#------------------------------------------------------------------------------
#$Date: 2017-03-09 01:48:00 +0200 (Thu, 09 Mar 2017) $
#$Revision: 194094 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/55/4345527.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_4345527
loop_
_publ_author_name
'Xie, Zhen-ni'
'Mei, Lei'
'Hu, Kong-qiu'
'Xia, Liang-shu'
'Chai, Zhi-fang'
'Shi, Wei-qun'
_publ_section_title
;
 Mixed-Ligand Uranyl Polyrotaxanes Incorporating a Sulfate/Oxalate
 Coligand: Achieving Structural Diversity via pH-Dependent Competitive
 Effect
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b02515
_journal_year                    2017
_chemical_formula_sum            'C31 H30 N13 O21 U2'
_chemical_formula_weight         1396.74
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                97.075(8)
_cell_angle_beta                 109.271(7)
_cell_angle_gamma                104.827(7)
_cell_formula_units_Z            2
_cell_length_a                   11.5890(19)
_cell_length_b                   12.452(2)
_cell_length_c                   16.987(3)
_cell_measurement_reflns_used    9402
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      3.01
_cell_volume                     2178.3(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-III CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            60375
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.736
_exptl_absorpt_coefficient_mu    7.521
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.129
_exptl_crystal_description       block
_exptl_crystal_F_000             1318
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.722
_refine_diff_density_min         -1.599
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0211P)²+21.4540P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8121
_reflns_number_total             9948
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02515_si_002.cif
_cod_data_source_block           UPO3
_cod_original_cell_volume        2178.4(7)
_cod_database_code               4345527
_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.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
U1 U 1.79162(2) 0.32349(3) 0.53805(2) 0.03582(8) Uani 1 1 d . .
N1 N 0.8530(6) 0.4090(5) 0.1201(4) 0.0348(14) Uani 1 1 d . .
C1 C 2.0519(6) 0.5023(7) 0.5436(4) 0.0358(17) Uani 1 1 d . .
O1 O 1.8984(6) 0.2813(7) 0.6709(5) 0.0665(19) Uani 1 1 d . .
H1A H 1.8917 0.3234 0.7151 0.100 Uiso 1 1 d R U
H1B H 1.9830 0.2956 0.6821 0.100 Uiso 1 1 d R U
O3 O 1.7580(6) 0.4354(6) 0.5913(4) 0.0542(15) Uani 1 1 d . .
C3 C 1.4854(7) 0.2347(7) 0.4323(5) 0.0384(17) Uani 1 1 d . .
N3 N 0.5754(6) 0.8949(5) 0.0786(4) 0.0405(15) Uani 1 1 d . .
U2 U 1.19408(2) 0.13391(2) 0.42545(2) 0.02649(7) Uani 1 1 d . .
N2 N 0.5862(6) 0.8755(5) -0.0500(4) 0.0401(15) Uani 1 1 d . .
C2 C 1.5024(7) 0.1793(7) 0.5093(5) 0.0360(16) Uani 1 1 d . .
O2 O 1.8234(7) 0.2144(6) 0.4832(5) 0.0660(19) Uani 1 1 d . .
O4 O 2.0139(5) 0.4419(6) 0.5888(3) 0.0483(15) Uani 1 1 d . .
N4 N 0.5228(6) 0.8040(5) 0.1856(4) 0.0355(14) Uani 1 1 d . .
C4 C 1.0567(6) -0.0086(6) 0.5353(4) 0.0296(14) Uani 1 1 d . .
O5 O 1.5853(5) 0.2907(5) 0.4242(4) 0.0481(15) Uani 1 1 d . .
N5 N 0.4364(7) 0.6635(6) 0.2381(4) 0.0427(16) Uani 1 1 d . .
C5 C 1.0373(6) 0.1820(6) 0.2343(5) 0.0331(15) Uani 1 1 d . .
O6 O 1.6149(5) 0.1927(6) 0.5575(4) 0.0496(15) Uani 1 1 d . .
N6 N 0.3329(7) 0.4602(6) 0.2117(5) 0.0457(16) Uani 1 1 d . .
C6 C 0.9739(6) 0.2648(6) 0.1944(4) 0.0279(14) Uani 1 1 d . .
O7 O 1.4030(4) 0.1254(5) 0.5175(3) 0.0394(12) Uani 1 1 d . .
N7 N 0.2553(7) 0.2902(7) 0.1225(5) 0.0497(18) Uani 1 1 d . .
