#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:16:36 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180420 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/89/7208908.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_7208908
loop_
_publ_author_name
'Hu, Feilong'
'Zou, Huahong'
'Zhao, Xuebo'
'Mi, Yan'
'Luo, Caili'
'Wang, Yunxiao'
_publ_section_title
;
 Second ligands-assisted structural variation of entangled coordination
 polymers with polycatenated or polythreaded features
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1068
_journal_paper_doi               10.1039/c2ce26165k
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C55 H49 N4 Ni2 O19'
_chemical_formula_weight         1187.40
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.211(6)
_cell_angle_beta                 100.988(5)
_cell_angle_gamma                104.960(5)
_cell_formula_units_Z            2
_cell_length_a                   11.275(5)
_cell_length_b                   13.288(6)
_cell_length_c                   18.774(8)
_cell_measurement_temperature    293(2)
_cell_volume                     2656(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14970
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  0.8579
_exptl_absorpt_correction_T_min  0.8579
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1230
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         9205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0698P)²+1.2495P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                6486
_reflns_number_total             9205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26165k.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7208908
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.950719(8) 1.390532(8) 0.071731(5) 0.02648(3) Uani 1 1 d . . .
Ni2 Ni 0.5000 0.5000 0.5000 0.03257(5) Uani 1 2 d S . .
Ni3 Ni 0.5000 0.0000 0.0000 0.03744(5) Uani 1 2 d S . .
O1 O 0.21979(6) 0.77547(7) -0.40412(4) 0.0750(3) Uani 1 1 d . . .
H1 H 0.1526 0.7357 -0.4251 0.113 Uiso 1 1 d R . .
O2 O 0.28448(7) 0.72678(6) -0.50092(4) 0.0706(3) Uani 1 1 d . . .
O3 O 0.76034(8) 1.08404(8) -0.34477(4) 0.1242(4) Uani 1 1 d . . .
O4 O 0.89722(5) 1.33574(5) -0.03366(3) 0.03895(19) Uani 1 1 d . . .
O5 O 0.99055(5) 1.45436(4) -0.10021(3) 0.0424(2) Uani 1 1 d . . .
O6 O 0.97708(5) 1.36398(5) 0.18274(3) 0.0421(2) Uani 1 1 d . . .
O7 O 0.90300(6) 1.22651(5) 0.10431(3) 0.0467(2) Uani 1 1 d . . .
O8 O 1.03000(6) 1.02497(5) 0.40340(3) 0.0547(2) Uani 1 1 d . . .
O9 O 0.80552(6) 0.58991(5) 0.51094(4) 0.0609(2) Uani 1 1 d . . .
O10 O 0.62552(5) 0.62746(5) 0.46989(3) 0.0411(2) Uani 1 1 d . . .
O11 O 0.46078(8) -0.26726(8) 0.22658(5) 0.0632(3) Uani 0.7417(11) 1 d P A 1
C46 C 0.57573(10) -0.25679(8) 0.21720(6) 0.0571(5) Uani 0.7417(11) 1 d P A 1
C50 C 0.74359(9) -0.19055(8) 0.15513(5) 0.0498(5) Uani 0.7417(11) 1 d P A 1
H50 H 0.7746 -0.1505 0.1198 0.060 Uiso 0.7417(11) 1 calc PR A 1
O11' O 0.7855(2) -0.1432(2) 0.11306(15) 0.0632(3) Uani 0.2583(11) 1 d P A 2
C50' C 0.57573(10) -0.25679(8) 0.21720(6) 0.0571(15) Uani 0.2583(11) 1 d P A 2
C46' C 0.74359(9) -0.19055(8) 0.15513(5) 0.0498(11) Uani 0.2583(11) 1 d P A 2
H46 H 0.5022 -0.2590 0.2217 0.060 Uiso 0.2583(11) 1 d PR A 2
O12 O 0.90829(11) 0.47654(9) 0.29428(6) 0.1411(5) Uani 1 1 d . . .
H12C H 0.9306 0.4408 0.2633 0.169 Uiso 1 1 d R . .
H12D H 0.9251 0.4541 0.3358 0.169 Uiso 1 1 d R . .
C47 C 0.65258(11) -0.30948(9) 0.25942(6) 0.0689(4) Uani 1 1 d . . .
H47 H 0.6227 -0.3505 0.2946 0.083 Uiso 1 1 d R A .
C48 C 0.77128(11) -0.30100(9) 0.24926(7) 0.0782(4) Uani 1 1 d . A .
H48 H 0.8213 -0.3356 0.2784 0.094 Uiso 1 1 calc R . .
C49 C 0.81978(11) -0.24212(9) 0.19654(6) 0.0699(4) Uani 1 1 d . . .
H49 H 0.9003 -0.2377 0.1895 0.084 Uiso 1 1 calc R A 1
O13 O 0.95647(7) 0.41083(6) 0.43472(4) 0.0755(3) Uani 1 1 d . . .
H13D H 0.9328 0.4506 0.4623 0.091 Uiso 1 1 d R . .
H13C H 1.0297 0.4051 0.4515 0.091 Uiso 1 1 d R . .
O14 O 0.34814(19) 0.54918(13) 0.29219(9) 0.2387(11) Uani 1 1 d . . .
