#------------------------------------------------------------------------------
#$Date: 2022-02-06 06:39:45 +0200 (Sun, 06 Feb 2022) $
#$Revision: 272819 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/57/1565720.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_1565720
loop_
_publ_author_name
'Zhang, Yusheng'
'Duan, Wuhua'
'Wang, Qiang'
'Zheng, Lei'
'Wang, Jianchen'
'Chen, Jing'
'Sun, Taoxiang'
_publ_section_title
;
 Covalency between the uranyl ion and dithiophosphinate by sulfur
 K-edge X-ray absorption spectroscopy and density functional theory
;
_journal_issue                   1
_journal_name_full               'Journal of Synchrotron Radiation'
_journal_page_first              11
_journal_page_last               20
_journal_paper_doi               10.1107/S160057752101198X
_journal_volume                  29
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H22 F12 O3 P2 S4 U, C2 H6 O'
_chemical_formula_sum            'C32 H28 F12 O4 P2 S4 U'
_chemical_formula_weight         1132.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.5607(6)
_cell_length_b                   8.1303(3)
_cell_length_c                   59.7044(13)
_cell_measurement_reflns_used    4125
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      70.7010
_cell_measurement_theta_min      5.3930
_cell_volume                     8038.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4273
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -89.00 -55.00   1.00    2.00    --  -40.81 -38.00 -30.00   34
  2  ω    -92.00  -3.00   1.00    2.00    --  -40.81 125.00-150.00   89
  3  ω     26.00  64.00   1.00    2.00    --   40.81-125.00  90.00   38
  4  ω    110.00 169.00   1.00    7.00    --  100.91 125.00-120.00   59
  5  ω     44.00 121.00   1.00    7.00    --  100.91 -45.00-150.00   77
  6  ω     57.00 130.00   1.00    7.00    --  100.91 -61.00  90.00   73
  7  ω     98.00 144.00   1.00    7.00    --  100.91  45.00 -60.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0064878000
_diffrn_orient_matrix_UB_12      0.1167562000
_diffrn_orient_matrix_UB_13      0.0202921000
_diffrn_orient_matrix_UB_21      -0.0603441000
_diffrn_orient_matrix_UB_22      0.1184981000
_diffrn_orient_matrix_UB_23      -0.0111690000
_diffrn_orient_matrix_UB_31      -0.0703694000
_diffrn_orient_matrix_UB_32      -0.0907803000
_diffrn_orient_matrix_UB_33      0.0114271000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0822
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            19109
_diffrn_reflns_point_group_measured_fraction_full 0.784
_diffrn_reflns_point_group_measured_fraction_max 0.755
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.570
_diffrn_reflns_theta_min         4.443
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.900
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_description       plate
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         6.197
_refine_diff_density_min         -2.112
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details
;
 Flack x determined using 2747 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.147(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         11827
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0900P)²+51.5220P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1675
_refine_ls_wR_factor_ref         0.1779
_reflns_Friedel_coverage         0.535
_reflns_Friedel_fraction_full    0.569
_reflns_Friedel_fraction_max     0.532
_reflns_number_gt                9865
_reflns_number_total             11827
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            yw5001sup1.cif
_cod_data_source_block           IV
_cod_depositor_comments
'Adding full bibliography for 1565717--1565720.cif.'
_cod_database_code               1565720
_cod_database_fobs_code          1565720
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.755
_shelx_estimated_absorpt_t_min   0.199
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 C30-C29
 1.54 with sigma of 0.02
 O7-H7
 0.85 with sigma of 0.01
 C62A-C61
 1.54 with sigma of 0.02
 C62A-C61 = C62B-C61
 1.54 with sigma of 0.02
 U1-H3
 2.891388 with sigma of 0.02
 C29-H3
 1.940519 with sigma of 0.02
 U2-H7
 2.860598 with sigma of 0.02
 C61-H7
 1.876164 with sigma of 0.02
 O7-C62A
 2.42 with sigma of 0.04
 O7-C62B
 2.42 with sigma of 0.04
 F6A-C14A \\sim F5A-C14A \\sim F5B-C14B \\sim F4A-C14A \\sim F4B-C14B \\sim
F6B-C14B
 with sigma of 0.02
 C14A-C13 \\sim C14B-C13
 with sigma of 0.02
 F6A-F5A \\sim F5B-F6B
 with sigma of 0.02
 F6A-F4A \\sim F4B-F6B
 with sigma of 0.02
 F4A-F5A \\sim F4B-F5B
 with sigma of 0.02
3. Rigid bond restraints
 C8, F4A, C13, F5A, F6A, C12, C14A, C9, C10, C11, F6B, C14B, F5B, F4B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15, F7, F9, F8, C20, C17, C21, C16, C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F19, F21, F20, C51, C52, C53, C50, C48, C49, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F23, C55, F22, F24, C59, C58, C54, C60, C56, C57
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F16, F18, C45, C41, F17, C40, C43, C42, C44, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F15, F14, F13, C33, C39, C38, C34, C37, C36, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O7, C61, C62A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C62B, C61, O7, C62A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(F18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C62B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(F6B)=Sof(C14B)=Sof(F4B)=Sof(F5B)=1-FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(C14A)=FVAR(1)
 Sof(H61C)=Sof(H61D)=Sof(C62B)=Sof(H62D)=Sof(H62E)=Sof(H62F)=1-FVAR(2)
 Sof(H61A)=Sof(H61B)=Sof(C62A)=Sof(H62A)=Sof(H62B)=Sof(H62C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C29(H29A,H29B), C61(H61A,H61B), C61(H61C,H61D), C63(H63A,H63B)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C3(H3A), C55(H55), C24(H24), C25(H25),
 C51(H51), C4(H4), C2(H2), C17(H17), C58(H58), C5(H5), C23(H23), C16(H16),
 C50(H50), C48(H48), C18(H18), C26(H26), C49(H49), C19(H19), C34(H34), C44(H44),
  C43(H43), C42(H42), C41(H41), C56(H56), C37(H37), C36(H36), C57(H57), C35(H35)
6.c Fitted hexagon refined as free rotating group:
 C8(C9,C10,C11,C12,C13), C40(C45,C44,C43,C42,C41)
6.d Tetrahedral OH refined with riding coordinates:
 O4(H4A), O8(H8)
6.e Idealised Me refined with riding coordinates:
 C62B(H62D,H62E,H62F)
6.f Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C62A(H62A,H62B,
 H62C)
6.g Idealised tetrahedral OH refined with riding coordinates:
 O7(H7), O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.540
_oxdiff_exptl_absorpt_empirical_full_min 0.725
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.49022(4) 0.91342(10) 0.62177(2) 0.0348(2) Uani 1 1 d D . . . .
