#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:30:56 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179064 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/26/4302667.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_4302667
loop_
_publ_author_name
'Peter Comba'
'Christina Haaf'
'Hubert Wadepohl'
_publ_section_title
;
Novel Bispidine Ligands and Their First-Row Transition Metal Complexes:
Trigonal Bipyramidal and Trigonal Prismatic Geometries
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6604
_journal_page_last               6614
_journal_paper_doi               10.1021/ic900571v
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C33 H41.53 Cl2 N5 Ni O9.27'
_chemical_formula_weight         786.25
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                co_ch13
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.471(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.739(7)
_cell_length_b                   19.904(11)
_cell_length_c                   16.368(9)
_cell_measurement_reflns_used    8148
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.85
_cell_measurement_theta_min      2.30
_cell_volume                     3388(3)
_computing_cell_refinement
;

SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors

 from Monte Carlo simulations.

;
_computing_data_collection       'SMART (Bruker AXS, 1997-2003)'
_computing_data_reduction        'SAINT (Bruker AXS, 1997-2008)'
_computing_molecular_graphics    'PLATON (Spek, 1980-2009)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'PLATON/FLIPPER (Spek, 2007-2009)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'CCD area detector (Bruker AXS Smart 1000)'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            73062
_diffrn_reflns_theta_full        32.11
_diffrn_reflns_theta_max         32.11
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

multi-scan from symmetry-related measurements (Blessing 1995)

SADABS (Sheldrick & Bruker AXS, 2004-2008)

;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1643
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         11145
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.332
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0308P)²+6.4967P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                7803
_reflns_number_total             11145
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900571v_si_001_10.cif
_cod_data_source_block           co_ch13
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4302667
#BEGIN Tags that were not found in dictionaries:
_audit_block_refno               793
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ni Ni 1.08733(3) 0.137858(18) 0.25751(2) 0.01320(9) Uani 1 1 d . . .
O1 O 0.5906(2) 0.10664(11) 0.22199(15) 0.0218(5) Uani 1 1 d . . .
N7 N 0.9814(2) 0.08238(12) 0.32356(15) 0.0138(4) Uani 1 1 d . . .
N3 N 0.9155(2) 0.18706(11) 0.20698(15) 0.0134(4) Uani 1 1 d . . .
N1 N 1.1461(2) 0.17045(12) 0.14907(16) 0.0174(5) Uani 1 1 d . . .
N2 N 1.1592(2) 0.23110(12) 0.29499(15) 0.0152(5) Uani 1 1 d . . .
N4 N 1.2244(2) 0.06720(12) 0.30453(16) 0.0166(5) Uani 1 1 d . . .
C1 C 0.8939(3) 0.11546(14) 0.36890(18) 0.0156(5) Uani 1 1 d . . .
H1A H 0.9451 0.1461 0.4122 0.019 Uiso 1 1 calc R . .
H1B H 0.8561 0.0806 0.3986 0.019 Uiso 1 1 calc R . .
C2 C 0.7840(3) 0.15583(14) 0.31114(18) 0.0145(5) Uani 1 1 d . . .
C3 C 0.7066(3) 0.11074(14) 0.24126(19) 0.0153(5) Uani 1 1 d . . .
C4 C 0.7933(3) 0.07804(14) 0.19133(18) 0.0149(5) Uani 1 1 d . . .
C5 C 0.9053(3) 0.04072(14) 0.25267(18) 0.0153(5) Uani 1 1 d . . .
H5A H 0.8696 0.0017 0.2767 0.018 Uiso 1 1 calc R . .
H5B H 0.9643 0.0231 0.2200 0.018 Uiso 1 1 calc R . .
C6 C 0.8369(3) 0.21187(14) 0.26392(19) 0.0153(5) Uani 1 1 d . . .
H6A H 0.7636 0.2381 0.2301 0.018 Uiso 1 1 calc R . .
H6B H 0.8902 0.2427 0.3060 0.018 Uiso 1 1 calc R . .
C7 C 0.8394(3) 0.13820(14) 0.14567(18) 0.0153(5) Uani 1 1 d . . .
H7A H 0.8928 0.1212 0.1088 0.018 Uiso 1 1 calc R . .
