#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:48:26 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262585 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/21/7242114.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_7242114
loop_
_publ_author_name
'Zhang, Mei-Li'
'Bai, Ye'
'Ren, Yi-Xia'
'Wang, Ji-Jiang'
'Yang, Xiao-Gang'
'Ma, Lu-Fang'
_publ_section_title
;
 Structural diversity and photocatalytic activity of six Co(ii)/Ni(ii)
 complexes with three flexible phenylenediacetate isomers
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1616
_journal_page_last               1627
_journal_paper_doi               10.1039/D0CE01702G
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C78 H72 N16 Ni3 O16, 2(H2 O)'
_chemical_formula_sum            'C78 H76 N16 Ni3 O18'
_chemical_formula_weight         1701.67
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-28 deposited with the CCDC.	2021-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                103.4100(10)
_cell_angle_beta                 108.6770(10)
_cell_angle_gamma                95.7550(10)
_cell_formula_units_Z            1
_cell_length_a                   11.0003(6)
_cell_length_b                   12.7408(7)
_cell_length_c                   15.3439(8)
_cell_measurement_reflns_used    8142
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      30.672
_cell_measurement_theta_min      2.345
_cell_volume                     1945.82(18)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.793
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0106
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.793
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12865
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.837
_diffrn_reflns_theta_min         2.634
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0434 before and 0.0212 after correction. The Ratio of minimum to maximum transmission is 0.8385. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         9695
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0470P)²+2.3386P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1408
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8515
_reflns_number_total             9695
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01702g2.cif
_cod_data_source_block           yd0686_0m
_cod_depositor_comments
'Adding full bibliography for 7242112--7242117.cif.'
_cod_database_code               7242114
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C13-C14 = C9-C10 = C11-C12
 1.4 with sigma of 0.02
3. Others
 Fixed Sof: O5(0.5) O10(0.5) C8(0.5) H8C(0.5) H8D(0.5) C9(0.5) C14(0.5)
 H14(0.5) C13(0.5) H13(0.5) C12(0.5) H12(0.5) C11(0.5) H11(0.5) C10(0.5)
 C43(0.5) H43A(0.5) H43B(0.5) C45(0.5) C46(0.5)
4.a Free rotating group:
 O9(H9A,H9B)
4.b Rotating group:
 O6(H6A,H6B), O8(H8A,H8B)
4.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5A,H5B), C8(H8C,H8D), C43(H43A,H43B)
4.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C12(H12), C11(H11), C15(H15), C17(H17), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
;
_olex2_submission_special_instructions 'No special instructions were received'
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 0.000000 0.000000 1.000000 0.03017(12) Uani 1 2 d S T P . .
Ni2 Ni 0.42406(3) 0.31693(3) 0.73398(2) 0.03138(10) Uani 1 1 d . . . . .
O1 O 0.0524(2) 0.05425(17) 0.89772(14) 0.0408(5) Uani 1 1 d . . . . .
O2 O -0.0853(3) -0.0696(3) 0.76624(17) 0.0723(9) Uani 1 1 d . . . . .
O3 O 0.3796(2) 0.20289(18) 0.79974(14) 0.0427(5) Uani 1 1 d . . . . .
O4 O 0.4589(2) 0.42116(17) 0.65546(15) 0.0416(5) Uani 1 1 d . . . . .
O5 O 0.3845(7) 0.4281(5) 0.2717(5) 0.0741(18) Uani 0.5 1 d . . . A 1
O10 O 0.5537(10) 0.5713(5) 0.7679(4) 0.108(3) Uani 0.5 1 d . . . B 2
O6 O 0.4728(3) 0.4439(2) 0.86396(18) 0.0563(6) Uani 1 1 d . . . . .
H6A H 0.544074 0.489008 0.874356 0.085 Uiso 1 1 d GR . . . .
H6B H 0.493352 0.416638 0.912486 0.085 Uiso 1 1 d GR . . . .
O7 O 0.4523(2) 0.2911(2) 0.95556(16) 0.0506(6) Uani 1 1 d . . . . .
O8 O -0.1870(2) -0.07687(18) 0.90092(15) 0.0440(5) Uani 1 1 d . . . . .
H8A H -0.208044 -0.141436 0.906565 0.066 Uiso 1 1 d GR . . . .
H8B H -0.186463 -0.089857 0.843285 0.066 Uiso 1 1 d GR . . . .
N1 N 0.6149(2) 0.2922(2) 0.77640(17) 0.0359(5) Uani 1 1 d . . . . .
N2 N 0.8301(2) 0.33484(18) 0.83106(16) 0.0321(5) Uani 1 1 d . . . . .
N3 N 1.1139(2) 0.69229(19) 0.93306(17) 0.0348(5) Uani 1 1 d . . . . .
N4 N 1.0777(2) 0.86138(19) 0.96604(17) 0.0352(5) Uani 1 1 d . . . . .
