#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:27:03 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180435 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/04/7210413.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_7210413
loop_
_publ_author_name
'Thuéry, Pierre'
_publ_section_title
;
 Uranyl--3d block metal ion heterometallic carboxylate complexes including
 additional chelating nitrogen donors
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              6533
_journal_paper_doi               10.1039/c3ce40941d
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C46 H44 N6 Ni O25 U2'
_chemical_formula_weight         1615.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.575(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2664(2)
_cell_length_b                   24.6040(9)
_cell_length_c                   25.7372(10)
_cell_measurement_reflns_used    154599
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.90
_cell_volume                     5232.6(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-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 2° steps (528 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  0.0484
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            154599
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.90
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.624
_exptl_absorpt_correction_T_max  0.516
_exptl_absorpt_correction_T_min  0.402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.810
_refine_diff_density_min         -1.744
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         15934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0161P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0543
_reflns_number_gt                11760
_reflns_number_total             15934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40941d.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7210413
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.262966(13) 0.598414(5) 0.229282(4) 0.01899(3) Uani 1 1 d .
U2 U 0.659789(13) 0.755157(5) 0.473278(4) 0.01888(3) Uani 1 1 d .
Ni Ni 0.50391(5) 0.850038(17) 0.243664(15) 0.02383(10) Uani 1 1 d .
O1 O 0.3023(2) 0.52807(9) 0.23021(9) 0.0308(6) Uani 1 1 d .
O2 O 0.2249(2) 0.66936(9) 0.22986(9) 0.0296(5) Uani 1 1 d .
O3 O 0.6165(2) 0.70880(9) 0.52383(8) 0.0268(5) Uani 1 1 d .
O4 O 0.7036(2) 0.79959(9) 0.42159(8) 0.0279(5) Uani 1 1 d .
O5 O 0.3911(2) 0.60560(9) 0.31782(8) 0.0248(5) Uani 1 1 d .
O6 O 0.1278(2) 0.59508(9) 0.31372(8) 0.0230(5) Uani 1 1 d .
O7 O 0.3589(2) 0.75273(9) 0.45560(8) 0.0237(5) Uani 1 1 d .
O8 O 0.5089(2) 0.69657(9) 0.41163(8) 0.0264(5) Uani 1 1 d .
O9 O -0.1753(2) 0.68438(9) 0.43209(8) 0.0279(5) Uani 1 1 d .
O10 O -0.0492(2) 0.73668(9) 0.48819(8) 0.0261(5) Uani 1 1 d .
O11 O 0.0127(3) 0.56749(9) 0.50370(9) 0.0397(6) Uani 1 1 d .
O12 O 0.0845(3) 0.51414(9) 0.43825(9) 0.0389(6) Uani 1 1 d .
H12 H 0.0599 0.4853 0.4589 0.047 Uiso 1 1 d R
O13 O -0.0286(2) 0.58150(10) 0.21983(8) 0.0265(5) Uani 1 1 d .
O14 O 0.1005(2) 0.58761(11) 0.14778(8) 0.0372(6) Uani 1 1 d .
O15 O -0.5919(3) 0.60998(11) 0.14908(8) 0.0418(7) Uani 1 1 d .
O16 O -0.4409(2) 0.61505(10) 0.21973(8) 0.0280(5) Uani 1 1 d .
O17 O -0.2097(2) 0.68245(9) 0.03650(8) 0.0282(5) Uani 1 1 d .
O18 O -0.4663(2) 0.66900(9) 0.01772(8) 0.0262(5) Uani 1 1 d .
O19 O -0.1433(3) 0.47566(11) 0.07521(10) 0.0509(8) Uani 1 1 d .
O20 O -0.2472(3) 0.52007(10) 0.00696(9) 0.0454(7) Uani 1 1 d .
H20 H -0.2549 0.4885 -0.0045 0.054 Uiso 1 1 d R
O21 O -0.2492(3) 0.43182(10) -0.04589(8) 0.0358(6) Uani 1 1 d .
