#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:20:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179447 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/44/4334400.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_4334400
loop_
_publ_author_name
'Julia R. Khusnutdinova'
'Jia Luo'
'Nigam P. Rath'
'Liviu M. Mirica'
_publ_section_title
;
 Late First-Row Transition Metal Complexes of a Tetradentate Pyridinophane
 Ligand: Electronic Properties and Reactivity Implications
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3920
_journal_page_last               3932
_journal_paper_doi               10.1021/ic400260z
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         '3(C22 H32 Cl2 N4 Ni), C H2 Cl2, H2 O'
_chemical_formula_sum            'C67 H100 Cl8 N12 Ni3 O'
_chemical_formula_weight         1549.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 127.2250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.6002(9)
_cell_length_b                   22.2611(8)
_cell_length_c                   19.2269(11)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.35
_cell_volume                     8043.2(6)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            68765
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.8412
_exptl_absorpt_correction_T_min  0.8249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs v2008/1'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         8263
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1015P)²+50.4668P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.2145
_reflns_number_gt                5950
_reflns_number_total             8263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400260z_si_002_11.cif
_cod_data_source_block           l19711
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4334400
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.31177(3) 0.43012(3) 0.73361(4) 0.0369(2) Uani 1 1 d . . .
Ni2 Ni 0.0000 0.40466(3) 0.2500 0.0297(2) Uani 1 2 d S . .
Cl1 Cl 0.19501(6) 0.46807(6) 0.65495(9) 0.0470(3) Uani 1 1 d . . .
Cl2 Cl 0.32085(9) 0.41371(8) 0.86248(11) 0.0652(5) Uani 1 1 d . . .
Cl3 Cl -0.09046(6) 0.33040(5) 0.16497(8) 0.0365(3) Uani 1 1 d . . .
N1 N 0.3121(3) 0.4455(2) 0.6307(3) 0.0486(11) Uani 1 1 d . . .
N2 N 0.4099(2) 0.3958(2) 0.7952(3) 0.0470(11) Uani 1 1 d . . .
N3 N 0.3843(3) 0.5152(2) 0.7810(4) 0.0642(15) Uani 1 1 d . . .
N4 N 0.2844(2) 0.3389(2) 0.6649(3) 0.0516(12) Uani 1 1 d . . .
N5 N 0.07214(18) 0.47147(16) 0.3136(3) 0.0311(8) Uani 1 1 d . . .
N6 N -0.01438(19) 0.43491(16) 0.3547(3) 0.0331(9) Uani 1 1 d . . .
C1 C 0.2711(3) 0.4101(3) 0.5602(4) 0.0624(18) Uani 1 1 d . . .
C2 C 0.2612(5) 0.4231(5) 0.4825(5) 0.090(3) Uani 1 1 d . . .
H2 H 0.2329 0.3981 0.4324 0.107 Uiso 1 1 calc R . .
C3 C 0.2940(6) 0.4731(6) 0.4816(7) 0.106(4) Uani 1 1 d . . .
H3 H 0.2858 0.4841 0.4285 0.127 Uiso 1 1 calc R . .
C4 C 0.3382(5) 0.5083(4) 0.5535(7) 0.091(3) Uani 1 1 d . . .
H4 H 0.3614 0.5424 0.5516 0.109 Uiso 1 1 calc R . .
C5 C 0.3476(4) 0.4918(3) 0.6304(5) 0.0649(19) Uani 1 1 d . . .
C6 C 0.4023(4) 0.5180(3) 0.7168(6) 0.079(2) Uani 1 1 d . . .
H6A H 0.4094 0.5605 0.7089 0.095 Uiso 1 1 calc R . .
H6B H 0.4478 0.4966 0.7427 0.095 Uiso 1 1 calc R . .
C7 C 0.4459(4) 0.4927(4) 0.8666(6) 0.087(3) Uani 1 1 d . . .
H7A H 0.4350 0.4944 0.9088 0.105 Uiso 1 1 calc R . .
H7B H 0.4875 0.5190 0.8886 0.105 Uiso 1 1 calc R . .
C8 C 0.4646(3) 0.4283(4) 0.8604(5) 0.072(2) Uani 1 1 d . . .