U2 U 0.75773(4) 0.41835(10) 0.37663(2) 0.0364(2) Uani 1 1 d D . . . .
S4 S 0.6133(3) 0.7646(8) 0.59452(8) 0.0342(12) Uani 1 1 d . . . . .
P2 P 0.5720(3) 0.8953(8) 0.56810(9) 0.0302(11) Uani 1 1 d . . . . .
S8 S 0.6343(3) 0.2671(8) 0.40388(9) 0.0355(12) Uani 1 1 d . . . . .
S7 S 0.7708(4) 0.5310(12) 0.42119(15) 0.0476(18) Uani 1 1 d . . . . .
P4 P 0.6758(3) 0.3955(8) 0.43041(10) 0.0319(12) Uani 1 1 d . . . . .
S3 S 0.4742(5) 1.0265(10) 0.57667(11) 0.0413(17) Uani 1 1 d . . . . .
P1 P 0.5296(4) 0.7648(10) 0.67560(9) 0.0466(17) Uani 1 1 d . . . . .
S2 S 0.5792(5) 0.6775(12) 0.64741(10) 0.058(2) Uani 1 1 d . . . . .
S5 S 0.7989(6) 0.4501(16) 0.33033(13) 0.077(3) Uani 1 1 d . . . . .
P3 P 0.7178(4) 0.2759(11) 0.32244(11) 0.0490(17) Uani 1 1 d . . . . .
S6 S 0.6647(5) 0.1933(13) 0.35068(12) 0.071(3) Uani 1 1 d . . . . .
S1 S 0.4448(5) 0.9324(15) 0.66781(13) 0.069(3) Uani 1 1 d . . . . .
F23 F 0.744(2) 0.468(3) 0.5052(4) 0.086(7) Uani 1 1 d . U . . .
C15 C 0.6562(17) 1.022(3) 0.5587(4) 0.031(4) Uani 1 1 d . U . . .
O7 O 0.8699(8) 0.600(2) 0.3759(4) 0.045(4) Uani 1 1 d D U . . .
H7 H 0.9110 0.5591 0.3707 0.067 Uiso 1 1 calc DR . . . .
F7 F 0.7925(12) 0.735(3) 0.5669(3) 0.071(5) Uani 1 1 d . U . . .
F9 F 0.6961(9) 0.702(2) 0.5440(3) 0.057(4) Uani 1 1 d . U . . .
O3 O 0.3793(9) 1.0921(19) 0.6222(4) 0.049(4) Uani 1 1 d D U . . .
H3 H 0.3323 1.0638 0.6242 0.074 Uiso 1 1 calc DR . . . .
F11 F 0.6143(12) 0.965(3) 0.5097(4) 0.070(6) Uani 1 1 d . . . . .
F8 F 0.8109(10) 0.787(2) 0.5319(3) 0.061(4) Uani 1 1 d . U . . .
F19 F 0.4521(10) 0.237(2) 0.4318(3) 0.064(4) Uani 1 1 d . U . . .
O6 O 0.8279(9) 0.269(3) 0.3814(4) 0.065(6) Uani 1 1 d . . . . .
O2 O 0.4190(9) 0.755(2) 0.6157(3) 0.040(4) Uani 1 1 d . . . . .
F2 F 0.5266(16) 0.970(4) 0.7483(4) 0.092(9) Uani 1 1 d . . . . .
F21 F 0.5505(9) 0.203(2) 0.4548(3) 0.057(4) Uani 1 1 d . U . . .
F16 F 0.5899(15) 0.054(4) 0.3065(7) 0.125(12) Uani 1 1 d . U . . .
O5 O 0.6893(11) 0.582(2) 0.3717(2) 0.037(4) Uani 1 1 d . U . . .
O4 O 0.2399(17) 0.964(4) 0.6253(8) 0.094(10) Uani 1 1 d . . . . .
H4A H 0.2243 0.9559 0.6123 0.141 Uiso 1 1 calc R . . . .
F20 F 0.4352(12) 0.288(2) 0.4664(3) 0.072(5) Uani 1 1 d . U . . .
C8 C 0.4822(11) 0.589(3) 0.6908(4) 0.050(6) Uani 1 1 d . U . . .
C9 C 0.3984(11) 0.593(3) 0.6918(4) 0.089(12) Uani 1 1 d G U . . .
H9 H 0.3703 0.6822 0.6861 0.107 Uiso 1 1 calc R . . . .
C10 C 0.3566(9) 0.462(4) 0.7014(5) 0.120(16) Uani 1 1 d G U . . .
H10 H 0.3005 0.4647 0.7021 0.144 Uiso 1 1 calc R . . A .
C11 C 0.3986(16) 0.328(3) 0.7100(5) 0.121(16) Uani 1 1 d G U . B 2
H11 H 0.3706 0.2412 0.7164 0.145 Uiso 1 1 calc R . . B 2
C12 C 0.4824(16) 0.325(2) 0.7090(5) 0.101(14) Uani 1 1 d G U . . .
H12 H 0.5105 0.2352 0.7147 0.121 Uiso 1 1 calc R . . B .
C13 C 0.5242(9) 0.455(3) 0.6993(4) 0.056(6) Uani 1 1 d DG U . . .
C3 C 0.740(3) 0.964(5) 0.6939(8) 0.066(10) Uani 1 1 d . . . . .
