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


data_global
_publ_contact_author_name        'Mary P. Neu'
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_year                    ?
_journal_page_first              ?

_publ_contact_author             
;
Mary P. Neu
MS J514
Los Alamos National Laboratory
Los Alamos, NM 87545
;
_publ_contact_author_phone       '505 667 7717'
_publ_contact_author_fax         '505 667 9905'
_publ_contact_author_email       mneu@lanl.gov
_publ_contact_letter             
;
Crystal data for [Pu(MECN)9](PF6)3
;
#=======================================================================

# 2.  AUTHOR LIST

loop_

_publ_author_name
_publ_author_address

'Mary P. Neu'
;
MS G739
Los Alamos National Lab
Los Alamos, NM 87545
;
'Alejandro Enriquez'
;
MS J514
Los Alamos National Lab
Los Alamos, NM 87545
;
'John H. Matonic'
;
MS E502
Los Alamos National Lab
Los Alamos, NM 87545
;
'Brian L. Scott'
;
MS J514
Los Alamos National Lab
Los Alamos, NM 87545
;

#======================================================================
data_xl
_database_code_CSD               207441

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H27 F18 N10 P3 Pu'
_chemical_formula_weight         1084.43

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'
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'
Pu Pu -9.4100 4.3056 '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                   11.9803(6)
_cell_length_b                   12.9930(6)
_cell_length_c                   13.3702(6)
_cell_angle_alpha                92.0600(10)
_cell_angle_beta                 96.4600(10)
_cell_angle_gamma                103.4470(10)
_cell_volume                     2007.14(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4192
_cell_measurement_theta_min      2
_cell_measurement_theta_max      23

_exptl_crystal_description       rectangular
_exptl_crystal_colour            blue-green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1036
_exptl_absorpt_coefficient_mu    1.873
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.34
_exptl_absorpt_correction_T_max  0.54
_exptl_absorpt_process_details   'SADABS (Shedrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      203
_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  'Siemens P4/PC'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15026
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         28.35
_reflns_number_total             8032
_reflns_number_gt                7046
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Siemens SMART (v. 4.202, Siemens 1996)'
_computing_cell_refinement       'Bruker SAINT (v. 5.00, Bruker 1998)'
_computing_data_reduction        'Bruker SAINT (v. 5.00, Bruker 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker AXS SHEXTL (v. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0308P)^2^+1.7667P] 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         8032
_refine_ls_number_parameters     561
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0768
_refine_ls_wR_factor_gt          0.0726
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001