C9 C 0.5317(4) 0.4013(6) 0.9113(5) 0.102(3) Uani 1 1 d . . .
H9 H 0.5717 0.4233 0.9573 0.122 Uiso 1 1 calc R . .
C10 C 0.5404(3) 0.3417(5) 0.8946(5) 0.093(3) Uani 1 1 d . . .
H10 H 0.5851 0.3222 0.9321 0.111 Uiso 1 1 calc R . .
C11 C 0.4845(3) 0.3125(4) 0.8248(5) 0.069(2) Uani 1 1 d . . .
H11 H 0.4902 0.2734 0.8100 0.083 Uiso 1 1 calc R . .
C12 C 0.4179(3) 0.3409(3) 0.7744(4) 0.0465(13) Uani 1 1 d . . .
C13 C 0.3548(3) 0.3169(3) 0.6892(4) 0.0551(15) Uani 1 1 d . . .
H13A H 0.3556 0.2724 0.6921 0.066 Uiso 1 1 calc R . .
H13B H 0.3587 0.3285 0.6425 0.066 Uiso 1 1 calc R . .
C14 C 0.2396(3) 0.3579(3) 0.5721(4) 0.071(2) Uani 1 1 d . . .
H14A H 0.2350 0.3243 0.5353 0.086 Uiso 1 1 calc R . .
H14B H 0.1914 0.3683 0.5531 0.086 Uiso 1 1 calc R . .
C15 C 0.3577(5) 0.5761(3) 0.7867(7) 0.087(3) Uani 1 1 d . . .
C16 C 0.2989(5) 0.5980(3) 0.6945(7) 0.091(3) Uani 1 1 d . . .
H16A H 0.2777 0.6348 0.6976 0.136 Uiso 1 1 calc R . .
H16B H 0.2622 0.5669 0.6631 0.136 Uiso 1 1 calc R . .
H16C H 0.3191 0.6063 0.6635 0.136 Uiso 1 1 calc R . .
C17 C 0.4169(6) 0.6230(5) 0.8360(10) 0.151(6) Uani 1 1 d . . .
H17A H 0.4338 0.6332 0.8019 0.227 Uiso 1 1 calc R . .
H17B H 0.4564 0.6067 0.8928 0.227 Uiso 1 1 calc R . .
H17C H 0.3985 0.6592 0.8451 0.227 Uiso 1 1 calc R . .
C18 C 0.3260(5) 0.5663(4) 0.8368(6) 0.089(3) Uani 1 1 d . . .
H18A H 0.3079 0.6045 0.8414 0.133 Uiso 1 1 calc R . .
H18B H 0.3631 0.5509 0.8954 0.133 Uiso 1 1 calc R . .
H18C H 0.2870 0.5371 0.8051 0.133 Uiso 1 1 calc R . .
C19 C 0.2472(3) 0.2896(3) 0.6785(6) 0.079(3) Uani 1 1 d . . .
C20 C 0.3000(4) 0.2678(3) 0.7721(7) 0.098(3) Uani 1 1 d . . .
H20A H 0.3389 0.2462 0.7781 0.146 Uiso 1 1 calc R . .
H20B H 0.2757 0.2409 0.7868 0.146 Uiso 1 1 calc R . .
H20C H 0.3193 0.3024 0.8118 0.146 Uiso 1 1 calc R . .
C21 C 0.2217(5) 0.2374(4) 0.6148(8) 0.129(5) Uani 1 1 d . . .
H21A H 0.1811 0.2503 0.5564 0.193 Uiso 1 1 calc R . .
H21B H 0.2071 0.2040 0.6341 0.193 Uiso 1 1 calc R . .
H21C H 0.2603 0.2241 0.6130 0.193 Uiso 1 1 calc R . .
C22 C 0.1828(4) 0.3170(3) 0.6697(7) 0.091(3) Uani 1 1 d . . .
H22A H 0.1997 0.3461 0.7168 0.136 Uiso 1 1 calc R . .
H22B H 0.1564 0.2849 0.6736 0.136 Uiso 1 1 calc R . .
H22C H 0.1515 0.3373 0.6131 0.136 Uiso 1 1 calc R . .
