#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/25/4342521.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_4342521
loop_
_publ_author_name
'Thuéry, Pierre'
'Rivière, Eric'
'Harrowfield, Jack'
_publ_section_title
;
 Uranyl and uranyl-3d block cation complexes with
 1,3-adamantanedicarboxylate: crystal structures, luminescence, and
 magnetic properties.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2838
_journal_page_last               2850
_journal_paper_doi               10.1021/ic503004j
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C44 H45 N4 Ni O10.5 U'
_chemical_formula_weight         1094.58
_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                 109.587(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4567(9)
_cell_length_b                   13.7860(5)
_cell_length_c                   19.9056(11)
_cell_measurement_reflns_used    142929
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.46
_cell_volume                     4254.7(4)
_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    'SHELXT (Sheldrick, 2014)'
_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
'two φ and five ω scans with 2° steps (450 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  0.0477
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            142929
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.308
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light pink'
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         8072
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0354
_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)+(0.0244P)²+3.0434P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                6415
_reflns_number_total             8072
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic503004j_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4342516--4342524.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C44 H45 N4 Ni O10.50 U'
_cod_database_code               4342521
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 0.218307(11) 0.308739(13) 0.767435(9) 0.02669(6) Uani 1 1 d .
Ni1 Ni 0.67612(4) 0.35454(4) 0.62025(3) 0.02802(14) Uani 1 1 d .
O1 O 0.2658(2) 0.1932(2) 0.78933(16) 0.0359(8) Uani 1 1 d .
O2 O 0.1716(2) 0.4251(2) 0.74636(16) 0.0357(8) Uani 1 1 d .
O3 O 0.2072(2) 0.2935(3) 0.63982(16) 0.0380(8) Uani 1 1 d .
O4 O 0.1001(2) 0.2357(2) 0.66942(15) 0.0331(8) Uani 1 1 d .
O5 O 0.0947(2) 0.2422(2) 0.30228(16) 0.0329(8) Uani 1 1 d .
O6 O 0.2025(2) 0.1804(2) 0.38810(15) 0.0319(7) Uani 1 1 d .
O7 O 0.3510(2) 0.3777(2) 0.85653(16) 0.0348(8) Uani 1 1 d .
O8 O 0.3461(2) 0.3632(3) 0.74605(16) 0.0384(8) Uani 1 1 d .
O9 O 0.6264(2) 0.4607(2) 0.67294(16) 0.0331(8) Uani 1 1 d .
O10 O 0.6561(2) 0.3123(2) 0.71379(16) 0.0327(7) Uani 1 1 d .
O11 O 0.7453(8) 0.1339(7) 0.7884(4) 0.092(3) Uani 0.50 1 d PU
H11A H 0.7707 0.0810 0.7795 0.110 Uiso 0.50 1 d PR
H11B H 0.6997 0.1513 0.7629 0.110 Uiso 0.50 1 d PR
N1 N 0.5518(2) 0.3253(3) 0.5543(2) 0.0308(9) Uani 1 1 d .
N2 N 0.6766(2) 0.4179(3) 0.5257(2) 0.0318(9) Uani 1 1 d .
N3 N 0.7444(3) 0.2316(3) 0.61715(19) 0.0302(9) Uani 1 1 d .
N4 N 0.7989(2) 0.4010(3) 0.67490(19) 0.0300(9) Uani 1 1 d .
C1 C 0.0776(3) 0.2457(3) 0.5436(2) 0.0281(11) Uani 1 1 d .
C2 C 0.1334(3) 0.2362(3) 0.4950(2) 0.0270(10) Uani 1 1 d .
H2A H 0.1717 0.2933 0.5015 0.032 Uiso 1 1 calc R
H2B H 0.1699 0.1775 0.5082 0.032 Uiso 1 1 calc R
C3 C 0.0748(3) 0.2293(3) 0.4168(2) 0.0268(10) Uani 1 1 d .
C4 C 0.0155(3) 0.1400(4) 0.4071(3) 0.0387(13) Uani 1 1 d .