N5 N 0.2361(2) 0.3507(2) 0.69971(19) 0.0413(6) Uani 1 1 d . . . . .
N6 N 0.0212(2) 0.3223(2) 0.64281(18) 0.0380(5) Uani 1 1 d . . . . .
N7 N -0.2922(2) -0.02151(19) 0.49113(16) 0.0350(5) Uani 1 1 d . . . . .
N8 N -0.3610(2) -0.18713(19) 0.39080(16) 0.0333(5) Uani 1 1 d . . . . .
C1 C 0.0146(3) 0.0037(3) 0.8109(2) 0.0415(7) Uani 1 1 d . . . . .
C2 C 0.0999(3) 0.0331(3) 0.7548(2) 0.0457(7) Uani 1 1 d . . . . .
H2A H 0.044620 0.022990 0.688801 0.055 Uiso 1 1 calc R . . . .
H2B H 0.141304 0.110009 0.781910 0.055 Uiso 1 1 calc R . . . .
C3 C 0.2042(3) -0.0357(3) 0.7564(2) 0.0439(7) Uani 1 1 d . . . . .
C4 C 0.3290(3) -0.0038(3) 0.8258(2) 0.0430(7) Uani 1 1 d . . . . .
C5 C 0.3675(3) 0.0993(3) 0.9082(2) 0.0449(7) Uani 1 1 d . . . . .
H5A H 0.441376 0.091319 0.959862 0.054 Uiso 1 1 calc R . . . .
H5B H 0.295471 0.105464 0.931483 0.054 Uiso 1 1 calc R . . . .
C6 C 0.4036(3) 0.2063(3) 0.8858(2) 0.0354(6) Uani 1 1 d . . . . .
C8 C 0.5069(10) 0.5806(9) 0.6078(7) 0.046(2) Uani 0.5 1 d . . . A -1
H8C H 0.435796 0.545390 0.547559 0.055 Uiso 0.5 1 calc R . . A -1
H8D H 0.494794 0.654982 0.630876 0.055 Uiso 0.5 1 calc R . . A -1
C9 C 0.6347(6) 0.5841(5) 0.5915(4) 0.0388(12) Uani 0.5 1 d D . . A -1
C14 C 0.7554(9) 0.6589(6) 0.6659(5) 0.060(2) Uani 0.5 1 d D . . A -1
H14 H 0.745418 0.703921 0.719334 0.072 Uiso 0.5 1 calc R . . A -1
C13 C 0.8610(7) 0.6662(6) 0.6633(7) 0.065(2) Uani 0.5 1 d D . . A -1
H13 H 0.932108 0.709262 0.715594 0.078 Uiso 0.5 1 calc R . . A -1
C12 C 0.8799(7) 0.6024(7) 0.5705(7) 0.066(2) Uani 0.5 1 d D . . A -1
H12 H 0.960093 0.612715 0.562386 0.079 Uiso 0.5 1 calc R . . A -1
C11 C 0.7780(8) 0.5334(6) 0.5042(5) 0.0531(18) Uani 0.5 1 d D . . A -1
H11 H 0.789721 0.490711 0.450498 0.064 Uiso 0.5 1 calc R . . A -1
C10 C 0.6492(6) 0.5199(4) 0.5093(4) 0.0381(12) Uani 0.5 1 d D . . A -1
C15 C 0.7158(3) 0.3711(2) 0.8035(2) 0.0346(6) Uani 1 1 d . . . . .
H15 H 0.710005 0.443531 0.803811 0.041 Uiso 1 1 calc R . . . .
C16 C 0.9576(3) 0.3998(2) 0.86690(18) 0.0313(5) Uani 1 1 d . . . . .
C17 C 0.9727(3) 0.5126(2) 0.8795(2) 0.0337(6) Uani 1 1 d . . . . .
H17 H 0.899830 0.545001 0.862083 0.040 Uiso 1 1 calc R . . . .
C18 C 1.0970(3) 0.5761(2) 0.91817(19) 0.0325(5) Uani 1 1 d . . . . .
C19 C 1.0281(3) 0.7570(2) 0.9474(2) 0.0334(5) Uani 1 1 d . . . . .
H19 H 0.944359 0.730983 0.944455 0.040 Uiso 1 1 calc R . . . .
C20 C 1.2015(3) 0.8633(3) 0.9632(2) 0.0436(7) Uani 1 1 d . . . . .
H20 H 1.260170 0.926777 0.973724 0.052 Uiso 1 1 calc R . . . .
C21 C 1.2264(3) 0.7611(3) 0.9433(3) 0.0465(7) Uani 1 1 d . . . . .
H21 H 1.303026 0.740849 0.937636 0.056 Uiso 1 1 calc R . . . .