H7B H 0.7637 0.1612 0.1096 0.018 Uiso 1 1 calc R . .
C8 C 0.9713(3) 0.24611(14) 0.16837(18) 0.0145(5) Uani 1 1 d . . .
C9 C 1.0420(3) 0.21751(14) 0.10617(19) 0.0172(5) Uani 1 1 d . . .
H9A H 0.9802 0.1934 0.0606 0.021 Uiso 1 1 calc R . .
H9B H 1.0798 0.2548 0.0802 0.021 Uiso 1 1 calc R . .
C10 C 1.2685(3) 0.20911(16) 0.1813(2) 0.0209(6) Uani 1 1 d . . .
H10A H 1.2678 0.2494 0.1457 0.025 Uiso 1 1 calc R . .
H10B H 1.3424 0.1808 0.1770 0.025 Uiso 1 1 calc R . .
C11 C 1.2854(3) 0.23085(15) 0.2730(2) 0.0198(6) Uani 1 1 d . . .
H11A H 1.3449 0.1996 0.3108 0.024 Uiso 1 1 calc R . .
H11B H 1.3235 0.2764 0.2811 0.024 Uiso 1 1 calc R . .
C12 C 1.0689(3) 0.28073(14) 0.24148(18) 0.0154(5) Uani 1 1 d . . .
H12A H 1.1192 0.3140 0.2181 0.018 Uiso 1 1 calc R . .
H12B H 1.0219 0.3052 0.2771 0.018 Uiso 1 1 calc R . .
C13 C 1.0700(3) 0.03874(14) 0.38509(19) 0.0163(5) Uani 1 1 d . . .
H13A H 1.0260 -0.0040 0.3909 0.020 Uiso 1 1 calc R . .
H13B H 1.0920 0.0611 0.4409 0.020 Uiso 1 1 calc R . .
C14 C 1.1917(3) 0.02387(14) 0.35884(19) 0.0161(5) Uani 1 1 d . . .
C15 C 1.2680(3) -0.03028(16) 0.3925(2) 0.0260(7) Uani 1 1 d . . .
H15 H 1.2433 -0.0594 0.4317 0.031 Uiso 1 1 calc R . .
C16 C 1.3807(3) -0.04156(18) 0.3683(3) 0.0336(8) Uani 1 1 d . . .
H16 H 1.4336 -0.0790 0.3897 0.040 Uiso 1 1 calc R . .
C17 C 1.4152(3) 0.00256(17) 0.3124(2) 0.0284(7) Uani 1 1 d . . .
H17 H 1.4922 -0.0040 0.2948 0.034 Uiso 1 1 calc R . .
C18 C 1.3360(3) 0.05602(16) 0.2829(2) 0.0216(6) Uani 1 1 d . . .
H18 H 1.3610 0.0867 0.2454 0.026 Uiso 1 1 calc R . .
C19 C 0.7011(3) 0.18432(15) 0.36634(19) 0.0172(5) Uani 1 1 d . . .
C20 C 0.6947(3) 0.25251(15) 0.3825(2) 0.0198(6) Uani 1 1 d . . .
H20 H 0.7417 0.2835 0.3578 0.024 Uiso 1 1 calc R . .
C21 C 0.6193(3) 0.27594(17) 0.4351(2) 0.0233(6) Uani 1 1 d . . .
H21 H 0.6167 0.3226 0.4467 0.028 Uiso 1 1 calc R . .
C22 C 0.5486(3) 0.23153(18) 0.4702(2) 0.0244(7) Uani 1 1 d . . .
H22 H 0.4970 0.2475 0.5055 0.029 Uiso 1 1 calc R . .
C23 C 0.5535(3) 0.16345(18) 0.4537(2) 0.0238(6) Uani 1 1 d . . .
H23 H 0.5042 0.1328 0.4771 0.029 Uiso 1 1 calc R . .
C24 C 0.6302(3) 0.13986(16) 0.4030(2) 0.0202(6) Uani 1 1 d . . .
H24 H 0.6345 0.0930 0.3931 0.024 Uiso 1 1 calc R . .
C25 C 0.7218(3) 0.02595(14) 0.12861(19) 0.0172(5) Uani 1 1 d . . .
