# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182


_publ_contact_author_name        'Dr Baoqing Ma'
_publ_contact_author_address     
;
Department of Chemistry
Peking University
Beijing
100871
CHINA
;

_publ_contact_author_email       CHEM9978@ACSU.BUFFALO.EDU

_publ_section_title              
;
The design and synthesis of non-centric
diamond-like networks based NH4+ ion
;

data_p-4n2
_database_code_CSD               200424

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H21 F6 N5 O4.50 P'
_chemical_formula_weight         548.39

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           Tetragonal
_symmetry_space_group_name_H-M   P-4n2

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

_cell_length_a                   17.9935(13)
_cell_length_b                   17.9935(13)
_cell_length_c                   7.2554(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2349.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1124
_exptl_absorpt_coefficient_mu    0.205
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(1)
_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  'SMART CCD 1000'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18737
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         29.37
_reflns_number_total             2998
_reflns_number_gt                2627
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART CCD 1000'
_computing_cell_refinement       SMART
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    XP
_computing_publication_material  XCIF

_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^)+(0.1122P)^2^+2.1535P] 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     SHELXL
_refine_ls_extinction_coef       0.0174(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(4)
_refine_ls_number_reflns         2998
_refine_ls_number_parameters     248
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.1871
_refine_ls_wR_factor_gt          0.1816
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.114
_refine_ls_shift/su_mean         0.002

