#------------------------------------------------------------------------------
#$Date: 2016-03-05 11:13:25 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177763 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/40/7224008.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_7224008
loop_
_publ_author_name
'Thuéry, Pierre'
'Harrowfield, Jack'
_publ_section_title
;
 Counter-ion control of structure in uranyl ion complexes with
 2,5-thiophenedicarboxylate
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1550
_journal_paper_doi               10.1039/C5CE02294K
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C53 H42 N8 Ni O21 S3 U2'
_chemical_formula_weight         1757.89
_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
_audit_update_record
;
2015-11-19 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                108.577(2)
_cell_angle_beta                 110.263(3)
_cell_angle_gamma                97.592(3)
_cell_formula_units_Z            2
_cell_length_a                   13.8935(5)
_cell_length_b                   14.0662(8)
_cell_length_c                   18.2195(11)
_cell_measurement_reflns_used    171362
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.21
_cell_volume                     3046.3(3)
_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 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'2 φ and 13 ω scans with 2° steps (750 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  0.0566
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            171362
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.212
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.793
_exptl_absorpt_correction_T_max  0.629
_exptl_absorpt_correction_T_min  0.388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.736
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         11564
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0403P)²+2.8650P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9122
_reflns_number_total             11564
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce02294k1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7224008--7224013.cif.'
_cod_database_code               7224008
_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
_atom_site_refinement_flags_occupancy
U1 U 0.22104(2) 0.55626(2) 0.87835(2) 0.03614(8) Uani 1 1 d . . .
U2 U 0.78269(2) 0.75827(2) 0.63696(2) 0.03285(7) Uani 1 1 d . . .
Ni1 Ni 0.38940(5) 0.96618(5) 0.70344(5) 0.02920(16) Uani 1 1 d . . .
S1 S 0.49351(11) 0.66012(10) 0.74858(9) 0.0347(3) Uani 1 1 d . . .
S2 S 0.00119(12) 0.16101(11) 0.75893(10) 0.0395(4) Uani 1 1 d . . .
S3 S 1.02042(12) 0.71014(12) 0.46463(11) 0.0401(4) Uani 1 1 d . . .
O1 O 0.1229(3) 0.6022(3) 0.8199(3) 0.0442(10) Uani 1 1 d . . .
O2 O 0.3227(4) 0.5174(3) 0.9425(3) 0.0457(11) Uani 1 1 d . . .
O3 O 0.6934(3) 0.7738(3) 0.5479(3) 0.0404(10) Uani 1 1 d . . .
O4 O 0.8730(3) 0.7425(3) 0.7253(3) 0.0390(9) Uani 1 1 d . . .
O5 O 0.3529(3) 0.6386(3) 0.8400(3) 0.0408(10) Uani 1 1 d . . .
O6 O 0.2638(3) 0.4751(3) 0.7578(3) 0.0406(10) Uani 1 1 d . . .
O7 O 0.6447(3) 0.5985(3) 0.6005(3) 0.0378(9) Uani 1 1 d . . .
O8 O 0.6470(3) 0.7452(3) 0.6936(3) 0.0425(10) Uani 1 1 d . . .
O9 O 0.1226(3) 0.3743(3) 0.7977(3) 0.0469(11) Uani 1 1 d . . .
O10 O 0.0858(4) 0.4575(3) 0.9047(3) 0.0546(13) Uani 1 1 d . . .
O11 O -0.2151(3) -0.0702(3) 0.7359(3) 0.0444(10) Uani 1 1 d . . .
O12 O -0.0990(3) -0.0686(3) 0.6791(3) 0.0395(10) Uani 1 1 d . . .
O13 O 0.9153(3) 0.7584(3) 0.5774(3) 0.0404(10) Uani 1 1 d . . .
O14 O 0.8097(3) 0.6033(3) 0.5373(3) 0.0360(9) Uani 1 1 d . . .
O15 O 1.1297(4) 0.5614(3) 0.3052(3) 0.0555(13) Uani 1 1 d . . .
H15 H 1.1798 0.5802 0.2828 0.067 Uiso 1 1 d R U .
O16 O 1.1648(3) 0.7325(3) 0.3790(3) 0.0459(11) Uani 1 1 d . . .
O17 O 0.2058(4) 0.6588(4) 1.0138(3) 0.0570(13) Uani 1 1 d . . .