H21A H -0.2395 0.4315 -0.0779 0.043 Uiso 1 1 d R
H21B H -0.2115 0.3985 -0.0429 0.043 Uiso 1 1 d R
O22 O 0.6683(3) 0.58770(10) 0.38410(9) 0.0377(6) Uani 1 1 d .
H22A H 0.7215 0.6194 0.4002 0.045 Uiso 1 1 d R
H22B H 0.6796 0.5615 0.4092 0.045 Uiso 1 1 d R
O23 O 0.1527(3) 0.83274(10) 0.51309(10) 0.0446(7) Uani 1 1 d .
H23A H 0.1981 0.8075 0.4998 0.053 Uiso 1 1 d R
H23B H 0.0492 0.8177 0.5173 0.053 Uiso 1 1 d R
O24 O 0.4388(4) 0.59157(13) 0.51365(11) 0.0698(9) Uani 1 1 d .
H24A H 0.4941 0.6259 0.5211 0.084 Uiso 1 1 d R
H24B H 0.4919 0.5796 0.4906 0.084 Uiso 1 1 d R
O25A O 0.6733(5) 0.51980(19) 0.46650(17) 0.0597(18) Uani 0.662(7) 1 d P
O25B O 0.5191(13) 0.4972(4) 0.4338(5) 0.092(5) Uani 0.338(7) 1 d P
N1 N 0.3687(3) 0.81323(11) 0.18274(10) 0.0224(6) Uani 1 1 d .
N2 N 0.3708(3) 0.91565(11) 0.21553(10) 0.0250(6) Uani 1 1 d .
N3 N 0.3416(3) 0.83819(11) 0.30256(10) 0.0297(7) Uani 1 1 d .
N4 N 0.6200(3) 0.89034(11) 0.30376(10) 0.0298(7) Uani 1 1 d .
N5 N 0.6425(3) 0.78140(11) 0.25718(10) 0.0235(6) Uani 1 1 d .
N6 N 0.6839(3) 0.85902(12) 0.18801(10) 0.0296(7) Uani 1 1 d .
C1 C 0.2467(3) 0.61841(12) 0.39653(11) 0.0172(6) Uani 1 1 d .
H1 H 0.3385 0.6031 0.4165 0.021 Uiso 1 1 calc R
C2 C 0.2251(3) 0.67994(12) 0.40874(11) 0.0179(6) Uani 1 1 d .
H2 H 0.1690 0.6982 0.3796 0.021 Uiso 1 1 calc R
C3 C 0.1022(3) 0.66377(12) 0.45112(11) 0.0170(6) Uani 1 1 d .
H3 H 0.1589 0.6596 0.4848 0.020 Uiso 1 1 calc R
C4 C 0.0860(3) 0.60868(12) 0.42435(11) 0.0189(7) Uani 1 1 d .
H4 H -0.0035 0.6103 0.3987 0.023 Uiso 1 1 calc R
C5 C 0.2562(3) 0.60439(12) 0.34011(11) 0.0177(6) Uani 1 1 d .
C6 C 0.3707(3) 0.71184(13) 0.42604(11) 0.0192(7) Uani 1 1 d .
C7 C -0.0479(3) 0.69714(13) 0.45734(12) 0.0207(7) Uani 1 1 d .
C8 C 0.0615(4) 0.56095(14) 0.45915(12) 0.0251(7) Uani 1 1 d .
C9 C -0.1861(3) 0.57102(13) 0.14036(11) 0.0193(7) Uani 1 1 d .
H9 H -0.2398 0.5380 0.1525 0.023 Uiso 1 1 calc R
C10 C -0.3092(3) 0.61915(13) 0.13721(11) 0.0188(7) Uani 1 1 d .
H10 H -0.2541 0.6540 0.1427 0.023 Uiso 1 1 calc R
C11 C -0.3361(3) 0.60729(12) 0.07810(11) 0.0188(7) Uani 1 1 d .
H11 H -0.4327 0.5848 0.0722 0.023 Uiso 1 1 calc R
C12 C -0.1819(3) 0.57129(13) 0.08082(11) 0.0200(7) Uani 1 1 d .