H4A H -0.0216 0.1343 0.3566 0.046 Uiso 1 1 calc R
H4B H 0.0508 0.0804 0.4205 0.046 Uiso 1 1 calc R
C5 C -0.0408(4) 0.1513(4) 0.4545(3) 0.0438(14) Uani 1 1 d .
H5 H -0.0796 0.0937 0.4479 0.053 Uiso 1 1 calc R
C6 C 0.0176(3) 0.1568(4) 0.5327(2) 0.0373(12) Uani 1 1 d .
H6A H 0.0525 0.0969 0.5458 0.045 Uiso 1 1 calc R
H6B H -0.0182 0.1623 0.5638 0.045 Uiso 1 1 calc R
C7 C 0.0208(3) 0.3377(4) 0.5225(2) 0.0354(12) Uani 1 1 d .
H7A H -0.0152 0.3441 0.5534 0.042 Uiso 1 1 calc R
H7B H 0.0580 0.3959 0.5294 0.042 Uiso 1 1 calc R
C8 C -0.0373(3) 0.3308(4) 0.4443(2) 0.0398(13) Uani 1 1 d .
H8 H -0.0734 0.3907 0.4309 0.048 Uiso 1 1 calc R
C9 C 0.0186(3) 0.3209(4) 0.3962(2) 0.0380(12) Uani 1 1 d .
H9A H -0.0190 0.3166 0.3457 0.046 Uiso 1 1 calc R
H9B H 0.0559 0.3788 0.4017 0.046 Uiso 1 1 calc R
C10 C -0.0954(3) 0.2428(5) 0.4346(3) 0.0512(16) Uani 1 1 d .
H10A H -0.1339 0.2387 0.3843 0.061 Uiso 1 1 calc R
H10B H -0.1317 0.2491 0.4652 0.061 Uiso 1 1 calc R
C11 C 0.1325(3) 0.2572(3) 0.6214(2) 0.0316(11) Uani 1 1 d .
C12 C 0.1271(3) 0.2169(3) 0.3669(2) 0.0279(11) Uani 1 1 d .
C13 C 0.4819(3) 0.4138(4) 0.8309(2) 0.0313(11) Uani 1 1 d .
C14 C 0.5145(3) 0.3908(3) 0.7686(2) 0.0281(11) Uani 1 1 d .
H14A H 0.5104 0.3202 0.7592 0.034 Uiso 1 1 calc R
H14B H 0.4777 0.4243 0.7250 0.034 Uiso 1 1 calc R
C15 C 0.6084(3) 0.4239(4) 0.7863(2) 0.0330(11) Uani 1 1 d .
C16 C 0.6642(3) 0.3704(4) 0.8530(3) 0.0437(14) Uani 1 1 d .
H16A H 0.7253 0.3901 0.8647 0.052 Uiso 1 1 calc R
H16B H 0.6604 0.2995 0.8443 0.052 Uiso 1 1 calc R
C17 C 0.6328(3) 0.3950(5) 0.9153(3) 0.0484(15) Uani 1 1 d .
H17 H 0.6699 0.3607 0.9592 0.058 Uiso 1 1 calc R
C18 C 0.5389(3) 0.3615(4) 0.8979(2) 0.0409(13) Uani 1 1 d .
H18A H 0.5350 0.2905 0.8901 0.049 Uiso 1 1 calc R
H18B H 0.5188 0.3765 0.9384 0.049 Uiso 1 1 calc R
C19 C 0.4878(3) 0.5245(4) 0.8439(3) 0.0419(13) Uani 1 1 d .
H19A H 0.4512 0.5587 0.8007 0.050 Uiso 1 1 calc R
H19B H 0.4666 0.5407 0.8836 0.050 Uiso 1 1 calc R
C20 C 0.5824(4) 0.5573(4) 0.8626(3) 0.0489(15) Uani 1 1 d .
H20 H 0.5865 0.6287 0.8717 0.059 Uiso 1 1 calc R
C21 C 0.6138(3) 0.5339(4) 0.7994(3) 0.0436(13) Uani 1 1 d .
