#------------------------------------------------------------------------------
#$Date: 2020-07-07 04:22:46 +0300 (Tue, 07 Jul 2020) $
#$Revision: 254044 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/08/7240833.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_7240833
loop_
_publ_author_name
'Yang, Dong-Dong'
'Lu, Liping'
'Zhu, Miaoli'
_publ_section_title
;
 Structural Diversity, Magnetic Properties, or Luminescent Sensing Based
 Ni(II)/Zn(II) Coordination Polymers of the semirigid ligand of
 3,3'-((5-car-boxy-1,3-phe-nylene)bis(oxy))diben¬zate
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE01998G
_journal_year                    2020
_chemical_formula_sum            'C105 H83 N21 Ni3 O19'
_chemical_formula_weight         2119.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-09-23 deposited with the CCDC.	2020-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                97.812(2)
_cell_angle_beta                 103.166(2)
_cell_angle_gamma                94.058(2)
_cell_formula_units_Z            1
_cell_length_a                   13.4660(6)
_cell_length_b                   13.6070(6)
_cell_length_c                   13.7158(6)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.71
_cell_measurement_theta_min      3.04
_cell_volume                     2410.88(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51719
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.791
_diffrn_reflns_theta_min         3.039
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABAS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       blocck
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.7466
_exptl_transmission_factor_min   0.6817
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         19067
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0577
_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)+(0.0619P)²+2.1319P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12869
_reflns_number_total             19067
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce01998g2.cif
_cod_data_source_block           l80+z19
_cod_database_code               7240833
_shelx_shelxl_version_number     2014/7
_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.
;
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.37319(2) 0.26849(2) 0.18176(2) 0.02104(6) Uani 1 1 d . . . . .
Ni2 Ni 0.0000 0.0000 -0.5000 0.02156(8) Uani 1 2 d S . P . .
C1 C 0.16129(16) 0.15254(15) 0.21662(15) 0.0252(4) Uani 1 1 d . . . . .
C2 C 0.05098(17) 0.13772(15) 0.15421(15) 0.0270(4) Uani 1 1 d . . . . .
C3 C -0.0228(2) 0.07484(18) 0.17882(18) 0.0380(5) Uani 1 1 d . . . . .
H3 H -0.0040 0.0384 0.2316 0.046 Uiso 1 1 calc R U . . .
C4 C -0.1241(2) 0.0666(2) 0.1247(2) 0.0474(7) Uani 1 1 d . . . . .
H4 H -0.1733 0.0265 0.1432 0.057 Uiso 1 1 calc R U . . .
C5 C -0.1531(2) 0.1169(2) 0.04392(19) 0.0416(6) Uani 1 1 d . . . . .
H5 H -0.2213 0.1110 0.0079 0.050 Uiso 1 1 calc R U . . .
C6 C -0.07904(17) 0.17657(17) 0.01711(15) 0.0297(4) Uani 1 1 d . . . . .
C7 C 0.02213(17) 0.18878(16) 0.07172(15) 0.0284(4) Uani 1 1 d . . . . .
H7 H 0.0706 0.2305 0.0539 0.034 Uiso 1 1 calc R U . . .
C8 C -0.05046(16) 0.26487(18) -0.11553(16) 0.0304(4) Uani 1 1 d . . . . .
C9 C -0.03676(18) 0.20937(16) -0.20308(17) 0.0311(4) Uani 1 1 d . . . . .
H9 H -0.0640 0.1429 -0.2220 0.037 Uiso 1 1 calc R U . . .
C10 C -0.00843(18) 0.36207(19) -0.08418(17) 0.0343(5) Uani 1 1 d . . . . .
H10 H -0.0174 0.3979 -0.0246 0.041 Uiso 1 1 calc R U . . .
C11 C 0.04792(17) 0.40605(17) -0.14317(17) 0.0319(5) Uani 1 1 d . . . . .
C12 C 0.06070(17) 0.35423(16) -0.23261(16) 0.0295(4) Uani 1 1 d . . . . .
H12 H 0.0968 0.3850 -0.2725 0.035 Uiso 1 1 calc R U . . .
C13 C 0.01840(17) 0.25463(16) -0.26206(16) 0.0280(4) Uani 1 1 d . . . . .
C14 C 0.03016(19) 0.19726(17) -0.36035(17) 0.0339(5) Uani 1 1 d . . . . .
C15 C 0.1429(2) 0.55742(18) -0.1585(2) 0.0410(6) Uani 1 1 d . . . . .
C16 C 0.24784(19) 0.55672(17) -0.13507(18) 0.0336(5) Uani 1 1 d . . . . .
H16 H 0.2786 0.5150 -0.0914 0.040 Uiso 1 1 calc R U . . .
C17 C 0.30811(18) 0.61887(16) -0.17712(16) 0.0300(4) Uani 1 1 d . . . . .
C18 C 0.2596(2) 0.6786(2) -0.2436(2) 0.0431(6) Uani 1 1 d . . . . .
H18 H 0.2986 0.7198 -0.2727 0.052 Uiso 1 1 calc R U . . .
C19 C 0.1540(2) 0.6778(3) -0.2672(3) 0.0583(8) Uani 1 1 d . . . . .
H19 H 0.1226 0.7182 -0.3120 0.070 Uiso 1 1 calc R U . . .