C23 C 0.0926(2) 0.5038(2) 0.2743(3) 0.0358(11) Uani 1 1 d . . .
C24 C 0.1427(3) 0.5496(2) 0.3192(4) 0.0477(14) Uani 1 1 d . . .
H24 H 0.1598 0.5709 0.2925 0.057 Uiso 1 1 calc R . .
C25 C 0.1668(3) 0.5631(2) 0.4021(4) 0.0526(15) Uani 1 1 d . . .
H25 H 0.2003 0.5946 0.4331 0.063 Uiso 1 1 calc R . .
C26 C 0.1423(3) 0.5310(2) 0.4418(4) 0.0462(13) Uani 1 1 d . . .
H26 H 0.1577 0.5408 0.4989 0.055 Uiso 1 1 calc R . .
C27 C 0.0950(2) 0.4845(2) 0.3948(3) 0.0368(11) Uani 1 1 d . . .
C28 C 0.0624(2) 0.4467(2) 0.4274(3) 0.0362(11) Uani 1 1 d . . .
H28A H 0.0882 0.4081 0.4503 0.043 Uiso 1 1 calc R . .
H28B H 0.0665 0.4678 0.4756 0.043 Uiso 1 1 calc R . .
C29 C -0.0534(2) 0.4935(2) 0.3222(3) 0.0354(11) Uani 1 1 d . . .
H29A H -0.0188 0.5266 0.3547 0.043 Uiso 1 1 calc R . .
H29B H -0.0880 0.4952 0.3354 0.043 Uiso 1 1 calc R . .
C30 C -0.0489(3) 0.3933(2) 0.3825(3) 0.0385(11) Uani 1 1 d . . .
C31 C -0.0391(3) 0.4167(2) 0.4639(4) 0.0479(13) Uani 1 1 d . . .
H31A H -0.0582 0.4576 0.4531 0.072 Uiso 1 1 calc R . .
H31B H 0.0117 0.4171 0.5133 0.072 Uiso 1 1 calc R . .
H31C H -0.0645 0.3905 0.4775 0.072 Uiso 1 1 calc R . .
C32 C -0.0160(3) 0.3307(2) 0.4006(4) 0.0462(13) Uani 1 1 d . . .
H32A H -0.0413 0.3029 0.4126 0.069 Uiso 1 1 calc R . .
H32B H 0.0343 0.3324 0.4514 0.069 Uiso 1 1 calc R . .
H32C H -0.0199 0.3168 0.3495 0.069 Uiso 1 1 calc R . .
C33 C -0.1283(3) 0.3885(2) 0.3073(4) 0.0462(13) Uani 1 1 d . . .
H33A H -0.1516 0.4268 0.3004 0.069 Uiso 1 1 calc R . .
H33B H -0.1495 0.3567 0.3200 0.069 Uiso 1 1 calc R . .
H33C H -0.1347 0.3789 0.2532 0.069 Uiso 1 1 calc R . .
C1S C 0.4047(16) 0.7457(8) 0.5768(13) 0.285(16) Uani 0.50 1 d PDU . .
H1S1 H 0.4547 0.7474 0.5979 0.342 Uiso 0.50 1 calc PR A 1
H1S2 H 0.4026 0.7708 0.6177 0.342 Uiso 0.50 1 calc PR A 1
Cl4 Cl 0.3938(8) 0.6784(5) 0.5956(11) 0.134(6) Uani 0.228(6) 1 d PDU B 1
Cl5 Cl 0.3603(10) 0.7823(6) 0.4865(10) 0.149(7) Uani 0.228(6) 1 d PDU B 1
Cl4' Cl 0.414(2) 0.7084(14) 0.5128(19) 0.38(2) Uani 0.272(6) 1 d PDU B 2
Cl5' Cl 0.3213(18) 0.750(2) 0.531(3) 0.46(2) Uani 0.272(6) 1 d PDU B 2
O1S O 0.4896(12) 0.8196(9) 0.7105(17) 0.082(5) Uani 0.225(8) 1 d PU C -3
O2S O 0.4609(15) 0.6608(12) 0.706(2) 0.082(5) Uani 0.175(7) 1 d PU D -3
O3S O 0.523(3) 0.811(2) 0.679(4) 0.082(5) Uani 0.101(8) 1 d PU E -4
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
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
N2 Ni1 N1 87.43(18) . .
