#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:03:44 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178800 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/54/4105428.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4105428
loop_
_publ_author_name
'David D. Schnaars'
'Guang Wu'
'Trevor W. Hayton'
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_contact_author_name        'Trevor W Hayton'
_publ_section_title
;
 Reduction of Pentavalent Uranyl to U(IV) Facilitated by Oxo
 Functionalization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17532
_journal_page_last               17533
_journal_paper_doi               10.1021/ja906880d
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C94 H85 B2 Cl2 Co F30 N O4 U'
_chemical_formula_weight         2252.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.010(2)
_cell_angle_beta                 97.933(2)
_cell_angle_gamma                91.626(2)
_cell_formula_units_Z            2
_cell_length_a                   13.443(2)
_cell_length_b                   16.074(2)
_cell_length_c                   21.500(3)
_cell_measurement_temperature    150(2)
_cell_volume                     4524.7(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_sigmaI/netI    0.2035
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37164
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         0.97
_exptl_absorpt_coefficient_mu    2.144
_exptl_absorpt_correction_T_max  0.32753
_exptl_absorpt_correction_T_min  0.25815
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       Block
_exptl_crystal_F_000             2242
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.160
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         18084
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0812P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1868
_reflns_number_gt                8421
_reflns_number_total             18084
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906880d_si_002_1.cif
_cod_data_source_block           5
_cod_original_cell_volume        4524.7(12)
_cod_database_code               4105428
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C64 C 0.6933(16) 0.8645(16) 0.9715(11) 0.166(9) Uani 1 1 d U
C93B C 0.550(2) 0.833(6) 0.057(4) 0.242(19) Uiso 0.30 1 d PD
B2 B 0.5254(8) 0.7488(7) 0.6617(5) 0.032(3) Uani 1 1 d .
B1 B 0.9492(9) 0.7726(7) 0.8386(5) 0.035(3) Uani 1 1 d .
C85 C 0.8395(9) 0.5230(8) 0.1913(6) 0.069(4) Uani 1 1 d .
H85A H 0.8043 0.4685 0.1745 0.082 Uiso 1 1 calc R
H85B H 0.8849 0.5173 0.2293 0.082 Uiso 1 1 calc R
C37 C 0.6383(7) 0.5698(6) 0.8561(4) 0.031(2) Uani 1 1 d .
C53 C 0.6571(7) 0.4906(6) 0.6840(4) 0.033(2) Uani 1 1 d .
H53 H 0.6307 0.4431 0.6545 0.039 Uiso 1 1 calc R
C47 C 0.5866(7) 0.4173(6) 0.7609(5) 0.035(2) Uani 1 1 d .
C19 C 0.5990(7) 0.7549(6) 0.6068(4) 0.033(2) Uani 1 1 d .
C20 C 0.7019(7) 0.7737(6) 0.6200(5) 0.036(2) Uani 1 1 d .
C52 C 0.6198(8) 0.3851(6) 0.8147(5) 0.045(3) Uani 1 1 d .
H52 H 0.6717 0.4135 0.8445 0.054 Uiso 1 1 calc R
C38 C 0.5436(8) 0.5851(6) 0.8732(5) 0.041(3) Uani 1 1 d .
C39 C 0.5349(8) 0.5938(7) 0.9373(5) 0.053(3) Uani 1 1 d .
H39 H 0.4714 0.6011 0.9495 0.063 Uiso 1 1 calc R
C42 C 0.7210(7) 0.5653(6) 0.9024(5) 0.037(2) Uani 1 1 d .
C55 C 0.7554(7) 0.5300(6) 0.6003(4) 0.029(2) Uani 1 1 d .
C14 C 1.0057(7) 0.6679(6) 0.7423(4) 0.033(2) Uani 1 1 d .
C13 C 0.9971(7) 0.7519(6) 0.7711(4) 0.031(2) Uani 1 1 d .
C7 C 1.0179(7) 0.7325(6) 0.8964(4) 0.036(2) Uani 1 1 d .
C36 C 0.3722(7) 0.6561(7) 0.6808(4) 0.036(2) Uani 1 1 d .
C26 C 0.5196(8) 0.9140(6) 0.6948(5) 0.041(3) Uani 1 1 d .
C60 C 0.8283(7) 0.5827(6) 0.5887(4) 0.036(2) Uani 1 1 d .
H60 H 0.8506 0.6306 0.6190 0.043 Uiso 1 1 calc R
C25 C 0.4681(7) 0.8392(6) 0.6651(4) 0.034(2) Uani 1 1 d .
C15 C 1.0407(7) 0.6429(6) 0.6862(5) 0.038(3) Uani 1 1 d .
C31 C 0.4480(7) 0.6630(6) 0.6440(4) 0.032(2) Uani 1 1 d .
C48 C 0.5086(7) 0.3732(7) 0.7169(5) 0.043(3) Uani 1 1 d .
H48 H 0.4873 0.3935 0.6796 0.051 Uiso 1 1 calc R
C18 C 1.0286(7) 0.8084(6) 0.7358(5) 0.037(3) Uani 1 1 d .
C34 C 0.3354(8) 0.5088(7) 0.6410(5) 0.043(3) Uani 1 1 d .
C6 C 1.0184(9) 0.9274(7) 0.9009(5) 0.046(3) Uani 1 1 d .
C2 C 0.8564(8) 0.9176(6) 0.8504(5) 0.038(3) Uani 1 1 d .