C20 C 0.0949(2) 0.6171(2) -0.2241(3) 0.0553(8) Uani 1 1 d . . . . .
H20 H 0.0239 0.6166 -0.2393 0.066 Uiso 1 1 calc R U . . .
C21 C 0.42377(17) 0.62157(15) -0.14571(15) 0.0273(4) Uani 1 1 d . . . . .
C22 C -0.19210(18) 0.0747(2) -0.62454(19) 0.0395(5) Uani 1 1 d . . . . .
H22 H -0.1592 0.0935 -0.6729 0.047 Uiso 1 1 calc R U . . .
C23 C -0.29293(19) 0.0772(2) -0.6290(2) 0.0448(6) Uani 1 1 d . . . . .
H23 H -0.3418 0.0971 -0.6801 0.054 Uiso 1 1 calc R U . . .
C24 C -0.21748(15) 0.02295(17) -0.49018(16) 0.0283(4) Uani 1 1 d . . . . .
H24 H -0.2069 -0.0007 -0.4285 0.034 Uiso 1 1 calc R U . . .
C25 C -0.40558(15) 0.02291(17) -0.51976(16) 0.0274(4) Uani 1 1 d . . . . .
C26 C -0.48980(16) 0.06751(18) -0.56549(17) 0.0316(4) Uani 1 1 d . . . . .
H26 H -0.4828 0.1129 -0.6091 0.038 Uiso 1 1 calc R U . . .
C27 C -0.41586(16) -0.04412(18) -0.45408(18) 0.0326(5) Uani 1 1 d . . . . .
H27 H -0.3591 -0.0734 -0.4231 0.039 Uiso 1 1 calc R U . . .
C28 C 0.50732(19) 0.09593(17) 0.14153(18) 0.0338(5) Uani 1 1 d . . . . .
H28 H 0.5567 0.1385 0.1262 0.041 Uiso 1 1 calc R U . . .
C29 C 0.37287(18) 0.04296(15) 0.18653(17) 0.0295(4) Uani 1 1 d . . . . .
H29 H 0.3119 0.0408 0.2076 0.035 Uiso 1 1 calc R U . . .
C30 C 0.5078(2) -0.00444(17) 0.1357(2) 0.0367(5) Uani 1 1 d . . . . .
H30 H 0.5563 -0.0428 0.1158 0.044 Uiso 1 1 calc R U . . .
C31 C 0.38910(18) -0.13890(15) 0.17098(17) 0.0294(4) Uani 1 1 d . . . . .
C32 C 0.4046(2) -0.21514(16) 0.10010(17) 0.0346(5) Uani 1 1 d . . . . .
H32 H 0.4356 -0.2008 0.0489 0.042 Uiso 1 1 calc R U . . .
C33 C 0.3735(2) -0.31293(16) 0.10598(17) 0.0348(5) Uani 1 1 d . . . . .
H33 H 0.3834 -0.3647 0.0585 0.042 Uiso 1 1 calc R U . . .
C34 C 0.32775(18) -0.33339(15) 0.18275(17) 0.0303(4) Uani 1 1 d . . . . .
C35 C 0.3117(2) -0.25705(17) 0.25355(19) 0.0378(5) Uani 1 1 d . . . . .
H35 H 0.2804 -0.2712 0.3047 0.045 Uiso 1 1 calc R U . . .
C36 C 0.3428(2) -0.15949(16) 0.24704(19) 0.0388(5) Uani 1 1 d . . . . .
H36 H 0.3325 -0.1076 0.2941 0.047 Uiso 1 1 calc R U . . .
C37 C 0.35047(18) -0.51267(15) 0.16434(17) 0.0295(4) Uani 1 1 d . . . . .
H37 H 0.4053 -0.5085 0.1338 0.035 Uiso 1 1 calc R U . . .
C38 C 0.2239(2) -0.47039(19) 0.2322(3) 0.0499(7) Uani 1 1 d . . . . .
H38 H 0.1764 -0.4342 0.2570 0.060 Uiso 1 1 calc R U . . .
C39 C 0.2319(2) -0.56951(19) 0.2295(2) 0.0482(7) Uani 1 1 d . . . . .
H39 H 0.1897 -0.6134 0.2526 0.058 Uiso 1 1 calc R U . . .
C40 C 0.36471(17) 0.28469(16) 0.40533(14) 0.0288(4) Uani 1 1 d . . . . .
H40 H 0.2977 0.2541 0.3867 0.035 Uiso 1 1 calc R U . . .
C41 C 0.5138(2) 0.3454(2) 0.39906(17) 0.0427(6) Uani 1 1 d . . . . .
H41 H 0.5694 0.3651 0.3739 0.051 Uiso 1 1 calc R U . . .
C42 C 0.5122(2) 0.3582(2) 0.49864(18) 0.0459(7) Uani 1 1 d . . . . .
H42 H 0.5654 0.3869 0.5533 0.055 Uiso 1 1 calc R U . . .
C43 C 0.38162(17) 0.30717(16) 0.59130(14) 0.0280(4) Uani 1 1 d . . . . .
C44 C 0.4176(2) 0.37462(17) 0.67985(16) 0.0367(5) Uani 1 1 d . . . . .