O18 O 0.3173(3) 0.7398(3) 0.9811(3) 0.0399(10) Uani 1 1 d . . .
O19 O 0.3079(4) 0.8143(4) 1.1023(3) 0.0698(16) Uani 1 1 d . . .
O20 O 1.2777(5) 0.5955(4) 0.2529(4) 0.0801(19) Uani 1 1 d . . .
O21 O 0.9906(12) 0.1365(12) 0.0395(13) 0.084(6) Uani 0.3333 1 d . . P
O22 O 0.9734(9) 0.0297(12) 0.0229(8) 0.052(4) Uani 0.3333 1 d . . P
O23 O 0.9232(8) -0.0346(12) 0.0535(7) 0.044(3) Uani 0.3333 1 d . U P
N1 N 0.2778(4) 0.7411(4) 1.0354(4) 0.0486(14) Uani 1 1 d . . .
N2 N 0.2908(4) 0.9031(4) 0.7489(3) 0.0344(11) Uani 1 1 d . . .
N3 N 0.4979(3) 0.9347(3) 0.7986(3) 0.0313(10) Uani 1 1 d . . .
N4 N 0.3796(4) 0.8284(3) 0.6119(3) 0.0332(11) Uani 1 1 d . . .
N5 N 0.4992(4) 1.0179(4) 0.6624(3) 0.0331(11) Uani 1 1 d . . .
N6 N 0.2724(4) 1.0074(4) 0.6213(3) 0.0356(11) Uani 1 1 d . . .
N7 N 0.3940(4) 1.1136(4) 0.7849(3) 0.0352(11) Uani 1 1 d . . .
N8 N 1.3305(6) 0.4971(6) 0.1524(5) 0.1034(15) Uani 1 1 d D U .
C1 C 0.3332(4) 0.5567(5) 0.7764(4) 0.0353(13) Uani 1 1 d . . .
C2 C 0.3939(4) 0.5528(4) 0.7225(4) 0.0325(12) Uani 1 1 d . . .
C3 C 0.3833(4) 0.4709(4) 0.6528(4) 0.0348(13) Uani 1 1 d . . .
H3 H 0.3318 0.4056 0.6291 0.042 Uiso 1 1 calc R U .
C4 C 0.4570(4) 0.4940(4) 0.6199(4) 0.0328(13) Uani 1 1 d . . .
H4 H 0.4606 0.4460 0.5712 0.039 Uiso 1 1 calc R U .
C5 C 0.5228(4) 0.5926(4) 0.6655(4) 0.0305(12) Uani 1 1 d . . .
C6 C 0.6083(5) 0.6481(5) 0.6519(4) 0.0372(14) Uani 1 1 d . . .
C7 C 0.0724(5) 0.3748(5) 0.8447(4) 0.0433(16) Uani 1 1 d . . .
C8 C -0.0004(5) 0.2762(5) 0.8281(4) 0.0435(15) Uani 1 1 d . . .
C9 C -0.0728(5) 0.2632(5) 0.8604(5) 0.0502(18) Uani 1 1 d . . .
H9 H -0.0838 0.3188 0.9000 0.060 Uiso 1 1 calc R U .
C10 C -0.1303(5) 0.1576(5) 0.8288(5) 0.0501(17) Uani 1 1 d . . .
H10 H -0.1848 0.1341 0.8442 0.060 Uiso 1 1 calc R U .
C11 C -0.0981(5) 0.0927(4) 0.7729(4) 0.0383(14) Uani 1 1 d . . .
C12 C -0.1397(4) -0.0211(4) 0.7274(4) 0.0361(13) Uani 1 1 d . . .
C13 C 0.8819(4) 0.6616(5) 0.5322(4) 0.0365(13) Uani 1 1 d . . .
C14 C 0.9312(4) 0.6208(4) 0.4723(4) 0.0346(13) Uani 1 1 d . . .
C15 C 0.9193(5) 0.5212(5) 0.4219(4) 0.0409(14) Uani 1 1 d . . .
H15A H 0.8726 0.4618 0.4174 0.049 Uiso 1 1 calc R U .
C16 C 0.9861(5) 0.5162(5) 0.3759(4) 0.0400(14) Uani 1 1 d . . .
