#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:42:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179420 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/17/4331764.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4331764
loop_
_publ_author_name
'Pierre Thuéry'
_publ_section_title
;
 Sulfonate Complexes of Actinide Ions: Structural Diversity in Uranyl
 Complexes with 2-Sulfobenzoate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              435
_journal_page_last               447
_journal_paper_doi               10.1021/ic3022744
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C40 H54 N4 O38 S4 U5'
_chemical_formula_weight         2517.26
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.2807(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.34650(10)
_cell_length_b                   28.5557(3)
_cell_length_c                   16.3283(2)
_cell_measurement_reflns_used    207332
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      3.00
_cell_volume                     6172.84(11)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and six ω scans with 1° steps (1017 frames)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            207332
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.312
_exptl_absorpt_correction_T_max  0.514
_exptl_absorpt_correction_T_min  0.311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.709
_exptl_crystal_description       needle
_exptl_crystal_F_000             4600
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.611
_refine_diff_density_min         -1.823
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         15900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0555P)²+20.1732P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                13026
_reflns_number_total             15900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3022744_si_002_08.cif
_cod_data_source_block           8
_cod_original_cell_volume        6172.85(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4331764
loop_
_symmetry_equiv_pos_as_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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
U1 U 0.605596(13) 0.106719(7) 0.305259(11) 0.01596(5) Uani 1 1 d .
U2 U 0.329776(15) 0.122310(7) 0.186153(12) 0.01843(6) Uani 1 1 d .
U3 U 0.362171(15) 0.124516(8) 0.417091(12) 0.01854(6) Uani 1 1 d .
U4 U 0.882582(14) 0.119323(7) 0.422705(12) 0.01689(5) Uani 1 1 d .
U5 U 0.850388(14) 0.118516(7) 0.193661(12) 0.01649(5) Uani 1 1 d .
S1 S 0.41700(10) 0.14133(6) -0.01516(9) 0.0241(3) Uani 1 1 d .
S2 S 0.79290(10) 0.15144(5) 0.61673(8) 0.0200(3) Uani 1 1 d .
S3 S 0.35394(12) 0.13907(6) 0.63672(10) 0.0328(4) Uani 1 1 d .
S4 S 0.86588(12) 0.13746(6) -0.02421(9) 0.0277(3) Uani 1 1 d .
O1 O 0.6007(3) 0.04440(15) 0.3025(2) 0.0243(9) Uani 1 1 d .
O2 O 0.6091(3) 0.16891(16) 0.3067(3) 0.0318(10) Uani 1 1 d .
O3 O 0.3018(3) 0.06128(15) 0.1808(3) 0.0279(9) Uani 1 1 d .
O4 O 0.3512(3) 0.18411(16) 0.1882(3) 0.0263(9) Uani 1 1 d .
O5 O 0.3355(3) 0.06419(15) 0.4287(3) 0.0278(9) Uani 1 1 d .
O6 O 0.3867(3) 0.18580(17) 0.4097(3) 0.0330(10) Uani 1 1 d .
O7 O 0.9029(3) 0.05823(15) 0.4421(2) 0.0248(9) Uani 1 1 d .
O8 O 0.8662(3) 0.18109(15) 0.4100(3) 0.0244(9) Uani 1 1 d .
O9 O 0.8693(3) 0.05734(16) 0.1799(3) 0.0286(9) Uani 1 1 d .
O10 O 0.8328(3) 0.17998(15) 0.2030(3) 0.0285(9) Uani 1 1 d .
O11 O 0.4352(3) 0.11206(15) 0.3017(2) 0.0230(9) Uani 1 1 d .
O12 O 0.7750(3) 0.10676(14) 0.3076(2) 0.0196(8) Uani 1 1 d .
O13 O 0.2402(3) 0.13317(17) 0.2998(3) 0.0279(9) Uani 1 1 d .
H13 H 0.2046 0.1088 0.3004 0.034 Uiso 1 1 d R
O14 O 0.9721(3) 0.11787(15) 0.3097(2) 0.0247(9) Uani 1 1 d .
H14 H 1.0199 0.0926 0.3063 0.030 Uiso 1 1 d R
O15 O 0.5050(3) 0.10554(15) 0.1595(2) 0.0227(8) Uani 1 1 d .
O16 O 0.6671(3) 0.10470(16) 0.1612(2) 0.0255(9) Uani 1 1 d .
O17 O 0.3407(3) 0.12526(16) 0.0376(3) 0.0290(10) Uani 1 1 d .
O18 O 0.3703(3) 0.15400(18) -0.0963(3) 0.0353(11) Uani 1 1 d .
O19 O 0.4825(3) 0.17685(16) 0.0256(3) 0.0352(10) Uani 1 1 d .
O20 O 0.5430(3) 0.10452(16) 0.4492(2) 0.0272(9) Uani 1 1 d .
O21 O 0.7051(3) 0.10658(16) 0.4506(2) 0.0252(9) Uani 1 1 d .