N2 Ni1 N4 79.93(18) . .
N1 Ni1 N4 75.6(2) . .
N2 Ni1 N3 76.5(2) . .
N1 Ni1 N3 78.9(2) . .
N4 Ni1 N3 145.80(18) . .
N2 Ni1 Cl1 177.16(15) . .
N1 Ni1 Cl1 90.37(13) . .
N4 Ni1 Cl1 97.78(11) . .
N3 Ni1 Cl1 104.84(15) . .
N2 Ni1 Cl2 89.01(14) . .
N1 Ni1 Cl2 175.62(15) . .
N4 Ni1 Cl2 106.31(15) . .
N3 Ni1 Cl2 97.75(16) . .
Cl1 Ni1 Cl2 93.27(6) . .
N5 Ni2 N5 85.3(2) 2 .
N5 Ni2 N6 78.51(15) 2 .
N5 Ni2 N6 76.98(14) . .
N5 Ni2 N6 76.98(14) 2 2
N5 Ni2 N6 78.51(15) . 2
N6 Ni2 N6 146.46(19) . 2
N5 Ni2 Cl3 175.60(12) 2 2
N5 Ni2 Cl3 91.04(10) . 2
N6 Ni2 Cl3 98.34(10) . 2
N6 Ni2 Cl3 104.66(9) 2 2
N5 Ni2 Cl3 91.04(10) 2 .
N5 Ni2 Cl3 175.60(12) . .
N6 Ni2 Cl3 104.66(9) . .
N6 Ni2 Cl3 98.34(10) 2 .
Cl3 Ni2 Cl3 92.74(6) 2 .
C5 N1 C1 121.4(6) . .
C5 N1 Ni1 120.9(5) . .
C1 N1 Ni1 117.6(5) . .
C12 N2 C8 122.9(5) . .
C12 N2 Ni1 119.5(4) . .
C8 N2 Ni1 117.4(5) . .
C7 N3 C15 113.1(6) . .
C7 N3 C6 110.3(6) . .
C15 N3 C6 110.4(6) . .
C7 N3 Ni1 99.0(4) . .
C15 N3 Ni1 120.8(4) . .
C6 N3 Ni1 102.3(4) . .
C14 N4 C13 108.4(5) . .
C14 N4 C19 110.2(5) . .
C13 N4 C19 110.6(4) . .
C14 N4 Ni1 100.9(3) . .
C13 N4 Ni1 103.7(3) . .
C19 N4 Ni1 122.0(4) . .
C23 N5 C27 121.1(4) . .
C23 N5 Ni2 121.2(3) . .
C27 N5 Ni2 117.6(3) . .
C28 N6 C29 109.2(3) . .
C28 N6 C30 112.3(4) . .
C29 N6 C30 110.5(3) . .
C28 N6 Ni2 97.5(3) . .
C29 N6 Ni2 105.4(3) . .
C30 N6 Ni2 120.9(3) . .
N1 C1 C2 120.7(8) . .
N1 C1 C14 115.5(6) . .
C2 C1 C14 123.8(8) . .
C3 C2 C1 117.0(9) . .
C3 C2 H2 121.5 . .
C1 C2 H2 121.5 . .
C2 C3 C4 123.2(9) . .
C2 C3 H3 118.4 . .
C4 C3 H3 118.4 . .
C3 C4 C5 117.0(9) . .
C3 C4 H4 121.5 . .
C5 C4 H4 121.5 . .
N1 C5 C4 120.5(8) . .
N1 C5 C6 115.2(6) . .
C4 C5 C6 123.8(8) . .
C5 C6 N3 114.4(5) . .
C5 C6 H6A 108.7 . .
N3 C6 H6A 108.7 . .
C5 C6 H6B 108.7 . .
N3 C6 H6B 108.7 . .
H6A C6 H6B 107.6 . .
N3 C7 C8 111.6(6) . .
N3 C7 H7A 109.3 . .
C8 C7 H7A 109.3 . .
N3 C7 H7B 109.3 . .
C8 C7 H7B 109.3 . .