H16 H 0.9896 0.4532 0.3384 0.048 Uiso 1 1 calc R U .
C17 C 1.0431(5) 0.6125(5) 0.3928(4) 0.0366(13) Uani 1 1 d . . .
C18 C 1.1189(5) 0.6429(5) 0.3585(4) 0.0407(14) Uani 1 1 d . . .
C19 C 0.1841(5) 0.8880(5) 0.7191(4) 0.0440(15) Uani 1 1 d . . .
H19 H 0.1482 0.8976 0.6682 0.053 Uiso 1 1 calc R U .
C20 C 0.1257(5) 0.8594(6) 0.7596(5) 0.060(2) Uani 1 1 d . . .
H20 H 0.0506 0.8489 0.7373 0.072 Uiso 1 1 calc R U .
C21 C 0.1789(6) 0.8464(7) 0.8333(6) 0.076(3) Uani 1 1 d . . .
H21 H 0.1399 0.8250 0.8617 0.092 Uiso 1 1 calc R U .
C22 C 0.2879(6) 0.8642(6) 0.8666(5) 0.0565(19) Uani 1 1 d . . .
H22 H 0.3254 0.8585 0.9189 0.068 Uiso 1 1 calc R U .
C23 C 0.3417(5) 0.8907(4) 0.8210(4) 0.0345(13) Uani 1 1 d . . .
C24 C 0.4577(5) 0.9049(4) 0.8479(4) 0.0337(13) Uani 1 1 d . . .
C25 C 0.5224(5) 0.8880(5) 0.9182(4) 0.0441(15) Uani 1 1 d . . .
H25 H 0.4930 0.8688 0.9530 0.053 Uiso 1 1 calc R U .
C26 C 0.6297(5) 0.8996(5) 0.9363(4) 0.0477(16) Uani 1 1 d . . .
H26 H 0.6754 0.8896 0.9843 0.057 Uiso 1 1 calc R U .
C27 C 0.6682(5) 0.9254(5) 0.8841(4) 0.0467(16) Uani 1 1 d . . .
H27 H 0.7410 0.9315 0.8942 0.056 Uiso 1 1 calc R U .
C28 C 0.6015(4) 0.9430(4) 0.8164(4) 0.0376(14) Uani 1 1 d . . .
H28 H 0.6302 0.9616 0.7809 0.045 Uiso 1 1 calc R U .
C29 C 0.3171(5) 0.7341(4) 0.5889(4) 0.0390(14) Uani 1 1 d . . .
H29 H 0.2724 0.7275 0.6174 0.047 Uiso 1 1 calc R U .
C30 C 0.3138(5) 0.6452(5) 0.5257(4) 0.0405(14) Uani 1 1 d . . .
H30 H 0.2687 0.5793 0.5118 0.049 Uiso 1 1 calc R U .
C31 C 0.3766(5) 0.6546(5) 0.4843(4) 0.0466(16) Uani 1 1 d . . .
H31 H 0.3747 0.5952 0.4399 0.056 Uiso 1 1 calc R U .
C32 C 0.4438(5) 0.7511(5) 0.5067(4) 0.0404(14) Uani 1 1 d . . .
H32 H 0.4884 0.7582 0.4782 0.048 Uiso 1 1 calc R U .
C33 C 0.4447(4) 0.8375(4) 0.5718(4) 0.0326(12) Uani 1 1 d . . .
C34 C 0.5144(4) 0.9434(4) 0.6020(4) 0.0313(12) Uani 1 1 d . . .
C35 C 0.5909(5) 0.9681(5) 0.5737(4) 0.0410(15) Uani 1 1 d . . .
H35 H 0.6016 0.9151 0.5320 0.049 Uiso 1 1 calc R U .
C36 C 0.6519(5) 1.0701(5) 0.6062(4) 0.0433(15) Uani 1 1 d . . .
H36 H 0.7051 1.0875 0.5874 0.052 Uiso 1 1 calc R U .
C37 C 0.6346(5) 1.1453(5) 0.6655(4) 0.0448(16) Uani 1 1 d . . .
H37 H 0.6742 1.2161 0.6875 0.054 Uiso 1 1 calc R U .
C38 C 0.5584(5) 1.1168(5) 0.6929(4) 0.0413(14) Uani 1 1 d . . .