O22 O 0.8713(3) 0.13330(15) 0.5686(3) 0.0248(9) Uani 1 1 d .
O23 O 0.7240(3) 0.18365(15) 0.5701(3) 0.0304(10) Uani 1 1 d .
O24 O 0.8377(3) 0.16885(16) 0.6962(3) 0.0297(10) Uani 1 1 d .
O25 O 0.2110(3) 0.14008(17) 0.4745(3) 0.0328(10) Uani 1 1 d .
O26 O 0.0495(3) 0.13317(15) 0.4876(2) 0.0246(9) Uani 1 1 d .
O27 O 0.4060(3) 0.13027(17) 0.5645(3) 0.0313(10) Uani 1 1 d .
O28 O 0.3033(4) 0.18290(19) 0.6323(4) 0.0516(14) Uani 1 1 d .
O29 O 0.4236(4) 0.1326(2) 0.7128(3) 0.0498(15) Uani 1 1 d .
O30 O 1.0048(3) 0.13329(19) 0.1413(3) 0.0378(12) Uani 1 1 d .
O31 O 1.1636(3) 0.13308(15) 0.1205(3) 0.0253(9) Uani 1 1 d .
O32 O 0.8099(3) 0.12569(17) 0.0455(3) 0.0303(10) Uani 1 1 d .
O33 O 0.9206(4) 0.18104(17) -0.0112(4) 0.0466(13) Uani 1 1 d .
O34 O 0.7998(4) 0.1349(2) -0.1008(3) 0.0452(14) Uani 1 1 d .
O35 O 0.1684(4) 0.0027(2) 0.4343(3) 0.0498(14) Uani 1 1 d .
H35A H 0.1896 0.0281 0.4719 0.060 Uiso 1 1 d R
H35B H 0.1254 -0.0104 0.4744 0.060 Uiso 1 1 d R
O36 O 0.1163(3) 0.04832(18) 0.2911(3) 0.0408(12) Uani 1 1 d .
H36A H 0.1662 0.0390 0.2685 0.049 Uiso 1 1 d R
H36B H 0.1185 0.0301 0.3367 0.049 Uiso 1 1 d R
O37 O 0.2558(5) 0.22590(19) 0.0206(4) 0.067(2) Uani 1 1 d .
H37A H 0.2955 0.2311 0.0660 0.081 Uiso 1 1 d R
H37B H 0.2256 0.2553 0.0217 0.081 Uiso 1 1 d R
O38 O 0.4755(4) 0.27165(17) 0.0801(3) 0.0466(13) Uani 1 1 d .
H38A H 0.4855 0.2454 0.0643 0.056 Uiso 1 1 d R
H38B H 0.5131 0.2914 0.0634 0.056 Uiso 1 1 d R
N1 N 0.1553(6) 0.2258(3) 0.2921(5) 0.066(2) Uani 1 1 d .
H1 H 0.1954 0.1983 0.3029 0.079 Uiso 1 1 d R
N2 N 0.0357(6) 0.2931(3) 0.2792(5) 0.061(2) Uani 1 1 d .
H2 H -0.0125 0.3176 0.2733 0.073 Uiso 1 1 d R
N3 N 0.1646(4) 0.20699(18) -0.1292(3) 0.0263(11) Uani 1 1 d .
H3 H 0.2084 0.2057 -0.0784 0.032 Uiso 1 1 d R
N4 N 0.0439(4) 0.20883(18) -0.2582(3) 0.0287(11) Uani 1 1 d .
H4 H 0.0042 0.2139 -0.3018 0.034 Uiso 1 1 d R
C1 C 0.5808(4) 0.09845(19) 0.1222(3) 0.0177(10) Uani 1 1 d .
C2 C 0.5685(4) 0.07855(19) 0.0378(3) 0.0187(11) Uani 1 1 d .
C3 C 0.4937(4) 0.0922(2) -0.0259(3) 0.0216(11) Uani 1 1 d .
C4 C 0.4819(5) 0.0679(2) -0.0991(4) 0.0300(14) Uani 1 1 d .
H4A H 0.4341 0.0778 -0.1420 0.036 Uiso 1 1 calc R
C5 C 0.5399(5) 0.0288(2) -0.1101(4) 0.0346(15) Uani 1 1 d .
H5 H 0.5288 0.0118 -0.1590 0.041 Uiso 1 1 calc R
C6 C 0.6143(5) 0.0150(2) -0.0482(4) 0.0339(15) Uani 1 1 d .
H6 H 0.6533 -0.0113 -0.0555 0.041 Uiso 1 1 calc R
C7 C 0.6310(4) 0.0402(2) 0.0245(4) 0.0269(13) Uani 1 1 d .
H7 H 0.6836 0.0319 0.0648 0.032 Uiso 1 1 calc R
C8 C 0.6299(4) 0.10069(19) 0.4897(3) 0.0178(10) Uani 1 1 d .