H3A H 0.7879 0.9850 0.6864 0.079 Uiso 1 1 calc R . . . .
F10 F 0.5189(14) 1.078(2) 0.5261(3) 0.061(5) Uani 1 1 d . . . . .
C55 C 0.7371(19) 0.100(3) 0.4441(5) 0.043(5) Uani 1 1 d . U . . .
H55 H 0.7313 0.0772 0.4289 0.052 Uiso 1 1 calc R . . . .
F22 F 0.6300(17) 0.458(3) 0.4903(5) 0.087(6) Uani 1 1 d . U . . .
F1 F 0.4584(11) 0.886(3) 0.7194(3) 0.064(5) Uani 1 1 d . . . . .
F15 F 0.7331(16) 0.226(3) 0.2607(4) 0.095(7) Uani 1 1 d . U . . .
F24 F 0.7252(15) 0.578(2) 0.4731(3) 0.065(5) Uani 1 1 d . U . . .
C22 C 0.5335(13) 0.751(3) 0.5464(3) 0.034(5) Uani 1 1 d . . . . .
C24 C 0.473(2) 0.479(4) 0.5413(7) 0.050(7) Uani 1 1 d . . . . .
H24 H 0.4590 0.3776 0.5473 0.060 Uiso 1 1 calc R . . . .
F14 F 0.7944(11) 0.396(3) 0.2794(3) 0.065(5) Uani 1 1 d . U . . .
C20 C 0.7294(18) 0.976(4) 0.5530(4) 0.037(5) Uani 1 1 d . U . . .
C25 C 0.4573(17) 0.514(4) 0.5194(6) 0.043(7) Uani 1 1 d . . . . .
H25 H 0.4317 0.4365 0.5104 0.052 Uiso 1 1 calc R . . . .
F3 F 0.5270(14) 0.714(3) 0.7384(4) 0.087(7) Uani 1 1 d . . . . .
C51 C 0.4542(17) 0.595(4) 0.4494(4) 0.046(5) Uani 1 1 d . U . . .
H51 H 0.4041 0.5624 0.4548 0.055 Uiso 1 1 calc R . . . .
C27 C 0.5178(13) 0.789(3) 0.5238(4) 0.035(5) Uani 1 1 d . . . . .
C4 C 0.736(3) 1.000(4) 0.7160(10) 0.070(12) Uani 1 1 d . . . . .
H4 H 0.7804 1.0484 0.7230 0.084 Uiso 1 1 calc R . . . .
C1 C 0.6067(14) 0.856(3) 0.6940(4) 0.034(5) Uani 1 1 d . . . . .
C2 C 0.6770(16) 0.898(3) 0.6819(5) 0.046(6) Uani 1 1 d . . . . .
H2 H 0.6806 0.8818 0.6665 0.056 Uiso 1 1 calc R . . . .
C59 C 0.7301(16) 0.288(4) 0.4742(4) 0.042(5) Uani 1 1 d . U . . .
C52 C 0.5105(16) 0.484(3) 0.4466(6) 0.042(6) Uani 1 1 d . U . . .
C28 C 0.5371(16) 0.953(5) 0.5132(4) 0.044(6) Uani 1 1 d . . . . .
C17 C 0.702(2) 1.304(4) 0.5586(6) 0.060(7) Uani 1 1 d . U . . .
H17 H 0.6921 1.4155 0.5610 0.072 Uiso 1 1 calc R . . . .
F13 F 0.7381(19) 0.481(5) 0.2511(5) 0.113(11) Uani 1 1 d . U . . .
C58 C 0.7689(19) 0.169(4) 0.4877(4) 0.051(6) Uani 1 1 d . U . . .
H58 H 0.7848 0.1970 0.5021 0.061 Uiso 1 1 calc R . . . .
F12 F 0.4961(19) 0.972(3) 0.4941(4) 0.087(8) Uani 1 1 d . . . . .
C21 C 0.7623(17) 0.798(4) 0.5490(5) 0.048(5) Uani 1 1 d . U . . .
O1 O 0.5549(10) 1.070(3) 0.6276(3) 0.053(5) Uani 1 1 d . . . . .
C6 C 0.6008(17) 0.899(3) 0.7161(5) 0.043(6) Uani 1 1 d . . . . .
C5 C 0.666(2) 0.966(5) 0.7281(6) 0.058(8) Uani 1 1 d . . . . .
H5 H 0.6629 0.9856 0.7435 0.070 Uiso 1 1 calc R . . . .
C23 C 0.5108(16) 0.600(3) 0.5548(4) 0.038(6) Uani 1 1 d . . . . .
H23 H 0.5206 0.5765 0.5698 0.046 Uiso 1 1 calc R . . . .
C53 C 0.4904(12) 0.307(4) 0.4497(5) 0.042(5) Uani 1 1 d . U . . .
C54 C 0.7139(13) 0.251(3) 0.4519(4) 0.033(4) Uani 1 1 d . U . . .
C16 C 0.6442(18) 1.195(3) 0.5613(5) 0.048(5) Uani 1 1 d . U . . .
H16 H 0.5929 1.2325 0.5651 0.057 Uiso 1 1 calc R . . . .
F18 F 0.613(2) -0.193(4) 0.3114(6) 0.141(10) Uani 1 1 d . U . . .
C31 C 0.2326(19) 0.805(5) 0.6364(5) 0.071(10) Uani 1 1 d . . . . .
H31A H 0.1893 0.8100 0.6473 0.085 Uiso 1 1 calc R . . . .
H31B H 0.2823 0.7811 0.6444 0.085 Uiso 1 1 calc R . . . .
C50 C 0.466(2) 0.759(4) 0.4446(7) 0.070(9) Uani 1 1 d . U . . .
H50 H 0.4227 0.8310 0.4442 0.084 Uiso 1 1 calc R . . . .
C29 C 0.383(2) 1.273(3) 0.6198(4) 0.066(8) Uani 1 1 d D U . . .
H29A H 0.3421 1.3097 0.6093 0.079 Uiso 1 1 calc R . . . .
