#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:26:06 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224501 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/07/7700716.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_7700716
loop_
_publ_author_name
'Zhao, Qianyi'
'Guan, Xin-Ting'
'Dou, Ting'
'Cao, Hou-Ji'
'Ma, Na-Na'
'Xu, Ting'
'Gao, Peng-Hui'
'Kong, Xiao-Hua'
'Zhang, Jie'
'Chen, Xuenian'
_publ_section_title
;
 Synthesis and characterization of bis(pyrazolyl)borate Ni(ii) complexes:
 ligand rearrangement and transformation.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13242
_journal_page_last               13247
_journal_paper_doi               10.1039/c9dt02287b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C32 H44 B2 Br4 N8 Ni, C3 H7'
_chemical_formula_sum            'C35 H51 B2 Br4 N8 Ni'
_chemical_formula_weight         983.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-23 deposited with the CCDC.    2019-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.2210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1521(2)
_cell_length_b                   19.2678(3)
_cell_length_c                   18.7249(2)
_cell_measurement_reflns_used    9212
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      71.0640
_cell_measurement_theta_min      4.2470
_cell_volume                     3932.36(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0528
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -52.00  32.00   1.00    6.75    --  -35.37  57.00 -60.00   84
  2  ω   -103.00 -19.00   1.00    6.75    --  -35.37 -57.00  30.00   84
  3  ω   -103.00 -19.00   1.00    6.75    --  -35.37 -57.00 150.00   84
  4  ω      1.00  74.00   1.00    6.75    --   35.37 -99.00 120.00   73
  5  ω     19.00 103.00   1.00    6.75    --   35.37  57.00-120.00   84
  6  ω     23.00  89.00   1.00    6.75    --   35.37-125.00 -30.00   66
  7  ω     40.00 125.00   1.00   27.02    --  106.50 -61.00  90.00   85
  8  ω     37.00 109.00   1.00   27.02    --  106.50 -95.00-120.00   72
  9  ω     89.00 175.00   1.00   27.02    --  106.50  45.00-120.00   86
 10  ω     37.00  86.00   1.00   27.02    --  106.50 -95.00 120.00   49
 11  ω     43.00 100.00   1.00   27.02    --  106.50 -95.00  60.00   57
 12  ω     42.00 108.00   1.00   27.02    --  106.50 -95.00 -30.00   66
 13  ω    112.00 171.00   1.00   27.02    --  106.50  61.00  90.00   59
 14  ω     66.00 118.00   1.00   27.02    --  106.50 178.00   0.00   52
 15  ω     89.00 146.00   1.00   27.02    --  106.50  61.00-150.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0679458000
_diffrn_orient_matrix_UB_12      0.0700513000
_diffrn_orient_matrix_UB_13      -0.0127172000
_diffrn_orient_matrix_UB_21      0.1198754000
_diffrn_orient_matrix_UB_22      0.0358721000
_diffrn_orient_matrix_UB_23      -0.0081438000
_diffrn_orient_matrix_UB_31      -0.0318434000
_diffrn_orient_matrix_UB_32      -0.0143336000
_diffrn_orient_matrix_UB_33      -0.0827306000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18596
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.257
_diffrn_reflns_theta_min         4.259
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.758
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       block
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.365
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         7491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0414P)²+6.0362P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6779
_reflns_number_total             7491
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02287b2.cif
_cod_data_source_block           gxt-201812-20
_cod_depositor_comments
'Adding full bibliography for 7700714--7700718.cif.'
_cod_database_code               7700716
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 H1 B1 N1 Ni1 Br1 '
_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.
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C5(H5), C9(H9), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B),
  C16(H16A,H16B), C00U(H00A,H00B), C019(H01D,H01E)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C21(H21), C25(H25), C29(H29)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C32(H32A,H32B,
 H32C), C01B(H01A,H01B,H01C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.256
_oxdiff_exptl_absorpt_empirical_full_min 0.775
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Br1 Br 0.22639(4) 0.94996(2) 0.34234(2) 0.03430(10) Uani 1 1 d .
Br2 Br 0.60198(4) 0.66182(2) 0.64952(2) 0.04399(12) Uani 1 1 d .
Br3 Br 0.91614(4) 0.87948(2) 0.33384(2) 0.03828(11) Uani 1 1 d .
Br4 Br 0.82679(4) 0.42969(2) 0.35085(2) 0.03935(11) Uani 1 1 d .