H12A H -0.0881 0.5919 0.0692 0.024 Uiso 1 1 calc R
C13 C -0.0300(3) 0.58019(13) 0.17109(12) 0.0216(7) Uani 1 1 d .
C14 C -0.4547(3) 0.61461(13) 0.17093(12) 0.0212(7) Uani 1 1 d .
C15 C -0.3391(4) 0.65495(13) 0.04236(11) 0.0201(7) Uani 1 1 d .
C16 C -0.1884(4) 0.51700(14) 0.05480(12) 0.0257(7) Uani 1 1 d .
C17 C 0.3796(4) 0.76203(14) 0.16654(13) 0.0275(8) Uani 1 1 d .
H17 H 0.4266 0.7365 0.1890 0.033 Uiso 1 1 calc R
C18 C 0.3244(4) 0.74477(14) 0.11786(13) 0.0310(8) Uani 1 1 d .
H18 H 0.3309 0.7084 0.1081 0.037 Uiso 1 1 calc R
C19 C 0.2600(4) 0.78314(15) 0.08457(13) 0.0329(8) Uani 1 1 d .
H19A H 0.2263 0.7735 0.0511 0.039 Uiso 1 1 calc R
C20 C 0.2459(4) 0.83577(15) 0.10109(13) 0.0313(8) Uani 1 1 d .
H20A H 0.2025 0.8620 0.0788 0.038 Uiso 1 1 calc R
C21 C 0.2959(4) 0.84983(13) 0.15077(12) 0.0236(7) Uani 1 1 d .
C22 C 0.2782(4) 0.90481(13) 0.17263(12) 0.0237(7) Uani 1 1 d .
C23 C 0.1735(4) 0.94422(15) 0.15182(13) 0.0323(8) Uani 1 1 d .
H23 H 0.1107 0.9366 0.1222 0.039 Uiso 1 1 calc R
C24 C 0.1630(4) 0.99445(14) 0.17520(14) 0.0327(8) Uani 1 1 d .
H24 H 0.0909 1.0204 0.1621 0.039 Uiso 1 1 calc R
C25 C 0.2613(4) 1.00602(14) 0.21853(13) 0.0312(8) Uani 1 1 d .
H25 H 0.2592 1.0400 0.2344 0.037 Uiso 1 1 calc R
C26 C 0.3630(4) 0.96498(14) 0.23739(13) 0.0293(8) Uani 1 1 d .
H26 H 0.4286 0.9721 0.2665 0.035 Uiso 1 1 calc R
C27 C 0.1996(4) 0.81195(15) 0.29840(14) 0.0364(9) Uani 1 1 d .
H27 H 0.1746 0.7931 0.2679 0.044 Uiso 1 1 calc R
C28 C 0.0896(4) 0.81182(16) 0.33757(15) 0.0426(10) Uani 1 1 d .
H28 H -0.0087 0.7938 0.3333 0.051 Uiso 1 1 calc R
C29 C 0.1272(5) 0.83855(17) 0.38262(15) 0.0494(11) Uani 1 1 d .
H29 H 0.0539 0.8392 0.4094 0.059 Uiso 1 1 calc R
C30 C 0.2741(5) 0.86465(17) 0.38845(15) 0.0467(11) Uani 1 1 d .
H30 H 0.3021 0.8820 0.4195 0.056 Uiso 1 1 calc R
C31 C 0.3805(5) 0.86486(15) 0.34724(13) 0.0351(9) Uani 1 1 d .
C32 C 0.5394(5) 0.89177(14) 0.34862(13) 0.0347(9) Uani 1 1 d .
C33 C 0.6114(5) 0.91611(16) 0.39305(15) 0.0481(11) Uani 1 1 d .
H33 H 0.5563 0.9175 0.4240 0.058 Uiso 1 1 calc R
C34 C 0.7644(6) 0.93775(16) 0.39003(16) 0.0513(12) Uani 1 1 d .
H34 H 0.8127 0.9542 0.4190 0.062 Uiso 1 1 calc R
C35 C 0.8450(5) 0.93509(15) 0.34484(15) 0.0443(10) Uani 1 1 d .
