# Electronic Supplementary Material (ESI) for Green Chemistry.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[(LH)Ni(mu-Cl)2Ni(LH)]Cl2
_database_code_depnum_ccdc_archive 'CCDC 1878190'
loop_
_audit_author_name
_audit_author_address
'Ray J. Butcher'
;Howard University
United States of America
;
_audit_update_record             
;
2019-03-21 deposited with the CCDC.	2019-04-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H32 Cl2 N8 Ni2, 2(C H4 O), 2(Cl)'
_chemical_formula_sum            'C30 H40 Cl4 N8 Ni2 O2'
_chemical_formula_weight         803.92

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   17.2098(11)
_cell_length_b                   8.7962(5)
_cell_length_c                   12.4668(7)
_cell_angle_alpha                90
_cell_angle_beta                 112.273(2)
_cell_angle_gamma                90
_cell_volume                     1746.42(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3417
_cell_measurement_theta_min      2.553
_cell_measurement_theta_max      28.251

_exptl_crystal_description       prism
_exptl_crystal_colour            green-blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_F_000             832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    1.425
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5688
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Apex 2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8942
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.558
_diffrn_reflns_theta_max         28.347
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2313
_reflns_number_gt                1800
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Apex 2'
_computing_cell_refinement       'Bruker Apex 2'
_computing_data_reduction        'Bruker Saint'
_computing_structure_solution    'Shelxt (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0347P)²+2.8309P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2313
_refine_ls_number_parameters     132
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.0896
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Ni Ni 0.47307(3) 0.000000 0.62084(4) 0.01538(14) Uani 1 2 d S T P . .
Cl1 Cl 0.39878(5) 0.000000 0.41456(7) 0.0203(2) Uani 1 2 d S T P . .
Cl2 Cl 0.500000 0.500000 0.500000 0.0179(3) Uani 1 4 d S T P . .
Cl3 Cl 0.500000 0.500000 1.000000 0.0481(5) Uani 1 4 d S T P . .
N1 N 0.36518(18) 0.000000 0.6469(2) 0.0186(6) Uani 1 2 d S T P . .
N2 N 0.46478(15) 0.2370(2) 0.65602(18) 0.0216(5) Uani 1 1 d . . . . .
H2N H 0.4735(17) 0.293(3) 0.610(2) 0.025(8) Uiso 1 1 d . . . . .
N3 N 0.53534(18) 0.000000 0.7924(2) 0.0159(6) Uani 1 2 d S T P . .
C1 C 0.2175(3) 0.000000 0.6789(3) 0.0362(11) Uani 1 2 d S T P . .
H1A H 0.165013 0.000002 0.687596 0.043 Uiso 1 2 calc R U P . .
C2 C 0.25551(18) 0.1361(4) 0.6725(2) 0.0324(7) Uani 1 1 d . . . . .
H2A H 0.230584 0.230243 0.679118 0.039 Uiso 1 1 calc R U . . .
C3 C 0.33053(17) 0.1323(3) 0.6565(2) 0.0229(6) Uani 1 1 d . . . . .
C4 C 0.37811(19) 0.2714(3) 0.6448(3) 0.0311(7) Uani 1 1 d . . . . .
H4A H 0.347615 0.318893 0.568306 0.037 Uiso 1 1 calc R U . . .
H4B H 0.379880 0.346022 0.705183 0.037 Uiso 1 1 calc R U . . .
C5 C 0.5301(2) 0.2701(3) 0.7712(2) 0.0315(7) Uani 1 1 d . . . . .
H5A H 0.509823 0.351666 0.808824 0.038 Uiso 1 1 calc R U . . .
H5B H 0.581178 0.307671 0.761227 0.038 Uiso 1 1 calc R U . . .
C6 C 0.55207(17) 0.1327(3) 0.8483(2) 0.0200(5) Uani 1 1 d . . . . .
C7 C 0.58925(17) 0.1365(3) 0.9681(2) 0.0244(6) Uani 1 1 d . . . . .
H7A H 0.601650 0.230603 1.008500 0.029 Uiso 1 1 calc R U . . .
C8 C 0.6079(2) 0.000000 1.0274(3) 0.0265(9) Uani 1 2 d S T P . .
H8A H 0.633684 -0.000001 1.109653 0.032 Uiso 1 2 calc R U P . .
O1M O 0.3209(3) 0.500000 0.8302(3) 0.0728(13) Uani 1 2 d DS T P . .
H1M H 0.3771(16) 0.500000 0.875(5) 0.109 Uiso 1 2 d DS U P . .
C1M C 0.2660(3) 0.500000 0.8884(5) 0.0583(16) Uani 1 2 d DS T P . .
H1M1 H 0.229(2) 0.410(4) 0.864(3) 0.087 Uiso 1 1 d D U . . .
H1M2 H 0.292(3) 0.500000 0.980(3) 0.087 Uiso 1 2 d DS U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N3 1.996(3) . ?
Ni N1 2.002(3) . ?
Ni N2 2.146(2) . ?
Ni N2 2.146(2) 6 ?
Ni Cl1 2.3990(9) . ?
Ni Cl1 2.4076(10) 5_656 ?
N1 C3 1.334(3) . ?
N1 C3 1.334(3) 6 ?
N2 C4 1.476(4) . ?
N2 C5 1.479(3) . ?
N2 H2N 0.82(3) . ?
N3 C6 1.334(3) . ?
N3 C6 1.334(3) 6 ?
C1 C2 1.381(4) . ?
C1 C2 1.381(4) 6 ?
C1 H1A 0.9500 . ?
C2 C3 1.380(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.510(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.501(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.385(3) . ?
C7 C8 1.383(3) . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
O1M C1M 1.393(6) . ?
O1M H1M 0.92(2) . ?
C1M H1M1 0.99(3) . ?
C1M H1M2 1.05(3) . ?
C1M H1M1 0.99(3) 6_565 ?

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
N3 Ni N1 88.89(11) . . ?
N3 Ni N2 80.29(6) . . ?
N1 Ni N2 80.17(6) . . ?
N3 Ni N2 80.29(6) . 6 ?
N1 Ni N2 80.17(6) . 6 ?
N2 Ni N2 152.50(11) . 6 ?
N3 Ni Cl1 179.75(9) . . ?
N1 Ni Cl1 91.36(8) . . ?
N2 Ni Cl1 99.75(6) . . ?
N2 Ni Cl1 99.75(6) 6 . ?
N3 Ni Cl1 92.25(8) . 5_656 ?
N1 Ni Cl1 178.86(8) . 5_656 ?
N2 Ni Cl1 100.02(6) . 5_656 ?
N2 Ni Cl1 100.02(6) 6 5_656 ?
Cl1 Ni Cl1 87.50(3) . 5_656 ?
Ni Cl1 Ni 92.50(3) . 5_656 ?
C3 N1 C3 121.6(3) . 6 ?
C3 N1 Ni 119.21(16) . . ?
C3 N1 Ni 119.21(16) 6 . ?
C4 N2 C5 114.9(2) . . ?
C4 N2 Ni 108.87(16) . . ?
C5 N2 Ni 107.77(16) . . ?
C4 N2 H2N 105(2) . . ?
C5 N2 H2N 106.9(19) . . ?
Ni N2 H2N 114(2) . . ?
C6 N3 C6 122.1(3) . 6 ?
C6 N3 Ni 118.79(15) . . ?
C6 N3 Ni 118.79(15) 6 . ?
C2 C1 C2 120.3(4) . 6 ?
C2 C1 H1A 119.9 . . ?
C2 C1 H1A 119.9 6 . ?
C3 C2 C1 118.5(3) . . ?
C3 C2 H2A 120.8 . . ?
C1 C2 H2A 120.8 . . ?
N1 C3 C2 120.6(3) . . ?
N1 C3 C4 114.9(2) . . ?
C2 C3 C4 124.5(2) . . ?
N2 C4 C3 112.9(2) . . ?
N2 C4 H4A 109.0 . . ?
C3 C4 H4A 109.0 . . ?
N2 C4 H4B 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
N2 C5 C6 112.1(2) . . ?
N2 C5 H5A 109.2 . . ?
C6 C5 H5A 109.2 . . ?
N2 C5 H5B 109.2 . . ?
C6 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
N3 C6 C7 120.3(2) . . ?
N3 C6 C5 114.7(2) . . ?
C7 C6 C5 124.9(2) . . ?
C8 C7 C6 118.3(2) . . ?
C8 C7 H7A 120.8 . . ?
C6 C7 H7A 120.8 . . ?
C7 C8 C7 120.5(3) . 6 ?
C7 C8 H8A 119.7 . . ?
C7 C8 H8A 119.7 6 . ?
C1M O1M H1M 117(5) . . ?
O1M C1M H1M1 109(2) . . ?
O1M C1M H1M2 118(3) . . ?
H1M1 C1M H1M2 107(2) . . ?
O1M C1M H1M1 109(2) . 6_565 ?
H1M1 C1M H1M1 107(5) . 6_565 ?
H1M2 C1M H1M1 107(2) . 6_565 ?

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
C2 C1 C2 C3 1.9(6) 6 . . . ?
C3 N1 C3 C2 -2.4(5) 6 . . . ?
Ni N1 C3 C2 178.9(2) . . . . ?
C3 N1 C3 C4 179.3(2) 6 . . . ?
Ni N1 C3 C4 0.6(3) . . . . ?
C1 C2 C3 N1 0.2(4) . . . . ?
C1 C2 C3 C4 178.4(3) . . . . ?
C5 N2 C4 C3 -99.9(3) . . . . ?
Ni N2 C4 C3 21.0(3) . . . . ?
N1 C3 C4 N2 -15.3(3) . . . . ?
C2 C3 C4 N2 166.5(2) . . . . ?
C4 N2 C5 C6 94.7(3) . . . . ?
Ni N2 C5 C6 -26.9(3) . . . . ?
C6 N3 C6 C7 1.1(5) 6 . . . ?
Ni N3 C6 C7 174.9(2) . . . . ?
C6 N3 C6 C5 179.2(2) 6 . . . ?
Ni N3 C6 C5 -7.0(3) . . . . ?
N2 C5 C6 N3 23.4(4) . . . . ?
N2 C5 C6 C7 -158.5(2) . . . . ?
N3 C6 C7 C8 -0.3(4) . . . . ?
C5 C6 C7 C8 -178.3(3) . . . . ?
C6 C7 C8 C7 -0.3(5) . . . 6 ?

