#------------------------------------------------------------------------------
#$Date: 2021-06-05 21:52:02 +0300 (Sat, 05 Jun 2021) $
#$Revision: 266078 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/67/7706749.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_7706749
loop_
_publ_author_name
'Suzuki, Takashi'
'Sato, Akari'
'Oshita, Hiromi'
'Yajima, Tatsuo'
'Tani, Fumito'
'Abe, Hitoshi'
'Mieda-Higa, Kaoru'
'Yanagisawa, Sachiko'
'Ogura, Takashi'
'Shimazaki, Yuichi'
_publ_section_title
;
 Formation of Ni(II)-phenoxyl radical complexes by O₂: a
 mechanistic insight into the reaction of Ni(II)-phenol complexes with
 O₂.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5161
_journal_page_last               5170
_journal_paper_doi               10.1039/d1dt00105a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C40 H58 Cl N2 Ni O10'
_chemical_formula_sum            'C40 H58 Cl N2 Ni O10'
_chemical_formula_weight         821.06
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-01-05 deposited with the CCDC.	2021-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                63.7131(18)
_cell_angle_beta                 71.4309(18)
_cell_angle_gamma                68.2716(15)
_cell_formula_units_Z            2
_cell_length_a                   11.4551(7)
_cell_length_b                   14.5863(9)
_cell_length_c                   15.9271(11)
_cell_measurement_reflns_used    16294
_cell_measurement_temperature    133
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.54
_cell_volume                     2178.0(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2.4'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      133
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21129
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         2.541
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             874.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.87
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9718
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0935P)²+2.7010P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7106
_reflns_number_total             9718
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            d1dt00105a2.cif
_cod_data_source_block           120808
_cod_depositor_comments
'Adding full bibliography for 7706749--7706752.cif.'
_cod_database_code               7706749
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -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 0.34260(3) 0.74442(3) 0.59506(3) 0.01905(13) Uani 1 1 d . . . . .
Cl1 Cl -0.24922(10) 0.72467(10) 0.67343(8) 0.0495(3) Uani 1 1 d . . . . .
O1 O 0.3385(2) 0.72484(17) 0.74205(16) 0.0217(5) Uani 1 1 d D . . . .
H1 H 0.397(4) 0.659(3) 0.767(4) 0.078(18) Uiso 1 1 d D . . . .
O2 O 0.3803(2) 0.74106(18) 0.46747(16) 0.0232(5) Uani 1 1 d . . . . .
O3 O 0.4828(2) 0.8224(2) 0.55966(18) 0.0287(5) Uani 1 1 d D . . . .
H6 H 0.524(5) 0.782(4) 0.611(3) 0.09(2) Uiso 1 1 d D . . . .
O4 O 0.4842(2) 0.59560(18) 0.63548(18) 0.0290(5) Uani 1 1 d D . . . .
H9 H 0.507(4) 0.573(3) 0.694(2) 0.047(13) Uiso 1 1 d D . . . .
O5 O 0.4979(3) 0.5342(2) 0.8248(3) 0.0499(8) Uani 1 1 d D . . . .
H2 H 0.560(5) 0.544(5) 0.844(5) 0.09(2) Uiso 1 1 d D . . . .
O6 O 0.6648(3) 0.5450(3) 0.9044(3) 0.0619(9) Uani 1 1 d D . . . .
O7 O -0.1874(3) 0.6666(3) 0.7551(2) 0.0686(11) Uani 1 1 d . . . . .
O8 O -0.2758(5) 0.8355(3) 0.6525(4) 0.0851(13) Uani 1 1 d . . . . .
O9 O -0.3642(3) 0.6962(3) 0.6961(3) 0.0637(10) Uani 1 1 d . . . . .
O10 O -0.1677(3) 0.6985(3) 0.5939(3) 0.0651(10) Uani 1 1 d . . . . .
N1 N 0.1966(2) 0.8823(2) 0.58117(19) 0.0201(5) Uani 1 1 d . . . . .
N2 N 0.1900(2) 0.67698(19) 0.64584(18) 0.0174(5) Uani 1 1 d . . . . .
C1 C 0.2208(3) 0.7347(2) 0.8040(2) 0.0201(6) Uani 1 1 d . . . . .
C2 C 0.1851(3) 0.7989(2) 0.8574(2) 0.0210(6) Uani 1 1 d . . . . .
C3 C 0.0620(3) 0.8066(2) 0.9145(2) 0.0223(6) Uani 1 1 d . . . . .
H3 H 0.0344 0.8505 0.9507 0.027 Uiso 1 1 calc R U . . .
C4 C -0.0216(3) 0.7535(3) 0.9209(2) 0.0229(6) Uani 1 1 d . . . . .