H38 H 0.5474 1.1692 0.7349 0.050 Uiso 1 1 calc R U .
C39 C 0.2151(5) 0.9511(5) 0.5394(4) 0.0393(14) Uani 1 1 d . . .
H39 H 0.2223 0.8830 0.5160 0.047 Uiso 1 1 calc R U .
C40 C 0.1448(5) 0.9867(5) 0.4856(4) 0.0450(15) Uani 1 1 d . . .
H40 H 0.1057 0.9443 0.4268 0.054 Uiso 1 1 calc R U .
C41 C 0.1334(5) 1.0846(6) 0.5199(5) 0.0513(17) Uani 1 1 d . . .
H41 H 0.0878 1.1120 0.4847 0.062 Uiso 1 1 calc R U .
C42 C 0.1894(5) 1.1428(5) 0.6065(5) 0.0496(17) Uani 1 1 d . . .
H42 H 0.1794 1.2090 0.6318 0.060 Uiso 1 1 calc R U .
C43 C 0.2596(5) 1.1039(5) 0.6558(4) 0.0389(14) Uani 1 1 d . . .
C44 C 0.3233(5) 1.1596(5) 0.7480(4) 0.0379(14) Uani 1 1 d . . .
C45 C 0.3103(5) 1.2524(5) 0.7958(5) 0.0493(17) Uani 1 1 d . . .
H45 H 0.2603 1.2841 0.7693 0.059 Uiso 1 1 calc R U .
C46 C 0.3718(6) 1.2977(5) 0.8830(5) 0.0551(18) Uani 1 1 d . . .
H46 H 0.3635 1.3604 0.9169 0.066 Uiso 1 1 calc R U .
C47 C 0.4446(5) 1.2513(5) 0.9200(4) 0.0465(16) Uani 1 1 d . . .
H47 H 0.4882 1.2824 0.9793 0.056 Uiso 1 1 calc R U .
C48 C 0.4536(5) 1.1594(4) 0.8701(4) 0.0379(14) Uani 1 1 d . . .
H48 H 0.5032 1.1269 0.8961 0.045 Uiso 1 1 calc R U .
C49 C 1.2635(8) 0.5131(7) 0.1914(6) 0.1029(17) Uani 1 1 d D U .
C50 C 1.1731(8) 0.4121(7) 0.1490(7) 0.1104(18) Uani 1 1 d D U .
H50A H 1.1058 0.4220 0.1140 0.132 Uiso 1 1 calc R U .
H50B H 1.1618 0.3897 0.1924 0.132 Uiso 1 1 calc R U .
C51 C 1.2095(8) 0.3302(6) 0.0926(7) 0.1120(18) Uani 1 1 d D U .
H51A H 1.1499 0.2869 0.0368 0.134 Uiso 1 1 calc R U .
H51B H 1.2385 0.2844 0.1208 0.134 Uiso 1 1 calc R U .
C52 C 1.2978(8) 0.3986(7) 0.0825(6) 0.1028(17) Uani 1 1 d D U .
H52A H 1.3582 0.3675 0.0856 0.123 Uiso 1 1 calc R U .
H52B H 1.2691 0.4065 0.0275 0.123 Uiso 1 1 calc R U .
C53 C 1.4112(8) 0.5828(7) 0.1704(6) 0.0980(18) Uani 1 1 d D U .
H53A H 1.3794 0.6306 0.1469 0.147 Uiso 1 1 calc R U .
H53B H 1.4595 0.5589 0.1448 0.147 Uiso 1 1 calc R U .
H53C H 1.4511 0.6190 0.2321 0.147 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'
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'
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
O1 U1 O2 176.51(19) . .
O1 U1 O9 94.51(18) . .
O2 U1 O9 88.68(18) . .
O1 U1 O6 92.89(17) . .
O2 U1 O6 89.65(16) . .
O9 U1 O6 67.48(13) . .
O1 U1 O5 90.92(17) . .
O2 U1 O5 88.67(17) . .
O9 U1 O5 120.76(13) . .
O6 U1 O5 53.33(13) . .
O1 U1 O10 89.67(18) . .
O2 U1 O10 91.08(18) . .
O9 U1 O10 53.47(13) . .
O6 U1 O10 120.91(14) . .
O5 U1 O10 174.22(14) . .
O1 U1 O18 89.10(17) . .