H7A C7 H7B 108.0 . .
N2 C8 C9 117.7(8) . .
N2 C8 C7 114.8(6) . .
C9 C8 C7 127.4(7) . .
C8 C9 C10 120.3(8) . .
C8 C9 H9 119.9 . .
C10 C9 H9 119.9 . .
C11 C10 C9 119.4(7) . .
C11 C10 H10 120.3 . .
C9 C10 H10 120.3 . .
C10 C11 C12 118.9(8) . .
C10 C11 H11 120.5 . .
C12 C11 H11 120.5 . .
N2 C12 C11 120.5(6) . .
N2 C12 C13 115.4(4) . .
C11 C12 C13 123.6(6) . .
C12 C13 N4 113.7(5) . .
C12 C13 H13A 108.8 . .
N4 C13 H13A 108.8 . .
C12 C13 H13B 108.8 . .
N4 C13 H13B 108.8 . .
H13A C13 H13B 107.7 . .
C1 C14 N4 110.6(5) . .
C1 C14 H14A 109.5 . .
N4 C14 H14A 109.5 . .
C1 C14 H14B 109.5 . .
N4 C14 H14B 109.5 . .
H14A C14 H14B 108.1 . .
C16 C15 N3 108.9(6) . .
C16 C15 C17 110.4(9) . .
N3 C15 C17 112.9(7) . .
C16 C15 C18 109.1(7) . .
N3 C15 C18 107.1(7) . .
C17 C15 C18 108.4(8) . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C15 C18 H18A 109.5 . .
C15 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C15 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C20 C19 C21 110.5(7) . .
C20 C19 N4 106.8(5) . .
C21 C19 N4 113.7(8) . .
C20 C19 C22 107.5(8) . .
C21 C19 C22 109.1(6) . .
N4 C19 C22 109.1(5) . .
C19 C20 H20A 109.5 . .
C19 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C19 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C19 C21 H21A 109.5 . .
C19 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C19 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C19 C22 H22A 109.5 . .
C19 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C19 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
N5 C23 C24 120.5(5) . .
N5 C23 C29 117.0(4) . 2
C24 C23 C29 122.2(5) . 2
C25 C24 C23 118.8(5) . .
C25 C24 H24 120.6 . .
C23 C24 H24 120.6 . .
C24 C25 C26 120.5(5) . .
C24 C25 H25 119.7 . .
C26 C25 H25 119.7 . .
C27 C26 C25 117.5(5) . .
C27 C26 H26 121.3 . .
C25 C26 H26 121.3 . .
N5 C27 C26 121.4(5) . .
N5 C27 C28 114.6(4) . .
C26 C27 C28 124.0(5) . .
N6 C28 C27 110.1(4) . .
N6 C28 H28A 109.6 . .
C27 C28 H28A 109.6 . .
N6 C28 H28B 109.6 . .
C27 C28 H28B 109.6 . .
H28A C28 H28B 108.2 . .
N6 C29 C23 114.2(4) . 2
N6 C29 H29A 108.7 . .
C23 C29 H29A 108.7 2 .
N6 C29 H29B 108.7 . .
C23 C29 H29B 108.7 2 .
H29A C29 H29B 107.6 . .
N6 C30 C31 111.7(4) . .
N6 C30 C32 109.1(4) . .
C31 C30 C32 109.6(5) . .
N6 C30 C33 108.6(4) . .
C31 C30 C33 109.4(4) . .
C32 C30 C33 108.3(4) . .
C30 C31 H31A 109.5 . .
C30 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C30 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C30 C32 H32A 109.5 . .
C30 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C30 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C30 C33 H33A 109.5 . .
C30 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C30 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
Cl4 C1S Cl4' 78.5(19) . .
Cl4 C1S Cl5' 82(2) . .
Cl4' C1S Cl5' 107(3) . .
Cl4 C1S Cl5 129.2(15) . .
Cl4' C1S Cl5 74.6(18) . .
Cl5' C1S Cl5 66.1(18) . .
Cl4 C1S H1S1 105.0 . .
Cl4' C1S H1S1 69.9 . .
Cl5' C1S H1S1 171.1 . .
Cl5 C1S H1S1 105.0 . .