C7 C 0.9766(8) 0.3619(7) 0.2447(5) 0.0415(18) Uani 1 1 d . .
H7 H 1.0209 0.3796 0.3037 0.050 Uiso 1 1 calc R U
O009 O 2.1629(5) 0.5664(5) 0.5593(3) 0.0460(14) Uani 1 1 d . .
O9 O 1.2273(6) 0.2641(5) 0.4964(4) 0.0502(14) Uani 1 1 d . .
N9 N 0.7845(6) 0.8677(6) 0.1418(4) 0.0438(16) Uani 1 1 d . .
C9 C 0.8532(7) 0.3179(6) 0.0708(4) 0.0337(15) Uani 1 1 d . .
H9 H 0.8136 0.3049 0.0116 0.040 Uiso 1 1 calc R U
O8 O 1.3722(5) 0.2236(5) 0.3858(3) 0.0456(14) Uani 1 1 d . .
N8 N 0.7898(6) 0.8360(6) 0.0116(5) 0.0442(16) Uani 1 1 d . .
C8 C 0.9122(8) 0.4329(7) 0.2059(5) 0.047(2) Uani 1 1 d . .
H8 H 0.9100 0.4970 0.2392 0.057 Uiso 1 1 calc R U
O10 O 1.1631(5) 0.0040(5) 0.3564(3) 0.0390(12) Uani 1 1 d . .
N10 N 0.7406(7) 0.7970(6) 0.2576(4) 0.0456(17) Uani 1 1 d . .
C10 C 0.9112(7) 0.2421(6) 0.1061(4) 0.0330(15) Uani 1 1 d . .
H10 H 0.9085 0.1769 0.0714 0.040 Uiso 1 1 calc R U
O11 O 1.0945(5) 0.2108(5) 0.3155(3) 0.0434(13) Uani 1 1 d . .
N11 N 0.6467(6) 0.6336(6) 0.2851(4) 0.0413(15) Uani 1 1 d . .
C11 C 0.7855(8) 0.4879(7) 0.0786(6) 0.0444(19) Uani 1 1 d . .
H11A H 0.8186 0.5618 0.1181 0.053 Uiso 1 1 calc R U
H11B H 0.8040 0.4983 0.0279 0.053 Uiso 1 1 calc R U
O12 O 1.1674(4) 0.0376(5) 0.5379(3) 0.0370(12) Uani 1 1 d . .
N12 N 0.5434(6) 0.4306(6) 0.2602(4) 0.0415(15) Uani 1 1 d . .
C12 C 0.6425(8) 0.4422(8) 0.0541(6) 0.048(2) Uani 1 1 d . .
H12A H 0.6245 0.4312 0.1049 0.057 Uiso 1 1 calc R U
H12B H 0.6098 0.3683 0.0147 0.057 Uiso 1 1 calc R U
O13 O 1.0286(7) 0.0949(6) 0.1867(4) 0.0593(17) Uani 1 1 d . .
N13 N 0.4600(6) 0.2517(6) 0.1846(4) 0.0403(15) Uani 1 1 d . .
C13 C 0.5712(8) 0.5205(7) 0.0123(6) 0.047(2) Uani 1 1 d . .
H13A H 0.6056 0.5947 0.0516 0.056 Uiso 1 1 calc R U
H13B H 0.5893 0.5308 -0.0386 0.056 Uiso 1 1 calc R U
O14 O 1.0285(4) -0.0663(4) 0.5853(3) 0.0339(11) Uani 1 1 d . .
C14 C 0.5037(7) 0.8700(6) -0.0071(5) 0.0380(17) Uani 1 1 d . .
O15 O 0.3882(5) 0.8484(5) -0.0402(4) 0.0456(14) Uani 1 1 d . .
C15 C 0.5209(8) 0.8986(6) 0.1432(5) 0.0411(18) Uani 1 1 d . .
H15A H 0.4325 0.8978 0.1170 0.049 Uiso 1 1 calc R U
H15B H 0.5684 0.9696 0.1859 0.049 Uiso 1 1 calc R U
O19 O 0.8399(6) 0.6577(5) 0.2670(4) 0.0517(15) Uani 1 1 d . .
C19 C 0.1630(8) 0.1957(9) 0.0536(6) 0.054(2) Uani 1 1 d . .
H19A H 0.1393 0.1302 0.0773 0.064 Uiso 1 1 calc R U
H19B H 0.0858 0.2158 0.0273 0.064 Uiso 1 1 calc R U
O18 O 0.9080(6) 0.7612(5) 0.1140(4) 0.0547(16) Uani 1 1 d . .