H29B H 0.4355 1.3050 0.6141 0.079 Uiso 1 1 calc R . . . .
C61 C 0.878(2) 0.775(3) 0.3759(6) 0.082(10) Uani 1 1 d D U . . .
H61A H 0.9266 0.8054 0.3839 0.098 Uiso 0.54(6) 1 calc R . P C 1
H61B H 0.8323 0.8229 0.3838 0.098 Uiso 0.54(6) 1 calc R . P C 1
H61C H 0.9187 0.8090 0.3653 0.098 Uiso 0.46(6) 1 calc R . P C 2
H61D H 0.8936 0.8132 0.3907 0.098 Uiso 0.46(6) 1 calc R . P C 2
C60 C 0.710(2) 0.445(5) 0.4848(5) 0.056(6) Uani 1 1 d . U . . .
O8 O 1.0056(16) 0.457(5) 0.3729(8) 0.095(12) Uani 1 1 d . . . . .
H8 H 1.0489 0.5053 0.3732 0.143 Uiso 1 1 calc R . . . .
C48 C 0.607(2) 0.691(4) 0.4366(5) 0.055(6) Uani 1 1 d . U . . .
H48 H 0.6582 0.7258 0.4325 0.066 Uiso 1 1 calc R . . D .
C18 C 0.778(2) 1.254(4) 0.5523(5) 0.057(6) Uani 1 1 d . U . . .
H18 H 0.8184 1.3310 0.5500 0.069 Uiso 1 1 calc R . . . .
F4A F 0.655(2) 0.545(4) 0.6931(7) 0.058(10) Uani 0.63(4) 1 d D U P E 1
C26 C 0.4804(17) 0.671(4) 0.5103(5) 0.053(7) Uani 1 1 d . . . . .
H26 H 0.4704 0.6946 0.4953 0.064 Uiso 1 1 calc R . . . .
C64 C 1.031(3) 0.168(6) 0.3784(8) 0.095(13) Uani 1 1 d . . . . .
H64A H 1.0881 0.1516 0.3799 0.142 Uiso 1 1 calc GR . . . .
H64B H 1.0057 0.0674 0.3738 0.142 Uiso 1 1 calc GR . . . .
H64C H 1.0090 0.2031 0.3925 0.142 Uiso 1 1 calc GR . . . .
C33 C 0.6411(15) 0.376(4) 0.3044(5) 0.049(6) Uani 1 1 d . U . . .
F17 F 0.611(2) -0.125(6) 0.2805(6) 0.148(13) Uani 1 1 d . U . . .
C49 C 0.544(2) 0.816(4) 0.4402(7) 0.071(9) Uani 1 1 d . U . . .
H49 H 0.5560 0.9274 0.4396 0.085 Uiso 1 1 calc R . . . .
C39 C 0.727(2) 0.380(5) 0.2679(5) 0.064(6) Uani 1 1 d . U . . .
F5A F 0.639(3) 0.372(6) 0.7175(6) 0.107(16) Uani 0.63(4) 1 d D U P E 1
C38 C 0.6501(16) 0.412(3) 0.2812(5) 0.046(5) Uani 1 1 d . U . . .
C19 C 0.7943(16) 1.092(4) 0.5494(6) 0.052(6) Uani 1 1 d . U . . .
H19 H 0.8456 1.0570 0.5453 0.063 Uiso 1 1 calc R . . . .
C34 C 0.566(2) 0.415(4) 0.3137(7) 0.065(7) Uani 1 1 d . U . . .
H34 H 0.5569 0.3886 0.3286 0.078 Uiso 1 1 calc R . . F .
C63 C 1.016(2) 0.296(5) 0.3613(6) 0.074(10) Uani 1 1 d . . . . .
H63A H 0.9672 0.2701 0.3529 0.088 Uiso 1 1 calc R . . . .
H63B H 1.0607 0.3022 0.3509 0.088 Uiso 1 1 calc R . . . .
F6A F 0.628(2) 0.303(4) 0.6829(7) 0.087(11) Uani 0.63(4) 1 d D U P E 1
C40 C 0.7659(13) 0.096(3) 0.3084(4) 0.056(6) Uani 1 1 d . U . . .
C45 C 0.7244(10) -0.040(3) 0.3003(4) 0.064(7) Uani 1 1 d G U . . .
C44 C 0.7667(15) -0.170(3) 0.2907(4) 0.088(10) Uani 1 1 d G U . . .
H44 H 0.7390 -0.2608 0.2852 0.105 Uiso 1 1 calc R . . . .
C43 C 0.8504(15) -0.163(3) 0.2892(5) 0.088(9) Uani 1 1 d G U . . .
H43 H 0.8787 -0.2501 0.2828 0.105 Uiso 1 1 calc R . . . .
C42 C 0.8918(10) -0.027(3) 0.2973(5) 0.095(11) Uani 1 1 d G U . . .
H42 H 0.9479 -0.0227 0.2963 0.114 Uiso 1 1 calc R . . . .
C41 C 0.8496(13) 0.103(3) 0.3069(4) 0.067(7) Uani 1 1 d G U . . .
H41 H 0.8773 0.1939 0.3124 0.081 Uiso 1 1 calc R . . . .
C7 C 0.5268(18) 0.867(4) 0.7305(4) 0.053(8) Uani 1 1 d . . . . .
C14A C 0.611(2) 0.416(4) 0.6979(5) 0.048(7) Uani 0.63(4) 1 d D U P E 1
C30 C 0.369(4) 1.349(6) 0.6423(6) 0.106(17) Uani 1 1 d D U . . .
H30A H 0.3557 1.2649 0.6530 0.158 Uiso 1 1 calc GR . . . .
H30B H 0.3258 1.4269 0.6414 0.158 Uiso 1 1 calc GR . . . .
H30C H 0.4175 1.4044 0.6471 0.158 Uiso 1 1 calc GR . . . .
C56 C 0.7690(19) -0.020(4) 0.4581(7) 0.047(6) Uani 1 1 d . U . . .