H35 H 0.9494 0.9488 0.3428 0.053 Uiso 1 1 calc R
C36 C 0.7689(4) 0.91163(14) 0.30193(15) 0.0359(9) Uani 1 1 d .
H36 H 0.8229 0.9106 0.2707 0.043 Uiso 1 1 calc R
C37 C 0.6276(4) 0.74699(14) 0.29701(12) 0.0282(8) Uani 1 1 d .
H37 H 0.5457 0.7529 0.3204 0.034 Uiso 1 1 calc R
C38 C 0.7293(4) 0.70292(14) 0.30476(14) 0.0339(8) Uani 1 1 d .
H38 H 0.7152 0.6795 0.3326 0.041 Uiso 1 1 calc R
C39 C 0.8517(4) 0.69437(15) 0.27044(14) 0.0378(9) Uani 1 1 d .
H39 H 0.9224 0.6652 0.2750 0.045 Uiso 1 1 calc R
C40 C 0.8679(4) 0.72987(15) 0.22908(14) 0.0344(9) Uani 1 1 d .
H40 H 0.9497 0.7246 0.2055 0.041 Uiso 1 1 calc R
C41 C 0.7627(4) 0.77296(14) 0.22294(12) 0.0262(8) Uani 1 1 d .
C42 C 0.7699(4) 0.81308(15) 0.18043(13) 0.0279(8) Uani 1 1 d .
C43 C 0.8540(4) 0.80515(17) 0.13523(14) 0.0408(10) Uani 1 1 d .
H43 H 0.9116 0.7732 0.1304 0.049 Uiso 1 1 calc R
C44 C 0.8521(5) 0.8448(2) 0.09752(15) 0.0490(11) Uani 1 1 d .
H44 H 0.9057 0.8395 0.0666 0.059 Uiso 1 1 calc R
C45 C 0.7702(4) 0.89221(19) 0.10614(14) 0.0437(11) Uani 1 1 d .
H45 H 0.7707 0.9201 0.0817 0.052 Uiso 1 1 calc R
C46 C 0.6865(4) 0.89804(16) 0.15178(14) 0.0395(10) Uani 1 1 d .
H46 H 0.6303 0.9302 0.1574 0.047 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'
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 178.69(10) . .
O1 U1 O15 91.79(10) . 1_655
O2 U1 O15 89.06(10) . 1_655
O1 U1 O13 90.88(9) . .
O2 U1 O13 89.65(9) . .
O15 U1 O13 116.24(7) 1_655 .
O1 U1 O6 92.48(9) . .
O2 U1 O6 86.61(8) . .
O15 U1 O6 174.39(8) 1_655 .
O13 U1 O6 67.34(6) . .
O1 U1 O14 90.09(9) . .
O2 U1 O14 91.18(9) . .
O15 U1 O14 64.01(7) 1_655 .
O13 U1 O14 52.29(7) . .
O6 U1 O14 119.60(7) . .
O1 U1 O5 89.06(9) . .
O2 U1 O5 89.63(9) . .
O15 U1 O5 124.08(7) 1_655 .
O13 U1 O5 119.66(7) . .
O6 U1 O5 52.40(6) . .
O14 U1 O5 171.89(7) . .
O1 U1 O16 88.92(9) . 1_655
O2 U1 O16 90.80(9) . 1_655
O15 U1 O16 52.45(7) 1_655 1_655
O13 U1 O16 168.67(7) . 1_655
O6 U1 O16 124.00(6) . 1_655
O14 U1 O16 116.37(7) . 1_655
O5 U1 O16 71.67(7) . 1_655
O4 U2 O3 178.20(10) . .
O4 U2 O18 88.79(9) . 4_676
O3 U2 O18 92.90(9) . 4_676
O4 U2 O8 89.29(9) . .
O3 U2 O8 89.28(9) . .
O18 U2 O8 122.41(7) 4_676 .