C22 C 1.2067(3) 0.5288(3) 0.9429(2) 0.0438(7) Uani 1 1 d . . . . .
H22 H 1.290060 0.571987 0.969146 0.053 Uiso 1 1 calc R . . . .
C23 C 1.1897(3) 0.4163(3) 0.9279(3) 0.0490(8) Uani 1 1 d . . . . .
H23 H 1.262882 0.383872 0.943414 0.059 Uiso 1 1 calc R . . . .
C24 C 1.0663(3) 0.3504(3) 0.8902(2) 0.0418(7) Uani 1 1 d . . . . .
H24 H 1.056524 0.274765 0.880606 0.050 Uiso 1 1 calc R . . . .
C25 C 0.7967(3) 0.2235(3) 0.8205(3) 0.0461(7) Uani 1 1 d . . . . .
H25 H 0.853537 0.175194 0.833632 0.055 Uiso 1 1 calc R . . . .
C26 C 0.6649(3) 0.1996(3) 0.7872(2) 0.0467(7) Uani 1 1 d . . . . .
H26 H 0.615200 0.130363 0.773605 0.056 Uiso 1 1 calc R . . . .
C27 C 0.1293(3) 0.2766(3) 0.6618(2) 0.0405(6) Uani 1 1 d . . . . .
H27 H 0.127448 0.201351 0.649330 0.049 Uiso 1 1 calc R . . . .
C28 C -0.1114(3) 0.2646(2) 0.6029(2) 0.0354(6) Uani 1 1 d . . . . .
C29 C -0.1382(3) 0.1514(2) 0.5651(2) 0.0367(6) Uani 1 1 d . . . . .
H29 H -0.070580 0.112937 0.565254 0.044 Uiso 1 1 calc R . . . .
C30 C -0.2669(3) 0.0961(2) 0.52712(19) 0.0356(6) Uani 1 1 d . . . . .
C31 C -0.3502(3) -0.0810(2) 0.39890(19) 0.0349(6) Uani 1 1 d . . . . .
H31 H -0.378827 -0.051255 0.347676 0.042 Uiso 1 1 calc R . . . .
C32 C -0.3061(3) -0.1957(3) 0.4823(2) 0.0389(6) Uani 1 1 d . . . . .
H32 H -0.299975 -0.261456 0.498437 0.047 Uiso 1 1 calc R . . . .
C33 C -0.2625(3) -0.0949(3) 0.5454(2) 0.0426(7) Uani 1 1 d . . . . .
H33 H -0.221053 -0.078118 0.611455 0.051 Uiso 1 1 calc R . . . .
C34 C -0.3686(3) 0.1512(3) 0.5251(2) 0.0429(7) Uani 1 1 d . . . . .
H34 H -0.454564 0.113102 0.499130 0.051 Uiso 1 1 calc R . . . .
C35 C -0.3407(3) 0.2641(3) 0.5624(2) 0.0457(7) Uani 1 1 d . . . . .
H35 H -0.408677 0.302334 0.561187 0.055 Uiso 1 1 calc R . . . .
C36 C -0.2125(3) 0.3213(3) 0.6016(2) 0.0411(6) Uani 1 1 d . . . . .
H36 H -0.194702 0.397310 0.626728 0.049 Uiso 1 1 calc R . . . .
C37 C 0.0647(3) 0.4343(3) 0.6738(3) 0.0516(8) Uani 1 1 d . . . . .
H37 H 0.013603 0.488211 0.671717 0.062 Uiso 1 1 calc R . . . .
C38 C 0.1961(3) 0.4499(3) 0.7078(3) 0.0516(8) Uani 1 1 d . . . . .
H38 H 0.251656 0.518155 0.733012 0.062 Uiso 1 1 calc R . . . .
C39 C 0.4216(4) -0.0705(4) 0.8211(3) 0.0628(10) Uani 1 1 d . . . . .
H39 H 0.505557 -0.048601 0.866778 0.075 Uiso 1 1 calc R . . . .
C40 C 0.3904(6) -0.1683(4) 0.7497(4) 0.0859(15) Uani 1 1 d . . . . .
H40 H 0.452514 -0.212372 0.747934 0.103 Uiso 1 1 calc R . . . .
C41 C 0.2675(6) -0.1997(4) 0.6817(4) 0.0876(16) Uani 1 1 d . . . . .
H41 H 0.245863 -0.265215 0.633262 0.105 Uiso 1 1 calc R . . . .
C42 C 0.1757(5) -0.1340(3) 0.6851(3) 0.0633(10) Uani 1 1 d . . . . .
H42 H 0.092556 -0.156183 0.638393 0.076 Uiso 1 1 calc R . . . .
O9 O 0.6884(4) 0.7266(3) 0.9086(2) 0.0863(10) Uani 1 1 d . . . . .
H9A H 0.620993 0.723235 0.924279 0.129 Uiso 1 1 d G . . . .