C9 C 0.6431(4) 0.08494(19) 0.5758(3) 0.0183(10) Uani 1 1 d .
C10 C 0.7187(4) 0.10253(19) 0.6362(3) 0.0177(10) Uani 1 1 d .
C11 C 0.7336(4) 0.0827(2) 0.7145(4) 0.0255(12) Uani 1 1 d .
H11 H 0.7813 0.0954 0.7548 0.031 Uiso 1 1 calc R
C12 C 0.6780(5) 0.0444(2) 0.7327(4) 0.0306(14) Uani 1 1 d .
H12 H 0.6905 0.0304 0.7844 0.037 Uiso 1 1 calc R
C13 C 0.6023(5) 0.0261(2) 0.6735(4) 0.0332(15) Uani 1 1 d .
H13A H 0.5646 0.0002 0.6856 0.040 Uiso 1 1 calc R
C14 C 0.5850(5) 0.0473(2) 0.5972(4) 0.0285(13) Uani 1 1 d .
H14A H 0.5331 0.0361 0.5588 0.034 Uiso 1 1 calc R
C15 C 0.1415(4) 0.1251(2) 0.5120(3) 0.0207(11) Uani 1 1 d .
C16 C 0.1664(4) 0.0950(2) 0.5877(3) 0.0213(11) Uani 1 1 d .
C17 C 0.2590(4) 0.0958(2) 0.6391(4) 0.0263(13) Uani 1 1 d .
C18 C 0.2782(5) 0.0628(3) 0.7018(4) 0.0449(19) Uani 1 1 d .
H18 H 0.3406 0.0629 0.7343 0.054 Uiso 1 1 calc R
C19 C 0.2068(6) 0.0301(3) 0.7169(5) 0.048(2) Uani 1 1 d .
H19 H 0.2209 0.0080 0.7586 0.057 Uiso 1 1 calc R
C20 C 0.1133(5) 0.0308(3) 0.6686(5) 0.0396(17) Uani 1 1 d .
H20 H 0.0633 0.0097 0.6791 0.048 Uiso 1 1 calc R
C21 C 0.0948(5) 0.0623(2) 0.6059(4) 0.0283(13) Uani 1 1 d .
H21 H 0.0320 0.0620 0.5740 0.034 Uiso 1 1 calc R
C22 C 1.0732(4) 0.1213(2) 0.1004(3) 0.0216(11) Uani 1 1 d .
C23 C 1.0491(4) 0.0907(2) 0.0255(4) 0.0261(12) Uani 1 1 d .
C24 C 0.9590(4) 0.0930(2) -0.0293(4) 0.0243(12) Uani 1 1 d .
C25 C 0.9416(5) 0.0620(3) -0.0944(4) 0.0377(16) Uani 1 1 d .
H25 H 0.8815 0.0637 -0.1301 0.045 Uiso 1 1 calc R
C26 C 1.0128(6) 0.0284(3) -0.1071(5) 0.054(2) Uani 1 1 d .
H26 H 1.0003 0.0073 -0.1506 0.065 Uiso 1 1 calc R
C27 C 1.1028(6) 0.0262(3) -0.0546(5) 0.052(2) Uani 1 1 d .
H27 H 1.1513 0.0039 -0.0630 0.063 Uiso 1 1 calc R
C28 C 1.1197(5) 0.0572(3) 0.0099(4) 0.0411(18) Uani 1 1 d .
H28 H 1.1807 0.0557 0.0444 0.049 Uiso 1 1 calc R
C29 C 0.1173(9) 0.2320(4) 0.2107(7) 0.085(4) Uani 1 1 d .
H29A H 0.0773 0.2051 0.1907 0.102 Uiso 1 1 calc R
H29B H 0.1722 0.2355 0.1775 0.102 Uiso 1 1 calc R
C30 C 0.0530(8) 0.2752(4) 0.2040(9) 0.105(5) Uani 1 1 d .
H30A H 0.0857 0.2990 0.1743 0.126 Uiso 1 1 calc R
H30B H -0.0113 0.2679 0.1720 0.126 Uiso 1 1 calc R
C31 C 0.0730(6) 0.2171(3) 0.3479(7) 0.059(3) Uani 1 1 d .
H31A H 0.0983 0.2228 0.4053 0.071 Uiso 1 1 calc R
H31B H 0.0476 0.1853 0.3420 0.071 Uiso 1 1 calc R
C32 C -0.0100(6) 0.2529(4) 0.3163(7) 0.077(3) Uani 1 1 d .
H32A H -0.0594 0.2382 0.2755 0.093 Uiso 1 1 calc R
H32B H -0.0445 0.2634 0.3618 0.093 Uiso 1 1 calc R
C33 C 0.2126(7) 0.2688(4) 0.3210(6) 0.075(3) Uani 1 1 d .
