#------------------------------------------------------------------------------
#$Date: 2023-12-04 10:13:15 +0200 (Mon, 04 Dec 2023) $
#$Revision: 287959 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/76/8107698.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_8107698
loop_
_publ_author_name
'Chen, Xiao-Ming'
'Ou, Guang-Chuan'
_publ_section_title
;
 Crystal structure of bis(benzene-1 carboxylato-O 3,5-carboxyl-κ
 1O)-[(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ 4
 N,N′,N′′,N′′′)nickel(II)
 ─ benzene-1,3,5-tricarboxylic acid ─ water (1/2/4),
 C52H66N4NiO28
;
_journal_issue                   6
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              1189
_journal_page_last               1191
_journal_paper_doi               10.1515/ncrs-2023-0389
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C34 H46 N4 Ni O12, 4(H2 O), 2(C9 H6 O6)'
_chemical_formula_sum            'C52 H66 N4 Ni O28'
_chemical_formula_weight         1253.79
_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     iterative
_cell_angle_alpha                81.872(6)
_cell_angle_beta                 67.036(5)
_cell_angle_gamma                75.624(6)
_cell_formula_units_Z            1
_cell_length_a                   11.292(6)
_cell_length_b                   11.670(6)
_cell_length_c                   12.165(6)
_cell_measurement_reflns_used    4686
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.15
_cell_volume                     1428.0(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-beta (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker SMART II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15999
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.367
_diffrn_reflns_theta_min         1.804
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.9182
_exptl_absorpt_correction_T_min  0.8287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.92
_exptl_transmission_factor_min   0.83
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6262
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0728P)²+0.0750P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5008
_reflns_number_total             6262
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0389_suppl_001.cif
_cod_data_source_block           1
_cod_original_cell_volume        1428.1(12)
_cod_database_code               8107698
_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.
;
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.829
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 H1WA-H1WB = H2WB-H2WA
 1.39 with sigma of 0.01
 O1W-H1WA = O1W-H1WB = O2W-H2WB = O2W-H2WA
 0.86 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C21(H21), N1(H1), N2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C9(H9), C14(H14), C16(H16), C18(H18)
3.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
3.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O5(H5A), O8(H8), O10(H10), O11(H11)
;
_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
C1 C 0.66264(18) 0.35588(16) 0.75662(16) 0.0339(4) Uani 1 1 d . . . . .
C2 C 0.9167(2) 0.20218(18) 0.34066(17) 0.0426(5) Uani 1 1 d . . . . .
C3 C 0.62771(19) 0.60818(17) 0.40096(17) 0.0373(4) Uani 1 1 d . . . . .
C4 C 0.70477(18) 0.37100(16) 0.62174(15) 0.0320(4) Uani 1 1 d . . . . .
C5 C 0.79005(19) 0.28096(16) 0.54685(16) 0.0344(4) Uani 1 1 d . . . . .
H5 H 0.824435 0.209833 0.579530 0.041 Uiso 1 1 calc R U . . .
C6 C 0.82410(19) 0.29671(16) 0.42359(16) 0.0349(4) Uani 1 1 d . . . . .
C7 C 0.77190(19) 0.40215(16) 0.37390(16) 0.0348(4) Uani 1 1 d . . . . .
H7 H 0.793630 0.412135 0.291641 0.042 Uiso 1 1 calc R U . . .
C8 C 0.68708(18) 0.49255(16) 0.44781(16) 0.0324(4) Uani 1 1 d . . . . .
C9 C 0.65493(18) 0.47633(16) 0.57060(16) 0.0335(4) Uani 1 1 d . . . . .
H9 H 0.598828 0.537325 0.619609 0.040 Uiso 1 1 calc R U . . .
C19 C 0.6365(2) 0.30696(19) 1.1086(2) 0.0501(6) Uani 1 1 d . . . . .
H19A H 0.679127 0.224145 1.112072 0.060 Uiso 1 1 calc R U . . .
H19B H 0.595238 0.334277 1.189308 0.060 Uiso 1 1 calc R U . . .