O2 U1 O18 87.54(17) . .
O9 U1 O18 170.64(13) . .
O6 U1 O18 121.02(13) . .
O5 U1 O18 67.72(13) . .
O10 U1 O18 118.04(13) . .
O1 U1 O17 90.82(18) . .
O2 U1 O17 86.33(18) . .
O9 U1 O17 120.29(14) . .
O6 U1 O17 171.09(14) . .
O5 U1 O17 118.55(14) . .
O10 U1 O17 67.18(14) . .
O18 U1 O17 50.91(14) . .
O4 U2 O3 179.27(17) . .
O4 U2 O13 90.17(16) . .
O3 U2 O13 89.10(16) . .
O4 U2 O8 88.95(16) . .
O3 U2 O8 91.76(16) . .
O13 U2 O8 176.09(12) . .
O4 U2 O12 90.56(16) . 1_665
O3 U2 O12 89.22(17) . 1_665
O13 U2 O12 64.69(13) . 1_665
O8 U2 O12 119.12(12) . 1_665
O4 U2 O7 92.55(16) . .
O3 U2 O7 87.77(17) . .
O13 U2 O7 123.37(12) . .
O8 U2 O7 52.88(12) . .
O12 U2 O7 171.32(12) 1_665 .
O4 U2 O11 88.79(17) . 1_665
O3 U2 O11 91.64(17) . 1_665
O13 U2 O11 117.20(13) . 1_665
O8 U2 O11 66.59(13) . 1_665
O12 U2 O11 52.54(12) 1_665 1_665
O7 U2 O11 119.40(12) . 1_665
O4 U2 O14 90.34(16) . .
O3 U2 O14 89.14(16) . .
O13 U2 O14 52.63(12) . .
O8 U2 O14 123.57(12) . .
O12 U2 O14 117.32(12) 1_665 .
O7 U2 O14 70.79(11) . .
O11 U2 O14 169.80(12) 1_665 .
N4 Ni1 N5 79.09(18) . .
N4 Ni1 N2 97.49(18) . .
N5 Ni1 N2 173.07(17) . .
N4 Ni1 N3 90.98(17) . .
N5 Ni1 N3 95.42(17) . .
N2 Ni1 N3 78.53(18) . .
N4 Ni1 N6 95.84(18) . .
N5 Ni1 N6 90.64(18) . .
N2 Ni1 N6 95.73(18) . .
N3 Ni1 N6 171.63(17) . .
N4 Ni1 N7 172.99(18) . .
N5 Ni1 N7 97.23(18) . .
N2 Ni1 N7 86.78(18) . .
N3 Ni1 N7 95.32(18) . .
N6 Ni1 N7 78.15(19) . .
C2 S1 C5 90.7(3) . .
C11 S2 C8 91.1(3) . .
C14 S3 C17 91.2(3) . .
C1 O5 U1 92.5(3) . .
C1 O6 U1 93.0(3) . .
C6 O7 U2 92.4(3) . .
C6 O8 U2 94.2(3) . .
C7 O9 U1 93.6(4) . .
C7 O10 U1 92.5(3) . .
C12 O11 U2 92.7(3) . 1_445
C12 O12 U2 93.9(3) . 1_445
C13 O13 U2 94.6(3) . .
C13 O14 U2 91.0(3) . .
C18 O15 H15 112.5 . .
N1 O17 U1 96.2(3) . .
N1 O18 U1 97.5(3) . .
O19 N1 O17 122.6(5) . .
O19 N1 O18 122.3(5) . .
O17 N1 O18 115.1(5) . .
C23 N2 C19 119.0(5) . .
C23 N2 Ni1 114.8(4) . .
C19 N2 Ni1 125.6(4) . .
C28 N3 C24 117.9(5) . .
C28 N3 Ni1 127.3(4) . .
C24 N3 Ni1 114.8(3) . .
C29 N4 C33 118.1(5) . .
C29 N4 Ni1 126.9(4) . .
C33 N4 Ni1 115.0(4) . .
C38 N5 C34 118.7(5) . .
C38 N5 Ni1 125.5(4) . .
C34 N5 Ni1 115.8(4) . .
C39 N6 C43 118.5(5) . .
C39 N6 Ni1 125.6(4) . .
C43 N6 Ni1 115.7(4) . .