C26 C 0.6670(3) -0.02885(15) 0.1604(2) 0.0206(6) Uani 1 1 d . . .
H26 H 0.6711 -0.0311 0.2190 0.025 Uiso 1 1 calc R . .
C27 C 0.6067(3) -0.07980(16) 0.1073(2) 0.0248(7) Uani 1 1 d . . .
H27 H 0.5719 -0.1173 0.1297 0.030 Uiso 1 1 calc R . .
C28 C 0.5974(3) -0.07600(16) 0.0215(2) 0.0260(7) Uani 1 1 d . . .
H28 H 0.5557 -0.1108 -0.0150 0.031 Uiso 1 1 calc R . .
C29 C 0.6487(3) -0.02152(17) -0.0107(2) 0.0240(7) Uani 1 1 d . . .
H29 H 0.6407 -0.0184 -0.0697 0.029 Uiso 1 1 calc R . .
C30 C 0.7121(3) 0.02894(15) 0.0427(2) 0.0197(6) Uani 1 1 d . . .
H30 H 0.7490 0.0657 0.0201 0.024 Uiso 1 1 calc R . .
C31 C 0.8721(3) 0.29711(15) 0.1223(2) 0.0188(6) Uani 1 1 d . . .
H31A H 0.8072 0.2742 0.0784 0.028 Uiso 1 1 calc R . .
H31B H 0.9150 0.3316 0.0965 0.028 Uiso 1 1 calc R . .
H31C H 0.8304 0.3182 0.1626 0.028 Uiso 1 1 calc R . .
C32 C 1.1645(3) 0.11983(17) 0.0869(2) 0.0254(7) Uani 1 1 d . . .
H32A H 1.0837 0.0957 0.0645 0.038 Uiso 1 1 calc R . .
H32B H 1.2315 0.0879 0.1145 0.038 Uiso 1 1 calc R . .
H32C H 1.1906 0.1424 0.0406 0.038 Uiso 1 1 calc R . .
C33 C 1.1806(3) 0.24741(16) 0.38571(19) 0.0207(6) Uani 1 1 d . . .
H33A H 1.2343 0.2126 0.4195 0.031 Uiso 1 1 calc R . .
H33B H 1.0976 0.2494 0.4004 0.031 Uiso 1 1 calc R . .
H33C H 1.2239 0.2910 0.3972 0.031 Uiso 1 1 calc R . .
Cl1 Cl 0.25777(7) 0.40329(3) 0.09663(5) 0.01867(14) Uani 1 1 d D . .
O11 O 0.1251(2) 0.38337(14) 0.08156(19) 0.0383(7) Uani 1 1 d D . .
O12 O 0.3080(3) 0.38092(15) 0.02834(17) 0.0369(6) Uani 1 1 d D . .
O13 O 0.3310(3) 0.37453(13) 0.17412(16) 0.0379(6) Uani 1 1 d D . .
O14 O 0.2651(3) 0.47531(11) 0.10215(17) 0.0325(6) Uani 1 1 d D . .
Cl2 Cl 0.89861(9) 0.41288(4) 0.36395(5) 0.02698(18) Uani 1 1 d D . .
O21A O 0.7597(4) 0.4180(2) 0.3618(3) 0.0547(14) Uani 0.677(4) 1 d PD A 1
O22A O 0.9029(4) 0.41251(19) 0.2763(2) 0.0345(10) Uani 0.677(4) 1 d PD A 1
O23A O 0.9605(6) 0.4714(2) 0.4030(3) 0.0587(15) Uani 0.677(4) 1 d PD A 1
O24A O 0.9469(4) 0.35314(17) 0.4045(2) 0.0304(9) Uani 0.677(4) 1 d PD A 1
O21B O 1.0426(5) 0.4052(4) 0.3726(5) 0.036(2) Uani 0.323(4) 1 d PD A 2
O22B O 0.8411(7) 0.3740(3) 0.2931(4) 0.0258(17) Uani 0.323(4) 1 d PD A 2
O23B O 0.8768(9) 0.4810(3) 0.3630(6) 0.035(2) Uani 0.323(4) 1 d PD A 2
O24B O 0.8858(7) 0.3802(3) 0.4411(4) 0.0270(18) Uani 0.323(4) 1 d PD A 2
O2 O 1.4179(12) -0.1776(8) 0.2921(9) 0.063(5) Uani 0.269(11) 1 d PG B 3
H1O2 H 1.5028 -0.1587 0.3107 0.082 Uiso 0.269(11) 1 d PG B 3
H2O2 H 1.3713 -0.1513 0.2449 0.082 Uiso 0.269(11) 1 d PG B 3
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ni N2 109.25(10) . . ?
