# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1893014'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2019-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H42 N6 Ni O14 S2 U'
_chemical_formula_weight         1047.53

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.4686(3)
_cell_length_b                   9.9123(4)
_cell_length_c                   21.7475(8)
_cell_angle_alpha                90
_cell_angle_beta                 93.972(2)
_cell_angle_gamma                90
_cell_volume                     1821.17(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    48315
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      25.68

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_F_000             1032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    5.146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.428
_exptl_absorpt_correction_T_max  0.512
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and three ω scans with 2° steps (392 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            48315
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.784
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3452
_reflns_number_gt                2865
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms bound to O and N atoms were
 found on a difference Fourier map and all the others were introduced
 at calculated positions; all were treated as riding atoms with an isotropic
 displacement parameter equal to 1.2 times that of the parent atom (1.5
 for CH₃, with optimized geometry). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0475P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3452
_refine_ls_number_parameters     239
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0720
_refine_ls_wR_factor_gt          0.0689
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.001
_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_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 0.5000 0.5000 0.5000 0.02100(9) Uani 1 2 d S . P . .
Ni1 Ni 0.0000 0.5000 1.0000 0.02628(17) Uani 1 2 d S . P . .
S1 S 0.35397(10) 0.46614(10) 0.90062(4) 0.02699(18) Uani 1 1 d . . . . .
O1 O 0.6987(2) 0.5481(2) 0.51801(9) 0.0279(4) Uani 1 1 d . . . . .
O2 O 0.5147(2) 0.3952(2) 0.60337(9) 0.0286(5) Uani 1 1 d . . . . .
O3 O 0.4017(2) 0.5941(2) 0.59737(9) 0.0275(5) Uani 1 1 d . . . . .
O4 O 0.2515(3) 0.5730(2) 0.91615(10) 0.0420(6) Uani 1 1 d . . . . .
O5 O 0.2938(3) 0.3339(2) 0.91480(11) 0.0527(7) Uani 1 1 d . . . . .
O6 O 0.5137(4) 0.4820(4) 0.92615(16) 0.0938(18) Uani 1 1 d . U . . .
O7 O 0.4388(3) 0.7406(2) 0.49666(9) 0.0298(5) Uani 1 1 d . . . . .
H7A H 0.4198 0.7937 0.4646 0.036 Uiso 1 1 d R U . . .
H7B H 0.4981 0.7785 0.5281 0.036 Uiso 1 1 d R U . . .
N1 N -0.0488(3) 0.6925(3) 0.99759(12) 0.0316(6) Uani 1 1 d . . . . .
H1 H -0.1458 0.6897 1.0172 0.038 Uiso 1 1 d R U . . .
N2 N -0.1389(3) 0.4641(3) 0.92725(14) 0.0321(6) Uani 1 1 d . . . . .
H2 H -0.2356 0.4715 0.9373 0.039 Uiso 1 1 d R U . . .
N3 N 0.0605(4) 0.8526(3) 0.77354(16) 0.0512(8) Uani 1 1 d . . . . .
C1 C 0.4441(4) 0.4909(2) 0.62828(18) 0.0232(8) Uani 1 1 d . . . . .
C2 C 0.4106(4) 0.4799(3) 0.69487(16) 0.0227(7) Uani 1 1 d . . . . .
C3 C 0.4823(3) 0.3783(3) 0.73107(13) 0.0265(6) Uani 1 1 d . . . . .
H3 H 0.5460 0.3127 0.7128 0.032 Uiso 1 1 calc R U . . .
C4 C 0.4615(3) 0.3722(3) 0.79330(13) 0.0262(6) Uani 1 1 d . . . . .
H4 H 0.5104 0.3027 0.8179 0.031 Uiso 1 1 calc R U . . .
C5 C 0.3681(4) 0.4689(3) 0.81967(15) 0.0230(6) Uani 1 1 d . . . . .
C6 C 0.2911(3) 0.5671(3) 0.78374(13) 0.0236(6) Uani 1 1 d . . . . .
H6 H 0.2237 0.6301 0.8018 0.028 Uiso 1 1 calc R U . . .
C7 C 0.3128(3) 0.5732(3) 0.72143(13) 0.0238(6) Uani 1 1 d . . . . .
H7 H 0.2611 0.6411 0.6967 0.029 Uiso 1 1 calc R U . . .
C8 C -0.0625(4) 0.7636(4) 0.93765(18) 0.0429(10) Uani 1 1 d . . . . .
H8A H 0.0407 0.7608 0.9189 0.051 Uiso 1 1 calc R U . . .
H8B H -0.0896 0.8594 0.9444 0.051 Uiso 1 1 calc R U . . .
C9 C -0.1875(4) 0.7007(4) 0.89399(17) 0.0484(10) Uani 1 1 d . . . . .
H9A H -0.2891 0.6989 0.9139 0.058 Uiso 1 1 calc R U . . .
H9B H -0.2024 0.7576 0.8566 0.058 Uiso 1 1 calc R U . . .
C10 C -0.1471(4) 0.5599(4) 0.87519(16) 0.0432(9) Uani 1 1 d . . . . .
H10A H -0.2279 0.5283 0.8434 0.052 Uiso 1 1 calc R U . . .
H10B H -0.0437 0.5611 0.8565 0.052 Uiso 1 1 calc R U . . .
C11 C -0.1033(4) 0.3270(4) 0.90518(18) 0.0497(10) Uani 1 1 d . . . . .
H11A H -0.0102 0.3297 0.8801 0.060 Uiso 1 1 calc R U . . .
H11B H -0.1946 0.2917 0.8792 0.060 Uiso 1 1 calc R U . . .
C12 C -0.0703(4) 0.2380(4) 0.9597(2) 0.0495(11) Uani 1 1 d . . . . .
H12A H -0.0283 0.1500 0.9467 0.059 Uiso 1 1 calc R U . . .
H12B H -0.1687 0.2215 0.9806 0.059 Uiso 1 1 calc R U . . .
C13 C 0.1060(4) 0.9550(5) 0.79009(17) 0.0378(8) Uani 1 1 d . . . . .
C14 C 0.1643(5) 1.0879(4) 0.8096(2) 0.0544(11) Uani 1 1 d . . . . .
H14A H 0.2632 1.1070 0.7904 0.082 Uiso 1 1 calc R U . . .
H14B H 0.1835 1.0894 0.8545 0.082 Uiso 1 1 calc R U . . .
H14C H 0.0852 1.1564 0.7969 0.082 Uiso 1 1 calc R U . . .


_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 O1 1.766(2) 3_666 ?
U1 O1 1.766(2) . ?
U1 O7 2.441(2) . ?
U1 O7 2.441(2) 3_666 ?
U1 O2 2.4717(19) . ?
U1 O2 2.4717(19) 3_666 ?
U1 O3 2.5082(19) 3_666 ?
U1 O3 2.5083(19) . ?
Ni1 N2 1.938(3) 3_567 ?
Ni1 N2 1.938(3) . ?
Ni1 N1 1.952(3) . ?
Ni1 N1 1.952(3) 3_567 ?
S1 O4 1.424(2) . ?
S1 O6 1.435(3) . ?
S1 O5 1.447(3) . ?
S1 C5 1.773(3) . ?
O2 C1 1.263(4) . ?
O3 C1 1.262(4) . ?
O7 H7A 0.8798 . ?
O7 H7B 0.9011 . ?
N1 C8 1.480(4) . ?
N1 C12 1.492(5) 3_567 ?
N1 H1 0.9521 . ?
N2 C10 1.476(5) . ?
N2 C11 1.479(5) . ?
N2 H2 0.8651 . ?
N3 C13 1.135(5) . ?
C1 C2 1.499(5) . ?
C2 C3 1.391(4) . ?
C2 C7 1.393(4) . ?
C3 C4 1.378(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.383(4) . ?
C6 C7 1.381(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.508(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.500(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.489(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N1 1.492(5) 3_567 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.459(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

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 U1 O1 180.0 3_666 . ?
O1 U1 O7 93.44(9) 3_666 . ?
O1 U1 O7 86.56(9) . . ?
O1 U1 O7 86.56(9) 3_666 3_666 ?
O1 U1 O7 93.44(9) . 3_666 ?
O7 U1 O7 180.0 . 3_666 ?
O1 U1 O2 94.33(8) 3_666 . ?
O1 U1 O2 85.67(8) . . ?
O7 U1 O2 115.78(6) . . ?
O7 U1 O2 64.22(6) 3_666 . ?
O1 U1 O2 85.67(8) 3_666 3_666 ?
O1 U1 O2 94.33(8) . 3_666 ?
O7 U1 O2 64.22(6) . 3_666 ?
O7 U1 O2 115.78(6) 3_666 3_666 ?
O2 U1 O2 180.0 . 3_666 ?
O1 U1 O3 94.55(8) 3_666 3_666 ?
O1 U1 O3 85.45(8) . 3_666 ?
O7 U1 O3 114.86(7) . 3_666 ?
O7 U1 O3 65.14(7) 3_666 3_666 ?
O2 U1 O3 127.80(7) . 3_666 ?
O2 U1 O3 52.20(7) 3_666 3_666 ?
O1 U1 O3 85.46(8) 3_666 . ?
O1 U1 O3 94.55(8) . . ?
O7 U1 O3 65.14(7) . . ?
O7 U1 O3 114.86(7) 3_666 . ?
O2 U1 O3 52.20(7) . . ?
O2 U1 O3 127.80(7) 3_666 . ?
O3 U1 O3 180.0 3_666 . ?
N2 Ni1 N2 180.0 3_567 . ?
N2 Ni1 N1 87.58(12) 3_567 . ?
N2 Ni1 N1 92.42(12) . . ?
N2 Ni1 N1 92.42(12) 3_567 3_567 ?
N2 Ni1 N1 87.58(12) . 3_567 ?
N1 Ni1 N1 180.0 . 3_567 ?
O4 S1 O6 113.6(2) . . ?
O4 S1 O5 113.18(15) . . ?
O6 S1 O5 110.7(2) . . ?
O4 S1 C5 107.93(15) . . ?
O6 S1 C5 104.82(18) . . ?
O5 S1 C5 105.94(15) . . ?
C1 O2 U1 94.54(19) . . ?
C1 O3 U1 92.8(2) . . ?
U1 O7 H7A 129.4 . . ?
U1 O7 H7B 106.2 . . ?
H7A O7 H7B 114.5 . . ?
C8 N1 C12 109.7(3) . 3_567 ?
C8 N1 Ni1 119.5(2) . . ?
C12 N1 Ni1 107.6(2) 3_567 . ?
C8 N1 H1 113.0 . . ?
C12 N1 H1 107.5 3_567 . ?
Ni1 N1 H1 98.5 . . ?
C10 N2 C11 110.0(3) . . ?
C10 N2 Ni1 120.1(2) . . ?
C11 N2 Ni1 107.9(2) . . ?
C10 N2 H2 98.4 . . ?
C11 N2 H2 112.2 . . ?
Ni1 N2 H2 108.0 . . ?
O3 C1 O2 120.4(3) . . ?
O3 C1 C2 120.5(3) . . ?
O2 C1 C2 119.1(3) . . ?
C3 C2 C7 119.6(3) . . ?
C3 C2 C1 119.7(3) . . ?
C7 C2 C1 120.7(3) . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.3(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 120.7(3) . . ?
C6 C5 S1 120.7(2) . . ?
C4 C5 S1 118.5(2) . . ?
C7 C6 C5 119.7(3) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C6 C7 C2 120.1(3) . . ?
C6 C7 H7 120.0 . . ?
C2 C7 H7 120.0 . . ?
N1 C8 C9 111.5(3) . . ?
N1 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
N1 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
C10 C9 C8 113.2(3) . . ?
C10 C9 H9A 108.9 . . ?
C8 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
C8 C9 H9B 108.9 . . ?
H9A C9 H9B 107.8 . . ?
N2 C10 C9 112.9(3) . . ?
N2 C10 H10A 109.0 . . ?
C9 C10 H10A 109.0 . . ?
N2 C10 H10B 109.0 . . ?
C9 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
N2 C11 C12 108.5(3) . . ?
N2 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
N2 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
C11 C12 N1 107.7(3) . 3_567 ?
C11 C12 H12A 110.2 . . ?
N1 C12 H12A 110.2 3_567 . ?
C11 C12 H12B 110.2 . . ?
N1 C12 H12B 110.2 3_567 . ?
H12A C12 H12B 108.5 . . ?
N3 C13 C14 178.4(4) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7A O4 0.88 2.16 2.934(3) 146.0 4_575
O7 H7A O6 0.88 2.52 3.232(4) 138.1 4_575
O7 H7B O5 0.90 2.16 3.014(4) 159.0 2_656
O7 H7B O6 0.90 2.26 2.935(4) 131.9 2_656
N1 H1 O5 0.95 2.02 2.924(3) 158.6 3_567
N2 H2 O6 0.87 2.12 2.945(4) 158.6 1_455
C8 H8A O4 0.99 2.58 3.322(4) 131.4 .
C12 H12B O7 0.99 2.38 3.324(5) 159.0 2_546

_refine_diff_density_max         1.292
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.138

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 1893018'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2019-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H44 Cu N4 O18 S2 U2'
_chemical_formula_weight         1376.43

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'
O O 0.0106 0.0060 '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'
Cu Cu 0.3201 1.2651 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.3508(8)
_cell_length_b                   13.7624(5)
_cell_length_c                   14.1862(9)
_cell_angle_alpha                90
_cell_angle_beta                 103.615(3)
_cell_angle_gamma                90
_cell_volume                     2153.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    101431
_cell_measurement_theta_min      2.09
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.122
_exptl_crystal_F_000             1306
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    8.163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.323
_exptl_absorpt_correction_T_max  0.442
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 34 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and ten ω scans with 2° steps (720 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            101431
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.091
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4088
_reflns_number_gt                3300
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms bound to N atoms were found on a 
 difference Fourier map and all the others were introduced at calculated
 positions; all were treated as riding atoms with an isotropic displacement
 parameter equal to 1.2 times that of the parent atom (1.5 for CH₃, with
 optimized geometry). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0362P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4088
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0258
_refine_ls_wR_factor_ref         0.0676
_refine_ls_wR_factor_gt          0.0647
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.001
_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_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 0.24889(2) 0.49628(2) 0.43859(2) 0.03062(8) Uani 1 1 d . . . . .
Cu1 Cu 0.0000 0.5000 0.0000 0.03971(19) Uani 1 2 d S . P . .
S1 S 0.25433(9) 0.42066(7) 0.19929(7) 0.0330(2) Uani 1 1 d . . . . .
O1 O 0.2750(3) 0.3802(2) 0.4915(2) 0.0486(7) Uani 1 1 d . . . . .
O2 O 0.2185(2) 0.61139(19) 0.3843(2) 0.0434(7) Uani 1 1 d . . . . .
O3 O 0.4249(3) 0.48673(17) 0.3840(2) 0.0340(6) Uani 1 1 d . . . . .
O4 O 0.6124(3) 0.4346(3) 0.4303(2) 0.0616(9) Uani 1 1 d . . . . .
O5 O 0.2027(2) 0.41715(19) 0.28558(18) 0.0375(6) Uani 1 1 d . . . . .
O6 O 0.1680(2) 0.3794(2) 0.11698(19) 0.0427(7) Uani 1 1 d . . . . .
O7 O 0.2959(3) 0.51642(19) 0.1801(2) 0.0397(7) Uani 1 1 d . . . . .
O8 O 0.0348(2) 0.4572(2) 0.39420(19) 0.0421(7) Uani 1 1 d . . . . .
O9 O -0.1411(3) 0.4547(2) 0.4398(2) 0.0481(7) Uani 1 1 d . . . . .
N1 N -0.0485(3) 0.6057(2) 0.0828(2) 0.0450(9) Uani 1 1 d . . . . .
H1 H -0.1107 0.6313 0.0361 0.054 Uiso 1 1 d R U . . .
N2 N 0.1415(3) 0.5887(2) -0.0051(2) 0.0415(8) Uani 1 1 d . . . . .
H2 H 0.2050 0.5609 0.0462 0.050 Uiso 1 1 d R U . . .
C1 C 0.5098(3) 0.4304(3) 0.3754(3) 0.0343(9) Uani 1 1 d . . . . .
C2 C 0.4888(3) 0.3552(3) 0.2971(3) 0.0317(8) Uani 1 1 d . . . . .
C3 C 0.3834(3) 0.3422(2) 0.2230(3) 0.0292(8) Uani 1 1 d . . . . .
C4 C 0.3777(4) 0.2666(3) 0.1581(3) 0.0402(10) Uani 1 1 d . . . . .
H4 H 0.3061 0.2576 0.1084 0.048 Uiso 1 1 calc R U . . .
C5 C 0.4745(4) 0.2037(3) 0.1639(3) 0.0515(12) Uani 1 1 d . . . . .
H5 H 0.4692 0.1523 0.1183 0.062 Uiso 1 1 calc R U . . .
C6 C 0.5778(4) 0.2159(3) 0.2358(3) 0.0519(11) Uani 1 1 d . . . . .
H6 H 0.6441 0.1725 0.2406 0.062 Uiso 1 1 calc R U . . .
C7 C 0.5855(4) 0.2909(3) 0.3011(3) 0.0421(10) Uani 1 1 d . . . . .
H7 H 0.6580 0.2993 0.3500 0.051 Uiso 1 1 calc R U . . .
C8 C -0.0304(4) 0.4745(3) 0.4513(3) 0.0433(10) Uani 1 1 d . . . . .
C9 C 0.0531(4) 0.6741(3) 0.1101(3) 0.0467(11) Uani 1 1 d . . . . .
H9A H 0.1142 0.6486 0.1663 0.056 Uiso 1 1 calc R U . . .
H9B H 0.0239 0.7375 0.1284 0.056 Uiso 1 1 calc R U . . .
C10 C 0.1087(4) 0.6864(3) 0.0248(3) 0.0463(11) Uani 1 1 d . . . . .
H10A H 0.0501 0.7180 -0.0294 0.056 Uiso 1 1 calc R U . . .
H10B H 0.1818 0.7278 0.0427 0.056 Uiso 1 1 calc R U . . .
C11 C 0.2026(4) 0.5886(3) -0.0888(3) 0.0444(10) Uani 1 1 d . . . . .
C12 C 0.2199(5) 0.4831(3) -0.1192(4) 0.0492(12) Uani 1 1 d . . . . .
H12A H 0.2709 0.4845 -0.1670 0.059 Uiso 1 1 calc R U . . .
H12B H 0.2661 0.4478 -0.0614 0.059 Uiso 1 1 calc R U . . .
C13 C 0.1063(4) 0.4242(3) -0.1628(3) 0.0470(11) Uani 1 1 d . . . . .
H13 H 0.0482 0.4666 -0.2090 0.056 Uiso 1 1 calc R U . . .
C14 C 0.3301(4) 0.6333(3) -0.0539(3) 0.0545(12) Uani 1 1 d . . . . .
H14A H 0.3227 0.7016 -0.0367 0.082 Uiso 1 1 calc R U . . .
H14B H 0.3734 0.6290 -0.1060 0.082 Uiso 1 1 calc R U . . .
H14C H 0.3753 0.5977 0.0030 0.082 Uiso 1 1 calc R U . . .
C15 C 0.1289(4) 0.6466(3) -0.1747(3) 0.0490(11) Uani 1 1 d . . . . .
H15A H 0.0436 0.6270 -0.1873 0.074 Uiso 1 1 calc R U . . .
H15B H 0.1600 0.6337 -0.2323 0.074 Uiso 1 1 calc R U . . .
H15C H 0.1358 0.7161 -0.1595 0.074 Uiso 1 1 calc R U . . .
C16 C 0.1387(5) 0.3373(4) -0.2186(4) 0.0676(15) Uani 1 1 d . . . . .
H16A H 0.1961 0.2953 -0.1742 0.101 Uiso 1 1 calc R U . . .
H16B H 0.1759 0.3603 -0.2703 0.101 Uiso 1 1 calc R U . . .
H16C H 0.0651 0.3004 -0.2472 0.101 Uiso 1 1 calc R U . . .


_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 O2 1.760(3) . ?
U1 O1 1.760(3) . ?
U1 O3 2.311(3) . ?
U1 O4 2.337(3) 3_666 ?
U1 O5 2.374(2) . ?
U1 O8 2.423(3) . ?
U1 O9 2.434(3) 3_566 ?
Cu1 N1 2.026(3) 3_565 ?
Cu1 N1 2.026(3) . ?
Cu1 N2 2.032(3) 3_565 ?
Cu1 N2 2.032(3) . ?
Cu1 O6 2.767(3) . ?
S1 O7 1.447(3) . ?
S1 O6 1.451(3) . ?
S1 O5 1.477(3) . ?
S1 C3 1.787(4) . ?
O3 C1 1.264(4) . ?
O4 C1 1.241(4) . ?
O4 U1 2.338(3) 3_666 ?
O8 C8 1.242(5) . ?
O9 C8 1.258(5) . ?
O9 U1 2.434(3) 3_566 ?
N1 C9 1.469(5) . ?
N1 C13 1.495(5) 3_565 ?
N1 H1 0.9170 . ?
N2 C10 1.484(5) . ?
N2 C11 1.509(5) . ?
N2 H2 0.9742 . ?
C1 C2 1.496(5) . ?
C2 C7 1.400(5) . ?
C2 C3 1.406(5) . ?
C3 C4 1.381(5) . ?
C4 C5 1.386(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.372(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.376(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C8 1.558(9) 3_566 ?
C9 C10 1.500(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C15 1.531(6) . ?
C11 C12 1.540(6) . ?
C11 C14 1.543(6) . ?
C12 C13 1.526(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N1 1.495(5) 3_565 ?
C13 C16 1.527(6) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

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
O2 U1 O1 178.38(13) . . ?
O2 U1 O3 90.04(11) . . ?
O1 U1 O3 91.10(11) . . ?
O2 U1 O4 90.43(13) . 3_666 ?
O1 U1 O4 90.90(14) . 3_666 ?
O3 U1 O4 79.39(10) . 3_666 ?
O2 U1 O5 91.98(11) . . ?
O1 U1 O5 87.29(11) . . ?
O3 U1 O5 71.94(9) . . ?
O4 U1 O5 151.22(9) 3_666 . ?
O2 U1 O8 90.26(12) . . ?
O1 U1 O8 88.13(12) . . ?
O3 U1 O8 142.55(9) . . ?
O4 U1 O8 138.06(9) 3_666 . ?
O5 U1 O8 70.62(8) . . ?
O2 U1 O9 88.90(12) . 3_566 ?
O1 U1 O9 90.67(12) . 3_566 ?
O3 U1 O9 150.71(9) . 3_566 ?
O4 U1 O9 71.35(10) 3_666 3_566 ?
O5 U1 O9 137.35(9) . 3_566 ?
O8 U1 O9 66.73(9) . 3_566 ?
N1 Cu1 N1 180.00(19) 3_565 . ?
N1 Cu1 N2 85.10(13) 3_565 3_565 ?
N1 Cu1 N2 94.90(14) . 3_565 ?
N1 Cu1 N2 94.90(14) 3_565 . ?
N1 Cu1 N2 85.10(13) . . ?
N2 Cu1 N2 180.0 3_565 . ?
N1 Cu1 O6 70.97(11) 3_565 . ?
N1 Cu1 O6 109.03(11) . . ?
N2 Cu1 O6 93.29(11) 3_565 . ?
N2 Cu1 O6 86.71(11) . . ?
O7 S1 O6 113.14(18) . . ?
O7 S1 O5 113.32(17) . . ?
O6 S1 O5 109.24(16) . . ?
O7 S1 C3 107.26(17) . . ?
O6 S1 C3 106.47(17) . . ?
O5 S1 C3 106.98(16) . . ?
C1 O3 U1 143.7(2) . . ?
C1 O4 U1 151.1(3) . 3_666 ?
S1 O5 U1 134.20(15) . . ?
S1 O6 Cu1 119.18(15) . . ?
C8 O8 U1 120.2(3) . . ?
C8 O9 U1 120.1(3) . 3_566 ?
C9 N1 C13 115.7(3) . 3_565 ?
C9 N1 Cu1 108.0(3) . . ?
C13 N1 Cu1 118.0(2) 3_565 . ?
C9 N1 H1 111.6 . . ?
C13 N1 H1 104.7 3_565 . ?
Cu1 N1 H1 97.2 . . ?
C10 N2 C11 114.8(3) . . ?
C10 N2 Cu1 106.3(2) . . ?
C11 N2 Cu1 122.7(2) . . ?
C10 N2 H2 109.5 . . ?
C11 N2 H2 101.1 . . ?
Cu1 N2 H2 100.9 . . ?
O4 C1 O3 122.3(4) . . ?
O4 C1 C2 117.4(3) . . ?
O3 C1 C2 120.3(3) . . ?
C7 C2 C3 118.1(3) . . ?
C7 C2 C1 114.9(3) . . ?
C3 C2 C1 127.0(3) . . ?
C4 C3 C2 119.5(3) . . ?
C4 C3 S1 115.0(3) . . ?
C2 C3 S1 125.5(3) . . ?
C3 C4 C5 121.3(4) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C6 C5 C4 119.6(4) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C7 120.0(4) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C2 121.4(4) . . ?
C6 C7 H7 119.3 . . ?
C2 C7 H7 119.3 . . ?
O8 C8 O9 127.1(4) . . ?
O8 C8 C8 117.2(5) . 3_566 ?
O9 C8 C8 115.7(5) . 3_566 ?
N1 C9 C10 108.2(3) . . ?
N1 C9 H9A 110.1 . . ?
C10 C9 H9A 110.1 . . ?
N1 C9 H9B 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
N2 C10 C9 108.0(3) . . ?
N2 C10 H10A 110.1 . . ?
C9 C10 H10A 110.1 . . ?
N2 C10 H10B 110.1 . . ?
C9 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
N2 C11 C15 111.0(4) . . ?
N2 C11 C12 109.5(3) . . ?
C15 C11 C12 110.5(4) . . ?
N2 C11 C14 108.5(3) . . ?
C15 C11 C14 110.0(3) . . ?
C12 C11 C14 107.1(4) . . ?
C13 C12 C11 117.6(4) . . ?
C13 C12 H12A 107.9 . . ?
C11 C12 H12A 107.9 . . ?
C13 C12 H12B 107.9 . . ?
C11 C12 H12B 107.9 . . ?
H12A C12 H12B 107.2 . . ?
N1 C13 C12 108.6(4) 3_565 . ?
N1 C13 C16 112.4(4) 3_565 . ?
C12 C13 C16 110.0(4) . . ?
N1 C13 H13 108.6 3_565 . ?
C12 C13 H13 108.6 . . ?
C16 C13 H13 108.6 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O6 0.92 2.12 2.847(4) 135.3 3_565
N2 H2 O7 0.97 2.03 2.966(4) 160.3 .
C4 H4 O1 0.95 2.49 3.119(5) 123.7 4_565
C15 H15C O2 0.98 2.57 3.526(5) 163.6 4_575

_refine_diff_density_max         1.423
_refine_diff_density_min         -1.912
_refine_diff_density_rms         0.242

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1893017'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2019-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H92 Cu2 N8 O26 S4 U2'
_chemical_formula_weight         2072.79

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'
Cu Cu 0.3201 1.2651 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6903(6)
_cell_length_b                   11.6969(5)
_cell_length_c                   14.5245(8)
_cell_angle_alpha                94.145(3)
_cell_angle_beta                 97.373(3)
_cell_angle_gamma                107.703(3)
_cell_volume                     1863.32(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    105270
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_F_000             1022
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    5.090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.443
_exptl_absorpt_correction_T_max  0.666
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and twelve ω scans with 2° steps (791 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            105270
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.190
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7080
_reflns_number_gt                6532
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms bound to O and N atoms were
 found on a difference Fourier map and all the others were introduced at
 calculated positions; all were treated as riding atoms with an isotropic
 displacement parameter equal to 1.2 times that of the parent atom
 (1.5 for CH₃, with optimized geometry). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0227P)²+0.1636P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7080
_refine_ls_number_parameters     466
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0568
_refine_ls_wR_factor_gt          0.0556
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.002
_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_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 0.84446(2) 0.97729(2) 0.32676(2) 0.02062(5) Uani 1 1 d . . . . .
Cu1 Cu 0.73242(4) 0.48588(3) 0.23214(2) 0.02078(10) Uani 1 1 d . . . . .
S1 S 0.61001(8) 0.86408(7) 0.12075(5) 0.0244(2) Uani 1 1 d . . . . .
S2 S 0.74802(8) 1.22404(7) 0.42256(5) 0.0231(2) Uani 1 1 d . . . . .
O1 O 0.7445(2) 0.88223(19) 0.39196(15) 0.0261(6) Uani 1 1 d . . . . .
O2 O 0.9433(2) 1.07291(19) 0.26164(15) 0.0272(6) Uani 1 1 d . . . . .
O3 O 0.8253(2) 0.80117(19) 0.23038(14) 0.0264(6) Uani 1 1 d . . . . .
O4 O 0.8084(2) 0.63573(19) 0.13700(14) 0.0253(5) Uani 1 1 d . . . . .
O5 O 0.6760(2) 0.94840(19) 0.20570(14) 0.0294(6) Uani 1 1 d . . . . .
O6 O 0.5671(2) 0.74045(19) 0.14074(14) 0.0264(6) Uani 1 1 d . . . . .
O7 O 0.5177(2) 0.90756(19) 0.07298(15) 0.0290(6) Uani 1 1 d . . . . .
O8 O 0.9366(2) 1.09648(18) 0.46925(14) 0.0227(5) Uani 1 1 d . . . . .
O9 O 0.9914(2) 1.0944(2) 0.62051(14) 0.0266(6) Uani 1 1 d . . . . .
O10 O 0.7447(2) 1.12856(18) 0.34805(14) 0.0243(6) Uani 1 1 d . . . . .
O11 O 0.8676(2) 1.31321(19) 0.44693(15) 0.0288(6) Uani 1 1 d . . . . .
O12 O 0.6520(2) 1.2738(2) 0.39623(14) 0.0293(6) Uani 1 1 d . . . . .
O13 O 0.5627(2) 0.14387(19) 0.18017(15) 0.0308(6) Uani 1 1 d . . . . .
H13A H 0.5423 0.0752 0.1528 0.037 Uiso 1 1 d R U . . .
H13B H 0.5941 0.1270 0.2337 0.037 Uiso 1 1 d R U . . .
N1 N 0.7157(3) 0.3643(2) 0.12251(17) 0.0239(6) Uani 1 1 d . . . . .
H1 H 0.6793 0.2976 0.1401 0.029 Uiso 1 1 d R U . . .
N2 N 0.5609(3) 0.4836(2) 0.17737(17) 0.0229(6) Uani 1 1 d . . . . .
H2 H 0.5666 0.5596 0.1601 0.028 Uiso 1 1 d R U . . .
N3 N 0.7350(3) 0.5933(2) 0.34868(16) 0.0250(7) Uani 1 1 d . . . . .
H3 H 0.7473 0.6642 0.3316 0.030 Uiso 1 1 d R U . . .
N4 N 0.8959(3) 0.4802(2) 0.29419(18) 0.0262(7) Uani 1 1 d . . . . .
H4 H 0.8802 0.4245 0.3372 0.031 Uiso 1 1 d R U . . .
C1 C 0.8135(3) 0.7438(3) 0.1502(2) 0.0224(8) Uani 1 1 d . . . . .
C2 C 0.8065(3) 0.8110(3) 0.0656(2) 0.0234(8) Uani 1 1 d . . . . .
C3 C 0.7202(3) 0.8700(3) 0.0467(2) 0.0254(8) Uani 1 1 d . . . . .
C4 C 0.7175(4) 0.9305(3) -0.0321(2) 0.0309(9) Uani 1 1 d . . . . .
H4A H 0.6579 0.9696 -0.0452 0.037 Uiso 1 1 calc R U . . .
C5 C 0.8014(4) 0.9336(3) -0.0909(2) 0.0382(10) Uani 1 1 d . . . . .
H5 H 0.8004 0.9766 -0.1439 0.046 Uiso 1 1 calc R U . . .
C6 C 0.8874(4) 0.8751(3) -0.0742(2) 0.0366(9) Uani 1 1 d . . . . .
H6 H 0.9452 0.8781 -0.1151 0.044 Uiso 1 1 calc R U . . .
C7 C 0.8880(4) 0.8116(3) 0.0037(2) 0.0311(9) Uani 1 1 d . . . . .
H7 H 0.9445 0.7685 0.0145 0.037 Uiso 1 1 calc R U . . .
C8 C 0.9152(3) 1.0966(3) 0.5517(2) 0.0232(8) Uani 1 1 d . . . . .
C9 C 0.7926(3) 1.0977(3) 0.5737(2) 0.0258(8) Uani 1 1 d . . . . .
C10 C 0.7140(3) 1.1487(3) 0.5227(2) 0.0234(8) Uani 1 1 d . . . . .
C11 C 0.6040(4) 1.1454(3) 0.5515(2) 0.0355(9) Uani 1 1 d . . . . .
H11 H 0.5523 1.1821 0.5178 0.043 Uiso 1 1 calc R U . . .
C12 C 0.5692(4) 1.0889(4) 0.6289(3) 0.0465(11) Uani 1 1 d . . . . .
H12 H 0.4940 1.0870 0.6480 0.056 Uiso 1 1 calc R U . . .
C13 C 0.6444(4) 1.0356(4) 0.6779(3) 0.0507(12) Uani 1 1 d . . . . .
H13 H 0.6199 0.9946 0.7297 0.061 Uiso 1 1 calc R U . . .
C14 C 0.7555(4) 1.0419(3) 0.6514(2) 0.0369(10) Uani 1 1 d . . . . .
H14 H 0.8078 1.0074 0.6870 0.044 Uiso 1 1 calc R U . . .
C15 C 0.6288(3) 0.3902(3) 0.0484(2) 0.0277(8) Uani 1 1 d . . . . .
H15A H 0.6042 0.3260 -0.0052 0.033 Uiso 1 1 calc R U . . .
H15B H 0.6673 0.4685 0.0257 0.033 Uiso 1 1 calc R U . . .
C16 C 0.5203(3) 0.3946(3) 0.0918(2) 0.0258(8) Uani 1 1 d . . . . .
H16A H 0.4632 0.4185 0.0466 0.031 Uiso 1 1 calc R U . . .
H16B H 0.4773 0.3137 0.1082 0.031 Uiso 1 1 calc R U . . .
C17 C 0.4636(3) 0.4725(3) 0.2393(2) 0.0269(8) Uani 1 1 d . . . . .
C18 C 0.5171(3) 0.5698(3) 0.3240(2) 0.0298(8) Uani 1 1 d . . . . .
H18A H 0.5434 0.6493 0.3001 0.036 Uiso 1 1 calc R U . . .
H18B H 0.4508 0.5700 0.3600 0.036 Uiso 1 1 calc R U . . .
C19 C 0.6236(3) 0.5598(3) 0.3917(2) 0.0277(8) Uani 1 1 d . . . . .
H19 H 0.6053 0.4735 0.4037 0.033 Uiso 1 1 calc R U . . .
C20 C 0.3546(3) 0.4994(3) 0.1862(3) 0.0353(9) Uani 1 1 d . . . . .
H20A H 0.2983 0.5059 0.2293 0.053 Uiso 1 1 calc R U . . .
H20B H 0.3128 0.4339 0.1359 0.053 Uiso 1 1 calc R U . . .
H20C H 0.3829 0.5757 0.1595 0.053 Uiso 1 1 calc R U . . .
C21 C 0.4236(3) 0.3460(3) 0.2700(2) 0.0293(8) Uani 1 1 d . . . . .
H21A H 0.3750 0.3455 0.3203 0.044 Uiso 1 1 calc R U . . .
H21B H 0.4955 0.3234 0.2926 0.044 Uiso 1 1 calc R U . . .
H21C H 0.3746 0.2879 0.2168 0.044 Uiso 1 1 calc R U . . .
C22 C 0.6374(4) 0.6369(3) 0.4857(2) 0.0373(10) Uani 1 1 d . . . . .
H22A H 0.6997 0.6223 0.5310 0.056 Uiso 1 1 calc R U . . .
H22B H 0.5597 0.6146 0.5093 0.056 Uiso 1 1 calc R U . . .
H22C H 0.6617 0.7226 0.4766 0.056 Uiso 1 1 calc R U . . .
C23 C 0.8491(3) 0.6029(3) 0.4143(2) 0.0287(9) Uani 1 1 d . . . . .
H23A H 0.8766 0.6807 0.4553 0.034 Uiso 1 1 calc R U . . .
H23B H 0.8330 0.5365 0.4543 0.034 Uiso 1 1 calc R U . . .
C24 C 0.9454(3) 0.5953(3) 0.3578(2) 0.0331(9) Uani 1 1 d . . . . .
H24A H 0.9661 0.6649 0.3212 0.040 Uiso 1 1 calc R U . . .
H24B H 1.0198 0.5962 0.3994 0.040 Uiso 1 1 calc R U . . .
C25 C 0.9858(3) 0.4477(3) 0.2401(2) 0.0285(8) Uani 1 1 d . . . . .
C26 C 0.9151(3) 0.3379(3) 0.1687(2) 0.0324(9) Uani 1 1 d . . . . .
H26A H 0.9749 0.3068 0.1416 0.039 Uiso 1 1 calc R U . . .
H26B H 0.8681 0.2740 0.2029 0.039 Uiso 1 1 calc R U . . .
C27 C 0.8275(3) 0.3566(3) 0.0881(2) 0.0319(9) Uani 1 1 d . . . . .
H27 H 0.8675 0.4340 0.0634 0.038 Uiso 1 1 calc R U . . .
C28 C 1.0536(3) 0.5541(3) 0.1930(2) 0.0324(9) Uani 1 1 d . . . . .
H28A H 0.9952 0.5867 0.1586 0.049 Uiso 1 1 calc R U . . .
H28B H 1.1003 0.5272 0.1495 0.049 Uiso 1 1 calc R U . . .
H28C H 1.1092 0.6170 0.2405 0.049 Uiso 1 1 calc R U . . .
C29 C 1.0752(4) 0.4075(4) 0.3084(3) 0.0417(10) Uani 1 1 d . . . . .
H29A H 1.1230 0.4760 0.3548 0.063 Uiso 1 1 calc R U . . .
H29B H 1.1300 0.3797 0.2733 0.063 Uiso 1 1 calc R U . . .
H29C H 1.0294 0.3415 0.3402 0.063 Uiso 1 1 calc R U . . .
C30 C 0.7962(4) 0.2518(4) 0.0091(3) 0.0636(15) Uani 1 1 d . . . . .
H30A H 0.7644 0.1748 0.0343 0.095 Uiso 1 1 calc R U . . .
H30B H 0.8696 0.2532 -0.0173 0.095 Uiso 1 1 calc R U . . .
H30C H 0.7346 0.2606 -0.0399 0.095 Uiso 1 1 calc R U . . .


_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 O2 1.769(3) . ?
U1 O1 1.774(3) . ?
U1 O3 2.3401(19) . ?
U1 O8 2.3420(18) . ?
U1 O9 2.381(2) 2_776 ?
U1 O5 2.3882(19) . ?
U1 O10 2.4193(19) . ?
Cu1 N1 2.005(2) . ?
Cu1 N3 2.025(2) . ?
Cu1 N4 2.028(3) . ?
Cu1 N2 2.052(3) . ?
Cu1 O4 2.343(2) . ?
S1 O6 1.444(2) . ?
S1 O7 1.448(2) . ?
S1 O5 1.486(2) . ?
S1 C3 1.770(4) . ?
S2 O12 1.437(2) . ?
S2 O11 1.449(3) . ?
S2 O10 1.486(2) . ?
S2 C10 1.780(3) . ?
O3 C1 1.271(3) . ?
O4 C1 1.246(3) . ?
O8 C8 1.255(4) . ?
O9 C8 1.258(3) . ?
O9 U1 2.381(2) 2_776 ?
O13 H13A 0.8199 . ?
O13 H13B 0.8780 . ?
N1 C27 1.483(4) . ?
N1 C15 1.495(4) . ?
N1 H1 0.8424 . ?
N2 C16 1.489(4) . ?
N2 C17 1.519(4) . ?
N2 H2 0.9262 . ?
N3 C19 1.474(5) . ?
N3 C23 1.506(4) . ?
N3 H3 0.8581 . ?
N4 C24 1.487(4) . ?
N4 C25 1.509(5) . ?
N4 H4 0.9300 . ?
C1 C2 1.513(4) . ?
C2 C7 1.390(5) . ?
C2 C3 1.395(4) . ?
C3 C4 1.390(5) . ?
C4 C5 1.376(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.384(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.399(5) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.511(5) . ?
C9 C14 1.395(5) . ?
C9 C10 1.405(4) . ?
C10 C11 1.392(5) . ?
C11 C12 1.388(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(5) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.499(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C21 1.528(5) . ?
C17 C20 1.532(4) . ?
C17 C18 1.539(4) . ?
C18 C19 1.524(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C22 1.543(4) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.494(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C28 1.520(5) . ?
C25 C26 1.532(4) . ?
C25 C29 1.547(4) . ?
C26 C27 1.528(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C30 1.539(4) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

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
O2 U1 O1 179.49(9) . . ?
O2 U1 O3 93.96(9) . . ?
O1 U1 O3 86.34(9) . . ?
O2 U1 O8 93.56(9) . . ?
O1 U1 O8 86.41(9) . . ?
O3 U1 O8 145.90(7) . . ?
O2 U1 O9 87.31(10) . 2_776 ?
O1 U1 O9 93.18(9) . 2_776 ?
O3 U1 O9 71.51(7) . 2_776 ?
O8 U1 O9 75.70(7) . 2_776 ?
O2 U1 O5 90.83(9) . . ?
O1 U1 O5 88.86(9) . . ?
O3 U1 O5 72.91(7) . . ?
O8 U1 O5 140.13(7) . . ?
O9 U1 O5 144.14(7) 2_776 . ?
O2 U1 O10 89.70(9) . . ?
O1 U1 O10 89.80(9) . . ?
O3 U1 O10 141.04(7) . . ?
O8 U1 O10 72.16(6) . . ?
O9 U1 O10 147.46(6) 2_776 . ?
O5 U1 O10 68.25(6) . . ?
N1 Cu1 N3 173.36(12) . . ?
N1 Cu1 N4 95.58(10) . . ?
N3 Cu1 N4 86.10(10) . . ?
N1 Cu1 N2 85.62(10) . . ?
N3 Cu1 N2 92.22(10) . . ?
N4 Cu1 N2 175.41(12) . . ?
N1 Cu1 O4 87.20(10) . . ?
N3 Cu1 O4 99.00(9) . . ?
N4 Cu1 O4 96.64(10) . . ?
N2 Cu1 O4 87.84(10) . . ?
O6 S1 O7 114.90(14) . . ?
O6 S1 O5 112.09(13) . . ?
O7 S1 O5 110.10(12) . . ?
O6 S1 C3 106.20(14) . . ?
O7 S1 C3 107.62(15) . . ?
O5 S1 C3 105.30(15) . . ?
O12 S2 O11 114.25(14) . . ?
O12 S2 O10 109.44(12) . . ?
O11 S2 O10 112.05(15) . . ?
O12 S2 C10 107.00(16) . . ?
O11 S2 C10 107.82(14) . . ?
O10 S2 C10 105.79(13) . . ?
C1 O3 U1 151.5(2) . . ?
C1 O4 Cu1 126.1(2) . . ?
S1 O5 U1 139.82(12) . . ?
C8 O8 U1 135.5(2) . . ?
C8 O9 U1 145.5(2) . 2_776 ?
S2 O10 U1 137.20(11) . . ?
H13A O13 H13B 96.5 . . ?
C27 N1 C15 112.4(3) . . ?
C27 N1 Cu1 118.55(19) . . ?
C15 N1 Cu1 104.50(17) . . ?
C27 N1 H1 109.2 . . ?
C15 N1 H1 107.2 . . ?
Cu1 N1 H1 104.1 . . ?
C16 N2 C17 113.2(3) . . ?
C16 N2 Cu1 107.13(19) . . ?
C17 N2 Cu1 120.65(18) . . ?
C16 N2 H2 108.5 . . ?
C17 N2 H2 98.7 . . ?
Cu1 N2 H2 107.7 . . ?
C19 N3 C23 114.2(3) . . ?
C19 N3 Cu1 115.78(19) . . ?
C23 N3 Cu1 107.0(2) . . ?
C19 N3 H3 109.3 . . ?
C23 N3 H3 104.5 . . ?
Cu1 N3 H3 105.2 . . ?
C24 N4 C25 115.3(3) . . ?
C24 N4 Cu1 103.46(19) . . ?
C25 N4 Cu1 122.86(18) . . ?
C24 N4 H4 100.8 . . ?
C25 N4 H4 105.3 . . ?
Cu1 N4 H4 106.8 . . ?
O4 C1 O3 124.1(3) . . ?
O4 C1 C2 117.9(3) . . ?
O3 C1 C2 118.0(3) . . ?
C7 C2 C3 119.2(3) . . ?
C7 C2 C1 118.2(3) . . ?
C3 C2 C1 122.6(3) . . ?
C4 C3 C2 120.3(4) . . ?
C4 C3 S1 119.4(3) . . ?
C2 C3 S1 120.2(3) . . ?
C5 C4 C3 119.7(3) . . ?
C5 C4 H4A 120.1 . . ?
C3 C4 H4A 120.1 . . ?
C4 C5 C6 121.1(3) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C7 119.1(4) . . ?
C5 C6 H6 120.5 . . ?
C7 C6 H6 120.5 . . ?
C2 C7 C6 120.5(3) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
O8 C8 O9 123.4(3) . . ?
O8 C8 C9 120.8(3) . . ?
O9 C8 C9 115.7(3) . . ?
C14 C9 C10 118.0(3) . . ?
C14 C9 C8 116.2(3) . . ?
C10 C9 C8 125.8(3) . . ?
C11 C10 C9 120.0(3) . . ?
C11 C10 S2 116.3(2) . . ?
C9 C10 S2 123.7(3) . . ?
C12 C11 C10 120.7(3) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C13 C12 C11 119.6(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C14 119.9(4) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C9 121.6(3) . . ?
C13 C14 H14 119.2 . . ?
C9 C14 H14 119.2 . . ?
N1 C15 C16 107.0(3) . . ?
N1 C15 H15A 110.3 . . ?
C16 C15 H15A 110.3 . . ?
N1 C15 H15B 110.3 . . ?
C16 C15 H15B 110.3 . . ?
H15A C15 H15B 108.6 . . ?
N2 C16 C15 109.4(3) . . ?
N2 C16 H16A 109.8 . . ?
C15 C16 H16A 109.8 . . ?
N2 C16 H16B 109.8 . . ?
C15 C16 H16B 109.8 . . ?
H16A C16 H16B 108.2 . . ?
N2 C17 C21 110.6(3) . . ?
N2 C17 C20 109.6(3) . . ?
C21 C17 C20 110.2(3) . . ?
N2 C17 C18 107.7(3) . . ?
C21 C17 C18 111.2(3) . . ?
C20 C17 C18 107.4(3) . . ?
C19 C18 C17 118.0(3) . . ?
C19 C18 H18A 107.8 . . ?
C17 C18 H18A 107.8 . . ?
C19 C18 H18B 107.8 . . ?
C17 C18 H18B 107.8 . . ?
H18A C18 H18B 107.2 . . ?
N3 C19 C18 109.9(3) . . ?
N3 C19 C22 112.7(3) . . ?
C18 C19 C22 110.2(3) . . ?
N3 C19 H19 108.0 . . ?
C18 C19 H19 108.0 . . ?
C22 C19 H19 108.0 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 N3 108.7(2) . . ?
C24 C23 H23A 110.0 . . ?
N3 C23 H23A 110.0 . . ?
C24 C23 H23B 110.0 . . ?
N3 C23 H23B 110.0 . . ?
H23A C23 H23B 108.3 . . ?
N4 C24 C23 107.3(3) . . ?
N4 C24 H24A 110.3 . . ?
C23 C24 H24A 110.3 . . ?
N4 C24 H24B 110.3 . . ?
C23 C24 H24B 110.3 . . ?
H24A C24 H24B 108.5 . . ?
N4 C25 C28 110.8(3) . . ?
N4 C25 C26 107.7(3) . . ?
C28 C25 C26 111.6(3) . . ?
N4 C25 C29 108.6(3) . . ?
C28 C25 C29 110.9(3) . . ?
C26 C25 C29 107.1(3) . . ?
C27 C26 C25 117.6(3) . . ?
C27 C26 H26A 107.9 . . ?
C25 C26 H26A 107.9 . . ?
C27 C26 H26B 107.9 . . ?
C25 C26 H26B 107.9 . . ?
H26A C26 H26B 107.2 . . ?
N1 C27 C26 109.5(3) . . ?
N1 C27 C30 110.5(3) . . ?
C26 C27 C30 109.9(3) . . ?
N1 C27 H27 108.9 . . ?
C26 C27 H27 108.9 . . ?
C30 C27 H27 108.9 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
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 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O13 H13A O5 0.82 2.55 2.993(3) 115.2 1_545
O13 H13A O7 0.82 2.12 2.937(3) 170.3 1_545
O13 H13B O10 0.88 2.26 3.077(3) 155.8 1_545
N1 H1 O13 0.84 2.07 2.905(4) 169.8 .
N2 H2 O6 0.93 2.15 3.070(3) 170.4 .
N3 H3 O3 0.86 2.31 3.080(4) 148.7 .
N4 H4 O11 0.93 2.12 3.045(4) 171.9 1_545
C15 H15A O6 0.99 2.51 3.283(3) 134.5 2_665
C15 H15B O4 0.99 2.46 3.068(4) 119.2 .
C19 H19 O12 1.00 2.55 3.465(4) 151.5 1_545
C20 H20C O6 0.98 2.48 3.315(5) 143.5 .
C21 H21B O12 0.98 2.45 3.398(4) 161.8 1_545
C22 H22C O1 0.98 2.34 3.236(4) 151.9 .
C24 H24B O11 0.99 2.43 3.242(4) 139.2 2_776
C28 H28A O4 0.98 2.41 3.312(4) 152.9 .
C29 H29C O11 0.98 2.56 3.333(5) 136.1 1_545

_refine_diff_density_max         2.121
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.149

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_8
_database_code_depnum_ccdc_archive 'CCDC 1893021'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2019-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C176 H183 O58 P5 S8 U2'
_chemical_formula_weight         4113.60