H9B H 0.659717 0.694517 0.848830 0.129 Uiso 1 1 d G . . . .
C43 C 0.5374(11) 0.4429(8) 0.4273(6) 0.048(2) Uani 0.5 1 d . . . A -1
H43A H 0.467174 0.426122 0.450173 0.057 Uiso 0.5 1 calc R . . A -1
H43B H 0.565908 0.374659 0.407167 0.057 Uiso 0.5 1 calc R . . A -1
C45 C 0.483(3) 0.485(2) 0.3396(15) 0.038(3) Uani 0.5 1 d . . . . .
C46 C 0.503(3) 0.517(2) 0.6809(16) 0.042(3) Uani 0.5 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
_geom_angle_publ_flag
O1 Ni1 O1 180.0 2_557 . ?
O1 Ni1 O8 88.09(9) . 2_557 ?
O1 Ni1 O8 91.91(9) . . ?
O1 Ni1 O8 91.91(9) 2_557 2_557 ?
O1 Ni1 O8 88.09(9) 2_557 . ?
O1 Ni1 N4 88.67(9) 2_557 2_667 ?
O1 Ni1 N4 91.33(9) . 2_667 ?
O1 Ni1 N4 88.67(9) . 1_445 ?
O1 Ni1 N4 91.33(9) 2_557 1_445 ?
O8 Ni1 O8 180.0 . 2_557 ?
N4 Ni1 O8 87.56(9) 2_667 . ?
N4 Ni1 O8 92.44(9) 2_667 2_557 ?
N4 Ni1 O8 87.56(9) 1_445 2_557 ?
N4 Ni1 O8 92.44(9) 1_445 . ?
N4 Ni1 N4 180.0 2_667 1_445 ?
O3 Ni2 O4 174.62(8) . . ?
O3 Ni2 O6 90.14(9) . . ?
O3 Ni2 N1 88.72(9) . . ?
O3 Ni2 N5 91.57(10) . . ?
O3 Ni2 N8 86.06(9) . 2_556 ?
O4 Ni2 O6 94.98(9) . . ?
O4 Ni2 N5 87.07(10) . . ?
O4 Ni2 N8 88.73(9) . 2_556 ?
N1 Ni2 O4 92.99(9) . . ?
N1 Ni2 O6 89.48(10) . . ?
N1 Ni2 N5 176.11(10) . . ?
N1 Ni2 N8 94.17(9) . 2_556 ?
N5 Ni2 O6 86.64(11) . . ?
N5 Ni2 N8 89.72(10) . 2_556 ?
N8 Ni2 O6 174.66(9) 2_556 . ?
C1 O1 Ni1 125.2(2) . . ?
C6 O3 Ni2 132.6(2) . . ?
C45 O4 Ni2 144.9(10) 2_666 . ?
C46 O4 Ni2 130.1(9) . . ?
C46 O4 C45 17.9(12) . 2_666 ?
C45 O5 C46 18.1(11) . 2_666 ?
C46 O10 C45 11.3(18) . 2_666 ?
Ni2 O6 H6A 110.8 . . ?
Ni2 O6 H6B 110.1 . . ?
H6A O6 H6B 103.3 . . ?
Ni1 O8 H8A 110.4 . . ?
Ni1 O8 H8B 110.1 . . ?
H8A O8 H8B 103.7 . . ?
C15 N1 Ni2 123.1(2) . . ?
C15 N1 C26 105.8(2) . . ?
C26 N1 Ni2 131.0(2) . . ?
C15 N2 C16 126.3(2) . . ?
C15 N2 C25 106.2(2) . . ?
C25 N2 C16 127.5(2) . . ?
C19 N3 C18 126.9(2) . . ?
C19 N3 C21 106.9(2) . . ?
C21 N3 C18 126.0(2) . . ?
C19 N4 Ni1 130.3(2) . 1_665 ?
C19 N4 C20 105.2(2) . . ?
C20 N4 Ni1 124.4(2) . 1_665 ?
C27 N5 Ni2 124.8(2) . . ?
C27 N5 C38 105.5(3) . . ?
C38 N5 Ni2 129.7(2) . . ?
C27 N6 C28 126.3(3) . . ?
C27 N6 C37 106.3(3) . . ?
C37 N6 C28 127.4(3) . . ?
C31 N7 C30 126.5(2) . . ?
C31 N7 C33 107.3(2) . . ?
C33 N7 C30 126.2(2) . . ?
C31 N8 Ni2 128.13(18) . 2_556 ?
C31 N8 C32 105.9(2) . . ?
C32 N8 Ni2 125.53(19) . 2_556 ?
O1 C1 O2 125.7(3) . . ?
O1 C1 C2 116.8(3) . . ?
O2 C1 C2 117.4(3) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C3 C2 C1 112.8(3) . . ?