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
N2 H2N Cl2 0.82(3) 2.42(3) 3.225(2) 168(3) . yes
C4 H4B O1M 0.99 2.55 3.475(4) 155.8 . yes
C5 H5A Cl3 0.99 2.78 3.690(3) 153.4 . yes
C7 H7A Cl3 0.95 2.92 3.633(3) 132.5 . yes
O1M H1M Cl3 0.92(2) 2.10(2) 3.006(4) 171(6) . yes

_refine_diff_density_max         0.946
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.089

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[(LH)Ni(mu-H)2Ni(LH)]I2
_database_code_depnum_ccdc_archive 'CCDC 1878195'
loop_
_audit_author_name
_audit_author_address
'Sakthi Raje'
;Indian Institute of Technology Kanpur
India
;
_audit_update_record             
;
2018-11-09 deposited with the CCDC.	2019-04-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H34 N8 Ni2, I2'
_chemical_formula_sum            'C28 H34 I2 N8 Ni2'
_chemical_formula_weight         853.85

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.1186(6)
_cell_length_b                   18.4249(7)
_cell_length_c                   23.5902(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6571.3(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9902
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      24.57

_exptl_crystal_description       prism
_exptl_crystal_colour            green-brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_F_000             3360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    3.056
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5754
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5808
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.373
_diffrn_reflns_theta_max         25.091
_diffrn_reflns_theta_full        25.091
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5808
_reflns_number_gt                4078
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0573P)²+46.5065P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5808
_refine_ls_number_parameters     400
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0601
_refine_ls_wR_factor_ref         0.1510
_refine_ls_wR_factor_gt          0.1353
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
I1 I 0.69797(4) -0.03204(3) 0.66735(3) 0.0460(2) Uani 1 1 d . . . . .
I2A I 0.4400(17) 0.4913(5) 0.6008(4) 0.080(4) Uani 0.208(15) 1 d . U P A 1
I2B I 0.4863(10) 0.4933(3) 0.5991(4) 0.078(2) Uani 0.313(15) 1 d . U P B 2
I2C I 0.26698(16) 0.51607(9) 0.60099(8) 0.0578(9) Uani 0.337(2) 1 d . U P C 3
I2D I 0.1799(3) 0.5383(2) 0.6019(2) 0.0536(19) Uani 0.145(2) 1 d . U P D 4
Ni1 Ni 0.55434(6) 0.22836(5) 0.68155(4) 0.0273(2) Uani 1 1 d . . . . .
N1A N 0.4427(4) 0.2096(3) 0.7257(3) 0.0327(15) Uani 1 1 d . . . . .
N2A N 0.5847(4) 0.1219(4) 0.7193(3) 0.0388(17) Uani 1 1 d . . . . .
H2AB H 0.6172 0.0914 0.6911 0.047 Uiso 1 1 calc R U . . .
N3A N 0.6105(4) 0.2588(3) 0.7550(3) 0.0309(15) Uani 1 1 d . . . . .
N4A N 0.5040(4) 0.3392(3) 0.6899(3) 0.0372(16) Uani 1 1 d . . . . .
H4AB H 0.5046 0.3630 0.6518 0.045 Uiso 1 1 calc R U . . .
C1A C 0.3934(5) 0.2662(5) 0.7412(3) 0.0359(19) Uani 1 1 d . . . . .
C2A C 0.3292(5) 0.2584(5) 0.7832(3) 0.040(2) Uani 1 1 d . . . . .
H2AA H 0.2939 0.2987 0.7941 0.048 Uiso 1 1 calc R U . . .
C3A C 0.3173(5) 0.1918(5) 0.8087(4) 0.046(2) Uani 1 1 d . . . . .
H3AA H 0.2720 0.1855 0.8361 0.055 Uiso 1 1 calc R U . . .
C4A C 0.3718(6) 0.1338(5) 0.7942(4) 0.049(2) Uani 1 1 d . . . . .
H4AA H 0.3666 0.0881 0.8126 0.058 Uiso 1 1 calc R U . . .
C5A C 0.4342(5) 0.1452(4) 0.7516(4) 0.038(2) Uani 1 1 d . . . . .
C6A C 0.4977(6) 0.0892(5) 0.7311(4) 0.055(3) Uani 1 1 d . . . . .
H6AA H 0.5042 0.0508 0.7601 0.065 Uiso 1 1 calc R U . . .
H6AB H 0.4743 0.0664 0.6961 0.065 Uiso 1 1 calc R U . . .
C7A C 0.6391(6) 0.1319(5) 0.7693(4) 0.050(2) Uani 1 1 d . . . . .
H7AA H 0.6999 0.1152 0.7608 0.060 Uiso 1 1 calc R U . . .
H7AB H 0.6157 0.1008 0.8001 0.060 Uiso 1 1 calc R U . . .
C8A C 0.6432(5) 0.2090(5) 0.7902(3) 0.039(2) Uani 1 1 d . . . . .
C9A C 0.6807(6) 0.2286(7) 0.8410(4) 0.062(3) Uani 1 1 d . . . . .
H9AA H 0.7056 0.1931 0.8655 0.075 Uiso 1 1 calc R U . . .
C10A C 0.6812(7) 0.2994(8) 0.8551(4) 0.077(4) Uani 1 1 d . . . . .
H10A H 0.7074 0.3142 0.8898 0.093 Uiso 1 1 calc R U . . .
C11A C 0.6438(6) 0.3509(6) 0.8197(4) 0.058(3) Uani 1 1 d . . . . .
H11A H 0.6434 0.4007 0.8300 0.070 Uiso 1 1 calc R U . . .
C12A C 0.6074(5) 0.3285(5) 0.7691(3) 0.038(2) Uani 1 1 d . . . . .
C13A C 0.5656(6) 0.3769(5) 0.7271(4) 0.049(2) Uani 1 1 d . . . . .
H13A H 0.5337 0.4160 0.7473 0.058 Uiso 1 1 calc R U . . .
H13B H 0.6124 0.3998 0.7038 0.058 Uiso 1 1 calc R U . . .
C14A C 0.4124(5) 0.3358(5) 0.7106(4) 0.045(2) Uani 1 1 d . . . . .
H14A H 0.3714 0.3404 0.6780 0.054 Uiso 1 1 calc R U . . .
H14B H 0.4015 0.3771 0.7364 0.054 Uiso 1 1 calc R U . . .
Ni2 Ni 0.61030(6) 0.22141(5) 0.57845(4) 0.0296(3) Uani 1 1 d . . . . .
N1B N 0.7268(4) 0.2269(4) 0.5359(3) 0.0398(17) Uani 1 1 d . . . . .
N2B N 0.6046(5) 0.3337(4) 0.5469(3) 0.0495(19) Uani 1 1 d . . . . .
H2BB H 0.5757 0.3661 0.5755 0.059 Uiso 1 1 calc R U . . .
N3B N 0.5503(4) 0.2062(3) 0.5039(3) 0.0320(15) Uani 1 1 d . . . . .
N4B N 0.6365(4) 0.1053(3) 0.5637(3) 0.0326(15) Uani 1 1 d . . . . .
H4BB H 0.6331 0.0790 0.6008 0.039 Uiso 1 1 calc R U . . .
C1B C 0.7613(5) 0.1646(6) 0.5159(3) 0.047(2) Uani 1 1 d . . . . .
C2B C 0.8257(6) 0.1684(8) 0.4737(4) 0.067(3) Uani 1 1 d . . . . .
H2BA H 0.8495 0.1249 0.4584 0.080 Uiso 1 1 calc R U . . .
C3B C 0.8546(7) 0.2327(9) 0.4546(5) 0.079(4) Uani 1 1 d . . . . .
H3BA H 0.9015 0.2345 0.4279 0.095 Uiso 1 1 calc R U . . .
C4B C 0.8171(7) 0.2956(8) 0.4731(4) 0.071(4) Uani 1 1 d . . . . .
H4BA H 0.8347 0.3411 0.4579 0.085 Uiso 1 1 calc R U . . .
C5B C 0.7506(7) 0.2914(6) 0.5159(4) 0.060(3) Uani 1 1 d . . . . .
C6B C 0.7007(7) 0.3539(5) 0.5398(4) 0.061(3) Uani 1 1 d . . . . .
H6BA H 0.7058 0.3961 0.5141 0.074 Uiso 1 1 calc R U . . .
H6BB H 0.7260 0.3676 0.5770 0.074 Uiso 1 1 calc R U . . .
C7B C 0.5555(6) 0.3356(5) 0.4929(4) 0.047(2) Uani 1 1 d . . . . .
H7BA H 0.5928 0.3598 0.4640 0.057 Uiso 1 1 calc R U . . .
H7BB H 0.5017 0.3655 0.4981 0.057 Uiso 1 1 calc R U . . .
C8B C 0.5285(5) 0.2628(5) 0.4707(4) 0.040(2) Uani 1 1 d . . . . .
C9B C 0.4840(6) 0.2530(5) 0.4209(4) 0.052(2) Uani 1 1 d . . . . .
H9BA H 0.4680 0.2935 0.3982 0.062 Uiso 1 1 calc R U . . .
C10B C 0.4621(6) 0.1823(5) 0.4038(4) 0.047(2) Uani 1 1 d . . . . .
H10B H 0.4288 0.1746 0.3701 0.056 Uiso 1 1 calc R U . . .
C11B C 0.4892(6) 0.1247(5) 0.4359(3) 0.042(2) Uani 1 1 d . . . . .
H11B H 0.4776 0.0763 0.4241 0.050 Uiso 1 1 calc R U . . .
C12B C 0.5336(5) 0.1383(4) 0.4859(3) 0.0348(19) Uani 1 1 d . . . . .
C13B C 0.5643(5) 0.0802(4) 0.5271(3) 0.038(2) Uani 1 1 d . . . . .
H13C H 0.5138 0.0650 0.5510 0.046 Uiso 1 1 calc R U . . .
H13D H 0.5844 0.0372 0.5054 0.046 Uiso 1 1 calc R U . . .
C14B C 0.7255(6) 0.0962(5) 0.5402(4) 0.051(2) Uani 1 1 d . . . . .
H14C H 0.7239 0.0586 0.5102 0.061 Uiso 1 1 calc R U . . .
H14D H 0.7657 0.0789 0.5705 0.061 Uiso 1 1 calc R U . . .
H1 H 0.634(5) 0.232(4) 0.641(3) 0.05(2) Uiso 1 1 d . . . . .
H2 H 0.533(4) 0.203(3) 0.622(3) 0.024(18) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N3A 2.010(6) . ?
Ni1 N1A 2.014(6) . ?
Ni1 N4A 2.189(6) . ?
Ni1 N2A 2.202(6) . ?
Ni1 Ni2 2.5784(13) . ?
Ni1 H1 1.53(8) . ?
Ni1 H2 1.51(6) . ?
N1A C1A 1.332(10) . ?
N1A C5A 1.340(10) . ?
N2A C7A 1.451(11) . ?
N2A C6A 1.474(11) . ?
N2A H2AB 1.0000 . ?
N3A C12A 1.327(10) . ?
N3A C8A 1.332(10) . ?
N4A C13A 1.456(11) . ?
N4A C14A 1.470(10) . ?
N4A H4AB 1.0000 . ?
C1A C2A 1.394(11) . ?
C1A C14A 1.500(12) . ?
C2A C3A 1.377(12) . ?
C2A H2AA 0.9500 . ?
C3A C4A 1.392(12) . ?
C3A H3AA 0.9500 . ?
C4A C5A 1.393(11) . ?
C4A H4AA 0.9500 . ?
C5A C6A 1.491(11) . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C7A C8A 1.506(12) . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?
C8A C9A 1.374(12) . ?
C9A C10A 1.347(16) . ?
C9A H9AA 0.9500 . ?
C10A C11A 1.385(16) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.378(12) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.475(12) . ?
C13A H13A 0.9900 . ?
C13A H13B 0.9900 . ?
C14A H14A 0.9900 . ?
C14A H14B 0.9900 . ?
Ni2 N3B 1.999(6) . ?
Ni2 N1B 2.030(6) . ?
Ni2 N2B 2.201(7) . ?
Ni2 N4B 2.204(6) . ?
Ni2 H1 1.53(8) . ?
Ni2 H2 1.60(6) . ?
N1B C5B 1.327(11) . ?
N1B C1B 1.346(12) . ?
N2B C7B 1.476(11) . ?
N2B C6B 1.509(12) . ?
N2B H2BB 1.0000 . ?
N3B C8B 1.346(10) . ?
N3B C12B 1.346(10) . ?
N4B C14B 1.465(10) . ?
N4B C13B 1.467(9) . ?
N4B H4BB 1.0000 . ?
C1B C2B 1.394(12) . ?
C1B C14B 1.486(13) . ?
C2B C3B 1.342(17) . ?
C2B H2BA 0.9500 . ?
C3B C4B 1.361(17) . ?
C3B H3BA 0.9500 . ?
C4B C5B 1.427(14) . ?
C4B H4BA 0.9500 . ?
C5B C6B 1.487(15) . ?
C6B H6BA 0.9900 . ?
C6B H6BB 0.9900 . ?
C7B C8B 1.496(12) . ?
C7B H7BA 0.9900 . ?
C7B H7BB 0.9900 . ?
C8B C9B 1.365(12) . ?
C9B C10B 1.403(13) . ?
C9B H9BA 0.9500 . ?
C10B C11B 1.367(12) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.380(11) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.518(11) . ?
C13B H13C 0.9900 . ?
C13B H13D 0.9900 . ?
C14B H14C 0.9900 . ?
C14B H14D 0.9900 . ?