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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   16.8351(4)
_cell_length_b                   23.7794(12)
_cell_length_c                   23.8357(11)
_cell_angle_alpha                70.701(2)
_cell_angle_beta                 79.095(3)
_cell_angle_gamma                89.039(3)
_cell_volume                     8832.5(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    447630
_cell_measurement_theta_min      2.08
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_F_000             4180
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    2.059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'1 φ and 15 ω scans with 2° steps (792 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            447630
_diffrn_reflns_av_unetI/netI     0.0892
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.082
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             33494
_reflns_number_gt                23423
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms bound to O atoms were found on a 
 difference Fourier map, except for those of four lattice water molecules,
 and the C-bound H atoms were introduced at calculated positions; all
 were treated as riding atoms with an isotropic displacement parameter
 equal to 1.2 times that of the parent atom. Other water solvent molecules
 are present, which could not be modelled properly; their contribution to
 the structure factors was taken into account with the PLATON/SQUEEZE
 software (.fab file).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0360P)²+17.5005P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         33494
_refine_ls_number_parameters     2242
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1160
_refine_ls_wR_factor_gt          0.1078
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_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_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 0.60011(2) 0.02881(2) 0.21385(2) 0.02929(7) Uani 1 1 d . . . . .
U2 U 0.89272(2) 0.47013(2) 0.79897(2) 0.02991(7) Uani 1 1 d . . . . .
S1 S 0.63623(9) 0.18456(7) 0.20833(6) 0.0305(3) Uani 1 1 d . . . . .
S2 S 1.02743(8) 0.30741(6) 0.24544(6) 0.0263(3) Uani 1 1 d . . . . .
S3 S 0.77583(8) 0.53579(6) 0.24450(6) 0.0270(3) Uani 1 1 d . . . . .
S4 S 0.39547(8) 0.42484(6) 0.25731(6) 0.0274(3) Uani 1 1 d . . . . .
S5 S 0.86476(11) 0.31165(8) 0.80805(8) 0.0442(4) Uani 1 1 d . . . . .
S6 S 1.08908(12) 0.06791(8) 0.79356(7) 0.0542(5) Uani 1 1 d . . . . .
S7 S 0.71271(9) -0.05283(7) 0.76236(6) 0.0312(3) Uani 1 1 d . . . . .
S8 S 0.49789(8) 0.18828(6) 0.75185(6) 0.0285(3) Uani 1 1 d . . . . .
P1 P 0.71792(9) 0.45486(7) 0.07768(7) 0.0298(3) Uani 1 1 d . . . . .
P2 P 0.69404(8) 0.10574(6) 0.94295(6) 0.0254(3) Uani 1 1 d . . . . .
P3 P 0.24787(9) 0.06033(6) 0.51330(6) 0.0264(3) Uani 1 1 d . . . . .
P4 P 0.24920(9) 0.42647(6) 0.50846(6) 0.0266(3) Uani 1 1 d . . . . .
P5 P 0.15055(9) 0.21219(6) 1.01991(7) 0.0287(3) Uani 1 1 d . . . . .
O1 O 0.5590(3) -0.0012(2) 0.29112(18) 0.0554(13) Uani 1 1 d . . . . .
O2 O 0.6398(2) 0.05687(16) 0.13629(15) 0.0279(9) Uani 1 1 d . . . . .
O3 O 0.6391(2) 0.11923(18) 0.22150(19) 0.0399(10) Uani 1 1 d . . . . .
O4 O 0.7105(2) 0.21500(19) 0.16913(17) 0.0387(10) Uani 1 1 d . . . . .
O5 O 0.5621(2) 0.20561(17) 0.18670(16) 0.0332(9) Uani 1 1 d . . . . .
O6 O 0.9991(2) 0.35663(16) 0.19932(15) 0.0272(9) Uani 1 1 d . . . . .
O7 O 1.0401(2) 0.25471(16) 0.22829(17) 0.0340(10) Uani 1 1 d . . . . .
O8 O 1.0985(2) 0.32728(16) 0.26344(16) 0.0299(9) Uani 1 1 d . . . . .
O9 O 0.8538(2) 0.52087(18) 0.21653(17) 0.0417(11) Uani 1 1 d . . . . .
O10 O 0.7149(2) 0.53529(18) 0.20857(17) 0.0380(10) Uani 1 1 d . . . . .
O11 O 0.7800(3) 0.59134(18) 0.25690(19) 0.0505(12) Uani 1 1 d . . . . .
O12 O 0.3859(2) 0.38340(17) 0.22528(17) 0.0355(10) Uani 1 1 d . . . . .
O13 O 0.4522(2) 0.47408(18) 0.22153(18) 0.0437(11) Uani 1 1 d . . . . .
O14 O 0.3177(2) 0.44399(18) 0.28132(17) 0.0395(10) Uani 1 1 d . . . . .
O15 O 0.6231(2) 0.20317(16) 0.44952(15) 0.0274(9) Uani 1 1 d . . . . .
H15 H 0.6658 0.2130 0.4545 0.033 Uiso 1 1 d R U . . .
O16 O 0.7528(2) 0.25211(15) 0.45255(15) 0.0248(8) Uani 1 1 d . . . . .
O17 O 0.6802(2) 0.35182(16) 0.48580(15) 0.0282(9) Uani 1 1 d . . . . .
H17 H 0.6257 0.3334 0.4924 0.034 Uiso 1 1 d R U . . .
O18 O 0.5452(2) 0.29512(15) 0.46565(15) 0.0263(8) Uani 1 1 d . . . . .
H18 H 0.5435 0.2508 0.4820 0.032 Uiso 1 1 d R U . . .
O19 O 0.4912(2) 0.09809(17) 0.19727(18) 0.0358(10) Uani 1 1 d . . . . .
H19A H 0.5024 0.1347 0.1941 0.043 Uiso 1 1 d R U . . .
H19B H 0.4380 0.1047 0.2123 0.043 Uiso 1 1 d R U . . .
O20 O 0.4856(2) -0.01869(18) 0.1950(2) 0.0481(12) Uani 1 1 d . . . . .
H20A H 0.4325 -0.0040 0.1914 0.058 Uiso 1 1 d R U . . .
H20B H 0.4688 -0.0506 0.1948 0.058 Uiso 1 1 d R U . . .
O21 O 0.6422(3) -0.06653(17) 0.21335(19) 0.0480(12) Uani 1 1 d . . . . .
H21A H 0.6231 -0.1023 0.2358 0.058 Uiso 1 1 d R U . . .
H21B H 0.6734 -0.0796 0.1846 0.058 Uiso 1 1 d R U . . .
O22 O 0.7343(3) 0.02231(19) 0.23582(18) 0.0476(12) Uani 1 1 d . . . . .
H22A H 0.7606 -0.0012 0.2230 0.057 Uiso 1 1 d R U . . .
H22B H 0.7628 0.0547 0.2094 0.057 Uiso 1 1 d R U . . .
O23 O 0.9194(3) 0.5005(2) 0.72033(18) 0.0557(13) Uani 1 1 d . . . . .
O24 O 0.8668(2) 0.44104(16) 0.87795(16) 0.0277(9) Uani 1 1 d . . . . .
O25 O 0.8592(2) 0.37646(19) 0.7967(2) 0.0433(11) Uani 1 1 d . . . . .
O26 O 0.9361(3) 0.2906(3) 0.8328(2) 0.087(2) Uani 1 1 d . . . . .
O27 O 0.7891(3) 0.28074(19) 0.84324(18) 0.0499(12) Uani 1 1 d . . . . .
O28 O 1.0567(5) 0.0068(2) 0.8125(2) 0.115(3) Uani 1 1 d . . . . .
O29 O 1.1749(3) 0.0712(3) 0.7808(2) 0.109(3) Uani 1 1 d . . . . .
O30 O 1.0553(3) 0.09775(18) 0.83561(18) 0.0430(11) Uani 1 1 d . . . . .
O31 O 0.6639(2) -0.02415(18) 0.80139(16) 0.0364(10) Uani 1 1 d . . . . .
O32 O 0.7774(2) -0.08602(19) 0.78833(18) 0.0455(11) Uani 1 1 d . . . . .
O33 O 0.6603(2) -0.08862(16) 0.74268(17) 0.0339(9) Uani 1 1 d . . . . .
O34 O 0.4881(2) 0.23933(17) 0.77310(17) 0.0357(10) Uani 1 1 d . . . . .
O35 O 0.4277(2) 0.17536(17) 0.72931(17) 0.0337(9) Uani 1 1 d . . . . .
O36 O 0.5199(2) 0.13467(16) 0.79733(16) 0.0296(9) Uani 1 1 d . . . . .
O37 O 0.9104(2) 0.29387(19) 0.56389(16) 0.0400(10) Uani 1 1 d . . . . .
H37 H 0.8690 0.2948 0.5512 0.048 Uiso 1 1 d R U . . .
O38 O 0.9886(3) 0.19327(18) 0.56156(17) 0.0416(11) Uani 1 1 d . . . . .
H38 H 0.9709 0.1798 0.5400 0.050 Uiso 1 1 d R U . . .
O39 O 0.8589(3) 0.13988(19) 0.5380(2) 0.0564(14) Uani 1 1 d . . . . .
H39 H 0.8426 0.1722 0.5457 0.068 Uiso 1 1 d R U . . .
O40 O 0.7833(2) 0.24250(16) 0.55293(16) 0.0282(9) Uani 1 1 d . . . . .
H40 H 0.7636 0.2433 0.5194 0.034 Uiso 1 1 d R U . . .
O41 O 0.7539(2) 0.46834(17) 0.79092(16) 0.0325(9) Uani 1 1 d . . . . .
H41A H 0.7239 0.4971 0.7726 0.039 Uiso 1 1 d R U . . .
H41B H 0.7181 0.4395 0.7906 0.039 Uiso 1 1 d R U . . .
O42 O 0.8423(2) 0.56267(17) 0.80591(18) 0.0392(10) Uani 1 1 d . . . . .
H42A H 0.8608 0.5917 0.7821 0.047 Uiso 1 1 d R U . . .
H42B H 0.8017 0.5631 0.8282 0.047 Uiso 1 1 d R U . . .
O43 O 1.0061(2) 0.53061(17) 0.8045(2) 0.0442(11) Uani 1 1 d . . . . .
H43A H 1.0090 0.5648 0.8045 0.053 Uiso 1 1 d R U . . .
H43B H 1.0569 0.5228 0.7981 0.053 Uiso 1 1 d R U . . .
O44 O 1.0135(2) 0.41159(18) 0.80295(19) 0.0414(11) Uani 1 1 d . . . . .
H44A H 1.0625 0.4368 0.7839 0.050 Uiso 1 1 d R U . . .
H44B H 1.0062 0.3732 0.8091 0.050 Uiso 1 1 d R U . . .
O45 O 0.8208(2) 0.1241(2) 0.20646(18) 0.0440(11) Uani 1 1 d . . . . .
H45A H 0.7971 0.1547 0.1752 0.053 Uiso 1 1 d R U . . .
H45B H 0.8680 0.1502 0.1969 0.053 Uiso 1 1 d R U . . .
O46 O 0.4983(3) 0.3273(2) 0.1506(2) 0.0605(13) Uani 1 1 d . . . . .
H46A H 0.4819 0.3472 0.1772 0.073 Uiso 1 1 d R U . . .
H46B H 0.4696 0.3372 0.1203 0.073 Uiso 1 1 d R U . . .
O47 O 1.0822(2) 0.14136(18) 0.23155(18) 0.0414(10) Uani 1 1 d . . . . .
H47A H 1.0828 0.1857 0.2217 0.050 Uiso 1 1 d R U . . .
H47B H 1.1409 0.1417 0.2257 0.050 Uiso 1 1 d R U . . .
O48 O 1.2622(2) 0.28708(17) 0.27586(17) 0.0360(10) Uani 1 1 d . . . . .
H48A H 1.2068 0.3014 0.2752 0.043 Uiso 1 1 d R U . . .
H48B H 1.2853 0.3278 0.2610 0.043 Uiso 1 1 d R U . . .
O49 O 0.5510(2) 0.55698(17) 0.24053(17) 0.0369(10) Uani 1 1 d . . . . .
H49A H 0.6064 0.5494 0.2249 0.044 Uiso 1 1 d R U . . .
H49B H 0.5221 0.5336 0.2249 0.044 Uiso 1 1 d R U . . .
O50 O 0.3002(2) 0.42913(18) 0.12908(17) 0.0400(10) Uani 1 1 d . . . . .
H50A H 0.3226 0.4138 0.1583 0.048 Uiso 1 1 d R U . . .
H50B H 0.3220 0.4036 0.1061 0.048 Uiso 1 1 d R U . . .
O51 O 0.6695(2) 0.36652(18) 0.82042(19) 0.0442(11) Uani 1 1 d . . . . .
H51A H 0.7024 0.3409 0.8173 0.053 Uiso 1 1 d R U . . .
H51B H 0.6236 0.3677 0.8060 0.053 Uiso 1 1 d R U . . .
O52 O 1.0642(3) 0.2116(2) 0.8513(2) 0.0547(13) Uani 1 1 d . . . . .
H52A H 1.0230 0.2331 0.8491 0.066 Uiso 1 1 d R U . . .
H52B H 1.0630 0.1810 0.8352 0.066 Uiso 1 1 d R U . . .
O53 O 1.0232(2) -0.10870(19) 0.82696(18) 0.0432(11) Uani 1 1 d . . . . .
H53A H 1.0373 -0.0701 0.8206 0.052 Uiso 1 1 d R U . . .
H53B H 0.9923 -0.1074 0.8043 0.052 Uiso 1 1 d R U . . .
O54 O 0.6396(2) -0.18769(17) 0.69575(17) 0.0374(10) Uani 1 1 d . . . . .
H54A H 0.6404 -0.1662 0.7208 0.045 Uiso 1 1 d R U . . .
H54B H 0.6752 -0.2177 0.6977 0.045 Uiso 1 1 d R U . . .
O55 O 0.7544(4) -0.1053(3) 0.1472(3) 0.116(2) Uani 1 1 d . . . . .
O56 O 0.2644(5) 0.2087(3) 0.7448(3) 0.116(2) Uani 1 1 d . . . . .
O57 O 0.5367(3) 0.34515(18) 0.7820(2) 0.0483(12) Uani 1 1 d . . . . .
O58 O 0.4085(4) 0.3746(3) 0.0632(2) 0.0851(18) Uani 1 1 d . . . . .
C1 C 0.6308(3) 0.1923(2) 0.2796(2) 0.0217(12) Uani 1 1 d . . . . .
C2 C 0.7001(3) 0.1820(2) 0.3045(2) 0.0237(12) Uani 1 1 d . . . . .
H2 H 0.7486 0.1737 0.2816 0.028 Uiso 1 1 calc R U . . .
C3 C 0.6995(3) 0.1838(2) 0.3619(2) 0.0213(12) Uani 1 1 d . . . . .
C4 C 0.6275(3) 0.1986(2) 0.3935(2) 0.0236(12) Uani 1 1 d . . . . .
C5 C 0.5569(3) 0.2070(2) 0.3692(2) 0.0236(12) Uani 1 1 d . . . . .
C6 C 0.5588(3) 0.2041(2) 0.3119(2) 0.0257(12) Uani 1 1 d . . . . .
H6 H 0.5114 0.2100 0.2949 0.031 Uiso 1 1 calc R U . . .
C7 C 0.7760(3) 0.1706(2) 0.3887(2) 0.0234(12) Uani 1 1 d . . . . .
H7A H 0.7602 0.1538 0.4333 0.028 Uiso 1 1 calc R U . . .
H7B H 0.8054 0.1399 0.3744 0.028 Uiso 1 1 calc R U . . .
C8 C 0.8325(3) 0.2248(2) 0.3720(2) 0.0237(12) Uani 1 1 d . . . . .
C9 C 0.8979(3) 0.2376(2) 0.3245(2) 0.0239(12) Uani 1 1 d . . . . .
H9 H 0.9081 0.2119 0.3010 0.029 Uiso 1 1 calc R U . . .
C10 C 0.9496(3) 0.2879(2) 0.3104(2) 0.0231(12) Uani 1 1 d . . . . .
C11 C 0.9346(3) 0.3260(2) 0.3447(2) 0.0245(12) Uani 1 1 d . . . . .
H11 H 0.9701 0.3598 0.3356 0.029 Uiso 1 1 calc R U . . .
C12 C 0.8679(3) 0.3147(2) 0.3922(2) 0.0235(12) Uani 1 1 d . . . . .
C13 C 0.8178(3) 0.2638(2) 0.4064(2) 0.0218(12) Uani 1 1 d . . . . .
C14 C 0.8460(3) 0.3594(2) 0.4250(2) 0.0245(12) Uani 1 1 d . . . . .
H14A H 0.8255 0.3378 0.4686 0.029 Uiso 1 1 calc R U . . .
H14B H 0.8952 0.3837 0.4213 0.029 Uiso 1 1 calc R U . . .
C15 C 0.7822(3) 0.4002(2) 0.3991(2) 0.0247(12) Uani 1 1 d . . . . .
C16 C 0.8037(3) 0.4438(2) 0.3431(2) 0.0272(13) Uani 1 1 d . . . . .
H16 H 0.8590 0.4498 0.3234 0.033 Uiso 1 1 calc R U . . .
C17 C 0.7471(3) 0.4790(2) 0.3148(2) 0.0240(12) Uani 1 1 d . . . . .
C18 C 0.6664(3) 0.4709(2) 0.3432(2) 0.0236(12) Uani 1 1 d . . . . .
H18A H 0.6273 0.4945 0.3234 0.028 Uiso 1 1 calc R U . . .
C19 C 0.6418(3) 0.4282(2) 0.4009(2) 0.0230(12) Uani 1 1 d . . . . .
C20 C 0.7007(3) 0.3926(2) 0.4287(2) 0.0244(12) Uani 1 1 d . . . . .
C21 C 0.5520(3) 0.4194(2) 0.4295(2) 0.0246(12) Uani 1 1 d . . . . .
H21C H 0.5454 0.3970 0.4734 0.030 Uiso 1 1 calc R U . . .
H21D H 0.5285 0.4588 0.4248 0.030 Uiso 1 1 calc R U . . .
C22 C 0.5075(3) 0.3855(2) 0.4000(2) 0.0237(12) Uani 1 1 d . . . . .
C23 C 0.4712(3) 0.4149(2) 0.3514(2) 0.0274(13) Uani 1 1 d . . . . .
H23 H 0.4698 0.4572 0.3388 0.033 Uiso 1 1 calc R U . . .
C24 C 0.4368(3) 0.3842(2) 0.3207(2) 0.0229(12) Uani 1 1 d . . . . .
C25 C 0.4388(3) 0.3226(2) 0.3389(2) 0.0277(13) Uani 1 1 d . . . . .
H25 H 0.4158 0.3018 0.3175 0.033 Uiso 1 1 calc R U . . .
C26 C 0.4737(3) 0.2904(2) 0.3877(2) 0.0251(12) Uani 1 1 d . . . . .
C27 C 0.5084(3) 0.3224(2) 0.4177(2) 0.0231(12) Uani 1 1 d . . . . .
C28 C 0.4787(3) 0.2237(2) 0.4030(2) 0.0249(12) Uani 1 1 d . . . . .
H28A H 0.4318 0.2078 0.3924 0.030 Uiso 1 1 calc R U . . .
H28B H 0.4757 0.2051 0.4472 0.030 Uiso 1 1 calc R U . . .
C29 C 0.8788(3) 0.3054(2) 0.7357(2) 0.0298(13) Uani 1 1 d . . . . .
C30 C 0.9530(3) 0.2915(2) 0.7085(3) 0.0298(13) Uani 1 1 d . . . . .
H30 H 0.9969 0.2852 0.7293 0.036 Uiso 1 1 calc R U . . .
C31 C 0.9640(3) 0.2868(2) 0.6510(2) 0.0253(12) Uani 1 1 d . . . . .
C32 C 0.8981(3) 0.2979(2) 0.6213(2) 0.0271(13) Uani 1 1 d . . . . .
C33 C 0.8242(3) 0.3137(2) 0.6473(2) 0.0254(12) Uani 1 1 d . . . . .
C34 C 0.8147(4) 0.3164(2) 0.7049(2) 0.0298(13) Uani 1 1 d . . . . .
H34 H 0.7639 0.3259 0.7239 0.036 Uiso 1 1 calc R U . . .
C35 C 1.0426(3) 0.2650(2) 0.6242(3) 0.0315(13) Uani 1 1 d . . . . .
H35A H 1.0502 0.2801 0.5794 0.038 Uiso 1 1 calc R U . . .
H35B H 1.0886 0.2811 0.6356 0.038 Uiso 1 1 calc R U . . .
C36 C 1.0423(3) 0.1975(3) 0.6463(3) 0.0325(14) Uani 1 1 d . . . . .
C37 C 1.0668(3) 0.1672(3) 0.7003(2) 0.0345(14) Uani 1 1 d . . . . .
H37A H 1.0886 0.1890 0.7213 0.041 Uiso 1 1 calc R U . . .
C38 C 1.0597(4) 0.1054(3) 0.7237(3) 0.0369(15) Uani 1 1 d . . . . .
C39 C 1.0282(3) 0.0736(3) 0.6931(3) 0.0401(16) Uani 1 1 d . . . . .
H39A H 1.0227 0.0313 0.7100 0.048 Uiso 1 1 calc R U . . .
C40 C 1.0042(3) 0.1018(2) 0.6383(3) 0.0334(14) Uani 1 1 d . . . . .
C41 C 1.0112(3) 0.1639(3) 0.6156(2) 0.0312(14) Uani 1 1 d . . . . .
C42 C 0.9690(3) 0.0658(3) 0.6064(3) 0.0376(15) Uani 1 1 d . . . . .
H42C H 0.9930 0.0262 0.6160 0.045 Uiso 1 1 calc R U . . .
H42D H 0.9842 0.0862 0.5621 0.045 Uiso 1 1 calc R U . . .
C43 C 0.8769(3) 0.0571(2) 0.6246(2) 0.0285(13) Uani 1 1 d . . . . .
C44 C 0.8422(3) 0.0115(2) 0.6775(2) 0.0283(13) Uani 1 1 d . . . . .
H44 H 0.8759 -0.0146 0.7010 0.034 Uiso 1 1 calc R U . . .
C45 C 0.7586(3) 0.0042(2) 0.6958(2) 0.0246(12) Uani 1 1 d . . . . .
C46 C 0.7081(3) 0.0430(2) 0.6621(2) 0.0267(13) Uani 1 1 d . . . . .
H46 H 0.6510 0.0375 0.6747 0.032 Uiso 1 1 calc R U . . .
C47 C 0.7419(3) 0.0895(2) 0.6102(2) 0.0280(13) Uani 1 1 d . . . . .
C48 C 0.8264(4) 0.0963(3) 0.5912(3) 0.0364(15) Uani 1 1 d . . . . .
C49 C 0.6866(3) 0.1349(2) 0.5781(2) 0.0264(12) Uani 1 1 d . . . . .
H49C H 0.7140 0.1554 0.5356 0.032 Uiso 1 1 calc R U . . .
H49D H 0.6365 0.1141 0.5774 0.032 Uiso 1 1 calc R U . . .
C50 C 0.6646(3) 0.1808(2) 0.6091(2) 0.0262(12) Uani 1 1 d . . . . .
C51 C 0.5966(3) 0.1697(2) 0.6553(2) 0.0266(12) Uani 1 1 d . . . . .
H51 H 0.5613 0.1359 0.6636 0.032 Uiso 1 1 calc R U . . .
C52 C 0.5794(3) 0.2078(2) 0.6898(2) 0.0253(12) Uani 1 1 d . . . . .
C53 C 0.6296(3) 0.2582(2) 0.6761(2) 0.0252(12) Uani 1 1 d . . . . .
H53 H 0.6172 0.2844 0.6988 0.030 Uiso 1 1 calc R U . . .
C54 C 0.6977(3) 0.2712(2) 0.6297(2) 0.0249(12) Uani 1 1 d . . . . .
C55 C 0.7152(3) 0.2314(2) 0.5965(2) 0.0241(12) Uani 1 1 d . . . . .
C56 C 0.7524(3) 0.3259(2) 0.6152(2) 0.0249(12) Uani 1 1 d . . . . .
H56A H 0.7203 0.3569 0.6269 0.030 Uiso 1 1 calc R U . . .
H56B H 0.7729 0.3417 0.5709 0.030 Uiso 1 1 calc R U . . .
C57 C 0.6373(4) 0.5057(3) 0.0740(3) 0.0385(15) Uani 1 1 d . . . . .
C58 C 0.6482(4) 0.5615(3) 0.0797(3) 0.057(2) Uani 1 1 d . . . . .
H58 H 0.7009 0.5749 0.0799 0.068 Uiso 1 1 calc R U . . .
C59 C 0.5839(4) 0.5979(3) 0.0849(3) 0.0563(19) Uani 1 1 d . . . . .
H59 H 0.5924 0.6355 0.0892 0.068 Uiso 1 1 calc R U . . .
C60 C 0.5065(4) 0.5787(4) 0.0837(3) 0.060(2) Uani 1 1 d . . . . .
H60 H 0.4617 0.6030 0.0873 0.072 Uiso 1 1 calc R U . . .
C61 C 0.4961(4) 0.5236(3) 0.0771(3) 0.0512(18) Uani 1 1 d . . . . .
H61 H 0.4441 0.5112 0.0742 0.061 Uiso 1 1 calc R U . . .
C62 C 0.5594(4) 0.4866(3) 0.0747(3) 0.0384(15) Uani 1 1 d . . . . .
H62 H 0.5499 0.4478 0.0735 0.046 Uiso 1 1 calc R U . . .
C63 C 0.7183(3) 0.4140(2) 0.1554(2) 0.0257(12) Uani 1 1 d . . . . .
C64 C 0.6498(3) 0.4077(2) 0.1997(2) 0.0288(13) Uani 1 1 d . . . . .
H64 H 0.6022 0.4271 0.1893 0.035 Uiso 1 1 calc R U . . .
C65 C 0.6504(3) 0.3731(3) 0.2591(3) 0.0316(13) Uani 1 1 d . . . . .
H65 H 0.6028 0.3678 0.2894 0.038 Uiso 1 1 calc R U . . .
C66 C 0.7199(4) 0.3464(3) 0.2742(3) 0.0327(14) Uani 1 1 d . . . . .
H66 H 0.7200 0.3230 0.3151 0.039 Uiso 1 1 calc R U . . .
C67 C 0.7890(4) 0.3529(3) 0.2313(3) 0.0347(14) Uani 1 1 d . . . . .
H67 H 0.8368 0.3347 0.2426 0.042 Uiso 1 1 calc R U . . .
C68 C 0.7888(3) 0.3863(2) 0.1714(3) 0.0329(14) Uani 1 1 d . . . . .
H68 H 0.8362 0.3904 0.1413 0.040 Uiso 1 1 calc R U . . .
C69 C 0.8120(3) 0.4974(2) 0.0437(2) 0.0308(13) Uani 1 1 d . . . . .
C70 C 0.8481(4) 0.5229(3) 0.0783(3) 0.0361(15) Uani 1 1 d . . . . .
H70 H 0.8253 0.5148 0.1200 0.043 Uiso 1 1 calc R U . . .
C71 C 0.9172(4) 0.5598(3) 0.0519(3) 0.0433(16) Uani 1 1 d . . . . .
H71 H 0.9420 0.5768 0.0756 0.052 Uiso 1 1 calc R U . . .
C72 C 0.9500(4) 0.5720(3) -0.0086(3) 0.057(2) Uani 1 1 d . . . . .
H72 H 0.9965 0.5984 -0.0268 0.068 Uiso 1 1 calc R U . . .
C73 C 0.9154(4) 0.5459(3) -0.0437(3) 0.060(2) Uani 1 1 d . . . . .
H73 H 0.9388 0.5534 -0.0852 0.072 Uiso 1 1 calc R U . . .
C74 C 0.8466(4) 0.5090(3) -0.0166(3) 0.0434(17) Uani 1 1 d . . . . .
H74 H 0.8224 0.4913 -0.0400 0.052 Uiso 1 1 calc R U . . .
C75 C 0.7017(3) 0.4040(2) 0.0393(2) 0.0298(13) Uani 1 1 d . . . . .
C76 C 0.6924(4) 0.4264(3) -0.0209(3) 0.0395(15) Uani 1 1 d . . . . .
H76 H 0.6912 0.4682 -0.0406 0.047 Uiso 1 1 calc R U . . .
C77 C 0.6849(4) 0.3872(3) -0.0518(3) 0.0392(16) Uani 1 1 d . . . . .
H77 H 0.6796 0.4022 -0.0931 0.047 Uiso 1 1 calc R U . . .
C78 C 0.6849(4) 0.3266(3) -0.0229(3) 0.0399(16) Uani 1 1 d . . . . .
H78 H 0.6800 0.3001 -0.0445 0.048 Uiso 1 1 calc R U . . .
C79 C 0.6921(3) 0.3040(3) 0.0371(3) 0.0375(15) Uani 1 1 d . . . . .
H79 H 0.6908 0.2621 0.0568 0.045 Uiso 1 1 calc R U . . .
C80 C 0.7012(3) 0.3423(3) 0.0685(3) 0.0311(13) Uani 1 1 d . . . . .
H80 H 0.7070 0.3268 0.1096 0.037 Uiso 1 1 calc R U . . .
C81 C 0.6224(3) 0.1600(2) 0.9546(2) 0.0267(13) Uani 1 1 d . . . . .
C82 C 0.5866(3) 0.1974(2) 0.9085(3) 0.0318(14) Uani 1 1 d . . . . .
H82 H 0.6024 0.1967 0.8683 0.038 Uiso 1 1 calc R U . . .
C83 C 0.5285(3) 0.2354(3) 0.9210(3) 0.0335(14) Uani 1 1 d . . . . .
H83 H 0.5040 0.2603 0.8894 0.040 Uiso 1 1 calc R U . . .
C84 C 0.5054(4) 0.2375(3) 0.9793(3) 0.0365(15) Uani 1 1 d . . . . .
H84 H 0.4653 0.2637 0.9876 0.044 Uiso 1 1 calc R U . . .
C85 C 0.5413(3) 0.2009(3) 1.0254(3) 0.0342(14) Uani 1 1 d . . . . .
H85 H 0.5260 0.2024 1.0653 0.041 Uiso 1 1 calc R U . . .
C86 C 0.5996(3) 0.1622(2) 1.0133(3) 0.0305(13) Uani 1 1 d . . . . .
H86 H 0.6239 0.1372 1.0450 0.037 Uiso 1 1 calc R U . . .
C87 C 0.7454(3) 0.1248(2) 0.8655(2) 0.0254(12) Uani 1 1 d . . . . .
C88 C 0.7024(3) 0.1263(2) 0.8204(2) 0.0311(13) Uani 1 1 d . . . . .
H88 H 0.6453 0.1193 0.8303 0.037 Uiso 1 1 calc R U . . .
C89 C 0.7432(4) 0.1381(2) 0.7610(3) 0.0344(14) Uani 1 1 d . . . . .
H89 H 0.7140 0.1394 0.7302 0.041 Uiso 1 1 calc R U . . .
C90 C 0.8260(4) 0.1477(2) 0.7471(3) 0.0381(16) Uani 1 1 d . . . . .
H90 H 0.8541 0.1551 0.7067 0.046 Uiso 1 1 calc R U . . .
C91 C 0.8687(4) 0.1468(2) 0.7914(3) 0.0339(14) Uani 1 1 d . . . . .
H91 H 0.9257 0.1547 0.7810 0.041 Uiso 1 1 calc R U . . .
C92 C 0.8291(3) 0.1346(2) 0.8507(3) 0.0307(13) Uani 1 1 d . . . . .
H92 H 0.8589 0.1328 0.8813 0.037 Uiso 1 1 calc R U . . .
C93 C 0.7662(3) 0.1035(2) 0.9895(2) 0.0257(12) Uani 1 1 d . . . . .
C94 C 0.8024(4) 0.1577(3) 0.9862(3) 0.0411(16) Uani 1 1 d . . . . .
H94 H 0.7881 0.1945 0.9600 0.049 Uiso 1 1 calc R U . . .
C95 C 0.8587(4) 0.1569(3) 1.0215(3) 0.0502(18) Uani 1 1 d . . . . .
H95 H 0.8832 0.1934 1.0195 0.060 Uiso 1 1 calc R U . . .
C96 C 0.8801(4) 0.1041(3) 1.0594(3) 0.0439(17) Uani 1 1 d . . . . .
H96 H 0.9187 0.1043 1.0837 0.053 Uiso 1 1 calc R U . . .
C97 C 0.8458(4) 0.0504(3) 1.0625(3) 0.0401(16) Uani 1 1 d . . . . .
H97 H 0.8612 0.0139 1.0885 0.048 Uiso 1 1 calc R U . . .
C98 C 0.7883(3) 0.0501(3) 1.0271(2) 0.0329(14) Uani 1 1 d . . . . .
H98 H 0.7647 0.0134 1.0288 0.039 Uiso 1 1 calc R U . . .
C99 C 0.6448(3) 0.0326(2) 0.9669(2) 0.0266(12) Uani 1 1 d . . . . .
C100 C 0.5999(3) 0.0089(2) 1.0260(2) 0.0268(13) Uani 1 1 d . . . . .
H100 H 0.5917 0.0324 1.0518 0.032 Uiso 1 1 calc R U . . .
C101 C 0.5677(3) -0.0484(3) 1.0462(2) 0.0314(14) Uani 1 1 d . . . . .
H101 H 0.5383 -0.0650 1.0866 0.038 Uiso 1 1 calc R U . . .
C102 C 0.5775(3) -0.0826(3) 1.0084(3) 0.0311(13) Uani 1 1 d . . . . .
H102 H 0.5553 -0.1225 1.0232 0.037 Uiso 1 1 calc R U . . .
C103 C 0.6192(3) -0.0592(2) 0.9494(3) 0.0313(13) Uani 1 1 d . . . . .
H103 H 0.6241 -0.0822 0.9232 0.038 Uiso 1 1 calc R U . . .
C104 C 0.6543(3) -0.0012(2) 0.9285(2) 0.0296(13) Uani 1 1 d . . . . .
H104 H 0.6843 0.0150 0.8883 0.036 Uiso 1 1 calc R U . . .
C105 C 0.1765(3) 0.0019(2) 0.5643(2) 0.0282(13) Uani 1 1 d . . . . .
C106 C 0.1706(3) -0.0171(2) 0.6267(2) 0.0303(13) Uani 1 1 d . . . . .
H106 H 0.2079 -0.0018 0.6440 0.036 Uiso 1 1 calc R U . . .
C107 C 0.1098(3) -0.0586(2) 0.6636(3) 0.0321(14) Uani 1 1 d . . . . .
H107 H 0.1043 -0.0707 0.7064 0.039 Uiso 1 1 calc R U . . .
C108 C 0.0574(3) -0.0824(2) 0.6389(3) 0.0318(14) Uani 1 1 d . . . . .
H108 H 0.0154 -0.1103 0.6648 0.038 Uiso 1 1 calc R U . . .
C109 C 0.0649(3) -0.0663(2) 0.5766(3) 0.0321(14) Uani 1 1 d . . . . .
H109 H 0.0297 -0.0842 0.5598 0.038 Uiso 1 1 calc R U . . .
C110 C 0.1242(3) -0.0239(2) 0.5391(3) 0.0311(13) Uani 1 1 d . . . . .
H110 H 0.1296 -0.0122 0.4964 0.037 Uiso 1 1 calc R U . . .
C111 C 0.2855(3) 0.1015(2) 0.5548(2) 0.0283(13) Uani 1 1 d . . . . .
C112 C 0.2359(4) 0.1185(3) 0.5995(3) 0.0404(15) Uani 1 1 d . . . . .
H112 H 0.1791 0.1102 0.6075 0.048 Uiso 1 1 calc R U . . .
C113 C 0.2680(4) 0.1476(3) 0.6324(3) 0.0441(16) Uani 1 1 d . . . . .
H113 H 0.2333 0.1584 0.6631 0.053 Uiso 1 1 calc R U . . .
C114 C 0.3493(4) 0.1607(3) 0.6209(3) 0.0395(15) Uani 1 1 d . . . . .
H114 H 0.3708 0.1807 0.6437 0.047 Uiso 1 1 calc R U . . .
C115 C 0.4008(4) 0.1451(3) 0.5763(3) 0.0398(15) Uani 1 1 d . . . . .
H115 H 0.4571 0.1553 0.5680 0.048 Uiso 1 1 calc R U . . .
C116 C 0.3699(4) 0.1143(2) 0.5436(3) 0.0336(14) Uani 1 1 d . . . . .
H116 H 0.4053 0.1021 0.5141 0.040 Uiso 1 1 calc R U . . .
C117 C 0.3331(3) 0.0303(2) 0.4776(2) 0.0251(12) Uani 1 1 d . . . . .
C118 C 0.3559(3) -0.0276(2) 0.5072(2) 0.0291(13) Uani 1 1 d . . . . .
H118 H 0.3237 -0.0519 0.5444 0.035 Uiso 1 1 calc R U . . .
C119 C 0.4253(3) -0.0487(3) 0.4818(2) 0.0280(13) Uani 1 1 d . . . . .
H119 H 0.4417 -0.0874 0.5020 0.034 Uiso 1 1 calc R U . . .
C120 C 0.4714(3) -0.0139(3) 0.4271(2) 0.0304(13) Uani 1 1 d . . . . .
H120 H 0.5183 -0.0293 0.4094 0.036 Uiso 1 1 calc R U . . .
C121 C 0.4497(3) 0.0432(3) 0.3979(3) 0.0322(14) Uani 1 1 d . . . . .
H121 H 0.4824 0.0670 0.3607 0.039 Uiso 1 1 calc R U . . .
C122 C 0.3807(3) 0.0657(2) 0.4226(2) 0.0289(13) Uani 1 1 d . . . . .
H122 H 0.3657 0.1048 0.4024 0.035 Uiso 1 1 calc R U . . .
C123 C 0.1957(3) 0.1062(2) 0.4569(2) 0.0281(13) Uani 1 1 d . . . . .
C124 C 0.1440(4) 0.1478(3) 0.4705(3) 0.0378(15) Uani 1 1 d . . . . .
H124 H 0.1403 0.1544 0.5081 0.045 Uiso 1 1 calc R U . . .
C125 C 0.0981(4) 0.1797(3) 0.4296(3) 0.0383(15) Uani 1 1 d . . . . .
H125 H 0.0619 0.2076 0.4396 0.046 Uiso 1 1 calc R U . . .
C126 C 0.1043(4) 0.1713(3) 0.3742(3) 0.0364(15) Uani 1 1 d . . . . .
H126 H 0.0735 0.1942 0.3457 0.044 Uiso 1 1 calc R U . . .
C127 C 0.1552(4) 0.1298(3) 0.3606(3) 0.0384(15) Uani 1 1 d . . . . .
H127 H 0.1596 0.1239 0.3226 0.046 Uiso 1 1 calc R U . . .
C128 C 0.2000(4) 0.0965(3) 0.4021(3) 0.0366(15) Uani 1 1 d . . . . .
H128 H 0.2337 0.0670 0.3930 0.044 Uiso 1 1 calc R U . . .
C129 C 0.2070(3) 0.3830(2) 0.4715(2) 0.0266(12) Uani 1 1 d . . . . .
C130 C 0.2566(4) 0.3597(3) 0.4308(3) 0.0350(14) Uani 1 1 d . . . . .
H130 H 0.3138 0.3633 0.4261 0.042 Uiso 1 1 calc R U . . .
C131 C 0.2240(4) 0.3320(3) 0.3981(3) 0.0380(15) Uani 1 1 d . . . . .
H131 H 0.2583 0.3160 0.3713 0.046 Uiso 1 1 calc R U . . .
C132 C 0.1405(4) 0.3274(3) 0.4040(3) 0.0342(14) Uani 1 1 d . . . . .
H132 H 0.1178 0.3094 0.3800 0.041 Uiso 1 1 calc R U . . .
C133 C 0.0908(3) 0.3486(2) 0.4444(3) 0.0323(14) Uani 1 1 d . . . . .
H133 H 0.0337 0.3443 0.4491 0.039 Uiso 1 1 calc R U . . .
C134 C 0.1231(3) 0.3764(2) 0.4783(2) 0.0281(13) Uani 1 1 d . . . . .
H134 H 0.0882 0.3909 0.5063 0.034 Uiso 1 1 calc R U . . .
C135 C 0.3154(3) 0.4846(2) 0.4513(2) 0.0265(12) Uani 1 1 d . . . . .
C136 C 0.3069(3) 0.5024(2) 0.3900(2) 0.0277(13) Uani 1 1 d . . . . .
H136 H 0.2664 0.4839 0.3782 0.033 Uiso 1 1 calc R U . . .
C137 C 0.3589(3) 0.5474(2) 0.3476(3) 0.0303(13) Uani 1 1 d . . . . .
H137 H 0.3541 0.5600 0.3063 0.036 Uiso 1 1 calc R U . . .
C138 C 0.4179(3) 0.5743(2) 0.3649(3) 0.0310(13) Uani 1 1 d . . . . .
H138 H 0.4538 0.6046 0.3351 0.037 Uiso 1 1 calc R U . . .
C139 C 0.4255(3) 0.5576(2) 0.4249(3) 0.0310(13) Uani 1 1 d . . . . .
H139 H 0.4656 0.5769 0.4364 0.037 Uiso 1 1 calc R U . . .
C140 C 0.3739(3) 0.5124(2) 0.4686(3) 0.0302(13) Uani 1 1 d . . . . .
H140 H 0.3787 0.5006 0.5099 0.036 Uiso 1 1 calc R U . . .
C141 C 0.3073(3) 0.3847(2) 0.5627(2) 0.0273(13) Uani 1 1 d . . . . .
C142 C 0.3575(3) 0.3407(2) 0.5507(3) 0.0315(14) Uani 1 1 d . . . . .
H142 H 0.3564 0.3300 0.5158 0.038 Uiso 1 1 calc R U . . .
C143 C 0.4087(4) 0.3127(3) 0.5896(3) 0.0372(15) Uani 1 1 d . . . . .
H143 H 0.4430 0.2832 0.5811 0.045 Uiso 1 1 calc R U . . .
C144 C 0.4100(4) 0.3277(2) 0.6408(3) 0.0355(14) Uani 1 1 d . . . . .
H144 H 0.4447 0.3083 0.6677 0.043 Uiso 1 1 calc R U . . .
C145 C 0.3610(4) 0.3708(3) 0.6526(3) 0.0354(14) Uani 1 1 d . . . . .
H145 H 0.3623 0.3809 0.6878 0.042 Uiso 1 1 calc R U . . .
C146 C 0.3095(4) 0.3998(3) 0.6142(2) 0.0338(14) Uani 1 1 d . . . . .
H146 H 0.2761 0.4297 0.6228 0.041 Uiso 1 1 calc R U . . .
C147 C 0.1658(3) 0.4584(3) 0.5442(2) 0.0291(13) Uani 1 1 d . . . . .
C148 C 0.1211(3) 0.4268(3) 0.6011(3) 0.0333(14) Uani 1 1 d . . . . .
H148 H 0.1390 0.3900 0.6246 0.040 Uiso 1 1 calc R U . . .
C149 C 0.0498(4) 0.4496(3) 0.6234(3) 0.0355(14) Uani 1 1 d . . . . .
H149 H 0.0190 0.4283 0.6623 0.043 Uiso 1 1 calc R U . . .
C150 C 0.0238(3) 0.5031(3) 0.5889(3) 0.0359(15) Uani 1 1 d . . . . .
H150 H -0.0251 0.5183 0.6040 0.043 Uiso 1 1 calc R U . . .
C151 C 0.0688(3) 0.5344(3) 0.5324(3) 0.0299(13) Uani 1 1 d . . . . .
H151 H 0.0510 0.5713 0.5090 0.036 Uiso 1 1 calc R U . . .
C152 C 0.1394(3) 0.5125(3) 0.5096(2) 0.0290(13) Uani 1 1 d . . . . .
H152 H 0.1699 0.5341 0.4706 0.035 Uiso 1 1 calc R U . . .
C153 C 0.1286(3) 0.1339(2) 1.0397(3) 0.0306(13) Uani 1 1 d . . . . .
C154 C 0.0901(4) 0.1167(3) 1.0001(3) 0.0439(16) Uani 1 1 d . . . . .
H154 H 0.0763 0.1458 0.9655 0.053 Uiso 1 1 calc R U . . .
C155 C 0.0726(4) 0.0573(3) 1.0119(4) 0.056(2) Uani 1 1 d . . . . .
H155 H 0.0492 0.0449 0.9843 0.067 Uiso 1 1 calc R U . . .
C156 C 0.0892(4) 0.0151(3) 1.0643(4) 0.055(2) Uani 1 1 d . . . . .
H156 H 0.0737 -0.0257 1.0737 0.066 Uiso 1 1 calc R U . . .
C157 C 0.1278(4) 0.0320(3) 1.1029(3) 0.0462(18) Uani 1 1 d . . . . .
H157 H 0.1409 0.0028 1.1377 0.055 Uiso 1 1 calc R U . . .
C158 C 0.1473(4) 0.0917(3) 1.0905(3) 0.0398(15) Uani 1 1 d . . . . .
H158 H 0.1735 0.1037 1.1170 0.048 Uiso 1 1 calc R U . . .
C159 C 0.2153(3) 0.2376(3) 0.9466(2) 0.0313(14) Uani 1 1 d . . . . .
C160 C 0.2547(5) 0.1994(3) 0.9220(3) 0.068(2) Uani 1 1 d . . . . .
H160 H 0.2438 0.1577 0.9413 0.081 Uiso 1 1 calc R U . . .
C161 C 0.3111(6) 0.2205(4) 0.8686(4) 0.108(4) Uani 1 1 d . . . . .
H161 H 0.3400 0.1932 0.8520 0.129 Uiso 1 1 calc R U . . .
C162 C 0.3257(5) 0.2805(4) 0.8397(4) 0.078(3) Uani 1 1 d . . . . .
H162 H 0.3638 0.2948 0.8026 0.094 Uiso 1 1 calc R U . . .
C163 C 0.2862(4) 0.3186(3) 0.8637(3) 0.0535(19) Uani 1 1 d . . . . .
H163 H 0.2950 0.3603 0.8430 0.064 Uiso 1 1 calc R U . . .
C164 C 0.2327(4) 0.2981(3) 0.9180(3) 0.0410(16) Uani 1 1 d . . . . .
H164 H 0.2075 0.3256 0.9362 0.049 Uiso 1 1 calc R U . . .
C165 C 0.2061(4) 0.2273(3) 1.0710(3) 0.0335(14) Uani 1 1 d . . . . .
C166 C 0.2802(4) 0.1997(3) 1.0761(3) 0.0444(16) Uani 1 1 d . . . . .
H166 H 0.2981 0.1742 1.0534 0.053 Uiso 1 1 calc R U . . .
C167 C 0.3267(4) 0.2094(3) 1.1138(3) 0.0487(17) Uani 1 1 d . . . . .
H167 H 0.3757 0.1896 1.1183 0.058 Uiso 1 1 calc R U . . .
C168 C 0.3020(4) 0.2482(3) 1.1451(3) 0.0487(18) Uani 1 1 d . . . . .
H168 H 0.3348 0.2554 1.1706 0.058 Uiso 1 1 calc R U . . .
C169 C 0.2299(4) 0.2765(3) 1.1398(3) 0.0487(18) Uani 1 1 d . . . . .
H169 H 0.2133 0.3029 1.1617 0.058 Uiso 1 1 calc R U . . .
C170 C 0.1819(4) 0.2664(3) 1.1023(3) 0.0389(15) Uani 1 1 d . . . . .
H170 H 0.1328 0.2862 1.0981 0.047 Uiso 1 1 calc R U . . .
C171 C 0.0571(3) 0.2503(2) 1.0197(3) 0.0294(13) Uani 1 1 d . . . . .
C172 C 0.0062(3) 0.2466(3) 1.0740(3) 0.0356(14) Uani 1 1 d . . . . .
H172 H 0.0204 0.2244 1.1116 0.043 Uiso 1 1 calc R U . . .
C173 C -0.0656(4) 0.2757(3) 1.0726(3) 0.0424(16) Uani 1 1 d . . . . .
H173 H -0.1004 0.2735 1.1097 0.051 Uiso 1 1 calc R U . . .
C174 C -0.0878(4) 0.3077(3) 1.0189(3) 0.0408(16) Uani 1 1 d . . . . .
H174 H -0.1373 0.3276 1.0190 0.049 Uiso 1 1 calc R U . . .
C175 C -0.0379(4) 0.3110(3) 0.9648(3) 0.0405(16) Uani 1 1 d . . . . .
H175 H -0.0533 0.3328 0.9276 0.049 Uiso 1 1 calc R U . . .
C176 C 0.0344(4) 0.2825(3) 0.9645(3) 0.0364(14) Uani 1 1 d . . . . .
H176 H 0.0685 0.2848 0.9271 0.044 Uiso 1 1 calc R U . . .