C3 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
C4 C3 C2 122.6(3) . . ?
C42 C3 C2 119.0(3) . . ?
C42 C3 C4 118.4(3) . . ?
C3 C4 C5 122.2(3) . . ?
C3 C4 C39 119.3(3) . . ?
C39 C4 C5 118.5(3) . . ?
C4 C5 H5A 108.3 . . ?
C4 C5 H5B 108.3 . . ?
C4 C5 C6 115.9(2) . . ?
H5A C5 H5B 107.4 . . ?
C6 C5 H5A 108.3 . . ?
C6 C5 H5B 108.3 . . ?
O3 C6 O7 125.4(3) . . ?
O3 C6 C5 117.5(3) . . ?
O7 C6 C5 117.0(3) . . ?
H8C C8 H8D 108.0 . . ?
C9 C8 H8C 109.4 . . ?
C9 C8 H8D 109.4 . . ?
C9 C8 C46 111.1(12) . . ?
C46 C8 H8C 109.4 . . ?
C46 C8 H8D 109.4 . . ?
C14 C9 C8 119.8(6) . . ?
C10 C9 C8 123.6(6) . . ?
C10 C9 C14 116.6(6) . . ?
C9 C14 H14 116.9 . . ?
C13 C14 C9 126.3(7) . . ?
C13 C14 H14 116.9 . . ?
C14 C13 H13 120.7 . . ?
C14 C13 C12 118.6(7) . . ?
C12 C13 H13 120.7 . . ?
C13 C12 H12 121.4 . . ?
C11 C12 C13 117.2(7) . . ?
C11 C12 H12 121.4 . . ?
C12 C11 H11 118.0 . . ?
C12 C11 C10 124.0(7) . . ?
C10 C11 H11 118.0 . . ?
C9 C10 C11 116.8(6) . . ?
C9 C10 C43 123.2(7) . . ?
C11 C10 C43 120.0(7) . . ?
N1 C15 N2 111.9(2) . . ?
N1 C15 H15 124.1 . . ?
N2 C15 H15 124.1 . . ?
C17 C16 N2 119.7(2) . . ?
C17 C16 C24 120.5(3) . . ?
C24 C16 N2 119.8(3) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 C16 119.4(2) . . ?
C18 C17 H17 120.3 . . ?
C17 C18 N3 120.0(2) . . ?
C17 C18 C22 121.0(3) . . ?
C22 C18 N3 119.0(3) . . ?
N3 C19 H19 124.2 . . ?
N4 C19 N3 111.5(2) . . ?
N4 C19 H19 124.2 . . ?
N4 C20 H20 124.6 . . ?
C21 C20 N4 110.9(3) . . ?
C21 C20 H20 124.6 . . ?
N3 C21 H21 127.3 . . ?
C20 C21 N3 105.5(3) . . ?
C20 C21 H21 127.3 . . ?
C18 C22 H22 120.7 . . ?
C23 C22 C18 118.7(3) . . ?
C23 C22 H22 120.7 . . ?
C22 C23 H23 119.1 . . ?
C22 C23 C24 121.7(3) . . ?
C24 C23 H23 119.1 . . ?
C16 C24 H24 120.7 . . ?
C23 C24 C16 118.6(3) . . ?
C23 C24 H24 120.7 . . ?
N2 C25 H25 127.0 . . ?
C26 C25 N2 106.0(3) . . ?
C26 C25 H25 127.0 . . ?
N1 C26 H26 124.9 . . ?
C25 C26 N1 110.2(3) . . ?
C25 C26 H26 124.9 . . ?
N5 C27 N6 111.9(3) . . ?
N5 C27 H27 124.1 . . ?
N6 C27 H27 124.1 . . ?
C29 C28 N6 119.6(3) . . ?
C36 C28 N6 120.3(3) . . ?
C36 C28 C29 120.1(3) . . ?
C28 C29 H29 120.4 . . ?
C28 C29 C30 119.2(3) . . ?
C30 C29 H29 120.4 . . ?
C29 C30 N7 118.3(3) . . ?
C34 C30 N7 120.2(3) . . ?
C34 C30 C29 121.5(3) . . ?
N7 C31 H31 124.5 . . ?
N8 C31 N7 111.0(2) . . ?
N8 C31 H31 124.5 . . ?
N8 C32 H32 124.9 . . ?
C33 C32 N8 110.2(3) . . ?
C33 C32 H32 124.9 . . ?
N7 C33 H33 127.2 . . ?
C32 C33 N7 105.6(2) . . ?
C32 C33 H33 127.2 . . ?
C30 C34 H34 120.6 . . ?
C30 C34 C35 118.7(3) . . ?
C35 C34 H34 120.6 . . ?
C34 C35 H35 119.6 . . ?
C34 C35 C36 120.9(3) . . ?
C36 C35 H35 119.6 . . ?