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
N3A Ni1 N1A 87.5(2) . . ?
N3A Ni1 N4A 79.0(2) . . ?
N1A Ni1 N4A 79.8(3) . . ?
N3A Ni1 N2A 79.2(3) . . ?
N1A Ni1 N2A 79.2(2) . . ?
N4A Ni1 N2A 150.2(2) . . ?
N3A Ni1 Ni2 133.52(17) . . ?
N1A Ni1 Ni2 138.99(18) . . ?
N4A Ni1 Ni2 104.21(18) . . ?
N2A Ni1 Ni2 105.57(17) . . ?
N3A Ni1 H1 101(3) . . ?
N1A Ni1 H1 170(3) . . ?
N4A Ni1 H1 107(3) . . ?
N2A Ni1 H1 97(3) . . ?
Ni2 Ni1 H1 33(3) . . ?
N3A Ni1 H2 167(2) . . ?
N1A Ni1 H2 104(2) . . ?
N4A Ni1 H2 107(2) . . ?
N2A Ni1 H2 98(2) . . ?
Ni2 Ni1 H2 35(2) . . ?
H1 Ni1 H2 67(4) . . ?
C1A N1A C5A 120.9(7) . . ?
C1A N1A Ni1 118.4(5) . . ?
C5A N1A Ni1 117.9(5) . . ?
C7A N2A C6A 113.8(7) . . ?
C7A N2A Ni1 109.5(5) . . ?
C6A N2A Ni1 104.8(5) . . ?
C7A N2A H2AB 109.5 . . ?
C6A N2A H2AB 109.5 . . ?
Ni1 N2A H2AB 109.5 . . ?
C12A N3A C8A 121.5(7) . . ?
C12A N3A Ni1 118.1(5) . . ?
C8A N3A Ni1 120.1(5) . . ?
C13A N4A C14A 115.1(7) . . ?
C13A N4A Ni1 106.1(5) . . ?
C14A N4A Ni1 108.5(5) . . ?
C13A N4A H4AB 109.0 . . ?
C14A N4A H4AB 109.0 . . ?
Ni1 N4A H4AB 109.0 . . ?
N1A C1A C2A 120.2(8) . . ?
N1A C1A C14A 115.5(7) . . ?
C2A C1A C14A 124.3(8) . . ?
C3A C2A C1A 119.5(8) . . ?
C3A C2A H2AA 120.3 . . ?
C1A C2A H2AA 120.2 . . ?
C2A C3A C4A 120.0(8) . . ?
C2A C3A H3AA 120.0 . . ?
C4A C3A H3AA 120.0 . . ?
C3A C4A C5A 117.5(9) . . ?
C3A C4A H4AA 121.3 . . ?
C5A C4A H4AA 121.3 . . ?
N1A C5A C4A 121.8(8) . . ?
N1A C5A C6A 113.8(7) . . ?
C4A C5A C6A 124.4(8) . . ?
N2A C6A C5A 110.7(7) . . ?
N2A C6A H6AA 109.5 . . ?
C5A C6A H6AA 109.5 . . ?
N2A C6A H6AB 109.5 . . ?
C5A C6A H6AB 109.5 . . ?
H6AA C6A H6AB 108.1 . . ?
N2A C7A C8A 114.1(7) . . ?
N2A C7A H7AA 108.7 . . ?
C8A C7A H7AA 108.7 . . ?
N2A C7A H7AB 108.7 . . ?
C8A C7A H7AB 108.7 . . ?
H7AA C7A H7AB 107.6 . . ?
N3A C8A C9A 121.1(9) . . ?
N3A C8A C7A 115.5(7) . . ?
C9A C8A C7A 123.3(9) . . ?
C10A C9A C8A 118.1(10) . . ?
C10A C9A H9AA 120.9 . . ?
C8A C9A H9AA 120.9 . . ?
C9A C10A C11A 120.9(10) . . ?
C9A C10A H10A 119.6 . . ?
C11A C10A H10A 119.6 . . ?
C12A C11A C10A 118.7(10) . . ?
C12A C11A H11A 120.7 . . ?
C10A C11A H11A 120.7 . . ?
N3A C12A C11A 119.5(9) . . ?
N3A C12A C13A 115.6(7) . . ?
C11A C12A C13A 124.9(9) . . ?
N4A C13A C12A 113.0(7) . . ?
N4A C13A H13A 109.0 . . ?
C12A C13A H13A 109.0 . . ?
N4A C13A H13B 109.0 . . ?
C12A C13A H13B 109.0 . . ?
H13A C13A H13B 107.8 . . ?
N4A C14A C1A 112.1(7) . . ?
N4A C14A H14A 109.2 . . ?
C1A C14A H14A 109.2 . . ?
N4A C14A H14B 109.2 . . ?
C1A C14A H14B 109.2 . . ?
H14A C14A H14B 107.9 . . ?
N3B Ni2 N1B 88.0(2) . . ?
N3B Ni2 N2B 79.4(3) . . ?
N1B Ni2 N2B 79.6(3) . . ?
N3B Ni2 N4B 78.9(2) . . ?
N1B Ni2 N4B 79.3(3) . . ?
N2B Ni2 N4B 150.1(3) . . ?
N3B Ni2 Ni1 133.50(18) . . ?
N1B Ni2 Ni1 138.49(18) . . ?
N2B Ni2 Ni1 105.0(2) . . ?
N4B Ni2 Ni1 104.82(17) . . ?
N3B Ni2 H1 166(3) . . ?
N1B Ni2 H1 106(3) . . ?
N2B Ni2 H1 103(3) . . ?
N4B Ni2 H1 103(3) . . ?
Ni1 Ni2 H1 33(3) . . ?
N3B Ni2 H2 102(2) . . ?
N1B Ni2 H2 165(2) . . ?
N2B Ni2 H2 113(2) . . ?
N4B Ni2 H2 92(2) . . ?
Ni1 Ni2 H2 33(2) . . ?
H1 Ni2 H2 65(4) . . ?
C5B N1B C1B 122.3(8) . . ?
C5B N1B Ni2 117.1(7) . . ?
C1B N1B Ni2 117.8(6) . . ?
C7B N2B C6B 112.5(7) . . ?
C7B N2B Ni2 109.5(5) . . ?
C6B N2B Ni2 103.3(6) . . ?
C7B N2B H2BB 110.4 . . ?
C6B N2B H2BB 110.4 . . ?
Ni2 N2B H2BB 110.4 . . ?
C8B N3B C12B 119.5(7) . . ?
C8B N3B Ni2 121.0(6) . . ?
C12B N3B Ni2 119.5(5) . . ?
C14B N4B C13B 115.1(6) . . ?
C14B N4B Ni2 109.6(5) . . ?
C13B N4B Ni2 105.4(5) . . ?
C14B N4B H4BB 108.9 . . ?
C13B N4B H4BB 108.9 . . ?
Ni2 N4B H4BB 108.9 . . ?
N1B C1B C2B 118.5(10) . . ?
N1B C1B C14B 116.6(7) . . ?
C2B C1B C14B 124.8(10) . . ?
C3B C2B C1B 120.8(12) . . ?
C3B C2B H2BA 119.6 . . ?
C1B C2B H2BA 119.6 . . ?
C2B C3B C4B 120.5(11) . . ?
C2B C3B H3BA 119.7 . . ?
C4B C3B H3BA 119.7 . . ?
C3B C4B C5B 118.4(11) . . ?
C3B C4B H4BA 120.8 . . ?
C5B C4B H4BA 120.8 . . ?
N1B C5B C4B 119.3(11) . . ?
N1B C5B C6B 114.9(8) . . ?
C4B C5B C6B 125.7(10) . . ?
C5B C6B N2B 109.9(7) . . ?
C5B C6B H6BA 109.7 . . ?
N2B C6B H6BA 109.7 . . ?
C5B C6B H6BB 109.7 . . ?
N2B C6B H6BB 109.7 . . ?
H6BA C6B H6BB 108.2 . . ?
N2B C7B C8B 114.8(7) . . ?
N2B C7B H7BA 108.6 . . ?
C8B C7B H7BA 108.6 . . ?
N2B C7B H7BB 108.6 . . ?
C8B C7B H7BB 108.6 . . ?
H7BA C7B H7BB 107.5 . . ?
N3B C8B C9B 121.2(8) . . ?
N3B C8B C7B 115.1(7) . . ?
C9B C8B C7B 123.7(8) . . ?
C8B C9B C10B 119.2(8) . . ?
C8B C9B H9BA 120.4 . . ?
C10B C9B H9BA 120.4 . . ?
C11B C10B C9B 119.3(8) . . ?
C11B C10B H10B 120.3 . . ?
C9B C10B H10B 120.3 . . ?
C10B C11B C12B 118.6(8) . . ?
C10B C11B H11B 120.7 . . ?
C12B C11B H11B 120.7 . . ?
N3B C12B C11B 121.9(8) . . ?
N3B C12B C13B 113.4(7) . . ?
C11B C12B C13B 124.6(7) . . ?
N4B C13B C12B 112.5(6) . . ?
N4B C13B H13C 109.1 . . ?
C12B C13B H13C 109.1 . . ?
N4B C13B H13D 109.1 . . ?
C12B C13B H13D 109.1 . . ?
H13C C13B H13D 107.8 . . ?
N4B C14B C1B 112.5(8) . . ?
N4B C14B H14C 109.1 . . ?
C1B C14B H14C 109.1 . . ?
N4B C14B H14D 109.1 . . ?
C1B C14B H14D 109.1 . . ?
H14C C14B H14D 107.8 . . ?

