3 K O10 C6 -123.37(15) . . . . ?
O4 K O10 C6 -156.10(13) . . . . ?
O7 K O10 C6 124.45(14) . . . . ?
O1 K O10 C6 -21.63(13) . . . . ?
O12 K O10 C26 -150.35(13) 2_655 . . . ?
O9 K O10 C26 -6.55(12) . . . . ?
O2 K O10 C26 134.89(13) . . . . ?
O8 K O10 C26 -63.60(13) . . . . ?
O3 K O10 C26 75.55(13) . . . . ?
O4 K O10 C26 42.82(15) . . . . ?
O7 K O10 C26 -36.63(16) . . . . ?
O1 K O10 C26 177.29(15) . . . . ?
C7 O1 C1 C2 -33.0(3) . . . . ?
K O1 C1 C2 159.69(15) . . . . ?
C7 O1 C1 C6 147.87(18) . . . . ?
K O1 C1 C6 -19.5(2) . . . . ?
O1 C1 C2 C3 -177.40(18) . . . . ?
C6 C1 C2 C3 1.7(3) . . . . ?
C1 C2 C3 C4 0.1(3) . . . . ?
C1 C2 C3 C13 -178.62(18) . . . . ?
C2 C3 C4 C5 -1.9(3) . . . . ?
C13 C3 C4 C5 176.80(19) . . . . ?
C3 C4 C5 C6 1.7(3) . . . . ?
C26 O10 C6 C5 4.3(3) . . . . ?
K O10 C6 C5 -156.78(15) . . . . ?
C26 O10 C6 C1 -176.35(17) . . . . ?
K O10 C6 C1 22.6(2) . . . . ?
C4 C5 C6 O10 179.51(19) . . . . ?
C4 C5 C6 C1 0.2(3) . . . . ?
O1 C1 C6 O10 -2.1(3) . . . . ?
C2 C1 C6 O10 178.69(18) . . . . ?
O1 C1 C6 C5 177.31(18) . . . . ?
C2 C1 C6 C5 -1.9(3) . . . . ?
C1 O1 C7 C8 -171.37(17) . . . . ?
K O1 C7 C8 -3.1(2) . . . . ?
C9 O2 C8 C7 56.0(2) . . . . ?
K O2 C8 C7 -66.82(19) . . . . ?
O1 C7 C8 O2 44.5(2) . . . . ?
C8 O2 C9 C10 168.43(17) . . . . ?
K O2 C9 C10 -67.34(18) . . . . ?
C11 O3 C10 C9 -165.00(17) . . . . ?
K O3 C10 C9 -30.1(2) . . . . ?
O2 C9 C10 O3 65.5(2) . . . . ?
C10 O3 C11 C12 79.4(2) . . . . ?
K O3 C11 C12 -57.04(19) . . . . ?
C20 O4 C12 C11 -175.56(16) . . . . ?
K O4 C12 C11 -36.71(19) . . . . ?
O3 C11 C12 O4 62.2(2) . . . . ?
C14 O5 C13 O6 1.7(3) . . . . ?
C14 O5 C13 C3 -177.40(18) . . . . ?
C4 C3 C13 O6 -160.7(2) . . . . ?
C2 C3 C13 O6 18.0(3) . . . . ?
C4 C3 C13 O5 18.4(3) . . . . ?
C2 C3 C13 O5 -162.90(18) . . . . ?
C21 O7 C15 C16 3.5(3) . . . . ?
K O7 C15 C16 133.85(17) . . . . ?
C21 O7 C15 C20 -178.29(17) . . . . ?
K O7 C15 C20 -47.94(18) . . . . ?
O7 C15 C16 C17 179.37(18) . . . . ?
C20 C15 C16 C17 1.3(3) . . . . ?
C15 C16 C17 C18 -1.1(3) . . . . ?
C15 C16 C17 C27 -179.08(17) . . . . ?
C16 C17 C18 C19 -0.4(3) . . . . ?
C27 C17 C18 C19 177.60(18) . . . . ?
C17 C18 C19 C20 1.8(3) . . . . ?
C12 O4 C20 C19 6.5(3) . . . . ?
K O4 C20 C19 -134.45(16) . . . . ?
C12 O4 C20 C15 -174.91(17) . . . . ?
K O4 C20 C15 44.11(18) . . . . ?
C18 C19 C20 O4 176.81(18) . . . . ?
C18 C19 C20 C15 -1.7(3) . . . . ?
O7 C15 C20 O4 3.2(2) . . . . ?
C16 C15 C20 O4 -178.50(17) . . . . ?
O7 C15 C20 C19 -178.18(17) . . . . ?
C16 C15 C20 C19 0.1(3) . . . . ?
C15 O7 C21 C22 -170.13(17) . . . . ?
K O7 C21 C22 59.96(18) . . . . ?
C23 O8 C22 C21 167.50(17) . . . . ?
K O8 C22 C21 36.2(2) . . . . ?
O7 C21 C22 O8 -62.7(2) . . . . ?
C22 O8 C23 C24 -78.7(2) . . . . ?
K O8 C23 C24 59.48(19) . . . . ?
C25 O9 C24 C23 -113.92(18) . . . . ?
K O9 C24 C23 20.4(2) . . . . ?
O8 C23 C24 O9 -54.9(2) . . . . ?
C24 O9 C25 C26 69.2(2) . . . . ?
K O9 C25 C26 -69.39(18) . . . . ?
C6 O10 C26 C25 176.17(17) . . . . ?
K O10 C26 C25 -21.13(19) . . . . ?
O9 C25 C26 O10 59.8(2) . . . . ?
K O12 C27 O11 162.3(4) 2_655 . . . ?
K O12 C27 C17 -15.7(6) 2_655 . . . ?
C28 O11 C27 O12 -0.4(3) . . . . ?
C28 O11 C27 C17 177.87(19) . . . . ?
C18 C17 C27 O12 28.7(3) . . . . ?
C16 C17 C27 O12 -153.3(2) . . . . ?
C18 C17 C27 O11 -149.49(18) . . . . ?
C16 C17 C27 O11 28.5(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.12
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.612
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.178