C20 C 0.7366(2) 0.37871(19) 1.0326(2) 0.0493(5) Uani 1 1 d . . . . .
H20A H 0.801340 0.373328 1.068052 0.059 Uiso 1 1 calc R U . . .
H20B H 0.781831 0.347791 0.953443 0.059 Uiso 1 1 calc R U . . .
C21 C 0.7514(2) 0.5797(2) 0.9319(2) 0.0470(5) Uani 1 1 d . . . . .
H21 H 0.768627 0.553808 0.852924 0.056 Uiso 1 1 calc R U . . .
C22 C 0.6738(2) 0.7081(2) 0.9414(2) 0.0505(6) Uani 1 1 d . . . . .
H22A H 0.737063 0.758763 0.907535 0.061 Uiso 1 1 calc R U . . .
H22B H 0.629514 0.723319 1.025684 0.061 Uiso 1 1 calc R U . . .
C23 C 0.8831(3) 0.5696(3) 0.9434(3) 0.0796(9) Uani 1 1 d . . . . .
H23A H 0.868710 0.600545 1.017643 0.119 Uiso 1 1 calc R U . . .
H23B H 0.936033 0.613989 0.878208 0.119 Uiso 1 1 calc R U . . .
H23C H 0.927701 0.487931 0.941476 0.119 Uiso 1 1 calc R U . . .
C24 C 0.4296(2) 0.25161(17) 1.11695(18) 0.0450(5) Uani 1 1 d . . . . .
C25 C 0.3666(3) 0.2711(2) 1.25008(18) 0.0591(6) Uani 1 1 d . . . . .
H25A H 0.427405 0.231831 1.287754 0.089 Uiso 1 1 calc R U . . .
H25B H 0.288428 0.239267 1.284112 0.089 Uiso 1 1 calc R U . . .
H25C H 0.344034 0.354353 1.262553 0.089 Uiso 1 1 calc R U . . .
C26 C 0.4870(3) 0.11863(19) 1.0969(2) 0.0696(8) Uani 1 1 d . . . . .
H26A H 0.531384 0.106980 1.012853 0.104 Uiso 1 1 calc R U . . .
H26B H 0.417007 0.076126 1.129019 0.104 Uiso 1 1 calc R U . . .
H26C H 0.548252 0.089904 1.136474 0.104 Uiso 1 1 calc R U . . .
N1 N 0.53647(16) 0.32090(13) 1.05523(13) 0.0355(4) Uani 1 1 d . . . . .
H1 H 0.586543 0.281928 0.979462 0.043 Uiso 1 1 calc R U . . .
N2 N 0.66916(15) 0.50414(14) 1.02357(14) 0.0375(4) Uani 1 1 d . . . . .
H2 H 0.642911 0.537491 1.101240 0.045 Uiso 1 1 calc R U . . .
Ni1 Ni 0.500000 0.500000 1.000000 0.02938(12) Uani 1 2 d S . P . .
O1 O 0.60550(13) 0.44807(11) 0.81410(11) 0.0375(3) Uani 1 1 d . . . . .
O2 O 0.68410(17) 0.25269(12) 0.80202(12) 0.0556(4) Uani 1 1 d . . . . .
O3 O 0.97139(19) 0.11060(14) 0.39189(14) 0.0655(5) Uani 1 1 d . . . . .
H3 H 1.022357 0.063719 0.341249 0.098 Uiso 1 1 calc R U . . .
O4 O 0.93735(19) 0.21180(14) 0.23488(13) 0.0667(5) Uani 1 1 d . . . . .
O5 O 0.65296(17) 0.61709(13) 0.28578(12) 0.0514(4) Uani 1 1 d . . . . .
H5A H 0.614099 0.681868 0.268228 0.077 Uiso 1 1 calc R U . . .
O6 O 0.56134(18) 0.68777(13) 0.46685(14) 0.0586(5) Uani 1 1 d . . . . .
O1W O 0.52530(18) 0.82204(14) 0.23510(14) 0.0572(4) Uani 1 1 d D . . . .