N4 Ni N3 164.34(9) . . ?
N2 Ni N3 85.55(10) . . ?
N4 Ni N7 82.79(10) . . ?
N2 Ni N7 122.84(10) . . ?
N3 Ni N7 84.82(10) . . ?
N4 Ni N1 100.84(10) . . ?
N2 Ni N1 78.76(10) . . ?
N3 Ni N1 86.74(10) . . ?
N7 Ni N1 155.94(10) . . ?
C13 N7 C1 107.4(2) . . ?
C13 N7 C5 109.7(2) . . ?
C1 N7 C5 110.0(2) . . ?
C13 N7 Ni 108.85(17) . . ?
C1 N7 Ni 121.43(18) . . ?
C5 N7 Ni 98.94(17) . . ?
C7 N3 C6 109.7(2) . . ?
C7 N3 C8 115.5(2) . . ?
C6 N3 C8 110.3(2) . . ?
C7 N3 Ni 104.19(17) . . ?
C6 N3 Ni 119.66(18) . . ?
C8 N3 Ni 97.30(16) . . ?
C32 N1 C9 108.5(2) . . ?
C32 N1 C10 109.6(2) . . ?
C9 N1 C10 109.3(2) . . ?
C32 N1 Ni 119.0(2) . . ?
C9 N1 Ni 103.88(17) . . ?
C10 N1 Ni 106.21(18) . . ?
C33 N2 C11 108.8(2) . . ?
C33 N2 C12 110.9(2) . . ?
C11 N2 C12 110.8(2) . . ?
C33 N2 Ni 116.88(18) . . ?
C11 N2 Ni 102.88(17) . . ?
C12 N2 Ni 106.35(17) . . ?
C14 N4 C18 117.5(3) . . ?
C14 N4 Ni 114.08(19) . . ?
C18 N4 Ni 128.1(2) . . ?
N7 C1 C2 114.0(2) . . ?
N7 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
N7 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.6 . . ?
C3 C2 C19 111.9(2) . . ?
C3 C2 C1 110.1(2) . . ?
C19 C2 C1 107.5(2) . . ?
C3 C2 C6 104.4(2) . . ?
C19 C2 C6 111.7(2) . . ?
C1 C2 C6 111.3(2) . . ?
O1 C3 C2 124.6(3) . . ?
O1 C3 C4 123.9(3) . . ?
C2 C3 C4 111.1(2) . . ?
C25 C4 C3 112.2(2) . . ?
C25 C4 C5 106.8(2) . . ?
C3 C4 C5 109.6(2) . . ?
C25 C4 C7 111.5(2) . . ?
C3 C4 C7 103.8(2) . . ?
C5 C4 C7 113.0(2) . . ?
N7 C5 C4 115.0(2) . . ?
N7 C5 H5A 108.5 . . ?
C4 C5 H5A 108.5 . . ?
N7 C5 H5B 108.5 . . ?
C4 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
N3 C6 C2 114.2(2) . . ?
N3 C6 H6A 108.7 . . ?
C2 C6 H6A 108.7 . . ?
N3 C6 H6B 108.7 . . ?
C2 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
N3 C7 C4 111.5(2) . . ?
N3 C7 H7A 109.3 . . ?
C4 C7 H7A 109.3 . . ?
N3 C7 H7B 109.3 . . ?
C4 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C9 C8 N3 107.6(2) . . ?
C9 C8 C31 108.7(2) . . ?
N3 C8 C31 114.7(2) . . ?
C9 C8 C12 109.3(2) . . ?
N3 C8 C12 106.5(2) . . ?
C31 C8 C12 109.9(2) . . ?
N1 C9 C8 111.1(2) . . ?
N1 C9 H9A 109.4 . . ?
C8 C9 H9A 109.4 . . ?