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
C5A N1A C1A C2A -2.8(11) . . . . ?
Ni1 N1A C1A C2A -163.7(6) . . . . ?
C5A N1A C1A C14A 177.4(7) . . . . ?
Ni1 N1A C1A C14A 16.5(9) . . . . ?
N1A C1A C2A C3A 0.2(12) . . . . ?
C14A C1A C2A C3A -179.9(8) . . . . ?
C1A C2A C3A C4A 2.7(12) . . . . ?
C2A C3A C4A C5A -3.1(13) . . . . ?
C1A N1A C5A C4A 2.4(12) . . . . ?
Ni1 N1A C5A C4A 163.4(6) . . . . ?
C1A N1A C5A C6A -176.9(7) . . . . ?
Ni1 N1A C5A C6A -15.9(10) . . . . ?
C3A C4A C5A N1A 0.6(13) . . . . ?
C3A C4A C5A C6A 179.8(8) . . . . ?
C7A N2A C6A C5A 81.3(9) . . . . ?
Ni1 N2A C6A C5A -38.3(9) . . . . ?
N1A C5A C6A N2A 37.9(11) . . . . ?
C4A C5A C6A N2A -141.4(8) . . . . ?
C6A N2A C7A C8A -103.6(8) . . . . ?
Ni1 N2A C7A C8A 13.3(8) . . . . ?
C12A N3A C8A C9A -4.7(12) . . . . ?
Ni1 N3A C8A C9A -179.1(6) . . . . ?
C12A N3A C8A C7A 177.7(7) . . . . ?
Ni1 N3A C8A C7A 3.3(9) . . . . ?
N2A C7A C8A N3A -11.6(10) . . . . ?
N2A C7A C8A C9A 170.8(8) . . . . ?
N3A C8A C9A C10A 2.0(14) . . . . ?
C7A C8A C9A C10A 179.5(9) . . . . ?
C8A C9A C10A C11A 0.8(16) . . . . ?
C9A C10A C11A C12A -1.0(16) . . . . ?
C8A N3A C12A C11A 4.3(11) . . . . ?
Ni1 N3A C12A C11A 178.8(6) . . . . ?
C8A N3A C12A C13A -177.2(7) . . . . ?
Ni1 N3A C12A C13A -2.7(9) . . . . ?
C10A C11A C12A N3A -1.5(13) . . . . ?
C10A C11A C12A C13A -179.8(9) . . . . ?
C14A N4A C13A C12A 89.2(9) . . . . ?
Ni1 N4A C13A C12A -30.8(8) . . . . ?
N3A C12A C13A N4A 24.1(10) . . . . ?
C11A C12A C13A N4A -157.5(8) . . . . ?
C13A N4A C14A C1A -95.5(9) . . . . ?
Ni1 N4A C14A C1A 23.1(8) . . . . ?
N1A C1A C14A N4A -26.8(10) . . . . ?
C2A C1A C14A N4A 153.3(7) . . . . ?
C5B N1B C1B C2B 1.6(12) . . . . ?
Ni2 N1B C1B C2B 162.0(6) . . . . ?
C5B N1B C1B C14B -177.2(8) . . . . ?
Ni2 N1B C1B C14B -16.8(9) . . . . ?
N1B C1B C2B C3B 1.8(14) . . . . ?
C14B C1B C2B C3B -179.5(9) . . . . ?
C1B C2B C3B C4B -4.6(16) . . . . ?
C2B C3B C4B C5B 3.9(16) . . . . ?
C1B N1B C5B C4B -2.2(12) . . . . ?
Ni2 N1B C5B C4B -162.7(6) . . . . ?
C1B N1B C5B C6B 175.5(7) . . . . ?
Ni2 N1B C5B C6B 14.9(10) . . . . ?
C3B C4B C5B N1B -0.6(14) . . . . ?
C3B C4B C5B C6B -177.9(9) . . . . ?
N1B C5B C6B N2B -39.0(11) . . . . ?
C4B C5B C6B N2B 138.5(9) . . . . ?
C7B N2B C6B C5B -77.7(9) . . . . ?
Ni2 N2B C6B C5B 40.2(8) . . . . ?
C6B N2B C7B C8B 109.8(9) . . . . ?
Ni2 N2B C7B C8B -4.5(9) . . . . ?
C12B N3B C8B C9B 4.8(12) . . . . ?
Ni2 N3B C8B C9B -177.0(6) . . . . ?
C12B N3B C8B C7B -176.0(7) . . . . ?
Ni2 N3B C8B C7B 2.2(10) . . . . ?
N2B C7B C8B N3B 1.9(11) . . . . ?
N2B C7B C8B C9B -178.9(8) . . . . ?
N3B C8B C9B C10B -1.2(13) . . . . ?
C7B C8B C9B C10B 179.7(8) . . . . ?
C8B C9B C10B C11B -2.8(13) . . . . ?
C9B C10B C11B C12B 3.1(13) . . . . ?
C8B N3B C12B C11B -4.5(11) . . . . ?
Ni2 N3B C12B C11B 177.3(6) . . . . ?
C8B N3B C12B C13B 178.3(7) . . . . ?
Ni2 N3B C12B C13B 0.1(9) . . . . ?
C10B C11B C12B N3B 0.5(12) . . . . ?
C10B C11B C12B C13B 177.4(8) . . . . ?
C14B N4B C13B C12B -87.0(8) . . . . ?
Ni2 N4B C13B C12B 33.8(7) . . . . ?
N3B C12B C13B N4B -24.8(9) . . . . ?
C11B C12B C13B N4B 158.1(7) . . . . ?
C13B N4B C14B C1B 100.2(8) . . . . ?
Ni2 N4B C14B C1B -18.3(8) . . . . ?
N1B C1B C14B N4B 23.6(10) . . . . ?
C2B C1B C14B N4B -155.1(8) . . . . ?

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
N2A H2AB I1 1.00 2.64 3.532(7) 148.4 .
N4A H4AB I2A 1.00 2.83 3.634(11) 138.3 .
N4A H4AB I2B 1.00 2.72 3.566(9) 142.9 .
C2A H2AA I1 0.95 3.25 4.055(9) 143.6 3_656
C6A H6AB I2D 0.99 3.26 4.169(12) 152.8 8_655
C7A H7AB I2A 0.99 3.20 4.186(12) 173.8 3_646
C7A H7AB I2C 0.99 3.32 3.991(9) 126.6 3_646
C11A H11A I2C 0.95 3.26 4.028(9) 138.9 6_657
C11A H11A I2D 0.95 3.05 3.955(10) 159.5 6_657
C13A H13B I1 0.99 3.25 4.192(9) 160.5 8_765
C14A H14B I1 0.99 3.20 4.125(9) 156.9 3_656
N2B H2BB I2A 1.00 3.14 4.029(14) 148.2 .
N2B H2BB I2B 1.00 2.76 3.654(14) 148.7 .
N4B H4BB I1 1.00 2.76 3.638(6) 146.9 .
C2B H2BA I2A 0.95 2.90 3.84(2) 170.1 4_556
C2B H2BA I2B 0.95 3.30 4.210(14) 162.1 4_556
C2B H2BA I2C 0.95 3.20 3.930(13) 134.7 4_556
C4B H4BA I2D 0.95 2.64 3.536(13) 156.9 5_666
C6B H6BA I2C 0.99 3.19 4.125(9) 158.6 5_666
C6B H6BB I1 0.99 3.05 3.977(9) 157.0 8_765
C7B H7BA I2A 0.99 3.18 3.881(11) 129.1 5_666
C7B H7BA I2B 0.99 3.31 3.880(10) 118.2 5_666
C13B H13C I2D 0.99 3.20 4.165(9) 164.3 8_655
C13B H13D I2D 0.99 3.23 4.133(9) 152.4 4_556
C14B H14C I2C 0.99 3.03 3.970(9) 158.4 4_556
C14B H14C I2D 0.99 3.26 4.225(11) 165.5 4_556
C14B H14D I1 0.99 3.23 3.841(9) 121.2 .

_refine_diff_density_max         2.289
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.135

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[(LH)Ni(mu-Br)2Ni(LH)]Br2
_database_code_depnum_ccdc_archive 'CCDC 1878191'
loop_
_audit_author_name
_audit_author_address
'Sakthi Raje'
;Indian Institute of Technology Kanpur
India
;
_audit_update_record             
;
2018-11-09 deposited with the CCDC.	2019-04-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H32 Br4 N8 Ni2'
_chemical_formula_sum            'C28 H32 Br4 N8 Ni2'
_chemical_formula_weight         917.67

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'
Br Br -0.2901 2.4595 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   15.109(3)
_cell_length_b                   15.035(3)
_cell_length_c                   10.6611(19)
_cell_angle_alpha                90
_cell_angle_beta                 116.240(6)
_cell_angle_gamma                90
_cell_volume                     2172.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5409
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      27.98

_exptl_crystal_description       prism
_exptl_crystal_colour            light-blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_F_000             904
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    4.570
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5583
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2825
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.709
_diffrn_reflns_theta_max         28.392
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2825
_reflns_number_gt                2079
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick 2008)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0966P)²+6.7611P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2825
_refine_ls_number_parameters     102
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1679
_refine_ls_wR_factor_gt          0.1555
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Ni Ni 0.38834(6) 0.5000 0.52569(9) 0.0178(2) Uani 1 2 d S T P . .
Br1 Br 0.5000 0.61628(4) 0.5000 0.0254(2) Uani 1 2 d S T P . .
Br2 Br 0.30271(7) 0.5000 0.02804(9) 0.0565(4) Uani 1 2 d S T P . .
N1 N 0.4507(4) 0.5000 0.7491(6) 0.0222(12) Uani 1 2 d S T P . .
H1C H 0.5243 0.5000 0.7877 0.027 Uiso 1 2 calc R U P . .
N2 N 0.3022(3) 0.4084(3) 0.5523(4) 0.0183(8) Uani 1 1 d . . . . .
N3 N 0.2665(4) 0.5000 0.3194(6) 0.0226(12) Uani 1 2 d S T P . .
H3B H 0.2933 0.5000 0.2488 0.027 Uiso 1 2 calc R U P . .
C1 C 0.4194(4) 0.4170(3) 0.7931(5) 0.0231(10) Uani 1 1 d . . . . .
H1A H 0.4144 0.4278 0.8814 0.028 Uiso 1 1 calc R U . . .
H1B H 0.4699 0.3704 0.8112 0.028 Uiso 1 1 calc R U . . .
C2 C 0.3209(4) 0.3844(3) 0.6828(5) 0.0221(10) Uani 1 1 d . . . . .
C3 C 0.2551(4) 0.3334(3) 0.7081(6) 0.0277(11) Uani 1 1 d . . . . .
H3A H 0.2682 0.3173 0.8008 0.033 Uiso 1 1 calc R U . . .
C4 C 0.1692(4) 0.3060(3) 0.5955(6) 0.0301(12) Uani 1 1 d . . . . .
H4A H 0.1234 0.2699 0.6110 0.036 Uiso 1 1 calc R U . . .
C5 C 0.1493(4) 0.3308(3) 0.4606(6) 0.0295(12) Uani 1 1 d . . . . .
H5A H 0.0907 0.3120 0.3828 0.035 Uiso 1 1 calc R U . . .
C6 C 0.2183(4) 0.3842(3) 0.4425(5) 0.0232(10) Uani 1 1 d . . . . .
C7 C 0.2091(4) 0.4173(3) 0.3028(6) 0.0285(11) Uani 1 1 d . . . . .
H7A H 0.2332 0.3709 0.2596 0.034 Uiso 1 1 calc R U . . .
H7B H 0.1388 0.4287 0.2394 0.034 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N2 2.000(4) 6_565 ?
Ni N2 2.000(4) . ?
Ni N1 2.139(6) . ?
Ni N3 2.156(6) . ?
Ni Br1 2.5269(8) 5_666 ?
Ni Br1 2.5270(8) . ?
Br1 Ni 2.5270(8) 5_666 ?
N1 C1 1.483(5) . ?
N1 C1 1.483(5) 6_565 ?
N1 H1C 1.0000 . ?
N2 C2 1.340(6) . ?
N2 C6 1.341(6) . ?
N3 C7 1.481(6) . ?
N3 C7 1.481(6) 6_565 ?
N3 H3B 1.0000 . ?
C1 C2 1.513(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.373(7) . ?
C3 C4 1.385(7) . ?
C3 H3A 0.9500 . ?
C4 C5 1.385(8) . ?
C4 H4A 0.9500 . ?
C5 C6 1.394(7) . ?
C5 H5A 0.9500 . ?
C6 C7 1.518(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?