Cl4 C1S H1S2 105.0 . .
Cl4' C1S H1S2 175.3 . .
Cl5' C1S H1S2 76.4 . .
Cl5 C1S H1S2 105.0 . .
H1S1 C1S H1S2 105.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N2 2.008(4) .
Ni1 N1 2.013(5) .
Ni1 N4 2.292(5) .
Ni1 N3 2.336(5) .
Ni1 Cl1 2.3563(13) .
Ni1 Cl2 2.3825(17) .
Ni2 N5 2.022(4) 2
Ni2 N5 2.022(4) .
Ni2 N6 2.334(4) .
Ni2 N6 2.334(4) 2
Ni2 Cl3 2.3959(12) 2
Ni2 Cl3 2.3959(12) .
N1 C5 1.331(8) .
N1 C1 1.344(8) .
N2 C12 1.335(8) .
N2 C8 1.342(8) .
N3 C7 1.475(11) .
N3 C15 1.527(9) .
N3 C6 1.530(9) .
N4 C14 1.482(9) .
N4 C13 1.510(6) .
N4 C19 1.524(8) .
N5 C23 1.329(6) .
N5 C27 1.339(6) .
N6 C28 1.496(6) .
N6 C29 1.498(6) .
N6 C30 1.527(6) .
C1 C2 1.397(11) .
C1 C14 1.469(11) .
C2 C3 1.363(15) .
C2 H2 0.9500 .
C3 C4 1.366(15) .
C3 H3 0.9500 .
C4 C5 1.404(11) .
C4 H4 0.9500 .
C5 C6 1.474(11) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.526(12) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.396(11) .
C9 C10 1.411(14) .
C9 H9 0.9500 .
C10 C11 1.349(12) .
C10 H10 0.9500 .
C11 C12 1.403(7) .
C11 H11 0.9500 .
C12 C13 1.495(9) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C16 1.527(13) .
C15 C17 1.530(11) .
C15 C18 1.548(11) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 C20 1.522(12) .
C19 C21 1.523(12) .
C19 C22 1.551(8) .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 C24 1.395(7) .
C23 C29 1.508(7) 2
C24 C25 1.364(9) .
C24 H24 0.9500 .
C25 C26 1.400(8) .
C25 H25 0.9500 .
C26 C27 1.383(7) .
C26 H26 0.9500 .
C27 C28 1.511(7) .
C28 H28A 0.9900 .
C28 H28B 0.9900 .
C29 C23 1.508(7) 2
C29 H29A 0.9900 .
C29 H29B 0.9900 .
C30 C31 1.528(7) .
C30 C32 1.529(7) .
C30 C33 1.529(7) .
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 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
C1S Cl4 1.597(8) .
C1S Cl4' 1.598(8) .
C1S Cl5' 1.601(8) .
C1S Cl5 1.606(8) .
C1S H1S1 0.9900 .
C1S H1S2 0.9900 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N2 Ni1 N1 C5 -77.5(4) . .
N4 Ni1 N1 C5 -157.8(5) . .
N3 Ni1 N1 C5 -0.8(4) . .
Cl1 Ni1 N1 C5 104.3(4) . .
N2 Ni1 N1 C1 107.3(4) . .
N4 Ni1 N1 C1 27.0(4) . .
N3 Ni1 N1 C1 -176.0(4) . .
Cl1 Ni1 N1 C1 -70.9(4) . .
N1 Ni1 N2 C12 -76.6(4) . .
N4 Ni1 N2 C12 -0.8(4) . .
N3 Ni1 N2 C12 -155.8(4) . .
Cl2 Ni1 N2 C12 105.9(4) . .
N1 Ni1 N2 C8 108.0(5) . .
N4 Ni1 N2 C8 -176.2(5) . .
N3 Ni1 N2 C8 28.8(5) . .
Cl2 Ni1 N2 C8 -69.4(5) . .
N2 Ni1 N3 C7 -38.0(4) . .
N1 Ni1 N3 C7 -128.0(4) . .
N4 Ni1 N3 C7 -85.7(5) . .
Cl1 Ni1 N3 C7 144.6(4) . .
Cl2 Ni1 N3 C7 49.1(4) . .