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 0.48154(4) 0.37549(4) 0.02430(10) 0.02241(18) Uani 1 1 d . . .
O2 O 0.13476(4) 0.00380(4) -0.03908(10) 0.02390(18) Uani 1 1 d . . .
O3 O 0.52027(17) 0.02027(17) -0.2500 0.1097(19) Uani 0.50 2 d SP . .
H3 H 0.5000 0.0000 -0.122(2) 0.000(3) Uiso 1 2 d S . .
N1 N 0.43141(5) 0.32998(5) 0.09229(12) 0.0188(2) Uani 1 1 d . . .
N2 N 0.18270(5) 0.05290(5) -0.10113(12) 0.0189(2) Uani 1 1 d . . .
N3 N 0.0000 0.0000 -0.24538(16) 0.0187(3) Uani 1 2 d SD . .
H2 H -0.0039(8) 0.0467(5) -0.3584(13) 0.026(3) Uiso 1 1 d D . .
C1 C 0.35883(6) 0.35008(6) 0.09673(14) 0.0192(2) Uani 1 1 d . . .
C2 C 0.30526(6) 0.30089(6) 0.15978(14) 0.0190(2) Uani 1 1 d . . .
H2A H 0.2474(8) 0.3168(8) 0.152(2) 0.028(3) Uiso 1 1 d . . .
C3 C 0.32560(5) 0.22961(5) 0.21912(14) 0.0172(2) Uani 1 1 d . . .
C4 C 0.40172(6) 0.21222(6) 0.21768(15) 0.0207(2) Uani 1 1 d . . .
H4A H 0.4196(6) 0.1648(7) 0.2659(17) 0.015(3) Uiso 1 1 d . . .
C5 C 0.45287(6) 0.26247(6) 0.15500(15) 0.0211(2) Uani 1 1 d . . .
H5A H 0.5051(7) 0.2506(7) 0.1437(17) 0.020(3) Uiso 1 1 d . . .
C6 C 0.25131(6) 0.03076(6) -0.15688(16) 0.0232(2) Uani 1 1 d . . .
H6A H 0.2647(7) -0.0164(7) -0.1495(18) 0.023(3) Uiso 1 1 d . . .
C7 C 0.30324(6) 0.08150(6) -0.21709(15) 0.0213(2) Uani 1 1 d . . .
H7A H 0.3596(6) 0.0607(7) -0.2491(17) 0.015(3) Uiso 1 1 d . . .
C8 C 0.28680(5) 0.15783(5) -0.22002(14) 0.0178(2) Uani 1 1 d . . .
C9 C 0.21523(6) 0.17834(6) -0.16420(15) 0.0188(2) Uani 1 1 d . . .
H9A H 0.1985(8) 0.2331(8) -0.138(2) 0.028(4) Uiso 1 1 d . . .
C10 C 0.16419(6) 0.12557(6) -0.10554(14) 0.0196(2) Uani 1 1 d . . .
H10A H 0.1129(8) 0.1354(8) -0.064(2) 0.033(4) Uiso 1 1 d . . .
P1 P 0.60841(5) 0.10841(5) 0.2500 0.0688(4) Uani 0.50 2 d SP . .
P2 P 0.60444(7) 0.10743(7) 0.0912(2) 0.0325(3) Uani 0.25 1 d P . .
F1 F 0.66239(15) 0.07819(18) 0.1811(10) 0.291(3) Uani 0.50 1 d P . .
F2 F 0.53587(14) 0.09939(12) 0.1878(6) 0.1325(14) Uani 0.50 1 d P . .
F3 F 0.61875(9) 0.18768(10) 0.1472(3) 0.0486(5) Uani 0.50 1 d P . .
F4 F 0.6574(2) 0.12180(17) -0.0740(9) 0.3748(19) Uani 0.50 1 d P . .
F5 F 0.5452(3) 0.1237(2) 0.0119(10) 0.409(2) Uani 0.50 1 d P . .
F6 F 0.59905(18) 0.02618(17) 0.0254(10) 0.213(3) Uani 0.50 1 d P . .
H1A H 0.3456(7) 0.3988(6) 0.0514(16) 0.013(3) Uiso 1 1 d . . .
H1 H 0.0468(5) 0.0105(10) -0.1366(15) 0.052(5) Uiso 1 1 d 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
O1 0.0219(3) 0.0188(3) 0.0265(3) -0.0008(3) 0.0077(3) -0.0053(3)
O2 0.0188(3) 0.0249(3) 0.0279(3) 0.0084(3) -0.0024(3) -0.0099(3)
O3 0.0817(19) 0.0817(19) 0.166(5) 0.022(3) -0.022(3) -0.001(2)
N1 0.0189(4) 0.0185(4) 0.0192(4) -0.0025(3) 0.0018(3) -0.0035(3)
N2 0.0166(4) 0.0214(4) 0.0188(3) 0.0037(3) -0.0041(3) -0.0057(3)
N3 0.0175(5) 0.0160(5) 0.0226(6) 0.000 0.000 0.0000(4)
C1 0.0221(4) 0.0173(4) 0.0183(4) 0.0022(4) 0.0021(4) 0.0002(4)
C2 0.0208(4) 0.0169(4) 0.0194(4) -0.0013(4) 0.0003(4) -0.0002(4)
C3 0.0181(4) 0.0169(4) 0.0166(4) 0.0015(4) 0.0013(4) -0.0036(4)
C4 0.0202(4) 0.0192(4) 0.0227(4) 0.0021(4) 0.0006(4) -0.0024(4)
C5 0.0192(4) 0.0197(4) 0.0244(5) 0.0013(4) 0.0012(4) -0.0005(4)
C6 0.0224(5) 0.0167(4) 0.0305(5) 0.0009(4) -0.0006(4) -0.0017(4)
C7 0.0198(4) 0.0197(4) 0.0242(5) 0.0014(4) 0.0009(4) -0.0004(4)
C8 0.0204(4) 0.0170(4) 0.0160(4) 0.0012(4) -0.0003(4) -0.0018(4)
C9 0.0173(4) 0.0189(4) 0.0204(4) 0.0008(4) -0.0009(4) 0.0001(4)
C10 0.0167(4) 0.0217(4) 0.0202(4) 0.0016(4) -0.0002(4) 0.0000(4)
P1 0.0390(3) 0.0390(3) 0.1284(12) -0.0173(5) 0.0173(5) 0.0035(5)
P2 0.0185(4) 0.0204(5) 0.0585(8) -0.0024(5) -0.0072(5) 0.0125(4)
F1 0.0817(12) 0.2001(18) 0.591(8) 0.237(3) 0.072(3) 0.1151(11)
F2 0.0626(12) 0.0521(11) 0.283(4) 0.0510(19) 0.0672(18) 0.0289(10)
F3 0.0294(7) 0.0424(9) 0.0739(11) 0.0006(9) -0.0127(8) -0.0037(7)
F4 0.360(3) 0.0635(14) 0.701(5) -0.146(2) 0.433(3) -0.0849(18)
F5 0.337(3) 0.253(2) 0.636(5) -0.345(3) -0.368(3) 0.231(2)
F6 0.0897(18) 0.0628(17) 0.487(8) -0.015(3) 0.105(3) 0.0222(15)