H14C H 0.3544 0.5584 0.3380 0.286 Uiso 1 1 d R . .
H14D H 0.3828 0.6069 0.2772 0.286 Uiso 1 1 d R . .
O15 O 0.58789(5) -0.08746(5) 0.06941(3) 0.0445(2) Uani 1 1 d . . .
O16 O 0.43217(6) -0.15289(6) 0.12630(4) 0.0619(2) Uani 1 1 d . . .
O17 O 0.68128(6) 0.08883(5) -0.00687(3) 0.0506(2) Uani 1 1 d . . .
H17B H 0.6723 0.1397 0.0184 0.061 Uiso 1 1 d R . .
H17 H 0.6768 0.1213 -0.0431 0.076 Uiso 1 1 d R . .
O18 O 0.35739(5) 0.55757(5) 0.44441(3) 0.0428(2) Uani 1 1 d . . .
H18C H 0.3728 0.6211 0.4610 0.051 Uiso 1 1 d R . .
H18 H 0.2902 0.5262 0.4538 0.051 Uiso 1 1 d R . .
O19 O 0.01759(18) 0.04533(18) 0.04268(13) 0.2437(14) Uani 0.7206(13) 1 d P B 1
H19A H -0.0436 -0.0063 0.0457 0.292 Uiso 0.7206(13) 1 d PR B 1
H19B H 0.0695 0.1043 0.0583 0.292 Uiso 0.7206(13) 1 d PR B 1
O19' O -0.1079(3) 0.0560(3) 0.02740(17) 0.0999(14) Uani 0.2794(13) 1 d P B 2
H19D H -0.0823 0.1107 0.0572 0.120 Uiso 0.2794(13) 1 d PR B 2
H19E H -0.1839 0.0504 0.0075 0.120 Uiso 0.2794(13) 1 d PR B 2
C1 C 0.30266(8) 0.78430(8) -0.44670(6) 0.0520(3) Uani 1 1 d . . .
C2 C 0.41953(8) 0.86842(7) -0.41838(5) 0.0467(3) Uani 1 1 d . . .
C3 C 0.43261(9) 0.93829(8) -0.35942(6) 0.0526(3) Uani 1 1 d . . .
H3 H 0.3647 0.9360 -0.3375 0.063 Uiso 1 1 calc R . .
C4 C 0.54531(10) 1.01148(9) -0.33257(6) 0.0719(4) Uani 1 1 d . . .
H4 H 0.5538 1.0585 -0.2927 0.086 Uiso 1 1 calc R . .
C5 C 0.64570(10) 1.01436(10) -0.36538(6) 0.0730(4) Uani 1 1 d . . .
C6 C 0.63332(10) 0.94512(9) -0.42465(6) 0.0698(4) Uani 1 1 d . . .
H6 H 0.7012 0.9474 -0.4466 0.084 Uiso 1 1 calc R . .
C7 C 0.52062(10) 0.87305(8) -0.45105(6) 0.0596(4) Uani 1 1 d . . .
H7 H 0.5119 0.8268 -0.4913 0.072 Uiso 1 1 calc R . .
C8 C 0.79291(10) 1.15120(10) -0.28129(6) 0.0818(4) Uani 1 1 d . . .
C9 C 0.80210(11) 1.11319(9) -0.21452(6) 0.0824(4) Uani 1 1 d . . .
H9 H 0.7813 1.0415 -0.2105 0.099 Uiso 1 1 calc R . .
C10 C 0.84336(9) 1.18407(8) -0.15246(6) 0.0560(3) Uani 1 1 d . . .
H10 H 0.8472 1.1593 -0.1066 0.067 Uiso 1 1 calc R . .
C11 C 0.87831(7) 1.28960(7) -0.15799(5) 0.0356(3) Uani 1 1 d . . .
C12 C 0.87172(9) 1.32573(9) -0.22682(5) 0.0553(4) Uani 1 1 d . . .
H12 H 0.8974 1.3972 -0.2312 0.066 Uiso 1 1 calc R . .
C13 C 0.82722(10) 1.25626(10) -0.28885(6) 0.0722(5) Uani 1 1 d . . .
H13 H 0.8207 1.2805 -0.3349 0.087 Uiso 1 1 calc R . .
C14 C 0.92462(7) 1.36636(6) -0.09199(5) 0.0304(2) Uani 1 1 d . . .
C15 C 1.17016(7) 1.34062(7) 0.02099(5) 0.0426(3) Uani 1 1 d . . .
H15 H 1.1069 1.3005 -0.0162 0.051 Uiso 1 1 calc R . .
C16 C 0.29172(8) 1.34578(7) 0.01797(5) 0.0465(3) Uani 1 1 d . . .
H16 H 0.3087 1.3102 -0.0209 0.056 Uiso 1 1 calc R . .
C17 C 0.38942(7) 1.40299(6) 0.07177(4) 0.0272(2) Uani 1 1 d . . .
C18 C 0.35520(7) 1.45240(7) 0.12760(5) 0.0459(3) Uani 1 1 d . . .
H18A H 0.4165 1.4916 0.1660 0.055 Uiso 1 1 calc R . .
C19 C 1.23003(7) 1.44365(8) 0.12634(5) 0.0451(3) Uani 1 1 d . . .