H1WA H 0.497(2) 0.864(2) 0.2961(16) 0.069 Uiso 1 1 d D U . . .
H1WB H 0.4581(17) 0.817(2) 0.220(2) 0.069 Uiso 1 1 d D U . . .
O2W O 0.1396(2) 0.96551(16) 0.22827(15) 0.0766(6) Uani 1 1 d D . . . .
H2WA H 0.136(3) 0.982(2) 0.1578(14) 0.092 Uiso 1 1 d D U . . .
H2WB H 0.193(2) 0.8964(14) 0.223(2) 0.092 Uiso 1 1 d D U . . .
C10 C 0.3485(2) -0.04332(18) 0.53520(18) 0.0441(5) Uani 1 1 d . . . . .
C11 C 0.1006(2) 0.10963(18) 0.94265(18) 0.0444(5) Uani 1 1 d . . . . .
C12 C 0.05830(19) 0.35574(17) 0.58011(17) 0.0381(4) Uani 1 1 d . . . . .
C13 C 0.2524(2) 0.05118(17) 0.61571(17) 0.0385(4) Uani 1 1 d . . . . .
C14 C 0.2198(2) 0.03788(17) 0.73836(17) 0.0408(5) Uani 1 1 d . . . . .
H14 H 0.256160 -0.031537 0.771998 0.049 Uiso 1 1 calc R U . . .
C15 C 0.1326(2) 0.12821(17) 0.81121(16) 0.0374(4) Uani 1 1 d . . . . .
C16 C 0.07906(19) 0.23208(17) 0.76055(17) 0.0378(4) Uani 1 1 d . . . . .
H16 H 0.021331 0.292916 0.808991 0.045 Uiso 1 1 calc R U . . .
C17 C 0.11176(19) 0.24515(16) 0.63752(16) 0.0358(4) Uani 1 1 d . . . . .
C18 C 0.1982(2) 0.15438(17) 0.56546(17) 0.0394(5) Uani 1 1 d . . . . .
H18 H 0.219675 0.162867 0.483182 0.047 Uiso 1 1 calc R U . . .
O7 O 0.3891(2) -0.03012(15) 0.42746(14) 0.0719(6) Uani 1 1 d . . . . .
O8 O 0.38297(18) -0.14101(13) 0.59355(13) 0.0612(5) Uani 1 1 d . . . . .
H8 H 0.437129 -0.189255 0.545831 0.092 Uiso 1 1 calc R U . . .
O9 O 0.14899(19) 0.02202(15) 0.98884(13) 0.0682(5) Uani 1 1 d . . . . .
O10 O 0.01397(18) 0.19926(14) 1.00279(13) 0.0635(5) Uani 1 1 d . . . . .
H10 H -0.003650 0.184057 1.074601 0.095 Uiso 1 1 calc R U . . .
O11 O -0.01802(17) 0.43939(13) 0.65136(13) 0.0554(4) Uani 1 1 d . . . . .
H11 H -0.040820 0.497604 0.612177 0.083 Uiso 1 1 calc R U . . .
O12 O 0.08764(16) 0.36566(13) 0.47047(13) 0.0543(4) 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
O1 C1 C4 116.66(16) . .
O1 C1 O2 125.38(17) . .
O2 C1 C4 117.94(16) . .
O3 C2 C6 114.70(17) . .
O4 C2 C6 121.66(19) . .
O4 C2 O3 123.64(18) . .
O5 C3 C8 115.87(16) . .
O6 C3 C8 120.96(17) . .
O6 C3 O5 123.16(18) . .
C5 C4 C1 122.00(17) . .
C9 C4 C1 119.42(16) . .
C9 C4 C5 118.55(16) . .
C4 C5 H5 119.7 . .
C6 C5 C4 120.52(17) . .
C6 C5 H5 119.7 . .
C5 C6 C2 121.78(17) . .
C7 C6 C2 118.00(16) . .
C7 C6 C5 120.21(16) . .