H33A H 0.2590 0.2775 0.2825 0.090 Uiso 1 1 calc R
H33B H 0.2508 0.2636 0.3748 0.090 Uiso 1 1 calc R
C34 C 0.1295(7) 0.3089(3) 0.3259(8) 0.077(3) Uani 1 1 d .
H34A H 0.1198 0.3146 0.3829 0.093 Uiso 1 1 calc R
H34B H 0.1515 0.3379 0.3027 0.093 Uiso 1 1 calc R
C35 C 0.2158(4) 0.2279(2) -0.1958(4) 0.0311(14) Uani 1 1 d .
H35C H 0.2693 0.2073 -0.2091 0.037 Uiso 1 1 calc R
H35D H 0.2455 0.2577 -0.1779 0.037 Uiso 1 1 calc R
C36 C 0.1372(5) 0.2347(3) -0.2719(4) 0.0329(14) Uani 1 1 d .
H36C H 0.1223 0.2677 -0.2801 0.040 Uiso 1 1 calc R
H36D H 0.1631 0.2228 -0.3207 0.040 Uiso 1 1 calc R
C37 C 0.0732(4) 0.2348(2) -0.1145(4) 0.0270(13) Uani 1 1 d .
H37C H 0.0915 0.2674 -0.1044 0.032 Uiso 1 1 calc R
H37D H 0.0454 0.2228 -0.0666 0.032 Uiso 1 1 calc R
C38 C -0.0049(4) 0.2307(2) -0.1914(4) 0.0292(13) Uani 1 1 d .
H38C H -0.0614 0.2117 -0.1792 0.035 Uiso 1 1 calc R
H38D H -0.0301 0.2615 -0.2084 0.035 Uiso 1 1 calc R
C39 C 0.1324(5) 0.1577(2) -0.1521(5) 0.0378(16) Uani 1 1 d .
H39A H 0.0928 0.1450 -0.1115 0.045 Uiso 1 1 calc R
H39B H 0.1914 0.1380 -0.1537 0.045 Uiso 1 1 calc R
C40 C 0.0699(5) 0.1587(2) -0.2363(5) 0.0401(17) Uani 1 1 d .
H40A H 0.1080 0.1452 -0.2773 0.048 Uiso 1 1 calc R
H40B H 0.0087 0.1406 -0.2352 0.048 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 U1 O1 179.17(19) . .
O2 U1 O12 88.54(16) . .
O1 U1 O12 91.96(15) . .
O2 U1 O11 87.58(17) . .
O1 U1 O11 91.91(16) . .
O12 U1 O11 176.09(16) . .
O2 U1 O21 88.83(17) . .
O1 U1 O21 91.97(16) . .
O12 U1 O21 65.48(13) . .
O11 U1 O21 114.96(13) . .
O2 U1 O15 92.01(17) . .
O1 U1 O15 87.18(16) . .
O12 U1 O15 114.74(12) . .
O11 U1 O15 64.89(13) . .
O21 U1 O15 179.14(15) . .
O2 U1 O16 91.35(17) . .
O1 U1 O16 88.27(16) . .
O12 U1 O16 65.33(13) . .
O11 U1 O16 114.22(13) . .
O21 U1 O16 130.78(12) . .
O15 U1 O16 49.41(12) . .
O2 U1 O20 91.33(17) . .
O1 U1 O20 89.06(16) . .
O12 U1 O20 114.97(13) . .
O11 U1 O20 65.68(13) . .
O21 U1 O20 49.51(12) . .
O15 U1 O20 130.24(12) . .
O16 U1 O20 177.32(15) . .
O3 U2 O4 176.82(18) . .
O3 U2 O11 91.07(17) . .
O4 U2 O11 91.80(17) . .
O3 U2 O13 92.46(18) . .
O4 U2 O13 87.17(17) . .
O11 U2 O13 71.23(14) . .
O3 U2 O31 85.76(17) . 1_455
O4 U2 O31 91.07(17) . 1_455
O11 U2 O31 149.26(14) . 1_455
O13 U2 O31 78.36(14) . 1_455
O3 U2 O17 91.37(18) . .
O4 U2 O17 87.45(17) . .
O11 U2 O17 137.20(13) . .
O13 U2 O17 151.23(14) . .
O31 U2 O17 73.51(14) 1_455 .
O3 U2 O15 89.95(17) . .
O4 U2 O15 92.42(16) . .
O11 U2 O15 67.32(13) . .
O13 U2 O15 138.52(13) . .
O31 U2 O15 143.08(13) 1_455 .
O17 U2 O15 69.96(13) . .
O5 U3 O6 177.38(19) . .
O5 U3 O11 92.85(18) . .
O6 U3 O11 89.77(18) . .
O5 U3 O13 93.48(18) . .
O6 U3 O13 87.48(19) . .
O11 U3 O13 70.48(13) . .
O5 U3 O25 86.98(18) . .
O6 U3 O25 90.88(18) . .
O11 U3 O25 146.97(15) . .
O13 U3 O25 76.56(15) . .
O5 U3 O27 89.22(18) . .