H44 H 0.4599 0.4318 0.6802 0.044 Uiso 1 1 calc R U . . .
C45 C 0.3903(2) 0.35665(17) 0.76816(15) 0.0344(5) Uani 1 1 d . . . . .
H45 H 0.4142 0.4019 0.8277 0.041 Uiso 1 1 calc R U . . .
C46 C 0.3138(2) 0.22607(19) 0.58977(16) 0.0396(6) Uani 1 1 d . . . . .
H46 H 0.2859 0.1833 0.5292 0.048 Uiso 1 1 calc R U . . .
C47 C 0.2868(2) 0.20771(19) 0.67773(16) 0.0384(6) Uani 1 1 d . . . . .
H47 H 0.2412 0.1526 0.6763 0.046 Uiso 1 1 calc R U . . .
C48 C 0.32770(16) 0.27153(15) 0.76751(14) 0.0258(4) Uani 1 1 d . . . . .
C49 C 0.35773(17) 0.28818(16) 0.95571(14) 0.0274(4) Uani 1 1 d . . . . .
H49 H 0.4097 0.3407 0.9718 0.033 Uiso 1 1 calc R U . . .
C50 C 0.23538(18) 0.17293(17) 0.86777(16) 0.0329(5) Uani 1 1 d . . . . .
H50 H 0.1886 0.1320 0.8149 0.039 Uiso 1 1 calc R U . . .
C51 C 0.24774(19) 0.17089(17) 0.96825(16) 0.0336(5) Uani 1 1 d . . . . .
H51 H 0.2100 0.1272 0.9962 0.040 Uiso 1 1 calc R U . . .
C52 C 0.1623(7) 0.6409(10) 0.4624(7) 0.079(3) Uani 0.5 1 d . . P . .
H52 H 0.1226 0.6782 0.4766 0.095 Uiso 0.5 1 d R U P . .
C53 C 0.2113(12) 0.4757(11) 0.5200(11) 0.166(7) Uani 0.5 1 d . . P . .
H53A H 0.2569 0.5079 0.5001 0.249 Uiso 0.5 1 d R U P . .
H53B H 0.1897 0.4118 0.4782 0.249 Uiso 0.5 1 d R U P . .
H53C H 0.2152 0.4691 0.5895 0.249 Uiso 0.5 1 d R U P . .
C54 C 0.0232(16) 0.5213(16) 0.4982(18) 0.151(6) Uani 0.5 1 d . U P . .
H54A H 0.0393 0.5065 0.5609 0.226 Uiso 0.5 1 d R U P . .
H54C H 0.0175 0.5877 0.4841 0.226 Uiso 0.5 1 d R U P . .
H54B H 0.0266 0.5032 0.4200 0.226 Uiso 0.5 1 d R U P . .
N1 N 0.42310(14) 0.12513(12) 0.17352(13) 0.0265(3) Uani 1 1 d . . . . .
N2 N 0.42193(15) -0.03796(13) 0.16513(14) 0.0305(4) Uani 1 1 d . . . . .
N3 N 0.30013(16) -0.43449(13) 0.19077(15) 0.0316(4) Uani 1 1 d . . . . .
N4 N 0.31169(15) -0.59537(13) 0.18745(14) 0.0288(4) Uani 1 1 d . . . . .
N5 N 0.42122(15) 0.29911(13) 0.34100(12) 0.0271(3) Uani 1 1 d . . . . .
N6 N 0.41629(15) 0.32005(15) 0.50234(12) 0.0307(4) Uani 1 1 d . . . . .
N7 N 0.30630(14) 0.24809(13) 0.85965(12) 0.0265(3) Uani 1 1 d . . . . .
N8 N 0.32452(14) 0.24316(13) 1.02297(12) 0.0260(3) Uani 1 1 d . . . . .
N9 N -0.14533(13) 0.04008(14) -0.53795(14) 0.0281(4) Uani 1 1 d . . . . .
N10 N -0.30916(13) 0.04422(15) -0.54255(14) 0.0299(4) Uani 1 1 d . . . . .
N11 N 0.1325(8) 0.5480(10) 0.4870(6) 0.123(4) Uani 0.5 1 d . . P . .
O1 O 0.22439(12) 0.20288(12) 0.18384(12) 0.0309(3) Uani 1 1 d . . . . .
O2 O 0.18235(13) 0.11389(14) 0.29653(13) 0.0388(4) Uani 1 1 d . . . . .
O3 O -0.11702(13) 0.22381(15) -0.06455(13) 0.0416(4) Uani 1 1 d . . . . .
O4 O 0.08532(16) 0.50397(14) -0.10640(16) 0.0545(6) Uani 1 1 d . . . . .
O5 O 0.02679(13) 0.10381(11) -0.36656(12) 0.0316(3) Uani 1 1 d . . . . .
O6 O 0.0423(2) 0.24684(15) -0.42769(15) 0.0688(8) Uani 1 1 d . . . . .
O7 O 0.04453(13) 0.11058(12) -0.57800(12) 0.0332(3) Uani 1 1 d . . . . .
H7A H 0.0617 0.1635 -0.5391 0.050 Uiso 1 1 d R U . . .
H7B H 0.0860 0.1120 -0.6247 0.050 Uiso 1 1 d R U . . .