H56 H 0.7803 -0.1237 0.4524 0.056 Uiso 1 1 calc R . . . .
C32 C 0.216(2) 0.666(5) 0.6201(7) 0.083(11) Uani 1 1 d . . . . .
H32A H 0.1627 0.6803 0.6138 0.125 Uiso 1 1 calc GR . . . .
H32B H 0.2180 0.5628 0.6279 0.125 Uiso 1 1 calc GR . . . .
H32C H 0.2551 0.6675 0.6084 0.125 Uiso 1 1 calc GR . . . .
C37 C 0.588(3) 0.492(4) 0.2707(8) 0.060(8) Uani 1 1 d . U . . .
H37 H 0.5964 0.5310 0.2563 0.072 Uiso 1 1 calc R . . . .
C62A C 0.881(4) 0.845(8) 0.3523(8) 0.09(3) Uani 0.54(6) 1 d D U P C 1
H62A H 0.9361 0.8477 0.3472 0.135 Uiso 0.54(6) 1 calc GR . P C 1
H62B H 0.8594 0.9546 0.3523 0.135 Uiso 0.54(6) 1 calc GR . P C 1
H62C H 0.8498 0.7770 0.3424 0.135 Uiso 0.54(6) 1 calc GR . P C 1
C36 C 0.513(2) 0.517(5) 0.2805(9) 0.063(8) Uani 1 1 d . U . . .
H36 H 0.4692 0.5505 0.2719 0.075 Uiso 1 1 calc R . . G .
C57 C 0.784(2) 0.011(4) 0.4800(6) 0.054(7) Uani 1 1 d . U . . .
H57 H 0.8033 -0.0704 0.4895 0.064 Uiso 1 1 calc R . . . .
C35 C 0.506(2) 0.491(4) 0.3020(7) 0.056(7) Uani 1 1 d . U . H 2
H35 H 0.4589 0.5249 0.3094 0.068 Uiso 1 1 calc R . . H 2
C47 C 0.5932(19) 0.532(4) 0.4390(5) 0.041(5) Uani 1 1 d . U . I 2
C46 C 0.632(3) -0.055(5) 0.2990(8) 0.077(8) Uani 1 1 d . U . J 2
F6B F 0.644(3) 0.546(7) 0.7198(6) 0.069(15) Uani 0.37(4) 1 d D U P E 2
C14B C 0.613(3) 0.452(5) 0.7035(7) 0.049(10) Uani 0.37(4) 1 d D U P E 2
F4B F 0.653(4) 0.504(6) 0.6856(6) 0.045(11) Uani 0.37(4) 1 d D U P E 2
F5B F 0.648(4) 0.305(5) 0.7060(13) 0.10(3) Uani 0.37(4) 1 d D U P E 2
C62B C 0.795(4) 0.848(9) 0.3695(18) 0.12(2) Uani 0.46(6) 1 d D U P C 2
H62D H 0.7805 0.8108 0.3548 0.176 Uiso 0.46(6) 1 calc R . P C 2
H62E H 0.7989 0.9663 0.3695 0.176 Uiso 0.46(6) 1 calc R . P C 2
H62F H 0.7554 0.8139 0.3801 0.176 Uiso 0.46(6) 1 calc R . P C 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 '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
S3 U1 S4 70.60(17) . . ?
S3 U1 S2 140.11(18) . . ?
S2 U1 S4 69.87(16) . . ?
S1 U1 S4 138.98(19) . . ?
S1 U1 S3 150.0(2) . . ?
S1 U1 S2 69.9(2) . . ?
O3 U1 S4 145.4(6) . . ?
O3 U1 S3 74.8(6) . . ?
O3 U1 S2 144.5(6) . . ?
O3 U1 S1 75.5(6) . . ?
O2 U1 S4 92.9(5) . . ?
O2 U1 S3 88.8(6) . . ?
O2 U1 S2 88.0(6) . . ?
O2 U1 S1 93.4(6) . . ?
O2 U1 O3 86.0(7) . . ?
O1 U1 S4 89.1(6) . . ?
O1 U1 S3 90.6(8) . . ?
O1 U1 S2 93.9(7) . . ?
O1 U1 S1 85.9(8) . . ?
O1 U1 O3 91.5(8) . . ?
O1 U1 O2 177.5(8) . . ?
S7 U2 S8 70.21(19) . . ?
S7 U2 S5 149.8(2) . . ?
S7 U2 S6 139.7(2) . . ?
S5 U2 S8 138.77(19) . . ?
S6 U2 S8 69.51(17) . . ?
S6 U2 S5 70.2(2) . . ?
O7 U2 S8 146.0(5) . . ?
O7 U2 S7 75.8(5) . . ?
O7 U2 S5 74.9(5) . . ?
O7 U2 S6 144.4(5) . . ?
O6 U2 S8 94.9(7) . . ?
O6 U2 S7 91.3(8) . . ?
O6 U2 S5 93.5(8) . . ?
O6 U2 S6 90.1(8) . . ?
O6 U2 O7 85.0(9) . . ?
O6 U2 O5 176.7(10) . . ?
O5 U2 S8 87.8(6) . . ?
O5 U2 S7 87.9(5) . . ?
O5 U2 S5 85.6(6) . . ?
O5 U2 S6 92.6(6) . . ?
O5 U2 O7 91.7(7) . . ?
P2 S4 U1 88.9(2) . . ?
S3 P2 S4 110.7(4) . . ?
C15 P2 S4 106.2(8) . . ?
C15 P2 S3 113.4(10) . . ?
C15 P2 C22 113.7(11) . . ?
C22 P2 S4 109.2(9) . . ?
C22 P2 S3 103.7(8) . . ?
P4 S8 U2 88.9(3) . . ?
P4 S7 U2 91.2(3) . . ?
S7 P4 S8 109.7(4) . . ?
C54 P4 S8 109.5(8) . . ?
C54 P4 S7 105.8(7) . . ?
C47 P4 S8 106.2(11) . . ?