C76 C 1.0256(8) 0.3017(7) 0.6781(5) 0.045(3) Uani 1 1 d .
C54 C 0.7158(7) 0.5485(6) 0.6623(5) 0.035(2) Uani 1 1 d .
C1 C 0.9404(8) 0.8745(6) 0.8629(4) 0.036(2) Uani 1 1 d .
C45 C 0.8236(7) 0.5466(6) 0.8834(5) 0.043(3) Uani 1 1 d .
H45A H 0.8190 0.4940 0.8539 0.064 Uiso 1 1 calc R
H45B H 0.8703 0.5427 0.9207 0.064 Uiso 1 1 calc R
H45C H 0.8465 0.5913 0.8636 0.064 Uiso 1 1 calc R
C58 C 0.8405(7) 0.4938(7) 0.4884(5) 0.044(3) Uani 1 1 d .
H58 H 0.8709 0.4809 0.4518 0.053 Uiso 1 1 calc R
C33 C 0.4123(8) 0.5122(6) 0.6028(5) 0.044(3) Uani 1 1 d .
C77 C 0.9440(8) 0.3253(7) 0.7136(5) 0.048(3) Uani 1 1 d .
C17 C 1.0656(8) 0.7857(7) 0.6787(5) 0.044(3) Uani 1 1 d .
C51 C 0.5748(9) 0.3081(7) 0.8249(5) 0.051(3) Uani 1 1 d .
H51 H 0.5976 0.2849 0.8606 0.061 Uiso 1 1 calc R
C32 C 0.4663(7) 0.5882(6) 0.6057(4) 0.034(2) Uani 1 1 d .
C56 C 0.7225(8) 0.4586(6) 0.5541(5) 0.041(3) Uani 1 1 d .
H56 H 0.6708 0.4228 0.5605 0.049 Uiso 1 1 calc R
C66 C 0.8253(10) 0.1857(7) 0.5925(6) 0.060(3) Uani 1 1 d .
C29 C 0.3311(8) 0.9283(8) 0.6350(6) 0.054(3) Uani 1 1 d .
C46 C 0.6332(7) 0.4970(6) 0.7475(4) 0.034(2) Uani 1 1 d .
C59 C 0.8706(7) 0.5667(7) 0.5324(5) 0.043(3) Uani 1 1 d .
H59 H 0.9187 0.6047 0.5245 0.051 Uiso 1 1 calc R
C57 C 0.7658(7) 0.4407(6) 0.4991(5) 0.040(3) Uani 1 1 d .
H57 H 0.7442 0.3924 0.4691 0.048 Uiso 1 1 calc R
C79 C 1.0225(8) 0.2183(7) 0.7567(6) 0.054(3) Uani 1 1 d .
C8 C 0.9782(8) 0.7226(6) 0.9505(5) 0.041(3) Uani 1 1 d .
C30 C 0.3707(8) 0.8506(6) 0.6352(5) 0.045(3) Uani 1 1 d .
C75 C 1.0755(8) 0.2355(7) 0.7059(5) 0.049(3) Uani 1 1 d .
C50 C 0.4962(9) 0.2690(7) 0.7799(6) 0.054(3) Uani 1 1 d .
H50 H 0.4655 0.2192 0.7862 0.065 Uiso 1 1 calc R
C35 C 0.3170(7) 0.5817(7) 0.6783(5) 0.039(3) Uani 1 1 d .
C22 C 0.7190(10) 0.7696(7) 0.5103(5) 0.054(3) Uani 1 1 d .
C24 C 0.5597(8) 0.7457(6) 0.5414(5) 0.041(3) Uani 1 1 d .
C21 C 0.7628(8) 0.7799(7) 0.5733(6) 0.049(3) Uani 1 1 d .
C67 C 0.7830(9) 0.1589(8) 0.6415(6) 0.061(3) Uani 1 1 d .
C68 C 0.8386(10) 0.0928(8) 0.6627(6) 0.060(3) Uani 1 1 d .
C11 C 1.1662(10) 0.6682(8) 0.9450(6) 0.062(3) Uani 1 1 d .
C69 C 0.9158(9) 0.0779(7) 0.6252(6) 0.052(3) Uani 1 1 d .
C41 C 0.7055(8) 0.5759(7) 0.9657(5) 0.047(3) Uani 1 1 d .
H41 H 0.7597 0.5716 0.9967 0.056 Uiso 1 1 calc R
C4 C 0.9239(12) 1.0497(7) 0.9099(6) 0.059(4) Uani 1 1 d .
C49 C 0.4626(9) 0.3006(7) 0.7273(6) 0.055(3) Uani 1 1 d .
H49 H 0.4088 0.2735 0.6984 0.066 Uiso 1 1 calc R
C5 C 1.0104(11) 1.0130(7) 0.9238(5) 0.056(3) Uani 1 1 d .
C3 C 0.8464(10) 1.0023(7) 0.8728(5) 0.047(3) Uani 1 1 d .
C23 C 0.6183(9) 0.7512(7) 0.4934(5) 0.045(3) Uani 1 1 d .
C78 C 0.9427(8) 0.2726(8) 0.7607(5) 0.056(3) Uani 1 1 d .
C9 C 1.0254(9) 0.6875(7) 0.9994(5) 0.047(3) Uani 1 1 d .
C43 C 0.4551(8) 0.5878(8) 0.8241(5) 0.059(3) Uani 1 1 d .