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
N2 Ni N2 87.1(2) 6_565 . ?
N2 Ni N1 80.55(16) 6_565 . ?
N2 Ni N1 80.55(16) . . ?
N2 Ni N3 80.17(16) 6_565 . ?
N2 Ni N3 80.16(16) . . ?
N1 Ni N3 153.3(2) . . ?
N2 Ni Br1 178.26(12) 6_565 5_666 ?
N2 Ni Br1 92.66(11) . 5_666 ?
N1 Ni Br1 97.71(11) . 5_666 ?
N3 Ni Br1 101.49(11) . 5_666 ?
N2 Ni Br1 92.66(11) 6_565 . ?
N2 Ni Br1 178.26(12) . . ?
N1 Ni Br1 97.71(11) . . ?
N3 Ni Br1 101.49(11) . . ?
Br1 Ni Br1 87.55(4) 5_666 . ?
Ni Br1 Ni 92.45(4) . 5_666 ?
C1 N1 C1 114.7(5) . 6_565 ?
C1 N1 Ni 107.9(3) . . ?
C1 N1 Ni 107.9(3) 6_565 . ?
C1 N1 H1C 108.7 . . ?
C1 N1 H1C 108.7 6_565 . ?
Ni N1 H1C 108.7 . . ?
C2 N2 C6 121.1(4) . . ?
C2 N2 Ni 118.7(3) . . ?
C6 N2 Ni 119.1(3) . . ?
C7 N3 C7 114.2(6) . 6_565 ?
C7 N3 Ni 108.2(3) . . ?
C7 N3 Ni 108.2(3) 6_565 . ?
C7 N3 H3B 108.7 . . ?
C7 N3 H3B 108.7 6_565 . ?
Ni N3 H3B 108.7 . . ?
N1 C1 C2 111.6(4) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
N2 C2 C3 121.0(5) . . ?
N2 C2 C1 113.8(4) . . ?
C3 C2 C1 125.2(5) . . ?
C2 C3 C4 118.6(5) . . ?
C2 C3 H3A 120.7 . . ?
C4 C3 H3A 120.7 . . ?
C3 C4 C5 120.6(5) . . ?
C3 C4 H4A 119.7 . . ?
C5 C4 H4A 119.7 . . ?
C4 C5 C6 117.8(5) . . ?
C4 C5 H5A 121.1 . . ?
C6 C5 H5A 121.1 . . ?
N2 C6 C5 120.8(5) . . ?
N2 C6 C7 114.1(4) . . ?
C5 C6 C7 125.1(5) . . ?
N3 C7 C6 111.4(4) . . ?
N3 C7 H7A 109.4 . . ?
C6 C7 H7A 109.4 . . ?
N3 C7 H7B 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?

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
C1 N1 C1 C2 91.6(6) 6_565 . . . ?
Ni N1 C1 C2 -28.7(5) . . . . ?
C6 N2 C2 C3 0.7(7) . . . . ?
Ni N2 C2 C3 169.0(4) . . . . ?
C6 N2 C2 C1 179.5(4) . . . . ?
Ni N2 C2 C1 -12.2(5) . . . . ?
N1 C1 C2 N2 27.8(6) . . . . ?
N1 C1 C2 C3 -153.5(5) . . . . ?
N2 C2 C3 C4 0.9(7) . . . . ?
C1 C2 C3 C4 -177.8(5) . . . . ?
C2 C3 C4 C5 -1.0(8) . . . . ?
C3 C4 C5 C6 -0.3(8) . . . . ?
C2 N2 C6 C5 -2.1(7) . . . . ?
Ni N2 C6 C5 -170.4(4) . . . . ?
C2 N2 C6 C7 179.8(4) . . . . ?
Ni N2 C6 C7 11.5(5) . . . . ?
C4 C5 C6 N2 1.9(7) . . . . ?
C4 C5 C6 C7 179.8(5) . . . . ?
C7 N3 C7 C6 -92.6(6) 6_565 . . . ?
Ni N3 C7 C6 28.0(5) . . . . ?
N2 C6 C7 N3 -26.9(6) . . . . ?
C5 C6 C7 N3 155.1(5) . . . . ?

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
N1 H1C Br2 1.00 2.48 3.420(6) 156.5 5_666
N3 H3B Br2 1.00 2.42 3.383(6) 161.7 .
C1 H1A Br2 0.99 2.97 3.852(5) 149.4 1_556

_refine_diff_density_max         1.665
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.169



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[(LH)Ni(mu-I)2Ni(LH)]I2
_database_code_depnum_ccdc_archive 'CCDC 1878192'
loop_
_audit_author_name
_audit_author_address
'Ray J. Butcher'
;Howard University
United States of America
;
_audit_update_record             
;
2019-03-21 deposited with the CCDC.	2019-04-18 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_DIFMN02_[(LH)Ni(mu-I)2Ni(LH)]I2 
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00
RESPONSE: The structure was a pseudo-merohedral twin. A twin law was found but there are still some residual peaks near the heaviest atoms.
;
_vrf_PLAT084_[(LH)Ni(mu-I)2Ni(LH)]I2 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.37 Report
RESPONSE: The structure was a pseudo-merohedral twin. A twin law was found but still the R value is a little high.
;
_vrf_PLAT097_[(LH)Ni(mu-I)2Ni(LH)]I2 
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       6.72 eA-3
RESPONSE: The structure was a pseudo-merohedral twin. A twin law was found but there are still some residual peaks near the heaviest atoms.
;
_vrf_PLAT098_[(LH)Ni(mu-I)2Ni(LH)]I2 
;
PROBLEM: Large Reported Min.  (Negative) Residual Density      -7.66 eA-3
RESPONSE: The structure was a pseudo-merohedral twin. A twin law was found but there are still some residual peaks near the heaviest atoms. ;
;
_vrf_PLAT112_[(LH)Ni(mu-I)2Ni(LH)]I2 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         A         95 %Fit
RESPONSE: The structure could neither be refined or solved in a higher symmetry space group. Platon also indicated that the present space group was correct.
;
_vrf_PLAT342_[(LH)Ni(mu-I)2Ni(LH)]I2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0275 Ang.
RESPONSE: The structure was a pseudo-merohedral twin. A twin law was found but still the esd's on the metrical parameters are a little higher than normal.
;
# Added during the CSD deposition process: Thursday 21 March 2019 01:23 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H32 Ni2 I2 N8, 2(C H4 O), 2(I)'
_chemical_formula_sum            'C30 H40 I4 N8 Ni2 O2'
_chemical_formula_weight         1169.72

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   19.061(4)
_cell_length_b                   10.993(2)
_cell_length_c                   19.320(4)
_cell_angle_alpha                90
_cell_angle_beta                 112.098(5)
_cell_angle_gamma                90
_cell_volume                     3750.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9884
_cell_measurement_theta_min      2.306
_cell_measurement_theta_max      28.352