C5 C 0.0203(3) 0.6890(2) 0.8679(2) 0.0217(6) Uani 1 1 d . . . . .
H5 H -0.0340 0.6508 0.8719 0.026 Uiso 1 1 calc R U . . .
C6 C 0.1404(3) 0.6795(2) 0.8091(2) 0.0204(6) Uani 1 1 d . . . . .
C7 C 0.1813(3) 0.6120(2) 0.7496(2) 0.0206(6) Uani 1 1 d . . . . .
H7A H 0.2657 0.5612 0.7613 0.025 Uiso 1 1 calc R U . . .
H7B H 0.1191 0.5705 0.7697 0.025 Uiso 1 1 calc R U . . .
C8 C 0.0686(3) 0.7615(2) 0.6281(2) 0.0190(6) Uani 1 1 d . . . . .
H8A H -0.0009 0.7412 0.6825 0.023 Uiso 1 1 calc R U . . .
H8B H 0.0462 0.7679 0.5703 0.023 Uiso 1 1 calc R U . . .
C9 C 0.0785(3) 0.8672(2) 0.6152(2) 0.0195(6) Uani 1 1 d . . . . .
C10 C -0.0284(3) 0.9469(3) 0.6306(2) 0.0245(7) Uani 1 1 d . . . . .
H10 H -0.1101 0.9335 0.6572 0.029 Uiso 1 1 calc R U . . .
C11 C -0.0149(3) 1.0464(3) 0.6070(3) 0.0288(7) Uani 1 1 d . . . . .
H11 H -0.0871 1.1019 0.6174 0.035 Uiso 1 1 calc R U . . .
C12 C 0.1051(3) 1.0640(3) 0.5680(3) 0.0276(7) Uani 1 1 d . . . . .
H12 H 0.1164 1.1322 0.5491 0.033 Uiso 1 1 calc R U . . .
C13 C 0.2089(3) 0.9793(2) 0.5572(2) 0.0248(7) Uani 1 1 d . . . . .
H13 H 0.2916 0.9907 0.5318 0.030 Uiso 1 1 calc R U . . .
C14 C 0.2167(3) 0.6054(2) 0.5935(2) 0.0214(6) Uani 1 1 d . . . . .
H14A H 0.1509 0.5658 0.6214 0.026 Uiso 1 1 calc R U . . .
H14B H 0.3007 0.5529 0.6031 0.026 Uiso 1 1 calc R U . . .
C15 C 0.2179(3) 0.6631(2) 0.4877(2) 0.0212(6) Uani 1 1 d . . . . .
C16 C 0.3068(3) 0.7237(2) 0.4297(2) 0.0214(6) Uani 1 1 d . . . . .
C17 C 0.3162(3) 0.7636(2) 0.3284(2) 0.0235(6) Uani 1 1 d . . . . .
C18 C 0.2326(3) 0.7462(3) 0.2932(2) 0.0269(7) Uani 1 1 d . . . . .
H18 H 0.2392 0.7726 0.2260 0.032 Uiso 1 1 calc R U . . .
C19 C 0.1398(3) 0.6923(3) 0.3505(3) 0.0259(7) Uani 1 1 d . . . . .
C20 C 0.1349(3) 0.6504(2) 0.4480(2) 0.0242(7) Uani 1 1 d . . . . .
H20 H 0.0737 0.6123 0.4889 0.029 Uiso 1 1 calc R U . . .
C21 C 0.2740(3) 0.8575(3) 0.8568(2) 0.0259(7) Uani 1 1 d . . . . .
C22 C 0.3091(4) 0.9365(3) 0.7555(3) 0.0349(8) Uani 1 1 d . . . . .
H22A H 0.3497 0.8984 0.7116 0.042 Uiso 1 1 calc R U . . .
H22B H 0.2314 0.9907 0.7350 0.042 Uiso 1 1 calc R U . . .
H22C H 0.3685 0.9705 0.7556 0.042 Uiso 1 1 calc R U . . .
C23 C 0.3962(4) 0.7763(3) 0.8924(3) 0.0376(9) Uani 1 1 d . . . . .
H23A H 0.4392 0.7342 0.8519 0.045 Uiso 1 1 calc R U . . .
H23B H 0.4536 0.8139 0.8895 0.045 Uiso 1 1 calc R U . . .
H23C H 0.3737 0.7293 0.9583 0.045 Uiso 1 1 calc R U . . .
C24 C 0.2109(4) 0.9211(3) 0.9226(3) 0.0381(9) Uani 1 1 d . . . . .
H24A H 0.1324 0.9738 0.9019 0.046 Uiso 1 1 calc R U . . .