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
Pu1 Pu 0.890985(15) 0.727455(13) 0.735430(12) 0.03634(6) Uani 1 1 d . . .
N1 N 1.1122(4) 0.7657(3) 0.7559(3) 0.0531(10) Uani 1 1 d . . .
N2 N 0.7571(4) 0.5522(4) 0.7767(3) 0.0529(10) Uani 1 1 d . . .
N3 N 0.7530(4) 0.6433(4) 0.5770(3) 0.0541(11) Uani 1 1 d . . .
N4 N 0.9798(4) 0.9157(4) 0.8166(3) 0.0542(11) Uani 1 1 d . . .
N5 N 0.9622(4) 0.5689(4) 0.6703(3) 0.0574(11) Uani 1 1 d . . .
N6 N 0.7655(4) 0.8528(3) 0.6678(3) 0.0531(11) Uani 1 1 d . . .
N7 N 0.7519(4) 0.7569(3) 0.8590(3) 0.0510(10) Uani 1 1 d . . .
N8 N 0.9711(4) 0.6769(3) 0.9080(3) 0.0499(10) Uani 1 1 d . . .
N9 N 0.9744(4) 0.8115(4) 0.5786(3) 0.0525(10) Uani 1 1 d . . .
N10 N 0.3867(8) 0.1052(9) 0.7489(7) 0.169(4) Uani 1 1 d . . .
P2 P 0.66404(13) 0.27692(12) 0.52066(11) 0.0563(4) Uani 1 1 d . . .
F7 F 0.7565(4) 0.2638(4) 0.6109(3) 0.1017(14) Uani 1 1 d . . .
F8 F 0.7615(4) 0.3442(4) 0.4640(3) 0.1082(14) Uani 1 1 d . . .
F9 F 0.5653(4) 0.2082(4) 0.5763(3) 0.1035(13) Uani 1 1 d . . .
F10 F 0.6759(4) 0.1708(3) 0.4638(3) 0.0987(13) Uani 1 1 d . . .
F11 F 0.5704(3) 0.2889(3) 0.4311(3) 0.0863(11) Uani 1 1 d . . .
F12 F 0.6495(4) 0.3804(3) 0.5773(3) 0.0902(12) Uani 1 1 d . . .
C1 C 1.2085(5) 0.7745(4) 0.7700(4) 0.0501(12) Uani 1 1 d . . .
C2 C 1.3324(4) 0.7839(6) 0.7878(5) 0.0724(18) Uani 1 1 d . . .
H2A H 1.3490 0.7180 0.7674 0.109 Uiso 1 1 calc R . .
H2B H 1.3588 0.8007 0.8583 0.109 Uiso 1 1 calc R . .
H2C H 1.3712 0.8392 0.7494 0.109 Uiso 1 1 calc R . .
C3 C 0.6972(4) 0.4784(4) 0.7967(3) 0.0449(11) Uani 1 1 d . . .
C4 C 0.6191(5) 0.3823(5) 0.8228(5) 0.0662(16) Uani 1 1 d . . .
H4A H 0.6218 0.3240 0.7776 0.099 Uiso 1 1 calc R . .
H4B H 0.5416 0.3920 0.8172 0.099 Uiso 1 1 calc R . .
H4C H 0.6422 0.3674 0.8908 0.099 Uiso 1 1 calc R . .
C5 C 0.6911(5) 0.6126(4) 0.5068(4) 0.0504(12) Uani 1 1 d . . .
C6 C 0.6126(6) 0.5724(6) 0.4156(4) 0.078(2) Uani 1 1 d . . .
H6A H 0.6432 0.6069 0.3588 0.117 Uiso 1 1 calc R . .
H6B H 0.5385 0.5864 0.4220 0.117 Uiso 1 1 calc R . .
H6C H 0.6044 0.4973 0.4057 0.117 Uiso 1 1 calc R . .
C7 C 1.0185(5) 0.9978(4) 0.8516(4) 0.0514(12) Uani 1 1 d . . .
C8 C 1.0681(6) 1.1042(5) 0.8993(5) 0.082(2) Uani 1 1 d . . .
H8A H 1.0086 1.1425 0.8997 0.122 Uiso 1 1 calc R . .
H8B H 1.1276 1.1410 0.8622 0.122 Uiso 1 1 calc R . .
H8C H 1.1006 1.0989 0.9674 0.122 Uiso 1 1 calc R . .
C9 C 0.9933(4) 0.4987(4) 0.6428(4) 0.0530(13) Uani 1 1 d . . .
C10 C 1.0323(6) 0.4085(6) 0.6055(5) 0.088(2) Uani 1 1 d . . .
H10A H 1.0460 0.3655 0.6603 0.131 Uiso 1 1 calc R . .
H10B H 1.1027 0.4332 0.5765 0.131 Uiso 1 1 calc R . .
H10C H 0.9742 0.3673 0.5552 0.131 Uiso 1 1 calc R . .
C11 C 0.7010(4) 0.9009(4) 0.6455(4) 0.0474(11) Uani 1 1 d . . .
C12 C 0.6179(5) 0.9639(5) 0.6179(5) 0.0670(16) Uani 1 1 d . . .
H12A H 0.5653 0.9295 0.5605 0.101 Uiso 1 1 calc R . .
H12B H 0.6581 1.0329 0.6015 0.101 Uiso 1 1 calc R . .
H12C H 0.5754 0.9709 0.6735 0.101 Uiso 1 1 calc R . .
C13 C 0.6798(4) 0.7573(4) 0.9074(4) 0.0469(11) Uani 1 1 d . . .
C14 C 0.5890(5) 0.7583(5) 0.9693(5) 0.0685(16) Uani 1 1 d . . .
H14A H 0.5192 0.7094 0.9394 0.103 Uiso 1 1 calc R . .
H14B H 0.5760 0.8284 0.9741 0.103 Uiso 1 1 calc R . .
H14C H 0.6112 0.7378 1.0354 0.103 Uiso 1 1 calc R . .
C15 C 1.0164(4) 0.6558(4) 0.9803(4) 0.0471(11) Uani 1 1 d . . .
C16 C 1.0762(5) 0.6268(5) 1.0724(4) 0.0686(16) Uani 1 1 d . . .
H16A H 1.0234 0.5741 1.1036 0.103 Uiso 1 1 calc R . .
H16B H 1.1047 0.6885 1.1180 0.103 Uiso 1 1 calc R . .
H16C H 1.1398 0.5988 1.0560 0.103 Uiso 1 1 calc R . .
C17 C 1.0174(4) 0.8505(4) 0.5149(4) 0.0498(12) Uani 1 1 d . . .
C18 C 1.0736(6) 0.9026(6) 0.4324(5) 0.080(2) Uani 1 1 d . . .
H18A H 1.0166 0.9203 0.3841 0.120 Uiso 1 1 calc R . .
H18B H 1.1119 0.8557 0.4003 0.120 Uiso 1 1 calc R . .
H18C H 1.1294 0.9662 0.4587 0.120 Uiso 1 1 calc R . .
C21 C 0.2806(7) 0.0974(7) 0.6835(6) 0.093(2) Uani 1 1 d . . .
C22 C 0.2026(9) 0.0908(12) 0.6356(9) 0.171(6) Uani 1 1 d . . .
P1 P 0.3026(11) 0.9185(10) 0.0767(10) 0.103(5) Uani 0.39(2) 1 d P A 1
F1 F 0.200(3) 0.947(5) 0.096(4) 0.31(2) Uani 0.39(2) 1 d P A 1
F2 F 0.295(3) 0.8531(14) 0.1618(12) 0.168(11) Uani 0.39(2) 1 d P A 1
F3 F 0.242(3) 0.8213(19) 0.0111(10) 0.162(10) Uani 0.39(2) 1 d P A 1
F4 F 0.366(3) 1.0230(13) 0.1381(10) 0.141(10) Uani 0.39(2) 1 d P A 1
F5 F 0.310(4) 0.9873(17) -0.0143(15) 0.190(11) Uani 0.39(2) 1 d P A 1
F6 F 0.414(2) 0.903(3) 0.063(3) 0.259(18) Uani 0.39(2) 1 d P A 1
P3 P 0.2663(8) 0.4576(6) 0.8625(4) 0.0716(17) Uani 0.607(12) 1 d P B 1
F13 F 0.2807(13) 0.4198(9) 0.9705(6) 0.136(5) Uani 0.607(12) 1 d P B 1
F14 F 0.2572(7) 0.5065(7) 0.7586(5) 0.092(3) Uani 0.607(12) 1 d P B 1
F15 F 0.3412(13) 0.3834(11) 0.8283(8) 0.136(5) Uani 0.607(12) 1 d P B 1
F16 F 0.1562(11) 0.3687(10) 0.8355(11) 0.168(5) Uani 0.607(12) 1 d P B 1
F17 F 0.3791(11) 0.5379(11) 0.8869(10) 0.194(9) Uani 0.607(12) 1 d P B 1
F18 F 0.1856(10) 0.5231(10) 0.8915(10) 0.144(6) Uani 0.607(12) 1 d P B 1
P1B P 0.3044(3) 0.9235(3) 0.0730(2) 0.0347(13) Uani 0.61(2) 1 d PG A 2
F2B F 0.2618(3) 0.8702(3) 0.1716(2) 0.130(8) Uani 0.61(2) 1 d PG A 2
F3B F 0.3885(6) 0.8468(5) 0.0629(3) 0.138(6) Uani 0.61(2) 1 d PG A 2
F5B F 0.2194(6) 0.9986(6) 0.0811(3) 0.138(6) Uani 0.61(2) 1 d PG A 2
F1B F 0.2032(6) 0.8414(4) 0.0046(3) 0.121(6) Uani 0.61(2) 1 d PG A 2
F4B F 0.3452(3) 0.9773(4) -0.0251(3) 0.103(5) Uani 0.61(2) 1 d PG A 2
F6B F 0.4025(5) 1.0064(4) 0.1412(3) 0.096(5) Uani 0.61(2) 1 d PG A 2
P3B P 0.2905(7) 0.4693(5) 0.8728(3) 0.061(3) Uani 0.393(12) 1 d PG B 3
F18B F 0.2815(10) 0.5769(6) 0.9291(3) 0.124(7) Uani 0.393(12) 1 d PG B 3
F17B F 0.1804(6) 0.4698(8) 0.7942(5) 0.35(3) Uani 0.393(12) 1 d PG B 3
F16B F 0.4010(8) 0.4713(6) 0.9486(4) 0.169(10) Uani 0.393(12) 1 d PG B 3
F15B F 0.3724(6) 0.5353(5) 0.8003(3) 0.162(11) Uani 0.393(12) 1 d PG B 3
F14B F 0.3013(10) 0.3629(5) 0.8174(4) 0.161(13) Uani 0.393(12) 1 d PG B 3
F13B F 0.2119(8) 0.4051(7) 0.9469(4) 0.219(16) Uani 0.393(12) 1 d PG B 3