O4 U2 O17 90.95(9) . 4_676
O3 U2 O17 90.56(9) . 4_676
O18 U2 O17 53.01(6) 4_676 4_676
O8 U2 O17 175.40(7) . 4_676
O4 U2 O10 90.68(9) . 1_655
O3 U2 O10 89.02(8) . 1_655
O18 U2 O10 119.71(7) 4_676 1_655
O8 U2 O10 117.87(7) . 1_655
O17 U2 O10 66.72(7) 4_676 1_655
O4 U2 O9 89.20(9) . 1_655
O3 U2 O9 89.21(9) . 1_655
O18 U2 O9 171.79(7) 4_676 1_655
O8 U2 O9 65.52(7) . 1_655
O17 U2 O9 119.08(7) 4_676 1_655
O10 U2 O9 52.36(6) 1_655 1_655
O4 U2 O7 95.77(8) . .
O3 U2 O7 84.22(8) . .
O18 U2 O7 70.72(7) 4_676 .
O8 U2 O7 52.27(7) . .
O17 U2 O7 123.15(7) 4_676 .
O10 U2 O7 167.95(7) 1_655 .
O9 U2 O7 117.41(7) 1_655 .
N4 Ni N5 91.28(10) . .
N4 Ni N3 79.37(12) . .
N5 Ni N3 97.43(11) . .
N4 Ni N2 96.87(10) . .
N5 Ni N2 169.25(10) . .
N3 Ni N2 90.97(10) . .
N4 Ni N1 175.24(11) . .
N5 Ni N1 93.12(10) . .
N3 Ni N1 98.23(10) . .
N2 Ni N1 78.99(10) . .
N4 Ni N6 97.90(11) . .
N5 Ni N6 78.53(11) . .
N3 Ni N6 175.13(10) . .
N2 Ni N6 93.37(11) . .
N1 Ni N6 84.78(10) . .
C5 O5 U1 93.14(16) . .
C5 O6 U1 94.19(17) . .
C6 O7 U2 92.00(16) . .
C6 O8 U2 94.74(17) . .
C7 O9 U2 93.80(18) . 1_455
C7 O10 U2 94.01(17) . 1_455
C8 O12 H12 114.4 . .
C13 O13 U1 94.90(17) . .
C13 O14 U1 93.64(18) . .
C14 O15 U1 95.22(18) . 1_455
C14 O16 U1 92.00(17) . 1_455
C15 O17 U2 93.15(17) . 4_475
C15 O18 U2 94.84(18) . 4_475
C16 O20 H20 107.5 . .
H21A O21 H21B 92.0 . .
H22A O22 H22B 103.1 . .
H23A O23 H23B 100.4 . .
H24A O24 H24B 101.5 . .
C17 N1 C21 118.3(3) . .
C17 N1 Ni 127.0(2) . .
C21 N1 Ni 112.7(2) . .
C26 N2 C22 119.2(3) . .
C26 N2 Ni 126.2(2) . .
C22 N2 Ni 114.5(2) . .
C27 N3 C31 119.2(3) . .
C27 N3 Ni 126.3(2) . .
C31 N3 Ni 114.2(2) . .
C36 N4 C32 119.7(3) . .
C36 N4 Ni 125.0(2) . .
C32 N4 Ni 115.2(2) . .
C37 N5 C41 118.9(3) . .
C37 N5 Ni 125.8(2) . .
C41 N5 Ni 115.3(2) . .
C46 N6 C42 118.7(3) . .
C46 N6 Ni 125.0(2) . .
C42 N6 Ni 113.2(2) . .
C5 C1 C4 118.9(2) . .
C5 C1 C2 115.4(2) . .
C4 C1 C2 87.3(2) . .
C5 C1 H1 111.1 . .
C4 C1 H1 111.1 . .
C2 C1 H1 111.1 . .
C6 C2 C1 118.3(2) . .
C6 C2 C3 117.4(2) . .
C1 C2 C3 88.5(2) . .
C6 C2 H2 110.3 . .
C1 C2 H2 110.3 . .
C3 C2 H2 110.3 . .
C7 C3 C4 118.2(2) . .
C7 C3 C2 119.4(2) . .
C4 C3 C2 87.8(2) . .
C7 C3 H3 109.9 . .
C4 C3 H3 109.9 . .
C2 C3 H3 109.9 . .