C18 C 0.2405(9) 0.3953(8) 0.1347(6) 0.049(2) Uani 1 1 d . .
O17 O 0.3053(5) 0.7087(5) 0.1213(3) 0.0432(13) Uani 1 1 d . .
C17 C 0.3417(10) 0.5746(8) 0.2494(6) 0.054(2) Uani 1 1 d . .
H17A H 0.2583 0.5852 0.2245 0.065 Uiso 1 1 calc R U
H17B H 0.3614 0.5814 0.3103 0.065 Uiso 1 1 calc R U
O16 O 0.1576(6) 0.4263(6) 0.0855(4) 0.0590(17) Uani 1 1 d . .
C16 C 0.4110(7) 0.7237(7) 0.1760(4) 0.0350(16) Uani 1 1 d . .
O20 O 0.6778(5) 0.3372(5) 0.2310(4) 0.0447(13) Uani 1 1 d . .
C21 C 0.7126(7) 0.9365(6) 0.0983(5) 0.0411(18) Uani 1 1 d . .
H21 H 0.7500 1.0171 0.1281 0.049 Uiso 1 1 calc R U
C22 C 0.6266(8) 0.8123(7) 0.2666(5) 0.044(2) Uani 1 1 d . .
H22 H 0.6468 0.8826 0.3085 0.053 Uiso 1 1 calc R U
C23 C 0.5694(8) 0.7060(7) 0.2955(5) 0.0418(19) Uani 1 1 d . .
H23 H 0.5775 0.7253 0.3552 0.050 Uiso 1 1 calc R U
C24 C 0.4114(8) 0.3968(8) 0.2559(5) 0.0445(19) Uani 1 1 d . .
H24 H 0.4084 0.3960 0.3128 0.053 Uiso 1 1 calc R U
C25 C 0.3516(8) 0.2767(7) 0.1977(5) 0.046(2) Uani 1 1 d . .
H25 H 0.3120 0.2217 0.2253 0.055 Uiso 1 1 calc R U
C26 C 0.8342(7) 0.8161(7) 0.0914(6) 0.0441(19) Uani 1 1 d . .
C27 C 0.8277(7) 0.8770(7) 0.2330(5) 0.0429(19) Uani 1 1 d . .
H27A H 0.9111 0.8651 0.2529 0.051 Uiso 1 1 calc R U
H27B H 0.8386 0.9537 0.2611 0.051 Uiso 1 1 calc R U
C28 C 0.7506(8) 0.6925(7) 0.2693(5) 0.0413(19) Uani 1 1 d . .
C29 C 0.6439(8) 0.5322(7) 0.3181(5) 0.0444(19) Uani 1 1 d . .
H29A H 0.6313 0.5441 0.3718 0.053 Uiso 1 1 calc R U
H29B H 0.7267 0.5199 0.3300 0.053 Uiso 1 1 calc R U
C30 C 0.5730(8) 0.3411(7) 0.2272(5) 0.0405(18) Uani 1 1 d . .
C31 C 0.4553(8) 0.1432(6) 0.1423(5) 0.0422(19) Uani 1 1 d . .
H31A H 0.3973 0.0840 0.1559 0.051 Uiso 1 1 calc R U
H31B H 0.5404 0.1351 0.1650 0.051 Uiso 1 1 calc R U
C20 C 0.7192(7) 0.9174(7) 0.0078(5) 0.0418(19) Uani 1 1 d . .
H20 H 0.7652 0.9887 -0.0025 0.050 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 O3 178.5(3) . .
O2 U1 O009 87.6(3) . 2_966
O3 U1 O009 91.1(3) . 2_966
O2 U1 O1 90.4(3) . .
O3 U1 O1 91.0(3) . .
O009 U1 O1 140.4(2) 2_966 .
O2 U1 O6 92.8(3) . .
O3 U1 O6 87.7(3) . .
O009 U1 O6 141.35(16) 2_966 .
O1 U1 O6 78.3(2) . .
O2 U1 O4 91.4(3) . .
O3 U1 O4 88.8(3) . .
O009 U1 O4 66.79(17) 2_966 .
O1 U1 O4 73.7(2) . .
O6 U1 O4 151.68(17) . .
O2 U1 O5 92.5(3) . .
O3 U1 O5 86.4(3) . .
O009 U1 O5 74.44(16) 2_966 .