_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 O2 1.744(3) . ?
U1 O1 1.745(4) . ?
U1 O3 2.332(4) . ?
U1 O21 2.367(4) . ?
U1 O22 2.405(4) . ?
U1 O20 2.435(4) . ?
U1 O19 2.444(4) . ?
U2 O23 1.742(4) . ?
U2 O24 1.747(3) . ?
U2 O25 2.327(4) . ?
U2 O41 2.383(4) . ?
U2 O42 2.390(4) . ?
U2 O44 2.443(4) . ?
U2 O43 2.458(4) . ?
S1 O4 1.450(4) . ?
S1 O5 1.458(4) . ?
S1 O3 1.482(4) . ?
S1 C1 1.753(5) . ?
S2 O7 1.442(4) . ?
S2 O6 1.461(4) . ?
S2 O8 1.478(4) . ?
S2 C10 1.762(5) . ?
S3 O9 1.450(4) . ?
S3 O11 1.451(4) . ?
S3 O10 1.458(4) . ?
S3 C17 1.758(5) . ?
S4 O13 1.443(4) . ?
S4 O14 1.455(4) . ?
S4 O12 1.459(4) . ?
S4 C24 1.764(5) . ?
S5 O27 1.444(5) . ?
S5 O26 1.448(5) . ?
S5 O25 1.479(4) . ?
S5 C29 1.752(5) . ?
S6 O29 1.417(6) . ?
S6 O30 1.440(4) . ?
S6 O28 1.455(6) . ?
S6 C38 1.769(6) . ?
S7 O32 1.448(4) . ?
S7 O31 1.455(4) . ?
S7 O33 1.473(4) . ?
S7 C45 1.760(5) . ?
S8 O34 1.458(4) . ?
S8 O35 1.463(4) . ?
S8 O36 1.469(4) . ?
S8 C52 1.757(5) . ?
P1 C63 1.786(5) . ?
P1 C75 1.791(6) . ?
P1 C69 1.792(6) . ?
P1 C57 1.799(6) . ?
P2 C93 1.783(5) . ?
P2 C87 1.794(5) . ?
P2 C99 1.803(5) . ?
P2 C81 1.804(5) . ?
P3 C117 1.788(5) . ?
P3 C123 1.793(6) . ?
P3 C111 1.798(6) . ?
P3 C105 1.800(5) . ?
P4 C129 1.792(5) . ?
P4 C141 1.793(6) . ?
P4 C147 1.794(5) . ?
P4 C135 1.800(5) . ?
P5 C153 1.790(6) . ?
P5 C159 1.792(6) . ?
P5 C165 1.794(6) . ?
P5 C171 1.803(6) . ?
O15 C4 1.363(6) . ?
O15 H15 0.7999 . ?
O16 C13 1.355(6) . ?
O17 C20 1.368(6) . ?
O17 H17 0.9855 . ?
O18 C27 1.369(6) . ?
O18 H18 0.9936 . ?
O19 H19A 0.8697 . ?
O19 H19B 0.9313 . ?
O20 H20A 0.9630 . ?
O20 H20B 0.8164 . ?
O21 H21A 0.8695 . ?
O21 H21B 0.9179 . ?
O22 H22A 0.8108 . ?
O22 H22B 0.8921 . ?
O37 C32 1.380(6) . ?
O37 H37 0.8071 . ?
O38 C41 1.369(7) . ?
O38 H38 0.7924 . ?
O39 C48 1.367(7) . ?
O39 H39 0.8753 . ?
O40 C55 1.358(6) . ?
O40 H40 0.9151 . ?
O41 H41A 0.8885 . ?
O41 H41B 0.9226 . ?
O42 H42A 0.7604 . ?
O42 H42B 0.7846 . ?
O43 H43A 0.8142 . ?
O43 H43B 0.8672 . ?
O44 H44A 0.9713 . ?
O44 H44B 0.8834 . ?
O45 H45A 0.9935 . ?
O45 H45B 0.9604 . ?
O46 H46A 0.9112 . ?
O46 H46B 0.9090 . ?
O47 H47A 1.0015 . ?
O47 H47B 0.9709 . ?
O48 H48A 0.9884 . ?
O48 H48B 0.9731 . ?
O49 H49A 0.9745 . ?
O49 H49B 0.9485 . ?
O50 H50A 0.8299 . ?
O50 H50B 0.9698 . ?
O51 H51A 0.8286 . ?
O51 H51B 0.9005 . ?
O52 H52A 0.8533 . ?
O52 H52B 0.9301 . ?
O53 H53A 0.9081 . ?
O53 H53B 0.8110 . ?
O54 H54A 0.9069 . ?
O54 H54B 0.9199 . ?
C1 C6 1.385(7) . ?
C1 C2 1.388(7) . ?
C2 C3 1.382(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.406(7) . ?
C3 C7 1.525(7) . ?
C4 C5 1.403(7) . ?
C5 C6 1.386(7) . ?
C5 C28 1.527(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.511(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.379(7) . ?
C8 C13 1.418(7) . ?
C9 C10 1.400(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.399(7) . ?
C11 C12 1.395(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.394(7) . ?
C12 C14 1.519(7) . ?
C14 C15 1.514(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.380(7) . ?
C15 C20 1.404(7) . ?
C16 C17 1.380(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.383(7) . ?
C18 C19 1.402(7) . ?
C18 H18A 0.9500 . ?
C19 C20 1.411(7) . ?
C19 C21 1.523(7) . ?
C21 C22 1.516(7) . ?
C21 H21C 0.9900 . ?
C21 H21D 0.9900 . ?
C22 C23 1.387(7) . ?
C22 C27 1.420(7) . ?
C23 C24 1.391(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(7) . ?
C25 C26 1.393(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.401(7) . ?
C26 C28 1.510(7) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.382(8) . ?
C29 C34 1.391(7) . ?
C30 C31 1.388(7) . ?
C30 H30 0.9500 . ?
C31 C32 1.403(7) . ?
C31 C35 1.518(7) . ?
C32 C33 1.385(7) . ?
C33 C34 1.374(7) . ?
C33 C56 1.525(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.517(8) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.387(8) . ?
C36 C41 1.409(8) . ?
C37 C38 1.389(8) . ?
C37 H37A 0.9500 . ?
C38 C39 1.380(9) . ?
C39 C40 1.390(8) . ?
C39 H39A 0.9500 . ?
C40 C41 1.394(8) . ?
C40 C42 1.509(8) . ?
C42 C43 1.527(8) . ?
C42 H42C 0.9900 . ?
C42 H42D 0.9900 . ?
C43 C44 1.395(8) . ?
C43 C48 1.401(8) . ?
C44 C45 1.388(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.401(7) . ?
C46 C47 1.387(7) . ?
C46 H46 0.9500 . ?
C47 C48 1.405(8) . ?
C47 C49 1.520(7) . ?
C49 C50 1.513(7) . ?
C49 H49C 0.9900 . ?
C49 H49D 0.9900 . ?
C50 C51 1.390(7) . ?
C50 C55 1.401(7) . ?
C51 C52 1.407(7) . ?
C51 H51 0.9500 . ?
C52 C53 1.387(7) . ?
C53 C54 1.392(7) . ?
C53 H53 0.9500 . ?
C54 C55 1.415(7) . ?
C54 C56 1.510(7) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C62 1.391(8) . ?
C57 C58 1.395(9) . ?
C58 C59 1.388(9) . ?
C58 H58 0.9500 . ?
C59 C60 1.396(10) . ?
C59 H59 0.9500 . ?
C60 C61 1.389(10) . ?
C60 H60 0.9500 . ?
C61 C62 1.376(9) . ?
C61 H61 0.9500 . ?
C62 H62 0.9500 . ?
C63 C64 1.380(7) . ?
C63 C68 1.403(8) . ?
C64 C65 1.386(7) . ?
C64 H64 0.9500 . ?
C65 C66 1.373(8) . ?
C65 H65 0.9500 . ?
C66 C67 1.369(8) . ?
C66 H66 0.9500 . ?
C67 C68 1.386(8) . ?
C67 H67 0.9500 . ?
C68 H68 0.9500 . ?
C69 C74 1.383(8) . ?
C69 C70 1.396(8) . ?
C70 C71 1.382(8) . ?
C70 H70 0.9500 . ?
C71 C72 1.379(9) . ?
C71 H71 0.9500 . ?
C72 C73 1.401(9) . ?
C72 H72 0.9500 . ?
C73 C74 1.380(9) . ?
C73 H73 0.9500 . ?
C74 H74 0.9500 . ?
C75 C76 1.395(8) . ?
C75 C80 1.401(8) . ?
C76 C77 1.386(8) . ?
C76 H76 0.9500 . ?
C77 C78 1.376(8) . ?
C77 H77 0.9500 . ?
C78 C79 1.379(8) . ?
C78 H78 0.9500 . ?
C79 C80 1.381(8) . ?
C79 H79 0.9500 . ?
C80 H80 0.9500 . ?
C81 C82 1.394(7) . ?
C81 C86 1.398(7) . ?
C82 C83 1.378(8) . ?
C82 H82 0.9500 . ?
C83 C84 1.386(8) . ?
C83 H83 0.9500 . ?
C84 C85 1.390(8) . ?
C84 H84 0.9500 . ?
C85 C86 1.390(8) . ?
C85 H85 0.9500 . ?
C86 H86 0.9500 . ?
C87 C92 1.389(7) . ?
C87 C88 1.396(8) . ?
C88 C89 1.389(8) . ?
C88 H88 0.9500 . ?
C89 C90 1.376(8) . ?
C89 H89 0.9500 . ?
C90 C91 1.378(8) . ?
C90 H90 0.9500 . ?
C91 C92 1.381(7) . ?
C91 H91 0.9500 . ?
C92 H92 0.9500 . ?
C93 C98 1.384(7) . ?
C93 C94 1.407(8) . ?
C94 C95 1.376(9) . ?
C94 H94 0.9500 . ?
C95 C96 1.371(9) . ?
C95 H95 0.9500 . ?
C96 C97 1.384(9) . ?
C96 H96 0.9500 . ?
C97 C98 1.400(8) . ?
C97 H97 0.9500 . ?
C98 H98 0.9500 . ?
C99 C104 1.392(7) . ?
C99 C100 1.400(7) . ?
C100 C101 1.370(7) . ?
C100 H100 0.9500 . ?
C101 C102 1.388(8) . ?
C101 H101 0.9500 . ?
C102 C103 1.379(7) . ?
C102 H102 0.9500 . ?
C103 C104 1.400(8) . ?
C103 H103 0.9500 . ?
C104 H104 0.9500 . ?
C105 C106 1.389(7) . ?
C105 C110 1.403(8) . ?
C106 C107 1.383(8) . ?
C106 H106 0.9500 . ?
C107 C108 1.371(8) . ?
C107 H107 0.9500 . ?
C108 C109 1.386(8) . ?
C108 H108 0.9500 . ?
C109 C110 1.383(8) . ?
C109 H109 0.9500 . ?
C110 H110 0.9500 . ?
C111 C112 1.390(8) . ?
C111 C116 1.415(8) . ?
C112 C113 1.385(8) . ?
C112 H112 0.9500 . ?
C113 C114 1.363(8) . ?
C113 H113 0.9500 . ?
C114 C115 1.385(8) . ?
C114 H114 0.9500 . ?
C115 C116 1.400(8) . ?
C115 H115 0.9500 . ?
C116 H116 0.9500 . ?
C117 C122 1.402(7) . ?
C117 C118 1.409(8) . ?
C118 C119 1.379(7) . ?
C118 H118 0.9500 . ?
C119 C120 1.383(8) . ?
C119 H119 0.9500 . ?
C120 C121 1.384(8) . ?
C120 H120 0.9500 . ?
C121 C122 1.381(7) . ?
C121 H121 0.9500 . ?
C122 H122 0.9500 . ?
C123 C124 1.384(8) . ?
C123 C128 1.390(8) . ?
C124 C125 1.378(8) . ?
C124 H124 0.9500 . ?
C125 C126 1.386(8) . ?
C125 H125 0.9500 . ?
C126 C127 1.376(8) . ?
C126 H126 0.9500 . ?
C127 C128 1.386(8) . ?
C127 H127 0.9500 . ?
C128 H128 0.9500 . ?
C129 C134 1.396(7) . ?
C129 C130 1.407(7) . ?
C130 C131 1.362(8) . ?
C130 H130 0.9500 . ?
C131 C132 1.388(8) . ?
C131 H131 0.9500 . ?
C132 C133 1.374(8) . ?
C132 H132 0.9500 . ?
C133 C134 1.385(8) . ?
C133 H133 0.9500 . ?
C134 H134 0.9500 . ?
C135 C140 1.391(7) . ?
C135 C136 1.416(7) . ?
C136 C137 1.384(8) . ?
C136 H136 0.9500 . ?
C137 C138 1.384(8) . ?
C137 H137 0.9500 . ?
C138 C139 1.384(8) . ?
C138 H138 0.9500 . ?
C139 C140 1.394(8) . ?
C139 H139 0.9500 . ?
C140 H140 0.9500 . ?
C141 C146 1.395(8) . ?
C141 C142 1.402(7) . ?
C142 C143 1.386(8) . ?
C142 H142 0.9500 . ?
C143 C144 1.385(8) . ?
C143 H143 0.9500 . ?
C144 C145 1.371(8) . ?
C144 H144 0.9500 . ?
C145 C146 1.390(8) . ?
C145 H145 0.9500 . ?
C146 H146 0.9500 . ?
C147 C148 1.388(7) . ?
C147 C152 1.397(8) . ?
C148 C149 1.394(8) . ?
C148 H148 0.9500 . ?
C149 C150 1.383(8) . ?
C149 H149 0.9500 . ?
C150 C151 1.384(8) . ?
C150 H150 0.9500 . ?
C151 C152 1.378(7) . ?
C151 H151 0.9500 . ?
C152 H152 0.9500 . ?
C153 C158 1.379(8) . ?
C153 C154 1.407(8) . ?
C154 C155 1.370(9) . ?
C154 H154 0.9500 . ?
C155 C156 1.393(10) . ?
C155 H155 0.9500 . ?
C156 C157 1.381(10) . ?
C156 H156 0.9500 . ?
C157 C158 1.383(8) . ?
C157 H157 0.9500 . ?
C158 H158 0.9500 . ?
C159 C160 1.340(9) . ?
C159 C164 1.380(8) . ?
C160 C161 1.382(10) . ?
C160 H160 0.9500 . ?
C161 C162 1.365(11) . ?
C161 H161 0.9500 . ?
C162 C163 1.331(10) . ?
C162 H162 0.9500 . ?
C163 C164 1.373(9) . ?
C163 H163 0.9500 . ?
C164 H164 0.9500 . ?
C165 C170 1.384(8) . ?
C165 C166 1.407(8) . ?
C166 C167 1.372(9) . ?
C166 H166 0.9500 . ?
C167 C168 1.379(9) . ?
C167 H167 0.9500 . ?
C168 C169 1.385(9) . ?
C168 H168 0.9500 . ?
C169 C170 1.390(8) . ?
C169 H169 0.9500 . ?
C170 H170 0.9500 . ?
C171 C172 1.388(8) . ?
C171 C176 1.407(8) . ?
C172 C173 1.383(8) . ?
C172 H172 0.9500 . ?
C173 C174 1.374(9) . ?
C173 H173 0.9500 . ?
C174 C175 1.378(9) . ?
C174 H174 0.9500 . ?
C175 C176 1.382(8) . ?
C175 H175 0.9500 . ?
C176 H176 0.9500 . ?

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
O2 U1 O1 178.2(2) . . ?
O2 U1 O3 88.76(16) . . ?
O1 U1 O3 93.03(19) . . ?
O2 U1 O21 88.63(16) . . ?
O1 U1 O21 90.09(18) . . ?
O3 U1 O21 145.18(14) . . ?
O2 U1 O22 90.72(16) . . ?
O1 U1 O22 90.19(19) . . ?
O3 U1 O22 70.93(14) . . ?
O21 U1 O22 74.39(15) . . ?
O2 U1 O20 90.51(16) . . ?
O1 U1 O20 87.9(2) . . ?
O3 U1 O20 140.28(13) . . ?
O21 U1 O20 74.46(15) . . ?
O22 U1 O20 148.79(14) . . ?
O2 U1 O19 88.64(15) . . ?
O1 U1 O19 91.65(17) . . ?
O3 U1 O19 70.27(13) . . ?
O21 U1 O19 144.34(14) . . ?
O22 U1 O19 141.20(13) . . ?
O20 U1 O19 70.01(13) . . ?
O23 U2 O24 178.8(2) . . ?
O23 U2 O25 93.1(2) . . ?
O24 U2 O25 88.04(16) . . ?
O23 U2 O41 89.39(17) . . ?
O24 U2 O41 91.16(15) . . ?
O25 U2 O41 72.18(13) . . ?
O23 U2 O42 91.45(19) . . ?
O24 U2 O42 87.68(15) . . ?
O25 U2 O42 145.64(13) . . ?
O41 U2 O42 73.83(13) . . ?
O23 U2 O44 91.13(18) . . ?
O24 U2 O44 89.06(15) . . ?
O25 U2 O44 71.43(13) . . ?
O41 U2 O44 143.58(13) . . ?
O42 U2 O44 142.52(13) . . ?
O23 U2 O43 87.9(2) . . ?
O24 U2 O43 91.06(15) . . ?
O25 U2 O43 142.33(13) . . ?
O41 U2 O43 145.48(13) . . ?
O42 U2 O43 71.84(13) . . ?
O44 U2 O43 70.90(13) . . ?
O4 S1 O5 115.2(2) . . ?
O4 S1 O3 110.9(2) . . ?
O5 S1 O3 109.8(2) . . ?
O4 S1 C1 108.3(2) . . ?
O5 S1 C1 108.7(2) . . ?
O3 S1 C1 103.3(2) . . ?
O7 S2 O6 112.8(2) . . ?
O7 S2 O8 113.5(2) . . ?
O6 S2 O8 110.7(2) . . ?
O7 S2 C10 106.5(2) . . ?
O6 S2 C10 106.7(2) . . ?
O8 S2 C10 106.1(2) . . ?
O9 S3 O11 112.5(3) . . ?
O9 S3 O10 110.7(2) . . ?
O11 S3 O10 112.4(3) . . ?
O9 S3 C17 106.5(2) . . ?
O11 S3 C17 106.9(2) . . ?
O10 S3 C17 107.5(2) . . ?
O13 S4 O14 112.9(3) . . ?
O13 S4 O12 112.5(3) . . ?
O14 S4 O12 111.7(2) . . ?
O13 S4 C24 106.9(2) . . ?
O14 S4 C24 106.1(2) . . ?
O12 S4 C24 106.2(2) . . ?
O27 S5 O26 115.6(3) . . ?
O27 S5 O25 110.0(2) . . ?
O26 S5 O25 110.1(3) . . ?
O27 S5 C29 108.6(3) . . ?
O26 S5 C29 107.8(3) . . ?
O25 S5 C29 104.0(3) . . ?
O29 S6 O30 112.9(4) . . ?
O29 S6 O28 111.7(5) . . ?
O30 S6 O28 112.2(3) . . ?
O29 S6 C38 105.7(3) . . ?
O30 S6 C38 107.8(3) . . ?
O28 S6 C38 106.0(3) . . ?
O32 S7 O31 113.6(3) . . ?
O32 S7 O33 113.1(3) . . ?
O31 S7 O33 110.2(2) . . ?
O32 S7 C45 106.9(2) . . ?
O31 S7 C45 107.1(2) . . ?
O33 S7 C45 105.4(2) . . ?
O34 S8 O35 113.1(2) . . ?
O34 S8 O36 112.7(2) . . ?
O35 S8 O36 110.9(2) . . ?
O34 S8 C52 106.4(2) . . ?
O35 S8 C52 106.4(2) . . ?
O36 S8 C52 106.8(2) . . ?
C63 P1 C75 109.4(3) . . ?
C63 P1 C69 109.4(3) . . ?
C75 P1 C69 111.3(3) . . ?
C63 P1 C57 108.7(3) . . ?
C75 P1 C57 109.6(3) . . ?
C69 P1 C57 108.4(3) . . ?
C93 P2 C87 109.3(2) . . ?
C93 P2 C99 108.2(2) . . ?
C87 P2 C99 109.2(3) . . ?
C93 P2 C81 106.6(3) . . ?
C87 P2 C81 112.5(2) . . ?
C99 P2 C81 110.9(2) . . ?
C117 P3 C123 109.5(3) . . ?
C117 P3 C111 107.3(2) . . ?
C123 P3 C111 112.3(3) . . ?
C117 P3 C105 111.1(3) . . ?
C123 P3 C105 106.9(3) . . ?
C111 P3 C105 109.7(3) . . ?
C129 P4 C141 113.9(3) . . ?
C129 P4 C147 106.6(3) . . ?
C141 P4 C147 110.6(3) . . ?
C129 P4 C135 108.0(2) . . ?
C141 P4 C135 107.7(3) . . ?
C147 P4 C135 110.1(3) . . ?
C153 P5 C159 108.2(3) . . ?
C153 P5 C165 111.3(3) . . ?
C159 P5 C165 106.2(3) . . ?
C153 P5 C171 109.2(3) . . ?
C159 P5 C171 111.0(3) . . ?
C165 P5 C171 110.7(3) . . ?
S1 O3 U1 153.6(2) . . ?
C4 O15 H15 112.5 . . ?
C20 O17 H17 110.7 . . ?
C27 O18 H18 118.9 . . ?
U1 O19 H19A 116.8 . . ?
U1 O19 H19B 144.3 . . ?
H19A O19 H19B 86.2 . . ?
U1 O20 H20A 128.6 . . ?
U1 O20 H20B 142.4 . . ?
H20A O20 H20B 88.2 . . ?
U1 O21 H21A 131.6 . . ?
U1 O21 H21B 133.1 . . ?
H21A O21 H21B 93.3 . . ?
U1 O22 H22A 112.2 . . ?
U1 O22 H22B 106.5 . . ?
H22A O22 H22B 95.3 . . ?
S5 O25 U2 157.4(3) . . ?
C32 O37 H37 113.1 . . ?
C41 O38 H38 128.8 . . ?
C48 O39 H39 101.6 . . ?
C55 O40 H40 102.5 . . ?
U2 O41 H41A 130.8 . . ?
U2 O41 H41B 134.3 . . ?
H41A O41 H41B 91.0 . . ?
U2 O42 H42A 119.3 . . ?
U2 O42 H42B 120.2 . . ?
H42A O42 H42B 119.3 . . ?
U2 O43 H43A 131.4 . . ?
U2 O43 H43B 125.8 . . ?
H43A O43 H43B 101.4 . . ?
U2 O44 H44A 111.5 . . ?
U2 O44 H44B 116.6 . . ?
H44A O44 H44B 128.2 . . ?
H45A O45 H45B 89.6 . . ?
H46A O46 H46B 111.4 . . ?
H47A O47 H47B 91.4 . . ?
H48A O48 H48B 91.5 . . ?
H49A O49 H49B 100.1 . . ?
H50A O50 H50B 96.6 . . ?
H51A O51 H51B 119.5 . . ?
H52A O52 H52B 114.7 . . ?
H53A O53 H53B 105.4 . . ?
H54A O54 H54B 117.9 . . ?
C6 C1 C2 120.9(5) . . ?
C6 C1 S1 121.4(4) . . ?
C2 C1 S1 117.5(4) . . ?
C3 C2 C1 121.2(5) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 117.9(5) . . ?
C2 C3 C7 119.8(5) . . ?
C4 C3 C7 122.2(5) . . ?
O15 C4 C5 117.8(4) . . ?
O15 C4 C3 121.3(5) . . ?
C5 C4 C3 120.9(5) . . ?
C6 C5 C4 119.8(5) . . ?
C6 C5 C28 118.9(5) . . ?
C4 C5 C28 121.2(5) . . ?
C1 C6 C5 119.2(5) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C8 C7 C3 113.6(4) . . ?
C8 C7 H7A 108.9 . . ?
C3 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
C3 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C9 C8 C13 118.9(5) . . ?
C9 C8 C7 122.2(5) . . ?
C13 C8 C7 119.0(5) . . ?
C8 C9 C10 120.9(5) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 119.7(5) . . ?
C11 C10 S2 119.7(4) . . ?
C9 C10 S2 120.4(4) . . ?
C12 C11 C10 120.4(5) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C13 C12 C11 119.2(5) . . ?
C13 C12 C14 120.1(5) . . ?
C11 C12 C14 120.5(5) . . ?
O16 C13 C12 119.9(5) . . ?
O16 C13 C8 119.3(4) . . ?
C12 C13 C8 120.8(5) . . ?
C15 C14 C12 111.4(4) . . ?
C15 C14 H14A 109.4 . . ?
C12 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
C12 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C20 118.8(5) . . ?
C16 C15 C14 119.1(5) . . ?
C20 C15 C14 121.9(5) . . ?
C17 C16 C15 121.9(5) . . ?
C17 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C16 C17 C18 119.6(5) . . ?
C16 C17 S3 121.3(4) . . ?
C18 C17 S3 119.1(4) . . ?
C17 C18 C19 120.8(5) . . ?
C17 C18 H18A 119.6 . . ?
C19 C18 H18A 119.6 . . ?
C18 C19 C20 118.6(5) . . ?
C18 C19 C21 119.0(5) . . ?
C20 C19 C21 122.3(5) . . ?
O17 C20 C15 118.8(5) . . ?
O17 C20 C19 120.9(5) . . ?
C15 C20 C19 120.3(5) . . ?
C22 C21 C19 110.6(4) . . ?
C22 C21 H21C 109.5 . . ?
C19 C21 H21C 109.5 . . ?
C22 C21 H21D 109.5 . . ?
C19 C21 H21D 109.5 . . ?
H21C C21 H21D 108.1 . . ?
C23 C22 C27 117.6(5) . . ?
C23 C22 C21 121.6(5) . . ?
C27 C22 C21 120.6(5) . . ?
C22 C23 C24 121.7(5) . . ?
C22 C23 H23 119.1 . . ?
C24 C23 H23 119.1 . . ?
C25 C24 C23 119.4(5) . . ?
C25 C24 S4 121.4(4) . . ?
C23 C24 S4 119.2(4) . . ?
C24 C25 C26 121.7(5) . . ?
C24 C25 H25 119.2 . . ?
C26 C25 H25 119.2 . . ?
C25 C26 C27 117.9(5) . . ?
C25 C26 C28 119.2(5) . . ?
C27 C26 C28 122.7(5) . . ?
O18 C27 C26 122.5(5) . . ?
O18 C27 C22 115.8(4) . . ?
C26 C27 C22 121.7(5) . . ?
C26 C28 C5 112.0(4) . . ?
C26 C28 H28A 109.2 . . ?
C5 C28 H28A 109.2 . . ?
C26 C28 H28B 109.2 . . ?
C5 C28 H28B 109.2 . . ?
H28A C28 H28B 107.9 . . ?
C30 C29 C34 120.1(5) . . ?
C30 C29 S5 120.9(4) . . ?
C34 C29 S5 119.0(4) . . ?
C29 C30 C31 120.7(5) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 H30 119.6 . . ?
C30 C31 C32 117.7(5) . . ?
C30 C31 C35 120.5(5) . . ?
C32 C31 C35 121.5(5) . . ?
O37 C32 C33 120.9(5) . . ?
O37 C32 C31 117.0(5) . . ?
C33 C32 C31 122.1(5) . . ?
C34 C33 C32 118.7(5) . . ?
C34 C33 C56 119.0(5) . . ?
C32 C33 C56 122.2(5) . . ?
C33 C34 C29 120.6(5) . . ?
C33 C34 H34 119.7 . . ?
C29 C34 H34 119.7 . . ?
C36 C35 C31 111.2(4) . . ?
C36 C35 H35A 109.4 . . ?
C31 C35 H35A 109.4 . . ?
C36 C35 H35B 109.4 . . ?
C31 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
C37 C36 C41 118.5(5) . . ?
C37 C36 C35 120.0(6) . . ?
C41 C36 C35 121.3(5) . . ?
C36 C37 C38 120.4(6) . . ?
C36 C37 H37A 119.8 . . ?
C38 C37 H37A 119.8 . . ?
C39 C38 C37 120.0(6) . . ?
C39 C38 S6 120.5(5) . . ?
C37 C38 S6 119.5(5) . . ?
C38 C39 C40 121.7(6) . . ?
C38 C39 H39A 119.1 . . ?
C40 C39 H39A 119.1 . . ?
C39 C40 C41 117.5(6) . . ?
C39 C40 C42 120.4(5) . . ?
C41 C40 C42 122.0(5) . . ?
O38 C41 C40 119.2(5) . . ?
O38 C41 C36 119.0(5) . . ?
C40 C41 C36 121.8(5) . . ?
C40 C42 C43 112.8(5) . . ?
C40 C42 H42C 109.0 . . ?
C43 C42 H42C 109.0 . . ?
C40 C42 H42D 109.0 . . ?
C43 C42 H42D 109.0 . . ?
H42C C42 H42D 107.8 . . ?
C44 C43 C48 119.1(5) . . ?
C44 C43 C42 119.5(5) . . ?
C48 C43 C42 121.3(5) . . ?
C45 C44 C43 120.4(5) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C46 120.4(5) . . ?
C44 C45 S7 121.5(4) . . ?
C46 C45 S7 118.0(4) . . ?
C47 C46 C45 119.8(5) . . ?
C47 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C46 C47 C48 119.6(5) . . ?
C46 C47 C49 118.9(5) . . ?
C48 C47 C49 121.3(5) . . ?
O39 C48 C43 120.2(5) . . ?
O39 C48 C47 119.1(5) . . ?
C43 C48 C47 120.6(5) . . ?
C50 C49 C47 111.6(4) . . ?
C50 C49 H49C 109.3 . . ?
C47 C49 H49C 109.3 . . ?
C50 C49 H49D 109.3 . . ?
C47 C49 H49D 109.3 . . ?
H49C C49 H49D 108.0 . . ?
C51 C50 C55 119.0(5) . . ?
C51 C50 C49 119.1(5) . . ?
C55 C50 C49 121.5(5) . . ?
C50 C51 C52 120.7(5) . . ?
C50 C51 H51 119.6 . . ?
C52 C51 H51 119.6 . . ?
C53 C52 C51 119.4(5) . . ?
C53 C52 S8 121.6(4) . . ?
C51 C52 S8 118.9(4) . . ?
C52 C53 C54 121.5(5) . . ?
C52 C53 H53 119.2 . . ?
C54 C53 H53 119.2 . . ?
C53 C54 C55 118.3(5) . . ?
C53 C54 C56 121.3(5) . . ?
C55 C54 C56 120.4(5) . . ?
O40 C55 C50 120.3(5) . . ?
O40 C55 C54 118.6(5) . . ?
C50 C55 C54 121.0(5) . . ?
C54 C56 C33 113.3(4) . . ?
C54 C56 H56A 108.9 . . ?
C33 C56 H56A 108.9 . . ?
C54 C56 H56B 108.9 . . ?
C33 C56 H56B 108.9 . . ?
H56A C56 H56B 107.7 . . ?
C62 C57 C58 118.3(6) . . ?
C62 C57 P1 119.9(5) . . ?
C58 C57 P1 121.1(5) . . ?
C59 C58 C57 121.6(7) . . ?
C59 C58 H58 119.2 . . ?
C57 C58 H58 119.2 . . ?
C58 C59 C60 119.3(7) . . ?
C58 C59 H59 120.3 . . ?
C60 C59 H59 120.3 . . ?
C61 C60 C59 118.9(7) . . ?
C61 C60 H60 120.5 . . ?
C59 C60 H60 120.5 . . ?
C62 C61 C60 121.4(7) . . ?
C62 C61 H61 119.3 . . ?
C60 C61 H61 119.3 . . ?
C61 C62 C57 120.3(6) . . ?
C61 C62 H62 119.9 . . ?
C57 C62 H62 119.9 . . ?
C64 C63 C68 119.4(5) . . ?
C64 C63 P1 121.3(4) . . ?
C68 C63 P1 119.3(4) . . ?
C63 C64 C65 120.1(5) . . ?
C63 C64 H64 119.9 . . ?
C65 C64 H64 119.9 . . ?
C66 C65 C64 119.8(5) . . ?
C66 C65 H65 120.1 . . ?
C64 C65 H65 120.1 . . ?
C67 C66 C65 121.1(5) . . ?
C67 C66 H66 119.4 . . ?
C65 C66 H66 119.4 . . ?
C66 C67 C68 119.7(5) . . ?
C66 C67 H67 120.2 . . ?
C68 C67 H67 120.2 . . ?
C67 C68 C63 119.8(5) . . ?
C67 C68 H68 120.1 . . ?
C63 C68 H68 120.1 . . ?
C74 C69 C70 119.2(5) . . ?
C74 C69 P1 121.9(5) . . ?
C70 C69 P1 118.7(4) . . ?
C71 C70 C69 120.0(6) . . ?
C71 C70 H70 120.0 . . ?
C69 C70 H70 120.0 . . ?
C72 C71 C70 120.1(6) . . ?
C72 C71 H71 119.9 . . ?
C70 C71 H71 119.9 . . ?
C71 C72 C73 120.6(6) . . ?
C71 C72 H72 119.7 . . ?
C73 C72 H72 119.7 . . ?
C74 C73 C72 118.5(6) . . ?
C74 C73 H73 120.7 . . ?
C72 C73 H73 120.7 . . ?
C73 C74 C69 121.5(6) . . ?
C73 C74 H74 119.2 . . ?
C69 C74 H74 119.2 . . ?
C76 C75 C80 119.8(5) . . ?
C76 C75 P1 119.4(4) . . ?
C80 C75 P1 120.7(4) . . ?
C77 C76 C75 119.5(6) . . ?
C77 C76 H76 120.3 . . ?
C75 C76 H76 120.3 . . ?
C78 C77 C76 120.2(6) . . ?
C78 C77 H77 119.9 . . ?
C76 C77 H77 119.9 . . ?
C77 C78 C79 120.7(6) . . ?
C77 C78 H78 119.6 . . ?
C79 C78 H78 119.6 . . ?
C78 C79 C80 120.1(6) . . ?
C78 C79 H79 119.9 . . ?
C80 C79 H79 119.9 . . ?
C79 C80 C75 119.6(5) . . ?
C79 C80 H80 120.2 . . ?
C75 C80 H80 120.2 . . ?
C82 C81 C86 119.2(5) . . ?
C82 C81 P2 123.0(4) . . ?
C86 C81 P2 117.7(4) . . ?
C83 C82 C81 120.4(5) . . ?
C83 C82 H82 119.8 . . ?
C81 C82 H82 119.8 . . ?
C82 C83 C84 120.6(6) . . ?
C82 C83 H83 119.7 . . ?
C84 C83 H83 119.7 . . ?
C83 C84 C85 119.6(6) . . ?
C83 C84 H84 120.2 . . ?
C85 C84 H84 120.2 . . ?
C86 C85 C84 120.2(5) . . ?
C86 C85 H85 119.9 . . ?
C84 C85 H85 119.9 . . ?
C85 C86 C81 120.0(5) . . ?
C85 C86 H86 120.0 . . ?
C81 C86 H86 120.0 . . ?
C92 C87 C88 119.6(5) . . ?
C92 C87 P2 120.0(4) . . ?
C88 C87 P2 120.3(4) . . ?
C89 C88 C87 120.0(5) . . ?
C89 C88 H88 120.0 . . ?
C87 C88 H88 120.0 . . ?
C90 C89 C88 119.6(6) . . ?
C90 C89 H89 120.2 . . ?
C88 C89 H89 120.2 . . ?
C89 C90 C91 120.6(5) . . ?
C89 C90 H90 119.7 . . ?
C91 C90 H90 119.7 . . ?
C90 C91 C92 120.3(6) . . ?
C90 C91 H91 119.8 . . ?
C92 C91 H91 119.8 . . ?
C91 C92 C87 119.8(5) . . ?
C91 C92 H92 120.1 . . ?
C87 C92 H92 120.1 . . ?
C98 C93 C94 120.0(5) . . ?
C98 C93 P2 121.5(4) . . ?
C94 C93 P2 118.5(4) . . ?
C95 C94 C93 119.3(6) . . ?
C95 C94 H94 120.3 . . ?
C93 C94 H94 120.3 . . ?
C96 C95 C94 120.9(6) . . ?
C96 C95 H95 119.5 . . ?
C94 C95 H95 119.5 . . ?
C95 C96 C97 120.4(6) . . ?
C95 C96 H96 119.8 . . ?
C97 C96 H96 119.8 . . ?
C96 C97 C98 119.7(6) . . ?
C96 C97 H97 120.1 . . ?
C98 C97 H97 120.1 . . ?
C93 C98 C97 119.6(6) . . ?
C93 C98 H98 120.2 . . ?
C97 C98 H98 120.2 . . ?
C104 C99 C100 120.2(5) . . ?
C104 C99 P2 120.8(4) . . ?
C100 C99 P2 119.0(4) . . ?
C101 C100 C99 119.4(5) . . ?
C101 C100 H100 120.3 . . ?
C99 C100 H100 120.3 . . ?
C100 C101 C102 120.8(5) . . ?
C100 C101 H101 119.6 . . ?
C102 C101 H101 119.6 . . ?
C103 C102 C101 120.5(5) . . ?
C103 C102 H102 119.8 . . ?
C101 C102 H102 119.8 . . ?
C102 C103 C104 119.5(5) . . ?
C102 C103 H103 120.3 . . ?
C104 C103 H103 120.3 . . ?
C99 C104 C103 119.7(5) . . ?
C99 C104 H104 120.2 . . ?
C103 C104 H104 120.2 . . ?
C106 C105 C110 119.8(5) . . ?
C106 C105 P3 122.4(4) . . ?
C110 C105 P3 117.7(4) . . ?
C107 C106 C105 119.4(6) . . ?
C107 C106 H106 120.3 . . ?
C105 C106 H106 120.3 . . ?
C108 C107 C106 120.5(5) . . ?
C108 C107 H107 119.8 . . ?
C106 C107 H107 119.8 . . ?
C107 C108 C109 120.9(5) . . ?
C107 C108 H108 119.5 . . ?
C109 C108 H108 119.5 . . ?
C110 C109 C108 119.3(5) . . ?
C110 C109 H109 120.4 . . ?
C108 C109 H109 120.4 . . ?
C109 C110 C105 120.0(5) . . ?
C109 C110 H110 120.0 . . ?
C105 C110 H110 120.0 . . ?
C112 C111 C116 118.6(5) . . ?
C112 C111 P3 123.0(4) . . ?
C116 C111 P3 118.3(4) . . ?
C113 C112 C111 121.0(6) . . ?
C113 C112 H112 119.5 . . ?
C111 C112 H112 119.5 . . ?
C114 C113 C112 120.3(6) . . ?
C114 C113 H113 119.9 . . ?
C112 C113 H113 119.9 . . ?
C113 C114 C115 120.6(6) . . ?
C113 C114 H114 119.7 . . ?
C115 C114 H114 119.7 . . ?
C114 C115 C116 120.1(6) . . ?
C114 C115 H115 120.0 . . ?
C116 C115 H115 120.0 . . ?
C115 C116 C111 119.3(6) . . ?
C115 C116 H116 120.3 . . ?
C111 C116 H116 120.3 . . ?
C122 C117 C118 119.9(5) . . ?
C122 C117 P3 120.3(4) . . ?
C118 C117 P3 119.6(4) . . ?
C119 C118 C117 119.4(5) . . ?
C119 C118 H118 120.3 . . ?
C117 C118 H118 120.3 . . ?
C118 C119 C120 120.4(5) . . ?
C118 C119 H119 119.8 . . ?
C120 C119 H119 119.8 . . ?
C119 C120 C121 120.6(5) . . ?
C119 C120 H120 119.7 . . ?
C121 C120 H120 119.7 . . ?
C122 C121 C120 120.3(5) . . ?
C122 C121 H121 119.9 . . ?
C120 C121 H121 119.9 . . ?
C121 C122 C117 119.5(5) . . ?
C121 C122 H122 120.3 . . ?
C117 C122 H122 120.3 . . ?
C124 C123 C128 119.4(5) . . ?
C124 C123 P3 119.5(4) . . ?
C128 C123 P3 120.8(4) . . ?
C125 C124 C123 120.1(6) . . ?
C125 C124 H124 119.9 . . ?
C123 C124 H124 119.9 . . ?
C124 C125 C126 120.5(6) . . ?
C124 C125 H125 119.8 . . ?
C126 C125 H125 119.8 . . ?
C127 C126 C125 119.6(6) . . ?
C127 C126 H126 120.2 . . ?
C125 C126 H126 120.2 . . ?
C126 C127 C128 120.2(6) . . ?
C126 C127 H127 119.9 . . ?
C128 C127 H127 119.9 . . ?
C127 C128 C123 120.1(6) . . ?
C127 C128 H128 119.9 . . ?
C123 C128 H128 119.9 . . ?
C134 C129 C130 118.4(5) . . ?
C134 C129 P4 120.1(4) . . ?
C130 C129 P4 121.3(4) . . ?
C131 C130 C129 121.0(6) . . ?
C131 C130 H130 119.5 . . ?
C129 C130 H130 119.5 . . ?
C130 C131 C132 119.9(6) . . ?
C130 C131 H131 120.0 . . ?
C132 C131 H131 120.0 . . ?
C133 C132 C131 120.0(5) . . ?
C133 C132 H132 120.0 . . ?
C131 C132 H132 120.0 . . ?
C132 C133 C134 120.6(5) . . ?
C132 C133 H133 119.7 . . ?
C134 C133 H133 119.7 . . ?
C133 C134 C129 119.9(5) . . ?
C133 C134 H134 120.1 . . ?
C129 C134 H134 120.1 . . ?
C140 C135 C136 120.6(5) . . ?
C140 C135 P4 118.9(4) . . ?
C136 C135 P4 120.5(4) . . ?
C137 C136 C135 118.5(5) . . ?
C137 C136 H136 120.8 . . ?
C135 C136 H136 120.8 . . ?
C138 C137 C136 120.7(5) . . ?
C138 C137 H137 119.7 . . ?
C136 C137 H137 119.7 . . ?
C137 C138 C139 121.0(5) . . ?
C137 C138 H138 119.5 . . ?
C139 C138 H138 119.5 . . ?
C138 C139 C140 119.5(5) . . ?
C138 C139 H139 120.2 . . ?
C140 C139 H139 120.2 . . ?
C135 C140 C139 119.7(5) . . ?
C135 C140 H140 120.2 . . ?
C139 C140 H140 120.2 . . ?
C146 C141 C142 119.3(5) . . ?
C146 C141 P4 120.2(4) . . ?
C142 C141 P4 120.2(4) . . ?
C143 C142 C141 120.2(5) . . ?
C143 C142 H142 119.9 . . ?
C141 C142 H142 119.9 . . ?
C144 C143 C142 120.1(6) . . ?
C144 C143 H143 119.9 . . ?
C142 C143 H143 119.9 . . ?
C145 C144 C143 119.8(6) . . ?
C145 C144 H144 120.1 . . ?
C143 C144 H144 120.1 . . ?
C144 C145 C146 121.3(6) . . ?
C144 C145 H145 119.4 . . ?
C146 C145 H145 119.4 . . ?
C145 C146 C141 119.4(5) . . ?
C145 C146 H146 120.3 . . ?
C141 C146 H146 120.3 . . ?
C148 C147 C152 120.3(5) . . ?
C148 C147 P4 121.4(4) . . ?
C152 C147 P4 117.7(4) . . ?
C147 C148 C149 119.4(6) . . ?
C147 C148 H148 120.3 . . ?
C149 C148 H148 120.3 . . ?
C150 C149 C148 120.1(5) . . ?
C150 C149 H149 119.9 . . ?
C148 C149 H149 119.9 . . ?
C149 C150 C151 120.0(5) . . ?
C149 C150 H150 120.0 . . ?
C151 C150 H150 120.0 . . ?
C152 C151 C150 120.6(5) . . ?
C152 C151 H151 119.7 . . ?
C150 C151 H151 119.7 . . ?
C151 C152 C147 119.5(5) . . ?
C151 C152 H152 120.3 . . ?
C147 C152 H152 120.3 . . ?
C158 C153 C154 120.5(5) . . ?
C158 C153 P5 123.4(5) . . ?
C154 C153 P5 116.0(4) . . ?
C155 C154 C153 119.2(6) . . ?
C155 C154 H154 120.4 . . ?
C153 C154 H154 120.4 . . ?
C154 C155 C156 120.0(7) . . ?
C154 C155 H155 120.0 . . ?
C156 C155 H155 120.0 . . ?
C157 C156 C155 120.6(6) . . ?
C157 C156 H156 119.7 . . ?
C155 C156 H156 119.7 . . ?
C156 C157 C158 119.6(6) . . ?
C156 C157 H157 120.2 . . ?
C158 C157 H157 120.2 . . ?
C153 C158 C157 119.9(6) . . ?
C153 C158 H158 120.0 . . ?
C157 C158 H158 120.0 . . ?
C160 C159 C164 118.9(6) . . ?
C160 C159 P5 121.5(5) . . ?
C164 C159 P5 119.1(5) . . ?
C159 C160 C161 120.1(7) . . ?
C159 C160 H160 119.9 . . ?
C161 C160 H160 119.9 . . ?
C162 C161 C160 120.4(8) . . ?
C162 C161 H161 119.8 . . ?
C160 C161 H161 119.8 . . ?
C163 C162 C161 119.7(7) . . ?
C163 C162 H162 120.2 . . ?
C161 C162 H162 120.2 . . ?
C162 C163 C164 120.4(7) . . ?
C162 C163 H163 119.8 . . ?
C164 C163 H163 119.8 . . ?
C163 C164 C159 120.4(6) . . ?
C163 C164 H164 119.8 . . ?
C159 C164 H164 119.8 . . ?
C170 C165 C166 119.6(6) . . ?
C170 C165 P5 123.6(5) . . ?
C166 C165 P5 116.7(5) . . ?
C167 C166 C165 120.4(6) . . ?
C167 C166 H166 119.8 . . ?
C165 C166 H166 119.8 . . ?
C166 C167 C168 119.7(6) . . ?
C166 C167 H167 120.1 . . ?
C168 C167 H167 120.1 . . ?
C167 C168 C169 120.6(6) . . ?
C167 C168 H168 119.7 . . ?
C169 C168 H168 119.7 . . ?
C168 C169 C170 120.1(6) . . ?
C168 C169 H169 120.0 . . ?
C170 C169 H169 120.0 . . ?
C165 C170 C169 119.6(6) . . ?
C165 C170 H170 120.2 . . ?
C169 C170 H170 120.2 . . ?
C172 C171 C176 119.7(5) . . ?
C172 C171 P5 120.1(5) . . ?
C176 C171 P5 120.2(4) . . ?
C173 C172 C171 119.0(6) . . ?
C173 C172 H172 120.5 . . ?
C171 C172 H172 120.5 . . ?
C174 C173 C172 121.6(6) . . ?
C174 C173 H173 119.2 . . ?
C172 C173 H173 119.2 . . ?
C173 C174 C175 119.7(6) . . ?
C173 C174 H174 120.2 . . ?
C175 C174 H174 120.2 . . ?
C174 C175 C176 120.3(6) . . ?
C174 C175 H175 119.8 . . ?
C176 C175 H175 119.8 . . ?
C175 C176 C171 119.7(6) . . ?
C175 C176 H176 120.1 . . ?
C171 C176 H176 120.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O15 H15 O16 0.80 1.73 2.515(5) 165.0 .
O17 H17 O18 0.99 1.96 2.856(5) 150.7 .
O18 H18 O15 0.99 1.95 2.630(5) 123.0 .
O19 H19A O5 0.87 1.92 2.755(5) 161.0 .
O19 H19B O33 0.93 1.77 2.652(5) 158.1 2_656
O20 H20A O31 0.96 1.74 2.696(6) 168.7 2_656
O20 H20B O36 0.82 1.95 2.705(5) 152.5 2_656
O21 H21A O35 0.87 1.81 2.666(5) 168.6 2_656
O21 H21B O55 0.92 1.70 2.585(8) 160.1 .
O22 H22A O29 0.81 1.99 2.770(7) 161.8 2_756
O22 H22B O45 0.89 1.91 2.662(6) 141.2 .
O37 H37 O40 0.81 1.91 2.578(5) 140.0 .
O38 H38 O39 0.79 2.14 2.780(7) 137.9 .
O39 H39 O40 0.88 1.97 2.828(6) 165.3 .
O40 H40 O16 0.92 1.58 2.478(5) 164.8 .
O41 H41A O14 0.89 1.79 2.664(5) 165.2 2_666
O41 H41B O51 0.92 1.79 2.644(5) 152.8 .
O42 H42A O8 0.76 1.93 2.679(5) 166.9 2_766
O42 H42B O50 0.78 1.86 2.641(5) 171.6 2_666
O43 H43A O6 0.81 1.85 2.653(5) 171.4 2_766
O43 H43B O9 0.87 1.86 2.678(5) 157.2 2_766
O44 H44A O9 0.97 1.74 2.651(6) 154.4 2_766
O44 H44B O26 0.88 2.16 2.983(8) 155.3 .
O45 H45A O4 0.99 2.02 2.851(6) 139.9 .
O45 H45B O53 0.96 2.14 2.652(6) 112.1 2_756
O46 H46A O12 0.91 2.14 2.957(6) 148.9 .
O46 H46B O58 0.91 1.84 2.734(8) 165.8 .
O47 H47A O7 1.00 1.82 2.755(5) 153.4 .
O47 H47B O32 0.97 1.95 2.725(6) 134.7 2_756
O48 H48A O8 0.99 1.96 2.938(5) 172.1 .
O48 H48B O12 0.97 2.03 2.902(6) 147.8 1_655
O49 H49A O10 0.97 1.84 2.806(5) 169.6 .
O49 H49B O13 0.95 1.89 2.800(5) 160.9 .
O50 H50A O12 0.83 2.01 2.841(5) 174.2 .
O50 H50B O58 0.97 1.87 2.765(7) 151.9 .
O51 H51A O27 0.83 2.06 2.838(6) 156.0 .
O51 H51B O57 0.90 1.82 2.686(6) 161.8 .
O52 H52A O26 0.85 1.99 2.837(6) 171.8 .
O52 H52B O30 0.93 1.98 2.862(6) 157.2 .
O53 H53A O28 0.91 1.80 2.707(7) 174.7 .
O53 H53B O47 0.81 1.96 2.719(6) 155.0 2_756
O54 H54A O33 0.91 2.12 2.973(5) 155.6 .
O54 H54B O48 0.92 1.93 2.831(5) 165.0 2_756
C2 H2 O45 0.95 2.57 3.424(7) 149.9 .
C6 H6 O54 0.95 2.56 3.415(7) 150.2 2_656
C18 H18A O49 0.95 2.59 3.509(6) 162.4 .
C70 H70 O9 0.95 2.49 3.298(7) 143.3 .
C74 H74 O24 0.95 2.60 3.374(7) 138.8 1_554
C80 H80 O4 0.95 2.57 3.204(7) 124.2 .
C86 H86 O2 0.95 2.43 3.342(7) 160.3 1_556
C88 H88 O36 0.95 2.37 3.215(7) 147.8 .
C100 H100 O2 0.95 2.54 3.367(6) 145.6 1_556
C122 H122 O54 0.95 2.53 3.378(7) 149.0 2_656
C158 H158 O32 0.95 2.45 3.329(8) 153.3 2_657

_refine_diff_density_max         1.081
_refine_diff_density_min         -1.709
_refine_diff_density_rms         0.113

_shelxl_version_number           2014-3


# SQUEEZE RESULTS (Version = 110917)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.151 0.305 0.729 17 9 ' '
2 0.148 0.553 0.360 11 2 ' '
3 0.255 0.241 0.510 32 1 ' '
4 0.354 0.952 0.645 13 1 ' '
5 0.646 0.048 0.355 14 1 ' '
6 0.745 0.759 0.490 32 1 ' '
7 0.848 0.695 0.271 17 9 ' '
8 0.852 0.447 0.641 10 2 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 0 0 1.233
-1 1 0 1.495
0 1 0 0.908
1 1 0 1.567
0 2 0 1.817
1 2 0 2.246
-1 3 0 2.936
0 3 0 2.726
-1 -2 1 2.731
0 -2 1 2.296
-1 -1 1 2.076
0 -1 1 1.495
1 -1 1 1.790
-2 0 1 2.798
-1 0 1 1.678
0 0 1 0.923
1 0 1 1.389
-1 1 1 1.724
0 1 1 1.057
1 1 1 1.519
-2 2 1 3.093
-1 2 1 2.186
0 2 1 1.742
0 3 1 2.570
1 3 1 2.831
0 -2 2 2.992
1 -1 2 2.424
0 0 2 1.846
1 0 2 2.011
-1 1 2 2.326
0 1 2 1.765
1 1 2 1.965
-1 2 2 2.581
0 2 2 2.115
0 2 3 2.760
-2 -8 4 9.831
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL a         P -1         R = 0.06
CELL   16.8351   23.7794   23.8357     70.70     79.10     89.04
SPGR P-1
# Solvent Accessible Volume =       145
# Electrons Found in S.A.V. =        26
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.843 0.703 0.256 !       6.53 eA-3
Q102 0.899 0.681 0.225 !       4.19 eA-3
Q103 0.130 0.555 0.216 !       1.70 eA-3
Q104 0.517 0.647 0.037 !       1.54 eA-3
Q105 0.662 0.399 0.366 !       1.53 eA-3
Q106 0.836 0.578 0.257 !       1.49 eA-3
Q107 0.809 0.897 0.207 !       1.46 eA-3
Q108 0.161 0.891 0.372 !       1.33 eA-3
Q109 0.832 0.946 0.211 !       1.28 eA-3
Q110 0.016 0.149 0.039 !       1.22 eA-3
Q111 0.618 0.618 0.014 !       1.16 eA-3
Q112 0.883 0.906 0.204 !       1.13 eA-3
Q113 0.875 0.986 0.195 !       1.13 eA-3
Q114 0.538 0.596 0.022 !       1.12 eA-3
Q115 0.966 0.983 0.188 !       1.08 eA-3
Q116 0.638 0.040 0.227 !       1.07 eA-3
Q117 0.753 0.899 0.146 !       1.02 eA-3
Q118 0.741 0.795 0.256 !       1.00 eA-3
Q119 0.679 0.571 0.032 !       0.96 eA-3
Q120 0.938 0.923 0.220 !       0.93 eA-3
Q121 0.781 0.814 0.094 !       0.89 eA-3
Q122 0.973 0.203 0.024 !       0.89 eA-3
Q123 0.710 0.439 0.376 !       0.88 eA-3
Q124 0.907 0.922 0.243 !       0.88 eA-3
Q125 0.845 0.650 0.266 !       0.87 eA-3
Q126 0.998 0.678 0.029 !       0.87 eA-3
Q127 0.935 0.306 0.047 !       0.85 eA-3
Q128 0.230 0.547 0.297 !       0.84 eA-3
Q129 0.195 0.525 0.221 !       0.81 eA-3
Q130 0.606 0.382 0.357 !       0.81 eA-3
Q131 0.287 0.976 0.205 !       0.81 eA-3
Q132 0.212 0.931 0.385 !       0.81 eA-3
Q133 0.500 0.696 0.406 !       0.81 eA-3
Q134 0.550 0.796 0.041 !       0.81 eA-3
Q135 0.731 0.834 0.458 !       0.81 eA-3
Q136 0.921 0.955 0.194 !       0.80 eA-3
Q137 0.481 0.766 0.047 !       0.80 eA-3
Q138 0.836 0.985 0.163 !       0.80 eA-3
Q139 0.766 0.421 0.232 !       0.80 eA-3
Q140 0.122 0.251 0.323 !       0.80 eA-3
Q141 0.907 0.266 0.024 !       0.79 eA-3
Q142 0.754 0.204 0.306 !       0.78 eA-3
Q143 0.890 0.743 0.226 !       0.78 eA-3
Q144 0.139 0.552 0.334 !       0.78 eA-3
Q145 0.467 0.736 0.400 !       0.77 eA-3
Q146 0.800 0.062 0.229 !       0.77 eA-3
Q147 0.367 0.055 0.274 !       0.76 eA-3
Q148 0.948 0.447 0.015 !       0.76 eA-3
Q149 0.063 0.305 0.343 !       0.76 eA-3
Q150 0.909 0.391 0.042 !       0.76 eA-3
Q151 0.299 0.554 0.281 !       0.76 eA-3
Q152 0.122 0.537 0.303 !       0.76 eA-3
Q153 0.969 0.392 0.428 !       0.76 eA-3
Q154 0.405 0.866 0.283 !       0.75 eA-3
Q155 0.735 0.789 0.440 !       0.75 eA-3
Q156 0.427 0.944 0.008 !       0.75 eA-3
Q157 0.394 0.399 0.165 !       0.75 eA-3
Q158 0.372 0.039 0.225 !       0.75 eA-3
Q159 0.933 0.086 0.084 !       0.74 eA-3
Q160 0.903 0.383 0.186 !       0.74 eA-3
Q161 0.522 0.110 0.049 !       0.73 eA-3
Q162 0.966 0.413 0.022 !       0.73 eA-3
Q163 0.907 0.427 0.001 !       0.73 eA-3
Q164 0.128 0.861 0.429 !       0.73 eA-3
Q165 0.126 0.526 0.344 !       0.72 eA-3
Q166 0.439 0.181 0.000 !       0.72 eA-3
Q167 0.645 0.704 0.276 !       0.72 eA-3
Q168 0.287 0.147 0.281 !       0.72 eA-3
Q169 0.687 0.766 0.304 !       0.72 eA-3
Q170 0.663 0.116 0.341 !       0.72 eA-3
Q171 0.192 0.557 0.314 !       0.72 eA-3
Q172 0.714 0.483 0.258 !       0.72 eA-3
Q173 0.888 0.920 0.124 !       0.72 eA-3
Q174 0.544 0.628 0.455 !       0.72 eA-3
Q175 0.458 0.048 0.022 !       0.72 eA-3
Q176 0.692 0.169 0.343 !       0.71 eA-3
Q177 0.539 0.663 0.483 !       0.71 eA-3
Q178 0.428 0.429 0.101 !       0.71 eA-3
Q179 0.589 0.788 0.436 !       0.71 eA-3
Q180 0.073 0.482 0.421 !       0.71 eA-3
Q181 0.588 0.038 0.350 !       0.71 eA-3
Q182 0.561 1.001 0.181 !       0.71 eA-3
Q183 0.681 0.999 0.436 !       0.71 eA-3
Q184 0.250 0.164 0.345 !       0.71 eA-3
Q185 0.743 0.478 0.288 !       0.71 eA-3
Q186 0.441 0.554 0.105 !       0.71 eA-3
Q187 0.685 0.366 0.282 !       0.70 eA-3
Q188 0.477 0.883 0.032 !       0.70 eA-3
Q189 0.033 0.556 0.025 !       0.70 eA-3
Q190 0.217 0.846 0.320 !       0.70 eA-3
Q191 0.855 0.368 0.243 !       0.70 eA-3
Q192 0.451 0.625 0.046 !       0.70 eA-3
Q193 0.785 0.068 0.396 !       0.70 eA-3
Q194 0.716 0.599 0.470 !       0.70 eA-3
Q195 0.168 0.515 0.375 !       0.70 eA-3
Q196 0.457 0.478 0.001 !       0.70 eA-3
Q197 0.587 0.024 0.289 !       0.69 eA-3
Q198 0.194 0.048 0.392 !       0.69 eA-3
Q199 0.242 0.976 0.241 !       0.69 eA-3
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_10
_database_code_depnum_ccdc_archive 'CCDC 1893023'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2019-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C76 H88 O32 P2 S4 U'
_chemical_formula_weight         1941.67