C6 C7 H7 120.2 . .
C8 C7 C6 119.68(16) . .
C8 C7 H7 120.2 . .
C7 C8 C3 122.71(16) . .
C9 C8 C3 117.69(16) . .
C9 C8 C7 119.60(17) . .
C4 C9 C8 121.42(16) . .
C4 C9 H9 119.3 . .
C8 C9 H9 119.3 . .
H19A C19 H19B 108.4 . .
C20 C19 H19A 110.0 . .
C20 C19 H19B 110.0 . .
N1 C19 H19A 110.0 . .
N1 C19 H19B 110.0 . .
N1 C19 C20 108.53(16) . .
C19 C20 H20A 109.8 . .
C19 C20 H20B 109.8 . .
H20A C20 H20B 108.2 . .
N2 C20 C19 109.38(17) . .
N2 C20 H20A 109.8 . .
N2 C20 H20B 109.8 . .
C22 C21 H21 108.1 . .
C23 C21 H21 108.1 . .
C23 C21 C22 111.1(2) . .
N2 C21 H21 108.1 . .
N2 C21 C22 108.83(17) . .
N2 C21 C23 112.4(2) . .
C21 C22 H22A 107.5 . .
C21 C22 H22B 107.5 . .
C21 C22 C24 119.44(18) . 2_667
H22A C22 H22B 107.0 . .
C24 C22 H22A 107.5 2_667 .
C24 C22 H22B 107.5 2_667 .
C21 C23 H23A 109.5 . .
C21 C23 H23B 109.5 . .
C21 C23 H23C 109.5 . .
H23A C23 H23B 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C22 C24 C26 107.62(19) 2_667 .
C25 C24 C22 110.5(2) . 2_667
C25 C24 C26 109.56(18) . .
N1 C24 C22 107.86(16) . 2_667
N1 C24 C25 111.33(17) . .
N1 C24 C26 109.93(19) . .
C24 C25 H25A 109.5 . .
C24 C25 H25B 109.5 . .
C24 C25 H25C 109.5 . .
H25A C25 H25B 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C24 C26 H26A 109.5 . .
C24 C26 H26B 109.5 . .
C24 C26 H26C 109.5 . .
H26A C26 H26B 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C19 N1 C24 116.36(16) . .
C19 N1 H1 102.8 . .
C19 N1 Ni1 105.63(12) . .
C24 N1 H1 102.8 . .
C24 N1 Ni1 123.56(12) . .
Ni1 N1 H1 102.8 . .
C20 N2 C21 114.81(17) . .
C20 N2 H2 107.3 . .
C20 N2 Ni1 105.98(13) . .
C21 N2 H2 107.3 . .
C21 N2 Ni1 113.78(12) . .
Ni1 N2 H2 107.3 . .
N1 Ni1 N1 180.0 2_667 .
N1 Ni1 O1 91.46(6) . 2_667
N1 Ni1 O1 88.54(6) 2_667 2_667
N1 Ni1 O1 88.54(6) . .
N1 Ni1 O1 91.46(6) 2_667 .
N2 Ni1 N1 85.21(7) 2_667 2_667
N2 Ni1 N1 94.79(7) 2_667 .
N2 Ni1 N1 94.79(7) . 2_667
N2 Ni1 N1 85.21(7) . .
N2 Ni1 N2 180.0 2_667 .
N2 Ni1 O1 86.60(6) . 2_667
N2 Ni1 O1 86.60(6) 2_667 .
N2 Ni1 O1 93.40(6) . .
N2 Ni1 O1 93.40(6) 2_667 2_667
O1 Ni1 O1 180.0 . 2_667
C1 O1 Ni1 139.41(12) . .
C2 O3 H3 109.5 . .
C3 O5 H5A 109.5 . .
H1WA O1W H1WB 107.2(14) . .
H2WA O2W H2WB 105.1(14) . .
O7 C10 C13 122.87(19) . .
O7 C10 O8 124.04(19) . .
O8 C10 C13 113.10(17) . .