O1 U1 O5 145.2(2) . .
O6 U1 O5 66.92(16) . .
O4 U1 O5 140.82(17) . .
C9 N1 C8 121.6(6) . .
C9 N1 C11 119.0(6) . .
C8 N1 C11 119.4(7) . .
O009 C1 O4 128.3(6) . .
O009 C1 C1 115.8(8) . 2_966
O4 C1 C1 115.9(8) . 2_966
U1 O1 H1A 111.9 . .
U1 O1 H1B 111.4 . .
H1A O1 H1B 106.9 . .
O8 C3 O5 126.3(7) . .
O8 C3 C2 116.3(6) . .
O5 C3 C2 117.3(6) . .
C14 N3 C15 123.4(6) . .
C14 N3 C21 112.9(7) . .
C15 N3 C21 122.9(7) . .
O10 U2 O9 179.0(3) . .
O10 U2 O11 93.3(2) . .
O9 U2 O11 87.6(2) . .
O10 U2 O8 90.7(2) . .
O9 U2 O8 89.2(3) . .
O11 U2 O8 78.46(19) . .
O10 U2 O14 87.6(2) . 2_756
O9 U2 O14 92.8(2) . 2_756
O11 U2 O14 79.08(18) . 2_756
O8 U2 O14 157.33(16) . 2_756
O10 U2 O12 91.5(2) . .
O9 U2 O12 87.8(2) . .
O11 U2 O12 144.87(18) . .
O8 U2 O12 136.27(16) . .
O14 U2 O12 66.39(15) 2_756 .
O10 U2 O7 91.6(2) . .
O9 U2 O7 87.5(2) . .
O11 U2 O7 143.90(18) . .
O8 U2 O7 65.74(16) . .
O14 U2 O7 136.89(15) 2_756 .
O12 U2 O7 70.54(16) . .
C14 N2 C31 123.7(6) . 2_665
C14 N2 C20 111.9(7) . .
C31 N2 C20 123.9(7) 2_665 .
O7 C2 O6 126.2(7) . .
O7 C2 C3 116.9(6) . .
O6 C2 C3 116.9(6) . .
C1 O4 U1 120.1(4) . .
C16 N4 C15 120.9(6) . .
C16 N4 C22 111.0(6) . .
C15 N4 C22 122.6(6) . .
O14 C4 O12 126.4(6) . .
O14 C4 C4 116.4(7) . 2_756
O12 C4 C4 117.2(7) . 2_756
C3 O5 U1 118.6(4) . .
C16 N5 C17 124.7(7) . .
C16 N5 C23 111.9(7) . .
C17 N5 C23 123.3(7) . .
O13 C5 O11 126.6(7) . .
O13 C5 C6 118.2(7) . .
O11 C5 C6 115.2(7) . .
C2 O6 U1 119.3(4) . .
C18 N6 C24 112.0(7) . .
C18 N6 C17 124.4(7) . .
C24 N6 C17 123.3(7) . .
C7 C6 C10 119.6(6) . .
C7 C6 C5 120.9(6) . .
C10 C6 C5 119.5(6) . .
C2 O7 U2 119.7(4) . .
C18 N7 C19 122.8(7) . .
C18 N7 C25 111.7(8) . .
C19 N7 C25 123.5(7) . .
C6 C7 C8 119.0(7) . .
C6 C7 H7 120.5 . .
C8 C7 H7 120.5 . .
C1 O009 U1 121.3(4) . 2_966
C26 N9 C27 122.8(6) . .
C26 N9 C21 111.6(7) . .
C27 N9 C21 123.6(7) . .
N1 C9 C10 120.9(6) . .
N1 C9 H9 119.6 . .
C10 C9 H9 119.6 . .
C3 O8 U2 120.5(4) . .
C26 N8 C19 122.7(7) . 2_665
C26 N8 C20 111.9(7) . .
C19 N8 C20 123.4(7) 2_665 .
N1 C8 C7 119.9(7) . .
N1 C8 H8 120.0 . .
C7 C8 H8 120.0 . .
C28 N10 C27 124.0(7) . .
C28 N10 C22 111.4(8) . .
C27 N10 C22 124.4(7) . .
C9 C10 C6 118.9(7) . .
C9 C10 H10 120.6 . .
C6 C10 H10 120.6 . .
C5 O11 U2 138.4(5) . .
C28 N11 C29 121.8(6) . .
C28 N11 C23 110.9(7) . .
C29 N11 C23 123.5(7) . .