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_F_000             2240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    4.335
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6352
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Apex 2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9432
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.252
_diffrn_reflns_theta_max         28.518
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             9432
_reflns_number_gt                6860
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker Apex 2'
_computing_cell_refinement       'Bruker Apex 2'
_computing_data_reduction        'Bruker Saint'
_computing_structure_solution    'Bruker SHELXT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9432
_refine_ls_number_parameters     420
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.1157
_refine_ls_wR_factor_ref         0.3700
_refine_ls_wR_factor_gt          0.3284
_refine_ls_goodness_of_fit_ref   1.459
_refine_ls_restrained_S_all      1.457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
I1 I 0.35833(7) 1.34729(9) 0.86437(6) 0.0228(3) Uani 1 1 d . . . . .
I2 I 0.36489(7) 0.84162(9) 0.35585(6) 0.0235(3) Uani 1 1 d . . . . .
Ni1 Ni 0.43240(12) 0.89409(18) 0.92625(12) 0.0182(5) Uani 1 1 d . . . . .
I1A I 0.43426(7) 0.99409(10) 1.05652(6) 0.0254(3) Uani 1 1 d . . . . .
N1A N 0.3327(8) 0.8170(12) 0.9125(8) 0.019(3) Uani 1 1 d . . . . .
N2A N 0.3583(9) 1.0187(12) 0.8467(8) 0.025(3) Uani 1 1 d . U . . .
H2AA H 0.375742 1.103831 0.862059 0.030 Uiso 1 1 calc R U . . .
N3A N 0.4256(8) 0.8126(12) 0.8325(8) 0.020(3) Uani 1 1 d . . . . .
N4A N 0.4726(8) 0.7169(11) 0.9684(8) 0.021(3) Uani 1 1 d . . . . .
H4AB H 0.518677 0.725291 1.015198 0.025 Uiso 1 1 calc R U . . .
C1A C 0.4122(11) 0.6599(14) 0.9863(11) 0.027(4) Uani 1 1 d . . . . .
H1AA H 0.421136 0.675904 1.039377 0.033 Uiso 1 1 calc R U . . .
H1AB H 0.414128 0.570769 0.979892 0.033 Uiso 1 1 calc R U . . .
C2A C 0.3335(10) 0.7061(15) 0.9376(9) 0.020(3) Uani 1 1 d . U . . .
C3A C 0.2668(11) 0.6435(16) 0.9245(10) 0.026(4) Uani 1 1 d . . . . .
H3AA H 0.267339 0.562933 0.942421 0.031 Uiso 1 1 calc R U . . .
C4A C 0.1962(12) 0.7046(19) 0.8827(12) 0.035(5) Uani 1 1 d . . . . .
H4AA H 0.148757 0.666474 0.873458 0.042 Uiso 1 1 calc R U . . .
C5A C 0.2004(11) 0.8196(18) 0.8568(11) 0.030(4) Uani 1 1 d . . . . .
H5AA H 0.154824 0.861558 0.829151 0.037 Uiso 1 1 calc R U . . .
C6A C 0.2679(10) 0.8752(15) 0.8697(9) 0.021(3) Uani 1 1 d . . . . .
C7A C 0.2782(10) 1.0017(14) 0.8479(11) 0.026(4) Uani 1 1 d . . . . .
H7AA H 0.270781 1.059578 0.883828 0.032 Uiso 1 1 calc R U . . .
H7AB H 0.239650 1.019499 0.797771 0.032 Uiso 1 1 calc R U . . .
C8A C 0.3610(11) 0.9943(15) 0.7728(10) 0.029(4) Uani 1 1 d . . . . .
H8AA H 0.397344 1.050843 0.764143 0.034 Uiso 1 1 calc R U . . .
H8AB H 0.310453 1.009176 0.733618 0.034 Uiso 1 1 calc R U . . .
C9A C 0.3847(10) 0.8654(15) 0.7671(9) 0.021(3) Uani 1 1 d . . . . .
C10A C 0.3664(10) 0.8043(16) 0.7021(10) 0.024(4) Uani 1 1 d . . . . .
H10A H 0.336630 0.842106 0.656254 0.029 Uiso 1 1 calc R U . . .
C11A C 0.3919(11) 0.6843(16) 0.7029(10) 0.028(4) Uani 1 1 d . . . . .
H11A H 0.380476 0.640520 0.657615 0.033 Uiso 1 1 calc R U . . .
C12A C 0.4341(11) 0.6303(16) 0.7712(10) 0.028(4) Uani 1 1 d . U . . .
H12A H 0.452561 0.549505 0.773617 0.033 Uiso 1 1 calc R U . . .
C13A C 0.4482(9) 0.6980(14) 0.8351(9) 0.017(3) Uani 1 1 d . U . . .
C14A C 0.4933(10) 0.6512(15) 0.9112(11) 0.026(4) Uani 1 1 d . . . . .
H14A H 0.547918 0.662318 0.921976 0.031 Uiso 1 1 calc R U . . .
H14B H 0.483611 0.563056 0.913555 0.031 Uiso 1 1 calc R U . . .
Ni2 Ni 0.42989(13) 0.39117(18) 0.42786(12) 0.0185(5) Uani 1 1 d . . . . .
I1B I 0.44009(7) 0.48692(10) 0.56078(6) 0.0253(3) Uani 1 1 d . . . . .
N1B N 0.3354(9) 0.3004(13) 0.4187(8) 0.024(3) Uani 1 1 d . . . . .
N2B N 0.3468(10) 0.5133(14) 0.3550(9) 0.032(4) Uani 1 1 d . . . . .
H2BB H 0.361143 0.598776 0.372322 0.039 Uiso 1 1 calc R U . . .
N3B N 0.4210(8) 0.3201(11) 0.3308(8) 0.017(3) Uani 1 1 d . U . . .
N4B N 0.4789(9) 0.2157(12) 0.4657(8) 0.025(3) Uani 1 1 d . . . . .
H4BB H 0.526049 0.225522 0.511373 0.030 Uiso 1 1 calc R U . . .
C1B C 0.3403(10) 0.1853(15) 0.4399(9) 0.018(3) Uani 1 1 d . U . . .
C2B C 0.2747(12) 0.1151(16) 0.4263(11) 0.030(4) Uani 1 1 d . . . . .
H2BA H 0.278182 0.033234 0.443024 0.036 Uiso 1 1 calc R U . . .
C3B C 0.2059(10) 0.1676(17) 0.3887(10) 0.025(4) Uani 1 1 d . . . . .
H3BA H 0.161153 0.120688 0.377758 0.030 Uiso 1 1 calc R U . . .
C4B C 0.2003(10) 0.2849(18) 0.3668(10) 0.028(4) Uani 1 1 d . . . . .
H4BA H 0.152088 0.321494 0.342306 0.033 Uiso 1 1 calc R U . . .
C5B C 0.2678(11) 0.3528(15) 0.3809(10) 0.024(4) Uani 1 1 d . U . . .
C6B C 0.2698(12) 0.4838(16) 0.3592(11) 0.032(4) Uani 1 1 d . . . . .
H6BA H 0.261287 0.537176 0.396586 0.038 Uiso 1 1 calc R U . . .
H6BB H 0.228957 0.499162 0.310111 0.038 Uiso 1 1 calc R U . . .
C7B C 0.3466(11) 0.5000(14) 0.2806(10) 0.027(4) Uani 1 1 d . . . . .
H7BA H 0.377945 0.565193 0.271490 0.032 Uiso 1 1 calc R U . . .
H7BB H 0.294219 0.509884 0.243825 0.032 Uiso 1 1 calc R U . . .
C8B C 0.3770(10) 0.3767(15) 0.2685(10) 0.024(4) Uani 1 1 d . . . . .
C9B C 0.3613(11) 0.3238(16) 0.1997(10) 0.024(4) Uani 1 1 d . . . . .
H9BA H 0.331210 0.365286 0.155244 0.029 Uiso 1 1 calc R U . . .
C10B C 0.3898(10) 0.2099(16) 0.1963(10) 0.025(4) Uani 1 1 d . . . . .
H10B H 0.378453 0.171530 0.149269 0.029 Uiso 1 1 calc R U . . .
C11B C 0.4353(12) 0.1504(16) 0.2618(11) 0.029(4) Uani 1 1 d . . . . .
H11B H 0.455883 0.072190 0.260188 0.035 Uiso 1 1 calc R U . . .
C12B C 0.4495(10) 0.2095(15) 0.3292(10) 0.023(4) Uani 1 1 d . . . . .
C13B C 0.4982(11) 0.1583(14) 0.4044(10) 0.025(4) Uani 1 1 d . . . . .
H13A H 0.490507 0.069211 0.404457 0.030 Uiso 1 1 calc R U . . .
H13B H 0.552207 0.173309 0.413592 0.030 Uiso 1 1 calc R U . . .
C14B C 0.4219(10) 0.1417(14) 0.4845(10) 0.022(4) Uani 1 1 d . . . . .
H14C H 0.432673 0.148545 0.538635 0.026 Uiso 1 1 calc R U . . .
H14D H 0.426640 0.055004 0.473071 0.026 Uiso 1 1 calc R U . . .
O1M O 0.2842(13) 1.3535(14) 1.0059(10) 0.061(5) Uani 1 1 d . . . . .
H1M H 0.302899 1.351994 0.972839 0.092 Uiso 1 1 calc R U . . .
C1M C 0.2453(9) 1.2455(18) 1.0036(8) 0.031(5) Uani 1 1 d . . . . .
H1M1 H 0.281366 1.177909 1.019395 0.047 Uiso 1 1 calc R U . . .
H1M2 H 0.209300 1.230995 0.952535 0.047 Uiso 1 1 calc R U . . .
H1M3 H 0.217763 1.251580 1.037309 0.047 Uiso 1 1 calc R U . . .
O2M O 0.5086(10) 0.8523(14) 0.2842(12) 0.059(5) Uani 1 1 d . . . . .
H2M H 0.465561 0.870000 0.283838 0.089 Uiso 1 1 calc R U . . .
C2M C 0.5047(10) 0.744(3) 0.2476(10) 0.044(6) Uani 1 1 d . . . . .
H2M1 H 0.454082 0.734332 0.208778 0.066 Uiso 1 1 calc R U . . .
H2M2 H 0.514823 0.676616 0.283281 0.066 Uiso 1 1 calc R U . . .
H2M3 H 0.542559 0.743423 0.224486 0.066 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N3A 1.981(14) . ?
Ni1 N1A 2.006(14) . ?
Ni1 N4A 2.139(13) . ?
Ni1 N2A 2.145(14) . ?
Ni1 I1A 2.729(2) 3_677 ?
Ni1 I1A 2.734(2) . ?
N1A C2A 1.31(2) . ?
N1A C6A 1.36(2) . ?
N2A C8A 1.47(2) . ?
N2A C7A 1.55(2) . ?
N2A H2AA 1.0000 . ?
N3A C13A 1.327(19) . ?
N3A C9A 1.34(2) . ?
N4A C1A 1.46(2) . ?
N4A C14A 1.49(2) . ?
N4A H4AB 1.0000 . ?
C1A C2A 1.53(3) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C2A C3A 1.38(2) . ?
C3A C4A 1.45(3) . ?
C3A H3AA 0.9500 . ?
C4A C5A 1.37(3) . ?
C4A H4AA 0.9500 . ?
C5A C6A 1.36(2) . ?
C5A H5AA 0.9500 . ?
C6A C7A 1.49(2) . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?
C8A C9A 1.50(2) . ?
C8A H8AA 0.9900 . ?
C8A H8AB 0.9900 . ?
C9A C10A 1.35(2) . ?
C10A C11A 1.40(2) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.39(3) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.38(2) . ?
C12A H12A 0.9500 . ?
C13A C14A 1.49(3) . ?
C14A H14A 0.9900 . ?
C14A H14B 0.9900 . ?
Ni2 N3B 1.979(14) . ?
Ni2 N1B 2.007(16) . ?
Ni2 N4B 2.148(14) . ?
Ni2 N2B 2.148(17) . ?
Ni2 I1B 2.714(2) . ?
Ni2 I1B 2.753(2) 3_666 ?
N1B C1B 1.32(2) . ?
N1B C5B 1.35(2) . ?
N2B C7B 1.44(2) . ?
N2B C6B 1.53(3) . ?
N2B H2BB 1.0000 . ?
N3B C8B 1.33(2) . ?
N3B C12B 1.34(2) . ?
N4B C13B 1.51(2) . ?
N4B C14B 1.51(2) . ?
N4B H4BB 1.0000 . ?
C1B C2B 1.41(2) . ?
C1B C14B 1.54(2) . ?
C2B C3B 1.37(3) . ?
C2B H2BA 0.9500 . ?
C3B C4B 1.35(3) . ?
C3B H3BA 0.9500 . ?
C4B C5B 1.42(3) . ?
C4B H4BA 0.9500 . ?
C5B C6B 1.50(2) . ?
C6B H6BA 0.9900 . ?
C6B H6BB 0.9900 . ?
C7B C8B 1.53(2) . ?
C7B H7BA 0.9900 . ?
C7B H7BB 0.9900 . ?
C8B C9B 1.38(2) . ?
C9B C10B 1.38(2) . ?
C9B H9BA 0.9500 . ?
C10B C11B 1.40(3) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.39(2) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.51(3) . ?
C13B H13A 0.9900 . ?
C13B H13B 0.9900 . ?
C14B H14C 0.9900 . ?
C14B H14D 0.9900 . ?
O1M C1M 1.39(2) . ?
O1M H1M 0.8400 . ?
C1M H1M1 0.9800 . ?
C1M H1M2 0.9800 . ?
C1M H1M3 0.9800 . ?
O2M C2M 1.37(3) . ?
O2M H2M 0.8400 . ?
C2M H2M1 0.9800 . ?
C2M H2M2 0.9800 . ?
C2M H2M3 0.9800 . ?