C8 C4 C3 116.1(2) . .
C8 C4 C1 122.2(3) . .
C3 C4 C1 90.3(2) . .
C8 C4 H4 108.9 . .
C3 C4 H4 108.9 . .
C1 C4 H4 108.9 . .
O6 C5 O5 119.8(3) . .
O6 C5 C1 119.8(2) . .
O5 C5 C1 120.2(2) . .
O7 C6 O8 119.8(3) . .
O7 C6 C2 121.4(3) . .
O8 C6 C2 118.8(3) . .
O10 C7 O9 119.8(3) . .
O10 C7 C3 120.9(3) . .
O9 C7 C3 119.3(3) . .
O11 C8 O12 124.0(3) . .
O11 C8 C4 120.4(3) . .
O12 C8 C4 115.4(3) . .
C13 C9 C12 118.7(2) . .
C13 C9 C10 117.4(3) . .
C12 C9 C10 88.7(2) . .
C13 C9 H9 110.2 . .
C12 C9 H9 110.2 . .
C10 C9 H9 110.2 . .
C14 C10 C11 117.0(2) . .
C14 C10 C9 116.3(3) . .
C11 C10 C9 89.1(2) . .
C14 C10 H10 110.9 . .
C11 C10 H10 110.9 . .
C9 C10 H10 110.9 . .
C15 C11 C12 118.5(2) . .
C15 C11 C10 117.0(3) . .
C12 C11 C10 88.2(2) . .
C15 C11 H11 110.5 . .
C12 C11 H11 110.5 . .
C10 C11 H11 110.5 . .
C16 C12 C9 116.2(3) . .
C16 C12 C11 118.1(2) . .
C9 C12 C11 90.4(2) . .
C16 C12 H12A 110.2 . .
C9 C12 H12A 110.2 . .
C11 C12 H12A 110.2 . .
O13 C13 O14 119.2(3) . .
O13 C13 C9 120.7(3) . .
O14 C13 C9 120.1(3) . .
O15 C14 O16 120.2(3) . .
O15 C14 C10 118.3(3) . .
O16 C14 C10 121.5(3) . .
O18 C15 O17 119.0(3) . .
O18 C15 C11 121.7(3) . .
O17 C15 C11 119.3(3) . .
O19 C16 O20 124.2(3) . .
O19 C16 C12 123.7(3) . .
O20 C16 C12 112.1(3) . .
N1 C17 C18 123.3(3) . .
N1 C17 H17 118.4 . .
C18 C17 H17 118.4 . .
C19 C18 C17 117.7(3) . .
C19 C18 H18 121.1 . .
C17 C18 H18 121.1 . .
C20 C19 C18 119.5(3) . .
C20 C19 H19A 120.3 . .
C18 C19 H19A 120.3 . .
C19 C20 C21 120.0(3) . .
C19 C20 H20A 120.0 . .
C21 C20 H20A 120.0 . .
N1 C21 C20 121.0(3) . .
N1 C21 C22 115.3(3) . .
C20 C21 C22 123.7(3) . .
N2 C22 C23 120.5(3) . .
N2 C22 C21 115.6(3) . .
C23 C22 C21 123.9(3) . .
C24 C23 C22 120.1(3) . .
C24 C23 H23 120.0 . .
C22 C23 H23 120.0 . .
C23 C24 C25 119.4(3) . .
C23 C24 H24 120.3 . .
C25 C24 H24 120.3 . .
C24 C25 C26 117.7(3) . .
C24 C25 H25 121.2 . .
C26 C25 H25 121.2 . .
N2 C26 C25 123.1(3) . .
N2 C26 H26 118.4 . .
C25 C26 H26 118.4 . .
N3 C27 C28 122.5(4) . .
N3 C27 H27 118.8 . .
C28 C27 H27 118.8 . .
C29 C28 C27 118.9(4) . .
C29 C28 H28 120.6 . .
C27 C28 H28 120.6 . .
C28 C29 C30 119.8(4) . .
C28 C29 H29 120.1 . .
C30 C29 H29 120.1 . .
C29 C30 C31 119.4(4) . .