C12 C11 N1 111.9(6) . .
C12 C11 H11A 109.2 . .
N1 C11 H11A 109.2 . .
C12 C11 H11B 109.2 . .
N1 C11 H11B 109.2 . .
H11A C11 H11B 107.9 . .
C4 O12 U2 119.5(4) . .
C30 N12 C29 121.0(7) . .
C30 N12 C24 111.7(7) . .
C29 N12 C24 123.9(7) . .
C11 C12 C13 113.2(7) . .
C11 C12 H12A 108.9 . .
C13 C12 H12A 108.9 . .
C11 C12 H12B 108.9 . .
C13 C12 H12B 108.9 . .
H12A C12 H12B 107.8 . .
C30 N13 C31 123.3(7) . .
C30 N13 C25 111.7(7) . .
C31 N13 C25 124.5(7) . .
C13 C13 C12 115.2(9) 2_665 .
C13 C13 H13A 108.5 2_665 .
C12 C13 H13A 108.5 . .
C13 C13 H13B 108.5 2_665 .
C12 C13 H13B 108.5 . .
H13A C13 H13B 107.5 . .
C4 O14 U2 120.1(4) . 2_756
O15 C14 N3 126.5(8) . .
O15 C14 N2 125.5(8) . .
N3 C14 N2 108.0(6) . .
N3 C15 N4 113.3(6) . .
N3 C15 H15A 108.9 . .
N4 C15 H15A 108.9 . .
N3 C15 H15B 108.9 . .
N4 C15 H15B 108.9 . .
H15A C15 H15B 107.7 . .
N8 C19 N7 113.6(7) 2_665 .
N8 C19 H19A 108.8 2_665 .
N7 C19 H19A 108.8 . .
N8 C19 H19B 108.8 2_665 .
N7 C19 H19B 108.8 . .
H19A C19 H19B 107.7 . .
O16 C18 N7 125.8(9) . .
O16 C18 N6 125.8(9) . .
N7 C18 N6 108.5(7) . .
N5 C17 N6 114.5(7) . .
N5 C17 H17A 108.6 . .
N6 C17 H17A 108.6 . .
N5 C17 H17B 108.6 . .
N6 C17 H17B 108.6 . .
H17A C17 H17B 107.6 . .
O17 C16 N4 125.6(7) . .
O17 C16 N5 125.5(8) . .
N4 C16 N5 109.0(6) . .
N3 C21 N9 114.8(6) . .
N3 C21 C20 102.3(6) . .
N9 C21 C20 103.8(6) . .
N3 C21 H21 111.8 . .
N9 C21 H21 111.8 . .
C20 C21 H21 111.8 . .
N10 C22 N4 114.6(7) . .
N10 C22 C23 104.3(6) . .
N4 C22 C23 102.5(6) . .
N10 C22 H22 111.6 . .
N4 C22 H22 111.6 . .
C23 C22 H22 111.6 . .
N5 C23 N11 115.0(6) . .
N5 C23 C22 104.2(6) . .
N11 C23 C22 103.0(7) . .
N5 C23 H23 111.4 . .
N11 C23 H23 111.4 . .
C22 C23 H23 111.4 . .
N6 C24 N12 115.3(7) . .
N6 C24 C25 103.8(7) . .
N12 C24 C25 103.5(6) . .
N6 C24 H24 111.2 . .
N12 C24 H24 111.2 . .
C25 C24 H24 111.2 . .
N13 C25 N7 115.6(7) . .
N13 C25 C24 103.6(7) . .
N7 C25 C24 103.4(6) . .
N13 C25 H25 111.2 . .
N7 C25 H25 111.2 . .
C24 C25 H25 111.2 . .
O18 C26 N8 124.9(9) . .
O18 C26 N9 125.8(8) . .
N8 C26 N9 109.3(7) . .
N10 C27 N9 113.2(6) . .
N10 C27 H27A 108.9 . .
N9 C27 H27A 108.9 . .
N10 C27 H27B 108.9 . .
N9 C27 H27B 108.9 . .
H27A C27 H27B 107.7 . .
O19 C28 N10 125.3(9) . .
O19 C28 N11 125.4(7) . .
N10 C28 N11 109.3(7) . .
N11 C29 N12 113.6(6) . .
N11 C29 H29A 108.8 . .
N12 C29 H29A 108.9 . .
N11 C29 H29B 108.8 . .
N12 C29 H29B 108.8 . .
H29A C29 H29B 107.7 . .