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
Pu1 0.04274(10) 0.03020(10) 0.03859(9) 0.00351(6) 0.00833(6) 0.01198(7)
N1 0.052(3) 0.053(3) 0.057(3) 0.004(2) 0.011(2) 0.015(2)
N2 0.066(3) 0.037(3) 0.051(2) 0.0001(19) 0.012(2) 0.001(2)
N3 0.067(3) 0.049(3) 0.046(2) 0.0044(19) -0.001(2) 0.018(2)
N4 0.055(3) 0.044(3) 0.064(3) -0.004(2) 0.008(2) 0.013(2)
N5 0.056(3) 0.050(3) 0.069(3) -0.009(2) 0.008(2) 0.020(2)
N6 0.066(3) 0.051(3) 0.050(2) 0.0074(19) 0.011(2) 0.027(2)
N7 0.062(3) 0.044(3) 0.055(2) 0.0117(19) 0.020(2) 0.022(2)
N8 0.048(2) 0.050(3) 0.052(2) 0.0108(19) 0.0082(19) 0.011(2)
N9 0.054(2) 0.053(3) 0.053(2) 0.014(2) 0.016(2) 0.014(2)
N10 0.116(7) 0.229(12) 0.162(8) 0.049(8) 0.005(6) 0.038(7)
P2 0.0628(9) 0.0556(9) 0.0560(8) 0.0065(6) 0.0079(7) 0.0247(7)
F7 0.102(3) 0.134(4) 0.080(3) 0.014(2) -0.011(2) 0.060(3)
F8 0.085(3) 0.130(4) 0.104(3) 0.028(3) 0.029(2) 0.005(3)
F9 0.110(3) 0.099(3) 0.102(3) 0.020(2) 0.043(3) 0.009(3)
F10 0.143(4) 0.081(3) 0.091(3) -0.002(2) 0.017(3) 0.064(3)
F11 0.095(3) 0.088(3) 0.077(2) 0.000(2) -0.017(2) 0.039(2)
F12 0.122(3) 0.070(3) 0.082(2) -0.0177(19) -0.004(2) 0.039(2)
C1 0.048(3) 0.052(3) 0.052(3) 0.004(2) 0.009(2) 0.013(2)
C2 0.041(3) 0.094(5) 0.077(4) -0.015(4) 0.007(3) 0.009(3)
C3 0.052(3) 0.038(3) 0.044(3) 0.003(2) 0.003(2) 0.010(2)
C4 0.057(3) 0.059(4) 0.076(4) 0.017(3) 0.008(3) -0.002(3)
C5 0.055(3) 0.054(3) 0.049(3) 0.009(2) 0.010(2) 0.023(3)
C6 0.077(4) 0.112(6) 0.050(3) -0.004(3) -0.010(3) 0.040(4)
C7 0.053(3) 0.047(4) 0.055(3) -0.001(2) 0.007(2) 0.014(3)
C8 0.094(5) 0.049(4) 0.091(5) -0.019(3) 0.011(4) -0.001(4)
C9 0.052(3) 0.056(3) 0.053(3) -0.008(2) 0.002(2) 0.021(3)
C10 0.089(5) 0.091(5) 0.094(5) -0.032(4) -0.002(4) 0.055(4)
C11 0.056(3) 0.039(3) 0.049(3) 0.007(2) 0.007(2) 0.015(2)
C12 0.065(4) 0.058(4) 0.082(4) 0.009(3) -0.006(3) 0.027(3)
C13 0.054(3) 0.038(3) 0.051(3) 0.005(2) 0.009(2) 0.015(2)
C14 0.058(3) 0.066(4) 0.089(4) 0.013(3) 0.032(3) 0.020(3)
C15 0.045(3) 0.042(3) 0.053(3) 0.007(2) 0.005(2) 0.009(2)
C16 0.067(4) 0.065(4) 0.069(4) 0.019(3) -0.010(3) 0.011(3)
C17 0.050(3) 0.045(3) 0.059(3) 0.010(2) 0.013(2) 0.019(2)
C18 0.085(5) 0.087(5) 0.089(5) 0.043(4) 0.049(4) 0.039(4)
C21 0.080(5) 0.108(7) 0.086(5) 0.002(4) 0.004(4) 0.013(5)
C22 0.082(6) 0.252(16) 0.155(10) 0.036(10) -0.034(7) 0.012(8)
P1 0.114(10) 0.072(8) 0.135(10) 0.005(7) 0.008(7) 0.049(7)
F1 0.18(3) 0.38(5) 0.46(6) 0.05(5) 0.15(3) 0.21(3)
F2 0.36(3) 0.043(9) 0.079(11) 0.023(7) -0.030(14) 0.025(15)
F3 0.23(2) 0.126(14) 0.053(8) -0.030(8) 0.025(9) -0.112(14)
F4 0.32(3) 0.036(8) 0.066(9) 0.002(6) 0.031(11) 0.035(14)
F5 0.28(3) 0.134(19) 0.101(14) 0.052(13) -0.074(15) -0.018(17)
F6 0.105(13) 0.19(3) 0.49(5) -0.11(3) 0.010(19) 0.096(17)
P3 0.062(3) 0.093(4) 0.068(3) 0.031(3) 0.018(2) 0.025(2)
F13 0.226(15) 0.168(10) 0.063(4) 0.047(5) 0.052(7) 0.124(10)
F14 0.104(6) 0.120(7) 0.060(4) 0.028(4) 0.008(4) 0.043(5)
F15 0.147(8) 0.181(12) 0.130(9) 0.053(8) 0.063(6) 0.114(8)
F16 0.148(10) 0.135(10) 0.202(13) 0.037(8) 0.033(9) -0.018(7)
F17 0.131(10) 0.181(13) 0.201(13) 0.088(11) -0.082(10) -0.065(9)
F18 0.146(10) 0.171(11) 0.173(11) 0.080(9) 0.081(9) 0.111(10)
P1B 0.033(2) 0.036(3) 0.033(2) 0.0010(15) 0.0075(14) 0.0027(18)
F2B 0.189(12) 0.103(11) 0.062(6) -0.010(5) 0.062(7) -0.055(9)
F3B 0.161(12) 0.095(8) 0.192(11) 0.004(7) 0.039(8) 0.093(9)
F5B 0.108(8) 0.096(8) 0.228(15) -0.008(7) 0.024(8) 0.063(6)
F1B 0.100(7) 0.114(10) 0.105(9) 0.005(7) -0.026(6) -0.045(6)
F4B 0.145(9) 0.079(7) 0.064(6) 0.001(5) 0.051(7) -0.034(6)
F6B 0.071(5) 0.094(10) 0.094(7) 0.003(5) -0.026(4) -0.024(5)
P3B 0.059(5) 0.087(6) 0.042(3) 0.005(3) 0.013(3) 0.028(4)
F18B 0.178(16) 0.174(15) 0.062(6) -0.017(7) 0.023(8) 0.126(14)
F17B 0.21(3) 0.44(5) 0.28(4) 0.14(4) -0.21(3) -0.06(3)
F16B 0.129(14) 0.175(18) 0.20(2) -0.041(14) -0.061(13) 0.070(13)
F15B 0.26(3) 0.099(11) 0.163(17) 0.042(11) 0.152(19) 0.048(14)
F14B 0.32(3) 0.029(8) 0.106(12) -0.020(7) 0.105(15) -0.042(11)
F13B 0.108(15) 0.38(4) 0.20(3) 0.16(2) 0.104(17) 0.048(18)