O6 U3 O27 88.70(19) . .
O11 U3 O27 140.25(14) . .
O13 U3 O27 149.02(14) . .
O25 U3 O27 72.77(15) . .
O5 U3 O20 87.55(17) . .
O6 U3 O20 93.35(18) . .
O11 U3 O20 68.09(13) . .
O13 U3 O20 138.56(13) . .
O25 U3 O20 144.74(14) . .
O27 U3 O20 72.35(14) . .
O8 U4 O7 176.29(18) . .
O8 U4 O12 90.25(17) . .
O7 U4 O12 93.37(17) . .
O8 U4 O14 89.60(17) . .
O7 U4 O14 92.38(17) . .
O12 U4 O14 70.78(14) . .
O8 U4 O26 88.95(17) . 1_655
O7 U4 O26 88.34(17) . 1_655
O12 U4 O26 149.80(13) . 1_655
O14 U4 O26 79.02(14) . 1_655
O8 U4 O22 86.00(17) . .
O7 U4 O22 90.77(17) . .
O12 U4 O22 137.06(13) . .
O14 U4 O22 151.72(13) . .
O26 U4 O22 72.98(13) 1_655 .
O8 U4 O21 93.44(16) . .
O7 U4 O21 87.20(17) . .
O12 U4 O21 66.95(13) . .
O14 U4 O21 137.62(14) . .
O26 U4 O21 143.23(13) 1_655 .
O22 U4 O21 70.61(13) . .
O10 U5 O9 177.58(19) . .
O10 U5 O12 89.89(17) . .
O9 U5 O12 92.46(17) . .
O10 U5 O14 91.37(18) . .
O9 U5 O14 89.96(18) . .
O12 U5 O14 70.49(13) . .
O10 U5 O30 89.19(19) . .
O9 U5 O30 89.18(19) . .
O12 U5 O30 145.76(14) . .
O14 U5 O30 75.31(15) . .
O10 U5 O32 89.28(18) . .
O9 U5 O32 88.54(18) . .
O12 U5 O32 140.59(13) . .
O14 U5 O32 148.92(13) . .
O30 U5 O32 73.62(15) . .
O10 U5 O16 92.19(17) . .
O9 U5 O16 88.19(18) . .
O12 U5 O16 67.57(13) . .
O14 U5 O16 137.90(13) . .
O30 U5 O16 146.66(14) . .
O32 U5 O16 73.09(13) . .
O18 S1 O19 114.5(3) . .
O18 S1 O17 111.3(3) . .
O19 S1 O17 111.6(3) . .
O18 S1 C3 107.4(3) . .
O19 S1 C3 106.2(3) . .
O17 S1 C3 105.2(3) . .
O24 S2 O23 114.6(3) . .
O24 S2 O22 110.9(2) . .
O23 S2 O22 112.8(3) . .
O24 S2 C10 106.7(3) . .
O23 S2 C10 105.3(3) . .
O22 S2 C10 105.7(2) . .
O28 S3 O27 112.4(3) . .
O28 S3 O29 113.6(4) . .
O27 S3 O29 110.2(3) . .
O28 S3 C17 106.2(3) . .
O27 S3 C17 108.2(3) . .
O29 S3 C17 105.8(3) . .
O34 S4 O33 114.5(4) . .
O34 S4 O32 110.1(3) . .
O33 S4 O32 112.3(3) . .
O34 S4 C24 106.1(3) . .
O33 S4 C24 106.1(3) . .
O32 S4 C24 107.3(3) . .
U2 O11 U3 113.20(16) . .
U2 O11 U1 123.58(17) . .
U3 O11 U1 121.75(17) . .
U4 O12 U5 111.27(15) . .
U4 O12 U1 123.19(17) . .
U5 O12 U1 122.59(17) . .
U2 O13 U3 104.99(15) . .
U2 O13 H13 104.1 . .
U3 O13 H13 103.6 . .
U4 O14 U5 105.63(15) . .
U4 O14 H14 117.9 . .
U5 O14 H14 110.8 . .
C1 O15 U2 161.4(4) . .
C1 O15 U1 95.3(3) . .
U2 O15 U1 103.16(13) . .
C1 O16 U5 162.1(4) . .
C1 O16 U1 95.0(3) . .
U5 O16 U1 102.78(14) . .
S1 O17 U2 135.6(3) . .
C8 O20 U3 159.6(4) . .
C8 O20 U1 95.6(3) . .
U3 O20 U1 102.74(14) . .
C8 O21 U4 160.5(4) . .
C8 O21 U1 96.6(3) . .
U4 O21 U1 102.86(14) . .
S2 O22 U4 135.3(2) . .
C15 O25 U3 148.2(4) . .
C15 O26 U4 158.3(4) . 1_455
S3 O27 U3 137.4(3) . .
C22 O30 U5 151.1(4) . .
C22 O31 U2 154.3(4) . 1_655
S4 O32 U5 136.0(2) . .