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
N3A Ni1 N1A 87.4(6) . . ?
N3A Ni1 N4A 80.0(5) . . ?
N1A Ni1 N4A 81.5(5) . . ?
N3A Ni1 N2A 80.5(6) . . ?
N1A Ni1 N2A 80.7(6) . . ?
N4A Ni1 N2A 154.1(6) . . ?
N3A Ni1 I1A 93.0(4) . 3_677 ?
N1A Ni1 I1A 178.2(4) . 3_677 ?
N4A Ni1 I1A 100.4(4) . 3_677 ?
N2A Ni1 I1A 97.6(4) . 3_677 ?
N3A Ni1 I1A 175.7(4) . . ?
N1A Ni1 I1A 88.6(4) . . ?
N4A Ni1 I1A 97.9(4) . . ?
N2A Ni1 I1A 100.4(4) . . ?
I1A Ni1 I1A 91.01(7) 3_677 . ?
Ni1 I1A Ni1 88.99(7) 3_677 . ?
C2A N1A C6A 123.0(15) . . ?
C2A N1A Ni1 117.7(12) . . ?
C6A N1A Ni1 118.7(12) . . ?
C8A N2A C7A 112.8(14) . . ?
C8A N2A Ni1 108.9(11) . . ?
C7A N2A Ni1 107.4(10) . . ?
C8A N2A H2AA 109.2 . . ?
C7A N2A H2AA 109.2 . . ?
Ni1 N2A H2AA 109.2 . . ?
C13A N3A C9A 120.8(15) . . ?
C13A N3A Ni1 119.1(12) . . ?
C9A N3A Ni1 118.7(11) . . ?
C1A N4A C14A 114.7(13) . . ?
C1A N4A Ni1 106.2(10) . . ?
C14A N4A Ni1 108.4(10) . . ?
C1A N4A H4AB 109.1 . . ?
C14A N4A H4AB 109.1 . . ?
Ni1 N4A H4AB 109.1 . . ?
N4A C1A C2A 112.9(14) . . ?
N4A C1A H1AA 109.0 . . ?
C2A C1A H1AA 109.0 . . ?
N4A C1A H1AB 109.0 . . ?
C2A C1A H1AB 109.0 . . ?
H1AA C1A H1AB 107.8 . . ?
N1A C2A C3A 120.9(17) . . ?
N1A C2A C1A 114.2(15) . . ?
C3A C2A C1A 124.7(16) . . ?
C2A C3A C4A 118.0(16) . . ?
C2A C3A H3AA 121.0 . . ?
C4A C3A H3AA 121.0 . . ?
C5A C4A C3A 117.4(18) . . ?
C5A C4A H4AA 121.3 . . ?
C3A C4A H4AA 121.3 . . ?
C6A C5A C4A 122(2) . . ?
C6A C5A H5AA 119.1 . . ?
C4A C5A H5AA 119.1 . . ?
N1A C6A C5A 118.7(17) . . ?
N1A C6A C7A 115.2(15) . . ?
C5A C6A C7A 125.8(17) . . ?
C6A C7A N2A 110.7(13) . . ?
C6A C7A H7AA 109.5 . . ?
N2A C7A H7AA 109.5 . . ?
C6A C7A H7AB 109.5 . . ?
N2A C7A H7AB 109.5 . . ?
H7AA C7A H7AB 108.1 . . ?
N2A C8A C9A 111.3(14) . . ?
N2A C8A H8AA 109.4 . . ?
C9A C8A H8AA 109.4 . . ?
N2A C8A H8AB 109.4 . . ?
C9A C8A H8AB 109.4 . . ?
H8AA C8A H8AB 108.0 . . ?
N3A C9A C10A 121.1(16) . . ?
N3A C9A C8A 115.0(15) . . ?
C10A C9A C8A 123.9(17) . . ?
C9A C10A C11A 119.4(18) . . ?
C9A C10A H10A 120.3 . . ?
C11A C10A H10A 120.3 . . ?
C12A C11A C10A 119.0(17) . . ?
C12A C11A H11A 120.5 . . ?
C10A C11A H11A 120.5 . . ?
C13A C12A C11A 117.8(17) . . ?
C13A C12A H12A 121.1 . . ?
C11A C12A H12A 121.1 . . ?
N3A C13A C12A 121.8(17) . . ?
N3A C13A C14A 115.1(15) . . ?
C12A C13A C14A 123.0(15) . . ?
C13A C14A N4A 110.4(14) . . ?
C13A C14A H14A 109.6 . . ?
N4A C14A H14A 109.6 . . ?
C13A C14A H14B 109.6 . . ?
N4A C14A H14B 109.6 . . ?
H14A C14A H14B 108.1 . . ?
N3B Ni2 N1B 88.0(6) . . ?
N3B Ni2 N4B 80.8(5) . . ?
N1B Ni2 N4B 81.1(6) . . ?
N3B Ni2 N2B 81.2(5) . . ?
N1B Ni2 N2B 80.7(6) . . ?
N4B Ni2 N2B 154.6(6) . . ?
N3B Ni2 I1B 179.1(4) . . ?
N1B Ni2 I1B 91.1(4) . . ?
N4B Ni2 I1B 99.1(4) . . ?
N2B Ni2 I1B 98.7(4) . . ?
N3B Ni2 I1B 91.2(4) . 3_666 ?
N1B Ni2 I1B 179.2(4) . 3_666 ?
N4B Ni2 I1B 98.4(4) . 3_666 ?
N2B Ni2 I1B 99.6(5) . 3_666 ?
I1B Ni2 I1B 89.65(7) . 3_666 ?
Ni2 I1B Ni2 90.35(7) . 3_666 ?
C1B N1B C5B 121.2(16) . . ?
C1B N1B Ni2 119.5(13) . . ?
C5B N1B Ni2 118.6(12) . . ?
C7B N2B C6B 112.8(16) . . ?
C7B N2B Ni2 108.3(11) . . ?
C6B N2B Ni2 108.5(11) . . ?
C7B N2B H2BB 109.1 . . ?
C6B N2B H2BB 109.1 . . ?
Ni2 N2B H2BB 109.1 . . ?
C8B N3B C12B 121.8(16) . . ?
C8B N3B Ni2 118.2(11) . . ?
C12B N3B Ni2 119.3(12) . . ?
C13B N4B C14B 112.0(13) . . ?
C13B N4B Ni2 108.2(10) . . ?
C14B N4B Ni2 107.8(10) . . ?
C13B N4B H4BB 109.6 . . ?
C14B N4B H4BB 109.6 . . ?
Ni2 N4B H4BB 109.6 . . ?
N1B C1B C2B 120.9(17) . . ?
N1B C1B C14B 114.1(15) . . ?
C2B C1B C14B 124.8(16) . . ?
C3B C2B C1B 118.4(17) . . ?
C3B C2B H2BA 120.8 . . ?
C1B C2B H2BA 120.8 . . ?
C4B C3B C2B 121.2(18) . . ?
C4B C3B H3BA 119.4 . . ?
C2B C3B H3BA 119.4 . . ?
C3B C4B C5B 118.8(17) . . ?
C3B C4B H4BA 120.6 . . ?
C5B C4B H4BA 120.6 . . ?
N1B C5B C4B 119.4(16) . . ?
N1B C5B C6B 116.1(17) . . ?
C4B C5B C6B 124.4(17) . . ?
C5B C6B N2B 110.0(15) . . ?
C5B C6B H6BA 109.7 . . ?
N2B C6B H6BA 109.7 . . ?
C5B C6B H6BB 109.7 . . ?
N2B C6B H6BB 109.7 . . ?
H6BA C6B H6BB 108.2 . . ?
N2B C7B C8B 112.6(14) . . ?
N2B C7B H7BA 109.1 . . ?
C8B C7B H7BA 109.1 . . ?
N2B C7B H7BB 109.1 . . ?
C8B C7B H7BB 109.1 . . ?
H7BA C7B H7BB 107.8 . . ?
N3B C8B C9B 120.6(17) . . ?
N3B C8B C7B 115.0(15) . . ?
C9B C8B C7B 124.4(16) . . ?
C10B C9B C8B 118.9(18) . . ?
C10B C9B H9BA 120.5 . . ?
C8B C9B H9BA 120.5 . . ?
C9B C10B C11B 120.3(16) . . ?
C9B C10B H10B 119.8 . . ?
C11B C10B H10B 119.8 . . ?
C12B C11B C10B 117.7(16) . . ?
C12B C11B H11B 121.2 . . ?
C10B C11B H11B 121.2 . . ?
N3B C12B C11B 120.7(18) . . ?
N3B C12B C13B 115.2(15) . . ?
C11B C12B C13B 124.1(16) . . ?
N4B C13B C12B 110.9(14) . . ?
N4B C13B H13A 109.5 . . ?
C12B C13B H13A 109.5 . . ?
N4B C13B H13B 109.5 . . ?
C12B C13B H13B 109.5 . . ?
H13A C13B H13B 108.0 . . ?
N4B C14B C1B 111.3(13) . . ?
N4B C14B H14C 109.4 . . ?
C1B C14B H14C 109.4 . . ?
N4B C14B H14D 109.4 . . ?
C1B C14B H14D 109.4 . . ?
H14C C14B H14D 108.0 . . ?
C1M O1M H1M 109.5 . . ?
O1M C1M H1M1 109.5 . . ?
O1M C1M H1M2 109.5 . . ?
H1M1 C1M H1M2 109.5 . . ?
O1M C1M H1M3 109.5 . . ?
H1M1 C1M H1M3 109.5 . . ?
H1M2 C1M H1M3 109.5 . . ?
C2M O2M H2M 109.5 . . ?
O2M C2M H2M1 109.5 . . ?
O2M C2M H2M2 109.5 . . ?
H2M1 C2M H2M2 109.5 . . ?
O2M C2M H2M3 109.5 . . ?
H2M1 C2M H2M3 109.5 . . ?
H2M2 C2M H2M3 109.5 . . ?

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
C14A N4A C1A C2A -90.9(17) . . . . ?
Ni1 N4A C1A C2A 28.8(15) . . . . ?
C6A N1A C2A C3A -3(2) . . . . ?
Ni1 N1A C2A C3A -174.5(12) . . . . ?
C6A N1A C2A C1A -178.4(14) . . . . ?
Ni1 N1A C2A C1A 10.3(18) . . . . ?
N4A C1A C2A N1A -27(2) . . . . ?
N4A C1A C2A C3A 157.6(16) . . . . ?
N1A C2A C3A C4A 0(3) . . . . ?
C1A C2A C3A C4A 174.3(15) . . . . ?
C2A C3A C4A C5A 2(3) . . . . ?
C3A C4A C5A C6A 0(3) . . . . ?
C2A N1A C6A C5A 5(2) . . . . ?
Ni1 N1A C6A C5A 176.2(12) . . . . ?
C2A N1A C6A C7A 178.8(15) . . . . ?
Ni1 N1A C6A C7A -10.0(19) . . . . ?
C4A C5A C6A N1A -3(3) . . . . ?
C4A C5A C6A C7A -176.3(17) . . . . ?
N1A C6A C7A N2A 26(2) . . . . ?
C5A C6A C7A N2A -160.6(16) . . . . ?
C8A N2A C7A C6A 91.6(17) . . . . ?
Ni1 N2A C7A C6A -28.5(16) . . . . ?
C7A N2A C8A C9A -94.7(17) . . . . ?
Ni1 N2A C8A C9A 24.5(18) . . . . ?
C13A N3A C9A C10A -1(3) . . . . ?
Ni1 N3A C9A C10A -167.5(13) . . . . ?
C13A N3A C9A C8A 178.2(15) . . . . ?
Ni1 N3A C9A C8A 12(2) . . . . ?
N2A C8A C9A N3A -25(2) . . . . ?
N2A C8A C9A C10A 154.8(16) . . . . ?
N3A C9A C10A C11A -1(3) . . . . ?
C8A C9A C10A C11A 179.5(17) . . . . ?
C9A C10A C11A C12A 1(3) . . . . ?
C10A C11A C12A C13A 1(3) . . . . ?
C9A N3A C13A C12A 3(2) . . . . ?
Ni1 N3A C13A C12A 169.6(13) . . . . ?
C9A N3A C13A C14A 179.9(15) . . . . ?
Ni1 N3A C13A C14A -13.8(19) . . . . ?
C11A C12A C13A N3A -3(3) . . . . ?
C11A C12A C13A C14A -179.3(16) . . . . ?
N3A C13A C14A N4A 27.5(19) . . . . ?
C12A C13A C14A N4A -155.9(15) . . . . ?
C1A N4A C14A C13A 91.5(17) . . . . ?
Ni1 N4A C14A C13A -27.0(15) . . . . ?
C5B N1B C1B C2B -3(2) . . . . ?
Ni2 N1B C1B C2B -172.7(12) . . . . ?
C5B N1B C1B C14B -178.3(14) . . . . ?
Ni2 N1B C1B C14B 11.7(18) . . . . ?
N1B C1B C2B C3B 2(2) . . . . ?
C14B C1B C2B C3B 177.1(15) . . . . ?
C1B C2B C3B C4B -2(3) . . . . ?
C2B C3B C4B C5B 2(3) . . . . ?
C1B N1B C5B C4B 3(2) . . . . ?
Ni2 N1B C5B C4B 173.2(12) . . . . ?
C1B N1B C5B C6B -179.4(14) . . . . ?
Ni2 N1B C5B C6B -9.3(19) . . . . ?
C3B C4B C5B N1B -3(3) . . . . ?
C3B C4B C5B C6B 179.8(17) . . . . ?
N1B C5B C6B N2B 24(2) . . . . ?
C4B C5B C6B N2B -158.5(16) . . . . ?
C7B N2B C6B C5B 93.7(17) . . . . ?
Ni2 N2B C6B C5B -26.2(17) . . . . ?
C6B N2B C7B C8B -96.6(18) . . . . ?
Ni2 N2B C7B C8B 23.5(19) . . . . ?
C12B N3B C8B C9B -2(2) . . . . ?
Ni2 N3B C8B C9B -172.0(12) . . . . ?
C12B N3B C8B C7B 177.6(15) . . . . ?
Ni2 N3B C8B C7B 7.4(19) . . . . ?
N2B C7B C8B N3B -22(2) . . . . ?
N2B C7B C8B C9B 157.8(17) . . . . ?
N3B C8B C9B C10B 2(3) . . . . ?
C7B C8B C9B C10B -177.5(16) . . . . ?
C8B C9B C10B C11B -1(3) . . . . ?
C9B C10B C11B C12B 1(3) . . . . ?
C8B N3B C12B C11B 1(2) . . . . ?
Ni2 N3B C12B C11B 171.3(13) . . . . ?
C8B N3B C12B C13B 179.8(15) . . . . ?
Ni2 N3B C12B C13B -10.2(19) . . . . ?
C10B C11B C12B N3B -1(3) . . . . ?
C10B C11B C12B C13B -179.1(16) . . . . ?
C14B N4B C13B C12B 94.0(16) . . . . ?
Ni2 N4B C13B C12B -24.7(16) . . . . ?
N3B C12B C13B N4B 24(2) . . . . ?
C11B C12B C13B N4B -157.8(16) . . . . ?
C13B N4B C14B C1B -93.1(16) . . . . ?
Ni2 N4B C14B C1B 25.8(15) . . . . ?
N1B C1B C14B N4B -25.6(19) . . . . ?
C2B C1B C14B N4B 159.1(15) . . . . ?