_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
Pu1 N7 2.554(4) . ?
Pu1 N1 2.561(4) . ?
Pu1 N8 2.565(4) . ?
Pu1 N5 2.566(4) . ?
Pu1 N3 2.573(4) . ?
Pu1 N4 2.575(5) . ?
Pu1 N2 2.579(5) . ?
Pu1 N6 2.582(4) . ?
Pu1 N9 2.591(4) . ?
N1 C1 1.126(6) . ?
N2 C3 1.118(6) . ?
N3 C5 1.126(6) . ?
N4 C7 1.121(6) . ?
N5 C9 1.128(6) . ?
N6 C11 1.124(6) . ?
N7 C13 1.137(6) . ?
N8 C15 1.129(6) . ?
N9 C17 1.121(6) . ?
N10 C21 1.440(11) . ?
P2 F8 1.572(4) . ?
P2 F12 1.574(4) . ?
P2 F9 1.582(4) . ?
P2 F11 1.584(4) . ?
P2 F7 1.586(4) . ?
P2 F10 1.593(4) . ?
C1 C2 1.452(7) . ?
C3 C4 1.456(8) . ?
C5 C6 1.453(8) . ?
C7 C8 1.463(8) . ?
C9 C10 1.450(7) . ?
C11 C12 1.454(7) . ?
C13 C14 1.441(7) . ?
C15 C16 1.459(7) . ?
C17 C18 1.462(8) . ?
C21 C22 1.055(11) . ?
P1 F1 1.410(18) . ?
P1 F6 1.426(18) . ?
P1 F2 1.443(16) . ?
P1 F3 1.498(15) . ?
P1 F5 1.533(17) . ?
P1 F4 1.547(16) . ?
P3 F17 1.498(11) . ?
P3 F18 1.501(10) . ?
P3 F16 1.536(14) . ?
P3 F13 1.546(9) . ?
P3 F14 1.551(8) . ?
P3 F15 1.553(9) . ?
P1B F6B 1.5724 . ?
P1B F5B 1.5747 . ?
P1B F4B 1.5810 . ?
P1B F3B 1.5855 . ?
P1B F1B 1.5880 . ?
P1B F2B 1.5907 . ?
P3B F16B 1.5689 . ?
P3B F13B 1.5721 . ?
P3B F14B 1.5838 . ?
P3B F15B 1.5875 . ?
P3B F17B 1.5930 . ?
P3B F18B 1.5954 . ?