H35A O35 H35B 90.6 . .
H36A O36 H36B 103.4 . .
H37A O37 H37B 92.7 . .
H38A O38 H38B 113.4 . .
C29 N1 C33 108.1(8) . .
C29 N1 C31 113.1(9) . .
C33 N1 C31 108.8(8) . .
C29 N1 H1 114.5 . .
C33 N1 H1 111.5 . .
C31 N1 H1 100.8 . .
C30 N2 C34 110.7(9) . .
C30 N2 C32 101.7(10) . .
C34 N2 C32 113.8(8) . .
C30 N2 H2 111.8 . .
C34 N2 H2 110.6 . .
C32 N2 H2 107.9 . .
C35 N3 C37 111.4(5) . .
C35 N3 C39 109.7(5) . .
C37 N3 C39 108.9(5) . .
C35 N3 H3 111.4 . .
C37 N3 H3 107.7 . .
C39 N3 H3 107.7 . .
C38 N4 C36 110.9(5) . .
C38 N4 C40 109.7(5) . .
C36 N4 C40 109.5(5) . .
C38 N4 H4 105.3 . .
C36 N4 H4 103.6 . .
C40 N4 H4 117.6 . .
O16 C1 O15 118.2(5) . .
O16 C1 C2 120.9(5) . .
O15 C1 C2 120.7(5) . .
C3 C2 C7 118.7(5) . .
C3 C2 C1 124.6(5) . .
C7 C2 C1 116.4(5) . .
C4 C3 C2 119.8(5) . .
C4 C3 S1 119.1(5) . .
C2 C3 S1 121.1(4) . .
C3 C4 C5 121.1(6) . .
C3 C4 H4A 119.5 . .
C5 C4 H4A 119.5 . .
C6 C5 C4 119.9(6) . .
C6 C5 H5 120.1 . .
C4 C5 H5 120.1 . .
C5 C6 C7 120.2(6) . .
C5 C6 H6 119.9 . .
C7 C6 H6 119.9 . .
C6 C7 C2 120.2(6) . .
C6 C7 H7 119.9 . .
C2 C7 H7 119.9 . .
O20 C8 O21 117.2(5) . .
O20 C8 C9 121.3(5) . .
O21 C8 C9 121.2(5) . .
C14 C9 C10 118.0(5) . .
C14 C9 C8 118.3(5) . .
C10 C9 C8 123.4(5) . .
C11 C10 C9 120.3(5) . .
C11 C10 S2 118.0(4) . .
C9 C10 S2 121.6(4) . .
C12 C11 C10 120.3(6) . .
C12 C11 H11 119.9 . .
C10 C11 H11 119.9 . .
C11 C12 C13 120.5(6) . .
C11 C12 H12 119.8 . .
C13 C12 H12 119.8 . .
C14 C13 C12 118.8(6) . .
C14 C13 H13A 120.6 . .
C12 C13 H13A 120.6 . .
C13 C14 C9 122.0(6) . .
C13 C14 H14A 119.0 . .
C9 C14 H14A 119.0 . .
O25 C15 O26 122.3(5) . .
O25 C15 C16 119.8(5) . .
O26 C15 C16 117.9(5) . .
C21 C16 C17 117.3(5) . .
C21 C16 C15 118.1(5) . .
C17 C16 C15 124.5(5) . .
C18 C17 C16 119.7(6) . .
C18 C17 S3 115.0(5) . .
C16 C17 S3 125.2(5) . .
C19 C18 C17 121.5(6) . .
C19 C18 H18 119.2 . .
C17 C18 H18 119.2 . .
C18 C19 C20 118.7(7) . .
C18 C19 H19 120.7 . .
C20 C19 H19 120.7 . .
C21 C20 C19 120.0(7) . .
C21 C20 H20 120.0 . .
C19 C20 H20 120.0 . .
C20 C21 C16 122.6(6) . .
C20 C21 H21 118.7 . .
C16 C21 H21 118.7 . .
O30 C22 O31 122.0(5) . .
O30 C22 C23 120.0(5) . .
O31 C22 C23 117.9(5) . .
C28 C23 C24 117.4(6) . .
C28 C23 C22 118.0(5) . .
C24 C23 C22 124.6(5) . .
C25 C24 C23 120.4(5) . .
C25 C24 S4 116.2(5) . .
C23 C24 S4 123.2(5) . .
C24 C25 C26 120.5(6) . .
C24 C25 H25 119.7 . .
C26 C25 H25 119.7 . .
C25 C26 C27 119.8(7) . .
C25 C26 H26 120.1 . .
C27 C26 H26 120.1 . .
C28 C27 C26 119.4(7) . .
C28 C27 H27 120.3 . .
C26 C27 H27 120.3 . .
C27 C28 C23 122.4(6) . .
C27 C28 H28 118.8 . .
C23 C28 H28 118.8 . .
N1 C29 C30 108.4(10) . .
N1 C29 H29A 110.0 . .