Ni1 Ni 0.49826(5) 0.68103(3) 0.32242(3) 0.01870(12) Uani 1 1 d .
N1 N 0.3713(2) 0.76082(14) 0.31816(14) 0.0206(5) Uani 1 1 d .
N2 N 0.2818(2) 0.74453(14) 0.35566(13) 0.0190(5) Uani 1 1 d .
N3 N 0.5001(2) 0.66624(14) 0.42924(14) 0.0225(5) Uani 1 1 d .
N4 N 0.3876(2) 0.66273(14) 0.44744(14) 0.0203(5) Uani 1 1 d .
N5 N 0.6405(2) 0.74052(14) 0.30864(14) 0.0223(5) Uani 1 1 d .
N6 N 0.6878(2) 0.72493(14) 0.24867(14) 0.0211(5) Uani 1 1 d .
N7 N 0.5959(2) 0.59318(14) 0.30746(14) 0.0211(5) Uani 1 1 d .
N8 N 0.6581(2) 0.59867(14) 0.25211(14) 0.0213(5) Uani 1 1 d .
C1 C 0.2764(3) 0.61226(16) 0.31977(17) 0.0209(6) Uani 1 1 d .
H1 H 0.355269 0.617585 0.305242 0.025 Uiso 1 1 calc R
C2 C 0.1729(3) 0.6281(2) 0.25267(18) 0.0289(7) Uani 1 1 d .
H2A H 0.191114 0.671894 0.231659 0.035 Uiso 1 1 calc R
H2B H 0.173207 0.592338 0.216277 0.035 Uiso 1 1 calc R
C3 C 0.0447(4) 0.6324(3) 0.2684(2) 0.0413(9) Uani 1 1 d .
H3A H 0.013358 0.585570 0.269979 0.050 Uiso 1 1 calc R
H3B H -0.008166 0.656139 0.227979 0.050 Uiso 1 1 calc R
C4 C 0.0348(3) 0.6694(2) 0.3394(2) 0.0312(8) Uani 1 1 d .
H4A H -0.041686 0.655593 0.352132 0.037 Uiso 1 1 calc R
H4B H 0.030207 0.718975 0.330129 0.037 Uiso 1 1 calc R
C5 C 0.1407(3) 0.65582(18) 0.40650(18) 0.0255(7) Uani 1 1 d .
H5 H 0.133513 0.688769 0.445236 0.031 Uiso 1 1 calc R
C6 C 0.1336(4) 0.5815(2) 0.4356(2) 0.0347(8) Uani 1 1 d .
H6A H 0.191650 0.577459 0.482012 0.042 Uiso 1 1 calc R
H6B H 0.052189 0.574297 0.444928 0.042 Uiso 1 1 calc R
C7 C 0.1596(4) 0.5246(2) 0.3858(2) 0.0373(9) Uani 1 1 d .
H7A H 0.087726 0.518288 0.346888 0.045 Uiso 1 1 calc R
H7B H 0.173127 0.481657 0.413336 0.045 Uiso 1 1 calc R
C8 C 0.2711(3) 0.53854(18) 0.3516(2) 0.0301(7) Uani 1 1 d .
H8A H 0.270599 0.505018 0.312920 0.036 Uiso 1 1 calc R
H8B H 0.345142 0.530917 0.388584 0.036 Uiso 1 1 calc R
C9 C 0.4820(3) 0.67198(18) 0.17197(17) 0.0237(7) Uani 1 1 d .
H9 H 0.447630 0.679437 0.215403 0.028 Uiso 1 1 calc R
C10 C 0.4545(4) 0.7372(2) 0.1234(2) 0.0368(9) Uani 1 1 d .
H10A H 0.366489 0.740418 0.105423 0.044 Uiso 1 1 calc R
H10B H 0.479833 0.777771 0.153603 0.044 Uiso 1 1 calc R
C11 C 0.5168(4) 0.7396(2) 0.0579(2) 0.0413(10) Uani 1 1 d .
H11A H 0.473245 0.709018 0.020030 0.050 Uiso 1 1 calc R
H11B H 0.510848 0.786410 0.038265 0.050 Uiso 1 1 calc R
C12 C 0.6522(3) 0.7182(2) 0.07712(19) 0.0323(8) Uani 1 1 d .
H12A H 0.699572 0.756487 0.102434 0.039 Uiso 1 1 calc R
H12B H 0.680032 0.710420 0.032091 0.039 Uiso 1 1 calc R
C13 C 0.6796(3) 0.65260(18) 0.12507(17) 0.0257(7) Uani 1 1 d .
