#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/11/7001173.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_7001173
loop_
_publ_author_name
'Berthet, Jean-Claude'
'Siffredi, Gérald'
'Thuéry, Pierre'
'Ephritikhine, Michel'
_publ_section_title
;
 Synthesis and crystal structure of pentavalent uranyl complexes. The
 remarkable stability of UO2X (X = I, SO3CF3) in non-aqueous solutions
;
_journal_issue                   18
_journal_name_full               'Dalton Transactions'
_journal_page_first              3478
_journal_page_last               3494
_journal_paper_doi               10.1039/b820659g
_journal_year                    2009
_chemical_formula_moiety
'C37 H43 N9 O2 U, C F3 O3 S, C7.50 H7.50 N1.50'
_chemical_formula_sum            'C45.5 H50.5 F3 N10.5 O5 S U'
_chemical_formula_weight         1151.55
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.201(6)
_cell_angle_beta                 98.845(8)
_cell_angle_gamma                94.538(9)
_cell_formula_units_Z            2
_cell_length_a                   12.5854(12)
_cell_length_b                   14.1686(19)
_cell_length_c                   14.4513(19)
_cell_measurement_reflns_used    91211
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.91
_cell_volume                     2365.2(5)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and ten ω scans with 2° steps'
_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  0.0927
_diffrn_reflns_av_sigmaI/netI    0.0988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            91211
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.544
_exptl_absorpt_correction_T_max  0.609
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent dark brown-green'
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.336
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         8946
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0439P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                7820
_reflns_number_total             8946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b820659g.txt
_cod_data_source_block           15.1.5py
_cod_original_formula_sum        'C45.50 H50.50 F3 N10.50 O5 S U'
_cod_database_code               7001173
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
_atom_site_disorder_assembly
_atom_site_disorder_group
U U 0.766364(15) 0.520250(12) 0.518860(13) 0.03871(9) Uani 1 1 d . . .
S1 S 0.21485(14) 0.10860(10) 0.87635(10) 0.0499(4) Uani 1 1 d . . .
O1 O 0.6644(3) 0.5933(2) 0.4865(2) 0.0405(9) Uani 1 1 d . . .
O2 O 0.8662(3) 0.4434(3) 0.5485(3) 0.0442(9) Uani 1 1 d . . .
O3 O 0.2374(5) 0.2094(3) 0.8771(3) 0.0707(14) Uani 1 1 d . . .
O4 O 0.1411(4) 0.0976(3) 0.9403(3) 0.0714(15) Uani 1 1 d . . .
O5 O 0.2001(4) 0.0269(3) 0.7804(3) 0.0683(14) Uani 1 1 d . . .
N1 N 0.6213(4) 0.4044(3) 0.5512(3) 0.0395(10) Uani 1 1 d . . .
N2 N 0.7312(4) 0.5701(3) 0.7017(3) 0.0387(10) Uani 1 1 d . . .
N3 N 0.8773(4) 0.6885(3) 0.6520(3) 0.0386(10) Uani 1 1 d . . .
N4 N 0.8990(4) 0.6223(3) 0.4580(3) 0.0408(11) Uani 1 1 d . . .
N5 N 0.5677(4) 0.3230(3) 0.4720(3) 0.0398(11) Uani 1 1 d . . .
N6 N 0.5321(4) 0.3556(3) 0.6638(3) 0.0429(11) Uani 1 1 d . . .
N7 N 0.9060(4) 0.5862(3) 0.3604(3) 0.0406(10) Uani 1 1 d . . .
N8 N 1.0220(4) 0.7702(3) 0.4876(3) 0.0452(12) Uani 1 1 d . . .
N9 N 0.7193(4) 0.3905(3) 0.3413(3) 0.0495(12) Uani 1 1 d . . .
N10 N 0.1234(7) 0.7749(6) 0.0006(5) 0.106(3) Uani 1 1 d . . .
F1 F 0.3443(5) 0.0054(3) 0.9518(4) 0.1036(15) Uani 1 1 d U . .
F2 F 0.4253(4) 0.1045(4) 0.8962(4) 0.1106(16) Uani 1 1 d U . .
F3 F 0.3705(4) 0.1619(3) 1.0365(3) 0.0833(13) Uani 1 1 d . . .