H19 H 1.2098 1.4778 0.1646 0.054 Uiso 1 1 calc R . .
C20 C 0.94517(7) 1.26534(7) 0.16887(5) 0.0378(3) Uani 1 1 d . . .
C21 C 0.96194(7) 1.19826(7) 0.22926(5) 0.0365(3) Uani 1 1 d . . .
C22 C 0.91099(9) 1.09213(7) 0.22050(5) 0.0477(3) Uani 1 1 d . . .
H22 H 0.8633 1.0604 0.1754 0.057 Uiso 1 1 calc R . .
C23 C 0.92953(10) 1.03081(7) 0.27819(5) 0.0525(4) Uani 1 1 d . . .
H23 H 0.8949 0.9587 0.2717 0.063 Uiso 1 1 calc R . .
C24 C 0.99929(8) 1.07815(7) 0.34437(5) 0.0410(3) Uani 1 1 d . . .
C25 C 1.05038(8) 1.18459(7) 0.35418(5) 0.0440(3) Uani 1 1 d . . .
H25 H 1.0976 1.2159 0.3994 0.053 Uiso 1 1 calc R . .
C26 C 1.03212(9) 1.24516(7) 0.29748(5) 0.0444(3) Uani 1 1 d . . .
H26 H 1.0665 1.3173 0.3045 0.053 Uiso 1 1 calc R . .
C27 C 0.95146(8) 0.92955(7) 0.41305(5) 0.0427(3) Uani 1 1 d . . .
C28 C 0.82682(9) 0.91664(7) 0.41237(5) 0.0467(3) Uani 1 1 d . . .
H28 H 0.7890 0.9696 0.3994 0.056 Uiso 1 1 calc R . .
C29 C 0.75804(8) 0.82270(7) 0.43147(5) 0.0434(3) Uani 1 1 d . . .
H29 H 0.6730 0.8126 0.4307 0.052 Uiso 1 1 calc R . .
C30 C 0.81371(8) 0.74384(7) 0.45163(4) 0.0355(3) Uani 1 1 d . . .
C31 C 0.93830(8) 0.75811(7) 0.44859(5) 0.0447(3) Uani 1 1 d . . .
H31 H 0.9761 0.7045 0.4595 0.054 Uiso 1 1 calc R . .
C32 C 1.00728(9) 0.85106(7) 0.42953(5) 0.0487(3) Uani 1 1 d . . .
H32 H 1.0913 0.8603 0.4279 0.058 Uiso 1 1 calc R . .
C33 C 0.74269(8) 0.64581(7) 0.47877(4) 0.0404(3) Uani 1 1 d . . .
C34 C 0.38814(8) 0.34293(7) 0.36611(5) 0.0422(3) Uani 1 1 d . . .
H34 H 0.3152 0.3371 0.3837 0.051 Uiso 1 1 calc R . .
C35 C 0.38096(8) 0.27988(7) 0.30432(5) 0.0449(3) Uani 1 1 d . . .
H35 H 0.3059 0.2316 0.2823 0.054 Uiso 1 1 calc R . .
C36 C 0.48771(8) 0.28982(6) 0.27565(4) 0.0341(3) Uani 1 1 d . . .
C37 C 0.59578(8) 0.36398(7) 0.31127(5) 0.0418(3) Uani 1 1 d . . .
H37 H 0.6690 0.3750 0.2932 0.050 Uiso 1 1 calc R . .
C38 C 0.59395(8) 0.42120(7) 0.37345(5) 0.0418(3) Uani 1 1 d . . .
H38 H 0.6680 0.4696 0.3969 0.050 Uiso 1 1 calc R . .
C39 C 0.48833(7) 0.22218(6) 0.21089(4) 0.0326(3) Uani 1 1 d . . .
C40 C 0.38249(8) 0.18166(7) 0.15715(4) 0.0379(3) Uani 1 1 d . . .
H40 H 0.3072 0.1956 0.1611 0.045 Uiso 1 1 calc R . .
C41 C 0.38792(8) 0.12009(7) 0.09713(5) 0.0396(3) Uani 1 1 d . . .
H41 H 0.3158 0.0947 0.0610 0.048 Uiso 1 1 calc R . .
C42 C 0.59469(8) 0.13456(7) 0.14113(5) 0.0441(3) Uani 1 1 d . . .
H42 H 0.6685 0.1185 0.1363 0.053 Uiso 1 1 calc R . .
C43 C 0.59661(8) 0.19751(7) 0.20201(5) 0.0432(3) Uani 1 1 d . . .
H43 H 0.6705 0.2231 0.2368 0.052 Uiso 1 1 calc R . .
C44 C 0.54211(8) -0.14052(7) 0.11655(5) 0.0427(3) Uani 1 1 d . A .
C45 C 0.62387(9) -0.19561(7) 0.16371(5) 0.0444(3) Uani 1 1 d . . .
C51 C 0.52160(7) 1.40634(6) 0.07108(4) 0.0295(2) Uani 1 1 d . . .
C66 C 0.62264(7) 1.46474(8) 0.12289(5) 0.0444(3) Uani 1 1 d . . .
H66 H 0.6097 1.5075 0.1594 0.053 Uiso 1 1 calc R . .
C69 C 0.55057(7) 1.34912(7) 0.01760(5) 0.0493(3) Uani 1 1 d . . .