H13 H 0.768707 0.646341 0.138612 0.031 Uiso 1 1 calc R
C14 C 0.6225(4) 0.5870(2) 0.08387(19) 0.0328(8) Uani 1 1 d .
H14A H 0.645889 0.585735 0.036853 0.039 Uiso 1 1 calc R
H14B H 0.658427 0.546623 0.111198 0.039 Uiso 1 1 calc R
C15 C 0.4819(4) 0.5805(2) 0.0707(2) 0.0400(9) Uani 1 1 d .
H15A H 0.445802 0.607629 0.027844 0.048 Uiso 1 1 calc R
H15B H 0.459529 0.532390 0.060064 0.048 Uiso 1 1 calc R
C16 C 0.4261(3) 0.6046(2) 0.1350(2) 0.0355(8) Uani 1 1 d .
H16A H 0.436873 0.567955 0.171320 0.043 Uiso 1 1 calc R
H16B H 0.338676 0.611404 0.117432 0.043 Uiso 1 1 calc R
C17 C 0.2235(3) 0.80185(17) 0.36968(17) 0.0227(6) Uani 1 1 d .
H17 H 0.160369 0.804073 0.395088 0.027 Uiso 1 1 calc R
C18 C 0.2736(3) 0.85684(17) 0.33978(18) 0.0248(7) Uani 1 1 d .
C19 C 0.3657(3) 0.83020(17) 0.30764(18) 0.0244(7) Uani 1 1 d .
C20 C 0.4411(3) 0.87039(19) 0.2655(2) 0.0334(8) Uani 1 1 d .
H20A H 0.512201 0.843797 0.261477 0.050 Uiso 1 1 calc GR
H20B H 0.466509 0.913238 0.290303 0.050 Uiso 1 1 calc GR
H20C H 0.393434 0.880066 0.217569 0.050 Uiso 1 1 calc GR
C21 C 0.4032(3) 0.66123(17) 0.52011(17) 0.0252(7) Uani 1 1 d .
H21 H 0.340930 0.659738 0.546182 0.030 Uiso 1 1 calc R
C22 C 0.5274(3) 0.66228(18) 0.54992(18) 0.0278(7) Uani 1 1 d .
C23 C 0.5864(3) 0.66513(18) 0.49158(18) 0.0263(7) Uani 1 1 d .
C24 C 0.7199(3) 0.6634(2) 0.4918(2) 0.0400(9) Uani 1 1 d .
H24A H 0.731222 0.658248 0.442701 0.060 Uiso 1 1 calc GR
H24B H 0.757318 0.625001 0.520878 0.060 Uiso 1 1 calc GR
H24C H 0.757347 0.705916 0.512116 0.060 Uiso 1 1 calc GR
C25 C 0.7843(3) 0.76609(17) 0.24843(18) 0.0243(7) Uani 1 1 d .
H25 H 0.833194 0.765421 0.213899 0.029 Uiso 1 1 calc R
C26 C 0.7990(3) 0.80968(17) 0.30806(19) 0.0253(7) Uani 1 1 d .
C27 C 0.7075(3) 0.79222(17) 0.34512(18) 0.0254(7) Uani 1 1 d .
C28 C 0.6787(4) 0.8256(2) 0.4110(2) 0.0366(8) Uani 1 1 d .
H28A H 0.661431 0.873938 0.401353 0.055 Uiso 1 1 calc GR
H28B H 0.747740 0.821031 0.451242 0.055 Uiso 1 1 calc GR
H28C H 0.608469 0.803510 0.423084 0.055 Uiso 1 1 calc GR
C29 C 0.7420(3) 0.54836(17) 0.25810(18) 0.0247(7) Uani 1 1 d .
H29 H 0.796593 0.541349 0.227474 0.030 Uiso 1 1 calc R
C30 C 0.7330(3) 0.50886(17) 0.31787(18) 0.0264(7) Uani 1 1 d .
C31 C 0.6413(3) 0.53756(17) 0.34759(17) 0.0239(6) Uani 1 1 d .
C32 C 0.5986(4) 0.5103(2) 0.4120(2) 0.0407(9) Uani 1 1 d .