N2 Ni1 N3 C15 -161.7(6) . .
N1 Ni1 N3 C15 108.3(6) . .
N4 Ni1 N3 C15 150.6(6) . .
Cl1 Ni1 N3 C15 20.9(6) . .
Cl2 Ni1 N3 C15 -74.6(6) . .
N2 Ni1 N3 C6 75.2(4) . .
N1 Ni1 N3 C6 -14.8(4) . .
N4 Ni1 N3 C6 27.5(6) . .
Cl1 Ni1 N3 C6 -102.2(4) . .
Cl2 Ni1 N3 C6 162.3(4) . .
N2 Ni1 N4 C14 -126.9(4) . .
N1 Ni1 N4 C14 -36.9(4) . .
N3 Ni1 N4 C14 -80.0(5) . .
Cl1 Ni1 N4 C14 51.4(4) . .
Cl2 Ni1 N4 C14 147.2(4) . .
N2 Ni1 N4 C13 -14.7(4) . .
N1 Ni1 N4 C13 75.3(4) . .
N3 Ni1 N4 C13 32.3(6) . .
Cl1 Ni1 N4 C13 163.6(4) . .
Cl2 Ni1 N4 C13 -100.6(4) . .
N2 Ni1 N4 C19 110.8(4) . .
N1 Ni1 N4 C19 -159.3(5) . .
N3 Ni1 N4 C19 157.7(5) . .
Cl1 Ni1 N4 C19 -70.9(4) . .
Cl2 Ni1 N4 C19 24.8(4) . .
N5 Ni2 N5 C23 -73.9(3) 2 .
N6 Ni2 N5 C23 -153.1(3) . .
N6 Ni2 N5 C23 3.8(3) 2 .
Cl3 Ni2 N5 C23 108.5(3) 2 .
N5 Ni2 N5 C27 101.9(3) 2 .
N6 Ni2 N5 C27 22.6(3) . .
N6 Ni2 N5 C27 179.5(3) 2 .
Cl3 Ni2 N5 C27 -75.7(3) 2 .
N5 Ni2 N6 C28 -125.4(3) 2 .
N5 Ni2 N6 C28 -37.7(3) . .
N6 Ni2 N6 C28 -81.7(2) 2 .
Cl3 Ni2 N6 C28 51.5(3) 2 .
Cl3 Ni2 N6 C28 146.5(2) . .
N5 Ni2 N6 C29 -13.1(3) 2 .
N5 Ni2 N6 C29 74.7(3) . .
N6 Ni2 N6 C29 30.6(2) 2 .
Cl3 Ni2 N6 C29 163.8(2) 2 .
Cl3 Ni2 N6 C29 -101.1(2) . .
N5 Ni2 N6 C30 113.0(3) 2 .
N5 Ni2 N6 C30 -159.3(3) . .
N6 Ni2 N6 C30 156.7(3) 2 .
Cl3 Ni2 N6 C30 -70.2(3) 2 .
Cl3 Ni2 N6 C30 24.9(3) . .
C5 N1 C1 C2 -3.8(8) . .
Ni1 N1 C1 C2 171.4(4) . .
C5 N1 C1 C14 175.3(5) . .
Ni1 N1 C1 C14 -9.5(6) . .
N1 C1 C2 C3 -0.9(9) . .
C14 C1 C2 C3 -179.9(6) . .
C1 C2 C3 C4 3.6(12) . .
C2 C3 C4 C5 -1.7(12) . .
C1 N1 C5 C4 5.8(8) . .
Ni1 N1 C5 C4 -169.2(5) . .
C1 N1 C5 C6 -166.9(5) . .
Ni1 N1 C5 C6 18.0(7) . .
C3 C4 C5 N1 -3.1(10) . .
C3 C4 C5 C6 169.0(7) . .
N1 C5 C6 N3 -32.6(8) . .
C4 C5 C6 N3 154.9(6) . .
C7 N3 C6 C5 132.8(6) . .
C15 N3 C6 C5 -101.6(7) . .
Ni1 N3 C6 C5 28.2(7) . .
C15 N3 C7 C8 172.1(6) . .
C6 N3 C7 C8 -63.8(7) . .
Ni1 N3 C7 C8 43.0(6) . .