H24B H 0.1901 0.8727 0.9882 0.046 Uiso 1 1 calc R U . . .
H24C H 0.2701 0.9573 0.9195 0.046 Uiso 1 1 calc R U . . .
C25 C -0.1548(3) 0.7616(3) 0.9859(2) 0.0265(7) Uani 1 1 d . . . . .
C26 C -0.1508(4) 0.6566(3) 1.0718(3) 0.0369(8) Uani 1 1 d . . . . .
H26A H -0.0855 0.6432 1.1064 0.044 Uiso 1 1 calc R U . . .
H26B H -0.2345 0.6609 1.1143 0.044 Uiso 1 1 calc R U . . .
H26C H -0.1299 0.5985 1.0496 0.044 Uiso 1 1 calc R U . . .
C27 C -0.1939(3) 0.8528(3) 1.0217(3) 0.0358(8) Uani 1 1 d . . . . .
H27A H -0.1302 0.8418 1.0566 0.043 Uiso 1 1 calc R U . . .
H27B H -0.1990 0.9204 0.9673 0.043 Uiso 1 1 calc R U . . .
H27C H -0.2776 0.8543 1.0642 0.043 Uiso 1 1 calc R U . . .
C28 C -0.2570(3) 0.7823(4) 0.9320(3) 0.0377(9) Uani 1 1 d . . . . .
H28A H -0.2597 0.8494 0.8770 0.045 Uiso 1 1 calc R U . . .
H28B H -0.2360 0.7241 0.9099 0.045 Uiso 1 1 calc R U . . .
H28C H -0.3406 0.7866 0.9745 0.045 Uiso 1 1 calc R U . . .
C29 C 0.4142(3) 0.8258(3) 0.2618(2) 0.0301(7) Uani 1 1 d . . . . .
C30 C 0.3813(4) 0.9290(3) 0.2794(3) 0.0362(8) Uani 1 1 d . . . . .
H30A H 0.4437 0.9690 0.2369 0.043 Uiso 1 1 calc R U . . .
H30B H 0.2955 0.9721 0.2666 0.043 Uiso 1 1 calc R U . . .
H30C H 0.3838 0.9116 0.3458 0.043 Uiso 1 1 calc R U . . .
C31 C 0.5504(3) 0.7567(3) 0.2788(3) 0.0375(9) Uani 1 1 d . . . . .
H31A H 0.6125 0.7970 0.2361 0.045 Uiso 1 1 calc R U . . .
H31B H 0.5556 0.7371 0.3451 0.045 Uiso 1 1 calc R U . . .
H31C H 0.5694 0.6923 0.2661 0.045 Uiso 1 1 calc R U . . .
C32 C 0.4136(4) 0.8585(4) 0.1558(3) 0.0411(9) Uani 1 1 d . . . . .
H32A H 0.4775 0.8978 0.1163 0.049 Uiso 1 1 calc R U . . .
H32B H 0.4341 0.7947 0.1416 0.049 Uiso 1 1 calc R U . . .
H32C H 0.3287 0.9036 0.1420 0.049 Uiso 1 1 calc R U . . .
C33 C 0.0496(4) 0.6771(3) 0.3059(3) 0.0342(8) Uani 1 1 d . . . . .
C34 C -0.0297(11) 0.7935(8) 0.2485(8) 0.061(3) Uani 0.5 1 d . . P . .
C35 C 0.0658(10) 0.7393(8) 0.1969(7) 0.051(2) Uani 0.5 1 d . . P . .
C36 C 0.1235(11) 0.6225(12) 0.2366(11) 0.079(4) Uani 0.5 1 d . . P . .
C37 C 0.0964(8) 0.5553(7) 0.3183(7) 0.0409(19) Uani 0.5 1 d . . P . .
C38 C -0.0541(14) 0.6218(12) 0.3834(9) 0.075(4) Uani 0.5 1 d . . P . .
C39 C -0.0846(8) 0.7020(11) 0.3566(9) 0.056(3) Uani 0.5 1 d . . P . .
C40 C 0.5662(4) 0.8528(4) 0.4695(3) 0.0477(11) Uani 1 1 d . . . . .
H40A H 0.6223 0.8879 0.4723 0.057 Uiso 1 1 calc R U . . .
H40B H 0.6182 0.7895 0.4546 0.057 Uiso 1 1 calc R U . . .
H40C H 0.5152 0.9017 0.4199 0.057 Uiso 1 1 calc R U . . .
C41 C 0.5856(4) 0.5536(3) 0.5715(3) 0.0415(9) Uani 1 1 d . . . . .
H41A H 0.6370 0.4844 0.6079 0.050 Uiso 1 1 calc R U . . .