O8 O 0.46008(13) 0.56700(12) -0.08336(12) 0.0353(4) Uani 1 1 d . . . . .
O9 O 0.47481(13) 0.68048(12) -0.18453(12) 0.0337(3) Uani 1 1 d . . . . .
O10 O 0.2275(8) 0.6687(8) 0.4599(5) 0.135(4) Uani 0.5 1 d . . P . .
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
_geom_angle_publ_flag
N4 Ni1 N8 90.62(7) 1_565 1_554 ?
N4 Ni1 O9 98.93(7) 1_565 2_665 ?
N8 Ni1 O9 94.58(7) 1_554 2_665 ?
N4 Ni1 N1 175.33(7) 1_565 . ?
N8 Ni1 N1 88.21(7) 1_554 . ?
O9 Ni1 N1 85.68(7) 2_665 . ?
N4 Ni1 N5 87.49(7) 1_565 . ?
N8 Ni1 N5 178.03(7) 1_554 . ?
O9 Ni1 N5 85.19(7) 2_665 . ?
N1 Ni1 N5 93.72(7) . . ?
N4 Ni1 O1 86.64(7) 1_565 . ?
N8 Ni1 O1 87.25(6) 1_554 . ?
O9 Ni1 O1 174.11(6) 2_665 . ?
N1 Ni1 O1 88.79(7) . . ?
N5 Ni1 O1 93.17(6) . . ?
N9 Ni2 N9 180.0 2_554 . ?
N9 Ni2 O7 92.27(7) 2_554 . ?
N9 Ni2 O7 87.73(7) . . ?
N9 Ni2 O7 87.73(7) 2_554 2_554 ?
N9 Ni2 O7 92.27(7) . 2_554 ?
O7 Ni2 O7 180.0 . 2_554 ?
N9 Ni2 O5 91.56(7) 2_554 . ?
N9 Ni2 O5 88.44(7) . . ?
O7 Ni2 O5 90.60(6) . . ?
O7 Ni2 O5 89.40(6) 2_554 . ?
N9 Ni2 O5 88.44(7) 2_554 2_554 ?
N9 Ni2 O5 91.55(7) . 2_554 ?
O7 Ni2 O5 89.40(6) . 2_554 ?
O7 Ni2 O5 90.60(6) 2_554 2_554 ?
O5 Ni2 O5 180.0 . 2_554 ?
O1 C1 O2 125.2(2) . . ?
O1 C1 C2 116.52(18) . . ?
O2 C1 C2 118.29(17) . . ?
C3 C2 C7 119.3(2) . . ?
C3 C2 C1 120.78(19) . . ?
C7 C2 C1 119.95(17) . . ?
C4 C3 C2 120.0(2) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 121.1(2) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 118.9(2) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
O3 C6 C7 124.76(19) . . ?
O3 C6 C5 113.8(2) . . ?
C7 C6 C5 121.3(2) . . ?
C6 C7 C2 119.38(19) . . ?
C6 C7 H7 120.3 . . ?
C2 C7 H7 120.3 . . ?
C10 C8 C9 121.76(19) . . ?
C10 C8 O3 119.4(2) . . ?
C9 C8 O3 118.5(2) . . ?
C8 C9 C13 118.9(2) . . ?
C8 C9 H9 120.6 . . ?
C13 C9 H9 120.6 . . ?
C8 C10 C11 118.8(2) . . ?
C8 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
O4 C11 C12 124.32(19) . . ?
O4 C11 C10 114.39(19) . . ?
C12 C11 C10 121.3(2) . . ?
C11 C12 C13 118.83(19) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C9 C13 C12 120.47(19) . . ?
C9 C13 C14 119.90(19) . . ?
C12 C13 C14 119.60(18) . . ?
O6 C14 O5 126.2(2) . . ?
O6 C14 C13 117.0(2) . . ?
O5 C14 C13 116.85(19) . . ?
C20 C15 C16 121.6(2) . . ?
C20 C15 O4 119.3(3) . . ?
C16 C15 O4 118.8(3) . . ?
C15 C16 C17 119.8(2) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C18 C17 C16 118.5(2) . . ?
C18 C17 C21 122.33(19) . . ?
C16 C17 C21 119.1(2) . . ?
C19 C18 C17 121.0(3) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 C20 120.1(3) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C15 C20 C19 118.9(3) . . ?
C15 C20 H20 120.5 . . ?
C19 C20 H20 120.5 . . ?
O8 C21 O9 126.0(2) . . ?
O8 C21 C17 117.46(18) . . ?
O9 C21 C17 116.6(2) . . ?
C23 C22 N9 109.7(2) . . ?
C23 C22 H22 125.1 . . ?
N9 C22 H22 125.1 . . ?
C22 C23 N10 106.3(2) . . ?
C22 C23 H23 126.9 . . ?
N10 C23 H23 126.9 . . ?
N9 C24 N10 111.04(19) . . ?
N9 C24 H24 124.5 . . ?
N10 C24 H24 124.5 . . ?
C26 C25 C27 120.19(18) . . ?
C26 C25 N10 119.69(18) . . ?
C27 C25 N10 120.10(18) . . ?
C27 C26 C25 119.6(2) 2_454 . ?
C27 C26 H26 120.2 2_454 . ?
C25 C26 H26 120.2 . . ?