C47 P4 S7 109.4(11) . . ?
C47 P4 C54 116.2(12) . . ?
P2 S3 U1 89.7(3) . . ?
S2 P1 S1 109.4(4) . . ?
C8 P1 S2 108.0(8) . . ?
C8 P1 S1 109.7(8) . . ?
C1 P1 S2 111.2(8) . . ?
C1 P1 S1 110.4(8) . . ?
C1 P1 C8 108.2(10) . . ?
P1 S2 U1 90.1(3) . . ?
P3 S5 U2 90.2(3) . . ?
S5 P3 S6 109.3(4) . . ?
C33 P3 S5 106.5(10) . . ?
C33 P3 S6 109.5(10) . . ?
C33 P3 C40 112.1(11) . . ?
C40 P3 S5 111.9(9) . . ?
C40 P3 S6 107.6(9) . . ?
P3 S6 U2 90.3(3) . . ?
P1 S1 U1 90.1(3) . . ?
C20 C15 P2 129(2) . . ?
C20 C15 C16 116(3) . . ?
C16 C15 P2 114(2) . . ?
U2 O7 H7 113.6 . . ?
C61 O7 U2 133.7(17) . . ?
C61 O7 H7 109.5 . . ?
U1 O3 H3 124.8 . . ?
C29 O3 U1 125.7(16) . . ?
C29 O3 H3 109.5 . . ?
C31 O4 H4A 109.5 . . ?
C9 C8 P1 115.2(13) . . ?
C9 C8 C13 120.0 . . ?
C13 C8 P1 124.6(13) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.00(6) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0 . . ?
C13 C12 H12 120.0 . . ?
C8 C13 C14A 129.5(18) . . ?
C8 C13 C14B 125(2) . . ?
C12 C13 C8 120.0 . . ?
C12 C13 C14A 110.1(18) . . ?
C12 C13 C14B 114(2) . . ?
C4 C3 H3A 117.9 . . ?
C4 C3 C2 124(4) . . ?
C2 C3 H3A 117.9 . . ?
C54 C55 H55 118.9 . . ?
C54 C55 C56 122(3) . . ?
C56 C55 H55 118.9 . . ?
C27 C22 P2 126(2) . . ?
C23 C22 P2 113.6(17) . . ?
C23 C22 C27 120(2) . . ?
C25 C24 H24 120.4 . . ?
C25 C24 C23 119(3) . . ?
C23 C24 H24 120.4 . . ?
C15 C20 C21 128(3) . . ?
C15 C20 C19 123(3) . . ?
C19 C20 C21 109(2) . . ?
C24 C25 H25 120.2 . . ?
C24 C25 C26 120(3) . . ?
C26 C25 H25 120.2 . . ?
C52 C51 H51 118.7 . . ?
C52 C51 C50 123(3) . . ?
C50 C51 H51 118.7 . . ?
C22 C27 C28 124(2) . . ?
C26 C27 C22 119(3) . . ?
C26 C27 C28 117(2) . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120(4) . . ?
C5 C4 H4 120.0 . . ?
C2 C1 P1 111(2) . . ?
C6 C1 P1 129.0(19) . . ?
C6 C1 C2 119(3) . . ?
C3 C2 C1 117(3) . . ?
C3 C2 H2 121.5 . . ?
C1 C2 H2 121.5 . . ?
C58 C59 C60 117(2) . . ?
C54 C59 C58 119(3) . . ?
C54 C59 C60 124(2) . . ?
C51 C52 C53 120(3) . . ?
C51 C52 C47 121(3) . . ?
C53 C52 C47 120(2) . . ?
F11 C28 F10 106(3) . . ?
F11 C28 C27 110(3) . . ?
F11 C28 F12 111(2) . . ?
F10 C28 C27 113(2) . . ?
F10 C28 F12 107(3) . . ?
F12 C28 C27 110(2) . . ?
C16 C17 H17 120.1 . . ?
C16 C17 C18 120(3) . . ?
C18 C17 H17 120.1 . . ?
C59 C58 H58 119.0 . . ?
C57 C58 C59 122(3) . . ?
C57 C58 H58 119.0 . . ?
F7 C21 F9 106(2) . . ?
F7 C21 F8 113(3) . . ?
F7 C21 C20 112(2) . . ?
F9 C21 C20 106(2) . . ?
F8 C21 F9 107(2) . . ?
F8 C21 C20 113(2) . . ?
C1 C6 C5 122(3) . . ?
C1 C6 C7 124(3) . . ?
C5 C6 C7 113(3) . . ?
C4 C5 C6 117(4) . . ?
C4 C5 H5 121.6 . . ?
C6 C5 H5 121.6 . . ?
C22 C23 C24 122(2) . . ?
C22 C23 H23 119.0 . . ?
C24 C23 H23 119.0 . . ?
F19 C53 C52 114(3) . . ?
F21 C53 F19 105(2) . . ?
F21 C53 F20 105(2) . . ?
F21 C53 C52 118(2) . . ?
F20 C53 F19 102.4(19) . . ?
F20 C53 C52 110(2) . . ?
C55 C54 P4 115.3(18) . . ?
C55 C54 C59 118(2) . . ?
C59 C54 P4 126(2) . . ?
C15 C16 H16 118.4 . . ?
C17 C16 C15 123(3) . . ?
C17 C16 H16 118.4 . . ?
O4 C31 H31A 109.1 . . ?
O4 C31 H31B 109.1 . . ?
O4 C31 C32 113(3) . . ?
H31A C31 H31B 107.8 . . ?
C32 C31 H31A 109.1 . . ?
C32 C31 H31B 109.1 . . ?
C51 C50 H50 120.2 . . ?
C51 C50 C49 120(3) . . ?
C49 C50 H50 120.2 . . ?
O3 C29 H29A 110.0 . . ?
O3 C29 H29B 110.0 . . ?
O3 C29 C30 109(3) . . ?
H29A C29 H29B 108.3 . . ?
C30 C29 H29A 110.0 . . ?
C30 C29 H29B 110.0 . . ?