H43A H 0.4330 0.5312 0.8034 0.088 Uiso 1 1 calc R
H43B H 0.4733 0.6195 0.7931 0.088 Uiso 1 1 calc R
H43C H 0.4017 0.6143 0.8442 0.088 Uiso 1 1 calc R
C81 C 1.0595(9) 0.3438(7) 0.6289(5) 0.058(3) Uani 1 1 d .
H81A H 1.0958 0.3962 0.6487 0.087 Uiso 1 1 calc R
H81B H 1.0022 0.3551 0.6002 0.087 Uiso 1 1 calc R
H81C H 1.1026 0.3079 0.6055 0.087 Uiso 1 1 calc R
C16 C 1.0720(7) 0.7019(7) 0.6543(5) 0.042(3) Uani 1 1 d .
C12 C 1.1134(8) 0.7036(7) 0.8951(5) 0.049(3) Uani 1 1 d .
C27 C 0.4826(8) 0.9924(7) 0.6968(6) 0.054(3) Uani 1 1 d .
C82 C 0.8752(9) 0.3942(7) 0.7055(6) 0.062(3) Uani 1 1 d .
H82A H 0.8094 0.3775 0.7130 0.093 Uiso 1 1 calc R
H82B H 0.8715 0.4053 0.6628 0.093 Uiso 1 1 calc R
H82C H 0.9000 0.4444 0.7354 0.093 Uiso 1 1 calc R
C65 C 0.9069(10) 0.1327(9) 0.5817(6) 0.066(4) Uani 1 1 d .
C10 C 1.1210(10) 0.6576(7) 0.9953(6) 0.058(3) Uani 1 1 d .
C44 C 0.6024(11) 0.6053(10) 1.0532(6) 0.093(5) Uani 1 1 d .
H44A H 0.6281 0.5585 1.0716 0.139 Uiso 1 1 calc R
H44B H 0.5323 0.6091 1.0570 0.139 Uiso 1 1 calc R
H44C H 0.6385 0.6567 1.0754 0.139 Uiso 1 1 calc R
C28 C 0.3883(10) 1.0017(7) 0.6651(7) 0.063(4) Uani 1 1 d .
C40 C 0.6153(9) 0.5922(8) 0.9840(5) 0.054(3) Uani 1 1 d .
C80 C 1.1698(8) 0.1938(8) 0.6866(6) 0.063(4) Uani 1 1 d .
H80A H 1.1798 0.2048 0.6454 0.095 Uiso 1 1 calc R
H80B H 1.1620 0.1339 0.6849 0.095 Uiso 1 1 calc R
H80C H 1.2270 0.2165 0.7174 0.095 Uiso 1 1 calc R
C83 C 0.8715(9) 0.2783(9) 0.8093(6) 0.076(4) Uani 1 1 d .
H83A H 0.8626 0.2240 0.8211 0.113 Uiso 1 1 calc R
H83B H 0.8078 0.2958 0.7914 0.113 Uiso 1 1 calc R
H83C H 0.8988 0.3189 0.8464 0.113 Uiso 1 1 calc R
C84 C 1.0543(11) 0.1553(9) 0.8002(6) 0.089(5) Uani 1 1 d .
H84A H 1.0968 0.1841 0.8378 0.133 Uiso 1 1 calc R
H84B H 1.0904 0.1117 0.7780 0.133 Uiso 1 1 calc R
H84C H 0.9957 0.1304 0.8122 0.133 Uiso 1 1 calc R
C73 C 0.8146(12) 0.0438(10) 0.7126(7) 0.106(6) Uani 1 1 d .
H73A H 0.7728 0.0759 0.7396 0.159 Uiso 1 1 calc R
H73B H 0.8759 0.0330 0.7380 0.159 Uiso 1 1 calc R
H73C H 0.7799 -0.0090 0.6923 0.159 Uiso 1 1 calc R
C61 C 0.5325(10) 0.8383(10) 0.8578(6) 0.088(5) Uani 1 1 d U
H61A H 0.5153 0.8319 0.8118 0.105 Uiso 1 1 calc R
H61B H 0.5503 0.8977 0.8741 0.105 Uiso 1 1 calc R
C63 C 0.6524(12) 0.7895(12) 0.9337(7) 0.110(6) Uani 1 1 d U
H63A H 0.7026 0.7475 0.9354 0.132 Uiso 1 1 calc R
H63B H 0.5962 0.7703 0.9523 0.132 Uiso 1 1 calc R
C70 C 0.9710(13) 0.1354(10) 0.5287(7) 0.120(7) Uani 1 1 d .
H70A H 1.0393 0.1253 0.5438 0.180 Uiso 1 1 calc R
H70B H 0.9683 0.1900 0.5164 0.180 Uiso 1 1 calc R
H70C H 0.9456 0.0927 0.4925 0.180 Uiso 1 1 calc R
C71 C 0.7865(14) 0.2492(9) 0.5524(7) 0.121(7) Uani 1 1 d .
H71A H 0.7472 0.2202 0.5136 0.182 Uiso 1 1 calc R
H71B H 0.8423 0.2805 0.5423 0.182 Uiso 1 1 calc R
H71C H 0.7455 0.2875 0.5757 0.182 Uiso 1 1 calc R
C74 C 0.9877(12) 0.0111(9) 0.6278(8) 0.111(6) Uani 1 1 d .