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
N7 Pu1 N1 131.00(14) . . ?
N7 Pu1 N8 73.30(13) . . ?
N1 Pu1 N8 68.65(13) . . ?
N7 Pu1 N5 135.92(15) . . ?
N1 Pu1 N5 68.23(14) . . ?
N8 Pu1 N5 83.24(14) . . ?
N7 Pu1 N3 102.63(14) . . ?
N1 Pu1 N3 126.37(13) . . ?
N8 Pu1 N3 140.13(14) . . ?
N5 Pu1 N3 72.69(14) . . ?
N7 Pu1 N4 75.45(14) . . ?
N1 Pu1 N4 69.57(13) . . ?
N8 Pu1 N4 81.60(14) . . ?
N5 Pu1 N4 137.80(14) . . ?
N3 Pu1 N4 136.90(14) . . ?
N7 Pu1 N2 67.67(14) . . ?
N1 Pu1 N2 124.52(14) . . ?
N8 Pu1 N2 71.95(14) . . ?
N5 Pu1 N2 69.79(15) . . ?
N3 Pu1 N2 70.11(14) . . ?
N4 Pu1 N2 139.26(14) . . ?
N7 Pu1 N6 68.43(13) . . ?
N1 Pu1 N6 126.53(14) . . ?
N8 Pu1 N6 137.20(13) . . ?
N5 Pu1 N6 138.58(14) . . ?
N3 Pu1 N6 68.61(14) . . ?
N4 Pu1 N6 71.02(14) . . ?
N2 Pu1 N6 108.94(15) . . ?
N7 Pu1 N9 138.97(13) . . ?
N1 Pu1 N9 68.34(13) . . ?
N8 Pu1 N9 136.96(13) . . ?
N5 Pu1 N9 82.50(15) . . ?
N3 Pu1 N9 71.48(14) . . ?
N4 Pu1 N9 82.32(14) . . ?
N2 Pu1 N9 137.70(14) . . ?
N6 Pu1 N9 71.89(13) . . ?
C1 N1 Pu1 173.6(4) . . ?
C3 N2 Pu1 177.5(4) . . ?
C5 N3 Pu1 175.5(4) . . ?
C7 N4 Pu1 179.7(5) . . ?
C9 N5 Pu1 179.2(5) . . ?
C11 N6 Pu1 171.3(4) . . ?
C13 N7 Pu1 170.3(4) . . ?
C15 N8 Pu1 173.2(4) . . ?
C17 N9 Pu1 175.3(4) . . ?
F8 P2 F12 90.8(3) . . ?
F8 P2 F9 179.2(3) . . ?
F12 P2 F9 89.9(2) . . ?
F8 P2 F11 89.5(2) . . ?
F12 P2 F11 90.4(2) . . ?
F9 P2 F11 90.0(2) . . ?
F8 P2 F7 91.2(3) . . ?
F12 P2 F7 89.7(2) . . ?
F9 P2 F7 89.2(3) . . ?
F11 P2 F7 179.3(3) . . ?
F8 P2 F10 90.4(3) . . ?
F12 P2 F10 178.7(3) . . ?
F9 P2 F10 88.9(3) . . ?
F11 P2 F10 89.1(2) . . ?
F7 P2 F10 90.8(2) . . ?
N1 C1 C2 179.0(6) . . ?
N2 C3 C4 179.9(7) . . ?
N3 C5 C6 179.1(6) . . ?
N4 C7 C8 178.7(6) . . ?
N5 C9 C10 179.0(6) . . ?
N6 C11 C12 179.3(6) . . ?
N7 C13 C14 179.6(7) . . ?
N8 C15 C16 178.6(6) . . ?
N9 C17 C18 179.3(6) . . ?
C22 C21 N10 179.4(14) . . ?
F1 P1 F6 172(2) . . ?
F1 P1 F2 90(2) . . ?
F6 P1 F2 92(2) . . ?
F1 P1 F3 95(2) . . ?
F6 P1 F3 92.8(17) . . ?
F2 P1 F3 87.8(11) . . ?
F1 P1 F5 90(2) . . ?
F6 P1 F5 88.0(19) . . ?
F2 P1 F5 179.5(14) . . ?
F3 P1 F5 91.7(12) . . ?
F1 P1 F4 85(2) . . ?
F6 P1 F4 87.0(16) . . ?
F2 P1 F4 95.9(11) . . ?
F3 P1 F4 176.2(11) . . ?
F5 P1 F4 84.6(11) . . ?
F17 P3 F18 99.6(10) . . ?
F17 P3 F16 175.3(10) . . ?
F18 P3 F16 85.1(9) . . ?
F17 P3 F13 89.3(9) . . ?
F18 P3 F13 91.5(6) . . ?
F16 P3 F13 90.3(8) . . ?
F17 P3 F14 86.3(6) . . ?
F18 P3 F14 86.1(6) . . ?
F16 P3 F14 94.4(8) . . ?
F13 P3 F14 174.5(9) . . ?
F17 P3 F15 84.8(10) . . ?
F18 P3 F15 175.5(11) . . ?
F16 P3 F15 90.5(9) . . ?
F13 P3 F15 89.6(6) . . ?
F14 P3 F15 93.2(5) . . ?
F6B P1B F5B 90.1 . . ?
F6B P1B F4B 90.7 . . ?
F5B P1B F4B 90.4 . . ?
F6B P1B F3B 90.9 . . ?
F5B P1B F3B 178.8 . . ?
F4B P1B F3B 89.2 . . ?
F6B P1B F1B 178.6 . . ?
F5B P1B F1B 88.5 . . ?
F4B P1B F1B 89.5 . . ?
F3B P1B F1B 90.4 . . ?
F6B P1B F2B 89.5 . . ?
F5B P1B F2B 88.8 . . ?
F4B P1B F2B 179.2 . . ?
F3B P1B F2B 91.6 . . ?
F1B P1B F2B 90.3 . . ?
F16B P3B F13B 90.3 . . ?
F16B P3B F14B 91.0 . . ?
F13B P3B F14B 91.0 . . ?
F16B P3B F15B 88.4 . . ?
F13B P3B F15B 178.5 . . ?
F14B P3B F15B 89.6 . . ?
F16B P3B F17B 178.4 . . ?
F13B P3B F17B 91.3 . . ?
F14B P3B F17B 89.3 . . ?
F15B P3B F17B 90.1 . . ?
F16B P3B F18B 88.3 . . ?
F13B P3B F18B 89.3 . . ?
F14B P3B F18B 179.2 . . ?
F15B P3B F18B 90.1 . . ?
F17B P3B F18B 91.3 . . ?