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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.7110(9)
_cell_length_b                   13.9471(6)
_cell_length_c                   22.3786(16)
_cell_angle_alpha                105.108(4)
_cell_angle_beta                 100.002(3)
_cell_angle_gamma                96.077(4)
_cell_volume                     4017.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    199629
_cell_measurement_theta_min      2.09
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_F_000             1972
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    2.251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'1 φ and 14 ω scans with 2° steps (746 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            199629
_diffrn_reflns_av_unetI/netI     0.0922
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.093
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             15250
_reflns_number_gt                11972
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms bound to O atoms were found on a 
 difference Fourier map, except for those of some lattice water molecules
 (one of them with half-occupancy) and all the others were introduced at
 calculated positions; all were treated as riding atoms with an isotropic
 displacement parameter equal to 1.2 times that of the parent atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0371P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15250
_refine_ls_number_parameters     1042
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.0908
_refine_ls_wR_factor_gt          0.0865
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.970
_refine_ls_shift/su_max          0.002
_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_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 0.95413(2) 0.25133(2) 0.80717(2) 0.02465(6) Uani 1 1 d . . . . .
S1 S 0.80606(8) 0.44701(7) 0.77158(5) 0.0259(2) Uani 1 1 d . . . . .
S2 S 0.97953(8) 0.99519(8) 0.82010(5) 0.0266(2) Uani 1 1 d . . . . .
S3 S 0.44984(8) 0.97965(8) 0.81052(5) 0.0276(2) Uani 1 1 d . . . . .
S4 S 0.30873(8) 0.47049(8) 0.82056(5) 0.0290(3) Uani 1 1 d . . . . .
P1 P 0.54222(9) 0.61533(9) 0.63812(5) 0.0316(3) Uani 1 1 d . . . . .
P2 P 1.00635(9) 0.85342(8) 0.57741(6) 0.0307(3) Uani 1 1 d . . . . .
O1 O 0.9809(2) 0.32835(19) 0.88608(13) 0.0294(7) Uani 1 1 d . . . . .
O2 O 0.9236(2) 0.17383(19) 0.72859(13) 0.0250(7) Uani 1 1 d . . . . .
O3 O 0.8321(2) 0.34860(19) 0.77723(13) 0.0277(7) Uani 1 1 d . . . . .
O4 O 0.8814(2) 0.4973(2) 0.74642(14) 0.0295(7) Uani 1 1 d . . . . .
O5 O 0.7045(2) 0.4332(2) 0.73578(14) 0.0305(7) Uani 1 1 d . . . . .
O6 O 0.9962(2) 1.10692(19) 0.83860(13) 0.0267(7) Uani 1 1 d . . . . .
O7 O 0.8955(2) 0.9520(2) 0.76726(13) 0.0325(7) Uani 1 1 d . . . . .
O8 O 1.0709(2) 0.9560(2) 0.80968(14) 0.0322(7) Uani 1 1 d . . . . .
O9 O 0.3613(2) 0.9032(2) 0.78439(15) 0.0366(8) Uani 1 1 d . . . . .
O10 O 0.4238(2) 1.0808(2) 0.83122(14) 0.0317(7) Uani 1 1 d . . . . .
O11 O 0.5194(2) 0.9772(2) 0.76826(14) 0.0372(8) Uani 1 1 d . . . . .
O12 O 0.2787(2) 0.5376(2) 0.78312(15) 0.0380(8) Uani 1 1 d . . . . .
O13 O 0.2254(2) 0.4396(2) 0.84921(14) 0.0356(8) Uani 1 1 d . . . . .
O14 O 0.3482(2) 0.3846(2) 0.78732(14) 0.0352(8) Uani 1 1 d . . . . .
O15 O 0.8123(2) 0.6891(2) 1.03141(13) 0.0279(7) Uani 1 1 d . . . . .
H15 H 0.8583 0.7432 1.0353 0.033 Uiso 1 1 d R U . . .
O16 O 0.8441(2) 0.8816(2) 1.03094(13) 0.0272(7) Uani 1 1 d . . . . .
H16 H 0.7945 0.9088 1.0424 0.033 Uiso 1 1 d R U . . .
O17 O 0.6603(2) 0.9184(2) 1.04707(13) 0.0293(7) Uani 1 1 d . . . . .
H17 H 0.6459 0.8591 1.0490 0.035 Uiso 1 1 d R U . . .
O18 O 0.6222(2) 0.7180(2) 1.03720(13) 0.0289(7) Uani 1 1 d . . . . .
H18 H 0.6795 0.7040 1.0380 0.035 Uiso 1 1 d R U . . .
O19 O 0.8063(2) 0.1847(2) 0.83024(15) 0.0340(8) Uani 1 1 d . . . . .
H19A H 0.7644 0.1328 0.8088 0.041 Uiso 1 1 d R U . . .
H19B H 0.7698 0.2070 0.8590 0.041 Uiso 1 1 d R U . . .
O20 O 1.1304(2) 0.2512(2) 0.81307(13) 0.0288(7) Uani 1 1 d . . . . .
H20A H 1.1794 0.3071 0.8285 0.035 Uiso 1 1 d R U . . .
H20B H 1.1634 0.2128 0.8262 0.035 Uiso 1 1 d R U . . .
O21 O 1.0351(2) 0.3927(2) 0.77491(14) 0.0318(7) Uani 1 1 d . . . . .
H21A H 0.9941 0.4388 0.7707 0.038 Uiso 1 1 d R U . . .
H21B H 1.1026 0.4338 0.7895 0.038 Uiso 1 1 d R U . . .
O22 O 0.5292(3) 0.3282(2) 0.76098(15) 0.0445(9) Uani 1 1 d . . . . .
H22A H 0.5773 0.3767 0.7517 0.053 Uiso 1 1 d R U . . .
H22B H 0.4898 0.3667 0.7614 0.053 Uiso 1 1 d R U . . .
O23 O 0.7078(3) 0.0140(3) 0.75510(16) 0.0492(9) Uani 1 1 d . . . . .
H23A H 0.7625 -0.0243 0.7632 0.059 Uiso 1 1 d R U . . .
H23B H 0.6399 -0.0205 0.7505 0.059 Uiso 1 1 d R U . . .
O24 O 1.2303(2) 0.1173(2) 0.84381(14) 0.0324(7) Uani 1 1 d . . . . .
H24A H 1.1875 0.0505 0.8292 0.039 Uiso 1 1 d R U . . .
H24B H 1.2968 0.1092 0.8378 0.039 Uiso 1 1 d R U . . .
O25 O 1.2020(3) 0.8311(3) 0.83589(17) 0.0518(10) Uani 1 1 d . . . . .
H25A H 1.2542 0.8440 0.8130 0.062 Uiso 1 1 d R U . . .
H25B H 1.1779 0.7638 0.8127 0.062 Uiso 1 1 d R U . . .
O26 O 0.5611(3) 1.2596(2) 0.86748(17) 0.0496(10) Uani 1 1 d . . . . .
H26A H 0.5088 1.2024 0.8588 0.060 Uiso 1 1 d R U . . .
H26B H 0.5582 1.2866 0.8345 0.060 Uiso 1 1 d R U . . .
O27 O 0.1566(3) 0.5929(3) 0.9574(2) 0.0681(12) Uani 1 1 d . . . . .
H27A H 0.1432 0.6428 0.9436 0.082 Uiso 1 1 d R U . . .
H27B H 0.1068 0.5575 0.9718 0.082 Uiso 1 1 d R U . . .
O28 O 0.7440(3) 0.2554(2) 0.93449(17) 0.0488(9) Uani 1 1 d . . . . .
O29 O 0.1271(3) 0.6455(3) 0.84407(17) 0.0597(11) Uani 1 1 d . . . . .
O30 O 0.6571(4) 0.2150(4) 0.6364(3) 0.122(2) Uani 1 1 d . . . . .
O31 O 0.5139(4) 1.1248(3) 0.6889(2) 0.0991(17) Uani 1 1 d . . . . .
O32 O 1.0000 0.5000 1.0000 0.100(2) Uani 1 2 d S . P . .
O33 O 0.3255(5) 0.7008(4) 0.7234(3) 0.0427(18) Uani 0.5 1 d . . P . .
C1 C 0.8098(3) 0.5209(3) 0.8491(2) 0.0250(10) Uani 1 1 d . . . . .
C2 C 0.8823(3) 0.6058(3) 0.8771(2) 0.0265(10) Uani 1 1 d . . . . .
H2 H 0.9301 0.6241 0.8544 0.032 Uiso 1 1 calc R U . . .
C3 C 0.8850(3) 0.6647(3) 0.9388(2) 0.0238(9) Uani 1 1 d . . . . .
C4 C 0.8127(3) 0.6345(3) 0.97029(19) 0.0241(9) Uani 1 1 d . . . . .
C5 C 0.7394(3) 0.5491(3) 0.9424(2) 0.0237(9) Uani 1 1 d . . . . .
C6 C 0.7401(3) 0.4922(3) 0.8816(2) 0.0265(10) Uani 1 1 d . . . . .
H6 H 0.6922 0.4329 0.8620 0.032 Uiso 1 1 calc R U . . .
C7 C 0.9659(3) 0.7567(3) 0.9678(2) 0.0248(10) Uani 1 1 d . . . . .
H7A H 0.9792 0.7712 1.0145 0.030 Uiso 1 1 calc R U . . .
H7B H 1.0286 0.7413 0.9539 0.030 Uiso 1 1 calc R U . . .
C8 C 0.9386(3) 0.8497(3) 0.95036(19) 0.0230(9) Uani 1 1 d . . . . .
C9 C 0.9736(3) 0.8791(3) 0.90186(18) 0.0215(9) Uani 1 1 d . . . . .
H9 H 1.0169 0.8414 0.8799 0.026 Uiso 1 1 calc R U . . .
C10 C 0.9457(3) 0.9623(3) 0.88569(19) 0.0236(9) Uani 1 1 d . . . . .
C11 C 0.8806(3) 1.0172(3) 0.91574(19) 0.0233(9) Uani 1 1 d . . . . .
H11 H 0.8606 1.0733 0.9030 0.028 Uiso 1 1 calc R U . . .
C12 C 0.8445(3) 0.9904(3) 0.96426(18) 0.0210(9) Uani 1 1 d . . . . .
C13 C 0.8752(3) 0.9080(3) 0.98167(18) 0.0216(9) Uani 1 1 d . . . . .
C14 C 0.7676(3) 1.0468(3) 0.99387(19) 0.0216(9) Uani 1 1 d . . . . .
H14A H 0.7746 1.1154 0.9888 0.026 Uiso 1 1 calc R U . . .
H14B H 0.7804 1.0530 1.0397 0.026 Uiso 1 1 calc R U . . .
C15 C 0.6610(3) 0.9920(3) 0.96296(19) 0.0238(9) Uani 1 1 d . . . . .
C16 C 0.6112(3) 1.0041(3) 0.9066(2) 0.0255(10) Uani 1 1 d . . . . .
H16A H 0.6439 1.0467 0.8867 0.031 Uiso 1 1 calc R U . . .
C17 C 0.5142(3) 0.9547(3) 0.8790(2) 0.0252(10) Uani 1 1 d . . . . .
C18 C 0.4659(3) 0.8921(3) 0.9076(2) 0.0245(10) Uani 1 1 d . . . . .
H18A H 0.3993 0.8590 0.8884 0.029 Uiso 1 1 calc R U . . .
C19 C 0.5133(3) 0.8770(3) 0.9637(2) 0.0242(10) Uani 1 1 d . . . . .
C20 C 0.6112(3) 0.9279(3) 0.99064(19) 0.0233(9) Uani 1 1 d . . . . .
C21 C 0.4588(3) 0.8090(3) 0.9942(2) 0.0245(10) Uani 1 1 d . . . . .
H21C H 0.3870 0.8165 0.9880 0.029 Uiso 1 1 calc R U . . .
H21D H 0.4871 0.8294 1.0403 0.029 Uiso 1 1 calc R U . . .
C22 C 0.4681(3) 0.6989(3) 0.96583(19) 0.0236(9) Uani 1 1 d . . . . .
C23 C 0.3944(3) 0.6397(3) 0.91447(19) 0.0245(10) Uani 1 1 d . . . . .
H23 H 0.3373 0.6666 0.8996 0.029 Uiso 1 1 calc R U . . .
C24 C 0.4047(3) 0.5417(3) 0.8851(2) 0.0244(10) Uani 1 1 d . . . . .
C25 C 0.4875(3) 0.5025(3) 0.90625(19) 0.0234(10) Uani 1 1 d . . . . .
H25 H 0.4929 0.4349 0.8860 0.028 Uiso 1 1 calc R U . . .
C26 C 0.5635(3) 0.5595(3) 0.9565(2) 0.0246(10) Uani 1 1 d . . . . .
C27 C 0.5508(3) 0.6581(3) 0.98595(19) 0.0227(9) Uani 1 1 d . . . . .
C28 C 0.6582(3) 0.5192(3) 0.9759(2) 0.0248(10) Uani 1 1 d . . . . .
H28A H 0.6434 0.4450 0.9653 0.030 Uiso 1 1 calc R U . . .
H28B H 0.6828 0.5460 1.0223 0.030 Uiso 1 1 calc R U . . .
C29 C 0.4602(4) 0.5000(3) 0.6270(2) 0.0350(12) Uani 1 1 d . . . . .
C30 C 0.3674(4) 0.5076(4) 0.6432(2) 0.0436(13) Uani 1 1 d . . . . .
H30 H 0.3452 0.5711 0.6535 0.052 Uiso 1 1 calc R U . . .
C31 C 0.3067(4) 0.4210(4) 0.6442(2) 0.0496(15) Uani 1 1 d . . . . .
H31 H 0.2442 0.4254 0.6569 0.060 Uiso 1 1 calc R U . . .
C32 C 0.3387(4) 0.3287(4) 0.6267(2) 0.0507(15) Uani 1 1 d . . . . .
H32 H 0.2975 0.2699 0.6274 0.061 Uiso 1 1 calc R U . . .
C33 C 0.4292(4) 0.3203(4) 0.6081(2) 0.0487(14) Uani 1 1 d . . . . .
H33 H 0.4492 0.2562 0.5951 0.058 Uiso 1 1 calc R U . . .
C34 C 0.4907(4) 0.4067(3) 0.6088(2) 0.0403(12) Uani 1 1 d . . . . .
H34 H 0.5536 0.4020 0.5969 0.048 Uiso 1 1 calc R U . . .
C35 C 0.5943(3) 0.6685(3) 0.7209(2) 0.0289(10) Uani 1 1 d . . . . .
C36 C 0.5486(3) 0.6421(3) 0.7660(2) 0.0331(11) Uani 1 1 d . . . . .
H36 H 0.4880 0.5954 0.7534 0.040 Uiso 1 1 calc R U . . .
C37 C 0.5915(3) 0.6838(3) 0.8294(2) 0.0331(11) Uani 1 1 d . . . . .
H37 H 0.5610 0.6647 0.8604 0.040 Uiso 1 1 calc R U . . .
C38 C 0.6785(3) 0.7533(3) 0.8480(2) 0.0286(10) Uani 1 1 d . . . . .
H38 H 0.7069 0.7826 0.8917 0.034 Uiso 1 1 calc R U . . .
C39 C 0.7243(4) 0.7802(3) 0.8033(2) 0.0357(11) Uani 1 1 d . . . . .
H39 H 0.7847 0.8272 0.8163 0.043 Uiso 1 1 calc R U . . .
C40 C 0.6827(3) 0.7391(3) 0.7400(2) 0.0347(11) Uani 1 1 d . . . . .
H40 H 0.7137 0.7584 0.7093 0.042 Uiso 1 1 calc R U . . .
C41 C 0.4738(3) 0.6984(3) 0.6049(2) 0.0324(11) Uani 1 1 d . . . . .
C42 C 0.4865(4) 0.7996(3) 0.6371(2) 0.0396(12) Uani 1 1 d . . . . .
H42 H 0.5266 0.8243 0.6787 0.048 Uiso 1 1 calc R U . . .
C43 C 0.4407(4) 0.8641(4) 0.6084(3) 0.0474(14) Uani 1 1 d . . . . .
H43 H 0.4502 0.9337 0.6303 0.057 Uiso 1 1 calc R U . . .
C44 C 0.3812(4) 0.8294(4) 0.5485(3) 0.0468(13) Uani 1 1 d . . . . .
H44 H 0.3507 0.8747 0.5289 0.056 Uiso 1 1 calc R U . . .
C45 C 0.3662(4) 0.7267(4) 0.5166(2) 0.0448(13) Uani 1 1 d . . . . .
H45 H 0.3246 0.7017 0.4755 0.054 Uiso 1 1 calc R U . . .
C46 C 0.4118(4) 0.6619(3) 0.5450(2) 0.0388(12) Uani 1 1 d . . . . .
H46 H 0.4008 0.5920 0.5236 0.047 Uiso 1 1 calc R U . . .
C47 C 0.6467(3) 0.5926(3) 0.5993(2) 0.0311(11) Uani 1 1 d . . . . .
C48 C 0.7156(4) 0.5380(3) 0.6227(2) 0.0346(11) Uani 1 1 d . . . . .
H48 H 0.7076 0.5143 0.6580 0.042 Uiso 1 1 calc R U . . .
C49 C 0.7962(4) 0.5183(3) 0.5938(2) 0.0380(12) Uani 1 1 d . . . . .
H49 H 0.8428 0.4796 0.6087 0.046 Uiso 1 1 calc R U . . .
C50 C 0.8082(4) 0.5554(3) 0.5432(2) 0.0380(12) Uani 1 1 d . . . . .
H50 H 0.8628 0.5416 0.5231 0.046 Uiso 1 1 calc R U . . .
C51 C 0.7409(4) 0.6123(3) 0.5223(2) 0.0362(12) Uani 1 1 d . . . . .
H51 H 0.7506 0.6387 0.4883 0.043 Uiso 1 1 calc R U . . .
C52 C 0.6592(3) 0.6318(3) 0.5498(2) 0.0303(10) Uani 1 1 d . . . . .
H52 H 0.6130 0.6710 0.5351 0.036 Uiso 1 1 calc R U . . .
C53 C 1.0184(4) 0.7583(3) 0.6178(2) 0.0354(12) Uani 1 1 d . . . . .
C54 C 0.9734(4) 0.7586(4) 0.6688(2) 0.0495(15) Uani 1 1 d . . . . .
H54 H 0.9307 0.8063 0.6809 0.059 Uiso 1 1 calc R U . . .
C55 C 0.9911(5) 0.6888(4) 0.7021(3) 0.0604(18) Uani 1 1 d . . . . .
H55 H 0.9599 0.6884 0.7367 0.073 Uiso 1 1 calc R U . . .
C56 C 1.0536(5) 0.6204(4) 0.6851(3) 0.0551(16) Uani 1 1 d . . . . .
H56 H 1.0661 0.5738 0.7087 0.066 Uiso 1 1 calc R U . . .
C57 C 1.0976(5) 0.6185(4) 0.6353(3) 0.0578(16) Uani 1 1 d . . . . .
H57 H 1.1405 0.5707 0.6239 0.069 Uiso 1 1 calc R U . . .
C58 C 1.0797(4) 0.6872(4) 0.6008(3) 0.0465(13) Uani 1 1 d . . . . .
H58 H 1.1097 0.6853 0.5654 0.056 Uiso 1 1 calc R U . . .
C59 C 0.8819(3) 0.8853(3) 0.5643(2) 0.0336(11) Uani 1 1 d . . . . .
C60 C 0.8396(4) 0.9265(4) 0.6169(2) 0.0480(14) Uani 1 1 d . . . . .
H60 H 0.8765 0.9372 0.6588 0.058 Uiso 1 1 calc R U . . .
C61 C 0.7445(4) 0.9511(5) 0.6070(3) 0.0612(17) Uani 1 1 d . . . . .
H61 H 0.7158 0.9782 0.6422 0.073 Uiso 1 1 calc R U . . .
C62 C 0.6901(4) 0.9364(4) 0.5457(3) 0.0511(14) Uani 1 1 d . . . . .
H62 H 0.6234 0.9506 0.5391 0.061 Uiso 1 1 calc R U . . .
C63 C 0.7338(4) 0.9010(3) 0.4948(2) 0.0393(12) Uani 1 1 d . . . . .
H63 H 0.6985 0.8951 0.4532 0.047 Uiso 1 1 calc R U . . .
C64 C 0.8285(4) 0.8741(3) 0.5035(2) 0.0336(11) Uani 1 1 d . . . . .
H64 H 0.8569 0.8481 0.4680 0.040 Uiso 1 1 calc R U . . .
C65 C 1.0938(3) 0.9641(3) 0.6231(2) 0.0285(10) Uani 1 1 d . . . . .
C66 C 1.0675(3) 1.0595(3) 0.6315(2) 0.0307(10) Uani 1 1 d . . . . .
H66 H 1.0020 1.0676 0.6135 0.037 Uiso 1 1 calc R U . . .
C67 C 1.1384(4) 1.1431(3) 0.6669(2) 0.0363(12) Uani 1 1 d . . . . .
H67 H 1.1206 1.2085 0.6731 0.044 Uiso 1 1 calc R U . . .
C68 C 1.2337(4) 1.1326(3) 0.6928(2) 0.0365(12) Uani 1 1 d . . . . .
H68 H 1.2814 1.1902 0.7167 0.044 Uiso 1 1 calc R U . . .
C69 C 1.2594(4) 1.0370(3) 0.6837(2) 0.0371(12) Uani 1 1 d . . . . .
H69 H 1.3255 1.0294 0.7011 0.045 Uiso 1 1 calc R U . . .
C70 C 1.1902(4) 0.9529(3) 0.6498(2) 0.0359(11) Uani 1 1 d . . . . .
H70 H 1.2081 0.8877 0.6447 0.043 Uiso 1 1 calc R U . . .
C71 C 1.0384(3) 0.8046(3) 0.5017(2) 0.0301(10) Uani 1 1 d . . . . .
C72 C 1.1179(3) 0.8538(3) 0.4850(2) 0.0326(11) Uani 1 1 d . . . . .
H72 H 1.1549 0.9154 0.5128 0.039 Uiso 1 1 calc R U . . .
C73 C 1.1434(4) 0.8123(4) 0.4272(2) 0.0363(11) Uani 1 1 d . . . . .
H73 H 1.1980 0.8458 0.4156 0.044 Uiso 1 1 calc R U . . .
C74 C 1.0898(4) 0.7228(3) 0.3867(2) 0.0367(12) Uani 1 1 d . . . . .
H74 H 1.1077 0.6949 0.3474 0.044 Uiso 1 1 calc R U . . .
C75 C 1.0108(4) 0.6741(3) 0.4031(2) 0.0425(13) Uani 1 1 d . . . . .
H75 H 0.9741 0.6125 0.3751 0.051 Uiso 1 1 calc R U . . .
C76 C 0.9844(4) 0.7144(3) 0.4603(2) 0.0432(13) Uani 1 1 d . . . . .
H76 H 0.9295 0.6806 0.4715 0.052 Uiso 1 1 calc R U . . .


_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 O2 1.759(3) . ?
U1 O1 1.764(3) . ?
U1 O19 2.335(3) . ?
U1 O3 2.378(3) . ?
U1 O6 2.393(3) 1_545 ?
U1 O20 2.397(3) . ?
U1 O21 2.490(3) . ?
S1 O5 1.447(3) . ?
S1 O4 1.460(3) . ?
S1 O3 1.485(3) . ?
S1 C1 1.761(4) . ?
S2 O7 1.448(3) . ?
S2 O8 1.449(3) . ?
S2 O6 1.486(3) . ?
S2 C10 1.767(4) . ?
S3 O9 1.451(3) . ?
S3 O11 1.452(3) . ?
S3 O10 1.468(3) . ?
S3 C17 1.767(5) . ?
S4 O14 1.447(3) . ?
S4 O12 1.455(3) . ?
S4 O13 1.482(3) . ?
S4 C24 1.767(4) . ?
P1 C35 1.790(4) . ?
P1 C41 1.792(5) . ?
P1 C29 1.795(4) . ?
P1 C47 1.814(5) . ?
P2 C53 1.795(5) . ?
P2 C65 1.796(4) . ?
P2 C59 1.803(5) . ?
P2 C71 1.803(4) . ?
O6 U1 2.393(3) 1_565 ?
O15 C4 1.382(5) . ?
O15 H15 0.9061 . ?
O16 C13 1.369(5) . ?
O16 H16 0.8583 . ?
O17 C20 1.370(5) . ?
O17 H17 0.8441 . ?
O18 C27 1.381(5) . ?
O18 H18 0.8285 . ?
O19 H19A 0.8477 . ?
O19 H19B 0.8956 . ?
O20 H20A 0.9203 . ?
O20 H20B 0.8160 . ?
O21 H21A 0.9109 . ?
O21 H21B 0.9880 . ?
O22 H22A 0.9806 . ?
O22 H22B 0.8003 . ?
O23 H23A 0.9836 . ?
O23 H23B 0.9769 . ?
O24 H24A 0.9891 . ?
O24 H24B 0.9593 . ?
O25 H25A 0.9771 . ?
O25 H25B 0.9376 . ?
O26 H26A 0.9685 . ?
O26 H26B 0.9098 . ?
O27 H27A 0.8561 . ?
O27 H27B 0.9509 . ?
C1 C6 1.383(6) . ?
C1 C2 1.389(5) . ?
C2 C3 1.401(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.402(6) . ?
C3 C7 1.521(5) . ?
C4 C5 1.400(5) . ?
C5 C6 1.388(6) . ?
C5 C28 1.527(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.514(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.396(6) . ?
C8 C13 1.405(5) . ?
C9 C10 1.375(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(6) . ?
C11 C12 1.386(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(6) . ?
C12 C14 1.521(5) . ?
C14 C15 1.529(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.386(6) . ?
C15 C20 1.398(6) . ?
C16 C17 1.387(6) . ?
C16 H16A 0.9500 . ?
C17 C18 1.389(6) . ?
C18 C19 1.389(6) . ?
C18 H18A 0.9500 . ?
C19 C20 1.400(6) . ?
C19 C21 1.512(5) . ?
C21 C22 1.529(5) . ?
C21 H21C 0.9900 . ?
C21 H21D 0.9900 . ?
C22 C27 1.380(6) . ?
C22 C23 1.396(6) . ?
C23 C24 1.387(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.374(6) . ?
C25 C26 1.392(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.405(5) . ?
C26 C28 1.508(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.390(7) . ?
C29 C34 1.390(7) . ?
C30 C31 1.401(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.385(8) . ?
C31 H31 0.9500 . ?
C32 C33 1.382(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.391(6) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.382(6) . ?
C35 C40 1.402(6) . ?
C36 C37 1.380(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.381(6) . ?
C37 H37 0.9500 . ?
C38 C39 1.377(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.374(6) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 C42 1.384(6) . ?
C41 C46 1.392(6) . ?
C42 C43 1.379(7) . ?
C42 H42 0.9500 . ?
C43 C44 1.377(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.399(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.374(7) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C52 1.385(6) . ?
C47 C48 1.390(7) . ?
C48 C49 1.390(6) . ?
C48 H48 0.9500 . ?
C49 C50 1.389(7) . ?
C49 H49 0.9500 . ?
C50 C51 1.378(7) . ?
C50 H50 0.9500 . ?
C51 C52 1.387(6) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C53 C58 1.387(7) . ?
C53 C54 1.389(7) . ?
C54 C55 1.387(8) . ?
C54 H54 0.9500 . ?
C55 C56 1.374(8) . ?
C55 H55 0.9500 . ?
C56 C57 1.352(8) . ?
C56 H56 0.9500 . ?
C57 C58 1.396(7) . ?
C57 H57 0.9500 . ?
C58 H58 0.9500 . ?
C59 C64 1.390(6) . ?
C59 C60 1.417(6) . ?
C60 C61 1.378(8) . ?
C60 H60 0.9500 . ?
C61 C62 1.395(8) . ?
C61 H61 0.9500 . ?
C62 C63 1.383(7) . ?
C62 H62 0.9500 . ?
C63 C64 1.384(7) . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
C65 C66 1.388(6) . ?
C65 C70 1.396(7) . ?
C66 C67 1.394(6) . ?
C66 H66 0.9500 . ?
C67 C68 1.373(7) . ?
C67 H67 0.9500 . ?
C68 C69 1.389(6) . ?
C68 H68 0.9500 . ?
C69 C70 1.379(6) . ?
C69 H69 0.9500 . ?
C70 H70 0.9500 . ?
C71 C72 1.382(6) . ?
C71 C76 1.395(6) . ?
C72 C73 1.393(6) . ?
C72 H72 0.9500 . ?
C73 C74 1.380(6) . ?
C73 H73 0.9500 . ?
C74 C75 1.372(7) . ?
C74 H74 0.9500 . ?
C75 C76 1.384(6) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?

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
O2 U1 O1 178.23(13) . . ?
O2 U1 O19 92.64(11) . . ?
O1 U1 O19 85.69(12) . . ?
O2 U1 O3 87.88(12) . . ?
O1 U1 O3 91.12(12) . . ?
O19 U1 O3 74.54(10) . . ?
O2 U1 O6 87.58(11) . 1_545 ?
O1 U1 O6 92.57(12) . 1_545 ?
O19 U1 O6 76.24(10) . 1_545 ?
O3 U1 O6 150.17(9) . 1_545 ?
O2 U1 O20 92.48(11) . . ?
O1 U1 O20 89.24(12) . . ?
O19 U1 O20 147.62(11) . . ?
O3 U1 O20 137.61(9) . . ?
O6 U1 O20 72.06(9) 1_545 . ?
O2 U1 O21 91.65(11) . . ?
O1 U1 O21 89.39(11) . . ?
O19 U1 O21 144.24(10) . . ?
O3 U1 O21 70.16(10) . . ?
O6 U1 O21 139.43(10) 1_545 . ?
O20 U1 O21 67.45(10) . . ?
O5 S1 O4 114.39(19) . . ?
O5 S1 O3 109.82(17) . . ?
O4 S1 O3 110.38(17) . . ?
O5 S1 C1 107.79(19) . . ?
O4 S1 C1 107.89(18) . . ?
O3 S1 C1 106.19(18) . . ?
O7 S2 O8 112.97(18) . . ?
O7 S2 O6 112.16(19) . . ?
O8 S2 O6 111.30(17) . . ?
O7 S2 C10 106.44(18) . . ?
O8 S2 C10 108.1(2) . . ?
O6 S2 C10 105.38(17) . . ?
O9 S3 O11 113.32(19) . . ?
O9 S3 O10 111.97(19) . . ?
O11 S3 O10 110.71(18) . . ?
O9 S3 C17 107.14(19) . . ?
O11 S3 C17 106.7(2) . . ?
O10 S3 C17 106.54(18) . . ?
O14 S4 O12 114.76(19) . . ?
O14 S4 O13 111.60(18) . . ?
O12 S4 O13 110.2(2) . . ?
O14 S4 C24 107.4(2) . . ?
O12 S4 C24 106.99(19) . . ?
O13 S4 C24 105.23(18) . . ?
C35 P1 C41 112.4(2) . . ?
C35 P1 C29 108.7(2) . . ?
C41 P1 C29 109.4(2) . . ?
C35 P1 C47 106.8(2) . . ?
C41 P1 C47 108.4(2) . . ?
C29 P1 C47 111.1(2) . . ?
C53 P2 C65 108.3(2) . . ?
C53 P2 C59 113.9(2) . . ?
C65 P2 C59 109.4(2) . . ?
C53 P2 C71 106.7(2) . . ?
C65 P2 C71 109.9(2) . . ?
C59 P2 C71 108.6(2) . . ?
S1 O3 U1 149.55(17) . . ?
S2 O6 U1 144.65(18) . 1_565 ?
C4 O15 H15 99.3 . . ?
C13 O16 H16 114.5 . . ?
C20 O17 H17 110.2 . . ?
C27 O18 H18 114.4 . . ?
U1 O19 H19A 128.8 . . ?
U1 O19 H19B 134.3 . . ?
H19A O19 H19B 96.3 . . ?
U1 O20 H20A 125.5 . . ?
U1 O20 H20B 126.3 . . ?
H20A O20 H20B 96.4 . . ?
U1 O21 H21A 112.6 . . ?
U1 O21 H21B 132.3 . . ?
H21A O21 H21B 103.1 . . ?
H22A O22 H22B 89.0 . . ?
H23A O23 H23B 116.2 . . ?
H24A O24 H24B 108.9 . . ?
H25A O25 H25B 98.1 . . ?
H26A O26 H26B 112.2 . . ?
H27A O27 H27B 119.5 . . ?
C6 C1 C2 120.9(4) . . ?
C6 C1 S1 118.8(3) . . ?
C2 C1 S1 120.3(3) . . ?
C1 C2 C3 120.3(4) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C2 C3 C4 117.6(4) . . ?
C2 C3 C7 118.6(4) . . ?
C4 C3 C7 123.8(4) . . ?
O15 C4 C5 117.3(3) . . ?
O15 C4 C3 120.2(3) . . ?
C5 C4 C3 122.5(4) . . ?
C6 C5 C4 118.0(4) . . ?
C6 C5 C28 119.7(3) . . ?
C4 C5 C28 122.2(4) . . ?
C1 C6 C5 120.6(4) . . ?
C1 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C8 C7 C3 113.6(4) . . ?
C8 C7 H7A 108.8 . . ?
C3 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
C3 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C9 C8 C13 117.8(4) . . ?
C9 C8 C7 121.3(4) . . ?
C13 C8 C7 120.9(4) . . ?
C10 C9 C8 120.3(4) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 121.1(4) . . ?
C9 C10 S2 121.4(3) . . ?
C11 C10 S2 117.1(3) . . ?
C10 C11 C12 120.2(4) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 118.5(4) . . ?
C11 C12 C14 119.7(4) . . ?
C13 C12 C14 121.7(4) . . ?
O16 C13 C12 120.1(4) . . ?
O16 C13 C8 117.8(4) . . ?
C12 C13 C8 122.0(4) . . ?
C12 C14 C15 111.0(3) . . ?
C12 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
C12 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C20 118.2(4) . . ?
C16 C15 C14 120.9(4) . . ?
C20 C15 C14 120.9(4) . . ?
C15 C16 C17 120.7(4) . . ?
C15 C16 H16A 119.7 . . ?
C17 C16 H16A 119.7 . . ?
C16 C17 C18 120.1(4) . . ?
C16 C17 S3 119.3(3) . . ?
C18 C17 S3 120.4(3) . . ?
C17 C18 C19 121.1(4) . . ?
C17 C18 H18A 119.5 . . ?
C19 C18 H18A 119.5 . . ?
C18 C19 C20 117.6(4) . . ?
C18 C19 C21 120.1(4) . . ?
C20 C19 C21 122.4(4) . . ?
O17 C20 C15 117.6(4) . . ?
O17 C20 C19 120.1(4) . . ?
C15 C20 C19 122.3(4) . . ?
C19 C21 C22 111.2(3) . . ?
C19 C21 H21C 109.4 . . ?
C22 C21 H21C 109.4 . . ?
C19 C21 H21D 109.4 . . ?
C22 C21 H21D 109.4 . . ?
H21C C21 H21D 108.0 . . ?
C27 C22 C23 118.6(4) . . ?
C27 C22 C21 122.2(4) . . ?
C23 C22 C21 119.0(4) . . ?
C24 C23 C22 120.1(4) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C25 C24 C23 120.3(4) . . ?
C25 C24 S4 121.8(3) . . ?
C23 C24 S4 117.9(4) . . ?
C24 C25 C26 121.5(4) . . ?
C24 C25 H25 119.2 . . ?
C26 C25 H25 119.2 . . ?
C25 C26 C27 117.1(4) . . ?
C25 C26 C28 121.3(4) . . ?
C27 C26 C28 121.5(4) . . ?
C22 C27 O18 117.5(3) . . ?
C22 C27 C26 122.4(4) . . ?
O18 C27 C26 120.1(4) . . ?
C26 C28 C5 110.9(4) . . ?
C26 C28 H28A 109.5 . . ?
C5 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C5 C28 H28B 109.5 . . ?
H28A C28 H28B 108.0 . . ?
C30 C29 C34 120.5(4) . . ?
C30 C29 P1 117.2(4) . . ?
C34 C29 P1 122.0(4) . . ?
C29 C30 C31 119.4(5) . . ?
C29 C30 H30 120.3 . . ?
C31 C30 H30 120.3 . . ?
C32 C31 C30 119.3(5) . . ?
C32 C31 H31 120.3 . . ?
C30 C31 H31 120.3 . . ?
C33 C32 C31 121.4(5) . . ?
C33 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C32 C33 C34 119.3(5) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 H33 120.4 . . ?
C29 C34 C33 120.0(5) . . ?
C29 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C36 C35 C40 119.7(4) . . ?
C36 C35 P1 121.3(3) . . ?
C40 C35 P1 119.0(3) . . ?
C37 C36 C35 119.7(4) . . ?
C37 C36 H36 120.2 . . ?
C35 C36 H36 120.2 . . ?
C36 C37 C38 120.4(4) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C39 C38 C37 120.2(4) . . ?
C39 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
C40 C39 C38 120.1(4) . . ?
C40 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
C39 C40 C35 119.9(4) . . ?
C39 C40 H40 120.0 . . ?
C35 C40 H40 120.0 . . ?
C42 C41 C46 119.9(5) . . ?
C42 C41 P1 120.3(4) . . ?
C46 C41 P1 119.7(3) . . ?
C43 C42 C41 119.5(5) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C44 C43 C42 121.1(5) . . ?
C44 C43 H43 119.5 . . ?
C42 C43 H43 119.5 . . ?
C43 C44 C45 119.3(5) . . ?
C43 C44 H44 120.3 . . ?
C45 C44 H44 120.3 . . ?
C46 C45 C44 119.9(5) . . ?
C46 C45 H45 120.1 . . ?
C44 C45 H45 120.1 . . ?
C45 C46 C41 120.2(4) . . ?
C45 C46 H46 119.9 . . ?
C41 C46 H46 119.9 . . ?
C52 C47 C48 121.4(4) . . ?
C52 C47 P1 120.9(4) . . ?
C48 C47 P1 117.7(4) . . ?
C47 C48 C49 119.3(4) . . ?
C47 C48 H48 120.3 . . ?
C49 C48 H48 120.3 . . ?
C50 C49 C48 119.7(5) . . ?
C50 C49 H49 120.1 . . ?
C48 C49 H49 120.1 . . ?
C51 C50 C49 119.9(5) . . ?
C51 C50 H50 120.1 . . ?
C49 C50 H50 120.1 . . ?
C50 C51 C52 121.4(5) . . ?
C50 C51 H51 119.3 . . ?
C52 C51 H51 119.3 . . ?
C47 C52 C51 118.2(5) . . ?
C47 C52 H52 120.9 . . ?
C51 C52 H52 120.9 . . ?
C58 C53 C54 119.0(5) . . ?
C58 C53 P2 119.5(4) . . ?
C54 C53 P2 121.3(4) . . ?
C55 C54 C53 119.7(6) . . ?
C55 C54 H54 120.2 . . ?
C53 C54 H54 120.2 . . ?
C56 C55 C54 120.3(5) . . ?
C56 C55 H55 119.9 . . ?
C54 C55 H55 119.9 . . ?
C57 C56 C55 120.9(6) . . ?
C57 C56 H56 119.5 . . ?
C55 C56 H56 119.5 . . ?
C56 C57 C58 119.6(6) . . ?
C56 C57 H57 120.2 . . ?
C58 C57 H57 120.2 . . ?
C53 C58 C57 120.4(5) . . ?
C53 C58 H58 119.8 . . ?
C57 C58 H58 119.8 . . ?
C64 C59 C60 119.4(5) . . ?
C64 C59 P2 121.0(3) . . ?
C60 C59 P2 119.6(4) . . ?
C61 C60 C59 119.7(5) . . ?
C61 C60 H60 120.2 . . ?
C59 C60 H60 120.2 . . ?
C60 C61 C62 120.5(5) . . ?
C60 C61 H61 119.8 . . ?
C62 C61 H61 119.8 . . ?
C63 C62 C61 119.5(5) . . ?
C63 C62 H62 120.2 . . ?
C61 C62 H62 120.2 . . ?
C62 C63 C64 120.9(5) . . ?
C62 C63 H63 119.6 . . ?
C64 C63 H63 119.6 . . ?
C63 C64 C59 119.9(4) . . ?
C63 C64 H64 120.0 . . ?
C59 C64 H64 120.0 . . ?
C66 C65 C70 120.0(4) . . ?
C66 C65 P2 121.4(4) . . ?
C70 C65 P2 118.6(3) . . ?
C65 C66 C67 119.2(5) . . ?
C65 C66 H66 120.4 . . ?
C67 C66 H66 120.4 . . ?
C68 C67 C66 121.1(4) . . ?
C68 C67 H67 119.5 . . ?
C66 C67 H67 119.5 . . ?
C67 C68 C69 119.3(4) . . ?
C67 C68 H68 120.4 . . ?
C69 C68 H68 120.4 . . ?
C70 C69 C68 120.8(5) . . ?
C70 C69 H69 119.6 . . ?
C68 C69 H69 119.6 . . ?
C69 C70 C65 119.6(4) . . ?
C69 C70 H70 120.2 . . ?
C65 C70 H70 120.2 . . ?
C72 C71 C76 119.7(4) . . ?
C72 C71 P2 120.8(3) . . ?
C76 C71 P2 119.4(3) . . ?
C71 C72 C73 119.6(4) . . ?
C71 C72 H72 120.2 . . ?
C73 C72 H72 120.2 . . ?
C74 C73 C72 120.4(4) . . ?
C74 C73 H73 119.8 . . ?
C72 C73 H73 119.8 . . ?
C75 C74 C73 120.1(4) . . ?
C75 C74 H74 119.9 . . ?
C73 C74 H74 119.9 . . ?
C74 C75 C76 120.2(4) . . ?
C74 C75 H75 119.9 . . ?
C76 C75 H75 119.9 . . ?
C75 C76 C71 120.0(4) . . ?
C75 C76 H76 120.0 . . ?
C71 C76 H76 120.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O15 H15 O16 0.91 1.99 2.677(4) 131.9 .
O16 H16 O17 0.86 1.88 2.690(4) 157.3 .
O17 H17 O18 0.84 1.90 2.733(4) 168.2 .
O18 H18 O15 0.83 1.88 2.699(4) 169.7 .
O19 H19A O23 0.85 1.78 2.601(4) 163.3 .
O19 H19B O28 0.90 1.76 2.611(4) 157.7 .
O20 H20A O13 0.92 1.80 2.657(4) 154.1 1_655
O20 H20B O24 0.82 1.78 2.592(4) 171.9 .
O21 H21A O4 0.91 1.89 2.766(4) 162.0 .
O21 H21B O13 0.99 1.94 2.751(4) 137.5 1_655
O22 H22A O5 0.98 1.97 2.898(4) 158.0 .
O22 H22B O14 0.80 2.14 2.794(5) 138.7 .
O23 H23A O7 0.98 1.88 2.792(5) 153.2 1_545
O23 H23B O11 0.98 1.76 2.662(4) 151.1 1_545
O24 H24A O8 0.99 1.87 2.811(4) 158.1 1_545
O24 H24B O10 0.96 1.85 2.803(4) 172.8 1_645
O25 H25A O9 0.98 1.90 2.851(5) 164.8 1_655
O25 H25B O29 0.94 2.06 2.746(5) 129.0 1_655
O26 H26A O10 0.97 1.84 2.800(4) 168.5 .
O26 H26B O22 0.91 1.88 2.775(5) 169.6 1_565
O27 H27A O29 0.86 2.21 2.794(6) 125.3 .
O27 H27B O32 0.95 1.88 2.822(4) 173.3 1_455
C11 H11 O19 0.95 2.60 3.509(5) 160.0 1_565
C30 H30 O33 0.95 2.14 2.995(8) 149.6 .
C42 H42 O11 0.95 2.54 3.236(5) 130.1 .
C48 H48 O5 0.95 2.31 3.253(6) 169.2 .
C54 H54 O7 0.95 2.57 3.406(6) 147.6 .
C60 H60 O7 0.95 2.35 3.234(6) 154.9 .

_refine_diff_density_max         1.580
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.114

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1893016'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2019-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H34 N4 Ni O13 S2 U'
_chemical_formula_weight         947.41

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.8537(2)
_cell_length_b                   15.8019(6)
_cell_length_c                   20.3332(7)
_cell_angle_alpha                90
_cell_angle_beta                 99.894(2)
_cell_angle_gamma                90
_cell_volume                     3118.94(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    155921
_cell_measurement_theta_min      3.28
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.018
_exptl_crystal_F_000             1848
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    5.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_T_max  0.619
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and ten ω scans with 2° steps (601 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            155921
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.284
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5902
_reflns_number_gt                5292
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. The free water molecule is disordered over two sites which
 have been refined with occupancy parameters constrained to sum to 
 unity and restraints on displacement parameters. All non-hydrogen
 atoms were refined with anisotropic displacement parameters. The H
 atoms of the water molecule were not found. The C-bound H atoms 
 were introduced at calculated positions and were treated as riding
 atoms with an isotropic displacement parameter equal to 1.2 times
 that of the parent atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0390P)²+3.2241P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5902
_refine_ls_number_parameters     416
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0688
_refine_ls_wR_factor_gt          0.0670
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.004
_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_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 0.44124(2) 0.84773(2) 0.57318(2) 0.01611(6) Uani 1 1 d . . . . .
Ni1 Ni 0.17306(5) 0.64657(3) 0.36644(2) 0.01684(11) Uani 1 1 d . . . . .
S1 S 0.34277(11) 0.64516(6) 0.63358(5) 0.0260(2) Uani 1 1 d . . . . .
S2 S 0.67419(9) 0.93559(6) 0.71457(4) 0.01830(19) Uani 1 1 d . . . . .
O1 O 0.3059(3) 0.89204(18) 0.60731(13) 0.0253(6) Uani 1 1 d . . . . .
O2 O 0.5800(3) 0.80474(18) 0.53959(13) 0.0245(6) Uani 1 1 d . . . . .
O3 O 0.2849(3) 0.75672(17) 0.50820(12) 0.0212(6) Uani 1 1 d . . . . .
O4 O 0.1011(3) 0.69060(17) 0.45240(13) 0.0215(6) Uani 1 1 d . . . . .
O5 O 0.4298(3) 0.72200(17) 0.63886(13) 0.0241(6) Uani 1 1 d . . . . .
O6 O 0.3484(3) 0.59754(18) 0.57337(14) 0.0300(7) Uani 1 1 d . . . . .
O7 O 0.3712(4) 0.5963(2) 0.69400(15) 0.0438(9) Uani 1 1 d . . . . .
O8 O 0.5378(3) 0.98305(17) 0.57491(13) 0.0213(6) Uani 1 1 d . . . . .
O9 O 0.6412(3) 1.08975(18) 0.53281(13) 0.0280(6) Uani 1 1 d . . . . .
O10 O 0.5952(3) 0.86489(17) 0.67823(13) 0.0219(6) Uani 1 1 d . . . . .
O11 O 0.7461(2) 0.90440(17) 0.77891(12) 0.0200(6) Uani 1 1 d . . . . .
O12 O 0.5918(3) 1.00948(17) 0.71964(13) 0.0216(6) Uani 1 1 d . . . . .
O13A O 0.7151(10) 0.8815(6) 0.4342(4) 0.115(3) Uani 0.690(9) 1 d . U P . .
O13B O 0.678(2) 0.9106(11) 0.3181(8) 0.100(5) Uani 0.310(9) 1 d . U P . .
N1 N 0.0323(3) 0.7234(2) 0.30698(16) 0.0237(7) Uani 1 1 d . . . . .
H1 H 0.0316 0.7168 0.2588 0.028 Uiso 1 1 d R U . . .
N2 N 0.3101(3) 0.7445(2) 0.36517(15) 0.0201(7) Uani 1 1 d . . . . .
H2 H 0.3095 0.7759 0.4069 0.024 Uiso 1 1 d R U . . .
N3 N 0.3149(3) 0.5694(2) 0.42434(16) 0.0253(7) Uani 1 1 d . . . . .
H3 H 0.3376 0.5901 0.4686 0.030 Uiso 1 1 d R U . . .
N4 N 0.0366(3) 0.5456(2) 0.36599(16) 0.0282(8) Uani 1 1 d . . . . .
H4 H 0.0366 0.5211 0.3227 0.034 Uiso 1 1 d R U . . .
C1 C 0.1671(4) 0.7224(2) 0.50457(18) 0.0180(8) Uani 1 1 d . . . . .
C2 C 0.1021(4) 0.7180(3) 0.56611(19) 0.0223(8) Uani 1 1 d . . . . .
C3 C 0.1704(4) 0.6842(3) 0.6259(2) 0.0278(9) Uani 1 1 d . . . . .
C4 C 0.1061(5) 0.6733(4) 0.6807(2) 0.0427(13) Uani 1 1 d . . . . .
H4A H 0.1539 0.6478 0.7203 0.051 Uiso 1 1 calc R U . . .
C5 C -0.0266(5) 0.6995(4) 0.6772(3) 0.0548(16) Uani 1 1 d . . . . .
H5 H -0.0714 0.6920 0.7146 0.066 Uiso 1 1 calc R U . . .
C6 C -0.0976(5) 0.7374(4) 0.6191(3) 0.0507(15) Uani 1 1 d . . . . .
H6 H -0.1885 0.7581 0.6180 0.061 Uiso 1 1 calc R U . . .
C7 C -0.0339(4) 0.7448(3) 0.5623(2) 0.0365(11) Uani 1 1 d . . . . .
H7 H -0.0831 0.7678 0.5220 0.044 Uiso 1 1 calc R U . . .
C8 C 0.6437(4) 1.0250(2) 0.56852(18) 0.0210(8) Uani 1 1 d . . . . .
C9 C 0.7829(4) 0.9993(2) 0.60559(18) 0.0186(8) Uani 1 1 d . . . . .
C10 C 0.8075(4) 0.9608(2) 0.66876(18) 0.0187(7) Uani 1 1 d . . . . .
C11 C 0.9418(4) 0.9442(3) 0.6996(2) 0.0251(9) Uani 1 1 d . . . . .
H11 H 0.9589 0.9204 0.7431 0.030 Uiso 1 1 calc R U . . .
C12 C 1.0511(4) 0.9622(3) 0.6671(2) 0.0316(10) Uani 1 1 d . . . . .
H12 H 1.1426 0.9497 0.6883 0.038 Uiso 1 1 calc R U . . .
C13 C 1.0284(4) 0.9980(3) 0.6049(2) 0.0301(10) Uani 1 1 d . . . . .
H13 H 1.1037 1.0093 0.5826 0.036 Uiso 1 1 calc R U . . .
C14 C 0.8949(4) 1.0176(3) 0.57419(19) 0.0241(9) Uani 1 1 d . . . . .
H14 H 0.8797 1.0437 0.5315 0.029 Uiso 1 1 calc R U . . .
C15 C 0.0932(4) 0.8094(3) 0.3158(2) 0.0300(9) Uani 1 1 d . . . . .
H15A H 0.0823 0.8327 0.3598 0.036 Uiso 1 1 calc R U . . .
H15B H 0.0465 0.8478 0.2805 0.036 Uiso 1 1 calc R U . . .
C16 C 0.2436(4) 0.8015(3) 0.3113(2) 0.0262(9) Uani 1 1 d . . . . .
H16A H 0.2540 0.7782 0.2673 0.031 Uiso 1 1 calc R U . . .
H16B H 0.2879 0.8579 0.3163 0.031 Uiso 1 1 calc R U . . .
C17 C 0.4533(4) 0.7226(3) 0.3606(2) 0.0303(10) Uani 1 1 d . . . . .
H17A H 0.5096 0.7748 0.3648 0.036 Uiso 1 1 calc R U . . .
H17B H 0.4560 0.6977 0.3162 0.036 Uiso 1 1 calc R U . . .
C18 C 0.5157(4) 0.6600(3) 0.4146(2) 0.0308(10) Uani 1 1 d . . . . .
H18A H 0.6158 0.6561 0.4142 0.037 Uiso 1 1 calc R U . . .
H18B H 0.5045 0.6834 0.4585 0.037 Uiso 1 1 calc R U . . .
C19 C 0.4566(4) 0.5707(3) 0.4093(2) 0.0318(10) Uani 1 1 d . . . . .
H19A H 0.4556 0.5489 0.3635 0.038 Uiso 1 1 calc R U . . .
H19B H 0.5161 0.5331 0.4409 0.038 Uiso 1 1 calc R U . . .
C20 C 0.2529(5) 0.4834(3) 0.4197(2) 0.0348(10) Uani 1 1 d . . . . .
H20A H 0.2985 0.4477 0.4572 0.042 Uiso 1 1 calc R U . . .
H20B H 0.2648 0.4561 0.3773 0.042 Uiso 1 1 calc R U . . .
C21 C 0.1016(5) 0.4925(3) 0.4228(2) 0.0379(11) Uani 1 1 d . . . . .
H21A H 0.0573 0.4361 0.4203 0.045 Uiso 1 1 calc R U . . .
H21B H 0.0900 0.5194 0.4654 0.045 Uiso 1 1 calc R U . . .
C22 C -0.1078(4) 0.5691(3) 0.3685(2) 0.0349(11) Uani 1 1 d . . . . .
H22A H -0.1121 0.5964 0.4120 0.042 Uiso 1 1 calc R U . . .
H22B H -0.1650 0.5173 0.3653 0.042 Uiso 1 1 calc R U . . .
C23 C -0.1661(4) 0.6290(3) 0.3127(2) 0.0390(12) Uani 1 1 d . . . . .
H23A H -0.2674 0.6310 0.3098 0.047 Uiso 1 1 calc R U . . .
H23B H -0.1473 0.6052 0.2702 0.047 Uiso 1 1 calc R U . . .
C24 C -0.1115(4) 0.7187(3) 0.3192(2) 0.0343(11) Uani 1 1 d . . . . .
H24A H -0.1707 0.7555 0.2868 0.041 Uiso 1 1 calc R U . . .
H24B H -0.1153 0.7401 0.3646 0.041 Uiso 1 1 calc R U . . .