_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 N1 1.3144(11) . ?
O2 N2 1.3143(11) . ?
O3 O3 1.031(9) 2_655 ?
N1 C5 1.3533(14) . ?
N1 C1 1.3556(14) . ?
N2 C10 1.3498(14) . ?
N2 C6 1.3589(14) . ?
C1 C2 1.3862(14) . ?
C2 C3 1.4016(14) . ?
C3 C4 1.4050(14) . ?
C3 C3 1.4745(19) 8 ?
C4 C5 1.3680(15) . ?
C6 C7 1.3774(15) . ?
C7 C8 1.4052(14) . ?
C8 C9 1.3996(14) . ?
C8 C8 1.4745(19) 8_554 ?
C9 C10 1.3879(14) . ?
P1 P2 1.1547(16) 7_545 ?
P1 P2 1.1547(16) . ?
P1 F1 1.220(4) . ?
P1 F1 1.220(4) 7_545 ?
P1 F2 1.390(3) . ?
P1 F2 1.391(3) 7_545 ?
P1 F3 1.620(2) 7_545 ?
P1 F3 1.620(2) . ?
P1 F5 2.086(6) 7_545 ?
P1 F5 2.086(6) . ?
P1 F6 2.207(6) . ?
P1 F6 2.207(6) 7_545 ?
P2 F5 1.245(6) . ?
P2 F1 1.338(4) . ?
P2 F2 1.426(3) . ?
P2 F3 1.522(2) . ?
P2 F6 1.541(4) . ?
P2 F4 1.553(6) . ?
P2 F1 1.982(6) 7_545 ?
P2 F2 2.059(4) 7_545 ?
P2 P2 2.306(3) 7_545 ?
F1 F3 1.514(7) 7_545 ?
F1 F2 1.664(6) 7_545 ?
F1 P2 1.982(6) 7_545 ?
F2 F5 1.359(8) . ?
F2 F1 1.664(6) 7_545 ?
F2 P2 2.059(4) 7_545 ?
F3 F1 1.514(7) 7_545 ?