H74A H 1.0469 0.0268 0.6112 0.167 Uiso 1 1 calc R
H74B H 0.9575 -0.0410 0.6025 0.167 Uiso 1 1 calc R
H74C H 1.0056 0.0038 0.6712 0.167 Uiso 1 1 calc R
C72 C 0.6888(10) 0.1950(10) 0.6702(8) 0.119(7) Uani 1 1 d .
H72A H 0.6857 0.2539 0.6675 0.178 Uiso 1 1 calc R
H72B H 0.6940 0.1885 0.7140 0.178 Uiso 1 1 calc R
H72C H 0.6290 0.1648 0.6465 0.178 Uiso 1 1 calc R
H64A H 0.7582 0.8757 0.9659 0.178 Uiso 1 1 d R
H64B H 0.6941 0.8533 1.0170 0.178 Uiso 1 1 d R
H64C H 0.6498 0.9086 0.9675 0.178 Uiso 1 1 d R
C62 C 0.438(2) 0.815(2) 0.8849(16) 0.281(15) Uani 1 1 d U
H62A H 0.3822 0.8444 0.8682 0.422 Uiso 1 1 calc R
H62B H 0.4493 0.8298 0.9306 0.422 Uiso 1 1 calc R
H62C H 0.4223 0.7548 0.8729 0.422 Uiso 1 1 calc R
C86 C 0.7071(11) 0.9775(16) 0.5099(11) 0.209(11) Uiso 1 1 d D
H86A H 0.6967 0.9295 0.4759 0.313 Uiso 1 1 calc R
H86B H 0.7609 0.9678 0.5417 0.313 Uiso 1 1 calc R
H86C H 0.7241 1.0270 0.4934 0.313 Uiso 1 1 calc R
C88 C 0.5202(10) 0.9576(5) 0.4963(11) 0.178(10) Uiso 1 1 d D
H88A H 0.5304 0.9351 0.4529 0.214 Uiso 1 1 calc R
H88B H 0.4813 0.9170 0.5130 0.214 Uiso 1 1 calc R
C89A C 0.7209(9) 1.0976(6) 0.2051(6) 0.030(3) Uiso 0.70 1 d PD
C90A C 0.7533(10) 1.0103(7) 0.1978(9) 0.080(5) Uiso 0.70 1 d PD
C92A C 0.5923(13) 0.9525(13) 0.1325(12) 0.141(9) Uiso 0.70 1 d PD
C93A C 0.5187(19) 0.879(2) 0.1057(18) 0.242(19) Uiso 0.70 1 d PD
C89B C 0.357(2) 0.9437(14) -0.0147(13) 0.030(3) Uiso 0.30 1 d PD
C90B C 0.3013(19) 0.8657(19) -0.0066(18) 0.080(5) Uiso 0.30 1 d PD
C92B C 0.452(3) 0.863(2) 0.074(2) 0.141(9) Uiso 0.30 1 d PD
Cl1 Cl 0.7531(2) 0.5958(2) 0.21223(15) 0.0701(9) Uani 1 1 d .
Cl2 Cl 0.9104(3) 0.5501(2) 0.13409(16) 0.0798(10) Uani 1 1 d .
Co1 Co 0.92820(10) 0.19943(9) 0.67069(6) 0.0392(4) Uani 1 1 d .
F15 F 1.0243(5) 0.8925(4) 0.7568(3) 0.0556(17) Uani 1 1 d .
F14 F 1.0940(5) 0.8449(4) 0.6467(3) 0.069(2) Uani 1 1 d .
F12 F 1.0457(4) 0.5593(3) 0.6622(3) 0.0502(16) Uani 1 1 d .
F11 F 0.9789(4) 0.6049(3) 0.7732(3) 0.0467(15) Uani 1 1 d .
F30 F 0.3491(4) 0.7236(3) 0.7210(3) 0.0456(15) Uani 1 1 d .
F28 F 0.2847(5) 0.4344(4) 0.6374(3) 0.0599(18) Uani 1 1 d .
F27 F 0.4334(5) 0.4418(4) 0.5640(3) 0.0596(17) Uani 1 1 d .
F26 F 0.5384(4) 0.5842(3) 0.5679(3) 0.0438(15) Uani 1 1 d .
F21 F 0.6142(4) 0.9126(3) 0.7234(3) 0.0538(17) Uani 1 1 d .
F25 F 0.3100(4) 0.7832(4) 0.6025(3) 0.0535(16) Uani 1 1 d .
F24 F 0.2380(5) 0.9351(4) 0.6025(4) 0.081(2) Uani 1 1 d .
F29 F 0.2456(4) 0.5787(4) 0.7168(3) 0.0550(17) Uani 1 1 d .
F16 F 0.7524(4) 0.7895(3) 0.6811(3) 0.0401(14) Uani 1 1 d .
F17 F 0.8618(4) 0.7984(4) 0.5897(3) 0.0644(19) Uani 1 1 d .
F18 F 0.7780(5) 0.7747(5) 0.4645(3) 0.086(2) Uani 1 1 d .
F19 F 0.5757(5) 0.7440(4) 0.4333(3) 0.069(2) Uani 1 1 d .
F20 F 0.4603(4) 0.7306(4) 0.5233(3) 0.0452(15) Uani 1 1 d .
F6 F 0.8855(5) 0.7515(4) 0.9579(3) 0.0553(17) Uani 1 1 d .