_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 O1 1.751(3) . ?
U1 O2 1.766(3) . ?
U1 O8 2.338(3) . ?
U1 O3 2.342(2) . ?
U1 O9 2.383(3) 3_676 ?
U1 O5 2.407(3) . ?
U1 O10 2.413(3) . ?
Ni1 N2 2.057(3) . ?
Ni1 N3 2.064(3) . ?
Ni1 N1 2.070(3) . ?
Ni1 N4 2.086(3) . ?
Ni1 O4 2.113(3) . ?
Ni1 O11 2.185(3) 4_575 ?
S1 O7 1.437(3) . ?
S1 O6 1.446(3) . ?
S1 O5 1.480(3) . ?
S1 C3 1.789(4) . ?
S2 O12 1.436(3) . ?
S2 O11 1.462(3) . ?
S2 O10 1.484(3) . ?
S2 C10 1.781(4) . ?
O3 C1 1.271(4) . ?
O4 C1 1.251(4) . ?
O8 C8 1.262(5) . ?
O9 C8 1.252(5) . ?
O9 U1 2.383(3) 3_676 ?
O11 Ni1 2.185(3) 4_676 ?
N1 C24 1.482(5) . ?
N1 C15 1.484(5) . ?
N1 H1 0.9842 . ?
N2 C17 1.471(5) . ?
N2 C16 1.481(5) . ?
N2 H2 0.9839 . ?
N3 C19 1.480(5) . ?
N3 C20 1.487(5) . ?
N3 H3 0.9488 . ?
N4 C21 1.480(6) . ?
N4 C22 1.481(6) . ?
N4 H4 0.9607 . ?
C1 C2 1.502(5) . ?
C2 C3 1.391(6) . ?
C2 C7 1.395(6) . ?
C3 C4 1.384(6) . ?
C4 C5 1.361(8) . ?
C4 H4A 0.9500 . ?
C5 C6 1.400(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.411(7) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.503(5) . ?
C9 C14 1.397(5) . ?
C9 C10 1.404(5) . ?
C10 C11 1.389(5) . ?
C11 C12 1.386(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.369(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.390(6) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.506(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.527(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.522(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.509(7) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.513(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.515(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?

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 U1 O2 178.80(13) . . ?
O1 U1 O8 87.94(11) . . ?
O2 U1 O8 91.01(11) . . ?
O1 U1 O3 89.85(11) . . ?
O2 U1 O3 91.34(11) . . ?
O8 U1 O3 142.79(9) . . ?
O1 U1 O9 91.62(12) . 3_676 ?
O2 U1 O9 88.62(11) . 3_676 ?
O8 U1 O9 73.09(9) . 3_676 ?
O3 U1 O9 69.85(9) . 3_676 ?
O1 U1 O5 89.93(11) . . ?
O2 U1 O5 90.58(11) . . ?
O8 U1 O5 143.52(9) . . ?
O3 U1 O5 73.57(9) . . ?
O9 U1 O5 143.38(9) 3_676 . ?
O1 U1 O10 90.56(11) . . ?
O2 U1 O10 88.57(11) . . ?
O8 U1 O10 72.04(9) . . ?
O3 U1 O10 145.14(9) . . ?
O9 U1 O10 144.95(9) 3_676 . ?
O5 U1 O10 71.57(9) . . ?
N2 Ni1 N3 94.02(13) . . ?
N2 Ni1 N1 85.81(13) . . ?
N3 Ni1 N1 179.02(13) . . ?
N2 Ni1 N4 178.53(13) . . ?
N3 Ni1 N4 85.59(14) . . ?
N1 Ni1 N4 94.55(14) . . ?
N2 Ni1 O4 94.40(11) . . ?
N3 Ni1 O4 90.76(12) . . ?
N1 Ni1 O4 90.21(11) . . ?
N4 Ni1 O4 87.02(12) . . ?
N2 Ni1 O11 87.62(11) . 4_575 ?
N3 Ni1 O11 87.77(11) . 4_575 ?
N1 Ni1 O11 91.26(11) . 4_575 ?
N4 Ni1 O11 90.95(12) . 4_575 ?
O4 Ni1 O11 177.59(10) . 4_575 ?
O7 S1 O6 114.45(19) . . ?
O7 S1 O5 110.70(17) . . ?
O6 S1 O5 112.49(17) . . ?
O7 S1 C3 107.6(2) . . ?
O6 S1 C3 106.23(18) . . ?
O5 S1 C3 104.68(19) . . ?
O12 S2 O11 113.75(16) . . ?
O12 S2 O10 113.14(16) . . ?
O11 S2 O10 108.89(15) . . ?
O12 S2 C10 109.45(17) . . ?
O11 S2 C10 104.81(16) . . ?
O10 S2 C10 106.21(17) . . ?
C1 O3 U1 143.1(2) . . ?
C1 O4 Ni1 129.4(2) . . ?
S1 O5 U1 135.95(15) . . ?
C8 O8 U1 145.2(3) . . ?
C8 O9 U1 146.4(2) . 3_676 ?
S2 O10 U1 136.17(15) . . ?
S2 O11 Ni1 132.55(15) . 4_676 ?
C24 N1 C15 113.8(3) . . ?
C24 N1 Ni1 115.9(3) . . ?
C15 N1 Ni1 104.5(2) . . ?
C24 N1 H1 108.6 . . ?
C15 N1 H1 98.7 . . ?
Ni1 N1 H1 114.1 . . ?
C17 N2 C16 113.9(3) . . ?
C17 N2 Ni1 117.5(3) . . ?
C16 N2 Ni1 105.0(2) . . ?
C17 N2 H2 108.7 . . ?
C16 N2 H2 105.3 . . ?
Ni1 N2 H2 105.5 . . ?
C19 N3 C20 113.1(3) . . ?
C19 N3 Ni1 116.3(3) . . ?
C20 N3 Ni1 105.9(2) . . ?
C19 N3 H3 96.6 . . ?
C20 N3 H3 113.8 . . ?
Ni1 N3 H3 111.3 . . ?
C21 N4 C22 113.9(3) . . ?
C21 N4 Ni1 103.7(3) . . ?
C22 N4 Ni1 115.5(3) . . ?
C21 N4 H4 114.7 . . ?
C22 N4 H4 106.5 . . ?
Ni1 N4 H4 102.2 . . ?
O4 C1 O3 123.9(3) . . ?
O4 C1 C2 117.0(3) . . ?
O3 C1 C2 119.2(3) . . ?
C3 C2 C7 118.7(4) . . ?
C3 C2 C1 122.3(3) . . ?
C7 C2 C1 118.9(4) . . ?
C4 C3 C2 122.2(4) . . ?
C4 C3 S1 116.5(4) . . ?
C2 C3 S1 121.2(3) . . ?
C5 C4 C3 119.2(5) . . ?
C5 C4 H4A 120.4 . . ?
C3 C4 H4A 120.4 . . ?
C4 C5 C6 120.7(4) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C7 119.9(4) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C2 C7 C6 119.2(5) . . ?
C2 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
O9 C8 O8 123.7(3) . . ?
O9 C8 C9 115.9(3) . . ?
O8 C8 C9 120.4(3) . . ?
C14 C9 C10 118.8(3) . . ?
C14 C9 C8 116.1(3) . . ?
C10 C9 C8 125.1(3) . . ?
C11 C10 C9 119.7(3) . . ?
C11 C10 S2 117.0(3) . . ?
C9 C10 S2 123.2(3) . . ?
C12 C11 C10 120.3(4) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C13 C12 C11 120.5(4) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 119.9(4) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C9 120.6(4) . . ?
C13 C14 H14 119.7 . . ?
C9 C14 H14 119.7 . . ?
N1 C15 C16 107.4(3) . . ?
N1 C15 H15A 110.2 . . ?
C16 C15 H15A 110.2 . . ?
N1 C15 H15B 110.2 . . ?
C16 C15 H15B 110.2 . . ?
H15A C15 H15B 108.5 . . ?
N2 C16 C15 108.7(3) . . ?
N2 C16 H16A 109.9 . . ?
C15 C16 H16A 109.9 . . ?
N2 C16 H16B 109.9 . . ?
C15 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
N2 C17 C18 112.3(3) . . ?
N2 C17 H17A 109.1 . . ?
C18 C17 H17A 109.1 . . ?
N2 C17 H17B 109.1 . . ?
C18 C17 H17B 109.1 . . ?
H17A C17 H17B 107.9 . . ?
C19 C18 C17 116.5(3) . . ?
C19 C18 H18A 108.2 . . ?
C17 C18 H18A 108.2 . . ?
C19 C18 H18B 108.2 . . ?
C17 C18 H18B 108.2 . . ?
H18A C18 H18B 107.3 . . ?
N3 C19 C18 111.2(3) . . ?
N3 C19 H19A 109.4 . . ?
C18 C19 H19A 109.4 . . ?
N3 C19 H19B 109.4 . . ?
C18 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
N3 C20 C21 107.9(3) . . ?
N3 C20 H20A 110.1 . . ?
C21 C20 H20A 110.1 . . ?
N3 C20 H20B 110.1 . . ?
C21 C20 H20B 110.1 . . ?
H20A C20 H20B 108.4 . . ?
N4 C21 C20 108.7(4) . . ?
N4 C21 H21A 110.0 . . ?
C20 C21 H21A 110.0 . . ?
N4 C21 H21B 110.0 . . ?
C20 C21 H21B 110.0 . . ?
H21A C21 H21B 108.3 . . ?
N4 C22 C23 112.0(3) . . ?
N4 C22 H22A 109.2 . . ?
C23 C22 H22A 109.2 . . ?
N4 C22 H22B 109.2 . . ?
C23 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C22 C23 C24 115.9(4) . . ?
C22 C23 H23A 108.3 . . ?
C24 C23 H23A 108.3 . . ?
C22 C23 H23B 108.3 . . ?
C24 C23 H23B 108.3 . . ?
H23A C23 H23B 107.4 . . ?
N1 C24 C23 111.6(4) . . ?
N1 C24 H24A 109.3 . . ?
C23 C24 H24A 109.3 . . ?
N1 C24 H24B 109.3 . . ?
C23 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O10 0.98 2.26 3.121(4) 145.9 4_575
N2 H2 O3 0.98 2.14 2.967(4) 141.1 .
N2 H2 O9 0.98 2.46 3.324(4) 146.7 3_676
N3 H3 O6 0.95 2.12 3.024(4) 159.6 .
N4 H4 O12 0.96 2.31 3.234(4) 162.5 4_575
C15 H15B O7 0.99 2.41 3.358(5) 159.7 4_575
C16 H16B O12 0.99 2.57 3.507(5) 157.0 3_676
C18 H18B O2 0.99 2.55 3.397(5) 142.9 .
C19 H19A O11 0.99 2.56 3.097(5) 114.0 4_575
C19 H19B O6 0.99 2.50 3.264(5) 133.5 3_666
C22 H22A O4 0.99 2.59 3.102(5) 112.1 .

_refine_diff_density_max         1.394
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.126

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 1893019'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2019-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C69 H56 O21 P2 S3 U2'
_chemical_formula_weight         1855.31

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'
O O 0.0106 0.0060 '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'
U U -9.6767 9.6646 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   19.5550(8)
_cell_length_b                   19.7854(7)
_cell_length_c                   22.8580(8)
_cell_angle_alpha                67.635(3)
_cell_angle_beta                 65.121(2)
_cell_angle_gamma                60.589(2)
_cell_volume                     6817.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    345019
_cell_measurement_theta_min      2.06
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_F_000             3600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    4.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_T_max  0.673
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and ten ω scans with 2° steps (722 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            345019
_diffrn_reflns_av_unetI/netI     0.0816
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.055
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             25827
_reflns_number_gt                18227
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms were introduced at calculated
 positions and were treated as riding atoms with an isotropic displacement
 parameter equal to 1.2 times that of the parent atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0179P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         25827
_refine_ls_number_parameters     1748
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0639
_refine_ls_wR_factor_gt          0.0597
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_restrained_S_all      0.905
_refine_ls_shift/su_max          0.003
_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_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 1.08734(2) 0.31978(2) -0.14189(2) 0.01852(5) Uani 1 1 d . . . . .
U2 U 0.90245(2) 0.20259(2) 0.12396(2) 0.01832(5) Uani 1 1 d . . . . .
U3 U 0.59509(2) 0.28053(2) 0.36872(2) 0.01956(5) Uani 1 1 d . . . . .
U4 U 0.40172(2) 0.22347(2) 0.62278(2) 0.02167(5) Uani 1 1 d . . . . .
S1 S 0.72868(8) 0.38731(7) 0.09295(6) 0.0220(3) Uani 1 1 d . . . . .
S2 S 1.25910(7) 0.13174(7) -0.11220(6) 0.0227(3) Uani 1 1 d . . . . .
S3 S 1.05102(8) 0.49971(7) -0.27027(6) 0.0221(3) Uani 1 1 d . . . . .
S4 S 0.95148(8) 0.02741(7) 0.25573(6) 0.0219(3) Uani 1 1 d . . . . .
S5 S 0.52675(9) 0.01484(7) 0.65448(6) 0.0299(3) Uani 1 1 d . . . . .
S6 S 0.47990(8) 0.49292(7) 0.33957(6) 0.0226(3) Uani 1 1 d . . . . .
P1 P 0.11679(8) 0.14747(7) 0.40069(6) 0.0262(3) Uani 1 1 d . . . . .
P2 P 0.34086(8) 0.25435(7) 0.04249(6) 0.0216(3) Uani 1 1 d . . . . .
P3 P 0.32144(8) 0.78299(7) 0.03246(6) 0.0214(3) Uani 1 1 d . . . . .
P4 P 0.87383(8) 0.37962(7) 0.66380(6) 0.0242(3) Uani 1 1 d . . . . .
O1 O 1.12368(19) 0.36583(17) -0.11608(15) 0.0235(8) Uani 1 1 d . . . . .
O2 O 1.05372(19) 0.27183(17) -0.16861(14) 0.0221(8) Uani 1 1 d . . . . .
O3 O 0.92685(19) 0.25555(17) 0.15380(14) 0.0211(7) Uani 1 1 d . . . . .
O4 O 0.8757(2) 0.15187(17) 0.09364(15) 0.0242(8) Uani 1 1 d . . . . .
O5 O 0.65046(19) 0.27456(17) 0.41557(15) 0.0259(8) Uani 1 1 d . . . . .
O6 O 0.54121(19) 0.28329(17) 0.32157(14) 0.0226(8) Uani 1 1 d . . . . .
O7 O 0.4537(2) 0.22122(18) 0.67070(15) 0.0287(8) Uani 1 1 d . . . . .
O8 O 0.3466(2) 0.22833(18) 0.57585(15) 0.0280(8) Uani 1 1 d . . . . .
O9 O 0.95445(19) 0.37416(16) -0.06916(15) 0.0214(7) Uani 1 1 d . . . . .
O10 O 0.90747(18) 0.29424(17) 0.02104(14) 0.0201(7) Uani 1 1 d . . . . .
O11 O 0.77061(18) 0.30619(16) 0.12848(14) 0.0214(7) Uani 1 1 d . . . . .
O12 O 0.7257(2) 0.38738(18) 0.03051(15) 0.0258(8) Uani 1 1 d . . . . .
O13 O 0.65047(19) 0.42552(17) 0.13780(15) 0.0269(8) Uani 1 1 d . . . . .
O14 O 1.08336(18) 0.22790(16) -0.03865(14) 0.0204(7) Uani 1 1 d . . . . .
O15 O 1.03880(19) 0.15241(17) 0.05652(14) 0.0215(7) Uani 1 1 d . . . . .
O16 O 1.21736(19) 0.21167(17) -0.14920(15) 0.0239(8) Uani 1 1 d . . . . .
O17 O 1.2653(2) 0.13399(18) -0.05250(15) 0.0277(8) Uani 1 1 d . . . . .
O18 O 1.33572(18) 0.09059(17) -0.15664(15) 0.0246(8) Uani 1 1 d . . . . .
O19 O 1.18491(19) 0.32822(17) -0.25131(14) 0.0220(8) Uani 1 1 d . . . . .
O20 O 1.2909(2) 0.33812(17) -0.33786(15) 0.0284(8) Uani 1 1 d . . . . .
O21 O 1.02651(19) 0.44598(17) -0.20665(14) 0.0248(8) Uani 1 1 d . . . . .
O22 O 0.98865(19) 0.57994(17) -0.27315(15) 0.0268(8) Uani 1 1 d . . . . .
O23 O 1.0768(2) 0.46675(18) -0.32631(14) 0.0263(8) Uani 1 1 d . . . . .
O24 O 0.80337(19) 0.18697(17) 0.23121(14) 0.0218(8) Uani 1 1 d . . . . .
O25 O 0.70746(19) 0.17068(17) 0.32552(15) 0.0245(8) Uani 1 1 d . . . . .
O26 O 0.96894(19) 0.07841(17) 0.18886(14) 0.0225(8) Uani 1 1 d . . . . .
O27 O 0.92167(19) 0.06905(17) 0.30702(15) 0.0263(8) Uani 1 1 d . . . . .
O28 O 1.02134(19) -0.04771(17) 0.26062(15) 0.0277(8) Uani 1 1 d . . . . .
O29 O 0.5728(2) 0.16620(17) 0.44163(15) 0.0271(8) Uani 1 1 d . . . . .
O30 O 0.5249(2) 0.16368(17) 0.54816(15) 0.0257(8) Uani 1 1 d . . . . .
O31 O 0.44505(19) 0.08235(17) 0.65641(15) 0.0266(8) Uani 1 1 d . . . . .
O32 O 0.5858(2) 0.03598(19) 0.65722(16) 0.0363(9) Uani 1 1 d . . . . .
O33 O 0.5163(2) -0.05474(19) 0.70297(15) 0.0407(10) Uani 1 1 d . . . . .
O34 O 0.47087(19) 0.34244(16) 0.44073(14) 0.0220(8) Uani 1 1 d . . . . .
O35 O 0.4265(2) 0.33496(18) 0.54836(15) 0.0322(9) Uani 1 1 d . . . . .
O36 O 0.55762(18) 0.42111(16) 0.33862(14) 0.0212(7) Uani 1 1 d . . . . .
O37 O 0.41803(19) 0.48033(17) 0.33117(14) 0.0246(8) Uani 1 1 d . . . . .
O38 O 0.4966(2) 0.56111(17) 0.29447(15) 0.0299(8) Uani 1 1 d . . . . .
O39 O 0.68513(19) 0.32800(17) 0.26358(14) 0.0244(8) Uani 1 1 d . . . . .
H39A H 0.7390 0.3079 0.2311 0.029 Uiso 1 1 d R U . . .
H39B H 0.6603 0.3672 0.2386 0.029 Uiso 1 1 d R U . . .
O40 O 0.30334(19) 0.17995(17) 0.72221(14) 0.0264(8) Uani 1 1 d . . . . .
H40A H 0.2656 0.2281 0.7350 0.032 Uiso 1 1 d R U . . .
H40B H 0.3227 0.1495 0.7552 0.032 Uiso 1 1 d R U . . .
O41 O 0.4063(2) 0.3892(2) 0.26684(17) 0.0417(10) Uani 1 1 d . . . . .
H41A H 0.4459 0.3404 0.2807 0.050 Uiso 1 1 d R U . . .
H41B H 0.4171 0.4120 0.2859 0.050 Uiso 1 1 d R U . . .
O42 O 1.0409(2) -0.0288(2) 0.38090(17) 0.0411(10) Uani 1 1 d . . . . .
H42A H 1.0017 0.0182 0.3583 0.049 Uiso 1 1 d R U . . .
H42B H 1.0806 -0.0576 0.3454 0.049 Uiso 1 1 d R U . . .
C1 C 0.9112(3) 0.3615(3) -0.0103(2) 0.0196(11) Uani 1 1 d . . . . .
C2 C 0.8649(3) 0.4288(2) 0.0240(2) 0.0188(11) Uani 1 1 d . . . . .
C3 C 0.7894(3) 0.4403(3) 0.0744(2) 0.0191(11) Uani 1 1 d . . . . .
C4 C 0.7550(3) 0.5015(3) 0.1071(2) 0.0236(11) Uani 1 1 d . . . . .
H4 H 0.7037 0.5099 0.1404 0.028 Uiso 1 1 calc R U . . .
C5 C 0.7956(3) 0.5502(3) 0.0913(2) 0.0262(12) Uani 1 1 d . . . . .
H5 H 0.7727 0.5908 0.1146 0.031 Uiso 1 1 calc R U . . .
C6 C 0.8693(3) 0.5398(3) 0.0416(2) 0.0263(12) Uani 1 1 d . . . . .
H6 H 0.8966 0.5736 0.0304 0.032 Uiso 1 1 calc R U . . .
C7 C 0.9033(3) 0.4795(2) 0.0081(2) 0.0219(11) Uani 1 1 d . . . . .
H7 H 0.9535 0.4729 -0.0263 0.026 Uiso 1 1 calc R U . . .
C8 C 1.0806(3) 0.1621(2) -0.0037(2) 0.0184(11) Uani 1 1 d . . . . .
C9 C 1.1236(3) 0.0918(3) -0.0344(2) 0.0196(11) Uani 1 1 d . . . . .
C10 C 1.1969(3) 0.0797(3) -0.0881(2) 0.0211(11) Uani 1 1 d . . . . .
C11 C 1.2268(3) 0.0172(3) -0.1185(2) 0.0241(12) Uani 1 1 d . . . . .
H11 H 1.2755 0.0090 -0.1546 0.029 Uiso 1 1 calc R U . . .
C12 C 1.1859(3) -0.0333(3) -0.0965(2) 0.0224(11) Uani 1 1 d . . . . .
H12 H 1.2058 -0.0746 -0.1183 0.027 Uiso 1 1 calc R U . . .
C13 C 1.1169(3) -0.0230(3) -0.0431(2) 0.0236(11) Uani 1 1 d . . . . .
H13 H 1.0897 -0.0580 -0.0274 0.028 Uiso 1 1 calc R U . . .
C14 C 1.0865(3) 0.0386(3) -0.0120(2) 0.0229(11) Uani 1 1 d . . . . .
H14 H 1.0393 0.0443 0.0254 0.027 Uiso 1 1 calc R U . . .
C15 C 1.2310(3) 0.3648(3) -0.2910(2) 0.0227(11) Uani 1 1 d . . . . .
C16 C 1.2164(3) 0.4424(3) -0.2811(2) 0.0211(11) Uani 1 1 d . . . . .
C17 C 1.1395(3) 0.5045(3) -0.2695(2) 0.0217(11) Uani 1 1 d . . . . .
C18 C 1.1312(3) 0.5732(3) -0.2600(2) 0.0248(12) Uani 1 1 d . . . . .
H18 H 1.0786 0.6152 -0.2516 0.030 Uiso 1 1 calc R U . . .
C19 C 1.1986(3) 0.5820(3) -0.2624(2) 0.0313(13) Uani 1 1 d . . . . .
H19 H 1.1921 0.6295 -0.2554 0.038 Uiso 1 1 calc R U . . .
C20 C 1.2761(3) 0.5205(3) -0.2751(2) 0.0308(13) Uani 1 1 d . . . . .
H20 H 1.3228 0.5258 -0.2772 0.037 Uiso 1 1 calc R U . . .
C21 C 1.2841(3) 0.4514(3) -0.2848(2) 0.0248(12) Uani 1 1 d . . . . .
H21 H 1.3369 0.4097 -0.2942 0.030 Uiso 1 1 calc R U . . .
C22 C 0.7664(3) 0.1448(3) 0.2775(2) 0.0199(11) Uani 1 1 d . . . . .
C23 C 0.7889(3) 0.0618(3) 0.2745(2) 0.0185(11) Uani 1 1 d . . . . .
C24 C 0.8698(3) 0.0058(3) 0.2626(2) 0.0214(11) Uani 1 1 d . . . . .
C25 C 0.8856(3) -0.0706(3) 0.2604(2) 0.0256(12) Uani 1 1 d . . . . .
H25 H 0.9401 -0.1099 0.2540 0.031 Uiso 1 1 calc R U . . .
C26 C 0.8226(3) -0.0891(3) 0.2676(2) 0.0294(13) Uani 1 1 d . . . . .
H26 H 0.8342 -0.1401 0.2638 0.035 Uiso 1 1 calc R U . . .
C27 C 0.7423(3) -0.0330(3) 0.2802(2) 0.0294(13) Uani 1 1 d . . . . .
H27 H 0.6990 -0.0462 0.2859 0.035 Uiso 1 1 calc R U . . .
C28 C 0.7253(3) 0.0409(3) 0.2846(2) 0.0240(12) Uani 1 1 d . . . . .
H28 H 0.6701 0.0784 0.2946 0.029 Uiso 1 1 calc R U . . .
C29 C 0.5555(3) 0.1304(3) 0.5007(2) 0.0218(11) Uani 1 1 d . . . . .
C30 C 0.5742(3) 0.0434(3) 0.5129(2) 0.0207(11) Uani 1 1 d . . . . .
C31 C 0.5637(3) -0.0092(3) 0.5756(2) 0.0218(11) Uani 1 1 d . . . . .
C32 C 0.5848(3) -0.0881(3) 0.5787(2) 0.0260(12) Uani 1 1 d . . . . .
H32 H 0.5777 -0.1235 0.6207 0.031 Uiso 1 1 calc R U . . .
C33 C 0.6160(3) -0.1170(3) 0.5219(2) 0.0273(12) Uani 1 1 d . . . . .
H33 H 0.6306 -0.1714 0.5252 0.033 Uiso 1 1 calc R U . . .
C34 C 0.6256(3) -0.0659(3) 0.4611(2) 0.0262(12) Uani 1 1 d . . . . .
H34 H 0.6464 -0.0847 0.4220 0.031 Uiso 1 1 calc R U . . .
C35 C 0.6048(3) 0.0130(3) 0.4571(2) 0.0232(11) Uani 1 1 d . . . . .
H35 H 0.6117 0.0477 0.4147 0.028 Uiso 1 1 calc R U . . .
C36 C 0.4402(3) 0.3732(3) 0.4896(2) 0.0227(11) Uani 1 1 d . . . . .
C37 C 0.4203(3) 0.4600(3) 0.4811(2) 0.0212(11) Uani 1 1 d . . . . .
C38 C 0.4393(3) 0.5131(3) 0.4207(2) 0.0205(11) Uani 1 1 d . . . . .
C39 C 0.4237(3) 0.5891(3) 0.4212(2) 0.0260(12) Uani 1 1 d . . . . .
H39 H 0.4380 0.6245 0.3808 0.031 Uiso 1 1 calc R U . . .
C40 C 0.3872(3) 0.6141(3) 0.4805(3) 0.0346(14) Uani 1 1 d . . . . .
H40 H 0.3762 0.6666 0.4801 0.041 Uiso 1 1 calc R U . . .
C41 C 0.3669(3) 0.5642(3) 0.5390(2) 0.0323(13) Uani 1 1 d . . . . .
H41 H 0.3418 0.5815 0.5793 0.039 Uiso 1 1 calc R U . . .
C42 C 0.3836(3) 0.4881(3) 0.5388(2) 0.0294(13) Uani 1 1 d . . . . .
H42 H 0.3694 0.4534 0.5797 0.035 Uiso 1 1 calc R U . . .
C43 C 0.1211(3) 0.1255(3) 0.3301(2) 0.0250(12) Uani 1 1 d . . . . .
C44 C 0.0598(3) 0.1706(3) 0.2986(3) 0.0369(14) Uani 1 1 d . . . . .
H44 H 0.0138 0.2149 0.3145 0.044 Uiso 1 1 calc R U . . .
C45 C 0.0660(4) 0.1507(3) 0.2437(3) 0.0440(16) Uani 1 1 d . . . . .
H45 H 0.0242 0.1816 0.2222 0.053 Uiso 1 1 calc R U . . .
C46 C 0.1317(4) 0.0872(4) 0.2206(3) 0.0474(16) Uani 1 1 d . . . . .
H46 H 0.1350 0.0744 0.1832 0.057 Uiso 1 1 calc R U . . .
C47 C 0.1944(4) 0.0406(3) 0.2509(3) 0.0419(15) Uani 1 1 d . . . . .
H47 H 0.2401 -0.0033 0.2343 0.050 Uiso 1 1 calc R U . . .
C48 C 0.1888(3) 0.0595(3) 0.3061(2) 0.0318(13) Uani 1 1 d . . . . .
H48 H 0.2306 0.0280 0.3275 0.038 Uiso 1 1 calc R U . . .
C49 C 0.0148(3) 0.2097(3) 0.4390(2) 0.0270(12) Uani 1 1 d . . . . .
C50 C -0.0200(3) 0.2896(3) 0.4066(2) 0.0354(14) Uani 1 1 d . . . . .
H50 H 0.0107 0.3106 0.3649 0.043 Uiso 1 1 calc R U . . .
C51 C -0.0989(3) 0.3371(3) 0.4358(3) 0.0388(14) Uani 1 1 d . . . . .
H51 H -0.1224 0.3908 0.4137 0.047 Uiso 1 1 calc R U . . .
C52 C -0.1442(3) 0.3081(3) 0.4964(3) 0.0382(14) Uani 1 1 d . . . . .
H52 H -0.1986 0.3417 0.5158 0.046 Uiso 1 1 calc R U . . .
C53 C -0.1106(3) 0.2302(3) 0.5290(3) 0.0349(13) Uani 1 1 d . . . . .
H53 H -0.1417 0.2104 0.5710 0.042 Uiso 1 1 calc R U . . .
C54 C -0.0312(3) 0.1808(3) 0.5004(2) 0.0279(12) Uani 1 1 d . . . . .
H54 H -0.0084 0.1271 0.5228 0.034 Uiso 1 1 calc R U . . .
C55 C 0.1500(3) 0.0557(3) 0.4579(2) 0.0237(11) Uani 1 1 d . . . . .
C56 C 0.1200(3) -0.0010(3) 0.4699(2) 0.0269(12) Uani 1 1 d . . . . .
H56 H 0.0854 0.0085 0.4459 0.032 Uiso 1 1 calc R U . . .
C57 C 0.1407(3) -0.0711(3) 0.5170(2) 0.0296(12) Uani 1 1 d . . . . .
H57 H 0.1206 -0.1098 0.5251 0.035 Uiso 1 1 calc R U . . .
C58 C 0.1909(3) -0.0845(3) 0.5521(2) 0.0294(13) Uani 1 1 d . . . . .
H58 H 0.2049 -0.1325 0.5844 0.035 Uiso 1 1 calc R U . . .
C59 C 0.2206(3) -0.0286(3) 0.5405(2) 0.0263(12) Uani 1 1 d . . . . .
H59 H 0.2546 -0.0381 0.5651 0.032 Uiso 1 1 calc R U . . .
C60 C 0.2013(3) 0.0408(3) 0.4934(2) 0.0256(12) Uani 1 1 d . . . . .
H60 H 0.2227 0.0786 0.4849 0.031 Uiso 1 1 calc R U . . .
C61 C 0.1817(3) 0.1998(3) 0.3762(2) 0.0280(12) Uani 1 1 d . . . . .
C62 C 0.2540(3) 0.1833(3) 0.3249(2) 0.0327(13) Uani 1 1 d . . . . .
H62 H 0.2702 0.1436 0.3025 0.039 Uiso 1 1 calc R U . . .
C63 C 0.3025(3) 0.2247(3) 0.3065(3) 0.0399(14) Uani 1 1 d . . . . .
H63 H 0.3513 0.2141 0.2707 0.048 Uiso 1 1 calc R U . . .
C64 C 0.2809(3) 0.2811(3) 0.3394(3) 0.0372(14) Uani 1 1 d . . . . .
H64 H 0.3144 0.3096 0.3260 0.045 Uiso 1 1 calc R U . . .
C65 C 0.2100(3) 0.2962(3) 0.3923(3) 0.0358(14) Uani 1 1 d . . . . .
H65 H 0.1956 0.3337 0.4162 0.043 Uiso 1 1 calc R U . . .
C66 C 0.1606(3) 0.2560(3) 0.4097(2) 0.0305(13) Uani 1 1 d . . . . .
H66 H 0.1115 0.2670 0.4452 0.037 Uiso 1 1 calc R U . . .
C67 C 0.3811(3) 0.2657(3) -0.0455(2) 0.0230(11) Uani 1 1 d . . . . .
C68 C 0.3773(3) 0.2193(3) -0.0764(2) 0.0287(12) Uani 1 1 d . . . . .
H68 H 0.3569 0.1790 -0.0504 0.034 Uiso 1 1 calc R U . . .
C69 C 0.4029(3) 0.2315(3) -0.1442(2) 0.0337(13) Uani 1 1 d . . . . .
H69 H 0.3997 0.1998 -0.1647 0.040 Uiso 1 1 calc R U . . .
C70 C 0.4334(3) 0.2898(3) -0.1826(2) 0.0316(13) Uani 1 1 d . . . . .
H70 H 0.4499 0.2987 -0.2294 0.038 Uiso 1 1 calc R U . . .
C71 C 0.4398(3) 0.3350(3) -0.1533(2) 0.0300(13) Uani 1 1 d . . . . .
H71 H 0.4620 0.3739 -0.1798 0.036 Uiso 1 1 calc R U . . .
C72 C 0.4135(3) 0.3234(3) -0.0852(2) 0.0246(12) Uani 1 1 d . . . . .
H72 H 0.4176 0.3548 -0.0650 0.030 Uiso 1 1 calc R U . . .
C73 C 0.2313(3) 0.2837(3) 0.0702(2) 0.0227(11) Uani 1 1 d . . . . .
C74 C 0.1833(3) 0.3301(3) 0.1175(2) 0.0292(12) Uani 1 1 d . . . . .
H74 H 0.2084 0.3459 0.1348 0.035 Uiso 1 1 calc R U . . .
C75 C 0.0990(3) 0.3531(3) 0.1392(2) 0.0363(14) Uani 1 1 d . . . . .
H75 H 0.0664 0.3852 0.1710 0.044 Uiso 1 1 calc R U . . .
C76 C 0.0619(3) 0.3300(3) 0.1149(2) 0.0323(13) Uani 1 1 d . . . . .
H76 H 0.0040 0.3459 0.1299 0.039 Uiso 1 1 calc R U . . .
C77 C 0.1101(3) 0.2830(3) 0.0682(2) 0.0288(12) Uani 1 1 d . . . . .
H77 H 0.0849 0.2665 0.0517 0.035 Uiso 1 1 calc R U . . .
C78 C 0.1939(3) 0.2602(3) 0.0458(2) 0.0267(12) Uani 1 1 d . . . . .
H78 H 0.2262 0.2285 0.0137 0.032 Uiso 1 1 calc R U . . .
C79 C 0.3890(3) 0.1524(3) 0.0827(2) 0.0208(11) Uani 1 1 d . . . . .
C80 C 0.3516(3) 0.1275(3) 0.1493(2) 0.0243(12) Uani 1 1 d . . . . .
H80 H 0.2975 0.1601 0.1701 0.029 Uiso 1 1 calc R U . . .
C81 C 0.3940(3) 0.0548(3) 0.1850(2) 0.0261(12) Uani 1 1 d . . . . .
H81 H 0.3690 0.0377 0.2305 0.031 Uiso 1 1 calc R U . . .
C82 C 0.4714(3) 0.0079(3) 0.1549(2) 0.0276(12) Uani 1 1 d . . . . .
H82 H 0.5006 -0.0411 0.1800 0.033 Uiso 1 1 calc R U . . .
C83 C 0.5080(3) 0.0306(3) 0.0883(2) 0.0303(13) Uani 1 1 d . . . . .
H83 H 0.5610 -0.0036 0.0673 0.036 Uiso 1 1 calc R U . . .
C84 C 0.4669(3) 0.1040(3) 0.0522(2) 0.0275(12) Uani 1 1 d . . . . .
H84 H 0.4922 0.1207 0.0067 0.033 Uiso 1 1 calc R U . . .
C85 C 0.3609(3) 0.3152(3) 0.0697(2) 0.0211(11) Uani 1 1 d . . . . .
C86 C 0.4003(3) 0.2825(3) 0.1182(2) 0.0243(11) Uani 1 1 d . . . . .
H86 H 0.4223 0.2265 0.1341 0.029 Uiso 1 1 calc R U . . .
C87 C 0.4077(3) 0.3307(3) 0.1435(2) 0.0270(12) Uani 1 1 d . . . . .
H87 H 0.4344 0.3076 0.1771 0.032 Uiso 1 1 calc R U . . .
C88 C 0.3770(3) 0.4120(3) 0.1209(2) 0.0262(12) Uani 1 1 d . . . . .
H88 H 0.3822 0.4446 0.1390 0.031 Uiso 1 1 calc R U . . .
C89 C 0.3385(3) 0.4464(3) 0.0717(2) 0.0249(12) Uani 1 1 d . . . . .
H89 H 0.3187 0.5024 0.0551 0.030 Uiso 1 1 calc R U . . .
C90 C 0.3289(3) 0.3981(3) 0.0465(2) 0.0236(11) Uani 1 1 d . . . . .
H90 H 0.3009 0.4213 0.0139 0.028 Uiso 1 1 calc R U . . .
C91 C 0.3591(3) 0.7951(3) -0.0563(2) 0.0228(11) Uani 1 1 d . . . . .
C92 C 0.3543(3) 0.7479(3) -0.0852(2) 0.0288(12) Uani 1 1 d . . . . .
H92 H 0.3323 0.7088 -0.0585 0.035 Uiso 1 1 calc R U . . .
C93 C 0.3819(3) 0.7583(3) -0.1535(2) 0.0341(13) Uani 1 1 d . . . . .
H93 H 0.3780 0.7268 -0.1737 0.041 Uiso 1 1 calc R U . . .
C94 C 0.4152(3) 0.8144(3) -0.1921(2) 0.0306(13) Uani 1 1 d . . . . .
H94 H 0.4343 0.8210 -0.2388 0.037 Uiso 1 1 calc R U . . .
C95 C 0.4207(3) 0.8605(3) -0.1637(2) 0.0305(13) Uani 1 1 d . . . . .
H95 H 0.4437 0.8988 -0.1907 0.037 Uiso 1 1 calc R U . . .
C96 C 0.3929(3) 0.8512(3) -0.0952(2) 0.0240(11) Uani 1 1 d . . . . .
H96 H 0.3969 0.8829 -0.0753 0.029 Uiso 1 1 calc R U . . .
C97 C 0.2131(3) 0.8075(3) 0.0631(2) 0.0200(11) Uani 1 1 d . . . . .
C98 C 0.1627(3) 0.8609(3) 0.1053(2) 0.0265(12) Uani 1 1 d . . . . .
H98 H 0.1861 0.8838 0.1175 0.032 Uiso 1 1 calc R U . . .
C99 C 0.0791(3) 0.8802(3) 0.1291(2) 0.0278(12) Uani 1 1 d . . . . .
H99 H 0.0451 0.9177 0.1565 0.033 Uiso 1 1 calc R U . . .
C100 C 0.0446(3) 0.8452(3) 0.1134(2) 0.0238(11) Uani 1 1 d . . . . .
H100 H -0.0127 0.8575 0.1309 0.029 Uiso 1 1 calc R U . . .
C101 C 0.0931(3) 0.7926(3) 0.0724(2) 0.0251(12) Uani 1 1 d . . . . .
H101 H 0.0693 0.7688 0.0615 0.030 Uiso 1 1 calc R U . . .
C102 C 0.1766(3) 0.7742(3) 0.0469(2) 0.0252(12) Uani 1 1 d . . . . .
H102 H 0.2095 0.7384 0.0179 0.030 Uiso 1 1 calc R U . . .
C103 C 0.3737(3) 0.6824(3) 0.0710(2) 0.0219(11) Uani 1 1 d . . . . .
C104 C 0.3432(3) 0.6563(3) 0.1389(2) 0.0252(12) Uani 1 1 d . . . . .
H104 H 0.2920 0.6896 0.1628 0.030 Uiso 1 1 calc R U . . .
C105 C 0.3865(3) 0.5831(3) 0.1713(2) 0.0303(13) Uani 1 1 d . . . . .
H105 H 0.3657 0.5662 0.2177 0.036 Uiso 1 1 calc R U . . .
C106 C 0.4604(3) 0.5335(3) 0.1368(2) 0.0277(12) Uani 1 1 d . . . . .
H106 H 0.4906 0.4828 0.1595 0.033 Uiso 1 1 calc R U . . .
C107 C 0.4904(3) 0.5578(3) 0.0694(2) 0.0278(12) Uani 1 1 d . . . . .
H107 H 0.5406 0.5232 0.0457 0.033 Uiso 1 1 calc R U . . .
C108 C 0.4477(3) 0.6325(3) 0.0359(2) 0.0269(12) Uani 1 1 d . . . . .
H108 H 0.4688 0.6493 -0.0104 0.032 Uiso 1 1 calc R U . . .
C109 C 0.3387(3) 0.8479(3) 0.0576(2) 0.0208(11) Uani 1 1 d . . . . .
C110 C 0.3848(3) 0.8169(3) 0.1013(2) 0.0220(11) Uani 1 1 d . . . . .
H110 H 0.4108 0.7610 0.1158 0.026 Uiso 1 1 calc R U . . .
C111 C 0.3924(3) 0.8685(3) 0.1234(2) 0.0272(12) Uani 1 1 d . . . . .
H111 H 0.4245 0.8478 0.1527 0.033 Uiso 1 1 calc R U . . .
C112 C 0.3533(3) 0.9501(3) 0.1030(2) 0.0315(13) Uani 1 1 d . . . . .
H112 H 0.3578 0.9851 0.1192 0.038 Uiso 1 1 calc R U . . .
C113 C 0.3077(3) 0.9809(3) 0.0591(2) 0.0310(13) Uani 1 1 d . . . . .
H113 H 0.2815 1.0369 0.0449 0.037 Uiso 1 1 calc R U . . .
C114 C 0.3004(3) 0.9307(3) 0.0364(2) 0.0265(12) Uani 1 1 d . . . . .
H114 H 0.2694 0.9519 0.0062 0.032 Uiso 1 1 calc R U . . .
C115 C 0.8425(3) 0.4584(3) 0.5966(2) 0.0268(12) Uani 1 1 d . . . . .
C116 C 0.7645(3) 0.5197(3) 0.6093(3) 0.0309(13) Uani 1 1 d . . . . .
H116 H 0.7311 0.5215 0.6537 0.037 Uiso 1 1 calc R U . . .
C117 C 0.7354(4) 0.5780(3) 0.5575(3) 0.0394(15) Uani 1 1 d . . . . .
H117 H 0.6819 0.6189 0.5662 0.047 Uiso 1 1 calc R U . . .
C118 C 0.7851(4) 0.5757(3) 0.4934(3) 0.0443(16) Uani 1 1 d . . . . .
H118 H 0.7654 0.6150 0.4578 0.053 Uiso 1 1 calc R U . . .
C119 C 0.8635(4) 0.5167(3) 0.4802(3) 0.0455(16) Uani 1 1 d . . . . .
H119 H 0.8977 0.5169 0.4359 0.055 Uiso 1 1 calc R U . . .
C120 C 0.8923(3) 0.4574(3) 0.5315(2) 0.0357(14) Uani 1 1 d . . . . .
H120 H 0.9456 0.4165 0.5224 0.043 Uiso 1 1 calc R U . . .
C121 C 0.8208(3) 0.3149(3) 0.6895(2) 0.0240(12) Uani 1 1 d . . . . .
C122 C 0.7442(3) 0.3458(3) 0.6801(2) 0.0268(12) Uani 1 1 d . . . . .
H122 H 0.7205 0.4003 0.6596 0.032 Uiso 1 1 calc R U . . .
C123 C 0.7023(3) 0.2965(3) 0.7008(2) 0.0300(12) Uani 1 1 d . . . . .
H123 H 0.6497 0.3174 0.6950 0.036 Uiso 1 1 calc R U . . .
C124 C 0.7377(3) 0.2173(3) 0.7298(2) 0.0272(12) Uani 1 1 d . . . . .
H124 H 0.7096 0.1835 0.7435 0.033 Uiso 1 1 calc R U . . .
C125 C 0.8136(3) 0.1869(3) 0.7390(2) 0.0302(13) Uani 1 1 d . . . . .
H125 H 0.8373 0.1323 0.7592 0.036 Uiso 1 1 calc R U . . .
C126 C 0.8554(3) 0.2347(3) 0.7193(2) 0.0274(12) Uani 1 1 d . . . . .
H126 H 0.9076 0.2131 0.7259 0.033 Uiso 1 1 calc R U . . .
C127 C 0.9827(3) 0.3222(3) 0.6388(2) 0.0227(11) Uani 1 1 d . . . . .
C128 C 1.0144(3) 0.2636(3) 0.6046(2) 0.0328(13) Uani 1 1 d . . . . .
H128 H 0.9789 0.2523 0.5948 0.039 Uiso 1 1 calc R U . . .
C129 C 1.0987(3) 0.2217(3) 0.5847(2) 0.0354(14) Uani 1 1 d . . . . .
H129 H 1.1212 0.1812 0.5614 0.043 Uiso 1 1 calc R U . . .
C130 C 1.1500(3) 0.2390(3) 0.5988(2) 0.0336(13) Uani 1 1 d . . . . .
H130 H 1.2077 0.2106 0.5846 0.040 Uiso 1 1 calc R U . . .
C131 C 1.1186(3) 0.2967(3) 0.6331(3) 0.0345(13) Uani 1 1 d . . . . .
H131 H 1.1542 0.3081 0.6426 0.041 Uiso 1 1 calc R U . . .
C132 C 1.0345(3) 0.3382(3) 0.6538(2) 0.0278(12) Uani 1 1 d . . . . .
H132 H 1.0122 0.3775 0.6783 0.033 Uiso 1 1 calc R U . . .
C133 C 0.8516(3) 0.4224(3) 0.7287(2) 0.0231(11) Uani 1 1 d . . . . .
C134 C 0.8455(3) 0.3773(3) 0.7939(2) 0.0284(12) Uani 1 1 d . . . . .
H134 H 0.8458 0.3258 0.8049 0.034 Uiso 1 1 calc R U . . .
C135 C 0.8392(3) 0.4078(3) 0.8419(2) 0.0286(12) Uani 1 1 d . . . . .
H135 H 0.8352 0.3772 0.8859 0.034 Uiso 1 1 calc R U . . .
C136 C 0.8387(3) 0.4823(3) 0.8263(2) 0.0276(12) Uani 1 1 d . . . . .
H136 H 0.8357 0.5022 0.8595 0.033 Uiso 1 1 calc R U . . .
C137 C 0.8424(3) 0.5282(3) 0.7636(2) 0.0299(13) Uani 1 1 d . . . . .
H137 H 0.8403 0.5803 0.7536 0.036 Uiso 1 1 calc R U . . .
C138 C 0.8493(3) 0.4985(3) 0.7149(2) 0.0309(13) Uani 1 1 d . . . . .
H138 H 0.8526 0.5302 0.6713 0.037 Uiso 1 1 calc R U . . .