N1 C9 H9B 109.4 . . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N1 C10 C11 111.7(2) . . ?
N1 C10 H10A 109.3 . . ?
C11 C10 H10A 109.3 . . ?
N1 C10 H10B 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
N2 C11 C10 110.3(2) . . ?
N2 C11 H11A 109.6 . . ?
C10 C11 H11A 109.6 . . ?
N2 C11 H11B 109.6 . . ?
C10 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
N2 C12 C8 111.9(2) . . ?
N2 C12 H12A 109.2 . . ?
C8 C12 H12A 109.2 . . ?
N2 C12 H12B 109.2 . . ?
C8 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
N7 C13 C14 112.2(2) . . ?
N7 C13 H13A 109.2 . . ?
C14 C13 H13A 109.2 . . ?
N7 C13 H13B 109.2 . . ?
C14 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
N4 C14 C15 122.4(3) . . ?
N4 C14 C13 116.8(2) . . ?
C15 C14 C13 120.7(3) . . ?
C14 C15 C16 119.1(3) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C15 C16 C17 119.0(3) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C18 C17 C16 118.7(3) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
N4 C18 C17 123.2(3) . . ?
N4 C18 H18 118.4 . . ?
C17 C18 H18 118.4 . . ?
C20 C19 C24 118.6(3) . . ?
C20 C19 C2 122.7(3) . . ?
C24 C19 C2 118.7(3) . . ?
C19 C20 C21 120.5(3) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C22 C21 C20 120.3(3) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C23 119.6(3) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C22 C23 C24 120.3(3) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C19 120.7(3) . . ?
C23 C24 H24 119.6 . . ?
C19 C24 H24 119.6 . . ?
C30 C25 C26 118.6(3) . . ?
C30 C25 C4 123.5(3) . . ?
C26 C25 C4 117.9(3) . . ?
C27 C26 C25 120.7(3) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C28 C27 C26 120.0(3) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C29 C28 C27 119.7(3) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 120.4(3) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C25 C30 C29 120.5(3) . . ?
C25 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C8 C31 H31A 109.5 . . ?
C8 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C8 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N1 C32 H32A 109.5 . . ?
N1 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N1 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N2 C33 H33A 109.5 . . ?
N2 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N2 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O12 Cl1 O13 109.68(17) . . ?
O12 Cl1 O14 109.56(17) . . ?
O13 Cl1 O14 109.47(16) . . ?
O12 Cl1 O11 109.32(17) . . ?
O13 Cl1 O11 110.03(17) . . ?
O14 Cl1 O11 108.77(16) . . ?
O23B Cl2 O24A 152.4(4) . . ?
O23B Cl2 O22B 119.7(5) . . ?
O24A Cl2 O22B 87.6(3) . . ?
O23B Cl2 O23A 41.6(4) . . ?
O24A Cl2 O23A 114.2(3) . . ?
O22B Cl2 O23A 152.8(4) . . ?
O23B Cl2 O22A 92.4(4) . . ?
O24A Cl2 O22A 111.5(2) . . ?
O22B Cl2 O22A 45.1(3) . . ?
O23A Cl2 O22A 108.9(3) . . ?
O23B Cl2 O24B 113.4(4) . . ?
O24A Cl2 O24B 46.6(3) . . ?
O22B Cl2 O24B 110.6(4) . . ?
O23A Cl2 O24B 96.4(4) . . ?
O22A Cl2 O24B 152.9(3) . . ?
O23B Cl2 O21A 76.4(4) . . ?
O24A Cl2 O21A 108.7(2) . . ?
O22B Cl2 O21A 77.7(4) . . ?
O23A Cl2 O21A 108.1(3) . . ?
O22A Cl2 O21A 104.9(3) . . ?
O24B Cl2 O21A 74.9(4) . . ?
O23B Cl2 O21B 105.4(5) . . ?
O24A Cl2 O21B 67.9(4) . . ?
O22B Cl2 O21B 104.4(4) . . ?
O23A Cl2 O21B 71.8(4) . . ?
O22A Cl2 O21B 79.0(4) . . ?
O24B Cl2 O21B 100.8(4) . . ?
O21A Cl2 O21B 175.7(4) . . ?
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
Ni N4 2.042(3) . ?