F7 F 0.9786(5) 0.6793(5) 1.0499(3) 0.075(2) Uani 1 1 d .
F8 F 1.1688(6) 0.6227(5) 1.0424(3) 0.085(2) Uani 1 1 d .
F9 F 1.2587(6) 0.6393(5) 0.9392(3) 0.091(3) Uani 1 1 d .
F10 F 1.1658(5) 0.7110(5) 0.8470(3) 0.071(2) Uani 1 1 d .
F5 F 1.1091(5) 0.8953(4) 0.9159(3) 0.075(2) Uani 1 1 d .
F3 F 0.9161(7) 1.1321(4) 0.9322(3) 0.088(3) Uani 1 1 d .
F2 F 0.7592(6) 1.0393(4) 0.8573(3) 0.074(2) Uani 1 1 d .
F1 F 0.7743(5) 0.8788(3) 0.8097(3) 0.0553(17) Uani 1 1 d .
F13 F 1.1066(5) 0.6794(4) 0.5980(3) 0.0602(18) Uani 1 1 d .
F23 F 0.3483(5) 1.0775(4) 0.6648(5) 0.099(3) Uani 1 1 d .
F22 F 0.5364(5) 1.0630(4) 0.7262(4) 0.084(2) Uani 1 1 d .
F4 F 1.0914(6) 1.0579(4) 0.9597(4) 0.090(2) Uani 1 1 d .
N1 N 0.6543(6) 0.5659(5) 0.7907(4) 0.0341(19) Uani 1 1 d .
O2 O 0.5825(4) 0.7417(4) 0.7229(3) 0.0318(15) Uani 1 1 d .
O1 O 0.8473(5) 0.7316(4) 0.8255(3) 0.0337(16) Uani 1 1 d .
O3 O 0.7478(5) 0.6212(4) 0.6969(3) 0.0362(16) Uani 1 1 d .
O4 O 0.6195(6) 0.7921(5) 0.8707(3) 0.061(2) Uani 1 1 d U
C91A C 0.6844(8) 0.9337(5) 0.1744(5) 0.017(2) Uiso 0.70 1 d PD
C91B C 0.3632(18) 0.8125(13) 0.0327(11) 0.017(2) Uiso 0.30 1 d PD
U1 U 0.70381(3) 0.71157(3) 0.779991(19) 0.03528(14) Uani 1 1 d .
C87 C 0.6144(10) 0.9903(10) 0.5389(6) 0.092(5) Uiso 1 1 d D
H87A H 0.6097 1.0504 0.5536 0.111 Uiso 1 1 calc R
H87B H 0.6198 0.9631 0.5760 0.111 Uiso 1 1 calc R
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'
B B 0.0013 0.0007 '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'
Co Co 0.3494 0.9721 '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'
Cl Cl 0.1484 0.1585 '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'
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
O2 B2 C19 112.0(8) .
O2 B2 C25 111.8(8) .
C19 B2 C25 102.3(8) .
O2 B2 C31 103.8(8) .
C19 B2 C31 112.8(7) .
C25 B2 C31 114.4(8) .
O1 B1 C1 108.5(8) .
O1 B1 C13 106.4(8) .
C1 B1 C13 112.5(8) .
O1 B1 C7 109.3(8) .
C1 B1 C7 109.2(8) .
C13 B1 C7 110.9(8) .
Cl1 C85 Cl2 113.6(7) .
C38 C37 C42 120.9(9) .
C38 C37 N1 120.1(9) .
C42 C37 N1 118.8(8) .
C54 C53 C46 126.2(9) .
C52 C47 C48 118.6(10) .
C52 C47 C46 122.0(9) .
C48 C47 C46 119.3(9) .
C20 C19 C24 113.8(9) .
C20 C19 B2 124.4(8) .
C24 C19 B2 121.7(9) .
F16 C20 C19 122.2(8) .
F16 C20 C21 114.1(9) .
C19 C20 C21 123.8(10) .
C47 C52 C51 120.2(11) .
C39 C38 C37 117.1(10) .
C39 C38 C43 121.7(9) .
C37 C38 C43 121.1(9) .
C40 C39 C38 123.2(10) .
C41 C42 C37 118.0(9) .
C41 C42 C45 121.3(9) .
C37 C42 C45 120.7(9) .
C60 C55 C56 118.4(9) .
C60 C55 C54 119.0(9) .
C56 C55 C54 122.6(9) .
C15 C14 F11 116.3(9) .
C15 C14 C13 125.4(10) .
F11 C14 C13 118.3(8) .
C18 C13 C14 112.1(8) .
C18 C13 B1 128.0(9) .
C14 C13 B1 119.8(9) .
C8 C7 C12 113.6(9) .
C8 C7 B1 120.1(9) .
C12 C7 B1 126.3(9) .
F30 C36 C35 116.6(9) .
F30 C36 C31 120.2(9) .
C35 C36 C31 123.2(9) .
F21 C26 C27 115.3(10) .
F21 C26 C25 119.5(9) .
C27 C26 C25 125.2(10) .
C55 C60 C59 121.4(9) .
C26 C25 C30 113.2(9) .
C26 C25 B2 120.0(8) .
C30 C25 B2 126.5(9) .
C16 C15 C14 119.5(9) .
C16 C15 F12 119.9(9) .
C14 C15 F12 120.7(10) .
C32 C31 C36 114.6(9) .