_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 O1 1.755(3) . ?
U1 O2 1.760(3) . ?
U1 O21 2.365(3) . ?
U1 O14 2.366(3) . ?
U1 O16 2.375(3) . ?
U1 O9 2.378(3) . ?
U1 O19 2.430(3) . ?
U2 O3 1.760(3) . ?
U2 O4 1.763(3) . ?
U2 O10 2.359(3) . ?
U2 O15 2.362(3) . ?
U2 O11 2.368(3) . ?
U2 O26 2.375(3) . ?
U2 O24 2.424(3) . ?
U3 O5 1.757(3) . ?
U3 O6 1.769(3) . ?
U3 O34 2.315(3) . ?
U3 O29 2.360(3) . ?
U3 O25 2.376(3) . ?
U3 O36 2.390(3) . ?
U3 O39 2.471(3) . ?
U4 O7 1.758(3) . ?
U4 O8 1.765(3) . ?
U4 O30 2.322(3) . ?
U4 O35 2.344(3) . ?
U4 O31 2.387(3) . ?
U4 O20 2.395(3) 1_456 ?
U4 O40 2.463(3) . ?
S1 O13 1.448(3) . ?
S1 O12 1.452(3) . ?
S1 O11 1.478(3) . ?
S1 C3 1.774(5) . ?
S2 O17 1.438(3) . ?
S2 O18 1.446(3) . ?
S2 O16 1.476(3) . ?
S2 C10 1.754(5) . ?
S3 O23 1.445(3) . ?
S3 O22 1.449(3) . ?
S3 O21 1.487(3) . ?
S3 C17 1.786(5) . ?
S4 O27 1.442(3) . ?
S4 O28 1.448(3) . ?
S4 O26 1.482(3) . ?
S4 C24 1.780(5) . ?
S5 O32 1.437(4) . ?
S5 O33 1.446(3) . ?
S5 O31 1.493(3) . ?
S5 C31 1.794(4) . ?
S6 O38 1.443(3) . ?
S6 O37 1.446(3) . ?
S6 O36 1.485(3) . ?
S6 C38 1.801(4) . ?
P1 C55 1.782(5) . ?
P1 C43 1.785(5) . ?
P1 C49 1.789(5) . ?
P1 C61 1.803(5) . ?
P2 C67 1.792(5) . ?
P2 C85 1.797(5) . ?
P2 C73 1.802(5) . ?
P2 C79 1.803(4) . ?
P3 C103 1.791(4) . ?
P3 C97 1.793(5) . ?
P3 C109 1.800(5) . ?
P3 C91 1.807(5) . ?
P4 C133 1.779(5) . ?
P4 C115 1.787(5) . ?
P4 C127 1.802(5) . ?
P4 C121 1.810(5) . ?
O9 C1 1.259(5) . ?
O10 C1 1.270(5) . ?
O14 C8 1.256(5) . ?
O15 C8 1.267(5) . ?
O19 C15 1.269(5) . ?
O20 C15 1.251(5) . ?
O20 U4 2.395(3) 1_654 ?
O24 C22 1.272(5) . ?
O25 C22 1.256(5) . ?
O29 C29 1.249(5) . ?
O30 C29 1.258(5) . ?
O34 C36 1.255(5) . ?
O35 C36 1.253(5) . ?
O39 H39A 0.9874 . ?
O39 H39B 0.8307 . ?
O40 H40A 0.9365 . ?
O40 H40B 0.8623 . ?
O41 H41A 0.9339 . ?
O41 H41B 0.8703 . ?
O42 H42A 0.9935 . ?
O42 H42B 0.9862 . ?
C1 C2 1.490(6) . ?
C2 C7 1.390(6) . ?
C2 C3 1.413(6) . ?
C3 C4 1.394(6) . ?
C4 C5 1.391(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.393(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.494(6) . ?
C9 C14 1.388(6) . ?
C9 C10 1.423(6) . ?
C10 C11 1.399(6) . ?
C11 C12 1.398(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.373(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(6) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.508(6) . ?
C16 C21 1.384(6) . ?
C16 C17 1.393(6) . ?
C17 C18 1.379(6) . ?
C18 C19 1.387(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.396(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.391(6) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.498(6) . ?
C23 C24 1.396(6) . ?
C23 C28 1.399(6) . ?
C24 C25 1.403(6) . ?
C25 C26 1.379(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.390(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.366(6) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.507(6) . ?
C30 C35 1.391(6) . ?
C30 C31 1.418(6) . ?
C31 C32 1.385(6) . ?
C32 C33 1.393(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.373(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.382(6) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.513(6) . ?
C37 C42 1.390(6) . ?
C37 C38 1.413(6) . ?
C38 C39 1.384(6) . ?
C39 C40 1.393(6) . ?
C39 H39 0.9500 . ?
C40 C41 1.362(7) . ?
C40 H40 0.9500 . ?
C41 C42 1.377(6) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.391(7) . ?
C43 C48 1.412(7) . ?
C44 C45 1.396(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.361(8) . ?
C45 H45 0.9500 . ?
C46 C47 1.396(8) . ?
C46 H46 0.9500 . ?
C47 C48 1.394(6) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C54 1.392(6) . ?
C49 C50 1.410(6) . ?
C50 C51 1.376(7) . ?
C50 H50 0.9500 . ?
C51 C52 1.377(7) . ?
C51 H51 0.9500 . ?
C52 C53 1.380(7) . ?
C52 H52 0.9500 . ?
C53 C54 1.392(7) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C60 1.400(6) . ?
C55 C56 1.400(6) . ?
C56 C57 1.387(6) . ?
C56 H56 0.9500 . ?
C57 C58 1.387(7) . ?
C57 H57 0.9500 . ?
C58 C59 1.382(6) . ?
C58 H58 0.9500 . ?
C59 C60 1.378(6) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C61 C62 1.386(7) . ?
C61 C66 1.388(6) . ?
C62 C63 1.382(7) . ?
C62 H62 0.9500 . ?
C63 C64 1.378(7) . ?
C63 H63 0.9500 . ?
C64 C65 1.389(7) . ?
C64 H64 0.9500 . ?
C65 C66 1.383(7) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C67 C68 1.397(6) . ?
C67 C72 1.403(6) . ?
C68 C69 1.375(6) . ?
C68 H68 0.9500 . ?
C69 C70 1.386(7) . ?
C69 H69 0.9500 . ?
C70 C71 1.378(7) . ?
C70 H70 0.9500 . ?
C71 C72 1.383(6) . ?
C71 H71 0.9500 . ?
C72 H72 0.9500 . ?
C73 C78 1.391(6) . ?
C73 C74 1.394(6) . ?
C74 C75 1.384(7) . ?
C74 H74 0.9500 . ?
C75 C76 1.379(7) . ?
C75 H75 0.9500 . ?
C76 C77 1.393(6) . ?
C76 H76 0.9500 . ?
C77 C78 1.377(6) . ?
C77 H77 0.9500 . ?
C78 H78 0.9500 . ?
C79 C84 1.380(6) . ?
C79 C80 1.393(6) . ?
C80 C81 1.389(6) . ?
C80 H80 0.9500 . ?
C81 C82 1.362(6) . ?
C81 H81 0.9500 . ?
C82 C83 1.383(6) . ?
C82 H82 0.9500 . ?
C83 C84 1.391(6) . ?
C83 H83 0.9500 . ?
C84 H84 0.9500 . ?
C85 C86 1.388(6) . ?
C85 C90 1.404(6) . ?
C86 C87 1.374(6) . ?
C86 H86 0.9500 . ?
C87 C88 1.376(6) . ?
C87 H87 0.9500 . ?
C88 C89 1.386(6) . ?
C88 H88 0.9500 . ?
C89 C90 1.403(6) . ?
C89 H89 0.9500 . ?
C90 H90 0.9500 . ?
C91 C92 1.388(6) . ?
C91 C96 1.390(6) . ?
C92 C93 1.387(6) . ?
C92 H92 0.9500 . ?
C93 C94 1.383(7) . ?
C93 H93 0.9500 . ?
C94 C95 1.368(7) . ?
C94 H94 0.9500 . ?
C95 C96 1.394(6) . ?
C95 H95 0.9500 . ?
C96 H96 0.9500 . ?
C97 C102 1.398(6) . ?
C97 C98 1.403(6) . ?
C98 C99 1.382(6) . ?
C98 H98 0.9500 . ?
C99 C100 1.385(6) . ?
C99 H99 0.9500 . ?
C100 C101 1.372(6) . ?
C100 H100 0.9500 . ?
C101 C102 1.383(6) . ?
C101 H101 0.9500 . ?
C102 H102 0.9500 . ?
C103 C108 1.391(6) . ?
C103 C104 1.393(6) . ?
C104 C105 1.368(6) . ?
C104 H104 0.9500 . ?
C105 C106 1.382(6) . ?
C105 H105 0.9500 . ?
C106 C107 1.379(6) . ?
C106 H106 0.9500 . ?
C107 C108 1.390(6) . ?
C107 H107 0.9500 . ?
C108 H108 0.9500 . ?
C109 C110 1.391(6) . ?
C109 C114 1.407(6) . ?
C110 C111 1.387(6) . ?
C110 H110 0.9500 . ?
C111 C112 1.387(6) . ?
C111 H111 0.9500 . ?
C112 C113 1.389(7) . ?
C112 H112 0.9500 . ?
C113 C114 1.368(6) . ?
C113 H113 0.9500 . ?
C114 H114 0.9500 . ?
C115 C120 1.395(7) . ?
C115 C116 1.401(7) . ?
C116 C117 1.392(6) . ?
C116 H116 0.9500 . ?
C117 C118 1.380(7) . ?
C117 H117 0.9500 . ?
C118 C119 1.388(8) . ?
C118 H118 0.9500 . ?
C119 C120 1.389(7) . ?
C119 H119 0.9500 . ?
C120 H120 0.9500 . ?
C121 C122 1.392(6) . ?
C121 C126 1.397(6) . ?
C122 C123 1.398(6) . ?
C122 H122 0.9500 . ?
C123 C124 1.380(6) . ?
C123 H123 0.9500 . ?
C124 C125 1.378(7) . ?
C124 H124 0.9500 . ?
C125 C126 1.374(7) . ?
C125 H125 0.9500 . ?
C126 H126 0.9500 . ?
C127 C128 1.383(6) . ?
C127 C132 1.390(6) . ?
C128 C129 1.387(7) . ?
C128 H128 0.9500 . ?
C129 C130 1.388(7) . ?
C129 H129 0.9500 . ?
C130 C131 1.370(7) . ?
C130 H130 0.9500 . ?
C131 C132 1.384(7) . ?
C131 H131 0.9500 . ?
C132 H132 0.9500 . ?
C133 C138 1.397(6) . ?
C133 C134 1.405(6) . ?
C134 C135 1.378(6) . ?
C134 H134 0.9500 . ?
C135 C136 1.374(6) . ?
C135 H135 0.9500 . ?
C136 C137 1.369(6) . ?
C136 H136 0.9500 . ?
C137 C138 1.376(6) . ?
C137 H137 0.9500 . ?
C138 H138 0.9500 . ?

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 U1 O2 178.42(14) . . ?
O1 U1 O21 87.17(12) . . ?
O2 U1 O21 93.66(12) . . ?
O1 U1 O14 88.51(12) . . ?
O2 U1 O14 91.44(12) . . ?
O21 U1 O14 149.87(10) . . ?
O1 U1 O16 87.34(12) . . ?
O2 U1 O16 91.15(12) . . ?
O21 U1 O16 138.47(10) . . ?
O14 U1 O16 70.96(10) . . ?
O1 U1 O9 90.04(12) . . ?
O2 U1 O9 91.46(12) . . ?
O21 U1 O9 77.04(10) . . ?
O14 U1 O9 73.16(10) . . ?
O16 U1 O9 144.08(10) . . ?
O1 U1 O19 92.14(12) . . ?
O2 U1 O19 86.82(12) . . ?
O21 U1 O19 72.95(10) . . ?
O14 U1 O19 137.04(10) . . ?
O16 U1 O19 66.17(10) . . ?
O9 U1 O19 149.75(10) . . ?
O3 U2 O4 178.47(14) . . ?
O3 U2 O10 91.29(12) . . ?
O4 U2 O10 87.87(12) . . ?
O3 U2 O15 91.34(12) . . ?
O4 U2 O15 89.67(13) . . ?
O10 U2 O15 73.99(10) . . ?
O3 U2 O11 90.06(12) . . ?
O4 U2 O11 88.46(12) . . ?
O10 U2 O11 71.02(10) . . ?
O15 U2 O11 145.01(10) . . ?
O3 U2 O26 93.08(12) . . ?
O4 U2 O26 88.30(12) . . ?
O10 U2 O26 148.58(10) . . ?
O15 U2 O26 74.81(10) . . ?
O11 U2 O26 140.01(10) . . ?
O3 U2 O24 87.47(12) . . ?
O4 U2 O24 92.29(12) . . ?
O10 U2 O24 138.32(10) . . ?
O15 U2 O24 147.67(10) . . ?
O11 U2 O24 67.32(10) . . ?
O26 U2 O24 73.00(10) . . ?
O5 U3 O6 178.19(13) . . ?
O5 U3 O34 91.96(13) . . ?
O6 U3 O34 89.20(13) . . ?
O5 U3 O29 90.42(13) . . ?
O6 U3 O29 88.37(12) . . ?
O34 U3 O29 81.35(10) . . ?
O5 U3 O25 90.08(12) . . ?
O6 U3 O25 88.28(12) . . ?
O34 U3 O25 155.44(10) . . ?
O29 U3 O25 74.16(10) . . ?
O5 U3 O36 87.49(12) . . ?
O6 U3 O36 94.22(12) . . ?
O34 U3 O36 69.77(10) . . ?
O29 U3 O36 150.94(10) . . ?
O25 U3 O36 134.78(10) . . ?
O5 U3 O39 92.53(13) . . ?
O6 U3 O39 87.65(12) . . ?
O34 U3 O39 134.38(10) . . ?
O29 U3 O39 143.94(10) . . ?
O25 U3 O39 69.90(10) . . ?
O36 U3 O39 65.12(10) . . ?
O7 U4 O8 178.07(15) . . ?
O7 U4 O30 91.32(13) . . ?
O8 U4 O30 90.48(13) . . ?
O7 U4 O35 89.11(13) . . ?
O8 U4 O35 90.54(13) . . ?
O30 U4 O35 78.89(11) . . ?
O7 U4 O31 90.58(13) . . ?
O8 U4 O31 90.70(13) . . ?
O30 U4 O31 70.22(10) . . ?
O35 U4 O31 149.10(11) . . ?
O7 U4 O20 87.57(13) . 1_456 ?
O8 U4 O20 90.50(13) . 1_456 ?
O30 U4 O20 151.91(10) . 1_456 ?
O35 U4 O20 73.03(11) . 1_456 ?
O31 U4 O20 137.83(10) . 1_456 ?
O7 U4 O40 91.69(13) . . ?
O8 U4 O40 87.49(13) . . ?
O30 U4 O40 136.87(10) . . ?
O35 U4 O40 144.17(11) . . ?
O31 U4 O40 66.73(10) . . ?
O20 U4 O40 71.21(10) 1_456 . ?
O13 S1 O12 115.7(2) . . ?
O13 S1 O11 108.70(18) . . ?
O12 S1 O11 111.97(18) . . ?
O13 S1 C3 106.6(2) . . ?
O12 S1 C3 107.2(2) . . ?
O11 S1 C3 106.07(19) . . ?
O17 S2 O18 115.3(2) . . ?
O17 S2 O16 112.46(19) . . ?
O18 S2 O16 109.02(18) . . ?
O17 S2 C10 106.6(2) . . ?
O18 S2 C10 106.5(2) . . ?
O16 S2 C10 106.3(2) . . ?
O23 S3 O22 115.34(19) . . ?
O23 S3 O21 111.76(18) . . ?
O22 S3 O21 110.76(19) . . ?
O23 S3 C17 106.2(2) . . ?
O22 S3 C17 106.1(2) . . ?
O21 S3 C17 106.0(2) . . ?
O27 S4 O28 115.32(19) . . ?
O27 S4 O26 111.87(18) . . ?
O28 S4 O26 109.93(19) . . ?
O27 S4 C24 106.5(2) . . ?
O28 S4 C24 106.7(2) . . ?
O26 S4 C24 105.88(19) . . ?
O32 S5 O33 115.3(2) . . ?
O32 S5 O31 112.9(2) . . ?
O33 S5 O31 109.7(2) . . ?
O32 S5 C31 107.0(2) . . ?
O33 S5 C31 105.5(2) . . ?
O31 S5 C31 105.6(2) . . ?
O38 S6 O37 114.90(19) . . ?
O38 S6 O36 110.05(19) . . ?
O37 S6 O36 112.70(18) . . ?
O38 S6 C38 105.6(2) . . ?
O37 S6 C38 106.1(2) . . ?
O36 S6 C38 106.83(19) . . ?
C55 P1 C43 107.9(2) . . ?
C55 P1 C49 109.5(2) . . ?
C43 P1 C49 111.2(2) . . ?
C55 P1 C61 110.8(2) . . ?
C43 P1 C61 109.9(2) . . ?
C49 P1 C61 107.6(2) . . ?
C67 P2 C85 111.1(2) . . ?
C67 P2 C73 112.0(2) . . ?
C85 P2 C73 106.7(2) . . ?
C67 P2 C79 110.0(2) . . ?
C85 P2 C79 107.5(2) . . ?
C73 P2 C79 109.4(2) . . ?
C103 P3 C97 109.1(2) . . ?
C103 P3 C109 108.5(2) . . ?
C97 P3 C109 106.4(2) . . ?
C103 P3 C91 109.8(2) . . ?
C97 P3 C91 112.2(2) . . ?
C109 P3 C91 110.8(2) . . ?
C133 P4 C115 108.3(2) . . ?
C133 P4 C127 108.2(2) . . ?
C115 P4 C127 110.5(2) . . ?
C133 P4 C121 112.0(2) . . ?
C115 P4 C121 109.1(2) . . ?
C127 P4 C121 108.8(2) . . ?
C1 O9 U1 142.3(3) . . ?
C1 O10 U2 144.7(3) . . ?
S1 O11 U2 141.47(19) . . ?
C8 O14 U1 149.2(3) . . ?
C8 O15 U2 140.2(3) . . ?
S2 O16 U1 141.54(19) . . ?
C15 O19 U1 142.3(3) . . ?
C15 O20 U4 147.2(3) . 1_654 ?
S3 O21 U1 138.95(19) . . ?
C22 O24 U2 149.1(3) . . ?
C22 O25 U3 148.8(3) . . ?
S4 O26 U2 139.97(18) . . ?
C29 O29 U3 145.5(3) . . ?
C29 O30 U4 143.0(3) . . ?
S5 O31 U4 133.67(19) . . ?
C36 O34 U3 142.4(3) . . ?
C36 O35 U4 147.3(3) . . ?
S6 O36 U3 135.89(18) . . ?
U3 O39 H39A 140.8 . . ?
U3 O39 H39B 114.4 . . ?
H39A O39 H39B 99.4 . . ?
U4 O40 H40A 101.6 . . ?
U4 O40 H40B 115.0 . . ?
H40A O40 H40B 105.8 . . ?
H41A O41 H41B 90.0 . . ?
H42A O42 H42B 102.9 . . ?
O9 C1 O10 123.2(4) . . ?
O9 C1 C2 117.3(4) . . ?
O10 C1 C2 119.5(4) . . ?
C7 C2 C3 118.8(4) . . ?
C7 C2 C1 116.2(4) . . ?
C3 C2 C1 124.8(4) . . ?
C4 C3 C2 119.8(4) . . ?
C4 C3 S1 116.7(4) . . ?
C2 C3 S1 123.1(3) . . ?
C5 C4 C3 120.2(4) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C6 C5 C4 120.3(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 119.6(5) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C2 C7 C6 121.2(4) . . ?
C2 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
O14 C8 O15 123.4(4) . . ?
O14 C8 C9 119.6(4) . . ?
O15 C8 C9 116.9(4) . . ?
C14 C9 C10 118.6(4) . . ?
C14 C9 C8 117.7(4) . . ?
C10 C9 C8 123.6(4) . . ?
C11 C10 C9 119.1(4) . . ?
C11 C10 S2 117.3(4) . . ?
C9 C10 S2 123.1(3) . . ?
C12 C11 C10 120.9(4) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C13 C12 C11 119.7(4) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 120.2(4) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C9 C14 C13 121.5(5) . . ?
C9 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
O20 C15 O19 123.0(4) . . ?
O20 C15 C16 117.1(4) . . ?
O19 C15 C16 119.9(4) . . ?
C21 C16 C17 119.5(4) . . ?
C21 C16 C15 117.1(4) . . ?
C17 C16 C15 123.4(4) . . ?
C18 C17 C16 119.7(5) . . ?
C18 C17 S3 118.5(4) . . ?
C16 C17 S3 121.7(3) . . ?
C17 C18 C19 121.1(5) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C18 C19 C20 119.5(5) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C21 C20 C19 119.3(5) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C16 C21 C20 121.0(5) . . ?
C16 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
O25 C22 O24 122.9(4) . . ?
O25 C22 C23 116.8(4) . . ?
O24 C22 C23 120.2(4) . . ?
C24 C23 C28 119.9(4) . . ?
C24 C23 C22 122.4(4) . . ?
C28 C23 C22 117.6(4) . . ?
C23 C24 C25 118.8(4) . . ?
C23 C24 S4 121.4(3) . . ?
C25 C24 S4 119.7(4) . . ?
C26 C25 C24 120.5(4) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C25 C26 C27 119.9(5) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C28 C27 C26 120.4(5) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C23 120.3(5) . . ?
C27 C28 H28 119.8 . . ?
C23 C28 H28 119.8 . . ?
O29 C29 O30 122.8(4) . . ?
O29 C29 C30 116.5(4) . . ?
O30 C29 C30 120.7(4) . . ?
C35 C30 C31 117.8(4) . . ?
C35 C30 C29 116.3(4) . . ?
C31 C30 C29 125.9(4) . . ?
C32 C31 C30 119.0(4) . . ?
C32 C31 S5 114.6(3) . . ?
C30 C31 S5 126.5(3) . . ?
C31 C32 C33 121.9(4) . . ?
C31 C32 H32 119.1 . . ?
C33 C32 H32 119.1 . . ?
C34 C33 C32 119.2(4) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C33 C34 C35 119.8(4) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C34 C35 C30 122.3(4) . . ?
C34 C35 H35 118.8 . . ?
C30 C35 H35 118.8 . . ?
O35 C36 O34 123.5(4) . . ?
O35 C36 C37 115.1(4) . . ?
O34 C36 C37 121.4(4) . . ?
C42 C37 C38 117.7(4) . . ?
C42 C37 C36 116.2(4) . . ?
C38 C37 C36 126.0(4) . . ?
C39 C38 C37 119.5(4) . . ?
C39 C38 S6 114.6(3) . . ?
C37 C38 S6 125.8(3) . . ?
C38 C39 C40 120.4(5) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 H39 119.8 . . ?
C41 C40 C39 120.9(5) . . ?
C41 C40 H40 119.6 . . ?
C39 C40 H40 119.6 . . ?
C40 C41 C42 118.9(5) . . ?
C40 C41 H41 120.6 . . ?
C42 C41 H41 120.6 . . ?
C41 C42 C37 122.7(5) . . ?
C41 C42 H42 118.7 . . ?
C37 C42 H42 118.7 . . ?
C44 C43 C48 119.4(5) . . ?
C44 C43 P1 122.2(4) . . ?
C48 C43 P1 118.4(4) . . ?
C43 C44 C45 119.8(5) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C46 C45 C44 120.4(5) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C45 C46 C47 121.3(5) . . ?
C45 C46 H46 119.4 . . ?
C47 C46 H46 119.4 . . ?
C48 C47 C46 119.0(6) . . ?
C48 C47 H47 120.5 . . ?
C46 C47 H47 120.5 . . ?
C47 C48 C43 120.1(5) . . ?
C47 C48 H48 120.0 . . ?
C43 C48 H48 120.0 . . ?
C54 C49 C50 119.1(5) . . ?
C54 C49 P1 121.3(4) . . ?
C50 C49 P1 119.6(4) . . ?
C51 C50 C49 119.5(5) . . ?
C51 C50 H50 120.2 . . ?
C49 C50 H50 120.2 . . ?
C50 C51 C52 121.1(5) . . ?
C50 C51 H51 119.4 . . ?
C52 C51 H51 119.4 . . ?
C51 C52 C53 120.0(5) . . ?
C51 C52 H52 120.0 . . ?
C53 C52 H52 120.0 . . ?
C52 C53 C54 120.0(5) . . ?
C52 C53 H53 120.0 . . ?
C54 C53 H53 120.0 . . ?
C53 C54 C49 120.2(5) . . ?
C53 C54 H54 119.9 . . ?
C49 C54 H54 119.9 . . ?
C60 C55 C56 119.4(4) . . ?
C60 C55 P1 122.1(4) . . ?
C56 C55 P1 118.3(4) . . ?
C57 C56 C55 119.9(5) . . ?
C57 C56 H56 120.1 . . ?
C55 C56 H56 120.1 . . ?
C58 C57 C56 119.9(5) . . ?
C58 C57 H57 120.1 . . ?
C56 C57 H57 120.1 . . ?
C59 C58 C57 120.5(5) . . ?
C59 C58 H58 119.7 . . ?
C57 C58 H58 119.7 . . ?
C60 C59 C58 120.2(5) . . ?
C60 C59 H59 119.9 . . ?
C58 C59 H59 119.9 . . ?
C59 C60 C55 120.1(5) . . ?
C59 C60 H60 120.0 . . ?
C55 C60 H60 120.0 . . ?
C62 C61 C66 119.2(5) . . ?
C62 C61 P1 120.7(4) . . ?
C66 C61 P1 120.0(4) . . ?
C63 C62 C61 119.7(5) . . ?
C63 C62 H62 120.1 . . ?
C61 C62 H62 120.1 . . ?
C64 C63 C62 120.9(5) . . ?
C64 C63 H63 119.5 . . ?
C62 C63 H63 119.5 . . ?
C63 C64 C65 119.8(5) . . ?
C63 C64 H64 120.1 . . ?
C65 C64 H64 120.1 . . ?
C66 C65 C64 119.3(5) . . ?
C66 C65 H65 120.4 . . ?
C64 C65 H65 120.4 . . ?
C65 C66 C61 121.0(5) . . ?
C65 C66 H66 119.5 . . ?
C61 C66 H66 119.5 . . ?
C68 C67 C72 118.4(4) . . ?
C68 C67 P2 120.3(4) . . ?
C72 C67 P2 121.2(4) . . ?
C69 C68 C67 120.6(5) . . ?
C69 C68 H68 119.7 . . ?
C67 C68 H68 119.7 . . ?
C68 C69 C70 120.1(5) . . ?
C68 C69 H69 119.9 . . ?
C70 C69 H69 119.9 . . ?
C71 C70 C69 120.4(5) . . ?
C71 C70 H70 119.8 . . ?
C69 C70 H70 119.8 . . ?
C70 C71 C72 119.6(5) . . ?
C70 C71 H71 120.2 . . ?
C72 C71 H71 120.2 . . ?
C71 C72 C67 120.8(5) . . ?
C71 C72 H72 119.6 . . ?
C67 C72 H72 119.6 . . ?
C78 C73 C74 119.5(5) . . ?
C78 C73 P2 121.1(4) . . ?
C74 C73 P2 119.4(4) . . ?
C75 C74 C73 119.9(5) . . ?
C75 C74 H74 120.0 . . ?
C73 C74 H74 120.0 . . ?
C76 C75 C74 120.6(5) . . ?
C76 C75 H75 119.7 . . ?
C74 C75 H75 119.7 . . ?
C75 C76 C77 119.4(5) . . ?
C75 C76 H76 120.3 . . ?
C77 C76 H76 120.3 . . ?
C78 C77 C76 120.7(5) . . ?
C78 C77 H77 119.7 . . ?
C76 C77 H77 119.7 . . ?
C77 C78 C73 119.9(4) . . ?
C77 C78 H78 120.0 . . ?
C73 C78 H78 120.0 . . ?
C84 C79 C80 120.0(4) . . ?
C84 C79 P2 121.1(4) . . ?
C80 C79 P2 118.0(4) . . ?
C81 C80 C79 119.6(5) . . ?
C81 C80 H80 120.2 . . ?
C79 C80 H80 120.2 . . ?
C82 C81 C80 120.1(5) . . ?
C82 C81 H81 119.9 . . ?
C80 C81 H81 119.9 . . ?
C81 C82 C83 120.8(5) . . ?
C81 C82 H82 119.6 . . ?
C83 C82 H82 119.6 . . ?
C82 C83 C84 119.6(5) . . ?
C82 C83 H83 120.2 . . ?
C84 C83 H83 120.2 . . ?
C79 C84 C83 119.8(5) . . ?
C79 C84 H84 120.1 . . ?
C83 C84 H84 120.1 . . ?
C86 C85 C90 119.2(4) . . ?
C86 C85 P2 121.0(3) . . ?
C90 C85 P2 119.4(4) . . ?
C87 C86 C85 120.5(4) . . ?
C87 C86 H86 119.8 . . ?
C85 C86 H86 119.8 . . ?
C86 C87 C88 120.7(5) . . ?
C86 C87 H87 119.6 . . ?
C88 C87 H87 119.6 . . ?
C87 C88 C89 120.3(5) . . ?
C87 C88 H88 119.9 . . ?
C89 C88 H88 119.9 . . ?
C88 C89 C90 119.5(4) . . ?
C88 C89 H89 120.3 . . ?
C90 C89 H89 120.3 . . ?
C89 C90 C85 119.8(4) . . ?
C89 C90 H90 120.1 . . ?
C85 C90 H90 120.1 . . ?
C92 C91 C96 120.4(4) . . ?
C92 C91 P3 119.5(4) . . ?
C96 C91 P3 120.1(4) . . ?
C93 C92 C91 119.4(5) . . ?
C93 C92 H92 120.3 . . ?
C91 C92 H92 120.3 . . ?
C94 C93 C92 120.1(5) . . ?
C94 C93 H93 120.0 . . ?
C92 C93 H93 120.0 . . ?
C95 C94 C93 120.6(5) . . ?
C95 C94 H94 119.7 . . ?
C93 C94 H94 119.7 . . ?
C94 C95 C96 120.1(5) . . ?
C94 C95 H95 119.9 . . ?
C96 C95 H95 119.9 . . ?
C91 C96 C95 119.4(5) . . ?
C91 C96 H96 120.3 . . ?
C95 C96 H96 120.3 . . ?
C102 C97 C98 118.2(4) . . ?
C102 C97 P3 121.9(4) . . ?
C98 C97 P3 119.9(4) . . ?
C99 C98 C97 120.3(4) . . ?
C99 C98 H98 119.8 . . ?
C97 C98 H98 119.8 . . ?
C98 C99 C100 120.3(4) . . ?
C98 C99 H99 119.8 . . ?
C100 C99 H99 119.8 . . ?
C101 C100 C99 120.0(5) . . ?
C101 C100 H100 120.0 . . ?
C99 C100 H100 120.0 . . ?
C100 C101 C102 120.2(5) . . ?
C100 C101 H101 119.9 . . ?
C102 C101 H101 119.9 . . ?
C101 C102 C97 120.8(4) . . ?
C101 C102 H102 119.6 . . ?
C97 C102 H102 119.6 . . ?
C108 C103 C104 119.5(4) . . ?
C108 C103 P3 121.3(3) . . ?
C104 C103 P3 118.9(4) . . ?
C105 C104 C103 120.5(5) . . ?
C105 C104 H104 119.7 . . ?
C103 C104 H104 119.7 . . ?
C104 C105 C106 120.2(5) . . ?
C104 C105 H105 119.9 . . ?
C106 C105 H105 119.9 . . ?
C107 C106 C105 119.8(5) . . ?
C107 C106 H106 120.1 . . ?
C105 C106 H106 120.1 . . ?
C106 C107 C108 120.6(5) . . ?
C106 C107 H107 119.7 . . ?
C108 C107 H107 119.7 . . ?
C107 C108 C103 119.3(4) . . ?
C107 C108 H108 120.4 . . ?
C103 C108 H108 120.4 . . ?
C110 C109 C114 119.9(4) . . ?
C110 C109 P3 120.5(4) . . ?
C114 C109 P3 119.4(4) . . ?
C111 C110 C109 119.3(4) . . ?
C111 C110 H110 120.3 . . ?
C109 C110 H110 120.3 . . ?
C110 C111 C112 120.4(5) . . ?
C110 C111 H111 119.8 . . ?
C112 C111 H111 119.8 . . ?
C111 C112 C113 120.2(5) . . ?
C111 C112 H112 119.9 . . ?
C113 C112 H112 119.9 . . ?
C114 C113 C112 120.0(5) . . ?
C114 C113 H113 120.0 . . ?
C112 C113 H113 120.0 . . ?
C113 C114 C109 120.2(5) . . ?
C113 C114 H114 119.9 . . ?
C109 C114 H114 119.9 . . ?
C120 C115 C116 119.5(5) . . ?
C120 C115 P4 121.2(4) . . ?
C116 C115 P4 119.2(4) . . ?
C117 C116 C115 120.6(5) . . ?
C117 C116 H116 119.7 . . ?
C115 C116 H116 119.7 . . ?
C118 C117 C116 119.1(5) . . ?
C118 C117 H117 120.4 . . ?
C116 C117 H117 120.4 . . ?
C117 C118 C119 120.9(5) . . ?
C117 C118 H118 119.6 . . ?
C119 C118 H118 119.6 . . ?
C118 C119 C120 120.3(5) . . ?
C118 C119 H119 119.9 . . ?
C120 C119 H119 119.9 . . ?
C119 C120 C115 119.6(5) . . ?
C119 C120 H120 120.2 . . ?
C115 C120 H120 120.2 . . ?
C122 C121 C126 119.6(5) . . ?
C122 C121 P4 119.5(4) . . ?
C126 C121 P4 121.0(4) . . ?
C121 C122 C123 119.7(4) . . ?
C121 C122 H122 120.1 . . ?
C123 C122 H122 120.1 . . ?
C124 C123 C122 119.8(5) . . ?
C124 C123 H123 120.1 . . ?
C122 C123 H123 120.1 . . ?
C125 C124 C123 120.3(5) . . ?
C125 C124 H124 119.9 . . ?
C123 C124 H124 119.9 . . ?
C126 C125 C124 120.7(5) . . ?
C126 C125 H125 119.6 . . ?
C124 C125 H125 119.6 . . ?
C125 C126 C121 119.9(5) . . ?
C125 C126 H126 120.1 . . ?
C121 C126 H126 120.1 . . ?
C128 C127 C132 120.5(4) . . ?
C128 C127 P4 120.6(4) . . ?
C132 C127 P4 119.0(4) . . ?
C127 C128 C129 119.2(5) . . ?
C127 C128 H128 120.4 . . ?
C129 C128 H128 120.4 . . ?
C130 C129 C128 120.0(5) . . ?
C130 C129 H129 120.0 . . ?
C128 C129 H129 120.0 . . ?
C131 C130 C129 120.8(5) . . ?
C131 C130 H130 119.6 . . ?
C129 C130 H130 119.6 . . ?
C130 C131 C132 119.5(5) . . ?
C130 C131 H131 120.2 . . ?
C132 C131 H131 120.2 . . ?
C131 C132 C127 120.0(5) . . ?
C131 C132 H132 120.0 . . ?
C127 C132 H132 120.0 . . ?
C138 C133 C134 118.3(4) . . ?
C138 C133 P4 120.6(4) . . ?
C134 C133 P4 120.7(4) . . ?
C135 C134 C133 119.9(5) . . ?
C135 C134 H134 120.0 . . ?
C133 C134 H134 120.0 . . ?
C136 C135 C134 120.3(5) . . ?
C136 C135 H135 119.9 . . ?
C134 C135 H135 119.9 . . ?
C137 C136 C135 120.9(5) . . ?
C137 C136 H136 119.5 . . ?
C135 C136 H136 119.5 . . ?
C136 C137 C138 119.6(5) . . ?
C136 C137 H137 120.2 . . ?
C138 C137 H137 120.2 . . ?
C137 C138 C133 121.0(5) . . ?
C137 C138 H138 119.5 . . ?
C133 C138 H138 119.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O39 H39A O11 0.99 2.17 2.912(4) 130.8 .
O39 H39A O24 0.99 2.08 2.734(4) 121.5 .
O39 H39B O13 0.83 2.19 2.930(4) 147.9 .
O40 H40A O16 0.94 2.36 2.841(4) 111.9 1_456
O40 H40A O19 0.94 1.87 2.799(4) 170.9 1_456
O40 H40A O20 0.94 2.32 2.829(4) 113.9 1_456
O40 H40B O18 0.86 1.96 2.801(4) 164.8 1_456
O41 H41A O6 0.93 2.05 2.875(4) 145.9 .
O41 H41B O37 0.87 2.00 2.858(4) 168.2 .
O42 H42A O27 0.99 1.98 2.903(4) 152.8 .
O42 H42B O28 0.99 2.55 3.107(5) 115.5 .
C32 H32 O33 0.95 2.30 2.768(6) 109.9 .
C54 H54 O42 0.95 2.41 3.219(6) 142.7 2_656
C56 H56 O42 0.95 2.46 3.342(6) 154.0 1_455
C68 H68 O17 0.95 2.38 3.142(6) 136.7 1_455
C78 H78 O17 0.95 2.48 3.383(6) 158.8 1_455
C92 H92 O12 0.95 2.43 3.332(6) 158.4 2_665
C122 H122 O37 0.95 2.56 3.355(6) 140.9 2_666
C132 H132 O23 0.95 2.58 3.261(6) 128.6 1_556

_refine_diff_density_max         1.540
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.134

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7
_database_code_depnum_ccdc_archive 'CCDC 1893020'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2019-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C136 H252 Cu5 N20 O49 S8'
_chemical_formula_weight         3525.74

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.9382(9)
_cell_length_b                   16.2333(11)
_cell_length_c                   20.2169(14)
_cell_angle_alpha                74.324(3)
_cell_angle_beta                 68.424(3)
_cell_angle_gamma                64.208(3)
_cell_volume                     4069.1(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    195268
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_F_000             1873
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and ten ω scans with 2° steps (709 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            195268
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.325
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             15436
_reflns_number_gt                11140
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. One solvent water molecule was given an
 occupancy factor of 0.5 in order that it retains an acceptable displacement
 parameter. The H atoms bound to O and N atoms were found on a 
 difference Fourier map and all the others were introduced at calculated
 positions; all were treated as riding atoms with an isotropic displacement
 parameter equal to 1.2 times that of the parent atom (1.5 for CH₃, with
 optimized geometry). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0494P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15436
_refine_ls_number_parameters     1003
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.0971
_refine_ls_wR_factor_gt          0.0900
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.001
_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_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
Cu1 Cu 0.20366(3) 0.63245(2) 0.42971(2) 0.02633(9) Uani 1 1 d . . . . .
Cu2 Cu 0.61907(2) 1.03170(2) 0.26697(2) 0.02458(9) Uani 1 1 d . . . . .
Cu3 Cu 1.0000 0.5000 0.0000 0.02295(11) Uani 1 2 d S . P . .
S1 S 0.22092(5) 0.48852(4) 0.32203(4) 0.02489(15) Uani 1 1 d . . . . .
S2 S -0.15241(5) 1.04354(4) 0.29981(4) 0.02362(15) Uani 1 1 d . . . . .
S3 S 0.38561(5) 1.02892(4) 0.24311(4) 0.02452(15) Uani 1 1 d . . . . .
S4 S 0.76244(5) 0.55829(4) 0.15897(4) 0.02334(15) Uani 1 1 d . . . . .
O1 O 0.15508(14) 0.54982(12) 0.37749(10) 0.0273(4) Uani 1 1 d . . . . .
O2 O 0.17065(15) 0.43309(12) 0.31556(10) 0.0324(5) Uani 1 1 d . . . . .
O3 O 0.32436(14) 0.43396(12) 0.33085(10) 0.0303(4) Uani 1 1 d . . . . .
O4 O -0.22569(13) 0.99998(12) 0.31167(10) 0.0266(4) Uani 1 1 d . . . . .
O5 O -0.19271(14) 1.14193(12) 0.27298(10) 0.0273(4) Uani 1 1 d . . . . .
O6 O -0.11768(14) 1.02515(13) 0.36303(10) 0.0291(4) Uani 1 1 d . . . . .
O7 O 0.47871(14) 1.05129(12) 0.21760(10) 0.0271(4) Uani 1 1 d . . . . .
O8 O 0.39952(14) 0.94388(12) 0.29451(10) 0.0280(4) Uani 1 1 d . . . . .
O9 O 0.29117(14) 1.10414(13) 0.27119(11) 0.0318(5) Uani 1 1 d . . . . .
O10 O 0.85156(13) 0.57790(12) 0.10614(10) 0.0263(4) Uani 1 1 d . . . . .
O11 O 0.72913(14) 0.59395(12) 0.22601(10) 0.0295(4) Uani 1 1 d . . . . .
O12 O 0.77937(14) 0.46012(11) 0.16772(10) 0.0262(4) Uani 1 1 d . . . . .
O13 O 0.28274(13) 0.72411(11) 0.04309(9) 0.0229(4) Uani 1 1 d . . . . .
O14 O 0.18519(14) 0.89373(12) 0.04826(10) 0.0276(4) Uani 1 1 d . . . . .
H14 H 0.2147 0.8279 0.0479 0.033 Uiso 1 1 d R U . . .
O15 O 0.35855(13) 0.95154(12) -0.01677(9) 0.0247(4) Uani 1 1 d . . . . .
H15 H 0.3917 0.8840 -0.0203 0.030 Uiso 1 1 d R U . . .
O16 O 0.44177(13) 0.76247(11) 0.00610(9) 0.0244(4) Uani 1 1 d . . . . .
H16 H 0.3843 0.7515 0.0127 0.029 Uiso 1 1 d R U . . .
O17 O 0.18334(15) 1.29248(13) 0.24770(10) 0.0330(5) Uani 1 1 d . . . . .
H17A H 0.1974 1.3301 0.2618 0.040 Uiso 1 1 d R U . . .
H17B H 0.2337 1.2356 0.2587 0.040 Uiso 1 1 d R U . . .
O18 O -0.17024(15) 1.30818(13) 0.27168(11) 0.0346(5) Uani 1 1 d . . . . .
H18A H -0.1837 1.2574 0.2657 0.042 Uiso 1 1 d R U . . .
H18B H -0.1810 1.3558 0.2316 0.042 Uiso 1 1 d R U . . .
O19 O 0.03173(16) 1.07772(14) 0.37381(11) 0.0376(5) Uani 1 1 d . . . . .
H19A H -0.0106 1.0625 0.3629 0.045 Uiso 1 1 d R U . . .
H19B H 0.0541 1.1162 0.3305 0.045 Uiso 1 1 d R U . . .
O20 O -0.30363(19) 1.04218(18) 0.48346(14) 0.0648(7) Uani 1 1 d . . . . .
H20A H -0.2502 1.0372 0.4365 0.078 Uiso 1 1 d R U . . .
H20B H -0.2868 1.0451 0.5178 0.078 Uiso 1 1 d R U . . .
O21 O 0.21652(17) 0.95320(16) 0.40852(12) 0.0502(6) Uani 1 1 d . . . . .
H21A H 0.2785 0.9478 0.3714 0.060 Uiso 1 1 d R U . . .
H21B H 0.1657 1.0008 0.3993 0.060 Uiso 1 1 d R U . . .
O22 O 0.04374(16) 1.21407(14) 0.25785(11) 0.0373(5) Uani 1 1 d . . . . .
H22A H 0.0830 1.2468 0.2613 0.045 Uiso 1 1 d R U . . .
H22B H -0.0206 1.2542 0.2603 0.045 Uiso 1 1 d R U . . .
O23 O -0.25322(17) 1.32928(16) 0.41820(12) 0.0464(6) Uani 1 1 d . . . . .
H23A H -0.2298 1.3202 0.3671 0.056 Uiso 1 1 d R U . . .
H23B H -0.2045 1.2719 0.4318 0.056 Uiso 1 1 d R U . . .
O24 O -0.13284(16) 1.16606(14) 0.48782(11) 0.0392(5) Uani 1 1 d . . . . .
H24A H -0.0835 1.1353 0.4550 0.047 Uiso 1 1 d R U . . .
H24B H -0.1584 1.1184 0.5144 0.047 Uiso 1 1 d R U . . .
O25 O -0.4145(3) 1.2386(3) 0.4664(2) 0.0409(10) Uani 0.5 1 d . . P . .
H25A H -0.3849 1.1854 0.4582 0.049 Uiso 0.5 1 d R U P . .
H25B H -0.3696 1.2628 0.4445 0.049 Uiso 0.5 1 d R U P . .
N1 N 0.18987(18) 0.55839(15) 0.52788(12) 0.0297(5) Uani 1 1 d . . . . .
H1 H 0.2138 0.5818 0.5468 0.036 Uiso 1 1 d R U . . .
N2 N 0.35394(17) 0.54236(16) 0.40622(13) 0.0299(5) Uani 1 1 d . . . . .
H2 H 0.3596 0.5081 0.3721 0.036 Uiso 1 1 d R U . . .
N3 N 0.22792(18) 0.71552(15) 0.33435(12) 0.0289(5) Uani 1 1 d . . . . .
H3 H 0.2255 0.6857 0.3020 0.035 Uiso 1 1 d R U . . .
N4 N 0.06060(17) 0.73196(15) 0.45585(12) 0.0273(5) Uani 1 1 d . . . . .
H4 H 0.0747 0.7687 0.4788 0.033 Uiso 1 1 d R U . . .
N5 N 0.53378(17) 1.09004(14) 0.35810(12) 0.0270(5) Uani 1 1 d . . . . .
H5 H 0.5821 1.0880 0.3777 0.032 Uiso 1 1 d R U . . .
N6 N 0.59327(17) 0.91605(14) 0.32537(12) 0.0247(5) Uani 1 1 d . . . . .
H6 H 0.5356 0.9232 0.3095 0.030 Uiso 1 1 d R U . . .
N7 N 0.70463(16) 0.97406(14) 0.17537(11) 0.0225(5) Uani 1 1 d . . . . .
H7 H 0.6614 0.9802 0.1491 0.027 Uiso 1 1 d R U . . .
N8 N 0.64556(16) 1.14770(14) 0.20934(11) 0.0229(5) Uani 1 1 d . . . . .
H8 H 0.6974 1.1406 0.2261 0.028 Uiso 1 1 d R U . . .
N9 N 0.88260(17) 0.56147(14) -0.04689(12) 0.0229(5) Uani 1 1 d . . . . .
H9 H 0.8270 0.5863 -0.0052 0.028 Uiso 1 1 d R U . . .
N10 N 1.03510(17) 0.61300(14) -0.04484(12) 0.0233(5) Uani 1 1 d . . . . .
H10 H 1.0880 0.5965 -0.0895 0.028 Uiso 1 1 d R U . . .
C1 C 0.2404(2) 0.56195(17) 0.24004(14) 0.0237(6) Uani 1 1 d . . . . .
C2 C 0.1567(2) 0.63819(17) 0.22370(14) 0.0211(6) Uani 1 1 d . . . . .
H2A H 0.0899 0.6521 0.2578 0.025 Uiso 1 1 calc R U . . .
C3 C 0.1694(2) 0.69413(17) 0.15814(14) 0.0217(6) Uani 1 1 d . . . . .
C4 C 0.2690(2) 0.67337(17) 0.10742(14) 0.0221(6) Uani 1 1 d . . . . .
C5 C 0.3541(2) 0.59643(18) 0.12502(14) 0.0229(6) Uani 1 1 d . . . . .
C6 C 0.3383(2) 0.54210(17) 0.19096(14) 0.0225(6) Uani 1 1 d . . . . .
H6A H 0.3953 0.4906 0.2027 0.027 Uiso 1 1 calc R U . . .
C7 C 0.0758(2) 0.77442(17) 0.14054(15) 0.0229(6) Uani 1 1 d . . . . .
H7A H 0.0131 0.7597 0.1675 0.027 Uiso 1 1 calc R U . . .
H7B H 0.0842 0.7801 0.0888 0.027 Uiso 1 1 calc R U . . .
C8 C 0.05760(19) 0.86737(17) 0.15736(14) 0.0213(6) Uani 1 1 d . . . . .
C9 C -0.02080(19) 0.90510(17) 0.21695(14) 0.0217(6) Uani 1 1 d . . . . .
H9A H -0.0599 0.8700 0.2495 0.026 Uiso 1 1 calc R U . . .
C10 C -0.04325(19) 0.99253(17) 0.23002(14) 0.0221(6) Uani 1 1 d . . . . .
C11 C 0.01855(19) 1.04168(18) 0.18526(14) 0.0233(6) Uani 1 1 d . . . . .
H11 H 0.0051 1.1005 0.1953 0.028 Uiso 1 1 calc R U . . .
C12 C 0.09883(19) 1.00600(17) 0.12664(14) 0.0215(6) Uani 1 1 d . . . . .
C13 C 0.11537(19) 0.92010(17) 0.11055(14) 0.0231(6) Uani 1 1 d . . . . .
C14 C 0.16837(19) 1.05726(17) 0.07756(15) 0.0232(6) Uani 1 1 d . . . . .
H14A H 0.1329 1.1234 0.0841 0.028 Uiso 1 1 calc R U . . .
H14B H 0.1795 1.0527 0.0271 0.028 Uiso 1 1 calc R U . . .
C15 C 0.2731(2) 1.01982(17) 0.09177(14) 0.0217(6) Uani 1 1 d . . . . .
C16 C 0.2806(2) 1.04033(17) 0.15211(14) 0.0233(6) Uani 1 1 d . . . . .
H16A H 0.2207 1.0796 0.1829 0.028 Uiso 1 1 calc R U . . .
C17 C 0.3747(2) 1.00371(17) 0.16702(14) 0.0216(6) Uani 1 1 d . . . . .
C18 C 0.4624(2) 0.94523(17) 0.12277(14) 0.0228(6) Uani 1 1 d . . . . .
H18 H 0.5263 0.9195 0.1341 0.027 Uiso 1 1 calc R U . . .
C19 C 0.4583(2) 0.92361(17) 0.06228(14) 0.0222(6) Uani 1 1 d . . . . .
C20 C 0.3631(2) 0.96374(17) 0.04647(14) 0.0212(6) Uani 1 1 d . . . . .
C21 C 0.5547(2) 0.85761(17) 0.01641(14) 0.0230(6) Uani 1 1 d . . . . .
H21C H 0.6159 0.8705 0.0118 0.028 Uiso 1 1 calc R U . . .
H21D H 0.5476 0.8675 -0.0322 0.028 Uiso 1 1 calc R U . . .
C22 C 0.57178(19) 0.75789(17) 0.04881(14) 0.0215(6) Uani 1 1 d . . . . .
C23 C 0.64636(19) 0.70867(17) 0.08491(14) 0.0220(6) Uani 1 1 d . . . . .
H23 H 0.6884 0.7372 0.0876 0.026 Uiso 1 1 calc R U . . .
C24 C 0.66090(19) 0.61810(17) 0.11728(14) 0.0217(6) Uani 1 1 d . . . . .
C25 C 0.59960(19) 0.57649(17) 0.11411(14) 0.0219(6) Uani 1 1 d . . . . .
H25 H 0.6087 0.5152 0.1371 0.026 Uiso 1 1 calc R U . . .
C26 C 0.52432(19) 0.62335(17) 0.07752(14) 0.0218(6) Uani 1 1 d . . . . .
C27 C 0.51093(19) 0.71413(17) 0.04467(14) 0.0219(6) Uani 1 1 d . . . . .
C28 C 0.46141(19) 0.57409(17) 0.07143(15) 0.0232(6) Uani 1 1 d . . . . .
H28A H 0.4539 0.5911 0.0223 0.028 Uiso 1 1 calc R U . . .
H28B H 0.5005 0.5067 0.0783 0.028 Uiso 1 1 calc R U . . .
C29 C 0.2673(2) 0.4642(2) 0.51465(17) 0.0381(7) Uani 1 1 d . . . . .
H29A H 0.2458 0.4361 0.4883 0.046 Uiso 1 1 calc R U . . .
H29B H 0.2740 0.4244 0.5607 0.046 Uiso 1 1 calc R U . . .
C30 C 0.3688(2) 0.4744(2) 0.47064(17) 0.0402(8) Uani 1 1 d . . . . .
H30A H 0.3940 0.4953 0.4996 0.048 Uiso 1 1 calc R U . . .
H30B H 0.4215 0.4140 0.4561 0.048 Uiso 1 1 calc R U . . .
C31 C 0.4377(2) 0.5807(2) 0.37037(17) 0.0374(7) Uani 1 1 d . . . . .
C32 C 0.4195(2) 0.6400(2) 0.29960(16) 0.0354(7) Uani 1 1 d . . . . .
H32A H 0.4831 0.6529 0.2715 0.042 Uiso 1 1 calc R U . . .
H32B H 0.4125 0.6019 0.2723 0.042 Uiso 1 1 calc R U . . .
C33 C 0.3281(2) 0.7310(2) 0.30198(16) 0.0326(7) Uani 1 1 d . . . . .
H33 H 0.3309 0.7684 0.3327 0.039 Uiso 1 1 calc R U . . .
C34 C 0.4277(3) 0.6419(3) 0.42208(19) 0.0540(10) Uani 1 1 d . . . . .
H34A H 0.3580 0.6901 0.4321 0.081 Uiso 1 1 calc R U . . .
H34B H 0.4795 0.6705 0.3997 0.081 Uiso 1 1 calc R U . . .
H34C H 0.4394 0.6035 0.4670 0.081 Uiso 1 1 calc R U . . .
C35 C 0.5444(2) 0.5023(3) 0.3531(2) 0.0566(10) Uani 1 1 d . . . . .
H35A H 0.5575 0.4640 0.3977 0.085 Uiso 1 1 calc R U . . .
H35B H 0.5982 0.5284 0.3284 0.085 Uiso 1 1 calc R U . . .
H35C H 0.5458 0.4644 0.3221 0.085 Uiso 1 1 calc R U . . .
C36 C 0.3352(3) 0.7842(2) 0.22623(16) 0.0407(8) Uani 1 1 d . . . . .
H36A H 0.4018 0.7923 0.2060 0.061 Uiso 1 1 calc R U . . .
H36B H 0.2783 0.8447 0.2284 0.061 Uiso 1 1 calc R U . . .
H36C H 0.3301 0.7494 0.1958 0.061 Uiso 1 1 calc R U . . .
C37 C 0.1343(2) 0.80367(19) 0.33909(16) 0.0327(7) Uani 1 1 d . . . . .
H37A H 0.1260 0.8316 0.2907 0.039 Uiso 1 1 calc R U . . .
H37B H 0.1426 0.8481 0.3594 0.039 Uiso 1 1 calc R U . . .
C38 C 0.0400(2) 0.7823(2) 0.38672(15) 0.0328(7) Uani 1 1 d . . . . .
H38A H -0.0218 0.8402 0.3949 0.039 Uiso 1 1 calc R U . . .
H38B H 0.0266 0.7439 0.3637 0.039 Uiso 1 1 calc R U . . .
C39 C -0.0285(2) 0.7115(2) 0.51292(16) 0.0325(7) Uani 1 1 d . . . . .
C40 C 0.0080(2) 0.6583(2) 0.57905(15) 0.0325(7) Uani 1 1 d . . . . .
H40A H 0.0391 0.6935 0.5906 0.039 Uiso 1 1 calc R U . . .
H40B H -0.0543 0.6580 0.6197 0.039 Uiso 1 1 calc R U . . .
C41 C 0.0855(2) 0.5590(2) 0.57595(16) 0.0364(7) Uani 1 1 d . . . . .
H41 H 0.0615 0.5251 0.5557 0.044 Uiso 1 1 calc R U . . .
C42 C -0.1188(2) 0.8032(2) 0.53546(19) 0.0491(9) Uani 1 1 d . . . . .
H42A H -0.0937 0.8385 0.5519 0.074 Uiso 1 1 calc R U . . .
H42B H -0.1752 0.7895 0.5744 0.074 Uiso 1 1 calc R U . . .
H42C H -0.1445 0.8395 0.4943 0.074 Uiso 1 1 calc R U . . .
C43 C -0.0698(3) 0.6595(2) 0.48673(19) 0.0455(8) Uani 1 1 d . . . . .
H43A H -0.1059 0.7008 0.4514 0.068 Uiso 1 1 calc R U . . .
H43B H -0.1183 0.6373 0.5274 0.068 Uiso 1 1 calc R U . . .
H43C H -0.0119 0.6068 0.4644 0.068 Uiso 1 1 calc R U . . .
C44 C 0.0904(3) 0.5124(3) 0.65214(19) 0.0623(11) Uani 1 1 d . . . . .
H44A H 0.1372 0.4475 0.6506 0.093 Uiso 1 1 calc R U . . .
H44B H 0.0207 0.5161 0.6827 0.093 Uiso 1 1 calc R U . . .
H44C H 0.1162 0.5439 0.6717 0.093 Uiso 1 1 calc R U . . .
C45 C 0.4791(2) 1.02938(18) 0.40639(15) 0.0298(6) Uani 1 1 d . . . . .
H45A H 0.4181 1.0399 0.3918 0.036 Uiso 1 1 calc R U . . .
H45B H 0.4545 1.0430 0.4563 0.036 Uiso 1 1 calc R U . . .
C46 C 0.5541(2) 0.93026(18) 0.40176(15) 0.0291(6) Uani 1 1 d . . . . .
H46A H 0.6124 0.9182 0.4200 0.035 Uiso 1 1 calc R U . . .
H46B H 0.5183 0.8877 0.4310 0.035 Uiso 1 1 calc R U . . .
C47 C 0.6680(2) 0.81978(18) 0.31092(15) 0.0250(6) Uani 1 1 d . . . . .
C48 C 0.7023(2) 0.81813(17) 0.22917(14) 0.0246(6) Uani 1 1 d . . . . .
H48A H 0.7411 0.7529 0.2203 0.030 Uiso 1 1 calc R U . . .
H48B H 0.6390 0.8410 0.2137 0.030 Uiso 1 1 calc R U . . .
C49 C 0.7687(2) 0.87263(17) 0.18114(14) 0.0241(6) Uani 1 1 d . . . . .
H49 H 0.8234 0.8612 0.2035 0.029 Uiso 1 1 calc R U . . .
C50 C 0.6116(2) 0.75211(19) 0.34661(16) 0.0315(7) Uani 1 1 d . . . . .
H50A H 0.5896 0.7505 0.3988 0.047 Uiso 1 1 calc R U . . .
H50B H 0.6587 0.6903 0.3339 0.047 Uiso 1 1 calc R U . . .
H50C H 0.5506 0.7725 0.3298 0.047 Uiso 1 1 calc R U . . .
C51 C 0.7603(2) 0.79116(19) 0.33921(15) 0.0288(6) Uani 1 1 d . . . . .
H51A H 0.7865 0.8411 0.3247 0.043 Uiso 1 1 calc R U . . .
H51B H 0.8154 0.7355 0.3194 0.043 Uiso 1 1 calc R U . . .
H51C H 0.7384 0.7785 0.3917 0.043 Uiso 1 1 calc R U . . .
C52 C 0.8229(2) 0.83803(19) 0.10792(15) 0.0309(7) Uani 1 1 d . . . . .
H52A H 0.7713 0.8548 0.0827 0.046 Uiso 1 1 calc R U . . .
H52B H 0.8583 0.7708 0.1145 0.046 Uiso 1 1 calc R U . . .
H52C H 0.8739 0.8663 0.0796 0.046 Uiso 1 1 calc R U . . .
C53 C 0.7636(2) 1.03257(17) 0.12869(14) 0.0235(6) Uani 1 1 d . . . . .
H53A H 0.7898 1.0192 0.0786 0.028 Uiso 1 1 calc R U . . .
H53B H 0.8237 1.0198 0.1452 0.028 Uiso 1 1 calc R U . . .
C54 C 0.6911(2) 1.13201(18) 0.13288(14) 0.0267(6) Uani 1 1 d . . . . .
H54A H 0.7296 1.1730 0.1057 0.032 Uiso 1 1 calc R U . . .
H54B H 0.6352 1.1462 0.1115 0.032 Uiso 1 1 calc R U . . .
C55 C 0.5651(2) 1.24304(17) 0.22242(15) 0.0253(6) Uani 1 1 d . . . . .
C56 C 0.5277(2) 1.24674(18) 0.30369(15) 0.0302(7) Uani 1 1 d . . . . .
H56A H 0.5896 1.2268 0.3202 0.036 Uiso 1 1 calc R U . . .
H56B H 0.4860 1.3120 0.3117 0.036 Uiso 1 1 calc R U . . .
C57 C 0.4635(2) 1.18974(18) 0.35117(16) 0.0342(7) Uani 1 1 d . . . . .
H57 H 0.4124 1.1966 0.3272 0.041 Uiso 1 1 calc R U . . .
C58 C 0.4755(2) 1.26454(18) 0.19315(16) 0.0289(6) Uani 1 1 d . . . . .
H58A H 0.4989 1.2745 0.1406 0.043 Uiso 1 1 calc R U . . .
H58B H 0.4179 1.3203 0.2109 0.043 Uiso 1 1 calc R U . . .
H58C H 0.4523 1.2126 0.2091 0.043 Uiso 1 1 calc R U . . .
C59 C 0.6158(2) 1.31481(19) 0.18592(17) 0.0325(7) Uani 1 1 d . . . . .
H59A H 0.6753 1.2991 0.2032 0.049 Uiso 1 1 calc R U . . .
H59B H 0.5651 1.3762 0.1975 0.049 Uiso 1 1 calc R U . . .
H59C H 0.6394 1.3148 0.1338 0.049 Uiso 1 1 calc R U . . .
C60 C 0.4032(3) 1.2243(2) 0.42438(17) 0.0545(10) Uani 1 1 d . . . . .
H60A H 0.3656 1.1845 0.4550 0.082 Uiso 1 1 calc R U . . .
H60B H 0.3536 1.2877 0.4179 0.082 Uiso 1 1 calc R U . . .
H60C H 0.4517 1.2228 0.4471 0.082 Uiso 1 1 calc R U . . .
C61 C 0.9041(2) 0.63919(18) -0.10016(15) 0.0280(6) Uani 1 1 d . . . . .
H61A H 0.8397 0.6844 -0.1119 0.034 Uiso 1 1 calc R U . . .
H61B H 0.9563 0.6157 -0.1449 0.034 Uiso 1 1 calc R U . . .
C62 C 0.9445(2) 0.68465(17) -0.06792(15) 0.0263(6) Uani 1 1 d . . . . .
H62A H 0.9656 0.7330 -0.1038 0.032 Uiso 1 1 calc R U . . .
H62B H 0.8896 0.7141 -0.0262 0.032 Uiso 1 1 calc R U . . .
C63 C 1.0754(2) 0.64937(17) -0.00582(15) 0.0235(6) Uani 1 1 d . . . . .
H63 H 1.0199 0.6708 0.0391 0.028 Uiso 1 1 calc R U . . .
C64 C 1.1701(2) 0.57207(17) 0.01442(15) 0.0240(6) Uani 1 1 d . . . . .
H64A H 1.2057 0.6007 0.0286 0.029 Uiso 1 1 calc R U . . .
H64B H 1.2186 0.5433 -0.0292 0.029 Uiso 1 1 calc R U . . .
C65 C 1.1516(2) 0.49471(18) 0.07453(14) 0.0233(6) Uani 1 1 d . . . . .
C66 C 1.1052(2) 0.73072(18) -0.05170(15) 0.0287(6) Uani 1 1 d . . . . .
H66A H 1.1509 0.7135 -0.0991 0.043 Uiso 1 1 calc R U . . .
H66B H 1.1414 0.7467 -0.0282 0.043 Uiso 1 1 calc R U . . .
H66C H 1.0423 0.7840 -0.0571 0.043 Uiso 1 1 calc R U . . .
C67 C 1.2559(2) 0.43381(19) 0.09054(15) 0.0282(6) Uani 1 1 d . . . . .
H67A H 1.2470 0.3835 0.1288 0.042 Uiso 1 1 calc R U . . .
H67B H 1.2797 0.4712 0.1059 0.042 Uiso 1 1 calc R U . . .
H67C H 1.3076 0.4080 0.0471 0.042 Uiso 1 1 calc R U . . .
C68 C 1.0690(2) 0.53240(18) 0.14258(14) 0.0253(6) Uani 1 1 d . . . . .
H68A H 0.9999 0.5558 0.1359 0.038 Uiso 1 1 calc R U . . .
H68B H 1.0802 0.5826 0.1523 0.038 Uiso 1 1 calc R U . . .
H68C H 1.0739 0.4829 0.1832 0.038 Uiso 1 1 calc R U . . .