H21A H 0.5775 0.5682 0.7561 0.052 Uiso 1 1 calc R
H21B H 0.6741 0.5561 0.8105 0.052 Uiso 1 1 calc R
C22 C 0.6380(4) 0.5039(5) 0.9291(3) 0.0580(18) Uani 1 1 d .
H22A H 0.6176 0.5188 0.9694 0.070 Uiso 1 1 calc R
H22B H 0.6986 0.5257 0.9419 0.070 Uiso 1 1 calc R
C23 C 0.3883(3) 0.3842(3) 0.8108(2) 0.0309(11) Uani 1 1 d .
C24 C 0.6326(3) 0.3981(4) 0.7210(3) 0.0325(11) Uani 1 1 d .
C25 C 0.4908(3) 0.2821(4) 0.5739(3) 0.0400(13) Uani 1 1 d .
H25 H 0.5069 0.2524 0.6196 0.048 Uiso 1 1 calc R
C26 C 0.4049(3) 0.2787(4) 0.5308(3) 0.0441(14) Uani 1 1 d .
H26 H 0.3632 0.2468 0.5463 0.053 Uiso 1 1 calc R
C27 C 0.3816(3) 0.3225(3) 0.4651(3) 0.0380(12) Uani 1 1 d .
H27 H 0.3233 0.3212 0.4343 0.046 Uiso 1 1 calc R
C28 C 0.4435(3) 0.3681(3) 0.4444(2) 0.0327(11) Uani 1 1 d .
H28 H 0.4282 0.3984 0.3990 0.039 Uiso 1 1 calc R
C29 C 0.5285(3) 0.3702(3) 0.4898(2) 0.0284(11) Uani 1 1 d .
C30 C 0.5999(3) 0.4175(3) 0.4731(2) 0.0311(11) Uani 1 1 d .
C31 C 0.5890(4) 0.4604(4) 0.4070(3) 0.0440(14) Uani 1 1 d .
H31 H 0.5340 0.4613 0.3708 0.053 Uiso 1 1 calc R
C32 C 0.6598(4) 0.5016(4) 0.3950(3) 0.0513(15) Uani 1 1 d .
H32 H 0.6540 0.5304 0.3503 0.062 Uiso 1 1 calc R
C33 C 0.7380(3) 0.5002(4) 0.4482(3) 0.0463(14) Uani 1 1 d .
H33 H 0.7873 0.5273 0.4408 0.056 Uiso 1 1 calc R
C34 C 0.7445(3) 0.4587(4) 0.5135(3) 0.0401(13) Uani 1 1 d .
H34 H 0.7988 0.4592 0.5507 0.048 Uiso 1 1 calc R
C35 C 0.7118(4) 0.1428(4) 0.5984(3) 0.0370(12) Uani 1 1 d .
H35 H 0.6510 0.1359 0.5777 0.044 Uiso 1 1 calc R
C36 C 0.7629(4) 0.0600(4) 0.6079(2) 0.0373(12) Uani 1 1 d .
H36 H 0.7379 -0.0022 0.5946 0.045 Uiso 1 1 calc R
C37 C 0.8508(4) 0.0715(4) 0.6372(3) 0.0407(13) Uani 1 1 d .
H37 H 0.8875 0.0166 0.6437 0.049 Uiso 1 1 calc R
C38 C 0.8861(3) 0.1620(4) 0.6572(2) 0.0352(12) Uani 1 1 d .
H38 H 0.9468 0.1701 0.6772 0.042 Uiso 1 1 calc R
C39 C 0.8314(3) 0.2410(3) 0.6477(2) 0.0286(11) Uani 1 1 d .
C40 C 0.8614(3) 0.3404(3) 0.6722(2) 0.0284(11) Uani 1 1 d .
C41 C 0.9465(3) 0.3695(4) 0.6910(2) 0.0309(11) Uani 1 1 d .
H41 H 0.9896 0.3261 0.6873 0.037 Uiso 1 1 calc R
C42 C 0.9672(3) 0.4627(4) 0.7153(3) 0.0385(12) Uani 1 1 d .