O7 C61 H61A 109.2 . . ?
O7 C61 H61B 109.2 . . ?
O7 C61 H61C 110.2 . . ?
O7 C61 H61D 110.2 . . ?
O7 C61 C62A 112(3) . . ?
O7 C61 C62B 108(3) . . ?
H61A C61 H61B 107.9 . . ?
H61C C61 H61D 108.5 . . ?
C62A C61 H61A 109.2 . . ?
C62A C61 H61B 109.2 . . ?
C62B C61 H61C 110.2 . . ?
C62B C61 H61D 110.2 . . ?
F23 C60 C59 114(3) . . ?
F22 C60 F23 100(3) . . ?
F22 C60 C59 114(3) . . ?
F24 C60 F23 106(3) . . ?
F24 C60 F22 105(3) . . ?
F24 C60 C59 117(3) . . ?
C63 O8 H8 109.5 . . ?
C49 C48 H48 118.6 . . ?
C47 C48 H48 118.6 . . ?
C47 C48 C49 123(3) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 C17 121(3) . . ?
C19 C18 H18 119.6 . . ?
C25 C26 H26 119.8 . . ?
C27 C26 C25 120(3) . . ?
C27 C26 H26 119.8 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
C38 C33 P3 126(2) . . ?
C34 C33 P3 119(3) . . ?
C34 C33 C38 116(3) . . ?
C50 C49 C48 117(3) . . ?
C50 C49 H49 121.5 . . ?
C48 C49 H49 121.5 . . ?
F15 C39 C38 113(3) . . ?
F14 C39 F15 101(3) . . ?
F14 C39 C38 115(2) . . ?
F13 C39 F15 109(3) . . ?
F13 C39 F14 102(3) . . ?
F13 C39 C38 115(3) . . ?
C33 C38 C39 124(3) . . ?
C37 C38 C33 118(3) . . ?
C37 C38 C39 118(3) . . ?
C20 C19 H19 121.2 . . ?
C18 C19 C20 118(3) . . ?
C18 C19 H19 121.2 . . ?
C33 C34 H34 118.2 . . ?
C35 C34 C33 124(4) . . ?
C35 C34 H34 118.2 . . ?
O8 C63 H63A 110.0 . . ?
O8 C63 H63B 110.0 . . ?
C64 C63 O8 108(4) . . ?
C64 C63 H63A 110.0 . . ?
C64 C63 H63B 110.0 . . ?
H63A C63 H63B 108.4 . . ?
C45 C40 P3 124.8(13) . . ?
C45 C40 C41 120.0 . . ?
C41 C40 P3 115.2(13) . . ?
C40 C45 C46 125(2) . . ?
C44 C45 C40 120.0 . . ?
C44 C45 C46 115(2) . . ?
C45 C44 H44 120.0 . . ?
C45 C44 C43 120.0 . . ?
C43 C44 H44 120.0 . . ?
C44 C43 H43 120.0 . . ?
C44 C43 C42 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C42 H42 120.0 . . ?
C41 C42 C43 120.0 . . ?
C41 C42 H42 120.0 . . ?
C40 C41 H41 120.0 . . ?
C42 C41 C40 120.0 . . ?
C42 C41 H41 120.0 . . ?
F2 C7 C6 110(2) . . ?
F1 C7 F2 109(3) . . ?
F1 C7 F3 107(2) . . ?
F1 C7 C6 113(2) . . ?
F3 C7 F2 107(3) . . ?
F3 C7 C6 111(3) . . ?
F4A C14A C13 112(3) . . ?
F4A C14A F5A 102(3) . . ?
F4A C14A F6A 107(3) . . ?
F5A C14A C13 111(3) . . ?
F6A C14A C13 114(3) . . ?
F6A C14A F5A 110(4) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C55 C56 H56 119.4 . . ?
C57 C56 C55 121(3) . . ?
C57 C56 H56 119.4 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C38 C37 H37 118.3 . . ?
C38 C37 C36 123(4) . . ?
C36 C37 H37 118.3 . . ?
C61 C62A H62A 109.5 . . ?
C61 C62A H62B 109.5 . . ?
C61 C62A H62C 109.5 . . ?
H62A C62A H62B 109.5 . . ?
H62A C62A H62C 109.5 . . ?
H62B C62A H62C 109.5 . . ?
C37 C36 H36 120.8 . . ?
C35 C36 C37 118(4) . . ?
C35 C36 H36 120.8 . . ?
C58 C57 H57 121.3 . . ?
C56 C57 C58 117(3) . . ?
C56 C57 H57 121.3 . . ?
C34 C35 H35 119.9 . . ?
C36 C35 C34 120(4) . . ?
C36 C35 H35 119.9 . . ?
C52 C47 P4 128(2) . . ?
C48 C47 P4 116(2) . . ?
C48 C47 C52 116(3) . . ?
F16 C46 F18 105(4) . . ?
F16 C46 F17 119(4) . . ?
F16 C46 C45 120(3) . . ?
F18 C46 C45 105(4) . . ?
F17 C46 F18 92(4) . . ?
F17 C46 C45 110(3) . . ?
F6B C14B C13 119(4) . . ?
F4B C14B C13 111(4) . . ?
F4B C14B F6B 103(3) . . ?
F4B C14B F5B 99(3) . . ?
F5B C14B C13 117(5) . . ?
F5B C14B F6B 106(4) . . ?
C61 C62B H62D 109.5 . . ?
C61 C62B H62E 109.5 . . ?
C61 C62B H62F 109.5 . . ?
H62D C62B H62E 109.5 . . ?
H62D C62B H62F 109.5 . . ?
H62E C62B H62F 109.5 . . ?
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 S4 2.875(5) . ?
U1 S3 2.858(7) . ?
U1 S2 2.862(8) . ?
U1 S1 2.854(8) . ?
U1 O3 2.342(13) . ?
U1 O2 1.782(17) . ?
U1 O1 1.701(18) . ?
U2 S8 2.887(6) . ?
U2 S7 2.822(9) . ?