_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
Cu1 N1 2.013(2) . ?
Cu1 N4 2.021(2) . ?
Cu1 N2 2.034(2) . ?
Cu1 N3 2.043(2) . ?
Cu1 O1 2.3698(18) . ?
Cu2 N5 2.020(2) . ?
Cu2 N7 2.023(2) . ?
Cu2 N6 2.041(2) . ?
Cu2 N8 2.045(2) . ?
Cu2 O7 2.5062(17) . ?
Cu2 O4 2.5905(17) 1_655 ?
Cu3 N10 2.012(2) . ?
Cu3 N10 2.012(2) 2_765 ?
Cu3 N9 2.039(2) . ?
Cu3 N9 2.039(2) 2_765 ?
Cu3 O10 2.5783(18) . ?
S1 O2 1.4540(18) . ?
S1 O3 1.4595(19) . ?
S1 O1 1.4680(19) . ?
S1 C1 1.770(3) . ?
S2 O6 1.4625(19) . ?
S2 O5 1.4638(18) . ?
S2 O4 1.4645(18) . ?
S2 C10 1.761(3) . ?
S3 O9 1.4458(19) . ?
S3 O7 1.4638(18) . ?
S3 O8 1.4705(19) . ?
S3 C17 1.773(3) . ?
S4 O11 1.4480(19) . ?
S4 O10 1.4676(18) . ?
S4 O12 1.4713(18) . ?
S4 C24 1.781(3) . ?
O13 C4 1.336(3) . ?
O14 C13 1.339(3) . ?
O14 H14 0.9639 . ?
O15 C20 1.376(3) . ?
O15 H15 0.9982 . ?
O16 C27 1.359(3) . ?
O16 H16 0.9077 . ?
O17 H17A 0.8646 . ?
O17 H17B 0.9356 . ?
O18 H18A 0.9756 . ?
O18 H18B 0.9634 . ?
O19 H19A 0.8818 . ?
O19 H19B 0.9692 . ?
O20 H20A 0.9863 . ?
O20 H20B 0.8380 . ?
O21 H21A 0.9388 . ?
O21 H21B 0.8507 . ?
O22 H22A 0.9760 . ?
O22 H22B 0.8874 . ?
O23 H23A 0.9919 . ?
O23 H23B 0.9437 . ?
O24 H24A 0.8548 . ?
O24 H24B 0.9560 . ?
O25 H25A 0.8111 . ?
O25 H25B 0.8479 . ?
N1 C29 1.483(4) . ?
N1 C41 1.501(4) . ?
N1 H1 0.8470 . ?
N2 C30 1.479(4) . ?
N2 C31 1.499(4) . ?
N2 H2 0.9559 . ?
N3 C37 1.499(4) . ?
N3 C33 1.499(3) . ?
N3 H3 0.9326 . ?
N4 C38 1.482(3) . ?
N4 C39 1.504(3) . ?
N4 H4 0.9735 . ?
N5 C45 1.478(3) . ?
N5 C57 1.499(3) . ?
N5 H5 0.9283 . ?
N6 C46 1.480(3) . ?
N6 C47 1.504(3) . ?
N6 H6 0.9763 . ?
N7 C53 1.483(3) . ?
N7 C49 1.499(3) . ?
N7 H7 0.9374 . ?
N8 C54 1.485(3) . ?
N8 C55 1.510(3) . ?
N8 H8 0.9065 . ?
N9 C61 1.490(3) . ?
N9 C65 1.515(3) 2_765 ?
N9 H9 0.9701 . ?
N10 C62 1.484(3) . ?
N10 C63 1.498(3) . ?
N10 H10 0.9659 . ?
C1 C6 1.387(4) . ?
C1 C2 1.393(4) . ?
C2 C3 1.390(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.416(4) . ?
C3 C7 1.520(3) . ?
C4 C5 1.420(4) . ?
C5 C6 1.388(4) . ?
C5 C28 1.517(4) . ?
C6 H6A 0.9500 . ?
C7 C8 1.523(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.391(4) . ?
C8 C13 1.406(4) . ?
C9 C10 1.386(3) . ?
C9 H9A 0.9500 . ?
C10 C11 1.394(4) . ?
C11 C12 1.378(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.413(4) . ?
C12 C14 1.518(3) . ?
C14 C15 1.519(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.399(4) . ?
C15 C16 1.401(4) . ?
C16 C17 1.381(3) . ?
C16 H16A 0.9500 . ?
C17 C18 1.390(4) . ?
C18 C19 1.388(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.401(3) . ?
C19 C21 1.515(4) . ?
C21 C22 1.518(3) . ?
C21 H21C 0.9900 . ?
C21 H21D 0.9900 . ?
C22 C23 1.386(4) . ?
C22 C27 1.410(3) . ?
C23 C24 1.394(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(3) . ?
C25 C26 1.398(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.402(4) . ?
C26 C28 1.526(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.505(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C35 1.532(5) . ?
C31 C32 1.537(4) . ?
C31 C34 1.555(4) . ?
C32 C33 1.512(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C36 1.532(4) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.510(4) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C43 1.520(4) . ?
C39 C40 1.527(4) . ?
C39 C42 1.552(4) . ?
C40 C41 1.523(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C44 1.535(4) . ?
C41 H41 1.0000 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.513(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C51 1.525(4) . ?
C47 C50 1.538(4) . ?
C47 C48 1.544(4) . ?
C48 C49 1.517(4) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C52 1.528(4) . ?
C49 H49 1.0000 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.507(4) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C58 1.525(4) . ?
C55 C56 1.538(4) . ?
C55 C59 1.539(4) . ?
C56 C57 1.520(4) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C60 1.531(4) . ?
C57 H57 1.0000 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.507(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.532(4) . ?
C63 C66 1.532(4) . ?
C63 H63 1.0000 . ?
C64 C65 1.536(4) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 N9 1.515(3) 2_765 ?
C65 C68 1.530(4) . ?
C65 C67 1.539(4) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?

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 Cu1 N4 95.43(9) . . ?
N1 Cu1 N2 85.03(9) . . ?
N4 Cu1 N2 173.03(9) . . ?
N1 Cu1 N3 172.04(9) . . ?
N4 Cu1 N3 85.52(9) . . ?
N2 Cu1 N3 93.07(9) . . ?
N1 Cu1 O1 97.94(8) . . ?
N4 Cu1 O1 94.79(8) . . ?
N2 Cu1 O1 92.02(8) . . ?
N3 Cu1 O1 89.84(8) . . ?
N5 Cu2 N7 179.62(9) . . ?
N5 Cu2 N6 85.50(9) . . ?
N7 Cu2 N6 94.88(8) . . ?
N5 Cu2 N8 94.09(9) . . ?
N7 Cu2 N8 85.53(8) . . ?
N6 Cu2 N8 179.32(9) . . ?
N5 Cu2 O7 100.89(8) . . ?
N7 Cu2 O7 79.16(7) . . ?
N6 Cu2 O7 84.05(7) . . ?
N8 Cu2 O7 96.56(7) . . ?
N5 Cu2 O4 83.57(8) . 1_655 ?
N7 Cu2 O4 96.39(7) . 1_655 ?
N6 Cu2 O4 94.47(7) . 1_655 ?
N8 Cu2 O4 84.95(7) . 1_655 ?
O7 Cu2 O4 175.15(6) . 1_655 ?
N10 Cu3 N10 180.0 . 2_765 ?
N10 Cu3 N9 86.01(8) . . ?
N10 Cu3 N9 93.99(8) 2_765 . ?
N10 Cu3 N9 93.99(8) . 2_765 ?
N10 Cu3 N9 86.01(8) 2_765 2_765 ?
N9 Cu3 N9 180.00(10) . 2_765 ?
N10 Cu3 O10 94.01(7) . . ?
N10 Cu3 O10 85.99(7) 2_765 . ?
N9 Cu3 O10 80.89(7) . . ?
N9 Cu3 O10 99.11(7) 2_765 . ?
O2 S1 O3 113.26(11) . . ?
O2 S1 O1 112.41(11) . . ?
O3 S1 O1 111.95(11) . . ?
O2 S1 C1 107.46(12) . . ?
O3 S1 C1 105.30(12) . . ?
O1 S1 C1 105.80(11) . . ?
O6 S2 O5 112.94(11) . . ?
O6 S2 O4 111.94(11) . . ?
O5 S2 O4 112.02(11) . . ?
O6 S2 C10 107.72(12) . . ?
O5 S2 C10 105.51(12) . . ?
O4 S2 C10 106.16(11) . . ?
O9 S3 O7 113.73(11) . . ?
O9 S3 O8 111.98(12) . . ?
O7 S3 O8 110.81(11) . . ?
O9 S3 C17 107.83(12) . . ?
O7 S3 C17 105.75(11) . . ?
O8 S3 C17 106.21(11) . . ?
O11 S4 O10 113.60(11) . . ?
O11 S4 O12 113.87(11) . . ?
O10 S4 O12 111.32(11) . . ?
O11 S4 C24 107.98(12) . . ?
O10 S4 C24 103.89(11) . . ?
O12 S4 C24 105.25(11) . . ?
S1 O1 Cu1 128.22(10) . . ?
S3 O7 Cu2 136.92(11) . . ?
S4 O10 Cu3 134.99(10) . . ?
C13 O14 H14 113.6 . . ?
C20 O15 H15 107.7 . . ?
C27 O16 H16 124.2 . . ?
H17A O17 H17B 101.8 . . ?
H18A O18 H18B 108.3 . . ?
H19A O19 H19B 102.4 . . ?
H20A O20 H20B 116.3 . . ?
H21A O21 H21B 111.9 . . ?
H22A O22 H22B 107.8 . . ?
H23A O23 H23B 94.5 . . ?
H24A O24 H24B 97.9 . . ?
H25A O25 H25B 104.5 . . ?
C29 N1 C41 113.1(2) . . ?
C29 N1 Cu1 104.19(17) . . ?
C41 N1 Cu1 120.42(18) . . ?
C29 N1 H1 107.3 . . ?
C41 N1 H1 109.7 . . ?
Cu1 N1 H1 100.8 . . ?
C30 N2 C31 114.5(2) . . ?
C30 N2 Cu1 108.18(18) . . ?
C31 N2 Cu1 118.28(18) . . ?
C30 N2 H2 105.0 . . ?
C31 N2 H2 104.8 . . ?
Cu1 N2 H2 104.7 . . ?
C37 N3 C33 112.9(2) . . ?
C37 N3 Cu1 107.82(17) . . ?
C33 N3 Cu1 120.26(17) . . ?
C37 N3 H3 105.1 . . ?
C33 N3 H3 105.7 . . ?
Cu1 N3 H3 103.7 . . ?
C38 N4 C39 115.8(2) . . ?
C38 N4 Cu1 105.67(17) . . ?
C39 N4 Cu1 121.37(17) . . ?
C38 N4 H4 111.0 . . ?
C39 N4 H4 102.3 . . ?
Cu1 N4 H4 99.2 . . ?
C45 N5 C57 113.1(2) . . ?
C45 N5 Cu2 106.84(16) . . ?
C57 N5 Cu2 117.67(17) . . ?
C45 N5 H5 108.7 . . ?
C57 N5 H5 105.0 . . ?
Cu2 N5 H5 105.0 . . ?
C46 N6 C47 114.7(2) . . ?
C46 N6 Cu2 106.79(15) . . ?
C47 N6 Cu2 123.30(16) . . ?
C46 N6 H6 109.0 . . ?
C47 N6 H6 102.6 . . ?
Cu2 N6 H6 98.4 . . ?
C53 N7 C49 114.16(19) . . ?
C53 N7 Cu2 106.94(15) . . ?
C49 N7 Cu2 118.34(16) . . ?
C53 N7 H7 102.9 . . ?
C49 N7 H7 103.0 . . ?
Cu2 N7 H7 110.3 . . ?
C54 N8 C55 114.9(2) . . ?
C54 N8 Cu2 106.87(15) . . ?
C55 N8 Cu2 121.49(16) . . ?
C54 N8 H8 108.1 . . ?
C55 N8 H8 106.1 . . ?
Cu2 N8 H8 97.3 . . ?
C61 N9 C65 113.8(2) . 2_765 ?
C61 N9 Cu3 106.47(15) . . ?
C65 N9 Cu3 121.43(15) 2_765 . ?
C61 N9 H9 108.8 . . ?
C65 N9 H9 107.1 2_765 . ?
Cu3 N9 H9 97.6 . . ?
C62 N10 C63 112.78(19) . . ?
C62 N10 Cu3 107.09(15) . . ?
C63 N10 Cu3 119.77(16) . . ?
C62 N10 H10 103.7 . . ?
C63 N10 H10 107.4 . . ?
Cu3 N10 H10 104.6 . . ?
C6 C1 C2 119.9(2) . . ?
C6 C1 S1 120.1(2) . . ?
C2 C1 S1 120.0(2) . . ?
C3 C2 C1 120.9(2) . . ?
C3 C2 H2A 119.6 . . ?
C1 C2 H2A 119.6 . . ?
C2 C3 C4 119.5(2) . . ?
C2 C3 C7 119.7(2) . . ?
C4 C3 C7 120.8(2) . . ?
O13 C4 C3 120.7(2) . . ?
O13 C4 C5 120.0(2) . . ?
C3 C4 C5 119.2(2) . . ?
C6 C5 C4 119.6(2) . . ?
C6 C5 C28 120.7(2) . . ?
C4 C5 C28 119.7(2) . . ?
C1 C6 C5 120.9(2) . . ?
C1 C6 H6A 119.5 . . ?
C5 C6 H6A 119.5 . . ?
C3 C7 C8 115.3(2) . . ?
C3 C7 H7A 108.4 . . ?
C8 C7 H7A 108.4 . . ?
C3 C7 H7B 108.4 . . ?
C8 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
C9 C8 C13 118.1(2) . . ?
C9 C8 C7 121.0(2) . . ?
C13 C8 C7 120.8(2) . . ?
C10 C9 C8 121.6(2) . . ?
C10 C9 H9A 119.2 . . ?
C8 C9 H9A 119.2 . . ?
C9 C10 C11 119.4(2) . . ?
C9 C10 S2 120.4(2) . . ?
C11 C10 S2 120.11(19) . . ?
C12 C11 C10 120.9(2) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 119.1(2) . . ?
C11 C12 C14 122.1(2) . . ?
C13 C12 C14 118.9(2) . . ?
O14 C13 C8 122.4(2) . . ?
O14 C13 C12 117.0(2) . . ?
C8 C13 C12 120.6(2) . . ?
C12 C14 C15 112.8(2) . . ?
C12 C14 H14A 109.0 . . ?
C15 C14 H14A 109.0 . . ?
C12 C14 H14B 109.0 . . ?
C15 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C20 C15 C16 118.5(2) . . ?
C20 C15 C14 121.6(2) . . ?
C16 C15 C14 119.9(2) . . ?
C17 C16 C15 120.3(2) . . ?
C17 C16 H16A 119.9 . . ?
C15 C16 H16A 119.9 . . ?
C16 C17 C18 120.2(2) . . ?
C16 C17 S3 120.9(2) . . ?
C18 C17 S3 118.94(19) . . ?
C19 C18 C17 121.3(2) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C18 C19 C20 117.9(2) . . ?
C18 C19 C21 119.8(2) . . ?
C20 C19 C21 122.3(2) . . ?
O15 C20 C15 118.7(2) . . ?
O15 C20 C19 119.5(2) . . ?
C15 C20 C19 121.7(2) . . ?
C19 C21 C22 111.3(2) . . ?
C19 C21 H21C 109.4 . . ?
C22 C21 H21C 109.4 . . ?
C19 C21 H21D 109.4 . . ?
C22 C21 H21D 109.4 . . ?
H21C C21 H21D 108.0 . . ?
C23 C22 C27 118.6(2) . . ?
C23 C22 C21 120.2(2) . . ?
C27 C22 C21 121.2(2) . . ?
C22 C23 C24 121.2(2) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C25 C24 C23 119.8(2) . . ?
C25 C24 S4 122.02(19) . . ?
C23 C24 S4 118.18(19) . . ?
C24 C25 C26 120.8(2) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C27 118.9(2) . . ?
C25 C26 C28 119.8(2) . . ?
C27 C26 C28 121.2(2) . . ?
O16 C27 C26 122.0(2) . . ?
O16 C27 C22 117.3(2) . . ?
C26 C27 C22 120.7(2) . . ?
C5 C28 C26 114.0(2) . . ?
C5 C28 H28A 108.7 . . ?
C26 C28 H28A 108.7 . . ?
C5 C28 H28B 108.7 . . ?
C26 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
N1 C29 C30 106.7(2) . . ?
N1 C29 H29A 110.4 . . ?
C30 C29 H29A 110.4 . . ?
N1 C29 H29B 110.4 . . ?
C30 C29 H29B 110.4 . . ?
H29A C29 H29B 108.6 . . ?
N2 C30 C29 109.4(2) . . ?
N2 C30 H30A 109.8 . . ?
C29 C30 H30A 109.8 . . ?
N2 C30 H30B 109.8 . . ?
C29 C30 H30B 109.8 . . ?
H30A C30 H30B 108.2 . . ?
N2 C31 C35 110.4(3) . . ?
N2 C31 C32 108.5(2) . . ?
C35 C31 C32 108.4(3) . . ?
N2 C31 C34 106.9(2) . . ?
C35 C31 C34 112.6(3) . . ?
C32 C31 C34 110.0(3) . . ?
C33 C32 C31 119.2(3) . . ?
C33 C32 H32A 107.5 . . ?
C31 C32 H32A 107.5 . . ?
C33 C32 H32B 107.5 . . ?
C31 C32 H32B 107.5 . . ?
H32A C32 H32B 107.0 . . ?
N3 C33 C32 110.5(2) . . ?
N3 C33 C36 111.1(2) . . ?
C32 C33 C36 109.7(3) . . ?
N3 C33 H33 108.5 . . ?
C32 C33 H33 108.5 . . ?
C36 C33 H33 108.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C31 C35 H35A 109.5 . . ?
C31 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C31 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N3 C37 C38 108.5(2) . . ?
N3 C37 H37A 110.0 . . ?
C38 C37 H37A 110.0 . . ?
N3 C37 H37B 110.0 . . ?
C38 C37 H37B 110.0 . . ?
H37A C37 H37B 108.4 . . ?
N4 C38 C37 108.0(2) . . ?
N4 C38 H38A 110.1 . . ?
C37 C38 H38A 110.1 . . ?
N4 C38 H38B 110.1 . . ?
C37 C38 H38B 110.1 . . ?
H38A C38 H38B 108.4 . . ?
N4 C39 C43 111.9(2) . . ?
N4 C39 C40 108.1(2) . . ?
C43 C39 C40 112.1(3) . . ?
N4 C39 C42 109.7(2) . . ?
C43 C39 C42 108.0(2) . . ?
C40 C39 C42 107.0(3) . . ?
C41 C40 C39 118.5(3) . . ?
C41 C40 H40A 107.7 . . ?
C39 C40 H40A 107.7 . . ?
C41 C40 H40B 107.7 . . ?
C39 C40 H40B 107.7 . . ?
H40A C40 H40B 107.1 . . ?
N1 C41 C40 109.4(2) . . ?
N1 C41 C44 111.3(3) . . ?
C40 C41 C44 109.3(3) . . ?
N1 C41 H41 109.0 . . ?
C40 C41 H41 109.0 . . ?
C44 C41 H41 109.0 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C39 C43 H43A 109.5 . . ?
C39 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C39 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N5 C45 C46 108.3(2) . . ?
N5 C45 H45A 110.0 . . ?
C46 C45 H45A 110.0 . . ?
N5 C45 H45B 110.0 . . ?
C46 C45 H45B 110.0 . . ?
H45A C45 H45B 108.4 . . ?
N6 C46 C45 107.4(2) . . ?
N6 C46 H46A 110.2 . . ?
C45 C46 H46A 110.2 . . ?
N6 C46 H46B 110.2 . . ?
C45 C46 H46B 110.2 . . ?
H46A C46 H46B 108.5 . . ?
N6 C47 C51 110.8(2) . . ?
N6 C47 C50 109.5(2) . . ?
C51 C47 C50 109.9(2) . . ?
N6 C47 C48 107.6(2) . . ?
C51 C47 C48 111.7(2) . . ?
C50 C47 C48 107.1(2) . . ?
C49 C48 C47 118.1(2) . . ?
C49 C48 H48A 107.8 . . ?
C47 C48 H48A 107.8 . . ?
C49 C48 H48B 107.8 . . ?
C47 C48 H48B 107.8 . . ?
H48A C48 H48B 107.1 . . ?
N7 C49 C48 110.6(2) . . ?
N7 C49 C52 112.3(2) . . ?
C48 C49 C52 109.6(2) . . ?
N7 C49 H49 108.1 . . ?
C48 C49 H49 108.1 . . ?
C52 C49 H49 108.1 . . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C47 C51 H51A 109.5 . . ?
C47 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C47 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C49 C52 H52A 109.5 . . ?
C49 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C49 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N7 C53 C54 107.8(2) . . ?
N7 C53 H53A 110.1 . . ?
C54 C53 H53A 110.1 . . ?
N7 C53 H53B 110.1 . . ?
C54 C53 H53B 110.1 . . ?
H53A C53 H53B 108.5 . . ?
N8 C54 C53 108.9(2) . . ?
N8 C54 H54A 109.9 . . ?
C53 C54 H54A 109.9 . . ?
N8 C54 H54B 109.9 . . ?
C53 C54 H54B 109.9 . . ?
H54A C54 H54B 108.3 . . ?
N8 C55 C58 110.8(2) . . ?
N8 C55 C56 107.6(2) . . ?
C58 C55 C56 111.6(2) . . ?
N8 C55 C59 109.4(2) . . ?
C58 C55 C59 109.7(2) . . ?
C56 C55 C59 107.6(2) . . ?
C57 C56 C55 117.7(2) . . ?
C57 C56 H56A 107.9 . . ?
C55 C56 H56A 107.9 . . ?
C57 C56 H56B 107.9 . . ?
C55 C56 H56B 107.9 . . ?
H56A C56 H56B 107.2 . . ?
N5 C57 C56 109.1(2) . . ?
N5 C57 C60 111.9(2) . . ?
C56 C57 C60 110.9(3) . . ?
N5 C57 H57 108.3 . . ?
C56 C57 H57 108.3 . . ?
C60 C57 H57 108.3 . . ?
C55 C58 H58A 109.5 . . ?
C55 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C55 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C55 C59 H59A 109.5 . . ?
C55 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C55 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
N9 C61 C62 108.3(2) . . ?
N9 C61 H61A 110.0 . . ?
C62 C61 H61A 110.0 . . ?
N9 C61 H61B 110.0 . . ?
C62 C61 H61B 110.0 . . ?
H61A C61 H61B 108.4 . . ?
N10 C62 C61 108.4(2) . . ?
N10 C62 H62A 110.0 . . ?
C61 C62 H62A 110.0 . . ?
N10 C62 H62B 110.0 . . ?
C61 C62 H62B 110.0 . . ?
H62A C62 H62B 108.4 . . ?
N10 C63 C64 109.5(2) . . ?
N10 C63 C66 111.3(2) . . ?
C64 C63 C66 109.7(2) . . ?
N10 C63 H63 108.7 . . ?
C64 C63 H63 108.7 . . ?
C66 C63 H63 108.7 . . ?
C63 C64 C65 117.9(2) . . ?
C63 C64 H64A 107.8 . . ?
C65 C64 H64A 107.8 . . ?
C63 C64 H64B 107.8 . . ?
C65 C64 H64B 107.8 . . ?
H64A C64 H64B 107.2 . . ?
N9 C65 C68 109.6(2) 2_765 . ?
N9 C65 C64 107.9(2) 2_765 . ?
C68 C65 C64 112.2(2) . . ?
N9 C65 C67 109.7(2) 2_765 . ?
C68 C65 C67 110.1(2) . . ?
C64 C65 C67 107.2(2) . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C65 C67 H67A 109.5 . . ?
C65 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C65 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C65 C68 H68A 109.5 . . ?
C65 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C65 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O14 H14 O13 0.96 1.55 2.504(2) 168.8 .
O15 H15 O16 1.00 1.78 2.741(2) 159.9 .
O16 H16 O13 0.91 1.62 2.514(2) 166.9 .
O17 H17A O2 0.86 2.05 2.873(3) 157.8 1_565
O17 H17B O9 0.94 1.91 2.768(3) 152.2 .
O18 H18A O5 0.98 1.90 2.853(2) 165.2 .
O18 H18B O12 0.96 1.84 2.795(3) 169.3 1_465
O19 H19A O6 0.88 1.94 2.806(3) 166.6 .
O19 H19B O22 0.97 1.84 2.767(3) 158.4 .
O20 H20A O6 0.99 1.95 2.905(3) 161.1 .
O20 H20B O21 0.84 2.13 2.955(4) 169.5 2_576
O21 H21A O8 0.94 1.89 2.829(3) 176.7 .
O21 H21B O19 0.85 2.02 2.829(3) 159.4 .
O22 H22A O17 0.98 1.85 2.805(3) 164.8 .
O22 H22B O18 0.89 1.96 2.820(3) 162.6 .
O23 H23A O18 0.99 1.83 2.812(3) 171.3 .
O23 H23B O24 0.94 1.90 2.817(3) 162.3 .
O24 H24A O19 0.85 1.97 2.822(3) 173.6 .
O24 H24B O21 0.96 1.85 2.773(3) 160.3 2_576
O25 H25A O20 0.81 2.12 2.873(5) 154.2 .
O25 H25B O23 0.85 2.26 3.083(4) 163.7 .
N1 H1 O23 0.85 2.13 2.957(3) 166.2 2_576
N2 H2 O3 0.96 1.96 2.870(3) 158.2 .
N4 H4 O24 0.97 1.99 2.946(3) 168.2 2_576
N5 H5 O4 0.93 2.59 3.101(3) 115.2 1_655
N6 H6 O7 0.98 2.46 3.063(3) 120.0 .
N6 H6 O8 0.98 2.04 3.001(3) 169.7 .
N8 H8 O4 0.91 2.56 3.156(3) 123.6 1_655
N8 H8 O5 0.91 2.19 3.086(3) 171.7 1_655
N9 H9 O10 0.97 2.37 3.023(3) 124.2 .
N10 H10 O12 0.97 2.04 2.988(3) 166.1 2_765
C40 H40B O2 0.99 2.54 3.379(3) 142.6 2_566
C43 H43C O1 0.98 2.41 3.286(4) 148.4 .
C44 H44B O2 0.98 2.60 3.442(4) 144.5 2_566
C51 H51A O4 0.98 2.45 3.370(3) 155.9 1_655
C53 H53A O14 0.99 2.55 3.359(3) 138.8 2_675
C56 H56B O3 0.99 2.34 3.226(3) 148.7 1_565
C58 H58C O7 0.98 2.44 3.344(3) 153.2 .
C60 H60B O3 0.98 2.52 3.349(4) 142.8 1_565
C60 H60C O25 0.98 2.30 3.248(5) 162.8 1_655
C67 H67A O17 0.98 2.55 3.497(3) 163.1 1_645
C68 H68A O10 0.98 2.36 3.319(3) 165.5 .

_refine_diff_density_max         0.800
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.073

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1893015'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2019-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H36 N4 Ni O14 S2 U'
_chemical_formula_weight         965.43

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.6905(5)
_cell_length_b                   14.6528(6)
_cell_length_c                   9.9092(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.272(3)
_cell_angle_gamma                90
_cell_volume                     1551.85(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    41974
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_F_000             944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    6.027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.411
_exptl_absorpt_correction_T_max  0.515
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and three ω scans with 2° steps (400 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            41974
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.780
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2937
_reflns_number_gt                2522
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms were introduced at calculated
 positions and were treated as riding atoms with an isotropic displacement
 parameter equal to 1.2 times that of the parent atom. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0310P)²+0.3021P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2937
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0200
_refine_ls_wR_factor_ref         0.0525
_refine_ls_wR_factor_gt          0.0503
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_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_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 0.5000 1.0000 0.0000 0.01601(7) Uani 1 2 d S . P . .
Ni1 Ni 1.0000 0.5000 0.5000 0.01763(13) Uani 1 2 d S . P . .
S1 S 0.81227(6) 0.79567(4) 0.63812(6) 0.01774(14) Uani 1 1 d . . . . .
O1 O 0.55417(15) 1.11012(12) 0.04544(17) 0.0212(4) Uani 1 1 d . . . . .
O2 O 0.61142(16) 0.94683(12) 0.20083(17) 0.0217(4) Uani 1 1 d . . . . .
O3 O 0.40938(16) 0.96490(14) 0.22540(17) 0.0206(4) Uani 1 1 d . . . . .
O4 O 0.81748(16) 0.69581(12) 0.63564(18) 0.0220(4) Uani 1 1 d . . . . .
O5 O 0.81839(15) 0.83012(12) 0.77697(16) 0.0218(4) Uani 1 1 d . . . . .
O6 O 0.90304(16) 0.83842(13) 0.55188(17) 0.0242(4) Uani 1 1 d . . . . .
O7 O 0.28654(15) 1.06269(12) 0.03169(17) 0.0199(4) Uani 1 1 d . . . . .
H7A H 0.2640 1.1041 -0.0261 0.024 Uiso 1 1 d R U . . .
H7B H 0.2670 1.0860 0.1025 0.024 Uiso 1 1 d R U . . .
N1 N 0.96125(19) 0.43905(14) 0.6672(2) 0.0210(5) Uani 1 1 d . . . . .
H1 H 1.0345 0.3981 0.6769 0.025 Uiso 1 1 d R U . . .
N2 N 1.0508(2) 0.60240(15) 0.6117(2) 0.0227(5) Uani 1 1 d . . . . .
H2 H 0.9810 0.6442 0.6190 0.027 Uiso 1 1 d R U . . .
C1 C 0.5145(2) 0.93711(17) 0.2709(2) 0.0192(5) Uani 1 1 d . . . . .
C2 C 0.5269(2) 0.89309(17) 0.4058(2) 0.0185(5) Uani 1 1 d . . . . .
C3 C 0.6462(2) 0.86497(17) 0.4506(2) 0.0180(5) Uani 1 1 d . . . . .
H3 H 0.7164 0.8726 0.3946 0.022 Uiso 1 1 calc R U . . .
C4 C 0.6604(2) 0.82609(16) 0.5771(2) 0.0173(5) Uani 1 1 d . . . . .
C5 C 0.5578(2) 0.81221(17) 0.6585(2) 0.0210(5) Uani 1 1 d . . . . .
H5 H 0.5687 0.7847 0.7447 0.025 Uiso 1 1 calc R U . . .
C6 C 0.4398(2) 0.83857(19) 0.6136(2) 0.0220(6) Uani 1 1 d . . . . .
H6 H 0.3694 0.8288 0.6687 0.026 Uiso 1 1 calc R U . . .
C7 C 0.4244(2) 0.87962(17) 0.4870(2) 0.0200(6) Uani 1 1 d . . . . .
H7 H 0.3435 0.8983 0.4565 0.024 Uiso 1 1 calc R U . . .
C8 C 0.9570(3) 0.50699(17) 0.7779(4) 0.0272(7) Uani 1 1 d . . . . .
H8A H 0.9676 0.4766 0.8667 0.033 Uiso 1 1 calc R U . . .
H8B H 0.8761 0.5398 0.7757 0.033 Uiso 1 1 calc R U . . .
C9 C 1.0629(3) 0.5718(2) 0.7545(3) 0.0291(6) Uani 1 1 d . . . . .
H9A H 1.0577 0.6247 0.8163 0.035 Uiso 1 1 calc R U . . .
H9B H 1.1442 0.5409 0.7706 0.035 Uiso 1 1 calc R U . . .
C10 C 1.1605(2) 0.6584(2) 0.5753(3) 0.0298(6) Uani 1 1 d . . . . .
H10A H 1.2372 0.6208 0.5832 0.036 Uiso 1 1 calc R U . . .
H10B H 1.1692 0.7100 0.6394 0.036 Uiso 1 1 calc R U . . .
C11 C 1.1476(3) 0.6951(2) 0.4338(3) 0.0328(7) Uani 1 1 d . . . . .
H11A H 1.2167 0.7385 0.4178 0.039 Uiso 1 1 calc R U . . .
H11B H 1.0679 0.7292 0.4248 0.039 Uiso 1 1 calc R U . . .
C12 C 1.1498(2) 0.62116(19) 0.3274(3) 0.0278(6) Uani 1 1 d . . . . .
H12A H 1.1531 0.6498 0.2371 0.033 Uiso 1 1 calc R U . . .
H12B H 1.2264 0.5839 0.3406 0.033 Uiso 1 1 calc R U . . .


_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 O1 1.7691(17) 3_675 ?
U1 O1 1.7691(17) . ?
U1 O2 2.4251(16) 3_675 ?
U1 O2 2.4251(16) . ?
U1 O7 2.4863(17) . ?
U1 O7 2.4863(17) 3_675 ?
U1 O3 2.5075(18) . ?
U1 O3 2.5076(18) 3_675 ?
Ni1 N2 1.935(2) . ?
Ni1 N2 1.935(2) 3_766 ?
Ni1 N1 1.935(2) 3_766 ?
Ni1 N1 1.935(2) . ?
S1 O6 1.4495(18) . ?
S1 O4 1.4645(19) . ?
S1 O5 1.4656(17) . ?
S1 C4 1.777(2) . ?
O2 C1 1.268(3) . ?
O3 C1 1.269(3) . ?
O7 H7A 0.8642 . ?
O7 H7B 0.8118 . ?
N1 C12 1.481(3) 3_766 ?
N1 C8 1.483(4) . ?
N1 H1 0.9900 . ?
N2 C10 1.482(3) . ?
N2 C9 1.487(3) . ?
N2 H2 0.9700 . ?
C1 C2 1.487(4) . ?
C2 C7 1.388(4) . ?
C2 C3 1.403(4) . ?
C3 C4 1.382(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(3) . ?
C5 C6 1.383(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.398(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.499(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.505(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.513(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N1 1.481(3) 3_766 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?

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 U1 O1 180 3_675 . ?
O1 U1 O2 86.11(7) 3_675 3_675 ?
O1 U1 O2 93.89(7) . 3_675 ?
O1 U1 O2 93.89(7) 3_675 . ?
O1 U1 O2 86.11(7) . . ?
O2 U1 O2 180.0 3_675 . ?
O1 U1 O7 94.18(7) 3_675 . ?
O1 U1 O7 85.82(7) . . ?
O2 U1 O7 63.22(6) 3_675 . ?
O2 U1 O7 116.78(6) . . ?
O1 U1 O7 85.82(7) 3_675 3_675 ?
O1 U1 O7 94.18(7) . 3_675 ?
O2 U1 O7 116.78(6) 3_675 3_675 ?
O2 U1 O7 63.22(6) . 3_675 ?
O7 U1 O7 180.0 . 3_675 ?
O1 U1 O3 84.77(7) 3_675 . ?
O1 U1 O3 95.23(7) . . ?
O2 U1 O3 127.19(6) 3_675 . ?
O2 U1 O3 52.81(6) . . ?
O7 U1 O3 65.76(6) . . ?
O7 U1 O3 114.24(6) 3_675 . ?
O1 U1 O3 95.23(7) 3_675 3_675 ?
O1 U1 O3 84.77(7) . 3_675 ?
O2 U1 O3 52.81(6) 3_675 3_675 ?
O2 U1 O3 127.19(6) . 3_675 ?
O7 U1 O3 114.24(6) . 3_675 ?
O7 U1 O3 65.76(6) 3_675 3_675 ?
O3 U1 O3 180.0 . 3_675 ?
N2 Ni1 N2 180.0 . 3_766 ?
N2 Ni1 N1 93.97(9) . 3_766 ?
N2 Ni1 N1 86.03(9) 3_766 3_766 ?
N2 Ni1 N1 86.03(9) . . ?
N2 Ni1 N1 93.97(9) 3_766 . ?
N1 Ni1 N1 180.0 3_766 . ?
O6 S1 O4 113.31(11) . . ?
O6 S1 O5 112.84(11) . . ?
O4 S1 O5 111.04(11) . . ?
O6 S1 C4 108.02(11) . . ?
O4 S1 C4 106.24(11) . . ?
O5 S1 C4 104.76(11) . . ?
C1 O2 U1 95.34(14) . . ?
C1 O3 U1 91.47(15) . . ?
U1 O7 H7A 114.7 . . ?
U1 O7 H7B 121.2 . . ?
H7A O7 H7B 101.8 . . ?
C12 N1 C8 109.6(2) 3_766 . ?
C12 N1 Ni1 119.50(17) 3_766 . ?
C8 N1 Ni1 109.52(17) . . ?
C12 N1 H1 105.6 3_766 . ?
C8 N1 H1 111.9 . . ?
Ni1 N1 H1 100.3 . . ?
C10 N2 C9 110.2(2) . . ?
C10 N2 Ni1 120.27(17) . . ?
C9 N2 Ni1 109.15(17) . . ?
C10 N2 H2 106.4 . . ?
C9 N2 H2 99.8 . . ?
Ni1 N2 H2 109.0 . . ?
O2 C1 O3 119.8(2) . . ?
O2 C1 C2 118.9(2) . . ?
O3 C1 C2 121.3(2) . . ?
C7 C2 C3 119.9(2) . . ?
C7 C2 C1 121.8(2) . . ?
C3 C2 C1 118.3(2) . . ?
C4 C3 C2 119.3(2) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.9(2) . . ?
C3 C4 S1 119.60(19) . . ?
C5 C4 S1 119.49(18) . . ?
C6 C5 C4 119.9(2) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 119.8(2) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C2 C7 C6 120.2(2) . . ?
C2 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
N1 C8 C9 106.0(3) . . ?
N1 C8 H8A 110.5 . . ?
C9 C8 H8A 110.5 . . ?
N1 C8 H8B 110.5 . . ?
C9 C8 H8B 110.5 . . ?
H8A C8 H8B 108.7 . . ?
N2 C9 C8 106.8(2) . . ?
N2 C9 H9A 110.4 . . ?
C8 C9 H9A 110.4 . . ?
N2 C9 H9B 110.4 . . ?
C8 C9 H9B 110.4 . . ?
H9A C9 H9B 108.6 . . ?
N2 C10 C11 111.6(2) . . ?
N2 C10 H10A 109.3 . . ?
C11 C10 H10A 109.3 . . ?
N2 C10 H10B 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C10 C11 C12 113.0(2) . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N1 C12 C11 112.1(2) 3_766 . ?
N1 C12 H12A 109.2 3_766 . ?
C11 C12 H12A 109.2 . . ?
N1 C12 H12B 109.2 3_766 . ?
C11 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7A O4 0.86 1.92 2.777(2) 168.4 2_655
O7 H7B O5 0.81 1.95 2.723(2) 157.7 3_676
N1 H1 O5 0.99 1.91 2.889(3) 170.4 2_746
N2 H2 O4 0.97 1.91 2.860(3) 164.1 .
C8 H8A O6 0.99 2.57 3.327(4) 133.0 2_746
C10 H10A O1 0.99 2.60 3.377(3) 135.5 2_745

_refine_diff_density_max         0.596
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.141

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_9
_database_code_depnum_ccdc_archive 'CCDC 1893022'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2019-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C100 H103 O30 P3 S4 U'
_chemical_formula_weight         2244.00