C28 C36 C35 119.6(3) . . ?
C28 C36 H36 120.2 . . ?
C35 C36 H36 120.2 . . ?
N6 C37 H37 127.0 . . ?
C38 C37 N6 106.1(3) . . ?
C38 C37 H37 127.0 . . ?
N5 C38 H38 124.9 . . ?
C37 C38 N5 110.2(3) . . ?
C37 C38 H38 124.9 . . ?
C4 C39 H39 119.4 . . ?
C40 C39 C4 121.1(4) . . ?
C40 C39 H39 119.4 . . ?
C39 C40 H40 120.3 . . ?
C41 C40 C39 119.5(4) . . ?
C41 C40 H40 120.3 . . ?
C40 C41 H41 120.1 . . ?
C40 C41 C42 119.9(4) . . ?
C42 C41 H41 120.1 . . ?
C3 C42 H42 119.1 . . ?
C41 C42 C3 121.8(4) . . ?
C41 C42 H42 119.1 . . ?
H9A O9 H9B 104.5 . . ?
C10 C43 H43A 108.4 . . ?
C10 C43 H43B 108.4 . . ?
C10 C43 C45 115.6(12) . . ?
H43A C43 H43B 107.5 . . ?
C45 C43 H43A 108.4 . . ?
C45 C43 H43B 108.4 . . ?
O4 C45 O10 99.7(11) 2_666 2_666 ?
O4 C45 C43 115.7(19) 2_666 . ?
O5 C45 O4 126(2) . 2_666 ?
O5 C45 O10 42.6(8) . 2_666 ?
O5 C45 C43 118.6(16) . . ?
C43 C45 O10 130.8(18) . 2_666 ?
C46 C45 O4 70(7) 2_666 2_666 ?
C46 C45 O5 82(8) 2_666 . ?
C46 C45 O10 39(7) 2_666 2_666 ?
C46 C45 C43 124(9) 2_666 . ?
O4 C46 O5 133(3) . 2_666 ?
O4 C46 O10 122.7(18) . . ?
O4 C46 C8 120.9(17) . . ?
O5 C46 C8 84.8(14) 2_666 . ?
C45 C46 O4 92(7) 2_666 . ?
C45 C46 O5 80(8) 2_666 2_666 ?
C45 C46 O10 129(9) 2_666 . ?
C45 C46 C8 44(7) 2_666 . ?
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 O1 2.068(2) 2_557 ?
Ni1 O1 2.068(2) . ?
Ni1 O8 2.099(2) 2_557 ?
Ni1 O8 2.099(2) . ?
Ni1 N4 2.069(2) 1_445 ?
Ni1 N4 2.069(2) 2_667 ?
Ni2 O3 2.055(2) . ?
Ni2 O4 2.073(2) . ?
Ni2 O6 2.128(2) . ?
Ni2 N1 2.069(2) . ?
Ni2 N5 2.079(3) . ?
Ni2 N8 2.081(2) 2_556 ?
O1 C1 1.247(4) . ?
O2 C1 1.251(4) . ?
O3 C6 1.251(3) . ?
O4 C45 1.27(2) 2_666 ?
O4 C46 1.20(3) . ?
O5 C45 1.24(3) . ?
O5 C46 1.25(3) 2_666 ?
O10 C45 1.54(2) 2_666 ?
O10 C46 1.26(2) . ?
O6 H6A 0.8700 . ?
O6 H6B 0.8685 . ?
O7 C6 1.257(4) . ?
O8 H8A 0.8634 . ?
O8 H8B 0.8634 . ?
N1 C15 1.305(4) . ?
N1 C26 1.374(4) . ?
N2 C15 1.357(3) . ?
N2 C16 1.420(3) . ?
N2 C25 1.387(4) . ?
N3 C18 1.427(4) . ?
N3 C19 1.351(4) . ?
N3 C21 1.386(4) . ?
N4 C19 1.314(4) . ?
N4 C20 1.375(4) . ?
N5 C27 1.302(4) . ?
N5 C38 1.372(4) . ?
N6 C27 1.354(4) . ?
N6 C28 1.430(4) . ?
N6 C37 1.376(4) . ?
N7 C30 1.436(4) . ?
N7 C31 1.346(3) . ?
N7 C33 1.387(4) . ?
N8 C31 1.318(4) . ?
N8 C32 1.375(3) . ?
C1 C2 1.537(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.510(5) . ?
C3 C4 1.391(5) . ?
C3 C42 1.389(5) . ?
C4 C5 1.510(5) . ?
C4 C39 1.398(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.526(4) . ?
C8 H8C 0.9700 . ?
C8 H8D 0.9700 . ?
C8 C9 1.503(12) . ?
C8 C46 1.53(2) . ?
C9 C14 1.498(10) . ?
C9 C10 1.401(8) . ?