O20 C30 N12 127.9(8) . .
O20 C30 N13 123.9(8) . .
N12 C30 N13 108.2(7) . .
N13 C31 N2 115.0(6) . 2_665
N13 C31 H31A 108.5 . .
N2 C31 H31A 108.5 2_665 .
N13 C31 H31B 108.5 . .
N2 C31 H31B 108.5 2_665 .
H31A C31 H31B 107.5 . .
N2 C20 N8 115.7(7) . .
N2 C20 C21 104.1(6) . .
N8 C20 C21 102.8(6) . .
N2 C20 H20 111.2 . .
N8 C20 H20 111.2 . .
C21 C20 H20 111.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.738(7) .
U1 O3 1.764(6) .
U1 O009 2.379(5) 2_966
U1 O1 2.384(6) .
U1 O6 2.414(5) .
U1 O4 2.414(5) .
U1 O5 2.425(5) .
N1 C9 1.325(10) .
N1 C8 1.347(10) .
N1 C11 1.508(8) .
C1 O009 1.248(9) .
C1 O4 1.244(9) .
C1 C1 1.552(13) 2_966
O1 H1A 0.8993 .
O1 H1B 0.8980 .
C3 O8 1.249(8) .
C3 O5 1.250(8) .
C3 C2 1.531(9) .
N3 C14 1.366(10) .
N3 C15 1.437(11) .
N3 C21 1.446(9) .
U2 O10 1.754(5) .
U2 O9 1.768(6) .
U2 O11 2.307(5) .
U2 O8 2.426(5) .
U2 O14 2.436(5) 2_756
U2 O12 2.438(5) .
U2 O7 2.448(5) .
N2 C14 1.373(11) .
N2 C31 1.449(10) 2_665
N2 C20 1.441(9) .
C2 O7 1.237(8) .
C2 O6 1.245(8) .
N4 C16 1.364(10) .
N4 C15 1.455(9) .
N4 C22 1.470(9) .
C4 O14 1.248(8) .
C4 O12 1.248(8) .
C4 C4 1.543(13) 2_756
N5 C16 1.366(9) .
N5 C17 1.427(11) .
N5 C23 1.439(11) .
C5 O13 1.230(9) .
C5 O11 1.274(9) .
C5 C6 1.515(9) .
N6 C18 1.372(12) .
N6 C24 1.441(10) .
N6 C17 1.451(11) .
C6 C7 1.378(10) .
C6 C10 1.389(9) .
N7 C18 1.363(11) .
N7 C19 1.446(12) .
N7 C25 1.454(10) .
C7 C8 1.389(10) .
C7 H7 0.9300 .
O009 U1 2.379(5) 2_966
N9 C26 1.362(11) .
N9 C27 1.442(10) .
N9 C21 1.445(9) .
C9 C10 1.379(10) .
C9 H9 0.9300 .
N8 C26 1.362(11) .
N8 C19 1.443(11) 2_665
N8 C20 1.452(10) .
C8 H8 0.9300 .
N10 C28 1.368(10) .
N10 C27 1.433(11) .
N10 C22 1.435(10) .
C10 H10 0.9300 .
N11 C28 1.367(11) .
N11 C29 1.441(10) .
N11 C23 1.459(9) .
C11 C12 1.499(12) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
N12 C30 1.357(10) .
N12 C29 1.452(11) .
N12 C24 1.453(11) .
C12 C13 1.527(10) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
N13 C30 1.381(10) .
N13 C31 1.429(10) .
N13 C25 1.447(10) .
C13 C13 1.491(16) 2_665
C13 H13A 0.9700 .
C13 H13B 0.9700 .
O14 U2 2.436(5) 2_756
C14 O15 1.209(9) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
O19 C28 1.229(9) .
C19 N8 1.443(11) 2_665
C19 H19A 0.9700 .
C19 H19B 0.9700 .
O18 C26 1.222(9) .
C18 O16 1.229(10) .
O17 C16 1.220(9) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
O20 C30 1.208(10) .
C21 C20 1.556(12) .
C21 H21 0.9800 .
C22 C23 1.537(12) .
C22 H22 0.9800 .
C23 H23 0.9800 .
C24 C25 1.532(12) .
C24 H24 0.9800 .
C25 H25 0.9800 .
C27 H27A 0.9700 .
C27 H27B 0.9700 .
C29 H29A 0.9700 .
C29 H29B 0.9700 .
C31 N2 1.449(10) 2_665
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C20 H20 0.9800 .