C1 C 0.6009(5) 0.4176(4) 0.6422(4) 0.0427(13) Uani 1 1 d . . .
C2 C 0.6645(5) 0.5071(4) 0.7259(4) 0.0421(13) Uani 1 1 d . . .
C3 C 0.6536(5) 0.5237(4) 0.8247(4) 0.0536(16) Uani 1 1 d . . .
H3 H 0.6058 0.4796 0.8391 0.064 Uiso 1 1 calc R . .
C4 C 0.7160(5) 0.6079(4) 0.9011(4) 0.0563(17) Uani 1 1 d . . .
H4 H 0.7117 0.6201 0.9678 0.068 Uiso 1 1 calc R . .
C5 C 0.7840(5) 0.6727(4) 0.8771(4) 0.0511(15) Uani 1 1 d . . .
H5 H 0.8254 0.7295 0.9277 0.061 Uiso 1 1 calc R . .
C6 C 0.7910(5) 0.6539(4) 0.7782(4) 0.0415(12) Uani 1 1 d . . .
C7 C 0.8634(4) 0.7214(4) 0.7486(4) 0.0398(12) Uani 1 1 d . . .
C8 C 0.9137(5) 0.8161(4) 0.8181(4) 0.0490(14) Uani 1 1 d . . .
H8 H 0.9007 0.8385 0.8833 0.059 Uiso 1 1 calc R . .
C9 C 0.9828(5) 0.8761(4) 0.7887(4) 0.0546(16) Uani 1 1 d . . .
H9 H 1.0185 0.9386 0.8346 0.066 Uiso 1 1 calc R . .
C10 C 0.9987(5) 0.8432(4) 0.6912(4) 0.0486(14) Uani 1 1 d . . .
H10 H 1.0446 0.8829 0.6702 0.058 Uiso 1 1 calc R . .
C11 C 0.9448(5) 0.7495(4) 0.6250(4) 0.0424(12) Uani 1 1 d . . .
C12 C 0.9564(5) 0.7116(4) 0.5172(4) 0.0416(13) Uani 1 1 d . . .
C13 C 0.4969(5) 0.2599(3) 0.4872(4) 0.0396(12) Uani 1 1 d . . .
C14 C 0.4773(5) 0.2747(4) 0.5859(4) 0.0410(13) Uani 1 1 d . . .
C15 C 0.3992(5) 0.2024(4) 0.6094(4) 0.0494(15) Uani 1 1 d . . .
C16 C 0.3630(6) 0.1046(5) 0.5169(4) 0.068(2) Uani 1 1 d D . .
H16A H 0.4186 0.0607 0.5156 0.082 Uiso 1 1 calc R . .
H16B H 0.2973 0.0697 0.5245 0.082 Uiso 1 1 calc R . .
C17 C 0.3421(6) 0.1175(5) 0.4202(4) 0.071(2) Uani 1 1 d D . .
H17A H 0.2827 0.1570 0.4196 0.085 Uiso 1 1 calc R . .
H17B H 0.3183 0.0511 0.3679 0.085 Uiso 1 1 calc R . .
C18 C 0.4393(5) 0.1699(4) 0.3934(4) 0.0459(14) Uani 1 1 d . . .
C19 C 0.4585(6) 0.1723(5) 0.6926(5) 0.0564(16) Uani 1 1 d . . .
H19A H 0.4861 0.2322 0.7511 0.085 Uiso 1 1 calc R . .
H19B H 0.5178 0.1378 0.6704 0.085 Uiso 1 1 calc R . .
H19C H 0.4091 0.1281 0.7090 0.085 Uiso 1 1 calc R . .
C20 C 0.3034(6) 0.2546(5) 0.6419(6) 0.0650(18) Uani 1 1 d . . .
H20A H 0.3292 0.3219 0.6899 0.098 Uiso 1 1 calc R . .
H20B H 0.2633 0.2164 0.6719 0.098 Uiso 1 1 calc R . .
H20C H 0.2571 0.2585 0.5844 0.098 Uiso 1 1 calc R . .
C21 C 0.3971(5) 0.2082(4) 0.3104(4) 0.0568(15) Uani 1 1 d . . .
H21A H 0.3482 0.2560 0.3332 0.085 Uiso 1 1 calc R . .
H21B H 0.3596 0.1520 0.2521 0.085 Uiso 1 1 calc R . .