H69 H 0.4868 1.3105 -0.0199 0.059 Uiso 1 1 calc R . .
C88 C 0.74166(8) 1.45988(8) 0.12062(5) 0.0461(3) Uani 1 1 d . . .
H88 H 0.8074 1.4994 0.1567 0.055 Uiso 1 1 calc R . .
C91 C 0.67276(7) 1.34821(7) 0.01887(5) 0.0469(3) Uani 1 1 d . . .
H91 H 0.6886 1.3078 -0.0179 0.056 Uiso 1 1 calc R . .
N1 N 0.49318(6) 0.41170(5) 0.40213(4) 0.0369(2) Uani 1 1 d . . .
N2 N 0.49284(7) 0.09591(5) 0.08918(4) 0.0390(2) Uani 1 1 d . . .
N3 N 1.13735(5) 1.38935(5) 0.07369(4) 0.0315(2) Uani 1 1 d . . .
N4 N 0.76903(5) 1.40205(5) 0.06990(4) 0.0303(2) Uani 1 1 d . . .
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'
Ni Ni 0.3393 1.1124 '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'
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
O4 Ni1 O5 120.22(3) . 2_785
O4 Ni1 N4 89.10(3) . .
O5 Ni1 N4 87.04(3) 2_785 .
O4 Ni1 N3 91.91(3) . .
O5 Ni1 N3 89.43(3) 2_785 .
N4 Ni1 N3 176.36(3) . .
O4 Ni1 O6 150.23(3) . .
O5 Ni1 O6 89.53(3) 2_785 .
N4 Ni1 O6 91.69(3) . .
N3 Ni1 O6 89.17(3) . .
O4 Ni1 O7 90.27(3) . .
O5 Ni1 O7 149.45(3) 2_785 .
N4 Ni1 O7 91.89(3) . .
N3 Ni1 O7 91.60(3) . .
O6 Ni1 O7 59.97(2) . .
O4 Ni1 C20 120.01(4) . .
O5 Ni1 C20 119.77(4) 2_785 .
N4 Ni1 C20 94.02(3) . .
N3 Ni1 C20 88.51(3) . .
O6 Ni1 C20 30.26(3) . .
O7 Ni1 C20 29.82(2) . .
O18 Ni2 O18 180.000(1) . 2_666
O18 Ni2 O10 87.00(4) . .
O18 Ni2 O10 93.00(4) 2_666 .
O18 Ni2 O10 93.00(4) . 2_666
O18 Ni2 O10 87.00(4) 2_666 2_666
O10 Ni2 O10 180.0 . 2_666
O18 Ni2 N1 88.69(3) . .
O18 Ni2 N1 91.31(3) 2_666 .
O10 Ni2 N1 90.17(4) . .
O10 Ni2 N1 89.83(4) 2_666 .
O18 Ni2 N1 91.31(3) . 2_666
O18 Ni2 N1 88.69(3) 2_666 2_666
O10 Ni2 N1 89.83(4) . 2_666
O10 Ni2 N1 90.17(4) 2_666 2_666
N1 Ni2 N1 180.0 . 2_666
O15 Ni3 O15 180.00(5) . 2_655
O15 Ni3 N2 90.20(4) . .
O15 Ni3 N2 89.80(4) 2_655 .
O15 Ni3 N2 89.80(4) . 2_655
O15 Ni3 N2 90.20(4) 2_655 2_655
N2 Ni3 N2 180.00(5) . 2_655
O15 Ni3 O17 86.73(4) . .
O15 Ni3 O17 93.27(4) 2_655 .
N2 Ni3 O17 93.23(3) . .
N2 Ni3 O17 86.77(3) 2_655 .
O15 Ni3 O17 93.27(4) . 2_655
O15 Ni3 O17 86.73(4) 2_655 2_655
N2 Ni3 O17 86.77(3) . 2_655
N2 Ni3 O17 93.23(3) 2_655 2_655
O17 Ni3 O17 180.00(5) . 2_655
C5 O3 C8 122.01(10) . .
C14 O4 Ni1 135.89(5) . .
C14 O5 Ni1 149.33(7) . 2_785
C20 O6 Ni1 93.00(5) . .
C20 O7 Ni1 87.12(6) . .
C24 O8 C27 120.81(7) . .
C33 O10 Ni2 128.09(6) . .
O11 C46 C47 119.75(11) . .
O11 C46 C45 121.75(10) . .
C47 C46 C45 118.48(11) . .
C45 C50 C49 122.99(10) . .
C48 C47 C46 120.38(11) . .
C47 C48 C49 121.97(12) . .
C50 C49 C48 117.33(12) . .
C44 O15 Ni3 125.98(7) . .
O2 C1 O1 122.41(8) . .
O2 C1 C2 124.61(10) . .
O1 C1 C2 112.93(9) . .
C3 C2 C7 119.33(8) . .
C3 C2 C1 122.71(10) . .
C7 C2 C1 117.89(9) . .
C4 C3 C2 120.60(11) . .
C3 C4 C5 119.32(11) . .
O3 C5 C6 114.81(11) . .
O3 C5 C4 124.68(11) . .
C6 C5 C4 120.49(10) . .
C7 C6 C5 119.62(11) . .