Ni N2 2.044(3) . ?
Ni N3 2.070(3) . ?
Ni N7 2.073(2) . ?
Ni N1 2.129(3) . ?
O1 C3 1.209(3) . ?
N7 C13 1.482(4) . ?
N7 C1 1.488(3) . ?
N7 C5 1.492(4) . ?
N3 C7 1.487(4) . ?
N3 C6 1.490(4) . ?
N3 C8 1.526(4) . ?
N1 C32 1.480(4) . ?
N1 C9 1.493(4) . ?
N1 C10 1.501(4) . ?
N2 C33 1.481(4) . ?
N2 C11 1.487(4) . ?
N2 C12 1.503(4) . ?
N4 C14 1.346(4) . ?
N4 C18 1.352(4) . ?
C1 C2 1.541(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.526(4) . ?
C2 C19 1.527(4) . ?
C2 C6 1.544(4) . ?
C3 C4 1.530(4) . ?
C4 C25 1.524(4) . ?
C4 C5 1.550(4) . ?
C4 C7 1.556(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.524(4) . ?
C8 C31 1.527(4) . ?
C8 C12 1.542(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.528(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.503(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.382(4) . ?
C15 C16 1.382(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.384(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.372(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.388(4) . ?
C19 C24 1.397(4) . ?
C20 C21 1.401(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.380(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.385(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.389(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.385(4) . ?
C25 C26 1.400(4) . ?
C26 C27 1.386(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.384(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.380(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.392(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
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 . ?
Cl1 O12 1.428(2) . ?
Cl1 O13 1.434(3) . ?
Cl1 O14 1.437(2) . ?
Cl1 O11 1.440(3) . ?
Cl2 O23B 1.376(5) . ?
Cl2 O24A 1.397(3) . ?
Cl2 O22B 1.402(5) . ?
Cl2 O23A 1.412(4) . ?
Cl2 O22A 1.447(3) . ?
Cl2 O24B 1.458(5) . ?
Cl2 O21A 1.487(4) . ?
Cl2 O21B 1.525(5) . ?
O2 H1O2 0.9637 . ?
O2 H2O2 0.9635 . ?
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
N4 Ni N7 C13 16.67(18) . . . . ?
N2 Ni N7 C13 -91.62(19) . . . . ?
N3 Ni N7 C13 -172.92(18) . . . . ?
N1 Ni N7 C13 117.1(2) . . . . ?
N4 Ni N7 C1 142.0(2) . . . . ?
N2 Ni N7 C1 33.7(2) . . . . ?
N3 Ni N7 C1 -47.5(2) . . . . ?
N1 Ni N7 C1 -117.5(3) . . . . ?
N4 Ni N7 C5 -97.77(16) . . . . ?
N2 Ni N7 C5 153.94(15) . . . . ?
N3 Ni N7 C5 72.64(16) . . . . ?
N1 Ni N7 C5 2.7(3) . . . . ?
N4 Ni N3 C7 -36.9(4) . . . . ?
N2 Ni N3 C7 161.74(17) . . . . ?
N7 Ni N3 C7 -74.67(17) . . . . ?
N1 Ni N3 C7 82.77(17) . . . . ?
N4 Ni N3 C6 86.0(4) . . . . ?
N2 Ni N3 C6 -75.32(19) . . . . ?
N7 Ni N3 C6 48.27(19) . . . . ?
N1 Ni N3 C6 -154.3(2) . . . . ?
N4 Ni N3 C8 -155.6(3) . . . . ?
N2 Ni N3 C8 43.03(16) . . . . ?
N7 Ni N3 C8 166.63(16) . . . . ?
N1 Ni N3 C8 -35.93(16) . . . . ?
N4 Ni N1 C32 53.7(2) . . . . ?
N2 Ni N1 C32 161.4(2) . . . . ?
N3 Ni N1 C32 -112.5(2) . . . . ?
N7 Ni N1 C32 -42.9(4) . . . . ?
N4 Ni N1 C9 174.38(17) . . . . ?
N2 Ni N1 C9 -77.91(18) . . . . ?
N3 Ni N1 C9 8.19(17) . . . . ?
N7 Ni N1 C9 77.7(3) . . . . ?
N4 Ni N1 C10 -70.33(19) . . . . ?