C32 C31 B2 124.7(8) .
C36 C31 B2 118.8(8) .
C49 C48 C47 121.6(11) .
F15 C18 C13 119.6(8) .
F15 C18 C17 116.1(9) .
C13 C18 C17 124.4(9) .
F28 C34 C35 124.4(10) .
F28 C34 C33 118.5(10) .
C35 C34 C33 117.0(10) .
F5 C6 C5 116.6(11) .
F5 C6 C1 119.3(10) .
C5 C6 C1 124.1(11) .
C1 C2 F1 120.6(8) .
C1 C2 C3 125.4(10) .
F1 C2 C3 113.9(10) .
C77 C76 C75 106.8(9) .
C77 C76 C81 126.6(10) .
C75 C76 C81 126.1(9) .
C77 C76 Co1 70.3(6) .
C75 C76 Co1 69.6(6) .
C81 C76 Co1 130.8(8) .
O3 C54 C53 122.4(8) .
O3 C54 C55 114.2(9) .
C53 C54 C55 123.1(9) .
C2 C1 C6 111.5(9) .
C2 C1 B1 124.7(9) .
C6 C1 B1 123.7(9) .
C57 C58 C59 119.6(9) .
F27 C33 C32 120.3(10) .
F27 C33 C34 119.8(10) .
C32 C33 C34 119.9(9) .
C78 C77 C76 108.2(10) .
C78 C77 C82 124.9(10) .
C76 C77 C82 126.8(10) .
C78 C77 Co1 69.7(6) .
C76 C77 Co1 68.6(6) .
C82 C77 Co1 129.3(8) .
F14 C17 C16 119.9(9) .
F14 C17 C18 120.7(9) .
C16 C17 C18 119.5(10) .
C50 C51 C52 117.9(11) .
F26 C32 C31 121.8(9) .
F26 C32 C33 115.0(9) .
C31 C32 C33 123.2(9) .
C57 C56 C55 120.8(10) .
C67 C66 C65 105.9(11) .
C67 C66 C71 127.9(14) .
C65 C66 C71 125.7(14) .
C67 C66 Co1 70.6(7) .
C65 C66 Co1 69.2(7) .
C71 C66 Co1 130.6(9) .
F24 C29 C30 120.5(12) .
F24 C29 C28 119.2(11) .
C30 C29 C28 120.2(11) .
N1 C46 C53 122.4(9) .
N1 C46 C47 123.2(9) .
C53 C46 C47 114.4(8) .
C58 C59 C60 119.5(10) .
C58 C57 C56 120.3(10) .
C78 C79 C75 108.3(10) .
C78 C79 C84 127.2(11) .
C75 C79 C84 124.4(10) .
C78 C79 Co1 70.1(7) .
C75 C79 Co1 68.9(6) .
C84 C79 Co1 129.5(9) .
F6 C8 C9 116.0(9) .
F6 C8 C7 118.7(9) .
C9 C8 C7 125.3(10) .
F25 C30 C29 115.5(10) .
F25 C30 C25 120.9(9) .
C29 C30 C25 123.6(11) .
C76 C75 C79 107.8(9) .
C76 C75 C80 126.0(10) .
C79 C75 C80 126.1(10) .
C76 C75 Co1 69.1(6) .
C79 C75 Co1 70.0(6) .
C80 C75 Co1 128.3(8) .
C49 C50 C51 122.3(11) .
C34 C35 F29 117.6(9) .
C34 C35 C36 122.0(10) .
F29 C35 C36 120.3(9) .
F18 C22 C23 119.9(11) .
F18 C22 C21 119.3(11) .
C23 C22 C21 120.8(10) .
F20 C24 C23 117.0(9) .
F20 C24 C19 119.1(9) .
C23 C24 C19 123.9(10) .
F17 C21 C22 120.6(10) .
F17 C21 C20 120.4(10) .
C22 C21 C20 119.0(10) .
C66 C67 C68 109.6(11) .
C66 C67 C72 126.2(14) .
C68 C67 C72 124.2(13) .
C66 C67 Co1 69.0(7) .
C68 C67 Co1 70.1(7) .
C72 C67 Co1 127.0(9) .
C69 C68 C67 107.2(11) .
C69 C68 C73 126.3(13) .
C67 C68 C73 126.4(13) .
C69 C68 Co1 69.2(7) .
C67 C68 Co1 68.9(7) .
C73 C68 Co1 130.4(9) .
C10 C11 F9 120.5(11) .
C10 C11 C12 119.8(11) .
F9 C11 C12 119.5(11) .
C65 C69 C68 107.9(11) .
C65 C69 C74 126.0(13) .
C68 C69 C74 126.0(13) .
C65 C69 Co1 69.2(7) .
C68 C69 Co1 70.4(7) .
C74 C69 Co1 129.9(9) .
C40 C41 C42 122.7(10) .
C5 C4 F3 120.0(13) .
C5 C4 C3 118.6(10) .
F3 C4 C3 121.4(13) .
C50 C49 C48 119.4(12) .
C4 C5 F4 121.2(11) .
C4 C5 C6 120.1(11) .
F4 C5 C6 118.8(12) .
C4 C3 F2 119.0(10) .
C4 C3 C2 120.3(11) .
F2 C3 C2 120.7(11) .
F19 C23 C22 120.9(10) .
F19 C23 C24 120.4(10) .
C22 C23 C24 118.7(10) .
C79 C78 C77 108.8(10) .