C6 C7 C2 120.62(10) . .
C9 C8 C13 121.96(10) . .
C9 C8 O3 120.87(12) . .
C13 C8 O3 116.85(11) . .
C8 C9 C10 118.61(11) . .
C11 C10 C9 120.94(10) . .
C10 C11 C12 119.01(8) . .
C10 C11 C14 121.53(8) . .
C12 C11 C14 119.45(9) . .
C13 C12 C11 120.56(11) . .
C8 C13 C12 118.85(11) . .
O5 C14 O4 126.22(7) . .
O5 C14 C11 116.37(8) . .
O4 C14 C11 117.37(7) . .
N3 C15 C16 123.78(7) . 1_655
C15 C16 C17 120.78(9) 1_455 .
C16 C17 C18 115.52(8) . .
C16 C17 C51 121.68(8) . .
C18 C17 C51 122.73(6) . .
C19 C18 C17 120.06(7) 1_455 .
N3 C19 C18 123.62(9) . 1_655
O7 C20 O6 119.46(8) . .
O7 C20 C21 121.18(8) . .
O6 C20 C21 119.33(8) . .
O7 C20 Ni1 63.07(6) . .
O6 C20 Ni1 56.74(5) . .
C21 C20 Ni1 171.65(5) . .
C22 C21 C26 118.92(8) . .
C22 C21 C20 122.30(8) . .
C26 C21 C20 118.78(8) . .
C21 C22 C23 121.02(8) . .
C24 C23 C22 119.13(9) . .
C23 C24 C25 120.57(9) . .
C23 C24 O8 124.00(8) . .
C25 C24 O8 115.31(7) . .
C24 C25 C26 120.40(8) . .
C25 C26 C21 119.95(8) . .
C32 C27 C28 121.37(9) . .
C32 C27 O8 116.35(9) . .
C28 C27 O8 122.06(9) . .
C27 C28 C29 118.55(10) . .
C30 C29 C28 121.18(9) . .
C31 C30 C29 118.48(8) . .
C31 C30 C33 120.07(9) . .
C29 C30 C33 121.42(9) . .
C32 C31 C30 120.65(10) . .
C27 C32 C31 119.65(10) . .
O9 C33 O10 124.47(8) . .
O9 C33 C30 117.24(8) . .
O10 C33 C30 118.25(8) . .
N1 C34 C35 124.15(9) . .
C34 C35 C36 118.87(7) . .
C37 C36 C35 117.15(8) . .
C37 C36 C39 120.92(8) . .
C35 C36 C39 121.91(7) . .
C38 C37 C36 119.50(9) . .
N1 C38 C37 124.11(7) . .
C40 C39 C43 116.97(8) . .
C40 C39 C36 122.19(9) . .
C43 C39 C36 120.84(7) . .
C39 C40 C41 120.18(9) . .
N2 C41 C40 122.49(7) . .
N2 C42 C43 123.36(9) . .
C39 C43 C42 119.67(7) . .
O16 C44 O15 125.05(9) . .
O16 C44 C45 117.34(9) . .
O15 C44 C45 117.59(9) . .
C50 C45 C46 118.84(9) . .
C50 C45 C44 121.70(9) . .
C46 C45 C44 119.44(10) . .
C69 C51 C66 115.61(8) . .
C69 C51 C17 120.78(6) . .
C66 C51 C17 123.61(8) . .
C88 C66 C51 120.22(9) . .
C51 C69 C91 120.82(8) . .
N4 C88 C66 123.99(7) . .
N4 C91 C69 123.30(9) . .
C38 N1 C34 116.15(8) . .
C38 N1 Ni2 121.63(5) . .
C34 N1 Ni2 122.21(7) . .
C42 N2 C41 117.31(8) . .
C42 N2 Ni3 120.15(7) . .
C41 N2 Ni3 122.53(5) . .
C15 N3 C19 116.22(8) . .
C15 N3 Ni1 122.66(5) . .
C19 N3 Ni1 120.99(7) . .
C91 N4 C88 116.00(8) . .
C91 N4 Ni1 121.24(7) . .
C88 N4 Ni1 122.71(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O4 2.0040(10) .
Ni1 O5 2.0119(10) 2_785
Ni1 N4 2.0872(11) .
Ni1 N3 2.1017(12) .
Ni1 O6 2.1050(10) .
Ni1 O7 2.2443(11) .
Ni1 C20 2.5141(12) .
Ni2 O18 2.0777(9) .
Ni2 O18 2.0777(9) 2_666
Ni2 O10 2.0815(8) .
Ni2 O10 2.0815(8) 2_666
Ni2 N1 2.1195(10) .
Ni2 N1 2.1195(10) 2_666
Ni3 O15 2.0615(8) .
Ni3 O15 2.0615(8) 2_655
Ni3 N2 2.0914(10) .
Ni3 N2 2.0914(10) 2_655
Ni3 O17 2.1105(10) .
Ni3 O17 2.1105(10) 2_655
O1 C1 1.3272(14) .
O2 C1 1.2007(13) .
O3 C5 1.3570(13) .
O3 C8 1.3904(15) .
O4 C14 1.2486(11) .
O5 C14 1.2460(10) .
O5 Ni1 2.0119(10) 2_785
O6 C20 1.2688(12) .