H41B H 0.5497 0.5451 0.5280 0.050 Uiso 1 1 calc R U . . .
H41C H 0.6397 0.6024 0.5347 0.050 Uiso 1 1 calc R U . . .
C42 C 0.4855(6) 0.4307(4) 0.8683(4) 0.0671(16) Uani 1 1 d D . . . .
H42A H 0.5693 0.3808 0.8590 0.080 Uiso 1 1 calc DR U . . .
H42B H 0.4261 0.4241 0.8399 0.080 Uiso 1 1 calc DR U . . .
H42C H 0.4524 0.4146 0.9367 0.080 Uiso 1 1 calc DR U . . .
C43 C 0.7603(7) 0.4663(5) 0.9526(5) 0.0787(19) Uani 1 1 d D . . . .
H43A H 0.8214 0.4986 0.9531 0.094 Uiso 1 1 calc DR U . . .
H43B H 0.8049 0.4155 0.9205 0.094 Uiso 1 1 calc DR U . . .
H43C H 0.7221 0.4293 1.0183 0.094 Uiso 1 1 calc DR U . . .
H4 H 0.7198 0.5870 0.8460 0.024 Uiso 1 1 d D U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(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
O2 Ni1 N1 101.05(10) . . ?
O2 Ni1 N2 95.14(9) . . ?
N1 Ni1 N2 82.19(10) . . ?
O2 Ni1 O3 92.68(10) . . ?
N1 Ni1 O3 92.77(10) . . ?
N2 Ni1 O3 171.38(10) . . ?
O2 Ni1 O4 88.62(9) . . ?
N1 Ni1 O4 170.04(10) . . ?
N2 Ni1 O4 94.68(10) . . ?
O3 Ni1 O4 89.12(10) . . ?
O2 Ni1 O1 168.39(9) . . ?
N1 Ni1 O1 90.03(9) . . ?
N2 Ni1 O1 89.74(9) . . ?
O3 Ni1 O1 83.25(9) . . ?
O4 Ni1 O1 80.48(9) . . ?
O9 Cl1 O10 109.5(2) . . ?
O9 Cl1 O8 110.5(3) . . ?
O10 Cl1 O8 110.2(3) . . ?
O9 Cl1 O7 108.4(2) . . ?
O10 Cl1 O7 109.9(2) . . ?
O8 Cl1 O7 108.3(3) . . ?
C1 O1 Ni1 118.53(17) . . ?
C1 O1 H1 112(4) . . ?
Ni1 O1 H1 106(4) . . ?
C16 O2 Ni1 126.8(2) . . ?
C40 O3 Ni1 126.2(2) . . ?
C40 O3 H6 115(4) . . ?
Ni1 O3 H6 101(4) . . ?
C41 O4 Ni1 125.5(2) . . ?
C41 O4 H9 111(3) . . ?
Ni1 O4 H9 116(3) . . ?
C42 O5 H2 114(4) . . ?
C43 O6 H4 99.6 . . ?
C13 N1 C9 118.5(3) . . ?
C13 N1 Ni1 126.4(2) . . ?
C9 N1 Ni1 114.2(2) . . ?
C8 N2 C7 110.0(2) . . ?
C8 N2 C14 110.6(2) . . ?
C7 N2 C14 108.7(2) . . ?
C8 N2 Ni1 110.06(17) . . ?
C7 N2 Ni1 110.49(17) . . ?
C14 N2 Ni1 107.00(18) . . ?
C6 C1 O1 117.1(3) . . ?
C6 C1 C2 121.9(3) . . ?
O1 C1 C2 121.0(3) . . ?
C1 C2 C3 116.1(3) . . ?
C1 C2 C21 123.3(3) . . ?
C3 C2 C21 120.6(3) . . ?
C4 C3 C2 123.7(3) . . ?
C4 C3 H3 118.1 . . ?
C2 C3 H3 118.1 . . ?
C5 C4 C3 117.5(3) . . ?
C5 C4 C25 119.9(3) . . ?
C3 C4 C25 122.5(3) . . ?
C4 C5 C6 121.3(3) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 119.4(3) . . ?
C5 C6 C7 120.0(3) . . ?
C1 C6 C7 120.5(3) . . ?
N2 C7 C6 112.3(2) . . ?
N2 C7 H7A 109.1 . . ?
C6 C7 H7A 109.1 . . ?
N2 C7 H7B 109.1 . . ?
C6 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
N2 C8 C9 112.0(2) . . ?
N2 C8 H8A 109.2 . . ?
C9 C8 H8A 109.2 . . ?
N2 C8 H8B 109.2 . . ?