O9 C11 C15 123.67(18) . .
O9 C11 O10 123.73(19) . .
O10 C11 C15 112.60(17) . .
O11 C12 C17 115.99(17) . .
O12 C12 C17 120.71(17) . .
O12 C12 O11 123.30(18) . .
C14 C13 C10 121.11(18) . .
C18 C13 C10 118.82(17) . .
C18 C13 C14 120.05(17) . .
C13 C14 H14 120.0 . .
C13 C14 C15 120.08(18) . .
C15 C14 H14 120.0 . .
C14 C15 C11 118.02(17) . .
C16 C15 C11 122.19(17) . .
C16 C15 C14 119.79(17) . .
C15 C16 H16 120.0 . .
C15 C16 C17 120.04(17) . .
C17 C16 H16 120.0 . .
C16 C17 C12 121.50(16) . .
C18 C17 C12 118.63(17) . .
C18 C17 C16 119.86(17) . .
C13 C18 C17 120.18(18) . .
C13 C18 H18 119.9 . .
C17 C18 H18 119.9 . .
C10 O8 H8 109.5 . .
C11 O10 H10 109.5 . .
C12 O11 H11 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C4 1.517(3) .
C1 O1 1.257(2) .
C1 O2 1.259(2) .
C2 C6 1.499(3) .
C2 O3 1.302(2) .
C2 O4 1.209(2) .
C3 C8 1.492(3) .
C3 O5 1.310(2) .
C3 O6 1.210(2) .
C4 C5 1.395(2) .
C4 C9 1.389(3) .
C5 H5 0.9300 .
C5 C6 1.392(3) .
C6 C7 1.391(3) .
C7 H7 0.9300 .
C7 C8 1.390(2) .
C8 C9 1.389(3) .
C9 H9 0.9300 .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C19 C20 1.506(3) .
C19 N1 1.475(3) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C20 N2 1.483(3) .
C21 H21 0.9800 .
C21 C22 1.531(3) .
C21 C23 1.521(3) .
C21 N2 1.485(3) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C22 C24 1.539(3) 2_667
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 C25 1.518(3) .
C24 C26 1.540(3) .
C24 N1 1.510(3) .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C26 H26A 0.9600 .
C26 H26B 0.9600 .
C26 H26C 0.9600 .
N1 H1 0.9800 .
N1 Ni1 2.0932(17) .
N2 H2 0.9800 .
N2 Ni1 2.0518(18) .
Ni1 O1 2.1972(15) 2_667
Ni1 O1 2.1972(15) .
O3 H3 0.8200 .
O5 H5A 0.8200 .
O1W H1WA 0.853(9) .
O1W H1WB 0.861(9) .
O2W H2WA 0.866(10) .
O2W H2WB 0.870(10) .
C10 C13 1.495(3) .
C10 O7 1.209(3) .
C10 O8 1.312(2) .
C11 C15 1.491(3) .
C11 O9 1.208(2) .
C11 O10 1.318(2) .
C12 C17 1.485(3) .
C12 O11 1.298(2) .
C12 O12 1.238(2) .
C13 C14 1.385(3) .
C13 C18 1.385(3) .
C14 H14 0.9300 .
C14 C15 1.391(3) .
C15 C16 1.389(3) .
C16 H16 0.9300 .
C16 C17 1.390(3) .
C17 C18 1.387(3) .
C18 H18 0.9300 .
O8 H8 0.8200 .
O10 H10 0.8200 .
O11 H11 0.8200 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O2 0.98 2.04 2.988(2) 162.6 . yes
O3 H3 O2W 0.82 1.80 2.616(2) 177.2 1_645 yes
O5 H5A O1W 0.82 1.78 2.597(2) 178.0 . yes
O8 H8 O6 0.82 1.81 2.622(2) 168.4 1_545 yes
O10 H10 O4 0.82 1.85 2.625(2) 158.1 1_456 yes
O11 H11 O12 0.82 1.84 2.657(2) 175.9 2_566 yes
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
C1 C4 C5 C6 178.36(18) . . . .