C30 C29 H29A 110.0 . .
N1 C29 H29B 110.0 . .
C30 C29 H29B 110.0 . .
H29A C29 H29B 108.4 . .
N2 C30 C29 113.6(12) . .
N2 C30 H30A 108.9 . .
C29 C30 H30A 108.9 . .
N2 C30 H30B 108.9 . .
C29 C30 H30B 108.9 . .
H30A C30 H30B 107.7 . .
N1 C31 C32 103.4(7) . .
N1 C31 H31A 111.1 . .
C32 C31 H31A 111.1 . .
N1 C31 H31B 111.1 . .
C32 C31 H31B 111.1 . .
H31A C31 H31B 109.0 . .
N2 C32 C31 109.7(7) . .
N2 C32 H32A 109.7 . .
C31 C32 H32A 109.7 . .
N2 C32 H32B 109.7 . .
C31 C32 H32B 109.7 . .
H32A C32 H32B 108.2 . .
N1 C33 C34 106.0(7) . .
N1 C33 H33A 110.5 . .
C34 C33 H33A 110.5 . .
N1 C33 H33B 110.5 . .
C34 C33 H33B 110.5 . .
H33A C33 H33B 108.7 . .
N2 C34 C33 107.8(7) . .
N2 C34 H34A 110.1 . .
C33 C34 H34A 110.1 . .
N2 C34 H34B 110.1 . .
C33 C34 H34B 110.1 . .
H34A C34 H34B 108.5 . .
N3 C35 C36 108.3(5) . .
N3 C35 H35C 110.0 . .
C36 C35 H35C 110.0 . .
N3 C35 H35D 110.0 . .
C36 C35 H35D 110.0 . .
H35C C35 H35D 108.4 . .
N4 C36 C35 108.3(5) . .
N4 C36 H36C 110.0 . .
C35 C36 H36C 110.0 . .
N4 C36 H36D 110.0 . .
C35 C36 H36D 110.0 . .
H36C C36 H36D 108.4 . .
N3 C37 C38 108.1(5) . .
N3 C37 H37C 110.1 . .
C38 C37 H37C 110.1 . .
N3 C37 H37D 110.1 . .
C38 C37 H37D 110.1 . .
H37C C37 H37D 108.4 . .
N4 C38 C37 108.7(5) . .
N4 C38 H38C 110.0 . .
C37 C38 H38C 110.0 . .
N4 C38 H38D 110.0 . .
C37 C38 H38D 110.0 . .
H38C C38 H38D 108.3 . .
N3 C39 C40 108.4(5) . .
N3 C39 H39A 110.0 . .
C40 C39 H39A 110.0 . .
N3 C39 H39B 110.0 . .
C40 C39 H39B 110.0 . .
H39A C39 H39B 108.4 . .
N4 C40 C39 108.5(5) . .
N4 C40 H40A 110.0 . .
C39 C40 H40A 110.0 . .
N4 C40 H40B 110.0 . .
C39 C40 H40B 110.0 . .
H40A C40 H40B 108.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.777(5) .
U1 O1 1.781(4) .
U1 O12 2.256(4) .
U1 O11 2.273(4) .
U1 O21 2.569(4) .
U1 O15 2.580(4) .
U1 O16 2.588(4) .
U1 O20 2.592(4) .
U1 U5 3.9518(3) .
U1 U3 3.9562(3) .
U2 O3 1.782(4) .
U2 O4 1.787(4) .
U2 O11 2.226(4) .
U2 O13 2.352(4) .
U2 O31 2.358(4) 1_455
U2 O17 2.450(4) .
U2 O15 2.479(4) .
U2 U3 3.7412(3) .
U3 O5 1.774(4) .
U3 O6 1.787(5) .
U3 O11 2.256(4) .
U3 O13 2.364(4) .
U3 O25 2.372(4) .
U3 O27 2.410(4) .
U3 O20 2.471(4) .
U4 O8 1.786(4) .
U4 O7 1.787(4) .
U4 O12 2.245(4) .
U4 O14 2.322(4) .
U4 O26 2.375(4) 1_655
U4 O22 2.439(4) .
U4 O21 2.495(4) .
U4 U5 3.7101(3) .
U5 O10 1.780(4) .
U5 O9 1.783(4) .
U5 O12 2.249(4) .
U5 O14 2.334(4) .
U5 O30 2.367(4) .
U5 O32 2.420(4) .
U5 O16 2.468(4) .
S1 O18 1.437(4) .
S1 O19 1.445(5) .
S1 O17 1.488(5) .
S1 C3 1.758(6) .
S2 O24 1.446(4) .
S2 O23 1.447(4) .
S2 O22 1.480(4) .
S2 C10 1.764(5) .
S3 O28 1.420(6) .
S3 O27 1.464(4) .
S3 O29 1.467(6) .
S3 C17 1.774(6) .
S4 O34 1.437(5) .
S4 O33 1.445(5) .