H32A H 0.548340 0.544513 0.428795 0.061 Uiso 1 1 calc GR
H32B H 0.668185 0.499963 0.450340 0.061 Uiso 1 1 calc GR
H32C H 0.551560 0.468812 0.398576 0.061 Uiso 1 1 calc GR
B1 B 0.2700(3) 0.66867(18) 0.38292(18) 0.0187(7) Uani 1 1 d .
B2 B 0.6284(3) 0.66249(18) 0.19882(18) 0.0198(7) Uani 1 1 d .
C00U C 0.5169(3) 0.96157(18) 0.5009(2) 0.0316(8) Uani 1 1 d .
H00A H 0.490949 0.942412 0.452180 0.038 Uiso 1 1 calc R
H00B H 0.605443 0.957100 0.514933 0.038 Uiso 1 1 calc R
C01B C 0.4885(4) 0.8427(2) 0.5533(2) 0.0444(10) Uani 1 1 d .
H01A H 0.458841 0.824192 0.505253 0.067 Uiso 1 1 calc GR
H01B H 0.449407 0.819129 0.587442 0.067 Uiso 1 1 calc GR
H01C H 0.575628 0.836193 0.567258 0.067 Uiso 1 1 calc GR
C019 C 0.4591(4) 0.9198(2) 0.5535(2) 0.0406(9) Uani 1 1 d .
H01D H 0.370825 0.925814 0.540632 0.049 Uiso 1 1 calc R
H01E H 0.487699 0.937833 0.602491 0.049 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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
N3 Ni1 N1 90.36(11) . .
N3 Ni1 N5 111.35(11) . .
N3 Ni1 N7 97.12(11) . .
N5 Ni1 N1 97.03(11) . .
N5 Ni1 N7 89.83(11) . .
N7 Ni1 N1 167.28(11) . .
N2 N1 Ni1 111.97(19) . .
C19 N1 Ni1 138.3(2) . .
C19 N1 N2 106.5(3) . .
N1 N2 B1 120.1(2) . .
C17 N2 N1 110.4(3) . .
C17 N2 B1 129.1(3) . .
N4 N3 Ni1 115.88(19) . .
C23 N3 Ni1 135.8(2) . .
C23 N3 N4 107.9(3) . .
N3 N4 B1 117.4(2) . .
C21 N4 N3 109.1(3) . .
C21 N4 B1 133.2(3) . .
N6 N5 Ni1 115.4(2) . .
C27 N5 Ni1 136.5(2) . .
C27 N5 N6 108.1(3) . .
N5 N6 B2 117.7(2) . .
C25 N6 N5 108.8(3) . .
C25 N6 B2 133.3(3) . .
N8 N7 Ni1 113.97(19) . .
C31 N7 Ni1 136.5(2) . .
C31 N7 N8 107.1(3) . .
N7 N8 B2 117.9(2) . .
C29 N8 N7 109.8(3) . .
C29 N8 B2 132.0(3) . .
C2 C1 H1 108.2 . .
C2 C1 C8 114.4(3) . .
C2 C1 B1 108.7(3) . .
C8 C1 H1 108.2 . .
C8 C1 B1 108.9(3) . .
B1 C1 H1 108.2 . .
C1 C2 H2A 108.5 . .
C1 C2 H2B 108.5 . .
H2A C2 H2B 107.5 . .
C3 C2 C1 115.0(3) . .
C3 C2 H2A 108.5 . .
C3 C2 H2B 108.5 . .
C2 C3 H3A 108.3 . .
C2 C3 H3B 108.3 . .
C2 C3 C4 115.8(3) . .
H3A C3 H3B 107.4 . .
C4 C3 H3A 108.3 . .
C4 C3 H3B 108.3 . .
C3 C4 H4A 108.2 . .
C3 C4 H4B 108.2 . .
C3 C4 C5 116.1(3) . .
H4A C4 H4B 107.4 . .
C5 C4 H4A 108.2 . .
C5 C4 H4B 108.2 . .
C4 C5 H5 108.7 . .
C4 C5 B1 108.9(3) . .
C6 C5 C4 110.8(3) . .
C6 C5 H5 108.7 . .
C6 C5 B1 110.8(3) . .
B1 C5 H5 108.7 . .
C5 C6 H6A 108.5 . .
C5 C6 H6B 108.5 . .
H6A C6 H6B 107.5 . .
C7 C6 C5 115.2(3) . .
C7 C6 H6A 108.5 . .
C7 C6 H6B 108.5 . .
C6 C7 H7A 108.7 . .