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
O1 N1 C5 119.32(8) . . ?
O1 N1 C1 120.25(8) . . ?
C5 N1 C1 120.42(9) . . ?
O2 N2 C10 119.83(8) . . ?
O2 N2 C6 120.08(9) . . ?
C10 N2 C6 120.08(9) . . ?
N1 C1 C2 120.49(9) . . ?
C1 C2 C3 120.28(9) . . ?
C2 C3 C4 117.12(9) . . ?
C2 C3 C3 122.28(6) . 8 ?
C4 C3 C3 120.60(6) . 8 ?
C5 C4 C3 120.75(9) . . ?
N1 C5 C4 120.86(9) . . ?
N2 C6 C7 121.09(9) . . ?
C6 C7 C8 120.66(10) . . ?
C9 C8 C7 116.55(9) . . ?
C9 C8 C8 121.93(6) . 8_554 ?
C7 C8 C8 121.52(6) . 8_554 ?
C10 C9 C8 121.15(9) . . ?
N2 C10 C9 120.45(9) . . ?
P2 P1 P2 173.75(19) 7_545 . ?
P2 P1 F1 113.2(3) 7_545 . ?
P2 P1 F1 68.5(3) . . ?
P2 P1 F1 68.5(3) 7_545 7_545 ?
P2 P1 F1 113.2(3) . 7_545 ?
F1 P1 F1 151.3(3) . 7_545 ?
P2 P1 F2 107.6(2) 7_545 . ?
P2 P1 F2 67.4(2) . . ?
F1 P1 F2 124.2(3) . . ?
F1 P1 F2 78.9(2) 7_545 . ?
P2 P1 F2 67.4(2) 7_545 7_545 ?
P2 P1 F2 107.6(2) . 7_545 ?
F1 P1 F2 78.9(2) . 7_545 ?
F1 P1 F2 124.2(3) 7_545 7_545 ?
F2 P1 F2 83.5(2) . 7_545 ?
P2 P1 F3 63.96(10) 7_545 7_545 ?
P2 P1 F3 121.05(12) . 7_545 ?
F1 P1 F3 62.6(3) . 7_545 ?
F1 P1 F3 96.5(2) 7_545 7_545 ?
F2 P1 F3 171.5(2) . 7_545 ?
F2 P1 F3 93.49(13) 7_545 7_545 ?
P2 P1 F3 121.05(12) 7_545 . ?
P2 P1 F3 63.96(10) . . ?
F1 P1 F3 96.5(2) . . ?
F1 P1 F3 62.6(3) 7_545 . ?
F2 P1 F3 93.49(13) . . ?
F2 P1 F3 171.5(2) 7_545 . ?
F3 P1 F3 90.57(14) 7_545 . ?
P2 P1 F5 30.88(17) 7_545 7_545 ?
P2 P1 F5 145.72(19) . 7_545 ?
F1 P1 F5 89.5(3) . 7_545 ?
F1 P1 F5 98.8(3) 7_545 7_545 ?
F2 P1 F5 109.2(2) . 7_545 ?
F2 P1 F5 40.1(2) 7_545 7_545 ?
F3 P1 F5 64.24(14) 7_545 7_545 ?
F3 P1 F5 147.76(18) . 7_545 ?
P2 P1 F5 145.72(19) 7_545 . ?
P2 P1 F5 30.88(17) . . ?
F1 P1 F5 98.8(3) . . ?
F1 P1 F5 89.5(3) 7_545 . ?
F2 P1 F5 40.1(2) . . ?
F2 P1 F5 109.2(2) 7_545 . ?
F3 P1 F5 147.76(18) 7_545 . ?
F3 P1 F5 64.24(14) . . ?
F5 P1 F5 146.0(3) 7_545 . ?
P2 P1 F6 133.95(17) 7_545 . ?
P2 P1 F6 41.27(15) . . ?
F1 P1 F6 57.3(3) . . ?
F1 P1 F6 143.3(3) 7_545 . ?
F2 P1 F6 67.08(17) . . ?
F2 P1 F6 66.5(2) 7_545 . ?
F3 P1 F6 118.95(11) 7_545 . ?
F3 P1 F6 105.00(16) . . ?
F5 P1 F6 104.8(2) 7_545 . ?
F5 P1 F6 55.61(17) . . ?
P2 P1 F6 41.27(15) 7_545 7_545 ?
P2 P1 F6 133.95(17) . 7_545 ?
F1 P1 F6 143.3(3) . 7_545 ?