C79 C78 C83 125.6(12) .
C77 C78 C83 125.4(11) .
C79 C78 Co1 70.1(7) .
C77 C78 Co1 69.7(6) .
C83 C78 Co1 129.1(9) .
F7 C9 C8 120.5(11) .
F7 C9 C10 120.5(10) .
C8 C9 C10 119.0(11) .
F13 C16 C15 121.2(10) .
F13 C16 C17 119.6(10) .
C15 C16 C17 119.2(9) .
F10 C12 C7 122.0(10) .
F10 C12 C11 114.7(10) .
C7 C12 C11 123.3(11) .
F22 C27 C26 122.6(11) .
F22 C27 C28 117.2(11) .
C26 C27 C28 120.2(11) .
C69 C65 C66 109.4(11) .
C69 C65 C70 126.3(14) .
C66 C65 C70 124.3(14) .
C69 C65 Co1 70.4(7) .
C66 C65 Co1 69.0(7) .
C70 C65 Co1 128.4(9) .
F8 C10 C11 120.7(12) .
F8 C10 C9 120.3(12) .
C11 C10 C9 118.9(11) .
F23 C28 C27 122.8(12) .
F23 C28 C29 119.5(12) .
C27 C28 C29 117.6(11) .
C41 C40 C39 118.0(10) .
C41 C40 C44 120.9(11) .
C39 C40 C44 121.0(11) .
O4 C61 C62 117.5(18) .
O4 C63 C64 116.5(19) .
C88 C88 C87 91.5(13) 2_676
C89A C90A C91A 124.4(9) .
C93A C92A C91A 116.0(11) .
C89B C90B C91B 113.3(10) .
C93B C92B C91B 112.7(11) .
C66 Co1 C65 41.8(5) .
C66 Co1 C69 69.8(5) .
C65 Co1 C69 40.4(5) .
C66 Co1 C67 40.4(5) .
C65 Co1 C67 67.9(5) .
C69 Co1 C67 68.4(5) .
C66 Co1 C68 69.3(5) .
C65 Co1 C68 67.9(5) .
C69 Co1 C68 40.4(4) .
C67 Co1 C68 41.0(5) .
C66 Co1 C76 112.3(5) .
C65 Co1 C76 111.0(5) .
C69 Co1 C76 136.6(4) .
C67 Co1 C76 142.2(5) .
C68 Co1 C76 176.4(5) .
C66 Co1 C75 143.7(5) .
C65 Co1 C75 114.2(5) .
C69 Co1 C75 110.5(4) .
C67 Co1 C75 175.6(5) .
C68 Co1 C75 135.6(5) .
C76 Co1 C75 41.4(4) .
C66 Co1 C79 173.9(5) .
C65 Co1 C79 143.8(5) .
C69 Co1 C79 113.3(5) .
C67 Co1 C79 134.9(5) .
C68 Co1 C79 109.4(5) .
C76 Co1 C79 69.4(4) .
C75 Co1 C79 41.1(4) .
C66 Co1 C78 134.7(5) .
C65 Co1 C78 176.4(5) .
C69 Co1 C78 141.9(5) .
C67 Co1 C78 109.7(5) .
C68 Co1 C78 112.3(5) .
C76 Co1 C78 69.1(5) .
C75 Co1 C78 68.3(4) .
C79 Co1 C78 39.8(4) .
C66 Co1 C77 109.2(5) .
C65 Co1 C77 137.2(5) .
C69 Co1 C77 177.3(5) .
C67 Co1 C77 112.6(5) .
C68 Co1 C77 141.9(5) .
C76 Co1 C77 41.1(4) .
C75 Co1 C77 68.6(4) .
C79 Co1 C77 67.9(4) .
C78 Co1 C77 40.6(4) .
C20 F16 U1 124.7(5) .
C2 F1 U1 131.2(5) .
C46 N1 C37 122.3(8) .
C46 N1 U1 130.8(7) .
C37 N1 U1 106.5(5) .
B2 O2 U1 154.2(5) .
B1 O1 U1 154.4(6) .
C54 O3 U1 138.1(6) .
C63 O4 C61 116.7(10) .
C63 O4 U1 122.0(8) .
C61 O4 U1 121.2(7) .
C90A C91A C92A 111.7(8) .
C90B C91B C92B 111.9(10) .
O2 U1 O1 153.3(2) .
O2 U1 O3 90.1(2) .
O1 U1 O3 93.2(2) .
O2 U1 N1 101.7(2) .
O1 U1 N1 104.6(2) .
O3 U1 N1 71.6(2) .
O2 U1 O4 84.3(2) .
O1 U1 O4 96.8(2) .
O3 U1 O4 167.4(3) .
N1 U1 O4 98.4(3) .
O2 U1 F1 90.9(2) .
O1 U1 F1 64.9(2) .
O3 U1 F1 122.2(2) .
N1 U1 F1 161.7(2) .
O4 U1 F1 69.4(2) .
O2 U1 F16 66.2(2) .
O1 U1 F16 91.1(2) .
O3 U1 F16 66.02(19) .
N1 U1 F16 135.5(2) .
O4 U1 F16 121.2(2) .
F1 U1 F16 61.98(17) .
C86 C87 C88 115.3(10) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C64 C63 1.38(2) .
C93B C92B 1.496(11) .
B2 O2 1.453(12) .
B2 C19 1.655(14) .