C1 C4 C9 C8 -177.68(17) . . . .
C2 C6 C7 C8 -179.10(18) . . . .
C3 C8 C9 C4 179.34(18) . . . .
C4 C1 O1 Ni1 171.69(13) . . . .
C4 C5 C6 C2 179.27(18) . . . .
C4 C5 C6 C7 -0.8(3) . . . .
C5 C4 C9 C8 0.8(3) . . . .
C5 C6 C7 C8 1.0(3) . . . .
C6 C7 C8 C3 179.76(18) . . . .
C6 C7 C8 C9 -0.3(3) . . . .
C7 C8 C9 C4 -0.6(3) . . . .
C9 C4 C5 C6 0.0(3) . . . .
C19 C20 N2 C21 -168.20(17) . . . .
C19 C20 N2 Ni1 -41.73(19) . . . .
C20 C19 N1 C24 177.94(16) . . . .
C20 C19 N1 Ni1 -40.88(18) . . . .
C22 C21 N2 C20 -174.50(16) . . . .
C22 C21 N2 Ni1 63.16(19) . . . .
C22 C24 N1 C19 172.11(16) 2_667 . . .
C22 C24 N1 Ni1 38.5(2) 2_667 . . .
C23 C21 C22 C24 154.9(2) . . . 2_667
C23 C21 N2 C20 -51.0(2) . . . .
C23 C21 N2 Ni1 -173.34(16) . . . .
C25 C24 N1 C19 50.8(2) . . . .
C25 C24 N1 Ni1 -82.8(2) . . . .
C26 C24 N1 C19 -70.8(2) . . . .
C26 C24 N1 Ni1 155.60(15) . . . .
N1 C19 C20 N2 57.1(2) . . . .
N2 C21 C22 C24 -80.8(2) . . . 2_667
O1 C1 C4 C5 167.59(18) . . . .
O1 C1 C4 C9 -14.0(3) . . . .
O2 C1 C4 C5 -14.3(3) . . . .
O2 C1 C4 C9 164.08(19) . . . .
O2 C1 O1 Ni1 -6.2(3) . . . .
O3 C2 C6 C5 -6.3(3) . . . .
O3 C2 C6 C7 173.82(19) . . . .
O4 C2 C6 C5 173.5(2) . . . .
O4 C2 C6 C7 -6.4(3) . . . .
O5 C3 C8 C7 4.5(3) . . . .
O5 C3 C8 C9 -175.41(18) . . . .
O6 C3 C8 C7 -175.0(2) . . . .
O6 C3 C8 C9 5.0(3) . . . .
C10 C13 C14 C15 178.45(19) . . . .
C10 C13 C18 C17 -178.08(19) . . . .
C11 C15 C16 C17 -179.9(2) . . . .
C12 C17 C18 C13 178.40(18) . . . .
C13 C14 C15 C11 -179.94(19) . . . .
C13 C14 C15 C16 -0.4(3) . . . .
C14 C13 C18 C17 0.5(3) . . . .
C14 C15 C16 C17 0.6(3) . . . .
C15 C16 C17 C12 -178.91(19) . . . .
C15 C16 C17 C18 -0.2(3) . . . .
C16 C17 C18 C13 -0.4(3) . . . .
C18 C13 C14 C15 -0.1(3) . . . .
O7 C10 C13 C14 -172.5(2) . . . .
O7 C10 C13 C18 6.1(4) . . . .
O8 C10 C13 C14 7.7(3) . . . .
O8 C10 C13 C18 -173.7(2) . . . .
O9 C11 C15 C14 2.1(4) . . . .
O9 C11 C15 C16 -177.4(2) . . . .
O10 C11 C15 C14 -177.9(2) . . . .
O10 C11 C15 C16 2.6(3) . . . .
O11 C12 C17 C16 1.3(3) . . . .
O11 C12 C17 C18 -177.43(19) . . . .
O12 C12 C17 C16 -179.5(2) . . . .
O12 C12 C17 C18 1.8(3) . . . .