C9 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
N1 C9 C10 121.9(3) . . ?
N1 C9 C8 115.9(3) . . ?
C10 C9 C8 122.0(3) . . ?
C11 C10 C9 119.3(3) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C12 119.2(3) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
C11 C12 C13 118.4(3) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
N1 C13 C12 122.6(3) . . ?
N1 C13 H13 118.7 . . ?
C12 C13 H13 118.7 . . ?
N2 C14 C15 114.0(2) . . ?
N2 C14 H14A 108.8 . . ?
C15 C14 H14A 108.8 . . ?
N2 C14 H14B 108.8 . . ?
C15 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
C20 C15 C16 121.1(3) . . ?
C20 C15 C14 118.5(3) . . ?
C16 C15 C14 120.3(3) . . ?
O2 C16 C15 121.3(3) . . ?
O2 C16 C17 121.1(3) . . ?
C15 C16 C17 117.6(3) . . ?
C18 C17 C16 118.3(3) . . ?
C18 C17 C29 121.6(3) . . ?
C16 C17 C29 120.1(3) . . ?
C17 C18 C19 123.9(3) . . ?
C17 C18 H18 118.0 . . ?
C19 C18 H18 118.0 . . ?
C20 C19 C18 117.3(3) . . ?
C20 C19 C33 121.8(3) . . ?
C18 C19 C33 120.8(3) . . ?
C19 C20 C15 121.5(3) . . ?
C19 C20 H20 119.2 . . ?
C15 C20 H20 119.2 . . ?
C24 C21 C23 107.2(3) . . ?
C24 C21 C22 107.3(3) . . ?
C23 C21 C22 109.9(3) . . ?
C24 C21 C2 112.3(3) . . ?
C23 C21 C2 109.7(3) . . ?
C22 C21 C2 110.4(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C28 C25 C26 109.3(3) . . ?
C28 C25 C27 107.5(3) . . ?
C26 C25 C27 109.0(3) . . ?
C28 C25 C4 110.7(3) . . ?
C26 C25 C4 108.5(3) . . ?
C27 C25 C4 111.6(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C17 C29 C30 109.2(3) . . ?
C17 C29 C32 112.6(3) . . ?
C30 C29 C32 106.9(3) . . ?
C17 C29 C31 109.9(3) . . ?
C30 C29 C31 111.1(3) . . ?
C32 C29 C31 107.1(3) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C39 C33 C36 136.5(6) . . ?
C39 C33 C35 113.2(7) . . ?
C36 C33 C35 58.4(7) . . ?
C39 C33 C19 110.7(4) . . ?
C36 C33 C19 111.5(5) . . ?
C35 C33 C19 111.9(4) . . ?
C39 C33 C38 38.4(6) . . ?
C36 C33 C38 112.9(9) . . ?
C35 C33 C38 134.3(5) . . ?
C19 C33 C38 112.4(5) . . ?
C39 C33 C37 109.4(7) . . ?
C36 C33 C37 48.0(7) . . ?
C35 C33 C37 104.9(6) . . ?
C19 C33 C37 106.3(4) . . ?
C38 C33 C37 72.5(7) . . ?
C39 C33 C34 68.7(7) . . ?
C36 C33 C34 108.1(8) . . ?
C35 C33 C34 51.4(6) . . ?
C19 C33 C34 106.4(4) . . ?
C38 C33 C34 105.0(8) . . ?
C37 C33 C34 145.3(5) . . ?
C35 C34 C33 62.4(6) . . ?
C35 C34 C39 108.5(8) . . ?
C33 C34 C39 52.5(5) . . ?
C34 C35 C36 123.2(10) . . ?
C34 C35 C33 66.2(6) . . ?
C36 C35 C33 59.2(6) . . ?
C37 C36 C35 129.8(11) . . ?
C37 C36 C33 69.9(8) . . ?
C35 C36 C33 62.4(6) . . ?
C36 C37 C33 62.2(6) . . ?
C36 C37 C38 108.2(8) . . ?
C33 C37 C38 53.3(5) . . ?
C39 C38 C33 65.9(9) . . ?
C39 C38 C37 118.2(13) . . ?
C33 C38 C37 54.2(6) . . ?
C38 C39 C33 75.7(10) . . ?
C38 C39 C34 130.3(13) . . ?
C33 C39 C34 58.7(6) . . ?
O3 C40 H40A 109.5 . . ?
O3 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
O3 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O4 C41 H41A 109.5 . . ?
O4 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O4 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O5 C42 H42A 109.5 . . ?
O5 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
O5 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O6 C43 H43A 109.5 . . ?
O6 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O6 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
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 O2 1.958(2) . ?