C14 H14 0.9300 . ?
C14 C13 1.171(10) . ?
C13 H13 0.9300 . ?
C13 C12 1.555(14) . ?
C12 H12 0.9300 . ?
C12 C11 1.312(10) . ?
C11 H11 0.9300 . ?
C11 C10 1.440(10) . ?
C10 C43 1.501(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.390(4) . ?
C16 C24 1.392(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.384(4) . ?
C18 C22 1.386(4) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C20 C21 1.343(5) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C22 C23 1.382(5) . ?
C23 H23 0.9300 . ?
C23 C24 1.387(5) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C25 C26 1.349(5) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.386(4) . ?
C28 C36 1.383(4) . ?
C29 H29 0.9300 . ?
C29 C30 1.387(4) . ?
C30 C34 1.374(4) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C32 C33 1.348(4) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C34 C35 1.382(5) . ?
C35 H35 0.9300 . ?
C35 C36 1.389(4) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C37 C38 1.346(5) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C39 C40 1.383(7) . ?
C40 H40 0.9300 . ?
C40 C41 1.368(8) . ?
C41 H41 0.9300 . ?
C41 C42 1.380(7) . ?
C42 H42 0.9300 . ?
O9 H9A 0.8500 . ?
O9 H9B 0.8501 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 C45 1.53(3) . ?
C45 C46 0.39(2) 2_666 ?
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
Ni1 O1 C1 O2 21.1(5) . . . . ?
Ni1 O1 C1 C2 -157.8(2) . . . . ?
Ni1 N4 C19 N3 -176.98(19) 1_665 . . . ?
Ni1 N4 C20 C21 177.2(2) 1_665 . . . ?
Ni2 O3 C6 O7 8.6(5) . . . . ?
Ni2 O3 C6 C5 -173.1(2) . . . . ?
Ni2 O4 C46 O5 72.4(19) . . . 2_666 ?
Ni2 O4 C46 O10 10(4) . . . . ?
Ni2 O4 C46 C8 -173.5(10) . . . . ?
Ni2 O4 C46 C45 151(8) . . . 2_666 ?
Ni2 N1 C15 N2 177.76(18) . . . . ?
Ni2 N1 C26 C25 -177.4(2) . . . . ?
Ni2 N5 C27 N6 -176.9(2) . . . . ?
Ni2 N5 C38 C37 177.6(3) . . . . ?
Ni2 N8 C31 N7 -173.04(18) 2_556 . . . ?
Ni2 N8 C32 C33 172.8(2) 2_556 . . . ?
O1 C1 C2 C3 89.6(4) . . . . ?
O2 C1 C2 C3 -89.4(4) . . . . ?
N2 C16 C17 C18 177.3(2) . . . . ?
N2 C16 C24 C23 -178.0(3) . . . . ?
N2 C25 C26 N1 0.2(4) . . . . ?
N3 C18 C22 C23 -179.7(3) . . . . ?
N4 C20 C21 N3 0.1(4) . . . . ?
N6 C28 C29 C30 179.6(3) . . . . ?
N6 C28 C36 C35 179.9(3) . . . . ?
N6 C37 C38 N5 -0.6(4) . . . . ?
N7 C30 C34 C35 178.5(3) . . . . ?
N8 C32 C33 N7 0.5(4) . . . . ?
C1 C2 C3 C4 -91.1(4) . . . . ?
C1 C2 C3 C42 89.8(4) . . . . ?
C2 C3 C4 C5 3.4(4) . . . . ?
C2 C3 C4 C39 -178.2(3) . . . . ?
C2 C3 C42 C41 178.9(4) . . . . ?
C3 C4 C5 C6 -81.0(4) . . . . ?
C3 C4 C39 C40 -1.2(6) . . . . ?
C4 C3 C42 C41 -0.2(6) . . . . ?
C4 C5 C6 O3 10.8(4) . . . . ?
C4 C5 C6 O7 -170.9(3) . . . . ?
C4 C39 C40 C41 1.0(7) . . . . ?
C5 C4 C39 C40 177.2(4) . . . . ?
C8 C9 C14 C13 177.1(9) . . . . ?
C8 C9 C10 C11 179.5(6) . . . . ?
C8 C9 C10 C43 1.8(8) . . . . ?
C9 C8 C46 O4 -92(2) . . . . ?
C9 C8 C46 O5 45.2(14) . . . 2_666 ?
C9 C8 C46 C45 -36(11) . . . 2_666 ?
C9 C14 C13 C12 6.7(12) . . . . ?
C9 C10 C43 C45 101.5(12) . . . . ?
C14 C9 C10 C11 -0.8(8) . . . . ?
C14 C9 C10 C43 -178.5(6) . . . . ?
C14 C13 C12 C11 -7.8(11) . . . . ?
C13 C12 C11 C10 4.8(10) . . . . ?