U2 S5 2.859(8) . ?
U2 S6 2.850(8) . ?
U2 O7 2.376(13) . ?
U2 O6 1.704(19) . ?
U2 O5 1.773(18) . ?
S4 P2 2.021(8) . ?
P2 S3 2.005(9) . ?
P2 C15 1.82(3) . ?
P2 C22 1.86(2) . ?
S8 P4 2.018(8) . ?
S7 P4 1.998(10) . ?
P4 C54 1.85(2) . ?
P4 C47 1.83(3) . ?
P1 S2 2.003(9) . ?
P1 S1 2.011(11) . ?
P1 C8 1.865(19) . ?
P1 C1 1.84(3) . ?
S5 P3 2.008(11) . ?
P3 S6 2.017(10) . ?
P3 C33 1.85(3) . ?
P3 C40 1.86(2) . ?
F23 C60 1.36(4) . ?
C15 C20 1.31(4) . ?
C15 C16 1.43(4) . ?
O7 H7 0.8200 . ?
O7 C61 1.43(2) . ?
F7 C21 1.28(3) . ?
F9 C21 1.37(3) . ?
O3 H3 0.8200 . ?
O3 C29 1.48(2) . ?
F11 C28 1.30(3) . ?
F8 C21 1.31(3) . ?
F19 C53 1.36(3) . ?
F2 C7 1.35(4) . ?
F21 C53 1.34(3) . ?
F16 C46 1.21(5) . ?
O4 H4A 0.8200 . ?
O4 C31 1.46(5) . ?
F20 C53 1.36(3) . ?
C8 C9 1.3900 . ?
C8 C13 1.3900 . ?
C9 H9 0.9300 . ?
C9 C10 1.3900 . ?
C10 H10 0.9300 . ?
C10 C11 1.3900 . ?
C11 H11 0.9300 . ?
C11 C12 1.3900 . ?
C12 H12 0.9300 . ?
C12 C13 1.3900 . ?
C13 C14A 1.47(4) . ?
C13 C14B 1.50(4) . ?
C3 H3A 0.9300 . ?
C3 C4 1.35(7) . ?
C3 C2 1.37(5) . ?
F10 C28 1.31(4) . ?
C55 H55 0.9300 . ?
C55 C54 1.37(4) . ?
C55 C56 1.39(4) . ?
F22 C60 1.36(5) . ?
F1 C7 1.32(4) . ?
F15 C39 1.33(4) . ?
F24 C60 1.32(4) . ?
C22 C27 1.41(3) . ?
C22 C23 1.38(3) . ?
C24 H24 0.9300 . ?
C24 C25 1.36(5) . ?
C24 C23 1.42(4) . ?
F14 C39 1.32(4) . ?
C20 C21 1.57(4) . ?
C20 C19 1.45(4) . ?
C25 H25 0.9300 . ?
C25 C26 1.44(5) . ?
F3 C7 1.33(4) . ?
C51 H51 0.9300 . ?
C51 C52 1.31(4) . ?
C51 C50 1.37(5) . ?
C27 C28 1.51(4) . ?
C27 C26 1.40(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.40(6) . ?
C1 C2 1.41(3) . ?
C1 C6 1.37(4) . ?
C2 H2 0.9300 . ?
C59 C58 1.41(4) . ?
C59 C54 1.39(3) . ?
C59 C60 1.46(5) . ?
C52 C53 1.49(4) . ?
C52 C47 1.49(4) . ?
C28 F12 1.34(3) . ?
C17 H17 0.9300 . ?
C17 C16 1.32(4) . ?
C17 C18 1.37(5) . ?
F13 C39 1.31(5) . ?
C58 H58 0.9300 . ?
C58 C57 1.38(5) . ?
C6 C5 1.41(5) . ?
C6 C7 1.52(4) . ?
C5 H5 0.9300 . ?
C23 H23 0.9300 . ?
C16 H16 0.9300 . ?
F18 C46 1.38(5) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.51(5) . ?
C50 H50 0.9300 . ?
C50 C49 1.40(6) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.50(2) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C61 H61C 0.9700 . ?
C61 H61D 0.9700 . ?
C61 C62A 1.523(18) . ?
C61 C62B 1.54(3) . ?
O8 H8 0.8200 . ?
O8 C63 1.48(5) . ?
C48 H48 0.9300 . ?
C48 C49 1.46(5) . ?
C48 C47 1.32(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.35(5) . ?
F4A C14A 1.31(3) . ?
C26 H26 0.9300 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C64 C63 1.48(5) . ?
C33 C38 1.42(4) . ?
C33 C34 1.39(4) . ?
F17 C46 1.30(5) . ?
C49 H49 0.9300 . ?
C39 C38 1.52(4) . ?
F5A C14A 1.31(3) . ?
C38 C37 1.37(5) . ?
C19 H19 0.9300 . ?
C34 H34 0.9300 . ?
C34 C35 1.37(5) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
F6A C14A 1.31(3) . ?
C40 C45 1.3900 . ?
C40 C41 1.3900 . ?
C45 C44 1.3900 . ?
C45 C46 1.54(5) . ?
C44 H44 0.9300 . ?
C44 C43 1.3900 . ?
C43 H43 0.9300 . ?
C43 C42 1.3900 . ?
C42 H42 0.9300 . ?
C42 C41 1.3900 . ?
C41 H41 0.9300 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C56 H56 0.9300 . ?
C56 C57 1.35(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C37 H37 0.9300 . ?
C37 C36 1.38(6) . ?
C62A H62A 0.9600 . ?
C62A H62B 0.9600 . ?
C62A H62C 0.9600 . ?
C36 H36 0.9300 . ?
C36 C35 1.31(7) . ?
C57 H57 0.9300 . ?
C35 H35 0.9300 . ?
F6B C14B 1.34(3) . ?
C14B F4B 1.33(3) . ?
C14B F5B 1.33(3) . ?
C62B H62D 0.9600 . ?
C62B H62E 0.9600 . ?
C62B H62F 0.9600 . ?