H21C H 0.4571 0.2408 0.2934 0.085 Uiso 1 1 calc R . .
C22 C 0.5221(6) 0.0997(4) 0.3598(5) 0.0583(16) Uani 1 1 d . . .
H22A H 0.5830 0.1368 0.3487 0.087 Uiso 1 1 calc R . .
H22B H 0.4894 0.0447 0.2985 0.087 Uiso 1 1 calc R . .
H22C H 0.5464 0.0730 0.4108 0.087 Uiso 1 1 calc R . .
C23 C 0.9713(5) 0.6398(4) 0.3269(4) 0.0418(13) Uani 1 1 d . . .
C24 C 1.0318(5) 0.7344(4) 0.3926(4) 0.0431(13) Uani 1 1 d . . .
C25 C 1.1087(6) 0.7974(4) 0.3592(4) 0.0542(16) Uani 1 1 d . . .
C26 C 1.1207(8) 0.7474(6) 0.2560(5) 0.108(3) Uani 1 1 d DU . .
H26A H 1.1211 0.7992 0.2262 0.129 Uiso 1 1 calc R . .
H26B H 1.1928 0.7275 0.2591 0.129 Uiso 1 1 calc R . .
C27 C 1.0463(8) 0.6587(6) 0.1836(5) 0.111(3) Uani 1 1 d DU . .
H27A H 1.0902 0.6155 0.1422 0.134 Uiso 1 1 calc R . .
H27B H 0.9992 0.6833 0.1399 0.134 Uiso 1 1 calc R . .
C28 C 0.9746(5) 0.5917(4) 0.2158(4) 0.0520(15) Uani 1 1 d D . .
C29 C 1.0661(7) 0.9006(5) 0.3744(6) 0.080(2) Uani 1 1 d U . .
H29A H 0.9950 0.8890 0.3337 0.120 Uiso 1 1 calc R . .
H29B H 1.1146 0.9431 0.3552 0.120 Uiso 1 1 calc R . .
H29C H 1.0623 0.9336 0.4439 0.120 Uiso 1 1 calc R . .
C30 C 1.2222(6) 0.8158(5) 0.4236(6) 0.068(2) Uani 1 1 d . . .
H30A H 1.2182 0.8455 0.4933 0.103 Uiso 1 1 calc R . .
H30B H 1.2695 0.8611 0.4065 0.103 Uiso 1 1 calc R . .
H30C H 1.2501 0.7524 0.4113 0.103 Uiso 1 1 calc R . .
C31 C 0.8627(7) 0.5783(5) 0.1528(5) 0.077(2) Uani 1 1 d . . .
H31A H 0.8373 0.6431 0.1673 0.115 Uiso 1 1 calc R . .
H31B H 0.8135 0.5332 0.1682 0.115 Uiso 1 1 calc R . .
H31C H 0.8663 0.5503 0.0828 0.115 Uiso 1 1 calc R . .
C32 C 1.0106(7) 0.4905(5) 0.1947(5) 0.087(3) Uani 1 1 d . . .
H32A H 1.0166 0.4621 0.1253 0.131 Uiso 1 1 calc R . .
H32B H 0.9586 0.4464 0.2085 0.131 Uiso 1 1 calc R . .
H32C H 1.0801 0.4975 0.2365 0.131 Uiso 1 1 calc R . .
C33 C 0.7562(6) 0.2990(5) 0.3174(5) 0.0636(17) Uani 1 1 d . . .
H33 H 0.8087 0.2901 0.3653 0.076 Uiso 1 1 calc R . .
C34 C 0.7224(7) 0.2199(5) 0.2288(5) 0.073(2) Uani 1 1 d . . .
H34 H 0.7527 0.1599 0.2160 0.088 Uiso 1 1 calc R . .
C35 C 0.6422(7) 0.2305(5) 0.1586(5) 0.071(2) Uani 1 1 d . . .
H35 H 0.6160 0.1773 0.0977 0.085 Uiso 1 1 calc R . .
C36 C 0.6016(7) 0.3208(5) 0.1800(5) 0.082(2) Uani 1 1 d . . .
H36 H 0.5488 0.3308 0.1331 0.098 Uiso 1 1 calc R . .
C37 C 0.6403(7) 0.3965(5) 0.2722(4) 0.068(2) Uani 1 1 d . . .