_diffrn_measured_fraction_theta_max 0.801
_diffrn_reflns_theta_full        28.35
_diffrn_measured_fraction_theta_full 0.801
_refine_diff_density_max         1.114
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.101

data_ccd615
_database_code_CSD               207442

#======================================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H27 I3 N9 O0 U'
_chemical_formula_weight         988.22

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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3'

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

_cell_length_a                   10.974(4)
_cell_length_b                   10.974(4)
_cell_length_c                   24.475(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2552.7(16)
_cell_formula_units_Z            3
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       irregular
_exptl_crystal_colour            dark
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1347
_exptl_absorpt_coefficient_mu    7.508
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.1532
_exptl_absorpt_correction_T_max  0.3151
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      203(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  'Bruker P4/CCD'
_diffrn_measurement_method       '/f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        '< 2'
_diffrn_reflns_number            6253
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         28.47
_reflns_number_total             1329
_reflns_number_gt                1141
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0387P)^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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1329
_refine_ls_number_parameters     89
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0737
_refine_ls_wR_factor_ref         0.1296
_refine_ls_wR_factor_gt          0.1273
_refine_ls_goodness_of_fit_ref   2.052
_refine_ls_restrained_S_all      2.052
_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
U1 U 0.6667 0.3333 0.3333 0.0475(3) Uani 1 6 d S . .
I2 I 0.6667 0.3333 0.09592(3) 0.0489(3) Uani 1 3 d S . .
I3 I 1.0000 0.0000 0.55212(17) 0.0632(8) Uani 0.33 3 d SP . .
I4 I 1.0000 0.0000 0.5000 0.104(3) Uani 0.33 6 d SP . .
N1 N 0.8312(14) 0.3342(14) 0.4095(6) 0.058(3) Uani 0.50 1 d P . .
N2 N 0.6673(16) 0.0921(16) 0.3334(6) 0.070(4) Uani 0.50 1 d P . .
N3 N 0.6649(14) 0.1671(16) 0.4097(6) 0.062(4) Uani 0.50 1 d P . .
C1 C 0.8990(16) 0.3346(15) 0.4456(7) 0.052(4) Uani 0.50 1 d P . .
C2 C 0.996(2) 0.342(2) 0.4892(7) 0.049(5) Uani 0.50 1 d P . .
C3 C 0.663(3) -0.007(2) 0.3337(9) 0.092(8) Uani 0.50 1 d P . .
C4 C 0.6667 -0.1667 0.3333 0.190(13) Uani 1 2 d S . .
C5 C 0.6671(15) 0.1018(15) 0.4460(7) 0.050(4) Uani 0.50 1 d P . .
C6 C 0.658(2) 0.007(2) 0.4883(7) 0.050(5) Uani 0.50 1 d P . .

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
U1 0.0517(3) 0.0517(3) 0.0390(4) 0.000 0.000 0.02586(17)
I2 0.0483(3) 0.0483(3) 0.0501(6) 0.000 0.000 0.02417(17)
I3 0.0504(11) 0.0504(11) 0.089(2) 0.000 0.000 0.0252(6)
I4 0.0292(15) 0.0292(15) 0.255(11) 0.000 0.000 0.0146(8)
N1 0.054(8) 0.068(9) 0.055(8) 0.000(7) -0.001(6) 0.032(7)
N2 0.101(12) 0.071(10) 0.049(8) 0.005(7) 0.011(8) 0.050(9)
N3 0.069(9) 0.074(9) 0.056(8) -0.005(7) -0.004(7) 0.047(8)
C1 0.042(8) 0.042(8) 0.071(11) 0.000(7) 0.004(8) 0.020(7)
C2 0.075(12) 0.074(12) 0.013(8) -0.009(9) -0.009(9) 0.049(10)
C3 0.14(2) 0.088(16) 0.072(13) 0.038(11) 0.066(14) 0.079(16)
C4 0.22(3) 0.17(2) 0.20(3) 0.05(2) 0.11(2) 0.11(2)
C5 0.038(8) 0.040(8) 0.076(11) -0.014(8) -0.010(7) 0.022(7)
C6 0.074(12) 0.079(12) 0.014(8) 0.007(10) -0.008(9) 0.051(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
U1 N1 2.592(14) . ?
U1 N1 2.592(14) 3_665 ?
U1 N1 2.592(14) 2_655 ?
U1 N1 2.592(14) 16_655 ?
U1 N1 2.592(14) 18_545 ?
U1 N1 2.592(14) 17 ?
U1 N3 2.604(15) . ?
U1 N3 2.604(15) 2_655 ?
U1 N3 2.604(15) 3_665 ?
U1 N3 2.604(15) 16_655 ?
U1 N3 2.604(15) 17 ?
U1 N3 2.604(15) 18_545 ?
U1 N2 2.651(16) 16_655 ?
U1 N2 2.651(16) . ?
U1 N2 2.651(16) 17 ?
U1 N2 2.651(16) 2_655 ?
U1 N2 2.651(16) 3_665 ?
U1 N2 2.651(16) 18_545 ?
I3 I4 1.276(4) . ?
I3 I3 2.551(8) 10_756 ?
I4 I3 1.276(4) 10_756 ?
N1 C1 1.15(2) . ?
N1 N3 1.79(2) 2_655 ?
N1 N3 1.83(2) . ?
N2 C3 1.06(2) . ?
N3 C5 1.15(2) . ?
N3 N1 1.79(2) 3_665 ?
C1 C2 1.48(2) . ?
C1 C6 1.96(3) 11_666 ?
C2 C6 0.559(14) 11_666 ?
C2 C5 1.93(3) 11_666 ?
C3 C4 1.78(2) . ?
C4 C3 1.78(2) 16_645 ?
C5 C6 1.44(2) . ?
C5 C2 1.93(3) 12_546 ?
C6 C2 0.559(14) 12_546 ?
C6 C1 1.96(3) 12_546 ?