C12 N2 C8 C9 -3.8(10) . .
Ni1 N2 C8 C9 171.4(6) . .
C12 N2 C8 C7 172.8(6) . .
Ni1 N2 C8 C7 -12.0(8) . .
N3 C7 C8 N2 -26.5(9) . .
N3 C7 C8 C9 149.7(8) . .
N2 C8 C9 C10 -1.1(12) . .
C7 C8 C9 C10 -177.2(8) . .
C8 C9 C10 C11 5.3(13) . .
C9 C10 C11 C12 -4.7(11) . .
C8 N2 C12 C11 4.4(9) . .
Ni1 N2 C12 C11 -170.6(4) . .
C8 N2 C12 C13 -167.5(6) . .
Ni1 N2 C12 C13 17.4(6) . .
C10 C11 C12 N2 0.0(9) . .
C10 C11 C12 C13 171.2(6) . .
N2 C12 C13 N4 -31.5(7) . .
C11 C12 C13 N4 156.9(5) . .
C14 N4 C13 C12 134.0(5) . .
C19 N4 C13 C12 -105.1(6) . .
Ni1 N4 C13 C12 27.4(6) . .
N1 C1 C14 N4 -27.0(7) . .
C2 C1 C14 N4 152.0(6) . .
C13 N4 C14 C1 -65.3(6) . .
C19 N4 C14 C1 173.4(5) . .
Ni1 N4 C14 C1 43.2(5) . .
C7 N3 C15 C16 174.6(6) . .
C6 N3 C15 C16 50.5(7) . .
Ni1 N3 C15 C16 -68.6(7) . .
C7 N3 C15 C17 51.6(10) . .
C6 N3 C15 C17 -72.5(10) . .
Ni1 N3 C15 C17 168.3(7) . .
C7 N3 C15 C18 -67.6(8) . .
C6 N3 C15 C18 168.3(7) . .
Ni1 N3 C15 C18 49.2(9) . .
C14 N4 C19 C20 173.6(5) . .
C13 N4 C19 C20 53.7(7) . .
Ni1 N4 C19 C20 -68.5(6) . .
C14 N4 C19 C21 51.4(7) . .
C13 N4 C19 C21 -68.5(8) . .
Ni1 N4 C19 C21 169.3(5) . .
C14 N4 C19 C22 -70.5(8) . .
C13 N4 C19 C22 169.5(6) . .
Ni1 N4 C19 C22 47.3(8) . .
C27 N5 C23 C24 4.8(6) . .
Ni2 N5 C23 C24 -179.7(3) . .
C27 N5 C23 C29 -168.4(4) . 2
Ni2 N5 C23 C29 7.2(5) . 2
N5 C23 C24 C25 -4.3(7) . .
C29 C23 C24 C25 168.5(5) 2 .
C23 C24 C25 C26 1.0(8) . .
C24 C25 C26 C27 1.7(8) . .
C23 N5 C27 C26 -1.9(6) . .
Ni2 N5 C27 C26 -177.6(3) . .
C23 N5 C27 C28 175.4(4) . .
Ni2 N5 C27 C28 -0.4(5) . .
C25 C26 C27 N5 -1.4(7) . .
C25 C26 C27 C28 -178.4(4) . .
C29 N6 C28 C27 -60.8(5) . .
C30 N6 C28 C27 176.2(4) . .
Ni2 N6 C28 C27 48.4(4) . .
N5 C27 C28 N6 -37.7(5) . .
C26 C27 C28 N6 139.5(4) . .
C28 N6 C29 C23 124.1(4) . 2
C30 N6 C29 C23 -111.9(4) . 2
Ni2 N6 C29 C23 20.3(4) . 2
C28 N6 C30 C31 54.1(5) . .
C29 N6 C30 C31 -68.0(5) . .
Ni2 N6 C30 C31 168.3(3) . .
C28 N6 C30 C32 -67.2(5) . .
C29 N6 C30 C32 170.6(4) . .
Ni2 N6 C30 C32 46.9(5) . .
C28 N6 C30 C33 174.9(4) . .
C29 N6 C30 C33 52.7(5) . .
Ni2 N6 C30 C33 -70.9(4) . .