H42 H 1.0251 0.4846 0.7277 0.046 Uiso 1 1 calc R
C43 C 0.9040(3) 0.5249(4) 0.7215(3) 0.0379(12) Uani 1 1 d .
H43 H 0.9177 0.5885 0.7401 0.046 Uiso 1 1 calc R
C44 C 0.8200(3) 0.4905(3) 0.6996(3) 0.0348(12) Uani 1 1 d .
H44 H 0.7755 0.5327 0.7024 0.042 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'
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'
N N 0.0061 0.0033 '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 179.34(16) . .
O1 U1 O8 89.11(14) . .
O2 U1 O8 90.64(14) . .
O1 U1 O5 90.72(13) . 4_566
O2 U1 O5 89.47(13) . 4_566
O8 U1 O5 174.08(10) . 4_566
O1 U1 O4 89.65(13) . .
O2 U1 O4 91.00(13) . .
O8 U1 O4 119.59(10) . .
O5 U1 O4 66.32(10) 4_566 .
O1 U1 O7 87.62(13) . .
O2 U1 O7 91.74(13) . .
O8 U1 O7 52.92(10) . .
O5 U1 O7 121.16(10) 4_566 .
O4 U1 O7 172.05(9) . .
O1 U1 O3 92.90(13) . .
O2 U1 O3 87.56(13) . .
O8 U1 O3 67.39(11) . .
O5 U1 O3 118.53(10) 4_566 .
O4 U1 O3 52.38(10) . .
O7 U1 O3 120.29(10) . .
O1 U1 O6 89.82(12) . 4_566
O2 U1 O6 89.80(12) . 4_566
O8 U1 O6 121.97(11) . 4_566
O5 U1 O6 52.11(10) 4_566 4_566
O4 U1 O6 118.41(10) . 4_566
O7 U1 O6 69.07(10) . 4_566
O3 U1 O6 170.33(10) . 4_566
N3 Ni1 N4 79.72(16) . .
N3 Ni1 N1 104.85(15) . .
N4 Ni1 N1 171.02(15) . .
N3 Ni1 N2 98.76(15) . .
N4 Ni1 N2 92.68(15) . .
N1 Ni1 N2 79.06(15) . .
N3 Ni1 O10 92.77(13) . .
N4 Ni1 O10 92.09(13) . .
N1 Ni1 O10 95.36(14) . .
N2 Ni1 O10 168.14(14) . .
N3 Ni1 O9 153.46(13) . .
N4 Ni1 O9 89.84(14) . .
N1 Ni1 O9 89.09(14) . .
N2 Ni1 O9 106.10(14) . .
O10 Ni1 O9 63.06(12) . .
N3 Ni1 C24 123.29(16) . .
N4 Ni1 C24 89.75(15) . .
N1 Ni1 C24 93.98(15) . .
N2 Ni1 C24 137.57(16) . .
O10 Ni1 C24 31.60(14) . .
O9 Ni1 C24 31.51(14) . .
C11 O3 U1 93.5(3) . .
C11 O4 U1 94.6(3) . .
C12 O5 U1 95.8(3) . 4_565
C12 O6 U1 93.5(2) . 4_565
C23 O7 U1 92.1(3) . .
C23 O8 U1 96.0(3) . .
C24 O9 Ni1 87.5(3) . .
C24 O10 Ni1 89.2(3) . .
H11A O11 H11B 122.1 . .
C25 N1 C29 118.6(4) . .
C25 N1 Ni1 125.7(3) . .
C29 N1 Ni1 114.6(3) . .
C30 N2 C34 118.8(4) . .
C30 N2 Ni1 114.6(3) . .
C34 N2 Ni1 126.5(3) . .
C35 N3 C39 118.3(4) . .
C35 N3 Ni1 126.4(3) . .
C39 N3 Ni1 114.4(3) . .
C44 N4 C40 119.0(4) . .
C44 N4 Ni1 125.0(3) . .