F1 P1 F6 57.3(3) 7_545 7_545 ?
F2 P1 F6 66.5(2) . 7_545 ?
F2 P1 F6 67.08(17) 7_545 7_545 ?
F3 P1 F6 105.00(16) 7_545 7_545 ?
F3 P1 F6 118.95(11) . 7_545 ?
F5 P1 F6 55.61(17) 7_545 7_545 ?
F5 P1 F6 104.8(2) . 7_545 ?
F6 P1 F6 116.3(2) . 7_545 ?
P1 P2 F5 120.7(3) . . ?
P1 P2 F1 58.1(3) . . ?
F5 P2 F1 169.8(3) . . ?
P1 P2 F2 64.19(19) . . ?
F5 P2 F2 60.7(3) . . ?
F1 P2 F2 113.2(3) . . ?
P1 P2 F3 73.07(12) . . ?
F5 P2 F3 92.6(2) . . ?
F1 P2 F3 96.4(2) . . ?
F2 P2 F3 96.40(15) . . ?
P1 P2 F6 109.1(3) . . ?
F5 P2 F6 91.5(3) . . ?
F1 P2 F6 80.0(3) . . ?
F2 P2 F6 90.1(2) . . ?
F3 P2 F6 173.43(18) . . ?
P1 P2 F4 136.8(2) . . ?
F5 P2 F4 97.5(4) . . ?
F1 P2 F4 87.9(3) . . ?
F2 P2 F4 158.0(3) . . ?
F3 P2 F4 86.79(16) . . ?
F6 P2 F4 87.6(3) . . ?
P1 P2 F1 34.46(14) . 7_545 ?
F5 P2 F1 93.7(3) . 7_545 ?
F1 P2 F1 88.6(2) . 7_545 ?
F2 P2 F1 55.59(18) . 7_545 ?
F3 P2 F1 49.06(14) . 7_545 ?
F6 P2 F1 135.8(3) . 7_545 ?
F4 P2 F1 134.93(19) . 7_545 ?
P1 P2 F2 40.08(12) . 7_545 ?
F5 P2 F2 118.0(3) . 7_545 ?
F1 P2 F2 53.7(2) . 7_545 ?
F2 P2 F2 61.03(17) . 7_545 ?
F3 P2 F2 113.14(15) . 7_545 ?
F6 P2 F2 69.2(3) . 7_545 ?
F4 P2 F2 137.07(19) . 7_545 ?
F1 P2 F2 69.65(17) 7_545 7_545 ?
P1 P2 P2 3.13(9) . 7_545 ?
F5 P2 P2 119.2(3) . 7_545 ?
F1 P2 P2 59.0(3) . 7_545 ?
F2 P2 P2 61.75(18) . 7_545 ?
F3 P2 P2 75.61(10) . 7_545 ?
F6 P2 P2 106.8(3) . 7_545 ?
F4 P2 P2 139.5(2) . 7_545 ?
F1 P2 P2 35.35(14) 7_545 7_545 ?
F2 P2 P2 37.61(10) 7_545 7_545 ?
P1 F1 P2 53.43(13) . . ?
P1 F1 F3 71.8(3) . 7_545 ?
P2 F1 F3 116.5(3) . 7_545 ?
P1 F1 F2 55.1(2) . 7_545 ?
P2 F1 F2 85.9(2) . 7_545 ?
F3 F1 F2 87.4(4) 7_545 7_545 ?
P1 F1 P2 32.4(2) . 7_545 ?
P2 F1 P2 85.6(2) . 7_545 ?
F3 F1 P2 49.4(2) 7_545 7_545 ?
F2 F1 P2 45.01(19) 7_545 7_545 ?
F5 F2 P1 98.7(3) . . ?
F5 F2 P2 53.0(3) . . ?
P1 F2 P2 48.38(11) . . ?
F5 F2 F1 105.1(3) . 7_545 ?
P1 F2 F1 46.02(15) . 7_545 ?
P2 F2 F1 79.4(2) . 7_545 ?
F5 F2 P2 129.8(3) . 7_545 ?
P1 F2 P2 32.32(11) . 7_545 ?
P2 F2 P2 80.64(17) . 7_545 ?
F1 F2 P2 40.41(18) 7_545 7_545 ?
F1 F3 P2 81.54(18) 7_545 . ?
F1 F3 P1 45.66(13) 7_545 . ?
P2 F3 P1 42.98(8) . . ?
P2 F5 F2 66.2(3) . . ?
P2 F5 P1 28.43(19) . . ?
F2 F5 P1 41.2(2) . . ?
P2 F6 P1 29.62(14) . . ?