C29 C30 H30 120.3 . .
C31 C30 H30 120.3 . .
N3 C31 C30 120.2(4) . .
N3 C31 C32 115.4(3) . .
C30 C31 C32 124.4(4) . .
N4 C32 C33 119.9(4) . .
N4 C32 C31 115.4(3) . .
C33 C32 C31 124.6(4) . .
C34 C33 C32 119.1(4) . .
C34 C33 H33 120.4 . .
C32 C33 H33 120.4 . .
C35 C34 C33 120.2(4) . .
C35 C34 H34 119.9 . .
C33 C34 H34 119.9 . .
C34 C35 C36 118.8(4) . .
C34 C35 H35 120.6 . .
C36 C35 H35 120.6 . .
N4 C36 C35 122.3(4) . .
N4 C36 H36 118.9 . .
C35 C36 H36 118.9 . .
N5 C37 C38 122.6(3) . .
N5 C37 H37 118.7 . .
C38 C37 H37 118.7 . .
C39 C38 C37 118.8(3) . .
C39 C38 H38 120.6 . .
C37 C38 H38 120.6 . .
C38 C39 C40 118.9(3) . .
C38 C39 H39 120.5 . .
C40 C39 H39 120.5 . .
C41 C40 C39 119.9(3) . .
C41 C40 H40 120.0 . .
C39 C40 H40 120.0 . .
N5 C41 C40 120.8(3) . .
N5 C41 C42 115.0(3) . .
C40 C41 C42 124.2(3) . .
N6 C42 C43 121.1(3) . .
N6 C42 C41 114.8(3) . .
C43 C42 C41 124.0(3) . .
C44 C43 C42 119.7(4) . .
C44 C43 H43 120.1 . .
C42 C43 H43 120.1 . .
C45 C44 C43 119.1(4) . .
C45 C44 H44 120.5 . .
C43 C44 H44 120.5 . .
C44 C45 C46 119.0(4) . .
C44 C45 H45 120.5 . .
C46 C45 H45 120.5 . .
N6 C46 C45 122.2(4) . .
N6 C46 H46 118.9 . .
C45 C46 H46 118.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.761(2) .
U1 O2 1.774(2) .
U1 O15 2.433(2) 1_655
U1 O13 2.451(2) .
U1 O6 2.472(2) .
U1 O14 2.474(2) .
U1 O5 2.493(2) .
U1 O16 2.500(2) 1_655
U2 O4 1.767(2) .
U2 O3 1.774(2) .
U2 O18 2.438(2) 4_676
U2 O8 2.458(2) .
U2 O17 2.464(2) 4_676
U2 O10 2.468(2) 1_655
U2 O9 2.469(2) 1_655
U2 O7 2.517(2) .
Ni N4 2.053(3) .
Ni N5 2.065(3) .
Ni N3 2.072(3) .
Ni N2 2.073(3) .
Ni N1 2.105(2) .
Ni N6 2.105(3) .
O5 C5 1.269(3) .
O6 C5 1.265(3) .
O7 C6 1.267(3) .
O8 C6 1.268(3) .
O9 C7 1.262(3) .
O9 U2 2.469(2) 1_455
O10 C7 1.256(3) .
O10 U2 2.468(2) 1_455
O11 C8 1.236(4) .
O12 C8 1.288(4) .
O12 H12 0.9129 .
O13 C13 1.255(3) .
O14 C13 1.262(3) .
O15 C14 1.258(3) .
O15 U1 2.433(2) 1_455
O16 C14 1.258(3) .
O16 U1 2.500(2) 1_455
O17 C15 1.278(3) .
O17 U2 2.464(2) 4_475
O18 C15 1.261(3) .
O18 U2 2.438(2) 4_475
O19 C16 1.199(4) .
O20 C16 1.314(4) .
O20 H20 0.8314 .
O21 H21A 0.8286 .
O21 H21B 0.8807 .
O22 H22A 0.9812 .
O22 H22B 0.9152 .
O23 H23A 0.8073 .
O23 H23B 0.9410 .
O24 H24A 0.9769 .
O24 H24B 0.8039 .