C26 C27 C25 120.20(19) 2_454 . ?
C26 C27 H27 119.9 2_454 . ?
C25 C27 H27 119.9 . . ?
C30 C28 N1 109.8(2) . . ?
C30 C28 H28 125.1 . . ?
N1 C28 H28 125.1 . . ?
N1 C29 N2 111.01(19) . . ?
N1 C29 H29 124.5 . . ?
N2 C29 H29 124.5 . . ?
C28 C30 N2 106.1(2) . . ?
C28 C30 H30 126.9 . . ?
N2 C30 H30 126.9 . . ?
C36 C31 C32 120.6(2) . . ?
C36 C31 N2 120.03(19) . . ?
C32 C31 N2 119.36(19) . . ?
C31 C32 C33 119.5(2) . . ?
C31 C32 H32 120.3 . . ?
C33 C32 H32 120.3 . . ?
C34 C33 C32 119.8(2) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 120.8(2) . . ?
C33 C34 N3 119.33(19) . . ?
C35 C34 N3 119.8(2) . . ?
C36 C35 C34 119.0(2) . . ?
C36 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
C31 C36 C35 120.3(2) . . ?
C31 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
N4 C37 N3 111.12(19) . . ?
N4 C37 H37 124.4 . . ?
N3 C37 H37 124.4 . . ?
C39 C38 N3 105.9(2) . . ?
C39 C38 H38 127.0 . . ?
N3 C38 H38 127.0 . . ?
C38 C39 N4 109.8(2) . . ?
C38 C39 H39 125.1 . . ?
N4 C39 H39 125.1 . . ?
N5 C40 N6 111.55(19) . . ?
N5 C40 H40 124.2 . . ?
N6 C40 H40 124.2 . . ?
C42 C41 N5 109.9(2) . . ?
C42 C41 H41 125.0 . . ?
N5 C41 H41 125.0 . . ?
C41 C42 N6 106.2(2) . . ?
C41 C42 H42 126.9 . . ?
N6 C42 H42 126.9 . . ?
C46 C43 C44 119.67(18) . . ?
C46 C43 N6 119.89(18) . . ?
C44 C43 N6 120.42(19) . . ?
C43 C44 C45 119.85(19) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C48 C45 C44 119.98(19) . . ?
C48 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C43 C46 C47 120.5(2) . . ?
C43 C46 H46 119.8 . . ?
C47 C46 H46 119.8 . . ?
C48 C47 C46 119.8(2) . . ?
C48 C47 H47 120.1 . . ?
C46 C47 H47 120.1 . . ?
C47 C48 C45 119.94(18) . . ?
C47 C48 N7 119.66(18) . . ?
C45 C48 N7 120.39(17) . . ?
N8 C49 N7 111.28(18) . . ?
N8 C49 H49 124.4 . . ?
N7 C49 H49 124.4 . . ?
C51 C50 N7 106.15(19) . . ?
C51 C50 H50 126.9 . . ?
N7 C50 H50 126.9 . . ?
C50 C51 N8 109.88(18) . . ?
C50 C51 H51 125.1 . . ?
N8 C51 H51 125.1 . . ?
O10 C52 N11 129.8(13) . . ?
O10 C52 H52 117.9 . . ?
N11 C52 H52 106.8 . . ?
N11 C53 H53A 92.0 . . ?
N11 C53 H53B 109.0 . . ?
H53A C53 H53B 111.1 . . ?
N11 C53 H53C 109.2 . . ?
H53A C53 H53C 124.1 . . ?
H53B C53 H53C 109.5 . . ?
C54 C54 N11 150(5) 2_566 . ?
C54 C54 H54A 73.4 2_566 . ?
N11 C54 H54A 98.3 . . ?
C54 C54 H54C 128.6 2_566 . ?
N11 C54 H54C 80.4 . . ?
H54A C54 H54C 123.2 . . ?
C54 C54 H54B 101.8 2_566 . ?
N11 C54 H54B 69.7 . . ?
H54A C54 H54B 147.8 . . ?
H54C C54 H54B 85.3 . . ?
C29 N1 C28 106.08(18) . . ?
C29 N1 Ni1 126.48(15) . . ?
C28 N1 Ni1 126.99(14) . . ?
C29 N2 C30 106.97(18) . . ?
C29 N2 C31 126.05(19) . . ?
C30 N2 C31 126.97(19) . . ?
C37 N3 C38 107.23(18) . . ?
C37 N3 C34 125.14(19) . . ?
C38 N3 C34 127.49(19) . . ?
C37 N4 C39 105.87(19) . . ?
C37 N4 Ni1 126.40(15) . 1_545 ?
C39 N4 Ni1 127.13(15) . 1_545 ?
C40 N5 C41 105.60(17) . . ?
C40 N5 Ni1 126.37(15) . . ?
C41 N5 Ni1 127.82(14) . . ?
C40 N6 C42 106.73(17) . . ?
C40 N6 C43 125.97(18) . . ?
C42 N6 C43 126.78(19) . . ?
C49 N7 C50 106.75(16) . . ?
C49 N7 C48 126.95(17) . . ?
C50 N7 C48 126.02(17) . . ?
C49 N8 C51 105.94(16) . . ?
C49 N8 Ni1 129.80(14) . 1_556 ?