_diffrn_measured_fraction_theta_max 0.956
_diffrn_reflns_theta_full        29.37
_diffrn_measured_fraction_theta_full 0.956
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.087

data_i-4
_database_code_CSD               200425

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H30 F6 N5 O7 P'
_chemical_formula_weight         645.50

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           Tetragonal
_symmetry_space_group_name_H-M   I-42d

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   28.0095(18)
_cell_length_b                   28.0095(18)
_cell_length_c                   7.4018(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5807.0(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    90(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prismatic
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2672
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(1)
_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  'SMART CCD 1000'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20508
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         24.98
_reflns_number_total             2544
_reflns_number_gt                2083
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART CCD 1000'
_computing_cell_refinement       SMART
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    XP
_computing_publication_material  XCIF

_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^)+(0.1738P)^2^+13.4032P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_number_reflns         2544
_refine_ls_number_parameters     227
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0884
_refine_ls_wR_factor_ref         0.2546
_refine_ls_wR_factor_gt          0.2326
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_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
P1 P 0.59702(10) 0.2500 0.1250 0.0783(12) Uani 1 2 d S . .
O1 O 0.93334(11) 0.55225(10) 0.7047(4) 0.0236(8) Uani 1 1 d . . .
O2 O 0.93618(11) 0.94369(10) 0.0502(4) 0.0234(8) Uani 1 1 d . . .
O3 O 0.6002(14) 0.2500 -0.3750 0.187(7) Uiso 0.50 2 d SP . .
O3' O 0.5625(19) 0.2834(19) -0.467(8) 0.187(7) Uiso 0.25 1 d P . .
O4 O 0.7822(9) 0.7691(9) 0.315(4) 0.187(7) Uiso 0.50 1 d P . .
O4' O 0.7811(9) 0.7257(9) 0.435(4) 0.187(7) Uiso 0.50 1 d P . .
N1 N 0.92896(14) 0.59484(13) 0.6310(5) 0.0202(8) Uani 1 1 d . . .
N2 N 0.93655(14) 0.90064(13) 0.1248(5) 0.0225(8) Uani 1 1 d . . .
N3 N 1.0000 1.0000 0.2535(6) 0.0140(11) Uani 1 2 d SD . .
H2 H 0.9888(14) 1.0198(12) 0.332(5) 0.009(11) Uiso 1 1 d D . .
H1 H 1.0188(13) 1.0167(14) 0.186(5) 0.015(12) Uiso 1 1 d D . .
C1 C 0.96854(18) 0.62139(15) 0.5938(6) 0.0246(11) Uani 1 1 d . . .
H1A H 0.9986 0.6092 0.6199 0.029 Uiso 1 1 calc R . .
C2 C 0.9644(2) 0.66514(18) 0.5197(6) 0.0356(13) Uani 1 1 d . . .
H2A H 0.9915 0.6832 0.4953 0.043 Uiso 1 1 calc R . .
C3 C 0.9179(2) 0.68351(18) 0.4789(6) 0.0378(14) Uani 1 1 d . . .
C4 C 0.8793(2) 0.65644(17) 0.5166(6) 0.0325(12) Uani 1 1 d . . .
H4A H 0.8489 0.6679 0.4905 0.039 Uiso 1 1 calc R . .
C5 C 0.88439(18) 0.61220(17) 0.5929(7) 0.0305(11) Uani 1 1 d . . .
H5A H 0.8575 0.5939 0.6188 0.037 Uiso 1 1 calc R . .
C6 C 0.9090(3) 0.7316(2) 0.4005(8) 0.0165(13) Uani 0.75 1 d P . .
H4 H 0.877(2) 0.7452(19) 0.401(7) 0.032(15) Uiso 1 1 d . . .
C7 C 0.9457(3) 0.7614(3) 0.3579(9) 0.0153(14) Uani 0.75 1 d P . .
H3 H 0.972(3) 0.759(3) 0.342(10) 0.06(2) Uiso 1 1 d . . .
C7' C 0.9099(11) 0.7665(7) 0.346(3) 0.034(5) Uani 0.25 1 d P . .
C6' C 0.9447(15) 0.7375(12) 0.387(3) 0.043(10) Uani 0.25 1 d P . .
C8 C 0.9393(2) 0.80988(17) 0.2792(6) 0.0319(12) Uani 1 1 d . . .
C9 C 0.9797(2) 0.83257(17) 0.2248(6) 0.0334(12) Uani 1 1 d . . .
H9A H 1.0091 0.8174 0.2388 0.040 Uiso 1 1 calc R . .
C10 C 0.97815(18) 0.87729(15) 0.1497(6) 0.0259(10) Uani 1 1 d . . .
H10A H 1.0065 0.8919 0.1150 0.031 Uiso 1 1 calc R . .
C11 C 0.8952(2) 0.87968(18) 0.1774(6) 0.0325(12) Uani 1 1 d . . .
H11A H 0.8662 0.8954 0.1620 0.039 Uiso 1 1 calc R . .
C12 C 0.8966(2) 0.83401(19) 0.2553(6) 0.0398(15) Uani 1 1 d . . .
H12A H 0.8683 0.8196 0.2917 0.048 Uiso 1 1 calc R . .
F1 F 0.5994(7) 0.2188(3) -0.027(2) 0.321(12) Uani 1 1 d . . .
F2 F 0.6345(2) 0.2841(3) 0.049(2) 0.223(7) Uani 1 1 d . . .
F3 F 0.55901(17) 0.2817(2) 0.0320(10) 0.097(2) Uani 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
P1 0.0424(14) 0.0380(14) 0.154(3) 0.0177(17) 0.000 0.000
O1 0.0299(16) 0.0137(14) 0.0272(16) 0.0034(13) 0.0047(14) 0.0065(12)
O2 0.0313(17) 0.0156(15) 0.0233(15) 0.0061(13) -0.0067(14) -0.0025(13)
N1 0.035(2) 0.0160(17) 0.0100(16) -0.0017(14) -0.0035(15) 0.0058(15)
N2 0.035(2) 0.0170(17) 0.0151(17) 0.0006(15) -0.0009(17) -0.0127(17)
N3 0.017(2) 0.013(2) 0.012(2) 0.000 0.000 -0.0006(19)
C1 0.039(3) 0.018(2) 0.018(2) -0.0021(18) -0.0006(19) 0.0023(19)
C2 0.066(4) 0.023(2) 0.018(2) -0.003(2) 0.007(2) -0.010(2)
C3 0.074(4) 0.026(3) 0.013(2) -0.0045(19) -0.012(2) 0.029(3)
C4 0.043(3) 0.029(3) 0.025(3) -0.003(2) -0.009(2) 0.013(2)
C5 0.033(3) 0.030(3) 0.029(3) -0.006(2) -0.005(2) 0.007(2)
C6 0.020(3) 0.013(4) 0.017(3) 0.003(2) -0.001(2) -0.003(3)
C7 0.018(4) 0.012(4) 0.015(3) -0.003(3) 0.002(3) 0.001(3)
C7' 0.07(2) 0.021(12) 0.014(10) -0.005(8) 0.009(10) 0.003(11)
C6' 0.10(3) 0.010(13) 0.017(11) -0.011(10) 0.017(14) 0.016(17)
C8 0.059(3) 0.020(2) 0.018(2) -0.0018(19) 0.002(2) -0.008(2)
C9 0.061(4) 0.018(2) 0.020(2) 0.0020(19) -0.004(2) -0.002(2)
C10 0.041(3) 0.018(2) 0.019(2) 0.0030(19) -0.006(2) -0.0067(19)
C11 0.042(3) 0.031(3) 0.024(2) -0.010(2) 0.006(2) -0.011(2)
C12 0.067(4) 0.038(3) 0.014(2) -0.010(2) 0.016(2) -0.036(3)
F1 0.53(3) 0.108(7) 0.33(2) -0.068(10) 0.25(2) 0.033(12)
F2 0.073(4) 0.106(5) 0.491(19) 0.177(9) 0.009(7) 0.007(3)
F3 0.062(3) 0.095(4) 0.134(5) 0.049(3) -0.008(3) 0.006(3)