Ni1 N1 2.059(2) . ?
Ni1 N2 2.085(2) . ?
Ni1 O3 2.097(2) . ?
Ni1 O4 2.140(2) . ?
Ni1 O1 2.216(2) . ?
Cl1 O9 1.416(3) . ?
Cl1 O10 1.426(4) . ?
Cl1 O8 1.429(4) . ?
Cl1 O7 1.441(3) . ?
O1 C1 1.395(4) . ?
O1 H1 0.94(2) . ?
O2 C16 1.324(4) . ?
O3 C40 1.431(5) . ?
O3 H6 0.93(2) . ?
O4 C41 1.426(4) . ?
O4 H9 0.927(19) . ?
O5 C42 1.395(6) . ?
O5 H2 0.94(2) . ?
O6 C43 1.389(6) . ?
O6 H4 1.0223 . ?
N1 C13 1.343(4) . ?
N1 C9 1.350(4) . ?
N2 C8 1.485(4) . ?
N2 C7 1.489(4) . ?
N2 C14 1.501(4) . ?
C1 C6 1.395(4) . ?
C1 C2 1.403(4) . ?
C2 C3 1.409(4) . ?
C2 C21 1.548(4) . ?
C3 C4 1.394(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(5) . ?
C4 C25 1.543(4) . ?
C5 C6 1.393(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.513(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.505(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.386(4) . ?
C10 C11 1.385(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.385(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.512(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.397(4) . ?
C15 C16 1.420(5) . ?
C16 C17 1.433(4) . ?
C17 C18 1.395(5) . ?
C17 C29 1.535(5) . ?
C18 C19 1.395(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.385(5) . ?
C19 C33 1.548(5) . ?
C20 H20 0.9500 . ?
C21 C24 1.537(5) . ?
C21 C23 1.538(5) . ?
C21 C22 1.541(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C28 1.532(5) . ?
C25 C26 1.534(5) . ?
C25 C27 1.538(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.540(5) . ?
C29 C32 1.540(5) . ?
C29 C31 1.544(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C39 1.484(10) . ?
C33 C36 1.501(11) . ?
C33 C35 1.548(10) . ?
C33 C38 1.575(12) . ?
C33 C37 1.593(9) . ?
C33 C34 1.598(9) . ?
C34 C35 1.364(16) . ?
C34 C39 1.742(18) . ?
C35 C36 1.488(17) . ?
C36 C37 1.260(17) . ?
C37 C38 1.87(2) . ?
C38 C39 1.010(15) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1 O5 . . . 2.708(3) 0.943 1.768 174.5 no
O3 H6 O9 . . 1_655 2.771(4) 0.928 1.856 168.2 no
O4 H9 O5 . . . 2.779(5) 0.927 1.884 161.7 no
O5 H2 O6 . . . 2.690(7) 0.935 1.769 167.5 no
O5 H2 O9 . . 1_655 2.949(5) 0.935 2.589 103.4 no
O6 H4 O7 . . 1_655 2.755(5) 1.022(3) 1.737(4) 173.1(4) no
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 C6 47.6(3) . . . . ?
Ni1 O1 C1 C2 -131.5(2) . . . . ?
C6 C1 C2 C3 -1.7(4) . . . . ?
O1 C1 C2 C3 177.4(3) . . . . ?
C6 C1 C2 C21 177.3(3) . . . . ?
O1 C1 C2 C21 -3.6(4) . . . . ?
C1 C2 C3 C4 1.1(4) . . . . ?
C21 C2 C3 C4 -177.9(3) . . . . ?
C2 C3 C4 C5 0.3(5) . . . . ?
C2 C3 C4 C25 178.6(3) . . . . ?
C3 C4 C5 C6 -1.2(5) . . . . ?
C25 C4 C5 C6 -179.6(3) . . . . ?
C4 C5 C6 C1 0.7(5) . . . . ?
C4 C5 C6 C7 -177.7(3) . . . . ?
O1 C1 C6 C5 -178.2(3) . . . . ?
C2 C1 C6 C5 0.9(4) . . . . ?
O1 C1 C6 C7 0.2(4) . . . . ?
C2 C1 C6 C7 179.3(3) . . . . ?
C8 N2 C7 C6 -52.7(3) . . . . ?
C14 N2 C7 C6 -173.8(2) . . . . ?
Ni1 N2 C7 C6 69.1(3) . . . . ?
C5 C6 C7 N2 110.8(3) . . . . ?
C1 C6 C7 N2 -67.6(4) . . . . ?
C7 N2 C8 C9 100.1(3) . . . . ?
C14 N2 C8 C9 -139.9(3) . . . . ?