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
N1 U1 N1 74.0(5) . 3_665 ?
N1 U1 N1 74.0(5) . 2_655 ?
N1 U1 N1 74.0(5) 3_665 2_655 ?
N1 U1 N1 179.998(2) . 16_655 ?
N1 U1 N1 106.0(5) 3_665 16_655 ?
N1 U1 N1 106.0(5) 2_655 16_655 ?
N1 U1 N1 106.0(5) . 18_545 ?
N1 U1 N1 179.999(1) 3_665 18_545 ?
N1 U1 N1 106.0(5) 2_655 18_545 ?
N1 U1 N1 74.0(5) 16_655 18_545 ?
N1 U1 N1 106.0(5) . 17 ?
N1 U1 N1 106.0(5) 3_665 17 ?
N1 U1 N1 179.999(2) 2_655 17 ?
N1 U1 N1 74.0(5) 16_655 17 ?
N1 U1 N1 74.0(5) 18_545 17 ?
N1 U1 N3 41.2(5) . . ?
N1 U1 N3 40.2(4) 3_665 . ?
N1 U1 N3 88.2(4) 2_655 . ?
N1 U1 N3 138.8(5) 16_655 . ?
N1 U1 N3 139.8(4) 18_545 . ?
N1 U1 N3 91.8(4) 17 . ?
N1 U1 N3 40.2(4) . 2_655 ?
N1 U1 N3 88.2(4) 3_665 2_655 ?
N1 U1 N3 41.2(5) 2_655 2_655 ?
N1 U1 N3 139.8(4) 16_655 2_655 ?
N1 U1 N3 91.8(4) 18_545 2_655 ?
N1 U1 N3 138.8(5) 17 2_655 ?
N3 U1 N3 74.2(5) . 2_655 ?
N1 U1 N3 88.2(4) . 3_665 ?
N1 U1 N3 41.2(5) 3_665 3_665 ?
N1 U1 N3 40.2(4) 2_655 3_665 ?
N1 U1 N3 91.8(4) 16_655 3_665 ?
N1 U1 N3 138.8(5) 18_545 3_665 ?
N1 U1 N3 139.8(4) 17 3_665 ?
N3 U1 N3 74.2(5) . 3_665 ?
N3 U1 N3 74.2(5) 2_655 3_665 ?
N1 U1 N3 138.8(5) . 16_655 ?
N1 U1 N3 139.8(4) 3_665 16_655 ?
N1 U1 N3 91.8(4) 2_655 16_655 ?
N1 U1 N3 41.2(5) 16_655 16_655 ?
N1 U1 N3 40.2(4) 18_545 16_655 ?
N1 U1 N3 88.2(4) 17 16_655 ?
N3 U1 N3 179.998(2) . 16_655 ?
N3 U1 N3 105.8(5) 2_655 16_655 ?
N3 U1 N3 105.8(5) 3_665 16_655 ?
N1 U1 N3 139.8(4) . 17 ?
N1 U1 N3 91.8(4) 3_665 17 ?
N1 U1 N3 138.8(5) 2_655 17 ?
N1 U1 N3 40.2(4) 16_655 17 ?
N1 U1 N3 88.2(4) 18_545 17 ?
N1 U1 N3 41.2(5) 17 17 ?
N3 U1 N3 105.8(5) . 17 ?
N3 U1 N3 179.999(1) 2_655 17 ?
N3 U1 N3 105.8(5) 3_665 17 ?
N3 U1 N3 74.2(5) 16_655 17 ?
N1 U1 N3 91.8(4) . 18_545 ?
N1 U1 N3 138.8(5) 3_665 18_545 ?
N1 U1 N3 139.8(4) 2_655 18_545 ?
N1 U1 N3 88.2(4) 16_655 18_545 ?
N1 U1 N3 41.2(5) 18_545 18_545 ?
N1 U1 N3 40.2(4) 17 18_545 ?
N3 U1 N3 105.8(5) . 18_545 ?
N3 U1 N3 105.8(5) 2_655 18_545 ?
N3 U1 N3 180.0(10) 3_665 18_545 ?
N3 U1 N3 74.2(5) 16_655 18_545 ?
N3 U1 N3 74.2(5) 17 18_545 ?
N1 U1 N2 110.3(4) . 16_655 ?
N1 U1 N2 110.5(4) 3_665 16_655 ?
N1 U1 N2 46.0(4) 2_655 16_655 ?
N1 U1 N2 69.7(4) 16_655 16_655 ?
N1 U1 N2 69.5(4) 18_545 16_655 ?
N1 U1 N2 134.0(4) 17 16_655 ?
N3 U1 N2 134.2(4) . 16_655 ?
N3 U1 N2 70.1(4) 2_655 16_655 ?
N3 U1 N2 69.2(4) 3_665 16_655 ?
N3 U1 N2 45.8(4) 16_655 16_655 ?
N3 U1 N2 109.9(4) 17 16_655 ?
N3 U1 N2 110.8(4) 18_545 16_655 ?
N1 U1 N2 69.7(4) . . ?
N1 U1 N2 69.5(4) 3_665 . ?
N1 U1 N2 134.0(4) 2_655 . ?
N1 U1 N2 110.3(4) 16_655 . ?
N1 U1 N2 110.5(4) 18_545 . ?
N1 U1 N2 46.0(4) 17 . ?
N3 U1 N2 45.8(4) . . ?
N3 U1 N2 109.9(4) 2_655 . ?
N3 U1 N2 110.8(4) 3_665 . ?
N3 U1 N2 134.2(4) 16_655 . ?
N3 U1 N2 70.1(4) 17 . ?
N3 U1 N2 69.2(4) 18_545 . ?
N2 U1 N2 179.999(3) 16_655 . ?
N1 U1 N2 110.5(4) . 17 ?
N1 U1 N2 46.0(4) 3_665 17 ?
N1 U1 N2 110.3(4) 2_655 17 ?