C44 N7 C48 119.0(5) . .
C44 N7 Ni1 115.0(4) . .
C48 N7 Ni1 125.7(4) . .
C53 N8 C49 118.1(8) . .
C53 N8 C52 124.6(8) . .
C49 N8 C52 115.8(7) . .
O5 C1 O6 121.2(5) . .
O5 C1 C2 120.7(5) . .
O6 C1 C2 118.1(5) . .
C3 C2 C1 128.0(5) . .
C3 C2 S1 112.3(4) . .
C1 C2 S1 119.7(4) . .
C2 C3 C4 112.4(5) . .
C2 C3 H3 123.8 . .
C4 C3 H3 123.8 . .
C5 C4 C3 112.6(5) . .
C5 C4 H4 123.7 . .
C3 C4 H4 123.7 . .
C4 C5 C6 130.1(5) . .
C4 C5 S1 112.0(4) . .
C6 C5 S1 117.9(4) . .
O8 C6 O7 120.5(5) . .
O8 C6 C5 118.9(5) . .
O7 C6 C5 120.5(5) . .
O10 C7 O9 120.4(5) . .
O10 C7 C8 120.6(5) . .
O9 C7 C8 119.0(5) . .
C9 C8 C7 128.0(5) . .
C9 C8 S2 112.7(5) . .
C7 C8 S2 119.3(4) . .
C8 C9 C10 112.4(5) . .
C8 C9 H9 123.8 . .
C10 C9 H9 123.8 . .
C11 C10 C9 112.1(5) . .
C11 C10 H10 123.9 . .
C9 C10 H10 123.9 . .
C10 C11 C12 127.6(5) . .
C10 C11 S2 111.6(4) . .
C12 C11 S2 120.8(4) . .
O11 C12 O12 120.8(5) . .
O11 C12 C11 120.3(5) . .
O12 C12 C11 118.9(5) . .
O14 C13 O13 121.4(5) . .
O14 C13 C14 121.8(5) . .
O13 C13 C14 116.7(5) . .
C15 C14 C13 130.4(5) . .
C15 C14 S3 112.3(4) . .
C13 C14 S3 117.3(4) . .
C14 C15 C16 112.1(5) . .
C14 C15 H15A 123.9 . .
C16 C15 H15A 123.9 . .
C17 C16 C15 111.7(5) . .
C17 C16 H16 124.2 . .
C15 C16 H16 124.2 . .
C16 C17 C18 129.5(5) . .
C16 C17 S3 112.7(4) . .
C18 C17 S3 117.8(5) . .
O16 C18 O15 125.5(5) . .
O16 C18 C17 122.8(5) . .
O15 C18 C17 111.7(5) . .
N2 C19 C20 122.3(6) . .
N2 C19 H19 118.8 . .
C20 C19 H19 118.8 . .
C19 C20 C21 118.1(6) . .
C19 C20 H20 120.9 . .
C21 C20 H20 120.9 . .
C20 C21 C22 120.8(6) . .
C20 C21 H21 119.6 . .
C22 C21 H21 119.6 . .
C21 C22 C23 117.8(7) . .
C21 C22 H22 121.1 . .
C23 C22 H22 121.1 . .
N2 C23 C22 121.9(6) . .
N2 C23 C24 115.7(5) . .
C22 C23 C24 122.4(5) . .
N3 C24 C25 121.6(5) . .
N3 C24 C23 114.8(5) . .
C25 C24 C23 123.6(5) . .
C26 C25 C24 119.2(6) . .
C26 C25 H25 120.4 . .
C24 C25 H25 120.4 . .
C27 C26 C25 118.6(6) . .
C27 C26 H26 120.7 . .
C25 C26 H26 120.7 . .
C26 C27 C28 120.0(6) . .
C26 C27 H27 120.0 . .
C28 C27 H27 120.0 . .
N3 C28 C27 122.6(6) . .
N3 C28 H28 118.7 . .
C27 C28 H28 118.7 . .
N4 C29 C30 123.6(6) . .
N4 C29 H29 118.2 . .
C30 C29 H29 118.2 . .
C31 C30 C29 118.3(6) . .
C31 C30 H30 120.9 . .
C29 C30 H30 120.9 . .
C30 C31 C32 120.1(6) . .
C30 C31 H31 120.0 . .