C40 N4 Ni1 114.7(3) . .
C11 C1 C6 111.2(4) . .
C11 C1 C7 106.9(4) . .
C6 C1 C7 108.2(4) . .
C11 C1 C2 111.9(4) . .
C6 C1 C2 109.3(4) . .
C7 C1 C2 109.3(4) . .
C3 C2 C1 109.8(4) . .
C3 C2 H2A 109.7 . .
C1 C2 H2A 109.7 . .
C3 C2 H2B 109.7 . .
C1 C2 H2B 109.7 . .
H2A C2 H2B 108.2 . .
C12 C3 C2 111.6(4) . .
C12 C3 C9 109.8(4) . .
C2 C3 C9 109.6(4) . .
C12 C3 C4 107.5(3) . .
C2 C3 C4 109.4(4) . .
C9 C3 C4 108.8(4) . .
C5 C4 C3 109.2(4) . .
C5 C4 H4A 109.8 . .
C3 C4 H4A 109.8 . .
C5 C4 H4B 109.8 . .
C3 C4 H4B 109.8 . .
H4A C4 H4B 108.3 . .
C10 C5 C6 109.8(4) . .
C10 C5 C4 110.4(4) . .
C6 C5 C4 109.1(4) . .
C10 C5 H5 109.2 . .
C6 C5 H5 109.2 . .
C4 C5 H5 109.2 . .
C5 C6 C1 109.7(4) . .
C5 C6 H6A 109.7 . .
C1 C6 H6A 109.7 . .
C5 C6 H6B 109.7 . .
C1 C6 H6B 109.7 . .
H6A C6 H6B 108.2 . .
C8 C7 C1 109.8(4) . .
C8 C7 H7A 109.7 . .
C1 C7 H7A 109.7 . .
C8 C7 H7B 109.7 . .
C1 C7 H7B 109.7 . .
H7A C7 H7B 108.2 . .
C10 C8 C7 109.3(4) . .
C10 C8 C9 109.4(4) . .
C7 C8 C9 109.8(4) . .
C10 C8 H8 109.4 . .
C7 C8 H8 109.4 . .
C9 C8 H8 109.4 . .
C3 C9 C8 109.8(4) . .
C3 C9 H9A 109.7 . .
C8 C9 H9A 109.7 . .
C3 C9 H9B 109.7 . .
C8 C9 H9B 109.7 . .
H9A C9 H9B 108.2 . .
C8 C10 C5 109.7(4) . .
C8 C10 H10A 109.7 . .
C5 C10 H10A 109.7 . .
C8 C10 H10B 109.7 . .
C5 C10 H10B 109.7 . .
H10A C10 H10B 108.2 . .
O3 C11 O4 119.0(4) . .
O3 C11 C1 121.8(4) . .
O4 C11 C1 119.0(4) . .
O5 C12 O6 118.5(4) . .
O5 C12 C3 119.5(4) . .
O6 C12 C3 121.9(4) . .
C23 C13 C18 112.0(4) . .
C23 C13 C14 109.3(4) . .
C18 C13 C14 109.2(4) . .
C23 C13 C19 108.1(4) . .
C18 C13 C19 109.4(4) . .
C14 C13 C19 108.7(4) . .
C15 C14 C13 110.5(4) . .
C15 C14 H14A 109.5 . .
C13 C14 H14A 109.5 . .
C15 C14 H14B 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 108.1 . .
C24 C15 C16 112.1(4) . .
C24 C15 C14 105.5(4) . .
C16 C15 C14 108.8(4) . .
C24 C15 C21 111.0(4) . .
C16 C15 C21 110.1(4) . .
C14 C15 C21 109.2(4) . .
C15 C16 C17 109.2(4) . .
C15 C16 H16A 109.8 . .
C17 C16 H16A 109.8 . .
C15 C16 H16B 109.8 . .
C17 C16 H16B 109.8 . .
H16A C16 H16B 108.3 . .
C22 C17 C16 110.4(5) . .
C22 C17 C18 109.1(5) . .
C16 C17 C18 109.7(4) . .