N1 C17 1.331(4) .
N1 C21 1.350(4) .
N2 C26 1.340(4) .
N2 C22 1.353(4) .
N3 C27 1.341(4) .
N3 C31 1.355(4) .
N4 C36 1.340(4) .
N4 C32 1.349(4) .
N5 C37 1.338(4) .
N5 C41 1.361(4) .
N6 C46 1.339(4) .
N6 C42 1.352(4) .
C1 C5 1.497(4) .
C1 C4 1.545(4) .
C1 C2 1.557(4) .
C1 H1 0.9800 .
C2 C6 1.495(4) .
C2 C3 1.563(4) .
C2 H2 0.9800 .
C3 C7 1.500(4) .
C3 C4 1.525(4) .
C3 H3 0.9800 .
C4 C8 1.494(4) .
C4 H4 0.9800 .
C9 C13 1.512(4) .
C9 C12 1.534(4) .
C9 C10 1.562(4) .
C9 H9 0.9800 .
C10 C14 1.507(4) .
C10 C11 1.559(4) .
C10 H10 0.9800 .
C11 C15 1.490(4) .
C11 C12 1.552(4) .
C11 H11 0.9800 .
C12 C16 1.494(4) .
C12 H12A 0.9800 .
C17 C18 1.388(4) .
C17 H17 0.9300 .
C18 C19 1.373(5) .
C18 H18 0.9300 .
C19 C20 1.369(5) .
C19 H19A 0.9300 .
C20 C21 1.377(4) .
C20 H20A 0.9300 .
C21 C22 1.474(4) .
C22 C23 1.397(4) .
C23 C24 1.378(5) .
C23 H23 0.9300 .
C24 C25 1.391(4) .
C24 H24 0.9300 .
C25 C26 1.392(4) .
C25 H25 0.9300 .
C26 H26 0.9300 .
C27 C28 1.376(5) .
C27 H27 0.9300 .
C28 C29 1.361(5) .
C28 H28 0.9300 .
C29 C30 1.378(6) .
C29 H29 0.9300 .
C30 C31 1.396(5) .
C30 H30 0.9300 .
C31 C32 1.470(5) .
C32 C33 1.408(5) .
C33 C34 1.376(6) .
C33 H33 0.9300 .
C34 C35 1.358(6) .
C34 H34 0.9300 .
C35 C36 1.382(5) .
C35 H35 0.9300 .
C36 H36 0.9300 .
C37 C38 1.383(4) .
C37 H37 0.9300 .
C38 C39 1.378(5) .
C38 H38 0.9300 .
C39 C40 1.386(5) .
C39 H39 0.9300 .
C40 C41 1.378(5) .
C40 H40 0.9300 .
C41 C42 1.476(5) .
C42 C43 1.386(5) .
C43 C44 1.376(5) .
C43 H43 0.9300 .
C44 C45 1.370(6) .
C44 H44 0.9300 .
C45 C46 1.387(5) .
C45 H45 0.9300 .
C46 H46 0.9300 .
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
O12 H12 O11 0.91 1.73 2.642(3) 172.6 3_566
O20 H20 O21 0.83 1.76 2.562(3) 162.2 .
O21 H21A O14 0.83 2.21 2.965(3) 151.2 3_565
O21 H21A O15 0.83 2.49 3.106(3) 131.9 3_465
O21 H21B O23 0.88 1.85 2.693(3) 160.1 2_545
O22 H22A O9 0.98 1.98 2.961(3) 178.7 1_655
O22 H22B O25A 0.92 1.80 2.699(5) 167.3 .
O22 H22B O25B 0.92 2.17 2.864(9) 131.9 .
O23 H23A O7 0.81 2.23 3.018(3) 166.9 .
O23 H23B O17 0.94 2.21 3.094(3) 156.2 4_576
O23 H23B O10 0.94 2.27 2.953(3) 128.8 .
O24 H24A O3 0.98 2.28 3.244(4) 170.3 .
O24 H24B O25A 0.80 2.20 2.912(5) 147.5 .
O24 H24B O25B 0.80 2.51 3.182(11) 141.7 .