H37 H 0.6089 0.4559 0.2871 0.081 Uiso 1 1 calc R . .
C38 C 0.3468(7) 0.0920(5) 0.9418(6) 0.0657(19) Uani 1 1 d . . .
C39 C 0.1273(7) 0.8745(6) 0.0479(6) 0.079(2) Uani 1 1 d . . .
H39 H 0.0683 0.9079 0.0378 0.095 Uiso 1 1 calc R . .
C40 C 0.2236(9) 0.9261(6) 0.1130(7) 0.091(3) Uani 1 1 d U . .
H40 H 0.2293 0.9950 0.1504 0.109 Uiso 1 1 calc R . .
C41 C 0.3070(9) 0.8771(8) 0.1216(8) 0.100(3) Uani 1 1 d U . .
H41 H 0.3726 0.9143 0.1612 0.120 Uiso 1 1 calc R . .
C42 C 0.3026(8) 0.7797(7) 0.0777(7) 0.091(3) Uani 1 1 d . . .
H42 H 0.3635 0.7486 0.0877 0.110 Uiso 1 1 calc R . .
C43 C 0.2141(9) 0.7263(6) 0.0206(6) 0.084(3) Uani 1 1 d . . .
H43 H 0.2093 0.6560 -0.0076 0.100 Uiso 1 1 calc R . .
C44 C 0.5901(9) 0.4748(7) 0.0428(7) 0.102(3) Uani 1 1 d . . .
C45 C 0.5152(8) 0.3993(6) -0.0273(6) 0.084(2) Uani 1 1 d . . .
C46 C 0.4260(7) 0.4274(6) -0.0732(6) 0.080(2) Uani 1 1 d . . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U O2 178.25(13) . . ?
O1 U N9 90.11(16) . . ?
O2 U N9 88.37(16) . . ?
O1 U N1 90.79(15) . . ?
O2 U N1 88.17(16) . . ?
N9 U N1 83.62(14) . . ?
O1 U N4 86.66(15) . . ?
O2 U N4 94.16(16) . . ?
N9 U N4 88.05(14) . . ?
N1 U N4 171.29(13) . . ?
O1 U N2 92.07(15) . . ?
O2 U N2 88.70(15) . . ?
N9 U N2 146.05(13) . . ?
N1 U N2 62.48(12) . . ?
N4 U N2 125.90(12) . . ?
O1 U N3 89.03(14) . . ?
O2 U N3 92.72(15) . . ?
N9 U N3 150.80(14) . . ?
N1 U N3 125.57(13) . . ?
N4 U N3 62.76(12) . . ?
N2 U N3 63.14(12) . . ?
O3 S1 O5 116.6(3) . . ?
O3 S1 O4 114.7(3) . . ?
O5 S1 O4 115.5(2) . . ?
O3 S1 C38 101.9(3) . . ?
O5 S1 C38 101.9(3) . . ?
O4 S1 C38 103.0(3) . . ?
C1 N1 N5 119.1(4) . . ?
C1 N1 U 123.3(3) . . ?
N5 N1 U 117.5(3) . . ?
C2 N2 C6 118.1(4) . . ?
C2 N2 U 120.4(3) . . ?
C6 N2 U 120.9(3) . . ?
C7 N3 C11 117.8(4) . . ?
C7 N3 U 121.1(3) . . ?
C11 N3 U 120.9(3) . . ?
C12 N4 N7 118.7(4) . . ?
C12 N4 U 123.1(3) . . ?
N7 N4 U 118.1(3) . . ?
C13 N5 N1 118.8(4) . . ?
C1 N6 C14 116.3(4) . . ?
C23 N7 N4 118.9(4) . . ?
C24 N8 C12 116.7(4) . . ?
C37 N9 C33 114.6(5) . . ?
C37 N9 U 122.6(4) . . ?
C33 N9 U 121.2(4) . . ?
C39 N10 C43 119.9(8) . . ?
N1 C1 N6 125.5(5) . . ?
N1 C1 C2 116.1(4) . . ?
N6 C1 C2 118.3(4) . . ?
N2 C2 C3 122.7(5) . . ?
N2 C2 C1 117.1(4) . . ?
C3 C2 C1 120.2(4) . . ?
C4 C3 C2 118.3(5) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C5 C4 C3 119.3(5) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.3(5) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.8 . . ?