C22 C17 H17 109.2 . .
C16 C17 H17 109.2 . .
C18 C17 H17 109.2 . .
C13 C18 C17 109.4(4) . .
C13 C18 H18A 109.8 . .
C17 C18 H18A 109.8 . .
C13 C18 H18B 109.8 . .
C17 C18 H18B 109.8 . .
H18A C18 H18B 108.3 . .
C20 C19 C13 109.3(4) . .
C20 C19 H19A 109.8 . .
C13 C19 H19A 109.8 . .
C20 C19 H19B 109.8 . .
C13 C19 H19B 109.8 . .
H19A C19 H19B 108.3 . .
C22 C20 C19 109.3(5) . .
C22 C20 C21 109.8(5) . .
C19 C20 C21 109.3(4) . .
C22 C20 H20 109.5 . .
C19 C20 H20 109.5 . .
C21 C20 H20 109.5 . .
C15 C21 C20 109.2(4) . .
C15 C21 H21A 109.8 . .
C20 C21 H21A 109.8 . .
C15 C21 H21B 109.8 . .
C20 C21 H21B 109.8 . .
H21A C21 H21B 108.3 . .
C20 C22 C17 109.8(4) . .
C20 C22 H22A 109.7 . .
C17 C22 H22A 109.7 . .
C20 C22 H22B 109.7 . .
C17 C22 H22B 109.7 . .
H22A C22 H22B 108.2 . .
O7 C23 O8 118.8(4) . .
O7 C23 C13 121.9(4) . .
O8 C23 C13 119.3(4) . .
O9 C24 O10 120.1(4) . .
O9 C24 C15 120.5(4) . .
O10 C24 C15 119.4(4) . .
O9 C24 Ni1 61.0(2) . .
O10 C24 Ni1 59.2(2) . .
C15 C24 Ni1 177.8(4) . .
N1 C25 C26 123.0(5) . .
N1 C25 H25 118.5 . .
C26 C25 H25 118.5 . .
C27 C26 C25 118.4(5) . .
C27 C26 H26 120.8 . .
C25 C26 H26 120.8 . .
C28 C27 C26 119.2(5) . .
C28 C27 H27 120.4 . .
C26 C27 H27 120.4 . .
C27 C28 C29 120.2(4) . .
C27 C28 H28 119.9 . .
C29 C28 H28 119.9 . .
N1 C29 C28 120.5(4) . .
N1 C29 C30 114.8(4) . .
C28 C29 C30 124.6(4) . .
N2 C30 C31 121.5(4) . .
N2 C30 C29 116.0(4) . .
C31 C30 C29 122.5(4) . .
C32 C31 C30 119.0(5) . .
C32 C31 H31 120.5 . .
C30 C31 H31 120.5 . .
C33 C32 C31 119.3(5) . .
C33 C32 H32 120.4 . .
C31 C32 H32 120.4 . .
C32 C33 C34 119.2(5) . .
C32 C33 H33 120.4 . .
C34 C33 H33 120.4 . .
N2 C34 C33 122.2(5) . .
N2 C34 H34 118.9 . .
C33 C34 H34 118.9 . .
N3 C35 C36 123.0(5) . .
N3 C35 H35 118.5 . .
C36 C35 H35 118.5 . .
C37 C36 C35 117.7(5) . .
C37 C36 H36 121.2 . .
C35 C36 H36 121.2 . .
C36 C37 C38 120.6(5) . .
C36 C37 H37 119.7 . .
C38 C37 H37 119.7 . .
C37 C38 C39 118.7(5) . .
C37 C38 H38 120.6 . .
C39 C38 H38 120.6 . .
N3 C39 C38 121.6(5) . .
N3 C39 C40 114.8(4) . .
C38 C39 C40 123.5(4) . .
N4 C40 C41 122.0(4) . .
N4 C40 C39 114.4(4) . .
C41 C40 C39 123.5(4) . .
C42 C41 C40 118.4(5) . .
C42 C41 H41 120.8 . .
C40 C41 H41 120.8 . .