O7 C20 1.2517(11) .
O8 C24 1.3741(12) .
O8 C27 1.3870(11) .
O9 C33 1.2497(13) .
O10 C33 1.2566(12) .
O11 C46 1.3137(16) .
C46 C47 1.4013(17) .
C46 C45 1.4165(15) .
C50 C45 1.3745(16) .
C50 C49 1.3792(16) .
C47 C48 1.3643(19) .
C48 C49 1.3915(18) .
O15 C44 1.2574(12) .
O16 C44 1.2573(13) .
C1 C2 1.4815(12) .
C2 C3 1.3773(15) .
C2 C7 1.3828(16) .
C3 C4 1.3764(14) .
C4 C5 1.3812(18) .
C5 C6 1.3782(17) .
C6 C7 1.3684(14) .
C8 C9 1.3651(17) .
C8 C13 1.3698(19) .
C9 C10 1.3942(15) .
C10 C11 1.3689(14) .
C11 C12 1.3912(14) .
C11 C14 1.4931(12) .
C12 C13 1.3839(15) .
C15 N3 1.3224(13) .
C15 C16 1.3668(14) 1_655
C16 C15 1.3668(14) 1_455
C16 C17 1.3769(11) .
C17 C18 1.3821(14) .
C17 C51 1.4820(13) .
C18 C19 1.3814(14) 1_455
C19 N3 1.3234(10) .
C19 C18 1.3814(14) 1_655
C20 C21 1.4830(14) .
C21 C22 1.3687(13) .
C21 C26 1.3972(12) .
C22 C23 1.3966(15) .
C23 C24 1.3674(13) .
C24 C25 1.3730(13) .
C25 C26 1.3753(14) .
C27 C32 1.3671(15) .
C27 C28 1.3686(15) .
C28 C29 1.3888(14) .
C29 C30 1.3838(15) .
C30 C31 1.3807(14) .
C30 C33 1.5053(13) .
C31 C32 1.3793(14) .
C34 N1 1.3353(10) .
C34 C35 1.3815(14) .
C35 C36 1.3879(14) .
C36 C37 1.3862(11) .
C36 C39 1.4860(13) .
C37 C38 1.3747(14) .
C38 N1 1.3271(13) .
C39 C40 1.3781(11) .
C39 C43 1.3805(15) .
C40 C41 1.3871(13) .
C41 N2 1.3360(14) .
C42 N2 1.3280(11) .
C42 C43 1.3834(14) .
C44 C45 1.5024(14) .
C51 C69 1.3738(14) .
C51 C66 1.3816(11) .
C66 C88 1.3686(14) .
C69 C91 1.3766(14) .
C88 N4 1.3306(13) .
C91 N4 1.3257(10) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O5 Ni1 O4 C14 29.35(9) 2_785 .
N4 Ni1 O4 C14 115.40(9) . .
N3 Ni1 O4 C14 -61.10(9) . .
O6 Ni1 O4 C14 -152.76(8) . .
O7 Ni1 O4 C14 -152.71(9) . .
C20 Ni1 O4 C14 -150.48(8) . .
O4 Ni1 O6 C20 3.91(8) . .
O5 Ni1 O6 C20 -177.91(5) 2_785 .
N4 Ni1 O6 C20 95.07(5) . .
N3 Ni1 O6 C20 -88.47(5) . .
O7 Ni1 O6 C20 3.86(5) . .
O4 Ni1 O7 C20 176.11(5) . .
O5 Ni1 O7 C20 -7.40(8) 2_785 .
N4 Ni1 O7 C20 -94.78(6) . .
N3 Ni1 O7 C20 84.20(6) . .
O6 Ni1 O7 C20 -3.92(5) . .
O18 Ni2 O10 C33 -173.05(7) . .
O18 Ni2 O10 C33 6.95(7) 2_666 .
O10 Ni2 O10 C33 135(100) 2_666 .
N1 Ni2 O10 C33 -84.37(7) . .
N1 Ni2 O10 C33 95.63(7) 2_666 .
O11 C46 C47 C48 178.69(10) . .
C45 C46 C47 C48 0.48(15) . .
C46 C47 C48 C49 -1.13(17) . .
C45 C50 C49 C48 -0.33(15) . .
C47 C48 C49 C50 1.04(16) . .
O15 Ni3 O15 C44 -3.28(7) 2_655 .
N2 Ni3 O15 C44 63.02(7) . .
N2 Ni3 O15 C44 -116.98(7) 2_655 .
O17 Ni3 O15 C44 156.24(7) . .
O17 Ni3 O15 C44 -23.76(7) 2_655 .
O2 C1 C2 C3 174.41(11) . .
O1 C1 C2 C3 -8.10(15) . .
O2 C1 C2 C7 -8.52(16) . .
O1 C1 C2 C7 168.97(10) . .
C7 C2 C3 C4 -0.66(16) . .
C1 C2 C3 C4 176.38(10) . .
C2 C3 C4 C5 0.01(18) . .
C8 O3 C5 C6 -172.53(11) . .
C8 O3 C5 C4 9.07(19) . .
C3 C4 C5 O3 178.64(11) . .
C3 C4 C5 C6 0.33(19) . .
O3 C5 C6 C7 -178.49(11) . .