Ni1 N2 C8 C9 -21.9(3) . . . . ?
C13 N1 C9 C10 -3.6(5) . . . . ?
Ni1 N1 C9 C10 165.9(2) . . . . ?
C13 N1 C9 C8 172.0(3) . . . . ?
Ni1 N1 C9 C8 -18.6(3) . . . . ?
N2 C8 C9 N1 27.3(4) . . . . ?
N2 C8 C9 C10 -157.2(3) . . . . ?
N1 C9 C10 C11 2.7(5) . . . . ?
C8 C9 C10 C11 -172.6(3) . . . . ?
C9 C10 C11 C12 0.3(5) . . . . ?
C10 C11 C12 C13 -2.2(5) . . . . ?
C9 N1 C13 C12 1.5(5) . . . . ?
Ni1 N1 C13 C12 -166.5(2) . . . . ?
C11 C12 C13 N1 1.4(5) . . . . ?
C8 N2 C14 C15 54.8(3) . . . . ?
C7 N2 C14 C15 175.6(2) . . . . ?
Ni1 N2 C14 C15 -65.0(3) . . . . ?
N2 C14 C15 C20 -123.1(3) . . . . ?
N2 C14 C15 C16 60.4(4) . . . . ?
Ni1 O2 C16 C15 -26.8(4) . . . . ?
Ni1 O2 C16 C17 154.5(2) . . . . ?
C20 C15 C16 O2 175.9(3) . . . . ?
C14 C15 C16 O2 -7.7(4) . . . . ?
C20 C15 C16 C17 -5.3(4) . . . . ?
C14 C15 C16 C17 171.1(3) . . . . ?
O2 C16 C17 C18 -177.5(3) . . . . ?
C15 C16 C17 C18 3.8(4) . . . . ?
O2 C16 C17 C29 1.2(4) . . . . ?
C15 C16 C17 C29 -177.6(3) . . . . ?
C16 C17 C18 C19 0.2(5) . . . . ?
C29 C17 C18 C19 -178.5(3) . . . . ?
C17 C18 C19 C20 -2.7(5) . . . . ?
C17 C18 C19 C33 179.4(3) . . . . ?
C18 C19 C20 C15 1.1(5) . . . . ?
C33 C19 C20 C15 179.0(3) . . . . ?
C16 C15 C20 C19 2.9(5) . . . . ?
C14 C15 C20 C19 -173.5(3) . . . . ?
C1 C2 C21 C24 -179.4(3) . . . . ?
C3 C2 C21 C24 -0.5(4) . . . . ?
C1 C2 C21 C23 -60.3(4) . . . . ?
C3 C2 C21 C23 118.6(3) . . . . ?
C1 C2 C21 C22 60.9(4) . . . . ?
C3 C2 C21 C22 -120.1(3) . . . . ?
C5 C4 C25 C28 -48.6(4) . . . . ?
C3 C4 C25 C28 133.2(3) . . . . ?
C5 C4 C25 C26 71.5(4) . . . . ?
C3 C4 C25 C26 -106.8(4) . . . . ?
C5 C4 C25 C27 -168.4(3) . . . . ?
C3 C4 C25 C27 13.4(4) . . . . ?
C18 C17 C29 C30 115.0(3) . . . . ?
C16 C17 C29 C30 -63.6(4) . . . . ?
C18 C17 C29 C32 -3.6(5) . . . . ?
C16 C17 C29 C32 177.8(3) . . . . ?
C18 C17 C29 C31 -122.9(3) . . . . ?
C16 C17 C29 C31 58.5(4) . . . . ?
C20 C19 C33 C39 47.8(7) . . . . ?
C18 C19 C33 C39 -134.4(7) . . . . ?
C20 C19 C33 C36 -121.5(8) . . . . ?
C18 C19 C33 C36 56.3(8) . . . . ?
C20 C19 C33 C35 175.1(5) . . . . ?
C18 C19 C33 C35 -7.0(6) . . . . ?
C20 C19 C33 C38 6.4(8) . . . . ?
C18 C19 C33 C38 -175.8(7) . . . . ?
C20 C19 C33 C37 -70.9(5) . . . . ?
C18 C19 C33 C37 106.9(5) . . . . ?
C20 C19 C33 C34 120.8(6) . . . . ?
C18 C19 C33 C34 -61.4(6) . . . . ?
C39 C33 C34 C35 -148.5(7) . . . . ?
C36 C33 C34 C35 -14.7(8) . . . . ?
C19 C33 C34 C35 105.2(6) . . . . ?
C38 C33 C34 C35 -135.4(7) . . . . ?
C37 C33 C34 C35 -54.8(12) . . . . ?