N2 C6 C5 121.2(4) . . ?
N2 C6 C7 116.6(4) . . ?
C5 C6 C7 122.2(5) . . ?
N3 C7 C8 121.7(4) . . ?
N3 C7 C6 117.7(4) . . ?
C8 C7 C6 120.7(5) . . ?
C9 C8 C7 119.2(5) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C10 C9 C8 119.7(5) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 118.6(5) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
N3 C11 C10 123.0(5) . . ?
N3 C11 C12 116.3(4) . . ?
C10 C11 C12 120.7(5) . . ?
N4 C12 N8 125.3(5) . . ?
N4 C12 C11 116.8(4) . . ?
N8 C12 C11 117.9(4) . . ?
N5 C13 C14 121.2(4) . . ?
N5 C13 C18 115.5(4) . . ?
C14 C13 C18 123.3(4) . . ?
N6 C14 C13 119.1(4) . . ?
N6 C14 C15 117.0(5) . . ?
C13 C14 C15 123.9(5) . . ?
C20 C15 C19 110.4(5) . . ?
C20 C15 C14 109.2(5) . . ?
C19 C15 C14 109.1(5) . . ?
C20 C15 C16 111.7(6) . . ?
C19 C15 C16 106.8(5) . . ?
C14 C15 C16 109.6(4) . . ?
C17 C16 C15 115.9(5) . . ?
C17 C16 H16A 108.3 . . ?
C15 C16 H16A 108.3 . . ?
C17 C16 H16B 108.3 . . ?
C15 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C16 C17 C18 115.8(5) . . ?
C16 C17 H17A 108.3 . . ?
C18 C17 H17A 108.3 . . ?
C16 C17 H17B 108.3 . . ?
C18 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C22 C18 C21 109.4(5) . . ?
C22 C18 C13 107.7(5) . . ?
C21 C18 C13 109.5(4) . . ?
C22 C18 C17 112.7(5) . . ?
C21 C18 C17 109.1(5) . . ?
C13 C18 C17 108.5(4) . . ?
C15 C19 H19A 109.5 . . ?
C15 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C15 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N7 C23 C24 120.7(5) . . ?
N7 C23 C28 114.9(4) . . ?
C24 C23 C28 124.4(4) . . ?
N8 C24 C23 119.7(5) . . ?
N8 C24 C25 117.3(5) . . ?
C23 C24 C25 122.9(5) . . ?
C26 C25 C24 113.0(5) . . ?
C26 C25 C30 106.0(7) . . ?
C24 C25 C30 109.5(5) . . ?
C26 C25 C29 111.2(7) . . ?
C24 C25 C29 107.6(6) . . ?
C30 C25 C29 109.5(5) . . ?
C25 C26 C27 123.6(7) . . ?
C25 C26 H26A 106.4 . . ?
C27 C26 H26A 106.4 . . ?
C25 C26 H26B 106.4 . . ?
C27 C26 H26B 106.4 . . ?
H26A C26 H26B 106.5 . . ?
C26 C27 C28 122.3(6) . . ?
C26 C27 H27A 106.7 . . ?
C28 C27 H27A 106.7 . . ?
C26 C27 H27B 106.7 . . ?
C28 C27 H27B 106.7 . . ?
H27A C27 H27B 106.6 . . ?
C32 C28 C27 111.1(7) . . ?
C32 C28 C31 108.6(5) . . ?
C27 C28 C31 105.8(6) . . ?
C32 C28 C23 109.7(5) . . ?
C27 C28 C23 111.3(5) . . ?
C31 C28 C23 110.2(5) . . ?
C25 C29 H29A 109.5 . . ?
C25 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C25 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C25 C30 H30A 109.5 . . ?
C25 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C25 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C28 C32 H32A 109.5 . . ?
C28 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C28 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 N9 124.9(7) . . ?
C34 C33 H33 117.5 . . ?
N9 C33 H33 117.5 . . ?
C33 C34 C35 118.3(7) . . ?
C33 C34 H34 120.8 . . ?
C35 C34 H34 120.8 . . ?
C36 C35 C34 118.7(7) . . ?
C36 C35 H35 120.6 . . ?
C34 C35 H35 120.6 . . ?
C35 C36 C37 118.9(8) . . ?