C51 N8 Ni1 124.26(13) . 1_556 ?
C24 N9 C22 106.18(18) . . ?
C24 N9 Ni2 125.32(15) . . ?
C22 N9 Ni2 127.77(14) . . ?
C24 N10 C23 106.80(18) . . ?
C24 N10 C25 126.01(18) . . ?
C23 N10 C25 126.62(19) . . ?
C52 N11 C53 121.3(11) . . ?
C52 N11 C54 121.5(13) . . ?
C53 N11 C54 116.5(15) . . ?
C1 O1 Ni1 155.58(15) . . ?
C6 O3 C8 119.92(18) . . ?
C11 O4 C15 120.40(17) . . ?
C14 O5 Ni2 126.53(15) . . ?
Ni2 O7 H7A 109.6 . . ?
Ni2 O7 H7B 133.1 . . ?
H7A O7 H7B 105.1 . . ?
C21 O9 Ni1 141.37(16) . 2_665 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N4 2.0810(18) 1_565 ?
Ni1 N8 2.0989(16) 1_554 ?
Ni1 O9 2.1047(16) 2_665 ?
Ni1 N1 2.1047(17) . ?
Ni1 N5 2.1054(16) . ?
Ni1 O1 2.1430(15) . ?
Ni2 N9 2.0402(18) 2_554 ?
Ni2 N9 2.0402(18) . ?
Ni2 O7 2.0905(15) . ?
Ni2 O7 2.0905(15) 2_554 ?
Ni2 O5 2.0975(15) . ?
Ni2 O5 2.0975(15) 2_554 ?
C1 O1 1.253(2) . ?
C1 O2 1.263(2) . ?
C1 C2 1.520(3) . ?
C2 C3 1.394(3) . ?
C2 C7 1.402(3) . ?
C3 C4 1.386(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.376(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.387(3) . ?
C5 H5 0.9300 . ?
C6 O3 1.382(3) . ?
C6 C7 1.383(3) . ?
C7 H7 0.9300 . ?
C8 C10 1.372(3) . ?
C8 C9 1.386(3) . ?
C8 O3 1.388(2) . ?
C9 C13 1.389(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.391(3) . ?
C10 H10 0.9300 . ?
C11 O4 1.375(3) . ?
C11 C12 1.382(3) . ?
C12 C13 1.401(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.510(3) . ?
C14 O6 1.248(3) . ?
C14 O5 1.260(3) . ?
C15 C20 1.376(5) . ?
C15 C16 1.377(4) . ?
C15 O4 1.398(3) . ?
C16 C17 1.398(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.387(4) . ?
C17 C21 1.515(3) . ?
C18 C19 1.384(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.386(5) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 O8 1.247(3) . ?
C21 O9 1.266(2) . ?
C22 C23 1.348(3) . ?
C22 N9 1.372(3) . ?
C22 H22 0.9300 . ?
C23 N10 1.380(3) . ?
C23 H23 0.9300 . ?
C24 N9 1.314(2) . ?
C24 N10 1.352(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.387(3) . ?
C25 C27 1.387(3) . ?
C25 N10 1.423(3) . ?
C26 C27 1.381(3) 2_454 ?
C26 H26 0.9300 . ?
C27 C26 1.381(3) 2_454 ?
C27 H27 0.9300 . ?
C28 C30 1.358(3) . ?
C28 N1 1.371(3) . ?
C28 H28 0.9300 . ?
C29 N1 1.320(3) . ?
C29 N2 1.356(3) . ?
C29 H29 0.9300 . ?
C30 N2 1.377(3) . ?
C30 H30 0.9300 . ?
C31 C36 1.381(3) . ?
C31 C32 1.383(3) . ?
C31 N2 1.431(3) . ?
C32 C33 1.385(3) . ?
C32 H32 0.9300 . ?
C33 C34 1.385(3) . ?
C33 H33 0.9300 . ?
C34 C35 1.386(3) . ?
C34 N3 1.425(3) . ?
C35 C36 1.384(3) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 N4 1.315(3) . ?
C37 N3 1.353(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.357(4) . ?
C38 N3 1.373(3) . ?
C38 H38 0.9300 . ?
C39 N4 1.375(3) . ?
C39 H39 0.9300 . ?
C40 N5 1.315(3) . ?
C40 N6 1.357(3) . ?
C40 H40 0.9300 . ?
C41 C42 1.359(3) . ?
C41 N5 1.373(3) . ?
C41 H41 0.9300 . ?
C42 N6 1.372(3) . ?
C42 H42 0.9300 . ?
C43 C46 1.377(3) . ?
C43 C44 1.385(3) . ?
C43 N6 1.430(2) . ?
C44 C45 1.390(3) . ?
C44 H44 0.9300 . ?
C45 C48 1.381(3) . ?
C45 H45 0.9300 . ?
C46 C47 1.385(3) . ?
C46 H46 0.9300 . ?
C47 C48 1.381(3) . ?
C47 H47 0.9300 . ?
C48 N7 1.430(2) . ?
C49 N8 1.315(2) . ?
C49 N7 1.360(2) . ?
C49 H49 0.9300 . ?
C50 C51 1.354(3) . ?
C50 N7 1.383(3) . ?
C50 H50 0.9300 . ?