C41 C42 C43 120.3(5) . .
C41 C42 H42 119.9 . .
C43 C42 H42 119.9 . .
C42 C43 C44 117.4(5) . .
C42 C43 H43 121.3 . .
C44 C43 H43 121.3 . .
N4 C44 C43 122.8(5) . .
N4 C44 H44 118.6 . .
C43 C44 H44 118.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.763(3) .
U1 O2 1.768(3) .
U1 O8 2.401(3) .
U1 O5 2.461(3) 4_566
U1 O4 2.462(3) .
U1 O7 2.494(3) .
U1 O3 2.494(3) .
U1 O6 2.505(3) 4_566
Ni1 N3 2.046(4) .
Ni1 N4 2.051(4) .
Ni1 N1 2.067(4) .
Ni1 N2 2.078(4) .
Ni1 O10 2.080(3) .
Ni1 O9 2.119(3) .
Ni1 C24 2.420(5) .
O3 C11 1.262(6) .
O4 C11 1.277(5) .
O5 C12 1.265(5) .
O5 U1 2.461(3) 4_565
O6 C12 1.273(5) .
O6 U1 2.505(3) 4_565
O7 C23 1.260(5) .
O8 C23 1.276(5) .
O9 C24 1.266(5) .
O10 C24 1.269(5) .
O11 H11A 0.8876 .
O11 H11B 0.7895 .
N1 C25 1.333(6) .
N1 C29 1.361(6) .
N2 C30 1.342(6) .
N2 C34 1.344(6) .
N3 C35 1.339(6) .
N3 C39 1.361(6) .
N4 C44 1.330(6) .
N4 C40 1.340(6) .
C1 C11 1.516(6) .
C1 C6 1.544(6) .
C1 C7 1.547(7) .
C1 C2 1.546(5) .
C2 C3 1.535(6) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C12 1.525(6) .
C3 C9 1.538(6) .
C3 C4 1.543(6) .
C4 C5 1.536(6) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C10 1.522(8) .
C5 C6 1.532(7) .
C5 H5 1.0000 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.533(6) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C10 1.516(8) .
C8 C9 1.539(6) .
C8 H8 1.0000 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C13 C23 1.513(6) .
C13 C18 1.530(6) .
C13 C14 1.539(6) .
C13 C19 1.546(7) .
C14 C15 1.534(6) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C24 1.523(6) .
C15 C16 1.528(7) .
C15 C21 1.537(7) .
C16 C17 1.534(6) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C22 1.523(8) .
C17 C18 1.537(7) .
C17 H17 1.0000 .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 C20 1.542(7) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 C22 1.523(8) .
C20 C21 1.545(7) .
C20 H20 1.0000 .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C25 C26 1.388(7) .
C25 H25 0.9500 .
C26 C27 1.373(7) .
C26 H26 0.9500 .
C27 C28 1.373(7) .
C27 H27 0.9500 .
C28 C29 1.387(7) .
C28 H28 0.9500 .
C29 C30 1.476(6) .
C30 C31 1.399(6) .
C31 C32 1.386(7) .
C31 H31 0.9500 .
C32 C33 1.365(7) .
C32 H32 0.9500 .
C33 C34 1.390(7) .
C33 H33 0.9500 .
C34 H34 0.9500 .
C35 C36 1.392(7) .
C35 H35 0.9500 .
C36 C37 1.376(7) .
C36 H36 0.9500 .
C37 C38 1.377(7) .
C37 H37 0.9500 .
C38 C39 1.385(6) .
C38 H38 0.9500 .
C39 C40 1.483(7) .
C40 C41 1.381(7) .
C41 C42 1.375(7) .
C41 H41 0.9500 .
C42 C43 1.385(7) .
C42 H42 0.9500 .
C43 C44 1.387(7) .
C43 H43 0.9500 .
C44 H44 0.9500 .
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
O11 H11A O2 0.89 2.47 3.357(10) 174.4 2_646
O11 H11B O10 0.79 2.43 2.991(10) 128.7 .