N2 Ni N1 C10 37.37(17) . . . . ?
N3 Ni N1 C10 123.48(18) . . . . ?
N7 Ni N1 C10 -167.0(2) . . . . ?
N4 Ni N2 C33 -69.7(2) . . . . ?
N3 Ni N2 C33 105.1(2) . . . . ?
N7 Ni N2 C33 24.2(2) . . . . ?
N1 Ni N2 C33 -167.4(2) . . . . ?
N4 Ni N2 C11 49.4(2) . . . . ?
N3 Ni N2 C11 -135.85(18) . . . . ?
N7 Ni N2 C11 143.24(17) . . . . ?
N1 Ni N2 C11 -48.30(18) . . . . ?
N4 Ni N2 C12 165.95(16) . . . . ?
N3 Ni N2 C12 -19.30(17) . . . . ?
N7 Ni N2 C12 -100.20(18) . . . . ?
N1 Ni N2 C12 68.26(18) . . . . ?
N2 Ni N4 C14 116.9(2) . . . . ?
N3 Ni N4 C14 -43.4(5) . . . . ?
N7 Ni N4 C14 -5.4(2) . . . . ?
N1 Ni N4 C14 -161.3(2) . . . . ?
N2 Ni N4 C18 -68.8(3) . . . . ?
N3 Ni N4 C18 131.0(4) . . . . ?
N7 Ni N4 C18 168.9(3) . . . . ?
N1 Ni N4 C18 13.0(3) . . . . ?
C13 N7 C1 C2 -172.6(2) . . . . ?
C5 N7 C1 C2 -53.3(3) . . . . ?
Ni N7 C1 C2 61.3(3) . . . . ?
N7 C1 C2 C3 56.0(3) . . . . ?
N7 C1 C2 C19 178.1(2) . . . . ?
N7 C1 C2 C6 -59.3(3) . . . . ?
C19 C2 C3 O1 11.9(4) . . . . ?
C1 C2 C3 O1 131.4(3) . . . . ?
C6 C2 C3 O1 -109.1(3) . . . . ?
C19 C2 C3 C4 -175.2(2) . . . . ?
C1 C2 C3 C4 -55.8(3) . . . . ?
C6 C2 C3 C4 63.8(3) . . . . ?
O1 C3 C4 C25 -14.4(4) . . . . ?
C2 C3 C4 C25 172.7(2) . . . . ?
O1 C3 C4 C5 -132.8(3) . . . . ?
C2 C3 C4 C5 54.2(3) . . . . ?
O1 C3 C4 C7 106.2(3) . . . . ?
C2 C3 C4 C7 -66.8(3) . . . . ?
C13 N7 C5 C4 170.4(2) . . . . ?
C1 N7 C5 C4 52.5(3) . . . . ?
Ni N7 C5 C4 -75.8(2) . . . . ?
C25 C4 C5 N7 -175.4(2) . . . . ?
C3 C4 C5 N7 -53.7(3) . . . . ?
C7 C4 C5 N7 61.6(3) . . . . ?
C7 N3 C6 C2 55.8(3) . . . . ?
C8 N3 C6 C2 -175.9(2) . . . . ?
Ni N3 C6 C2 -64.4(3) . . . . ?
C3 C2 C6 N3 -57.2(3) . . . . ?
C19 C2 C6 N3 -178.3(2) . . . . ?
C1 C2 C6 N3 61.5(3) . . . . ?
C6 N3 C7 C4 -57.8(3) . . . . ?
C8 N3 C7 C4 176.9(2) . . . . ?
Ni N3 C7 C4 71.5(2) . . . . ?
C25 C4 C7 N3 -176.7(2) . . . . ?
C3 C4 C7 N3 62.2(3) . . . . ?
C5 C4 C7 N3 -56.4(3) . . . . ?
C7 N3 C8 C9 -50.9(3) . . . . ?
C6 N3 C8 C9 -175.9(2) . . . . ?
Ni N3 C8 C9 58.7(2) . . . . ?
C7 N3 C8 C31 70.3(3) . . . . ?
C6 N3 C8 C31 -54.8(3) . . . . ?
Ni N3 C8 C31 179.8(2) . . . . ?