N1 U1 N2 69.5(4) 16_655 17 ?
N1 U1 N2 134.0(4) 18_545 17 ?
N1 U1 N2 69.7(4) 17 17 ?
N3 U1 N2 69.2(4) . 17 ?
N3 U1 N2 134.2(4) 2_655 17 ?
N3 U1 N2 70.1(4) 3_665 17 ?
N3 U1 N2 110.8(4) 16_655 17 ?
N3 U1 N2 45.8(4) 17 17 ?
N3 U1 N2 109.9(4) 18_545 17 ?
N2 U1 N2 120.001(3) 16_655 17 ?
N2 U1 N2 59.999(4) . 17 ?
N1 U1 N2 69.5(4) . 2_655 ?
N1 U1 N2 134.0(4) 3_665 2_655 ?
N1 U1 N2 69.7(4) 2_655 2_655 ?
N1 U1 N2 110.5(4) 16_655 2_655 ?
N1 U1 N2 46.0(4) 18_545 2_655 ?
N1 U1 N2 110.3(4) 17 2_655 ?
N3 U1 N2 110.8(4) . 2_655 ?
N3 U1 N2 45.8(4) 2_655 2_655 ?
N3 U1 N2 109.9(4) 3_665 2_655 ?
N3 U1 N2 69.2(4) 16_655 2_655 ?
N3 U1 N2 134.2(4) 17 2_655 ?
N3 U1 N2 70.1(4) 18_545 2_655 ?
N2 U1 N2 60.000(3) 16_655 2_655 ?
N2 U1 N2 120.000(4) . 2_655 ?
N2 U1 N2 179.998(1) 17 2_655 ?
N1 U1 N2 134.0(4) . 3_665 ?
N1 U1 N2 69.7(4) 3_665 3_665 ?
N1 U1 N2 69.5(4) 2_655 3_665 ?
N1 U1 N2 46.0(4) 16_655 3_665 ?
N1 U1 N2 110.3(4) 18_545 3_665 ?
N1 U1 N2 110.5(4) 17 3_665 ?
N3 U1 N2 109.9(4) . 3_665 ?
N3 U1 N2 110.8(4) 2_655 3_665 ?
N3 U1 N2 45.8(4) 3_665 3_665 ?
N3 U1 N2 70.1(4) 16_655 3_665 ?
N3 U1 N2 69.2(4) 17 3_665 ?
N3 U1 N2 134.2(4) 18_545 3_665 ?
N2 U1 N2 60.001(4) 16_655 3_665 ?
N2 U1 N2 120.000(4) . 3_665 ?
N2 U1 N2 60.001(3) 17 3_665 ?
N2 U1 N2 120.000(3) 2_655 3_665 ?
N1 U1 N2 46.0(4) . 18_545 ?
N1 U1 N2 110.3(4) 3_665 18_545 ?
N1 U1 N2 110.5(4) 2_655 18_545 ?
N1 U1 N2 134.0(4) 16_655 18_545 ?
N1 U1 N2 69.7(4) 18_545 18_545 ?
N1 U1 N2 69.5(4) 17 18_545 ?
N3 U1 N2 70.1(4) . 18_545 ?
N3 U1 N2 69.2(4) 2_655 18_545 ?
N3 U1 N2 134.2(4) 3_665 18_545 ?
N3 U1 N2 109.9(4) 16_655 18_545 ?
N3 U1 N2 110.8(4) 17 18_545 ?
N3 U1 N2 45.8(4) 18_545 18_545 ?
N2 U1 N2 120.000(4) 16_655 18_545 ?
N2 U1 N2 60.000(4) . 18_545 ?
N2 U1 N2 119.998(2) 17 18_545 ?
N2 U1 N2 60.001(3) 2_655 18_545 ?
N2 U1 N2 180.0(7) 3_665 18_545 ?
I4 I3 I3 0.0 . 10_756 ?
I3 I4 I3 180.000(2) 10_756 . ?
C1 N1 N3 108.2(13) . 2_655 ?
C1 N1 N3 108.6(13) . . ?
N3 N1 N3 120.7(11) 2_655 . ?
C1 N1 U1 176.0(12) . . ?
N3 N1 U1 70.3(7) 2_655 . ?
N3 N1 U1 69.7(6) . . ?
C3 N2 U1 177.4(18) . . ?
C5 N3 N1 109.8(13) . 3_665 ?
C5 N3 N1 107.8(13) . . ?
N1 N3 N1 119.3(11) 3_665 . ?
C5 N3 U1 174.9(13) . . ?
N1 N3 U1 69.5(6) 3_665 . ?
N1 N3 U1 69.0(7) . . ?
N1 C1 C2 175.4(18) . . ?
N1 C1 C6 173.1(15) . 11_666 ?
C2 C1 C6 9.5(12) . 11_666 ?
C6 C2 C1 144(5) 11_666 . ?
C6 C2 C5 24(4) 11_666 11_666 ?
C1 C2 C5 148.2(15) . 11_666 ?
N2 C3 C4 176(2) . . ?
C3 C4 C3 179.998(4) . 16_645 ?
N3 C5 C6 173.5(17) . . ?
N3 C5 C2 173.2(15) . 12_546 ?
C6 C5 C2 9.3(13) . 12_546 ?
C2 C6 C5 146(5) 12_546 . ?
C2 C6 C1 26(4) 12_546 12_546 ?
C5 C6 C1 149.1(16) . 12_546 ?

_diffrn_measured_fraction_theta_max 0.925
_diffrn_reflns_theta_full        28.47
_diffrn_measured_fraction_theta_full 0.925
_refine_diff_density_max         2.273
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.178