C32 C31 H31 120.0 . .
C31 C32 C33 118.9(6) . .
C31 C32 H32 120.5 . .
C33 C32 H32 120.5 . .
N4 C33 C32 121.0(5) . .
N4 C33 C34 115.5(5) . .
C32 C33 C34 123.5(5) . .
N5 C34 C35 120.7(5) . .
N5 C34 C33 114.6(5) . .
C35 C34 C33 124.7(5) . .
C34 C35 C36 120.1(6) . .
C34 C35 H35 120.0 . .
C36 C35 H35 120.0 . .
C37 C36 C35 119.1(6) . .
C37 C36 H36 120.5 . .
C35 C36 H36 120.5 . .
C36 C37 C38 119.0(6) . .
C36 C37 H37 120.5 . .
C38 C37 H37 120.5 . .
N5 C38 C37 122.6(6) . .
N5 C38 H38 118.7 . .
C37 C38 H38 118.7 . .
N6 C39 C40 123.2(6) . .
N6 C39 H39 118.4 . .
C40 C39 H39 118.4 . .
C41 C40 C39 118.3(6) . .
C41 C40 H40 120.9 . .
C39 C40 H40 120.9 . .
C40 C41 C42 119.2(6) . .
C40 C41 H41 120.4 . .
C42 C41 H41 120.4 . .
C43 C42 C41 119.5(6) . .
C43 C42 H42 120.3 . .
C41 C42 H42 120.3 . .
N6 C43 C42 121.2(6) . .
N6 C43 C44 115.0(5) . .
C42 C43 C44 123.8(6) . .
N7 C44 C45 121.2(6) . .
N7 C44 C43 115.8(5) . .
C45 C44 C43 122.9(5) . .
C46 C45 C44 118.8(6) . .
C46 C45 H45 120.6 . .
C44 C45 H45 120.6 . .
C47 C46 C45 119.7(6) . .
C47 C46 H46 120.2 . .
C45 C46 H46 120.2 . .
C48 C47 C46 119.2(6) . .
C48 C47 H47 120.4 . .
C46 C47 H47 120.4 . .
N7 C48 C47 122.1(6) . .
N7 C48 H48 119.0 . .
C47 C48 H48 119.0 . .
O20 C49 N8 124.9(8) . .
O20 C49 C50 128.3(8) . .
N8 C49 C50 106.8(6) . .
C49 C50 C51 105.6(6) . .
C49 C50 H50A 110.6 . .
C51 C50 H50A 110.6 . .
C49 C50 H50B 110.6 . .
C51 C50 H50B 110.6 . .
H50A C50 H50B 108.7 . .
C50 C51 C52 103.0(5) . .
C50 C51 H51A 111.2 . .
C52 C51 H51A 111.2 . .
C50 C51 H51B 111.2 . .
C52 C51 H51B 111.2 . .
H51A C51 H51B 109.1 . .
N8 C52 C51 104.3(5) . .
N8 C52 H52A 110.9 . .
C51 C52 H52A 110.9 . .
N8 C52 H52B 110.9 . .
C51 C52 H52B 110.9 . .
H52A C52 H52B 108.9 . .
N8 C53 H53A 109.5 . .
N8 C53 H53B 109.5 . .
H53A C53 H53B 109.5 . .
N8 C53 H53C 109.5 . .
H53A C53 H53C 109.5 . .
H53B C53 H53C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.754(4) .
U1 O2 1.769(4) .
U1 O9 2.422(4) .
U1 O6 2.443(4) .
U1 O5 2.456(4) .
U1 O10 2.459(4) .
U1 O18 2.496(4) .
U1 O17 2.528(4) .
U2 O4 1.765(4) .
U2 O3 1.767(4) .
U2 O13 2.441(3) .
U2 O8 2.456(3) .
U2 O12 2.470(4) 1_665
U2 O7 2.490(4) .
U2 O11 2.499(4) 1_665
U2 O14 2.521(4) .
Ni1 N4 2.067(5) .
Ni1 N5 2.064(4) .
Ni1 N2 2.070(5) .
Ni1 N3 2.080(5) .
Ni1 N6 2.082(5) .
Ni1 N7 2.108(5) .
S1 C2 1.719(5) .
S1 C5 1.724(5) .
S2 C11 1.715(6) .