C35 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
N9 C37 C36 124.4(7) . . ?
N9 C37 H37 117.8 . . ?
C36 C37 H37 117.8 . . ?
F1 C38 F2 109.6(7) . . ?
F1 C38 F3 105.6(6) . . ?
F2 C38 F3 108.1(6) . . ?
F1 C38 S1 112.6(6) . . ?
F2 C38 S1 111.4(5) . . ?
F3 C38 S1 109.2(5) . . ?
N10 C39 C40 116.7(9) . . ?
N10 C39 H39 121.7 . . ?
C40 C39 H39 121.7 . . ?
C41 C40 C39 119.8(9) . . ?
C41 C40 H40 120.1 . . ?
C39 C40 H40 120.1 . . ?
C42 C41 C40 123.5(10) . . ?
C42 C41 H41 118.2 . . ?
C40 C41 H41 118.2 . . ?
C43 C42 C41 119.9(10) . . ?
C43 C42 H42 120.1 . . ?
C41 C42 H42 120.1 . . ?
C42 C43 N10 119.8(8) . . ?
C42 C43 H43 120.1 . . ?
N10 C43 H43 120.1 . . ?
C46 C44 C45 122.0(11) 2_665 . ?
C44 C45 C46 117.5(9) . . ?
C44 C46 C45 120.2(8) 2_665 . ?
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
U O1 1.816(4) . ?
U O2 1.822(4) . ?
U N9 2.533(4) . ?
U N1 2.562(4) . ?
U N4 2.570(4) . ?
U N2 2.606(4) . ?
U N3 2.611(4) . ?
S1 O3 1.430(4) . ?
S1 O5 1.441(4) . ?
S1 O4 1.442(4) . ?
S1 C38 1.855(9) . ?
N1 C1 1.331(7) . ?
N1 N5 1.351(6) . ?
N2 C2 1.346(6) . ?
N2 C6 1.377(6) . ?
N3 C7 1.355(6) . ?
N3 C11 1.356(6) . ?
N4 C12 1.331(6) . ?
N4 N7 1.344(6) . ?
N5 C13 1.310(6) . ?
N6 C1 1.331(6) . ?
N6 C14 1.342(6) . ?
N7 C23 1.328(6) . ?
N8 C24 1.319(7) . ?
N8 C12 1.341(6) . ?
N9 C37 1.326(8) . ?
N9 C33 1.361(7) . ?
N10 C39 1.332(10) . ?
N10 C43 1.423(11) . ?
F1 C38 1.282(8) . ?
F2 C38 1.303(8) . ?
F3 C38 1.354(8) . ?
C1 C2 1.482(7) . ?
C2 C3 1.395(7) . ?
C3 C4 1.391(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.372(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.379(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.479(7) . ?
C7 C8 1.396(7) . ?
C8 C9 1.382(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.374(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.385(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.498(7) . ?
C13 C14 1.431(7) . ?
C13 C18 1.532(7) . ?
C14 C15 1.522(7) . ?
C15 C20 1.515(9) . ?
C15 C19 1.521(9) . ?
C15 C16 1.532(8) . ?
C16 C17 1.458(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.548(7) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C22 1.516(8) . ?
C18 C21 1.522(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.420(7) . ?
C23 C28 1.521(8) . ?
C24 C25 1.508(7) . ?
C25 C26 1.450(9) . ?
C25 C30 1.528(10) . ?
C25 C29 1.554(10) . ?
C26 C27 1.468(12) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.494(11) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C32 1.483(8) . ?
C28 C31 1.515(10) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.358(9) . ?
C33 H33 0.9300 . ?
C34 C35 1.373(10) . ?
C34 H34 0.9300 . ?
C35 C36 1.368(10) . ?
C35 H35 0.9300 . ?
C36 C37 1.377(9) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C39 C40 1.386(12) . ?
C39 H39 0.9300 . ?
C40 C41 1.317(14) . ?
C40 H40 0.9300 . ?
C41 C42 1.297(13) . ?
C41 H41 0.9300 . ?
C42 C43 1.283(12) . ?
C42 H42 0.9300 . ?
C43 H43 0.9300 . ?
C44 C46 1.345(11) 2_665 ?
C44 C45 1.362(12) . ?
C45 C46 1.372(12) . ?
C46 C44 1.345(11) 2_665 ?