C51 N8 1.379(3) . ?
C51 H51 0.9300 . ?
C52 O10 0.940(11) . ?
C52 N11 1.407(15) . ?
C52 H52 0.8003 . ?
C53 N11 1.533(14) . ?
C53 H53A 0.8458 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 C54 0.84(3) 2_566 ?
C54 N11 1.54(2) . ?
C54 H54A 0.8929 . ?
C54 H54C 0.9536 . ?
C54 H54B 1.0786 . ?
N4 Ni1 2.0811(18) 1_545 ?
N8 Ni1 2.0989(16) 1_556 ?
O7 H7A 0.8200 . ?
O7 H7B 0.9416 . ?
O9 Ni1 2.1046(16) 2_665 ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 173.6(2) . . . . ?
O2 C1 C2 C3 -6.4(3) . . . . ?
O1 C1 C2 C7 -7.3(3) . . . . ?
O2 C1 C2 C7 172.6(2) . . . . ?
C7 C2 C3 C4 -2.7(4) . . . . ?
C1 C2 C3 C4 176.3(2) . . . . ?
C2 C3 C4 C5 2.4(4) . . . . ?
C3 C4 C5 C6 0.0(4) . . . . ?
C4 C5 C6 O3 -179.6(2) . . . . ?
C4 C5 C6 C7 -2.1(4) . . . . ?
O3 C6 C7 C2 179.0(2) . . . . ?
C5 C6 C7 C2 1.7(3) . . . . ?
C3 C2 C7 C6 0.7(3) . . . . ?
C1 C2 C7 C6 -178.39(19) . . . . ?
C10 C8 C9 C13 -2.0(4) . . . . ?
O3 C8 C9 C13 171.3(2) . . . . ?
C9 C8 C10 C11 1.1(4) . . . . ?
O3 C8 C10 C11 -172.2(2) . . . . ?
C8 C10 C11 O4 178.9(2) . . . . ?
C8 C10 C11 C12 1.0(4) . . . . ?
O4 C11 C12 C13 -179.7(2) . . . . ?
C10 C11 C12 C13 -2.0(4) . . . . ?
C8 C9 C13 C12 1.0(3) . . . . ?
C8 C9 C13 C14 -177.1(2) . . . . ?
C11 C12 C13 C9 1.0(4) . . . . ?
C11 C12 C13 C14 179.1(2) . . . . ?
C9 C13 C14 O6 152.4(3) . . . . ?
C12 C13 C14 O6 -25.7(4) . . . . ?
C9 C13 C14 O5 -27.6(3) . . . . ?
C12 C13 C14 O5 154.3(2) . . . . ?
C20 C15 C16 C17 1.0(4) . . . . ?
O4 C15 C16 C17 -172.36(19) . . . . ?
C15 C16 C17 C18 -1.3(3) . . . . ?
C15 C16 C17 C21 176.44(19) . . . . ?
C16 C17 C18 C19 0.7(4) . . . . ?
C21 C17 C18 C19 -177.0(3) . . . . ?
C17 C18 C19 C20 0.2(5) . . . . ?
C16 C15 C20 C19 -0.1(4) . . . . ?
O4 C15 C20 C19 173.2(3) . . . . ?
C18 C19 C20 C15 -0.5(5) . . . . ?
C18 C17 C21 O8 178.0(2) . . . . ?
C16 C17 C21 O8 0.4(3) . . . . ?
C18 C17 C21 O9 -1.0(3) . . . . ?
C16 C17 C21 O9 -178.69(19) . . . . ?
N9 C22 C23 N10 0.6(3) . . . . ?
C27 C25 C26 C27 -0.6(4) . . . 2_454 ?
N10 C25 C26 C27 177.8(2) . . . 2_454 ?
C26 C25 C27 C26 0.6(4) . . . 2_454 ?
N10 C25 C27 C26 -177.8(2) . . . 2_454 ?
N1 C28 C30 N2 -0.2(3) . . . . ?
C36 C31 C32 C33 -0.2(4) . . . . ?
N2 C31 C32 C33 179.6(2) . . . . ?
C31 C32 C33 C34 -0.3(4) . . . . ?
C32 C33 C34 C35 0.6(4) . . . . ?
C32 C33 C34 N3 -177.3(2) . . . . ?
C33 C34 C35 C36 -0.5(4) . . . . ?
N3 C34 C35 C36 177.4(2) . . . . ?
C32 C31 C36 C35 0.3(4) . . . . ?
N2 C31 C36 C35 -179.5(2) . . . . ?
C34 C35 C36 C31 0.0(4) . . . . ?
N3 C38 C39 N4 0.1(4) . . . . ?
N5 C41 C42 N6 -0.7(4) . . . . ?
C46 C43 C44 C45 4.2(4) . . . . ?
N6 C43 C44 C45 -174.4(2) . . . . ?
C43 C44 C45 C48 0.2(4) . . . . ?
C44 C43 C46 C47 -4.5(4) . . . . ?
N6 C43 C46 C47 174.1(2) . . . . ?
C43 C46 C47 C48 0.4(4) . . . . ?
C46 C47 C48 C45 4.0(4) . . . . ?
C46 C47 C48 N7 -174.9(2) . . . . ?
C44 C45 C48 C47 -4.3(4) . . . . ?