C6 C7 H7B 108.7 . .
C6 C7 C8 114.2(3) . .
H7A C7 H7B 107.6 . .
C8 C7 H7A 108.7 . .
C8 C7 H7B 108.7 . .
C1 C8 H8A 108.5 . .
C1 C8 H8B 108.5 . .
C7 C8 C1 114.9(3) . .
C7 C8 H8A 108.5 . .
C7 C8 H8B 108.5 . .
H8A C8 H8B 107.5 . .
C10 C9 H9 107.8 . .
C10 C9 B2 109.7(3) . .
C16 C9 H9 107.8 . .
C16 C9 C10 114.3(3) . .
C16 C9 B2 109.3(3) . .
B2 C9 H9 107.8 . .
C9 C10 H10A 108.4 . .
C9 C10 H10B 108.4 . .
H10A C10 H10B 107.5 . .
C11 C10 C9 115.4(3) . .
C11 C10 H10A 108.4 . .
C11 C10 H10B 108.4 . .
C10 C11 H11A 108.9 . .
C10 C11 H11B 108.9 . .
H11A C11 H11B 107.7 . .
C12 C11 C10 113.2(3) . .
C12 C11 H11A 108.9 . .
C12 C11 H11B 108.9 . .
C11 C12 H12A 108.5 . .
C11 C12 H12B 108.5 . .
C11 C12 C13 114.9(3) . .
H12A C12 H12B 107.5 . .
C13 C12 H12A 108.5 . .
C13 C12 H12B 108.5 . .
C12 C13 H13 108.4 . .
C12 C13 C14 111.7(3) . .
C12 C13 B2 109.8(3) . .
C14 C13 H13 108.4 . .
C14 C13 B2 109.9(3) . .
B2 C13 H13 108.4 . .
C13 C14 H14A 108.2 . .
C13 C14 H14B 108.2 . .
H14A C14 H14B 107.4 . .
C15 C14 C13 116.4(3) . .
C15 C14 H14A 108.2 . .
C15 C14 H14B 108.2 . .
C14 C15 H15A 108.6 . .
C14 C15 H15B 108.6 . .
H15A C15 H15B 107.6 . .
C16 C15 C14 114.6(3) . .
C16 C15 H15A 108.6 . .
C16 C15 H15B 108.6 . .
C9 C16 H16A 108.6 . .
C9 C16 H16B 108.6 . .
C15 C16 C9 114.5(3) . .
C15 C16 H16A 108.6 . .
C15 C16 H16B 108.6 . .
H16A C16 H16B 107.6 . .
N2 C17 H17 126.2 . .
N2 C17 C18 107.5(3) . .
C18 C17 H17 126.2 . .
C17 C18 Br1 126.0(3) . .
C17 C18 C19 107.0(3) . .
C19 C18 Br1 126.9(3) . .
N1 C19 C18 108.5(3) . .
N1 C19 C20 125.4(3) . .
C18 C19 C20 126.1(3) . .
C19 C20 H20A 109.5 . .
C19 C20 H20B 109.5 . .
C19 C20 H20C 109.5 . .
H20A C20 H20B 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
N4 C21 H21 125.8 . .
N4 C21 C22 108.3(3) . .
C22 C21 H21 125.8 . .
C21 C22 Br2 126.8(3) . .
C21 C22 C23 106.5(3) . .
C23 C22 Br2 126.7(3) . .
N3 C23 C22 108.1(3) . .
N3 C23 C24 122.3(3) . .
C22 C23 C24 129.5(3) . .
C23 C24 H24A 109.5 . .
C23 C24 H24B 109.5 . .
C23 C24 H24C 109.5 . .
H24A C24 H24B 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
N6 C25 H25 125.8 . .
N6 C25 C26 108.4(3) . .
C26 C25 H25 125.8 . .
C25 C26 Br3 127.2(3) . .
C25 C26 C27 106.4(3) . .
C27 C26 Br3 126.3(3) . .
N5 C27 C26 108.3(3) . .
N5 C27 C28 123.3(3) . .
C26 C27 C28 128.3(3) . .
C27 C28 H28A 109.5 . .
C27 C28 H28B 109.5 . .
C27 C28 H28C 109.5 . .
H28A C28 H28B 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
N8 C29 H29 126.3 . .
N8 C29 C30 107.4(3) . .
C30 C29 H29 126.3 . .
C29 C30 Br4 125.8(3) . .