C7 N3 C8 C12 -167.9(2) . . . . ?
C6 N3 C8 C12 67.1(3) . . . . ?
Ni N3 C8 C12 -58.3(2) . . . . ?
C32 N1 C9 C8 151.0(2) . . . . ?
C10 N1 C9 C8 -89.5(3) . . . . ?
Ni N1 C9 C8 23.5(3) . . . . ?
N3 C8 C9 N1 -58.8(3) . . . . ?
C31 C8 C9 N1 176.4(2) . . . . ?
C12 C8 C9 N1 56.4(3) . . . . ?
C32 N1 C10 C11 -147.8(3) . . . . ?
C9 N1 C10 C11 93.5(3) . . . . ?
Ni N1 C10 C11 -18.1(3) . . . . ?
C33 N2 C11 C10 175.8(2) . . . . ?
C12 N2 C11 C10 -62.1(3) . . . . ?
Ni N2 C11 C10 51.2(3) . . . . ?
N1 C10 C11 N2 -21.2(3) . . . . ?
C33 N2 C12 C8 -138.4(2) . . . . ?
C11 N2 C12 C8 100.7(3) . . . . ?
Ni N2 C12 C8 -10.4(3) . . . . ?
C9 C8 C12 N2 -67.5(3) . . . . ?
N3 C8 C12 N2 48.4(3) . . . . ?
C31 C8 C12 N2 173.3(2) . . . . ?
C1 N7 C13 C14 -157.9(2) . . . . ?
C5 N7 C13 C14 82.5(3) . . . . ?
Ni N7 C13 C14 -24.7(3) . . . . ?
C18 N4 C14 C15 0.3(4) . . . . ?
Ni N4 C14 C15 175.3(3) . . . . ?
C18 N4 C14 C13 177.5(3) . . . . ?
Ni N4 C14 C13 -7.6(3) . . . . ?
N7 C13 C14 N4 22.1(4) . . . . ?
N7 C13 C14 C15 -160.6(3) . . . . ?
N4 C14 C15 C16 -1.5(5) . . . . ?
C13 C14 C15 C16 -178.6(3) . . . . ?
C14 C15 C16 C17 1.3(6) . . . . ?
C15 C16 C17 C18 0.0(6) . . . . ?
C14 N4 C18 C17 1.1(5) . . . . ?
Ni N4 C18 C17 -173.1(3) . . . . ?
C16 C17 C18 N4 -1.2(6) . . . . ?
C3 C2 C19 C20 -127.3(3) . . . . ?
C1 C2 C19 C20 111.7(3) . . . . ?
C6 C2 C19 C20 -10.6(4) . . . . ?
C3 C2 C19 C24 53.6(4) . . . . ?
C1 C2 C19 C24 -67.3(3) . . . . ?
C6 C2 C19 C24 170.3(3) . . . . ?
C24 C19 C20 C21 0.5(5) . . . . ?
C2 C19 C20 C21 -178.6(3) . . . . ?
C19 C20 C21 C22 -1.2(5) . . . . ?
C20 C21 C22 C23 0.5(5) . . . . ?
C21 C22 C23 C24 0.8(5) . . . . ?
C22 C23 C24 C19 -1.5(5) . . . . ?
C20 C19 C24 C23 0.8(5) . . . . ?
C2 C19 C24 C23 180.0(3) . . . . ?
C3 C4 C25 C30 122.4(3) . . . . ?
C5 C4 C25 C30 -117.5(3) . . . . ?
C7 C4 C25 C30 6.5(4) . . . . ?
C3 C4 C25 C26 -59.7(3) . . . . ?
C5 C4 C25 C26 60.4(3) . . . . ?
C7 C4 C25 C26 -175.7(2) . . . . ?
C30 C25 C26 C27 1.4(4) . . . . ?
C4 C25 C26 C27 -176.5(3) . . . . ?
C25 C26 C27 C28 -1.7(5) . . . . ?
C26 C27 C28 C29 0.3(5) . . . . ?
C27 C28 C29 C30 1.3(5) . . . . ?
C26 C25 C30 C29 0.2(4) . . . . ?
C4 C25 C30 C29 178.0(3) . . . . ?
C28 C29 C30 C25 -1.5(4) . . . . ?