S4 O32 1.477(4) .
S4 C24 1.785(6) .
O13 H13 0.8433 .
O14 H14 0.9687 .
O15 C1 1.262(6) .
O16 C1 1.256(6) .
O20 C8 1.265(6) .
O21 C8 1.267(6) .
O25 C15 1.250(7) .
O26 C15 1.264(7) .
O26 U4 2.375(4) 1_455
O30 C22 1.246(7) .
O31 C22 1.256(7) .
O31 U2 2.358(4) 1_655
O35 H35A 0.9691 .
O35 H35B 0.9974 .
O36 H36A 0.8447 .
O36 H36B 0.9054 .
O37 H37A 0.8684 .
O37 H37B 0.9318 .
O38 H38A 0.8081 .
O38 H38B 0.8237 .
N1 C29 1.373(13) .
N1 C33 1.492(12) .
N1 C31 1.533(10) .
N1 H1 0.9540 .
N2 C30 1.377(14) .
N2 C34 1.453(11) .
N2 C32 1.465(11) .
N2 H2 0.9483 .
N3 C35 1.481(8) .
N3 C37 1.500(7) .
N3 C39 1.504(8) .
N3 H3 0.9527 .
N4 C38 1.477(8) .
N4 C36 1.489(8) .
N4 C40 1.504(8) .
N4 H4 0.8444 .
C1 C2 1.480(7) .
C2 C3 1.404(8) .
C2 C7 1.410(8) .
C3 C4 1.374(8) .
C4 C5 1.384(9) .
C4 H4A 0.9300 .
C5 C6 1.381(10) .
C5 H5 0.9300 .
C6 C7 1.383(9) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C8 C9 1.465(7) .
C9 C14 1.396(8) .
C9 C10 1.411(7) .
C10 C11 1.389(8) .
C11 C12 1.376(9) .
C11 H11 0.9300 .
C12 C13 1.407(9) .
C12 H12 0.9300 .
C13 C14 1.377(9) .
C13 H13A 0.9300 .
C14 H14A 0.9300 .
C15 C16 1.508(8) .
C16 C21 1.394(8) .
C16 C17 1.403(8) .
C17 C18 1.390(10) .
C18 C19 1.380(10) .
C18 H18 0.9300 .
C19 C20 1.389(10) .
C19 H19 0.9300 .
C20 C21 1.361(9) .
C20 H20 0.9300 .
C21 H21 0.9300 .
C22 C23 1.503(8) .
C23 C28 1.389(9) .
C23 C24 1.407(8) .
C24 C25 1.381(8) .
C25 C26 1.385(10) .
C25 H25 0.9300 .
C26 C27 1.385(10) .
C26 H26 0.9300 .
C27 C28 1.373(10) .
C27 H27 0.9300 .
C28 H28 0.9300 .
C29 C30 1.498(14) .
C29 H29A 0.9700 .
C29 H29B 0.9700 .
C30 H30A 0.9700 .
C30 H30B 0.9700 .
C31 C32 1.548(12) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C32 H32A 0.9700 .
C32 H32B 0.9700 .
C33 C34 1.604(14) .
C33 H33A 0.9700 .
C33 H33B 0.9700 .
C34 H34A 0.9700 .
C34 H34B 0.9700 .
C35 C36 1.534(9) .
C35 H35C 0.9700 .
C35 H35D 0.9700 .
C36 H36C 0.9700 .
C36 H36D 0.9700 .
C37 C38 1.531(9) .
C37 H37C 0.9700 .
C37 H37D 0.9700 .
C38 H38C 0.9700 .
C38 H38D 0.9700 .
C39 C40 1.515(10) .
C39 H39A 0.9700 .
C39 H39B 0.9700 .
C40 H40A 0.9700 .
C40 H40B 0.9700 .
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 H13 O36 0.84 2.09 2.927(7) 175.2 .
O14 H14 O36 0.97 1.84 2.808(6) 173.8 1_655
O35 H35A O5 0.97 2.39 2.848(6) 108.6 .
O35 H35B O7 1.00 2.00 2.915(6) 151.5 3_656
O36 H36A O3 0.84 2.53 3.262(7) 146.1 .
O36 H36B O35 0.91 1.82 2.689(7) 159.2 .
O37 H37A O4 0.87 2.44 3.107(7) 133.8 .
O37 H37B O23 0.93 1.92 2.755(6) 148.7 4_565
O38 H38A O19 0.81 2.06 2.855(7) 169.2 .
O38 H38B O26 0.82 2.56 3.319(7) 153.6 4_665
N1 H1 O13 0.95 1.96 2.873(9) 160.7 .
N2 H2 O29 0.95 1.87 2.739(9) 150.8 4_565
N3 H3 O37 0.95 1.76 2.646(8) 153.8 .
N4 H4 O38 0.84 1.96 2.741(8) 152.7 4_565
N4 H4 O24 0.84 2.56 2.985(6) 112.0 1_454