_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
P1 F1 1.428(13) . ?
P1 F1 1.428(13) 14_454 ?
P1 F2 1.527(7) . ?
P1 F2 1.527(7) 14_454 ?
P1 F3 1.548(5) 14_454 ?
P1 F3 1.548(5) . ?
O1 N1 1.318(5) . ?
O2 N2 1.326(5) . ?
O3 O3' 1.56(5) 14_453 ?
O3 O3' 1.56(5) . ?
O4 O4' 1.50(3) . ?
N1 C1 1.363(6) . ?
N1 C5 1.369(6) . ?
N2 C10 1.349(6) . ?
N2 C11 1.356(6) . ?
C1 C2 1.347(7) . ?
C2 C3 1.435(8) . ?
C3 C4 1.349(8) . ?
C3 C6 1.488(7) . ?
C3 C6' 1.82(4) . ?
C4 C5 1.369(7) . ?
C6 C6' 1.02(4) . ?
C6 C7' 1.06(2) . ?
C6 C7 1.361(10) . ?
C7 C6' 0.70(3) . ?
C7 C7' 1.02(3) . ?
C7 C8 1.490(11) . ?
C7' C6' 1.30(4) . ?
C7' C8 1.55(2) . ?
C8 C9 1.361(8) . ?
C8 C12 1.384(9) . ?
C9 C10 1.371(7) . ?
C11 C12 1.404(7) . ?