C36 C33 C34 C39 133.8(7) . . . . ?
C35 C33 C34 C39 148.5(7) . . . . ?
C19 C33 C34 C39 -106.3(5) . . . . ?
C38 C33 C34 C39 13.1(7) . . . . ?
C37 C33 C34 C39 93.8(11) . . . . ?
C33 C34 C35 C36 16.9(8) . . . . ?
C39 C34 C35 C36 -9.0(11) . . . . ?
C39 C34 C35 C33 -25.9(5) . . . . ?
C39 C33 C35 C34 32.0(8) . . . . ?
C36 C33 C35 C34 163.5(8) . . . . ?
C19 C33 C35 C34 -94.0(6) . . . . ?
C38 C33 C35 C34 71.4(12) . . . . ?
C37 C33 C35 C34 151.3(6) . . . . ?
C39 C33 C35 C36 -131.6(8) . . . . ?
C19 C33 C35 C36 102.5(6) . . . . ?
C38 C33 C35 C36 -92.1(12) . . . . ?
C37 C33 C35 C36 -12.3(7) . . . . ?
C34 C33 C35 C36 -163.5(8) . . . . ?
C34 C35 C36 C37 1.7(16) . . . . ?
C33 C35 C36 C37 19.7(9) . . . . ?
C34 C35 C36 C33 -18.1(8) . . . . ?
C39 C33 C36 C37 -72.5(12) . . . . ?
C35 C33 C36 C37 -163.9(8) . . . . ?
C19 C33 C36 C37 92.9(7) . . . . ?
C38 C33 C36 C37 -34.8(8) . . . . ?
C34 C33 C36 C37 -150.5(6) . . . . ?
C39 C33 C36 C35 91.4(12) . . . . ?
C19 C33 C36 C35 -103.2(5) . . . . ?
C38 C33 C36 C35 129.1(7) . . . . ?
C37 C33 C36 C35 163.9(8) . . . . ?
C34 C33 C36 C35 13.5(7) . . . . ?
C35 C36 C37 C33 -18.6(9) . . . . ?
C35 C36 C37 C38 9.2(13) . . . . ?
C33 C36 C37 C38 27.8(6) . . . . ?
C39 C33 C37 C36 135.9(8) . . . . ?
C35 C33 C37 C36 14.1(7) . . . . ?
C19 C33 C37 C36 -104.6(7) . . . . ?
C38 C33 C37 C36 146.5(8) . . . . ?
C34 C33 C37 C36 55.4(13) . . . . ?
C39 C33 C37 C38 -10.6(6) . . . . ?
C36 C33 C37 C38 -146.5(8) . . . . ?
C35 C33 C37 C38 -132.4(6) . . . . ?
C19 C33 C37 C38 108.9(5) . . . . ?
C34 C33 C37 C38 -91.1(12) . . . . ?
C36 C33 C38 C39 -137.4(10) . . . . ?
C35 C33 C38 C39 -69.9(13) . . . . ?
C19 C33 C38 C39 95.4(8) . . . . ?
C37 C33 C38 C39 -163.8(10) . . . . ?
C34 C33 C38 C39 -19.9(10) . . . . ?
C39 C33 C38 C37 163.8(10) . . . . ?
C36 C33 C38 C37 26.4(6) . . . . ?
C35 C33 C38 C37 93.9(10) . . . . ?
C19 C33 C38 C37 -100.8(5) . . . . ?
C34 C33 C38 C37 143.9(6) . . . . ?
C36 C37 C38 C39 -14.1(13) . . . . ?
C33 C37 C38 C39 16.8(9) . . . . ?
C36 C37 C38 C33 -30.9(7) . . . . ?
C37 C38 C39 C33 -14.9(8) . . . . ?
C33 C38 C39 C34 23.2(10) . . . . ?
C37 C38 C39 C34 8.4(17) . . . . ?
C36 C33 C39 C38 65.1(15) . . . . ?
C35 C33 C39 C38 133.0(9) . . . . ?
C19 C33 C39 C38 -100.4(9) . . . . ?
C37 C33 C39 C38 16.4(10) . . . . ?
C34 C33 C39 C38 159.4(10) . . . . ?
C36 C33 C39 C34 -94.3(12) . . . . ?
C35 C33 C39 C34 -26.3(6) . . . . ?
C19 C33 C39 C34 100.2(5) . . . . ?
C38 C33 C39 C34 -159.4(10) . . . . ?
C37 C33 C39 C34 -143.0(6) . . . . ?
C35 C34 C39 C38 2.6(15) . . . . ?
C33 C34 C39 C38 -26.6(12) . . . . ?
C35 C34 C39 C33 29.2(6) . . . . ?