C29 C30 C31 107.2(3) . .
C31 C30 Br4 127.0(3) . .
N7 C31 C30 108.5(3) . .
N7 C31 C32 126.1(3) . .
C30 C31 C32 125.4(3) . .
C31 C32 H32A 109.5 . .
C31 C32 H32B 109.5 . .
C31 C32 H32C 109.5 . .
H32A C32 H32B 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
N2 B1 N4 101.7(2) . .
N2 B1 C1 111.7(2) . .
N2 B1 C5 112.0(3) . .
N4 B1 C1 110.5(2) . .
N4 B1 C5 115.0(3) . .
C5 B1 C1 106.1(3) . .
N6 B2 C9 111.6(3) . .
N6 B2 C13 114.6(3) . .
N8 B2 N6 102.4(2) . .
N8 B2 C9 110.4(3) . .
N8 B2 C13 112.7(3) . .
C13 B2 C9 105.3(3) . .
C00U C00U H00A 109.0 3_676 .
C00U C00U H00B 109.0 3_676 .
H00A C00U H00B 107.8 . .
C019 C00U C00U 113.1(4) . 3_676
C019 C00U H00A 109.0 . .
C019 C00U H00B 109.0 . .
H01A C01B H01B 109.5 . .
H01A C01B H01C 109.5 . .
H01B C01B H01C 109.5 . .
C019 C01B H01A 109.5 . .
C019 C01B H01B 109.5 . .
C019 C01B H01C 109.5 . .
C00U C019 C01B 113.3(3) . .
C00U C019 H01D 108.9 . .
C00U C019 H01E 108.9 . .
C01B C019 H01D 108.9 . .
C01B C019 H01E 108.9 . .
H01D C019 H01E 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 C18 1.873(3) .
Br2 C22 1.874(3) .
Br3 C26 1.866(3) .
Br4 C30 1.879(3) .
Ni1 N1 2.080(3) .
Ni1 N3 2.016(3) .
Ni1 N5 2.017(3) .
Ni1 N7 2.063(3) .
N1 N2 1.372(4) .
N1 C19 1.351(4) .
N2 C17 1.336(4) .
N2 B1 1.563(4) .
N3 N4 1.369(4) .
N3 C23 1.347(4) .
N4 C21 1.335(4) .
N4 B1 1.588(4) .
N5 N6 1.371(4) .
N5 C27 1.342(4) .
N6 C25 1.338(4) .
N6 B2 1.580(4) .
N7 N8 1.368(4) .
N7 C31 1.345(4) .
N8 C29 1.336(4) .
N8 B2 1.574(4) .
C1 H1 0.9800 .
C1 C2 1.546(4) .
C1 C8 1.546(4) .
C1 B1 1.619(5) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C2 C3 1.523(5) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C3 C4 1.533(5) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 C5 1.554(5) .
C5 H5 0.9800 .
C5 C6 1.541(5) .
C5 B1 1.614(5) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 C7 1.506(6) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 C8 1.538(5) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 H9 0.9800 .
C9 C10 1.544(5) .
C9 C16 1.540(5) .
C9 B2 1.614(5) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C10 C11 1.534(5) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C11 C12 1.532(5) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C12 C13 1.544(5) .
C13 H13 0.9800 .
C13 C14 1.546(5) .
C13 B2 1.613(4) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C14 C15 1.540(5) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C15 C16 1.539(5) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 H17 0.9300 .
C17 C18 1.372(5) .
C18 C19 1.393(5) .
C19 C20 1.487(5) .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C21 H21 0.9300 .
C21 C22 1.380(5) .
C22 C23 1.391(5) .
C23 C24 1.488(5) .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C25 H25 0.9300 .
C25 C26 1.379(5) .
C26 C27 1.391(5) .
C27 C28 1.486(5) .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
C28 H28C 0.9600 .
C29 H29 0.9300 .
C29 C30 1.375(5) .
C30 C31 1.379(5) .
C31 C32 1.484(5) .
C32 H32A 0.9600 .
C32 H32B 0.9600 .
C32 H32C 0.9600 .
C00U C00U 1.527(7) 3_676
C00U H00A 0.9700 .
C00U H00B 0.9700 .
C00U C019 1.517(5) .
C01B H01A 0.9600 .
C01B H01B 0.9600 .
C01B H01C 0.9600 .
C01B C019 1.520(6) .
C019 H01D 0.9700 .
C019 H01E 0.9700 .