C4 C5 C6 C7 -0.01(19) . .
C5 C6 C7 C2 -0.64(18) . .
C3 C2 C7 C6 0.98(17) . .
C1 C2 C7 C6 -176.20(10) . .
C5 O3 C8 C9 65.36(17) . .
C5 O3 C8 C13 -121.04(13) . .
C13 C8 C9 C10 2.40(19) . .
O3 C8 C9 C10 175.67(10) . .
C8 C9 C10 C11 -2.30(17) . .
C9 C10 C11 C12 0.24(15) . .
C9 C10 C11 C14 -179.01(10) . .
C10 C11 C12 C13 1.78(15) . .
C14 C11 C12 C13 -178.95(10) . .
C9 C8 C13 C12 -0.43(19) . .
O3 C8 C13 C12 -173.96(11) . .
C11 C12 C13 C8 -1.71(17) . .
Ni1 O5 C14 O4 -32.95(16) 2_785 .
Ni1 O5 C14 C11 149.40(8) 2_785 .
Ni1 O4 C14 O5 -9.09(14) . .
Ni1 O4 C14 C11 168.53(6) . .
C10 C11 C14 O5 157.53(9) . .
C12 C11 C14 O5 -21.71(12) . .
C10 C11 C14 O4 -20.33(13) . .
C12 C11 C14 O4 160.43(9) . .
C15 C16 C17 C18 0.52(14) 1_455 .
C15 C16 C17 C51 177.59(8) 1_455 .
C16 C17 C18 C19 -0.87(13) . 1_455
C51 C17 C18 C19 -177.90(9) . 1_455
Ni1 O7 C20 O6 6.47(8) . .
Ni1 O7 C20 C21 -171.77(8) . .
Ni1 O6 C20 O7 -6.90(9) . .
Ni1 O6 C20 C21 171.37(7) . .
O4 Ni1 C20 O7 -4.49(6) . .
O5 Ni1 C20 O7 175.68(5) 2_785 .
N4 Ni1 C20 O7 86.79(6) . .
N3 Ni1 C20 O7 -95.83(5) . .
O6 Ni1 C20 O7 173.26(8) . .
O4 Ni1 C20 O6 -177.76(4) . .
O5 Ni1 C20 O6 2.41(6) 2_785 .
N4 Ni1 C20 O6 -86.47(5) . .
N3 Ni1 C20 O6 90.90(5) . .
O7 Ni1 C20 O6 -173.26(8) . .
O4 Ni1 C20 C21 118.0(5) . .
O5 Ni1 C20 C21 -61.8(5) 2_785 .
N4 Ni1 C20 C21 -150.7(5) . .
N3 Ni1 C20 C21 26.7(5) . .
O6 Ni1 C20 C21 -64.2(5) . .
O7 Ni1 C20 C21 122.5(5) . .
O7 C20 C21 C22 -12.88(14) . .
O6 C20 C21 C22 168.88(9) . .
Ni1 C20 C21 C22 -131.4(4) . .
O7 C20 C21 C26 167.19(9) . .
O6 C20 C21 C26 -11.06(13) . .
Ni1 C20 C21 C26 48.7(5) . .
C26 C21 C22 C23 -0.77(16) . .
C20 C21 C22 C23 179.29(10) . .
C21 C22 C23 C24 0.30(17) . .
C22 C23 C24 C25 0.12(16) . .
C22 C23 C24 O8 -175.75(10) . .
C27 O8 C24 C23 -29.77(15) . .
C27 O8 C24 C25 154.17(9) . .
C23 C24 C25 C26 -0.03(16) . .
O8 C24 C25 C26 176.18(9) . .
C24 C25 C26 C21 -0.46(16) . .
C22 C21 C26 C25 0.85(15) . .
C20 C21 C26 C25 -179.22(9) . .
C24 O8 C27 C32 132.60(9) . .
C24 O8 C27 C28 -52.83(13) . .
C32 C27 C28 C29 2.30(14) . .
O8 C27 C28 C29 -172.01(8) . .
C27 C28 C29 C30 0.73(14) . .
C28 C29 C30 C31 -3.49(13) . .
C28 C29 C30 C33 174.47(8) . .
C29 C30 C31 C32 3.32(13) . .
C33 C30 C31 C32 -174.67(8) . .
C28 C27 C32 C31 -2.47(14) . .
O8 C27 C32 C31 172.14(8) . .
C30 C31 C32 C27 -0.41(13) . .
Ni2 O10 C33 O9 -2.94(13) . .
Ni2 O10 C33 C30 179.59(5) . .
C31 C30 C33 O9 13.66(12) . .
C29 C30 C33 O9 -164.27(8) . .
C31 C30 C33 O10 -168.68(8) . .
C29 C30 C33 O10 13.38(12) . .
N1 C34 C35 C36 -2.17(15) . .
C34 C35 C36 C37 -0.41(14) . .
C34 C35 C36 C39 177.82(9) . .
C35 C36 C37 C38 1.94(14) . .
C39 C36 C37 C38 -176.30(8) . .
C36 C37 C38 N1 -1.14(15) . .
C37 C36 C39 C40 -152.02(9) . .
C35 C36 C39 C40 29.82(13) . .
C37 C36 C39 C43 27.74(13) . .