C44 C45 C48 N7 174.7(2) . . . . ?
N7 C50 C51 N8 0.1(3) . . . . ?
N2 C29 N1 C28 0.6(3) . . . . ?
N2 C29 N1 Ni1 173.33(14) . . . . ?
C30 C28 N1 C29 -0.2(3) . . . . ?
C30 C28 N1 Ni1 -172.90(17) . . . . ?
N1 C29 N2 C30 -0.8(3) . . . . ?
N1 C29 N2 C31 -179.9(2) . . . . ?
C28 C30 N2 C29 0.6(3) . . . . ?
C28 C30 N2 C31 179.8(2) . . . . ?
C36 C31 N2 C29 -36.8(4) . . . . ?
C32 C31 N2 C29 143.5(2) . . . . ?
C36 C31 N2 C30 144.2(3) . . . . ?
C32 C31 N2 C30 -35.5(4) . . . . ?
N4 C37 N3 C38 -0.7(3) . . . . ?
N4 C37 N3 C34 175.2(2) . . . . ?
C39 C38 N3 C37 0.4(3) . . . . ?
C39 C38 N3 C34 -175.5(3) . . . . ?
C33 C34 N3 C37 31.5(4) . . . . ?
C35 C34 N3 C37 -146.4(3) . . . . ?
C33 C34 N3 C38 -153.4(3) . . . . ?
C35 C34 N3 C38 28.7(4) . . . . ?
N3 C37 N4 C39 0.8(3) . . . . ?
N3 C37 N4 Ni1 -170.73(15) . . . 1_545 ?
C38 C39 N4 C37 -0.6(3) . . . . ?
C38 C39 N4 Ni1 170.9(2) . . . 1_545 ?
N6 C40 N5 C41 0.3(3) . . . . ?
N6 C40 N5 Ni1 -174.75(15) . . . . ?
C42 C41 N5 C40 0.2(3) . . . . ?
C42 C41 N5 Ni1 175.2(2) . . . . ?
N5 C40 N6 C42 -0.8(3) . . . . ?
N5 C40 N6 C43 -173.0(2) . . . . ?
C41 C42 N6 C40 0.9(3) . . . . ?
C41 C42 N6 C43 173.0(2) . . . . ?
C46 C43 N6 C40 26.4(4) . . . . ?
C44 C43 N6 C40 -155.0(2) . . . . ?
C46 C43 N6 C42 -144.2(3) . . . . ?
C44 C43 N6 C42 34.4(4) . . . . ?
N8 C49 N7 C50 0.4(3) . . . . ?
N8 C49 N7 C48 -173.8(2) . . . . ?
C51 C50 N7 C49 -0.3(3) . . . . ?
C51 C50 N7 C48 174.0(2) . . . . ?
C47 C48 N7 C49 163.3(2) . . . . ?
C45 C48 N7 C49 -15.6(4) . . . . ?
C47 C48 N7 C50 -9.8(4) . . . . ?
C45 C48 N7 C50 171.3(2) . . . . ?
N7 C49 N8 C51 -0.3(3) . . . . ?
N7 C49 N8 Ni1 179.13(14) . . . 1_556 ?
C50 C51 N8 C49 0.1(3) . . . . ?
C50 C51 N8 Ni1 -179.37(17) . . . 1_556 ?
N10 C24 N9 C22 0.5(3) . . . . ?
N10 C24 N9 Ni2 -170.35(15) . . . . ?
C23 C22 N9 C24 -0.7(3) . . . . ?
C23 C22 N9 Ni2 169.9(2) . . . . ?
N9 C24 N10 C23 -0.2(3) . . . . ?
N9 C24 N10 C25 171.7(2) . . . . ?
C22 C23 N10 C24 -0.3(3) . . . . ?
C22 C23 N10 C25 -172.0(2) . . . . ?
C26 C25 N10 C24 166.0(2) . . . . ?
C27 C25 N10 C24 -15.7(4) . . . . ?
C26 C25 N10 C23 -23.8(4) . . . . ?
C27 C25 N10 C23 154.6(3) . . . . ?
O10 C52 N11 C53 2.7(19) . . . . ?
O10 C52 N11 C54 173.0(15) . . . . ?
C54 C54 N11 C52 165(8) 2_566 . . . ?
C54 C54 N11 C53 -24(9) 2_566 . . . ?
O2 C1 O1 Ni1 5.0(5) . . . . ?
C2 C1 O1 Ni1 -175.1(3) . . . . ?
C7 C6 O3 C8 18.7(3) . . . . ?
C5 C6 O3 C8 -163.8(2) . . . . ?
C10 C8 O3 C6 -89.8(3) . . . . ?
C9 C8 O3 C6 96.7(3) . . . . ?
C12 C11 O4 C15 -1.8(4) . . . . ?
C10 C11 O4 C15 -179.7(3) . . . . ?
C20 C15 O4 C11 96.1(3) . . . . ?
C16 C15 O4 C11 -90.4(3) . . . . ?
O6 C14 O5 Ni2 -18.0(4) . . . . ?
C13 C14 O5 Ni2 161.98(15) . . . . ?
O8 C21 O9 Ni1 -1.0(4) . . . 2_665 ?
C17 C21 O9 Ni1 178.03(15) . . . 2_665 ?