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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   18.3929(3)
_cell_length_b                   25.4078(6)
_cell_length_c                   20.6753(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.6933(14)
_cell_angle_gamma                90
_cell_volume                     9642.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    329560
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_F_000             4576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    1.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and five ω scans with 2° steps (493 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            329560
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.460
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             18287
_reflns_number_gt                15381
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms bound to O atoms were found on a 
 difference Fourier map and all the others were introduced at calculated
 positions; all were treated as riding atoms with an isotropic displacement
 parameter equal to 1.2 times that of the parent atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0442P)²+17.9154P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18287
_refine_ls_number_parameters     1243
_refine_ls_number_restraints     69
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.0955
_refine_ls_wR_factor_gt          0.0915
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.002
_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_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 0.95106(2) 0.78257(2) 0.22277(2) 0.02553(5) Uani 1 1 d . . . . .
S1 S 0.79887(5) 0.71983(4) 0.30680(5) 0.0316(2) Uani 1 1 d . . . . .
S2 S 0.51070(5) 0.67072(4) 0.56203(5) 0.0337(2) Uani 1 1 d . . . . .
S3 S 0.19639(5) 0.71448(4) 0.34312(5) 0.0344(2) Uani 1 1 d . . . . .
S4 S 0.46023(6) 0.71718(4) 0.10973(5) 0.0312(2) Uani 1 1 d . . . . .
P1 P 0.85723(6) 0.52439(4) 0.39225(5) 0.0301(2) Uani 1 1 d . . . . .
P2 P 0.53394(5) 0.44602(4) 0.69727(4) 0.02236(19) Uani 1 1 d . . . . .
P3 P 0.74171(5) 1.00022(4) 0.50007(5) 0.0245(2) Uani 1 1 d . . . . .
O1 O 0.93365(16) 0.84710(11) 0.24922(13) 0.0397(7) Uani 1 1 d . . . . .
O2 O 0.96601(14) 0.71844(10) 0.19515(13) 0.0295(6) Uani 1 1 d . . . . .
O3 O 0.86448(14) 0.74968(13) 0.28999(14) 0.0420(7) Uani 1 1 d . . . . .
O4 O 0.76981(16) 0.68904(12) 0.25256(15) 0.0472(8) Uani 1 1 d . . . . .
O5 O 0.81450(14) 0.69076(11) 0.36617(14) 0.0376(7) Uani 1 1 d . . . . .
O6 O 0.48559(18) 0.67630(11) 0.62708(13) 0.0416(7) Uani 1 1 d . . . . .
O7 O 0.58090(18) 0.64775(14) 0.5581(2) 0.0726(12) Uani 1 1 d . . . . .
O8 O 0.4573(2) 0.64066(12) 0.52258(16) 0.0664(11) Uani 1 1 d . . . . .
O9 O 0.23849(16) 0.66912(11) 0.36680(18) 0.0513(9) Uani 1 1 d . . . . .
O10 O 0.17129(17) 0.70949(12) 0.27514(15) 0.0461(8) Uani 1 1 d . . . . .
O11 O 0.13630(14) 0.72670(11) 0.38351(13) 0.0333(6) Uani 1 1 d . . . . .
O12 O 0.41020(17) 0.73025(12) 0.05401(14) 0.0418(7) Uani 1 1 d . . . . .
O13 O 0.42967(16) 0.67764(10) 0.15145(13) 0.0372(7) Uani 1 1 d . . . . .
O14 O 0.53259(17) 0.70351(12) 0.09123(14) 0.0426(7) Uani 1 1 d . . . . .
O15 O 0.58588(13) 0.88579(10) 0.35267(12) 0.0282(6) Uani 1 1 d . . . . .
O16 O 0.50613(14) 0.88153(10) 0.44522(13) 0.0346(6) Uani 1 1 d . . . . .
H16 H 0.5469 0.8897 0.4297 0.042 Uiso 1 1 d R U . . .
O17 O 0.39685(15) 0.89546(11) 0.36358(14) 0.0401(7) Uani 1 1 d . . . . .
H17 H 0.4318 0.8909 0.3948 0.048 Uiso 1 1 d R U . . .
O18 O 0.48365(15) 0.91435(10) 0.26019(14) 0.0364(7) Uani 1 1 d . . . . .
H18A H 0.5225 0.9147 0.2857 0.044 Uiso 0.5 1 d R U P . .
H18B H 0.4501 0.9158 0.2910 0.044 Uiso 0.5 1 d R U P . .
O19 O 0.84092(15) 0.78259(11) 0.15385(13) 0.0355(6) Uani 1 1 d . . . . .
H19A H 0.8185 0.7534 0.1398 0.043 Uiso 1 1 d R U . . .
H19B H 0.8076 0.8068 0.1327 0.043 Uiso 1 1 d R U . . .
O20 O 1.08425(15) 0.79084(12) 0.23152(14) 0.0399(7) Uani 1 1 d . . . . .
H20A H 1.1068 0.7589 0.2492 0.048 Uiso 1 1 d R U . . .
H20B H 1.0977 0.8087 0.1988 0.048 Uiso 1 1 d R U . . .
O21 O 1.00571(13) 0.76584(10) 0.33313(12) 0.0290(6) Uani 1 1 d . . . . .
H21A H 1.0435 0.7576 0.3433 0.035 Uiso 1 1 d R U . . .
H21B H 0.9787 0.7520 0.3633 0.035 Uiso 1 1 d R U . . .
O22 O 0.65568(16) 0.65711(12) 0.16330(15) 0.0425(7) Uani 1 1 d . . . . .
H22A H 0.6763 0.6745 0.2030 0.051 Uiso 1 1 d R U . . .
H22B H 0.6123 0.6774 0.1592 0.051 Uiso 1 1 d R U . . .
O23 O 0.94052(15) 0.72669(11) 0.43394(13) 0.0346(6) Uani 1 1 d . . . . .
H23A H 0.8959 0.7138 0.4196 0.042 Uiso 1 1 d R U . . .
H23B H 0.9342 0.7384 0.4761 0.042 Uiso 1 1 d R U . . .
O24 O 0.6802(2) 0.68297(17) 0.64750(19) 0.0720(11) Uani 1 1 d . . . . .
H24A H 0.6622 0.6662 0.6109 0.086 Uiso 1 1 d R U . . .
H24B H 0.7065 0.7023 0.6282 0.086 Uiso 1 1 d R U . . .
O25 O 0.3145(2) 0.62892(14) 0.47676(18) 0.0673(10) Uani 1 1 d . . . . .
H25A H 0.3593 0.6385 0.4810 0.081 Uiso 1 1 d R U . . .
H25B H 0.3006 0.6384 0.4438 0.081 Uiso 1 1 d R U . . .
O26 O 0.28487(17) 0.66224(12) 0.18762(15) 0.0458(7) Uani 1 1 d . . . . .
H26A H 0.2642 0.6750 0.2254 0.055 Uiso 1 1 d R U . . .
H26B H 0.3351 0.6698 0.1892 0.055 Uiso 1 1 d R U . . .
O27 O 0.14301(15) 0.73867(11) 0.52347(13) 0.0351(6) Uani 1 1 d . . . . .
H27A H 0.1265 0.7342 0.4804 0.042 Uiso 1 1 d R U . . .
H27B H 0.1021 0.7524 0.5416 0.042 Uiso 1 1 d R U . . .
O28 O 0.25763(18) 0.73319(13) 0.08549(17) 0.0545(9) Uani 1 1 d . . . . .
H28A H 0.2991 0.7274 0.0650 0.065 Uiso 1 1 d R U . . .
H28B H 0.2622 0.7081 0.1191 0.065 Uiso 1 1 d R U . . .
O29 O 0.75643(15) 0.70982(11) 0.09199(13) 0.0344(6) Uani 1 1 d . . . . .
H29A H 0.7310 0.6914 0.1150 0.041 Uiso 1 1 d R U . . .
H29B H 0.7193 0.7287 0.0728 0.041 Uiso 1 1 d R U . . .
O30 O 0.74755(15) 0.84560(11) 0.08519(14) 0.0385(7) Uani 1 1 d . . . . .
H30A H 0.7599 0.8526 0.0432 0.046 Uiso 1 1 d R U . . .
H30B H 0.7064 0.8277 0.0711 0.046 Uiso 1 1 d R U . . .
C1 C 0.73486(18) 0.76877(14) 0.32240(18) 0.0248(8) Uani 1 1 d . . . . .
C2 C 0.71610(19) 0.77905(14) 0.38491(18) 0.0253(8) Uani 1 1 d . . . . .
H2 H 0.7371 0.7589 0.4200 0.030 Uiso 1 1 calc R U . . .
C3 C 0.66661(19) 0.81877(14) 0.39644(17) 0.0239(7) Uani 1 1 d . . . . .
C4 C 0.63466(19) 0.84742(14) 0.34411(18) 0.0249(8) Uani 1 1 d . . . . .
C5 C 0.65471(18) 0.83707(14) 0.28038(17) 0.0244(8) Uani 1 1 d . . . . .
C6 C 0.70481(19) 0.79789(15) 0.27023(18) 0.0266(8) Uani 1 1 d . . . . .
H6 H 0.7188 0.7908 0.2276 0.032 Uiso 1 1 calc R U . . .
C7 C 0.64711(19) 0.83143(15) 0.46525(17) 0.0272(8) Uani 1 1 d . . . . .
H7A H 0.6870 0.8190 0.4959 0.033 Uiso 1 1 calc R U . . .
H7B H 0.6437 0.8701 0.4699 0.033 Uiso 1 1 calc R U . . .
C8 C 0.5761(2) 0.80695(15) 0.48404(17) 0.0272(8) Uani 1 1 d . . . . .
C9 C 0.5765(2) 0.75739(15) 0.51171(18) 0.0299(8) Uani 1 1 d . . . . .
H9 H 0.6212 0.7389 0.5188 0.036 Uiso 1 1 calc R U . . .
C10 C 0.5122(2) 0.73445(15) 0.52926(19) 0.0305(8) Uani 1 1 d . . . . .
C11 C 0.4467(2) 0.76132(15) 0.52011(19) 0.0300(8) Uani 1 1 d . . . . .
H11 H 0.4030 0.7455 0.5328 0.036 Uiso 1 1 calc R U . . .
C12 C 0.4446(2) 0.81085(15) 0.49277(18) 0.0288(8) Uani 1 1 d . . . . .
C13 C 0.5095(2) 0.83380(14) 0.47372(17) 0.0269(8) Uani 1 1 d . . . . .
C14 C 0.3717(2) 0.83870(15) 0.48090(19) 0.0319(9) Uani 1 1 d . . . . .
H14A H 0.3393 0.8286 0.5152 0.038 Uiso 1 1 calc R U . . .
H14B H 0.3794 0.8772 0.4835 0.038 Uiso 1 1 calc R U . . .
C15 C 0.33528(19) 0.82512(15) 0.4156(2) 0.0300(8) Uani 1 1 d . . . . .
C16 C 0.2867(2) 0.78354(15) 0.4091(2) 0.0317(9) Uani 1 1 d . . . . .
H16A H 0.2747 0.7644 0.4464 0.038 Uiso 1 1 calc R U . . .
C17 C 0.2554(2) 0.76936(15) 0.3487(2) 0.0306(9) Uani 1 1 d . . . . .
C18 C 0.2721(2) 0.79692(15) 0.2938(2) 0.0307(9) Uani 1 1 d . . . . .
H18 H 0.2504 0.7869 0.2527 0.037 Uiso 1 1 calc R U . . .
C19 C 0.32037(19) 0.83918(14) 0.2984(2) 0.0297(8) Uani 1 1 d . . . . .
C20 C 0.35201(19) 0.85318(14) 0.3593(2) 0.0299(8) Uani 1 1 d . . . . .
C21 C 0.3415(2) 0.86791(15) 0.2384(2) 0.0328(9) Uani 1 1 d . . . . .
H21C H 0.3495 0.9056 0.2488 0.039 Uiso 1 1 calc R U . . .
H21D H 0.3013 0.8654 0.2044 0.039 Uiso 1 1 calc R U . . .
C22 C 0.41057(19) 0.84476(14) 0.21314(18) 0.0258(8) Uani 1 1 d . . . . .
C23 C 0.4067(2) 0.79835(15) 0.17763(18) 0.0274(8) Uani 1 1 d . . . . .
H23 H 0.3607 0.7822 0.1680 0.033 Uiso 1 1 calc R U . . .
C24 C 0.4693(2) 0.77515(14) 0.15597(17) 0.0256(8) Uani 1 1 d . . . . .
C25 C 0.53673(19) 0.79839(14) 0.17004(17) 0.0253(8) Uani 1 1 d . . . . .
H25 H 0.5793 0.7826 0.1550 0.030 Uiso 1 1 calc R U . . .
C26 C 0.54233(19) 0.84460(15) 0.20600(17) 0.0255(8) Uani 1 1 d . . . . .
C27 C 0.4790(2) 0.86785(14) 0.22676(18) 0.0264(8) Uani 1 1 d . . . . .
C28 C 0.61774(19) 0.86700(15) 0.22377(18) 0.0275(8) Uani 1 1 d . . . . .
H28C H 0.6479 0.8646 0.1859 0.033 Uiso 1 1 calc R U . . .
H28D H 0.6134 0.9046 0.2355 0.033 Uiso 1 1 calc R U . . .
C29 C 0.93549(19) 0.55017(14) 0.35461(17) 0.0253(8) Uani 1 1 d . . . . .
C30 C 0.9516(2) 0.60374(15) 0.35897(18) 0.0307(8) Uani 1 1 d . . . . .
H30 H 0.9228 0.6263 0.3837 0.037 Uiso 1 1 calc R U . . .
C31 C 1.0094(2) 0.62400(15) 0.32726(19) 0.0315(9) Uani 1 1 d . . . . .
H31 H 1.0196 0.6606 0.3296 0.038 Uiso 1 1 calc R U . . .
C32 C 1.0524(2) 0.59162(16) 0.29243(18) 0.0308(9) Uani 1 1 d . . . . .
H32 H 1.0930 0.6057 0.2722 0.037 Uiso 1 1 calc R U . . .
C33 C 1.0362(2) 0.53855(16) 0.28696(19) 0.0315(9) Uani 1 1 d . . . . .
H33 H 1.0655 0.5163 0.2624 0.038 Uiso 1 1 calc R U . . .
C34 C 0.9777(2) 0.51779(15) 0.31716(18) 0.0292(8) Uani 1 1 d . . . . .
H34 H 0.9661 0.4815 0.3125 0.035 Uiso 1 1 calc R U . . .
C35 C 0.8214(3) 0.5739(2) 0.4435(3) 0.0650(11) Uani 1 1 d . U . . .
C36 C 0.8657(4) 0.5963(2) 0.4920(3) 0.0777(12) Uani 1 1 d D U . . .
H36 H 0.9155 0.5869 0.4992 0.093 Uiso 1 1 calc R U . . .
C37 C 0.8312(4) 0.6360(2) 0.5321(3) 0.0880(13) Uani 1 1 d D U . . .
H37 H 0.8582 0.6521 0.5675 0.106 Uiso 1 1 calc R U . . .
C38 C 0.7601(4) 0.6493(3) 0.5180(3) 0.0926(13) Uani 1 1 d D U . . .
H38 H 0.7403 0.6765 0.5430 0.111 Uiso 1 1 calc R U . . .
C39 C 0.7167(4) 0.6273(3) 0.4723(3) 0.0866(12) Uani 1 1 d D U . . .
H39 H 0.6668 0.6367 0.4649 0.104 Uiso 1 1 calc R U . . .
C40 C 0.7495(4) 0.5899(2) 0.4365(3) 0.0711(11) Uani 1 1 d . U . . .
H40 H 0.7198 0.5732 0.4034 0.085 Uiso 1 1 calc R U . . .
C41 C 0.78928(19) 0.50819(14) 0.32986(18) 0.0263(8) Uani 1 1 d . . . . .
C42 C 0.7655(2) 0.54810(16) 0.2866(2) 0.0350(9) Uani 1 1 d . . . . .
H42 H 0.7858 0.5824 0.2905 0.042 Uiso 1 1 calc R U . . .
C43 C 0.7125(2) 0.53699(18) 0.2382(2) 0.0386(10) Uani 1 1 d . . . . .
H43 H 0.6954 0.5640 0.2093 0.046 Uiso 1 1 calc R U . . .
C44 C 0.6839(2) 0.48650(18) 0.2316(2) 0.0366(10) Uani 1 1 d . . . . .
H44 H 0.6476 0.4790 0.1981 0.044 Uiso 1 1 calc R U . . .
C45 C 0.7083(2) 0.44698(16) 0.27417(19) 0.0320(9) Uani 1 1 d . . . . .
H45 H 0.6893 0.4124 0.2691 0.038 Uiso 1 1 calc R U . . .
C46 C 0.76019(19) 0.45774(14) 0.32389(18) 0.0255(8) Uani 1 1 d . . . . .
H46 H 0.7758 0.4309 0.3537 0.031 Uiso 1 1 calc R U . . .
C47 C 0.8776(3) 0.46835(17) 0.4428(2) 0.0413(11) Uani 1 1 d . . . . .
C48 C 0.8397(3) 0.4624(2) 0.4988(2) 0.0570(14) Uani 1 1 d . . . . .
H48 H 0.8046 0.4880 0.5090 0.068 Uiso 1 1 calc R U . . .
C49 C 0.8524(4) 0.4202(3) 0.5392(3) 0.0735(19) Uani 1 1 d . . . . .
H49 H 0.8273 0.4174 0.5778 0.088 Uiso 1 1 calc R U . . .
C50 C 0.9006(4) 0.3824(2) 0.5242(3) 0.078(2) Uani 1 1 d . . . . .
H50 H 0.9080 0.3529 0.5520 0.094 Uiso 1 1 calc R U . . .
C51 C 0.9395(4) 0.38621(19) 0.4686(2) 0.0639(17) Uani 1 1 d . . . . .
H51 H 0.9733 0.3597 0.4586 0.077 Uiso 1 1 calc R U . . .
C52 C 0.9277(3) 0.42982(17) 0.4278(2) 0.0517(13) Uani 1 1 d . . . . .
H52 H 0.9540 0.4331 0.3899 0.062 Uiso 1 1 calc R U . . .
C53 C 0.62546(19) 0.46833(14) 0.68803(18) 0.0251(8) Uani 1 1 d . . . . .
C54 C 0.6389(2) 0.50528(17) 0.6411(2) 0.0357(9) Uani 1 1 d . . . . .
H54 H 0.6000 0.5182 0.6130 0.043 Uiso 1 1 calc R U . . .
C55 C 0.7097(2) 0.52356(18) 0.6353(2) 0.0419(10) Uani 1 1 d . . . . .
H55 H 0.7191 0.5493 0.6036 0.050 Uiso 1 1 calc R U . . .
C56 C 0.7657(2) 0.50416(17) 0.6754(2) 0.0376(10) Uani 1 1 d . . . . .
H56 H 0.8141 0.5158 0.6703 0.045 Uiso 1 1 calc R U . . .
C57 C 0.7526(2) 0.46800(16) 0.7231(2) 0.0375(10) Uani 1 1 d . . . . .
H57 H 0.7917 0.4554 0.7511 0.045 Uiso 1 1 calc R U . . .
C58 C 0.6824(2) 0.45005(15) 0.7301(2) 0.0304(8) Uani 1 1 d . . . . .
H58 H 0.6731 0.4255 0.7633 0.036 Uiso 1 1 calc R U . . .
C59 C 0.51019(19) 0.46632(15) 0.77657(17) 0.0263(8) Uani 1 1 d . . . . .
C60 C 0.5193(2) 0.51901(16) 0.7952(2) 0.0338(9) Uani 1 1 d . . . . .
H60 H 0.5393 0.5436 0.7666 0.041 Uiso 1 1 calc R U . . .
C61 C 0.4990(2) 0.53495(19) 0.8551(2) 0.0405(11) Uani 1 1 d . . . . .
H61 H 0.5042 0.5708 0.8674 0.049 Uiso 1 1 calc R U . . .
C62 C 0.4713(2) 0.49925(19) 0.8972(2) 0.0406(11) Uani 1 1 d . . . . .
H62 H 0.4575 0.5107 0.9384 0.049 Uiso 1 1 calc R U . . .
C63 C 0.4636(2) 0.44693(19) 0.8800(2) 0.0393(10) Uani 1 1 d . . . . .
H63 H 0.4451 0.4224 0.9095 0.047 Uiso 1 1 calc R U . . .
C64 C 0.4830(2) 0.43017(16) 0.81936(18) 0.0318(9) Uani 1 1 d . . . . .
H64 H 0.4777 0.3942 0.8073 0.038 Uiso 1 1 calc R U . . .
C65 C 0.47401(18) 0.47442(14) 0.63489(17) 0.0233(7) Uani 1 1 d . . . . .
C66 C 0.4401(2) 0.52290(14) 0.64221(19) 0.0282(8) Uani 1 1 d . . . . .
H66 H 0.4473 0.5419 0.6817 0.034 Uiso 1 1 calc R U . . .
C67 C 0.3958(2) 0.54332(16) 0.59144(19) 0.0332(9) Uani 1 1 d . . . . .
H67 H 0.3725 0.5763 0.5963 0.040 Uiso 1 1 calc R U . . .
C68 C 0.3853(2) 0.51599(16) 0.53382(19) 0.0330(9) Uani 1 1 d . . . . .
H68 H 0.3549 0.5302 0.4992 0.040 Uiso 1 1 calc R U . . .
C69 C 0.4194(2) 0.46775(16) 0.52666(19) 0.0352(9) Uani 1 1 d . . . . .
H69 H 0.4118 0.4488 0.4872 0.042 Uiso 1 1 calc R U . . .
C70 C 0.4639(2) 0.44710(15) 0.57629(18) 0.0295(8) Uani 1 1 d . . . . .
H70 H 0.4878 0.4144 0.5708 0.035 Uiso 1 1 calc R U . . .
C71 C 0.52457(19) 0.37626(14) 0.68863(17) 0.0229(7) Uani 1 1 d . . . . .
C72 C 0.45478(19) 0.35471(15) 0.69156(19) 0.0291(8) Uani 1 1 d . . . . .
H72 H 0.4148 0.3769 0.6997 0.035 Uiso 1 1 calc R U . . .
C73 C 0.4440(2) 0.30115(16) 0.6827(2) 0.0336(9) Uani 1 1 d . . . . .
H73 H 0.3967 0.2865 0.6850 0.040 Uiso 1 1 calc R U . . .
C74 C 0.5023(2) 0.26917(15) 0.6704(2) 0.0341(9) Uani 1 1 d . . . . .
H74 H 0.4949 0.2324 0.6647 0.041 Uiso 1 1 calc R U . . .
C75 C 0.5712(2) 0.29012(15) 0.6665(2) 0.0327(9) Uani 1 1 d . . . . .
H75 H 0.6107 0.2678 0.6573 0.039 Uiso 1 1 calc R U . . .
C76 C 0.58302(19) 0.34364(14) 0.67598(17) 0.0261(8) Uani 1 1 d . . . . .
H76 H 0.6305 0.3579 0.6738 0.031 Uiso 1 1 calc R U . . .
C77 C 0.79118(19) 1.04916(14) 0.54766(19) 0.0280(8) Uani 1 1 d . . . . .
C78 C 0.7793(2) 1.05515(16) 0.6133(2) 0.0336(9) Uani 1 1 d . . . . .
H78 H 0.7452 1.0333 0.6332 0.040 Uiso 1 1 calc R U . . .
C79 C 0.8178(2) 1.09354(18) 0.6494(2) 0.0463(12) Uani 1 1 d . . . . .
H79 H 0.8113 1.0972 0.6943 0.056 Uiso 1 1 calc R U . . .
C80 C 0.8653(2) 1.12616(18) 0.6199(3) 0.0511(13) Uani 1 1 d . . . . .
H80 H 0.8903 1.1529 0.6445 0.061 Uiso 1 1 calc R U . . .
C81 C 0.8774(2) 1.12051(17) 0.5546(3) 0.0470(12) Uani 1 1 d . . . . .
H81 H 0.9102 1.1434 0.5348 0.056 Uiso 1 1 calc R U . . .
C82 C 0.8413(2) 1.08118(16) 0.5183(2) 0.0366(9) Uani 1 1 d . . . . .
H82 H 0.8506 1.0762 0.4741 0.044 Uiso 1 1 calc R U . . .
C83 C 0.69335(19) 1.02893(14) 0.43047(17) 0.0244(8) Uani 1 1 d . . . . .
C84 C 0.70127(19) 1.08171(14) 0.41300(17) 0.0247(8) Uani 1 1 d . . . . .
H84 H 0.7342 1.1038 0.4377 0.030 Uiso 1 1 calc R U . . .
C85 C 0.6610(2) 1.10151(15) 0.35975(18) 0.0282(8) Uani 1 1 d . . . . .
H85 H 0.6657 1.1375 0.3484 0.034 Uiso 1 1 calc R U . . .
C86 C 0.6138(2) 1.06924(15) 0.32268(18) 0.0282(8) Uani 1 1 d . . . . .
H86 H 0.5867 1.0830 0.2858 0.034 Uiso 1 1 calc R U . . .
C87 C 0.6063(2) 1.01662(15) 0.33985(18) 0.0287(8) Uani 1 1 d . . . . .
H87 H 0.5742 0.9944 0.3144 0.034 Uiso 1 1 calc R U . . .
C88 C 0.64513(19) 0.99662(15) 0.39352(18) 0.0277(8) Uani 1 1 d . . . . .
H88 H 0.6392 0.9608 0.4054 0.033 Uiso 1 1 calc R U . . .
C89 C 0.67595(19) 0.96900(15) 0.54757(18) 0.0275(8) Uani 1 1 d . . . . .
C90 C 0.6057(2) 0.99033(19) 0.5477(2) 0.0412(10) Uani 1 1 d . . . . .
H90 H 0.5940 1.0218 0.5244 0.049 Uiso 1 1 calc R U . . .
C91 C 0.5535(2) 0.9653(2) 0.5818(2) 0.0535(13) Uani 1 1 d . . . . .
H91 H 0.5056 0.9794 0.5815 0.064 Uiso 1 1 calc R U . . .
C92 C 0.5704(2) 0.9203(2) 0.6162(2) 0.0461(11) Uani 1 1 d . . . . .
H92 H 0.5338 0.9031 0.6388 0.055 Uiso 1 1 calc R U . . .
C93 C 0.6404(2) 0.89956(17) 0.61836(19) 0.0372(9) Uani 1 1 d . . . . .
H93 H 0.6521 0.8690 0.6434 0.045 Uiso 1 1 calc R U . . .
C94 C 0.6932(2) 0.92363(15) 0.58382(18) 0.0301(8) Uani 1 1 d . . . . .
H94 H 0.7410 0.9094 0.5847 0.036 Uiso 1 1 calc R U . . .
C95 C 0.80486(19) 0.95101(14) 0.47559(18) 0.0257(8) Uani 1 1 d . . . . .
C96 C 0.7950(2) 0.92600(15) 0.41542(18) 0.0286(8) Uani 1 1 d . . . . .
H96 H 0.7572 0.9372 0.3851 0.034 Uiso 1 1 calc R U . . .
C97 C 0.8403(2) 0.88498(15) 0.4000(2) 0.0314(9) Uani 1 1 d . . . . .
H97 H 0.8335 0.8680 0.3590 0.038 Uiso 1 1 calc R U . . .
C98 C 0.8955(2) 0.86861(15) 0.4443(2) 0.0353(9) Uani 1 1 d . . . . .
H98 H 0.9262 0.8402 0.4340 0.042 Uiso 1 1 calc R U . . .
C99 C 0.9059(2) 0.89385(15) 0.5040(2) 0.0327(9) Uani 1 1 d . . . . .
H99 H 0.9440 0.8828 0.5341 0.039 Uiso 1 1 calc R U . . .
C100 C 0.8609(2) 0.93505(15) 0.51957(19) 0.0282(8) Uani 1 1 d . . . . .
H100 H 0.8683 0.9523 0.5602 0.034 Uiso 1 1 calc R U . . .


_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 O2 1.754(2) . ?
U1 O1 1.764(3) . ?
U1 O3 2.335(3) . ?
U1 O6 2.360(3) 4_675 ?
U1 O19 2.401(3) . ?
U1 O20 2.454(3) . ?
U1 O21 2.470(2) . ?
S1 O4 1.442(3) . ?
S1 O5 1.446(3) . ?
S1 O3 1.485(3) . ?
S1 C1 1.756(4) . ?
S2 O7 1.424(3) . ?
S2 O8 1.453(4) . ?
S2 O6 1.457(3) . ?
S2 C10 1.756(4) . ?
S3 O9 1.456(3) . ?
S3 O10 1.456(3) . ?
S3 O11 1.461(3) . ?
S3 C17 1.766(4) . ?
S4 O14 1.451(3) . ?
S4 O13 1.460(3) . ?
S4 O12 1.466(3) . ?
S4 C24 1.758(4) . ?
P1 C41 1.785(4) . ?
P1 C47 1.791(4) . ?
P1 C35 1.798(5) . ?
P1 C29 1.803(4) . ?
P2 C71 1.789(4) . ?
P2 C65 1.793(4) . ?
P2 C53 1.798(4) . ?
P2 C59 1.799(4) . ?
P3 C89 1.792(4) . ?
P3 C77 1.796(4) . ?
P3 C83 1.797(4) . ?
P3 C95 1.801(4) . ?
O6 U1 2.360(3) 4_576 ?
O15 C4 1.344(4) . ?
O16 C13 1.348(4) . ?
O16 H16 0.8593 . ?
O17 C20 1.354(5) . ?
O17 H17 0.8880 . ?
O18 C27 1.369(4) . ?
O18 H18A 0.8597 . ?
O18 H18B 0.9161 . ?
O19 H19A 0.8887 . ?
O19 H19B 0.9548 . ?
O20 H20A 0.9705 . ?
O20 H20B 0.8653 . ?
O21 H21A 0.7432 . ?
O21 H21B 0.8936 . ?
O22 H22A 0.9869 . ?
O22 H22B 0.9495 . ?
O23 H23A 0.9140 . ?
O23 H23B 0.9362 . ?
O24 H24A 0.9111 . ?
O24 H24B 0.8109 . ?
O25 H25A 0.8587 . ?
O25 H25B 0.7516 . ?
O26 H26A 0.9479 . ?
O26 H26B 0.9426 . ?
O27 H27A 0.9296 . ?
O27 H27B 0.9302 . ?
O28 H28A 0.9083 . ?
O28 H28B 0.9437 . ?
O29 H29A 0.8318 . ?
O29 H29B 0.9042 . ?
O30 H30A 0.9290 . ?
O30 H30B 0.9149 . ?
C1 C2 1.384(5) . ?
C1 C6 1.393(5) . ?
C2 C3 1.390(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.401(5) . ?
C3 C7 1.524(5) . ?
C4 C5 1.415(5) . ?
C5 C6 1.382(5) . ?
C5 C28 1.519(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.520(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.383(5) . ?
C8 C13 1.407(5) . ?
C9 C10 1.388(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(5) . ?
C11 C12 1.379(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.407(5) . ?
C12 C14 1.521(5) . ?
C14 C15 1.509(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.384(5) . ?
C15 C20 1.414(5) . ?
C16 C17 1.388(6) . ?
C16 H16A 0.9500 . ?
C17 C18 1.385(6) . ?
C18 C19 1.393(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.399(6) . ?
C19 C21 1.512(5) . ?
C21 C22 1.522(5) . ?
C21 H21C 0.9900 . ?
C21 H21D 0.9900 . ?
C22 C23 1.388(5) . ?
C22 C27 1.400(5) . ?
C23 C24 1.392(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(5) . ?
C25 C26 1.390(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.399(5) . ?
C26 C28 1.522(5) . ?
C28 H28C 0.9900 . ?
C28 H28D 0.9900 . ?
C29 C30 1.394(5) . ?
C29 C34 1.399(5) . ?
C30 C31 1.385(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.376(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.384(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.383(5) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.375(8) . ?
C35 C40 1.381(9) . ?
C36 C37 1.474(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.363(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.322(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.369(8) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 C46 1.392(5) . ?
C41 C42 1.403(5) . ?
C42 C43 1.381(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.390(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.391(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.384(5) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C52 1.393(7) . ?
C47 C48 1.399(7) . ?
C48 C49 1.369(8) . ?
C48 H48 0.9500 . ?
C49 C50 1.357(9) . ?
C49 H49 0.9500 . ?
C50 C51 1.395(9) . ?
C50 H50 0.9500 . ?
C51 C52 1.401(6) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C53 C54 1.383(5) . ?
C53 C58 1.397(5) . ?
C54 C55 1.395(6) . ?
C54 H54 0.9500 . ?
C55 C56 1.372(6) . ?
C55 H55 0.9500 . ?
C56 C57 1.381(6) . ?
C56 H56 0.9500 . ?
C57 C58 1.386(5) . ?
C57 H57 0.9500 . ?
C58 H58 0.9500 . ?
C59 C64 1.390(5) . ?
C59 C60 1.400(5) . ?
C60 C61 1.378(6) . ?
C60 H60 0.9500 . ?
C61 C62 1.378(6) . ?
C61 H61 0.9500 . ?
C62 C63 1.381(6) . ?
C62 H62 0.9500 . ?
C63 C64 1.392(6) . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
C65 C66 1.393(5) . ?
C65 C70 1.398(5) . ?
C66 C67 1.388(5) . ?
C66 H66 0.9500 . ?
C67 C68 1.382(6) . ?
C67 H67 0.9500 . ?
C68 C69 1.388(6) . ?
C68 H68 0.9500 . ?
C69 C70 1.376(5) . ?
C69 H69 0.9500 . ?
C70 H70 0.9500 . ?
C71 C76 1.396(5) . ?
C71 C72 1.400(5) . ?
C72 C73 1.386(5) . ?
C72 H72 0.9500 . ?
C73 C74 1.382(6) . ?
C73 H73 0.9500 . ?
C74 C75 1.382(6) . ?
C74 H74 0.9500 . ?
C75 C76 1.389(5) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
C77 C82 1.397(6) . ?
C77 C78 1.398(6) . ?
C78 C79 1.393(6) . ?
C78 H78 0.9500 . ?
C79 C80 1.375(7) . ?
C79 H79 0.9500 . ?
C80 C81 1.389(7) . ?
C80 H80 0.9500 . ?
C81 C82 1.392(6) . ?
C81 H81 0.9500 . ?
C82 H82 0.9500 . ?
C83 C84 1.399(5) . ?
C83 C88 1.399(5) . ?
C84 C85 1.381(5) . ?
C84 H84 0.9500 . ?
C85 C86 1.389(5) . ?
C85 H85 0.9500 . ?
C86 C87 1.392(5) . ?
C86 H86 0.9500 . ?
C87 C88 1.378(5) . ?
C87 H87 0.9500 . ?
C88 H88 0.9500 . ?
C89 C94 1.400(5) . ?
C89 C90 1.402(5) . ?
C90 C91 1.382(6) . ?
C90 H90 0.9500 . ?
C91 C92 1.372(7) . ?
C91 H91 0.9500 . ?
C92 C93 1.390(6) . ?
C92 H92 0.9500 . ?
C93 C94 1.383(5) . ?
C93 H93 0.9500 . ?
C94 H94 0.9500 . ?
C95 C100 1.390(5) . ?
C95 C96 1.398(5) . ?
C96 C97 1.384(5) . ?
C96 H96 0.9500 . ?
C97 C98 1.387(6) . ?
C97 H97 0.9500 . ?
C98 C99 1.393(6) . ?
C98 H98 0.9500 . ?
C99 C100 1.385(5) . ?
C99 H99 0.9500 . ?
C100 H100 0.9500 . ?

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
O2 U1 O1 178.37(13) . . ?
O2 U1 O3 89.34(12) . . ?
O1 U1 O3 90.22(13) . . ?
O2 U1 O6 94.71(11) . 4_675 ?
O1 U1 O6 84.98(12) . 4_675 ?
O3 U1 O6 152.63(11) . 4_675 ?
O2 U1 O19 87.19(11) . . ?
O1 U1 O19 91.19(12) . . ?
O3 U1 O19 76.79(10) . . ?
O6 U1 O19 76.40(10) 4_675 . ?
O2 U1 O20 85.81(11) . . ?
O1 U1 O20 95.62(12) . . ?
O3 U1 O20 134.65(10) . . ?
O6 U1 O20 72.70(11) 4_675 . ?
O19 U1 O20 147.58(10) . . ?
O2 U1 O21 94.47(11) . . ?
O1 U1 O21 86.84(11) . . ?
O3 U1 O21 68.97(9) . . ?
O6 U1 O21 137.30(10) 4_675 . ?
O19 U1 O21 145.68(9) . . ?
O20 U1 O21 66.53(9) . . ?
O4 S1 O5 115.26(19) . . ?
O4 S1 O3 111.18(19) . . ?
O5 S1 O3 109.83(17) . . ?
O4 S1 C1 107.92(17) . . ?
O5 S1 C1 107.75(17) . . ?
O3 S1 C1 104.23(17) . . ?
O7 S2 O8 109.6(3) . . ?
O7 S2 O6 115.8(2) . . ?
O8 S2 O6 109.0(2) . . ?
O7 S2 C10 108.63(19) . . ?
O8 S2 C10 107.1(2) . . ?
O6 S2 C10 106.26(17) . . ?
O9 S3 O10 112.6(2) . . ?
O9 S3 O11 112.44(18) . . ?
O10 S3 O11 111.45(18) . . ?
O9 S3 C17 106.97(18) . . ?
O10 S3 C17 106.69(18) . . ?
O11 S3 C17 106.21(17) . . ?
O14 S4 O13 112.69(18) . . ?
O14 S4 O12 112.79(18) . . ?
O13 S4 O12 111.98(18) . . ?
O14 S4 C24 106.73(18) . . ?
O13 S4 C24 106.37(17) . . ?
O12 S4 C24 105.67(17) . . ?
C41 P1 C47 110.40(18) . . ?
C41 P1 C35 108.7(3) . . ?
C47 P1 C35 106.5(2) . . ?
C41 P1 C29 108.24(16) . . ?
C47 P1 C29 113.4(2) . . ?
C35 P1 C29 109.5(2) . . ?
C71 P2 C65 106.03(16) . . ?
C71 P2 C53 112.74(17) . . ?
C65 P2 C53 109.45(17) . . ?
C71 P2 C59 110.33(17) . . ?
C65 P2 C59 111.48(17) . . ?
C53 P2 C59 106.88(17) . . ?
C89 P3 C77 110.02(18) . . ?
C89 P3 C83 107.57(17) . . ?
C77 P3 C83 111.40(17) . . ?
C89 P3 C95 108.48(17) . . ?
C77 P3 C95 108.75(17) . . ?
C83 P3 C95 110.59(17) . . ?
S1 O3 U1 156.58(19) . . ?
S2 O6 U1 159.29(18) . 4_576 ?
C13 O16 H16 111.5 . . ?
C20 O17 H17 110.7 . . ?
C27 O18 H18A 110.0 . . ?
C27 O18 H18B 111.3 . . ?
H18A O18 H18B 98.3 . . ?
U1 O19 H19A 123.4 . . ?
U1 O19 H19B 139.9 . . ?
H19A O19 H19B 96.7 . . ?
U1 O20 H20A 110.9 . . ?
U1 O20 H20B 108.8 . . ?
H20A O20 H20B 126.6 . . ?
U1 O21 H21A 128.8 . . ?
U1 O21 H21B 120.1 . . ?
H21A O21 H21B 104.2 . . ?
H22A O22 H22B 96.2 . . ?
H23A O23 H23B 104.7 . . ?
H24A O24 H24B 94.0 . . ?
H25A O25 H25B 105.6 . . ?
H26A O26 H26B 110.3 . . ?
H27A O27 H27B 102.0 . . ?
H28A O28 H28B 101.2 . . ?
H29A O29 H29B 96.4 . . ?
H30A O30 H30B 92.5 . . ?
C2 C1 C6 120.8(3) . . ?
C2 C1 S1 121.0(3) . . ?
C6 C1 S1 118.1(3) . . ?
C1 C2 C3 120.2(3) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C2 C3 C4 119.4(3) . . ?
C2 C3 C7 120.6(3) . . ?
C4 C3 C7 119.9(3) . . ?
O15 C4 C3 121.7(3) . . ?
O15 C4 C5 118.2(3) . . ?
C3 C4 C5 120.1(3) . . ?
C6 C5 C4 119.4(3) . . ?
C6 C5 C28 120.9(3) . . ?
C4 C5 C28 119.6(3) . . ?
C5 C6 C1 120.0(3) . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
C8 C7 C3 114.2(3) . . ?
C8 C7 H7A 108.7 . . ?
C3 C7 H7A 108.7 . . ?
C8 C7 H7B 108.7 . . ?
C3 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C9 C8 C13 119.1(3) . . ?
C9 C8 C7 119.7(3) . . ?
C13 C8 C7 121.2(3) . . ?
C8 C9 C10 120.5(4) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C11 C10 C9 120.3(4) . . ?
C11 C10 S2 118.2(3) . . ?
C9 C10 S2 121.5(3) . . ?
C12 C11 C10 120.5(4) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 119.4(3) . . ?
C11 C12 C14 119.5(3) . . ?
C13 C12 C14 121.1(3) . . ?
O16 C13 C8 121.1(3) . . ?
O16 C13 C12 118.7(3) . . ?
C8 C13 C12 120.2(3) . . ?
C15 C14 C12 112.0(3) . . ?
C15 C14 H14A 109.2 . . ?
C12 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C12 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C16 C15 C20 118.6(4) . . ?
C16 C15 C14 120.5(4) . . ?
C20 C15 C14 120.9(3) . . ?
C15 C16 C17 120.9(4) . . ?
C15 C16 H16A 119.5 . . ?
C17 C16 H16A 119.5 . . ?
C18 C17 C16 120.3(4) . . ?
C18 C17 S3 120.9(3) . . ?
C16 C17 S3 118.8(3) . . ?
C17 C18 C19 120.5(4) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C20 119.0(4) . . ?
C18 C19 C21 120.8(4) . . ?
C20 C19 C21 120.1(3) . . ?
O17 C20 C19 118.5(3) . . ?
O17 C20 C15 120.7(4) . . ?
C19 C20 C15 120.8(3) . . ?
C19 C21 C22 111.1(3) . . ?
C19 C21 H21C 109.4 . . ?
C22 C21 H21C 109.4 . . ?
C19 C21 H21D 109.4 . . ?
C22 C21 H21D 109.4 . . ?
H21C C21 H21D 108.0 . . ?
C23 C22 C27 118.5(3) . . ?
C23 C22 C21 119.6(3) . . ?
C27 C22 C21 121.8(3) . . ?
C22 C23 C24 121.0(3) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C25 C24 C23 119.9(3) . . ?
C25 C24 S4 121.5(3) . . ?
C23 C24 S4 118.6(3) . . ?
C24 C25 C26 120.4(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C27 119.1(3) . . ?
C25 C26 C28 118.7(3) . . ?
C27 C26 C28 122.2(3) . . ?
O18 C27 C26 119.5(3) . . ?
O18 C27 C22 119.3(3) . . ?
C26 C27 C22 121.1(3) . . ?
C5 C28 C26 110.8(3) . . ?
C5 C28 H28C 109.5 . . ?
C26 C28 H28C 109.5 . . ?
C5 C28 H28D 109.5 . . ?
C26 C28 H28D 109.5 . . ?
H28C C28 H28D 108.1 . . ?
C30 C29 C34 119.1(3) . . ?
C30 C29 P1 119.9(3) . . ?
C34 C29 P1 120.8(3) . . ?
C31 C30 C29 119.9(4) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C32 C31 C30 120.7(4) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C31 C32 C33 119.9(4) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C34 C33 C32 120.3(4) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C29 120.1(4) . . ?
C33 C34 H34 120.0 . . ?
C29 C34 H34 120.0 . . ?
C36 C35 C40 118.2(5) . . ?
C36 C35 P1 119.8(5) . . ?
C40 C35 P1 122.0(4) . . ?
C35 C36 C37 115.9(6) . . ?
C35 C36 H36 122.0 . . ?
C37 C36 H36 122.0 . . ?
C38 C37 C36 119.4(7) . . ?
C38 C37 H37 120.3 . . ?
C36 C37 H37 120.3 . . ?
C39 C38 C37 125.2(7) . . ?
C39 C38 H38 117.4 . . ?
C37 C38 H38 117.4 . . ?
C38 C39 C40 114.3(7) . . ?
C38 C39 H39 122.9 . . ?
C40 C39 H39 122.9 . . ?
C39 C40 C35 126.9(6) . . ?
C39 C40 H40 116.5 . . ?
C35 C40 H40 116.5 . . ?
C46 C41 C42 120.5(4) . . ?
C46 C41 P1 121.6(3) . . ?
C42 C41 P1 118.0(3) . . ?
C43 C42 C41 119.4(4) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C42 C43 C44 120.3(4) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C43 C44 C45 120.0(4) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C46 C45 C44 120.5(4) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C45 C46 C41 119.4(4) . . ?
C45 C46 H46 120.3 . . ?
C41 C46 H46 120.3 . . ?
C52 C47 C48 118.7(4) . . ?
C52 C47 P1 123.1(3) . . ?
C48 C47 P1 118.1(4) . . ?
C49 C48 C47 121.0(6) . . ?
C49 C48 H48 119.5 . . ?
C47 C48 H48 119.5 . . ?
C50 C49 C48 120.2(6) . . ?
C50 C49 H49 119.9 . . ?
C48 C49 H49 119.9 . . ?
C49 C50 C51 121.1(5) . . ?
C49 C50 H50 119.5 . . ?
C51 C50 H50 119.5 . . ?
C50 C51 C52 118.9(6) . . ?
C50 C51 H51 120.5 . . ?
C52 C51 H51 120.5 . . ?
C47 C52 C51 120.1(5) . . ?
C47 C52 H52 120.0 . . ?
C51 C52 H52 120.0 . . ?
C54 C53 C58 120.1(3) . . ?
C54 C53 P2 119.9(3) . . ?
C58 C53 P2 119.9(3) . . ?
C53 C54 C55 119.8(4) . . ?
C53 C54 H54 120.1 . . ?
C55 C54 H54 120.1 . . ?
C56 C55 C54 119.8(4) . . ?
C56 C55 H55 120.1 . . ?
C54 C55 H55 120.1 . . ?
C55 C56 C57 120.8(4) . . ?
C55 C56 H56 119.6 . . ?
C57 C56 H56 119.6 . . ?
C56 C57 C58 120.0(4) . . ?
C56 C57 H57 120.0 . . ?
C58 C57 H57 120.0 . . ?
C57 C58 C53 119.4(4) . . ?
C57 C58 H58 120.3 . . ?
C53 C58 H58 120.3 . . ?
C64 C59 C60 119.9(4) . . ?
C64 C59 P2 120.6(3) . . ?
C60 C59 P2 119.5(3) . . ?
C61 C60 C59 119.6(4) . . ?
C61 C60 H60 120.2 . . ?
C59 C60 H60 120.2 . . ?
C60 C61 C62 120.5(4) . . ?
C60 C61 H61 119.7 . . ?
C62 C61 H61 119.7 . . ?
C61 C62 C63 120.4(4) . . ?
C61 C62 H62 119.8 . . ?
C63 C62 H62 119.8 . . ?
C62 C63 C64 119.9(4) . . ?
C62 C63 H63 120.0 . . ?
C64 C63 H63 120.0 . . ?
C59 C64 C63 119.6(4) . . ?
C59 C64 H64 120.2 . . ?
C63 C64 H64 120.2 . . ?
C66 C65 C70 119.9(3) . . ?
C66 C65 P2 122.4(3) . . ?
C70 C65 P2 117.7(3) . . ?
C67 C66 C65 119.6(4) . . ?
C67 C66 H66 120.2 . . ?
C65 C66 H66 120.2 . . ?
C68 C67 C66 120.4(4) . . ?
C68 C67 H67 119.8 . . ?
C66 C67 H67 119.8 . . ?
C67 C68 C69 119.8(4) . . ?
C67 C68 H68 120.1 . . ?
C69 C68 H68 120.1 . . ?
C70 C69 C68 120.6(4) . . ?
C70 C69 H69 119.7 . . ?
C68 C69 H69 119.7 . . ?
C69 C70 C65 119.7(4) . . ?
C69 C70 H70 120.1 . . ?
C65 C70 H70 120.1 . . ?
C76 C71 C72 119.7(3) . . ?
C76 C71 P2 122.5(3) . . ?
C72 C71 P2 117.8(3) . . ?
C73 C72 C71 120.1(3) . . ?
C73 C72 H72 119.9 . . ?
C71 C72 H72 119.9 . . ?
C74 C73 C72 119.7(4) . . ?
C74 C73 H73 120.1 . . ?
C72 C73 H73 120.1 . . ?
C75 C74 C73 120.7(4) . . ?
C75 C74 H74 119.7 . . ?
C73 C74 H74 119.7 . . ?
C74 C75 C76 120.3(4) . . ?
C74 C75 H75 119.8 . . ?
C76 C75 H75 119.8 . . ?
C75 C76 C71 119.5(3) . . ?
C75 C76 H76 120.3 . . ?
C71 C76 H76 120.3 . . ?
C82 C77 C78 120.5(4) . . ?
C82 C77 P3 119.4(3) . . ?
C78 C77 P3 120.1(3) . . ?
C79 C78 C77 119.3(4) . . ?
C79 C78 H78 120.4 . . ?
C77 C78 H78 120.4 . . ?
C80 C79 C78 120.1(5) . . ?
C80 C79 H79 119.9 . . ?
C78 C79 H79 119.9 . . ?
C79 C80 C81 120.9(4) . . ?
C79 C80 H80 119.5 . . ?
C81 C80 H80 119.5 . . ?
C80 C81 C82 119.8(4) . . ?
C80 C81 H81 120.1 . . ?
C82 C81 H81 120.1 . . ?
C81 C82 C77 119.3(4) . . ?
C81 C82 H82 120.4 . . ?
C77 C82 H82 120.4 . . ?
C84 C83 C88 119.6(3) . . ?
C84 C83 P3 122.8(3) . . ?
C88 C83 P3 117.6(3) . . ?
C85 C84 C83 119.7(3) . . ?
C85 C84 H84 120.1 . . ?
C83 C84 H84 120.1 . . ?
C84 C85 C86 120.6(3) . . ?
C84 C85 H85 119.7 . . ?
C86 C85 H85 119.7 . . ?
C85 C86 C87 119.7(4) . . ?
C85 C86 H86 120.2 . . ?
C87 C86 H86 120.2 . . ?
C88 C87 C86 120.3(3) . . ?
C88 C87 H87 119.8 . . ?
C86 C87 H87 119.8 . . ?
C87 C88 C83 120.1(3) . . ?
C87 C88 H88 120.0 . . ?
C83 C88 H88 120.0 . . ?
C94 C89 C90 119.6(4) . . ?
C94 C89 P3 121.4(3) . . ?
C90 C89 P3 119.0(3) . . ?
C91 C90 C89 119.6(4) . . ?
C91 C90 H90 120.2 . . ?
C89 C90 H90 120.2 . . ?
C92 C91 C90 120.4(4) . . ?
C92 C91 H91 119.8 . . ?
C90 C91 H91 119.8 . . ?
C91 C92 C93 120.7(4) . . ?
C91 C92 H92 119.6 . . ?
C93 C92 H92 119.6 . . ?
C94 C93 C92 119.7(4) . . ?
C94 C93 H93 120.2 . . ?
C92 C93 H93 120.2 . . ?
C93 C94 C89 119.9(4) . . ?
C93 C94 H94 120.1 . . ?
C89 C94 H94 120.1 . . ?
C100 C95 C96 119.8(3) . . ?
C100 C95 P3 118.9(3) . . ?
C96 C95 P3 121.1(3) . . ?
C97 C96 C95 120.2(4) . . ?
C97 C96 H96 119.9 . . ?
C95 C96 H96 119.9 . . ?
C96 C97 C98 119.9(4) . . ?
C96 C97 H97 120.1 . . ?
C98 C97 H97 120.1 . . ?
C97 C98 C99 120.0(4) . . ?
C97 C98 H98 120.0 . . ?
C99 C98 H98 120.0 . . ?
C100 C99 C98 120.2(4) . . ?
C100 C99 H99 119.9 . . ?
C98 C99 H99 119.9 . . ?
C99 C100 C95 119.8(4) . . ?
C99 C100 H100 120.1 . . ?
C95 C100 H100 120.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O16 H16 O15 0.86 1.79 2.487(4) 136.6 .
O17 H17 O16 0.89 1.68 2.565(4) 171.7 .
O18 H18A O15 0.86 1.90 2.693(4) 152.8 .
O18 H18B O17 0.92 1.92 2.791(4) 159.2 .
O19 H19A O29 0.89 1.83 2.686(4) 160.2 .
O19 H19B O30 0.95 1.74 2.686(4) 172.4 .
O20 H20A O10 0.97 1.79 2.732(5) 163.6 1_655
O20 H20B O24 0.87 1.92 2.640(4) 140.0 4_675
O21 H21A O11 0.74 2.01 2.742(4) 168.7 1_655
O21 H21B O23 0.89 1.78 2.664(4) 168.6 .
O22 H22A O4 0.99 1.98 2.823(4) 142.1 .
O22 H22B O14 0.95 2.07 2.881(4) 142.0 .
O23 H23A O5 0.91 1.90 2.784(4) 163.3 .
O23 H23B O12 0.94 1.87 2.802(4) 170.4 4_676
O24 H24A O7 0.91 1.85 2.667(6) 147.4 .
O24 H24B O28 0.81 2.11 2.906(6) 166.0 4_676
O25 H25A O8 0.86 1.95 2.750(6) 155.3 .
O25 H25B O9 0.75 2.05 2.785(5) 164.6 .
O26 H26A O10 0.95 2.23 3.093(4) 150.9 .
O26 H26B O13 0.94 1.96 2.839(4) 154.1 .
O27 H27A O11 0.93 2.03 2.905(4) 155.8 .
O27 H27B O14 0.93 2.03 2.935(4) 164.7 4_576
O28 H28A O12 0.91 2.07 2.922(5) 155.5 .
O28 H28B O26 0.94 1.86 2.797(4) 171.8 .
O29 H29A O22 0.83 1.96 2.784(4) 169.0 .
O29 H29B O27 0.90 1.87 2.773(4) 172.1 4_675
O30 H30A O25 0.93 1.81 2.705(5) 159.6 4_675
O30 H30B O27 0.91 2.24 3.097(4) 155.5 4_675
C18 H18 O24 0.95 2.57 3.407(6) 146.7 4_575
C30 H30 O5 0.95 2.59 3.364(5) 139.2 .
C34 H34 O18 0.95 2.49 3.181(5) 129.6 2_645
C46 H46 O30 0.95 2.56 3.421(5) 150.9 2_645
C58 H58 O26 0.95 2.55 3.356(5) 142.8 3_666
C64 H64 O13 0.95 2.60 3.213(5) 122.3 3_666
C70 H70 O8 0.95 2.64 3.411(5) 138.9 3_666
C88 H88 O15 0.95 2.38 3.116(4) 134.4 .

_refine_diff_density_max         2.272
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.096

_shelxl_version_number           2014-3