C35 C36 C39 C43 -150.42(9) . .
C43 C39 C40 C41 -0.70(13) . .
C36 C39 C40 C41 179.07(8) . .
C39 C40 C41 N2 1.24(13) . .
C40 C39 C43 C42 -0.08(13) . .
C36 C39 C43 C42 -179.85(8) . .
N2 C42 C43 C39 0.41(14) . .
Ni3 O15 C44 O16 3.84(12) . .
Ni3 O15 C44 C45 -177.74(5) . .
C49 C50 C45 C46 -0.28(14) . .
C49 C50 C45 C44 -178.55(9) . .
O11 C46 C45 C50 -177.96(9) . .
C47 C46 C45 C50 0.21(13) . .
O11 C46 C45 C44 0.35(14) . .
C47 C46 C45 C44 178.52(8) . .
O16 C44 C45 C50 177.22(8) . .
O15 C44 C45 C50 -1.33(12) . .
O16 C44 C45 C46 -1.04(12) . .
O15 C44 C45 C46 -179.59(8) . .
C16 C17 C51 C69 -2.24(13) . .
C18 C17 C51 C69 174.61(9) . .
C16 C17 C51 C66 178.31(9) . .
C18 C17 C51 C66 -4.84(13) . .
C69 C51 C66 C88 -2.67(14) . .
C17 C51 C66 C88 176.81(9) . .
C66 C51 C69 C91 2.65(14) . .
C17 C51 C69 C91 -176.85(9) . .
C51 C66 C88 N4 0.90(15) . .
C51 C69 C91 N4 -0.85(15) . .
C37 C38 N1 C34 -1.29(14) . .
C37 C38 N1 Ni2 178.18(7) . .
C35 C34 N1 C38 2.98(14) . .
C35 C34 N1 Ni2 -176.49(7) . .
O18 Ni2 N1 C38 123.38(8) . .
O18 Ni2 N1 C38 -56.62(8) 2_666 .
O10 Ni2 N1 C38 36.39(7) . .
O10 Ni2 N1 C38 -143.61(7) 2_666 .
N1 Ni2 N1 C38 118(100) 2_666 .
O18 Ni2 N1 C34 -57.18(8) . .
O18 Ni2 N1 C34 122.82(8) 2_666 .
O10 Ni2 N1 C34 -144.17(7) . .
O10 Ni2 N1 C34 35.83(7) 2_666 .
N1 Ni2 N1 C34 -62(100) 2_666 .
C43 C42 N2 C41 0.08(13) . .
C43 C42 N2 Ni3 -179.26(7) . .
C40 C41 N2 C42 -0.90(13) . .
C40 C41 N2 Ni3 178.42(6) . .
O15 Ni3 N2 C42 48.18(7) . .
O15 Ni3 N2 C42 -131.82(7) 2_655 .
N2 Ni3 N2 C42 0.00(3) 2_655 .
O17 Ni3 N2 C42 -38.55(7) . .
O17 Ni3 N2 C42 141.45(7) 2_655 .
O15 Ni3 N2 C41 -131.12(7) . .
O15 Ni3 N2 C41 48.88(7) 2_655 .
N2 Ni3 N2 C41 0.00(7) 2_655 .
O17 Ni3 N2 C41 142.15(7) . .
O17 Ni3 N2 C41 -37.85(7) 2_655 .
C16 C15 N3 C19 -1.46(14) 1_655 .
C16 C15 N3 Ni1 174.40(7) 1_655 .
C18 C19 N3 C15 1.08(14) 1_655 .
C18 C19 N3 Ni1 -174.85(8) 1_655 .
O4 Ni1 N3 C15 -13.22(7) . .
O5 Ni1 N3 C15 -133.43(7) 2_785 .
N4 Ni1 N3 C15 -119.3(4) . .
O6 Ni1 N3 C15 137.03(7) . .
O7 Ni1 N3 C15 77.11(7) . .
C20 Ni1 N3 C15 106.76(8) . .
O4 Ni1 N3 C19 162.45(7) . .
O5 Ni1 N3 C19 42.23(7) 2_785 .
N4 Ni1 N3 C19 56.4(4) . .
O6 Ni1 N3 C19 -47.31(7) . .
O7 Ni1 N3 C19 -107.23(8) . .
C20 Ni1 N3 C19 -77.57(8) . .
C69 C91 N4 C88 -1.03(14) . .
C69 C91 N4 Ni1 176.55(8) . .
C66 C88 N4 C91 1.00(14) . .
C66 C88 N4 Ni1 -176.54(8) . .
O4 Ni1 N4 C91 20.07(7) . .
O5 Ni1 N4 C91 140.39(7) 2_785 .
N3 Ni1 N4 C91 126.2(4) . .
O6 Ni1 N4 C91 -130.16(7) . .
O7 Ni1 N4 C91 -70.16(8) . .
C20 Ni1 N4 C91 -99.95(8) . .
O4 Ni1 N4 C88 -162.51(7) . .
O5 Ni1 N4 C88 -42.19(7) 2_785 .
N3 Ni1 N4 C88 -56.4(4) . .
O6 Ni1 N4 C88 47.25(8) . .
O7 Ni1 N4 C88 107.25(8) . .
C20 Ni1 N4 C88 77.47(8) . .