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 F1 174.6(17) . 14_454 ?
F1 P1 F2 93.4(8) . . ?
F1 P1 F2 82.9(10) 14_454 . ?
F1 P1 F2 82.9(10) . 14_454 ?
F1 P1 F2 93.4(8) 14_454 14_454 ?
F2 P1 F2 93.0(5) . 14_454 ?
F1 P1 F3 91.9(6) . 14_454 ?
F1 P1 F3 91.8(9) 14_454 14_454 ?
F2 P1 F3 174.7(6) . 14_454 ?
F2 P1 F3 87.2(3) 14_454 14_454 ?
F1 P1 F3 91.8(9) . . ?
F1 P1 F3 91.9(6) 14_454 . ?
F2 P1 F3 87.2(3) . . ?
F2 P1 F3 174.7(6) 14_454 . ?
F3 P1 F3 93.1(4) 14_454 . ?
O3' O3 O3' 95(4) 14_453 . ?
O1 N1 C1 120.1(4) . . ?
O1 N1 C5 119.5(4) . . ?
C1 N1 C5 120.4(4) . . ?
O2 N2 C10 120.3(4) . . ?
O2 N2 C11 120.4(4) . . ?
C10 N2 C11 119.3(4) . . ?
C2 C1 N1 120.6(5) . . ?
C1 C2 C3 119.3(5) . . ?
C4 C3 C2 118.9(4) . . ?
C4 C3 C6 117.1(5) . . ?
C2 C3 C6 123.9(6) . . ?
C4 C3 C6' 151.0(13) . . ?
C2 C3 C6' 90.1(13) . . ?
C6 C3 C6' 34.0(11) . . ?
C3 C4 C5 120.7(5) . . ?
N1 C5 C4 120.1(5) . . ?
C6' C6 C7' 78(2) . . ?
C6' C6 C7 30.2(17) . . ?
C7' C6 C7 47.8(16) . . ?
C6' C6 C3 91(2) . . ?
C7' C6 C3 169.0(19) . . ?
C7 C6 C3 121.2(7) . . ?
C6' C7 C7' 97(4) . . ?
C6' C7 C6 47(4) . . ?
C7' C7 C6 50.3(13) . . ?
C6' C7 C8 169(4) . . ?
C7' C7 C8 73.6(14) . . ?
C6 C7 C8 123.9(7) . . ?
C7 C7' C6 82.0(19) . . ?
C7 C7' C6' 32(2) . . ?
C6 C7' C6' 50(2) . . ?
C7 C7' C8 67.4(16) . . ?
C6 C7' C8 149(3) . . ?
C6' C7' C8 100(3) . . ?
C7 C6' C6 103(4) . . ?
C7 C6' C7' 51(3) . . ?
C6 C6' C7' 52(2) . . ?
C7 C6' C3 157(5) . . ?
C6 C6' C3 54.7(19) . . ?
C7' C6' C3 107(3) . . ?
C9 C8 C12 117.0(4) . . ?
C9 C8 C7 116.2(5) . . ?
C12 C8 C7 126.9(5) . . ?
C9 C8 C7' 154.6(11) . . ?
C12 C8 C7' 88.0(11) . . ?
C7 C8 C7' 39.1(10) . . ?
C8 C9 C10 121.3(6) . . ?
N2 C10 C9 121.8(5) . . ?
N2 C11 C12 119.2(5) . . ?
C8 C12 C11 121.5(5) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.115