S2 C8 1.716(6) .
S3 C14 1.720(6) .
S3 C17 1.719(6) .
O5 C1 1.261(7) .
O6 C1 1.263(7) .
O7 C6 1.274(6) .
O8 C6 1.263(7) .
O9 C7 1.277(7) .
O10 C7 1.255(7) .
O11 C12 1.261(7) .
O11 U2 2.499(4) 1_445
O12 C12 1.269(7) .
O12 U2 2.470(4) 1_445
O13 C13 1.265(7) .
O14 C13 1.258(7) .
O15 C18 1.311(7) .
O15 H15 0.9682 .
O16 C18 1.207(7) .
O17 N1 1.276(7) .
O18 N1 1.284(6) .
O19 N1 1.207(7) .
O20 C49 1.264(9) .
N2 C23 1.337(7) .
N2 C19 1.350(7) .
N3 C28 1.341(7) .
N3 C24 1.350(7) .
N4 C29 1.334(7) .
N4 C33 1.360(7) .
N5 C38 1.346(7) .
N5 C34 1.356(7) .
N6 C39 1.321(8) .
N6 C43 1.366(7) .
N7 C44 1.350(7) .
N7 C48 1.357(8) .
N8 C53 1.398(8) .
N8 C49 1.355(8) .
N8 C52 1.434(8) .
C1 C2 1.493(7) .
C2 C3 1.362(8) .
C3 C4 1.405(7) .
C3 H3 0.9500 .
C4 C5 1.362(8) .
C4 H4 0.9500 .
C5 C6 1.470(7) .
C7 C8 1.479(8) .
C8 C9 1.349(8) .
C9 C10 1.414(8) .
C9 H9 0.9500 .
C10 C11 1.379(8) .
C10 H10 0.9500 .
C11 C12 1.470(8) .
C13 C14 1.488(8) .
C14 C15 1.360(8) .
C15 C16 1.444(8) .
C15 H15A 0.9500 .
C16 C17 1.357(8) .
C16 H16 0.9500 .
C17 C18 1.478(8) .
C19 C20 1.372(8) .
C19 H19 0.9500 .
C20 C21 1.374(11) .
C20 H20 0.9500 .
C21 C22 1.375(10) .
C21 H21 0.9500 .
C22 C23 1.393(8) .
C22 H22 0.9500 .
C23 C24 1.478(8) .
C24 C25 1.399(8) .
C25 C26 1.386(9) .
C25 H25 0.9500 .
C26 C27 1.359(9) .
C26 H26 0.9500 .
C27 C28 1.380(9) .
C27 H27 0.9500 .
C28 H28 0.9500 .
C29 C30 1.387(8) .
C29 H29 0.9500 .
C30 C31 1.356(9) .
C30 H30 0.9500 .
C31 C32 1.388(9) .
C31 H31 0.9500 .
C32 C33 1.397(8) .
C32 H32 0.9500 .
C33 C34 1.479(8) .
C34 C35 1.382(7) .
C35 C36 1.385(9) .
C35 H35 0.9500 .
C36 C37 1.365(9) .
C36 H36 0.9500 .
C37 C38 1.383(8) .
C37 H37 0.9500 .
C38 H38 0.9500 .
C39 C40 1.396(8) .
C39 H39 0.9500 .
C40 C41 1.374(9) .
C40 H40 0.9500 .
C41 C42 1.388(10) .
C41 H41 0.9500 .
C42 C43 1.381(8) .
C42 H42 0.9500 .
C43 C44 1.473(9) .
C44 C45 1.393(8) .
C45 C46 1.389(10) .
C45 H45 0.9500 .
C46 C47 1.373(9) .
C46 H46 0.9500 .
C47 C48 1.373(8) .
C47 H47 0.9500 .
C48 H48 0.9500 .
C49 C50 1.533(8) .
C50 C51 1.548(8) .
C50 H50A 0.9900 .
C50 H50B 0.9900 .
C51 C52 1.556(8) .
C51 H51A 0.9900 .
C51 H51B 0.9900 .
C52 H52A 0.9900 .
C52 H52B 0.9900 .
C53 H53A 0.9800 .
C53 H53B 0.9800 .
C53 H53C 0.9800 .
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
O15 H15 O20 0.97 1.64 2.599(6) 167.6