C12 C11 C10 C9 -0.9(9) . . . . ?
C12 C11 C10 C43 176.9(7) . . . . ?
C11 C10 C43 C45 -76.1(13) . . . . ?
C10 C9 C14 C13 -2.6(11) . . . . ?
C10 C43 C45 O4 3(2) . . . 2_666 ?
C10 C43 C45 O5 -175.5(14) . . . . ?
C10 C43 C45 C46 85(10) . . . 2_666 ?
C15 N1 C26 C25 -0.4(4) . . . . ?
C15 N2 C16 C17 2.4(4) . . . . ?
C15 N2 C16 C24 -178.4(3) . . . . ?
C15 N2 C25 C26 0.1(4) . . . . ?
C16 N2 C15 N1 -178.1(2) . . . . ?
C16 N2 C25 C26 177.9(3) . . . . ?
C16 C17 C18 N3 -178.9(2) . . . . ?
C16 C17 C18 C22 1.2(4) . . . . ?
C17 C16 C24 C23 1.3(5) . . . . ?
C17 C18 C22 C23 0.3(5) . . . . ?
C18 N3 C19 N4 175.1(3) . . . . ?
C18 N3 C21 C20 -175.3(3) . . . . ?
C18 C22 C23 C24 -1.0(5) . . . . ?
C19 N3 C18 C17 26.1(4) . . . . ?
C19 N3 C18 C22 -153.9(3) . . . . ?
C19 N3 C21 C20 0.0(4) . . . . ?
C19 N4 C20 C21 -0.1(4) . . . . ?
C20 N4 C19 N3 0.1(3) . . . . ?
C21 N3 C18 C17 -159.5(3) . . . . ?
C21 N3 C18 C22 20.4(4) . . . . ?
C21 N3 C19 N4 -0.1(3) . . . . ?
C22 C23 C24 C16 0.2(5) . . . . ?
C24 C16 C17 C18 -1.9(4) . . . . ?
C25 N2 C15 N1 -0.3(3) . . . . ?
C25 N2 C16 C17 -175.0(3) . . . . ?
C25 N2 C16 C24 4.3(4) . . . . ?
C26 N1 C15 N2 0.4(3) . . . . ?
C27 N5 C38 C37 -0.4(4) . . . . ?
C27 N6 C28 C29 -10.9(4) . . . . ?
C27 N6 C28 C36 169.4(3) . . . . ?
C27 N6 C37 C38 1.3(4) . . . . ?
C28 N6 C27 N5 -178.8(3) . . . . ?
C28 N6 C37 C38 178.4(3) . . . . ?
C28 C29 C30 N7 -178.0(3) . . . . ?
C28 C29 C30 C34 0.7(4) . . . . ?
C29 C28 C36 C35 0.2(5) . . . . ?
C29 C30 C34 C35 -0.3(5) . . . . ?
C30 N7 C31 N8 -178.6(3) . . . . ?
C30 N7 C33 C32 178.6(3) . . . . ?
C30 C34 C35 C36 -0.2(5) . . . . ?
C31 N7 C30 C29 -111.7(3) . . . . ?
C31 N7 C30 C34 69.5(4) . . . . ?
C31 N7 C33 C32 -0.8(3) . . . . ?
C31 N8 C32 C33 0.1(3) . . . . ?
C32 N8 C31 N7 -0.6(3) . . . . ?
C33 N7 C30 C29 69.0(4) . . . . ?
C33 N7 C30 C34 -109.8(3) . . . . ?
C33 N7 C31 N8 0.9(3) . . . . ?
C34 C35 C36 C28 0.3(5) . . . . ?
C36 C28 C29 C30 -0.7(4) . . . . ?
C37 N6 C27 N5 -1.6(4) . . . . ?
C37 N6 C28 C29 172.5(3) . . . . ?
C37 N6 C28 C36 -7.2(5) . . . . ?
C38 N5 C27 N6 1.3(4) . . . . ?
C39 C4 C5 C6 100.6(4) . . . . ?
C39 C40 C41 C42 -0.3(8) . . . . ?
C40 C41 C42 C3 -0.1(7) . . . . ?
C42 C3 C4 C5 -177.6(3) . . . . ?
C42 C3 C4 C39 0.8(5) . . . . ?
C45 O4 C46 O5 -79(9) 2_666 . . 2_666 ?
C45 O4 C46 O10 -141(11) 2_666 . . . ?
C45 O4 C46 C8 35(7) 2_666 . . . ?
C45 O10 C46 O4 126(14) 2_666 . . . ?
C46 O5 C45 O4 58(7) 2_666 . . 2_666 ?
C46 O5 C45 C43 -124(9) 2_666 . . . ?
C46 C8 C9 C14 -75.0(13) . . . . ?
C46 C8 C9 C10 104.7(12) . . . . ?