B2 C25 1.658(14) .
B2 C31 1.661(15) .
B1 O1 1.473(13) .
B1 C1 1.642(15) .
B1 C13 1.652(14) .
B1 C7 1.676(15) .
C85 Cl1 1.720(12) .
C85 Cl2 1.760(12) .
C37 C38 1.389(12) .
C37 C42 1.399(13) .
C37 N1 1.443(11) .
C53 C54 1.384(13) .
C53 C46 1.433(12) .
C47 C52 1.371(14) .
C47 C48 1.396(13) .
C47 C46 1.500(14) .
C19 C20 1.386(13) .
C19 C24 1.414(13) .
C20 F16 1.371(11) .
C20 C21 1.394(13) .
C52 C51 1.426(14) .
C38 C39 1.384(13) .
C38 C43 1.483(14) .
C39 C40 1.374(15) .
C42 C41 1.388(13) .
C42 C45 1.514(13) .
C55 C60 1.354(13) .
C55 C56 1.397(13) .
C55 C54 1.489(12) .
C14 C15 1.354(13) .
C14 F11 1.369(10) .
C14 C13 1.400(13) .
C13 C18 1.375(13) .
C7 C8 1.377(13) .
C7 C12 1.380(14) .
C36 F30 1.337(10) .
C36 C35 1.379(14) .
C36 C31 1.386(12) .
C26 F21 1.337(11) .
C26 C27 1.363(14) .
C26 C25 1.376(13) .
C60 C59 1.395(12) .
C25 C30 1.409(14) .
C15 C16 1.353(14) .
C15 F12 1.361(11) .
C31 C32 1.383(12) .
C48 C49 1.371(14) .
C18 F15 1.355(11) .
C18 C17 1.381(13) .
C34 F28 1.344(12) .
C34 C35 1.350(14) .
C34 C33 1.411(14) .
C6 F5 1.357(12) .
C6 C5 1.391(15) .
C6 C1 1.401(13) .
C2 C1 1.362(13) .
C2 F1 1.369(11) .
C2 C3 1.380(13) .
C76 C77 1.443(14) .
C76 C75 1.445(14) .
C76 C81 1.467(14) .
C76 Co1 2.042(11) .
C54 O3 1.297(11) .
C58 C57 1.367(14) .
C58 C59 1.383(14) .
C33 F27 1.346(11) .
C33 C32 1.391(14) .
C77 C78 1.431(15) .
C77 C82 1.481(14) .
C77 Co1 2.065(11) .
C17 F14 1.344(11) .
C17 C16 1.367(14) .
C51 C50 1.385(15) .
C32 F26 1.343(10) .
C56 C57 1.379(13) .
C66 C67 1.389(16) .
C66 C65 1.428(17) .
C66 C71 1.507(17) .
C66 Co1 2.000(12) .
C29 F24 1.364(12) .
C29 C30 1.372(14) .
C29 C28 1.394(16) .
C46 N1 1.312(11) .
C79 C78 1.404(14) .
C79 C75 1.445(14) .
C79 C84 1.525(16) .
C79 Co1 2.063(12) .
C8 F6 1.362(11) .
C8 C9 1.366(14) .
C30 F25 1.363(11) .
C75 C80 1.525(14) .
C75 Co1 2.049(11) .
C50 C49 1.345(16) .
C35 F29 1.355(11) .
C22 F18 1.358(11) .
C22 C23 1.362(15) .
C22 C21 1.381(15) .
C24 F20 1.341(11) .
C24 C23 1.394(13) .
C21 F17 1.340(12) .
C67 C68 1.419(16) .
C67 C72 1.566(16) .
C67 Co1 2.020(12) .
C68 C69 1.401(15) .
C68 C73 1.501(16) .
C68 Co1 2.035(12) .
C11 C10 1.344(16) .
C11 F9 1.355(13) .
C11 C12 1.414(15) .
C69 C65 1.389(16) .
C69 C74 1.467(16) .
C69 Co1 2.018(11) .
C41 C40 1.344(14) .
C4 C5 1.339(17) .
C4 F3 1.339(12) .
C4 C3 1.347(16) .
C5 F4 1.354(13) .
C3 F2 1.356(12) .
C23 F19 1.324(12) .
C78 C83 1.503(15) .
C78 Co1 2.064(11) .
C9 F7 1.351(12) .
C9 C10 1.394(16) .
C16 F13 1.351(10) .
C12 F10 1.348(12) .
C27 F22 1.336(12) .
C27 C28 1.380(16) .
C65 C70 1.526(17) .
C65 Co1 2.003(12) .
C10 F8 1.338(12) .
C44 C40 1.502(15) .
C28 F23 1.346(12) .
C61 O4 1.423(14) .
C61 C62 1.54(3) .
C63 O4 1.374(15) .
C86 C87 1.472(9) .
C88 C88 1.473(10) 2_676
C88 C87 1.481(9) .
C89A C90A 1.470(9) .
C90A C91A 1.489(9) .
C92A C93A 1.495(10) .
C92A C91A 1.497(10) .
C89B C90B 1.493(10) .
C90B C91B 1.495(10) .
C92B C91B 1.503(10) .
F16 U1 2.789(5) .
F1 U1 2.762(6) .
N1 U1 2.474(8) .
O2 U1 2.025(6) .
O1 U1 2.029(6) .
O3 U1 2.256(6) .
O4 U1 2.566(7) .