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
N2A H2AA I1 1.00 2.70 3.628(14) 154.6 . yes
N4A H4AB I1 1.00 2.73 3.673(15) 157.7 3_677 yes
C1A H1AB I1 0.99 3.22 4.074(17) 145.5 1_545 yes
C3A H3AA O1M 0.95 2.57 3.52(2) 172.4 1_545 yes
C8A H8AA O2M 0.99 2.55 3.51(2) 163.3 3_676 yes
C14A H14B I1 0.99 3.24 4.104(17) 146.2 1_545 yes
N2B H2BB I2 1.00 2.69 3.625(15) 155.2 . yes
N4B H4BB I2 1.00 2.73 3.664(16) 156.1 3_666 yes
C11B H11B O2M 0.95 2.59 3.52(2) 167.1 1_545 yes
C14B H14D I2 0.99 3.16 4.026(17) 146.4 1_545 yes
O1M H1M I1 0.84 2.68 3.519(14) 178.3 . yes
C1M H1M3 I2 0.98 3.19 4.146(14) 165.8 2_556 yes
O2M H2M I2 0.84 2.78 3.505(14) 145.6 . yes
C2M H2M3 I1 0.98 3.15 4.092(17) 160.6 3_676 yes

_refine_diff_density_max         6.718
_refine_diff_density_min         -7.661
_refine_diff_density_rms         0.424

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[(LH)Ni(CH3CN)2](BPh4)2
_database_code_depnum_ccdc_archive 'CCDC 1878193'
loop_
_audit_author_name
_audit_author_address
'Sakthi Raje'
;Indian Institute of Technology Kanpur
India
;
_audit_update_record             
;
2018-11-09 deposited with the CCDC.	2019-04-18 downloaded from the CCDC.
;
_audit_creation_date             2018-10-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H22 N6 Ni, 2(C24 H20 B), C2 H3 N'
_chemical_formula_sum            'C68 H65 B2 N7 Ni'
_chemical_formula_weight         1060.60
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5825(5)
_cell_length_b                   13.5215(6)
_cell_length_c                   19.6576(8)
_cell_angle_alpha                98.7500(10)
_cell_angle_beta                 101.4640(10)
_cell_angle_gamma                103.6170(10)
_cell_volume                     2867.7(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.30
_shelx_estimated_absorpt_T_max   0.934
_shelx_estimated_absorpt_T_min   0.920
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1176 before and 0.0507 after correction. The Ratio of minimum to maximum transmission is 0.8516. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35330
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.119
_diffrn_reflns_theta_max         25.119
_diffrn_reflns_theta_min         2.090
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8203
_reflns_number_total             10208
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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)'
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         10208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0419
_refine_ls_restrained_S_all      0.964
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1326
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N4(H4), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C00O(H00A,H00B), C00R(H00C,H00D), C00U(H00F,H00G), C01Q(H01A,H01B)
2.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00C(H00H), C00E(H00E), C00G(H00J), C00I(H00I), C00J(H00K),
 C00M(H00M), C00N(H00N), C00P(H00P), C00Q(H00Q), C00S(H00S), C00T(H00T),
 C00V(H00V), C00W(H00W), C00Z(H00Z), C010(H010), C012(H012), C014(H014),
 C015(H015), C017(H017), C018(H018), C019(H019), C01A(H01J), C01B(H01G),
 C01C(H01C), C01D(H01M), C01E(H01H), C01F(H01P), C01G(H01I), C01H(H01Q),
 C01I(H01S), C01J(H01T), C01K(H01K), C01L(H01L), C01M(H01U), C01N(H01N),
 C01O(H01O), C01P(H01W), C01R(H01R), C01S(H01Z), C01T(H01), C01U(H0AA),
 C01V(H01V), C01X(H01X), C01Y(H01Y), C021(H021)
2.d Idealised Me refined as rotating group:
 C01Z(H01D,H01E,H01F), C020(H02D,H02E,H02F), C025(H02A,H02B,H02C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -0.01820(2) 0.22148(2) 0.71312(2) 0.01870(11) Uani 1 1 d . . . . .
N1 N 0.01127(15) 0.12122(13) 0.77501(9) 0.0167(4) Uani 1 1 d . . . . .
N3 N -0.16915(15) 0.22054(13) 0.74842(9) 0.0173(4) Uani 1 1 d . . . . .
N1S N -0.04454(17) 0.32921(14) 0.65314(9) 0.0245(4) Uani 1 1 d . . . . .
N4 N 0.06319(15) 0.32905(13) 0.81328(9) 0.0199(4) Uani 1 1 d . . . . .
H4 H 0.123726 0.390353 0.806104 0.024 Uiso 1 1 calc R . . . .
N2S N 0.14182(18) 0.22179(15) 0.68308(10) 0.0257(4) Uani 1 1 d . . . . .
N2 N -0.14110(16) 0.07849(13) 0.64573(9) 0.0215(4) Uani 1 1 d . . . . .
H2 H -0.132843 0.075672 0.595845 0.026 Uiso 1 1 calc R . . . .
C008 C 0.07175(18) 0.15871(16) 0.84301(10) 0.0176(4) Uani 1 1 d . . . . .
C009 C 1.01357(19) 0.75007(15) 0.96202(11) 0.0204(5) Uani 1 1 d . . . . .
H009 H 0.980826 0.758130 1.002512 0.025 Uiso 1 1 calc R . . . .
C00A C -0.15745(19) 0.28365(16) 0.81010(11) 0.0196(5) Uani 1 1 d . . . . .
C00B C -0.04232(18) 0.01940(16) 0.75046(11) 0.0191(5) Uani 1 1 d . . . . .
C00C C -0.02539(19) 0.22460(15) 0.34438(11) 0.0204(5) Uani 1 1 d . . . . .
H00H H -0.072371 0.200834 0.296659 0.024 Uiso 1 1 calc R . . . .
C00D C 0.75405(19) 0.55089(16) 0.92866(10) 0.0184(5) Uani 1 1 d . . . . .
C00E C 0.08323(18) 0.09271(16) 0.88992(11) 0.0197(5) Uani 1 1 d . . . . .
H00E H 0.125667 0.119326 0.938309 0.024 Uiso 1 1 calc R . . . .
C00F C -0.27179(19) 0.14415(16) 0.71758(11) 0.0212(5) Uani 1 1 d . . . . .
C00G C -0.17021(19) 0.01125(16) 0.45650(10) 0.0187(5) Uani 1 1 d . . . . .
H00J H -0.087619 0.039243 0.455089 0.022 Uiso 1 1 calc R . . . .
C00H C -0.25785(18) 0.05967(15) 0.42907(10) 0.0170(4) Uani 1 1 d . . . . .
C00I C 0.8031(2) 0.44617(16) 1.01598(11) 0.0211(5) Uani 1 1 d . . . . .
H00I H 0.863160 0.430503 1.049945 0.025 Uiso 1 1 calc R . . . .
C00J C -0.00819(19) 0.24790(15) 0.46814(11) 0.0201(5) Uani 1 1 d . . . . .
H00K H -0.043742 0.240329 0.507298 0.024 Uiso 1 1 calc R . . . .
C00K C -0.28037(18) 0.25450(16) 0.41982(10) 0.0179(4) Uani 1 1 d . . . . .
C00L C -0.30204(18) 0.10704(15) 0.30509(11) 0.0172(4) Uani 1 1 d . . . . .
C00M C 0.65694(18) 0.73441(17) 0.97109(11) 0.0203(5) Uani 1 1 d . . . . .
H00M H 0.629292 0.668931 0.983117 0.024 Uiso 1 1 calc R . . . .
C00N C -0.2533(2) 0.27353(17) 0.84331(12) 0.0245(5) Uani 1 1 d . . . . .
H00N H -0.245969 0.319221 0.886688 0.029 Uiso 1 1 calc R . . . .
C00O C 0.12853(19) 0.27525(16) 0.86178(11) 0.0213(5) Uani 1 1 d . . . . .
H00A H 0.126530 0.302366 0.911115 0.026 Uiso 1 1 calc R . . . .
H00B H 0.215334 0.290403 0.859353 0.026 Uiso 1 1 calc R . . . .
C00P C -0.37795(19) 0.01321(16) 0.43271(11) 0.0200(5) Uani 1 1 d . . . . .
H00P H -0.441620 0.041817 0.413637 0.024 Uiso 1 1 calc R . . . .
C00Q C -0.1987(2) -0.07652(16) 0.48591(11) 0.0219(5) Uani 1 1 d . . . . .
H00Q H -0.136211 -0.107447 0.503213 0.026 Uiso 1 1 calc R . . . .
C00R C -0.1045(2) -0.00948(16) 0.67203(11) 0.0241(5) Uani 1 1 d . . . . .
H00C H -0.047938 -0.031786 0.645176 0.029 Uiso 1 1 calc R . . . .
H00D H -0.178049 -0.068974 0.663316 0.029 Uiso 1 1 calc R . . . .
C00S C 0.66302(18) 0.66775(17) 0.76154(11) 0.0201(5) Uani 1 1 d . . . . .
H00S H 0.663945 0.736082 0.782614 0.024 Uiso 1 1 calc R . . . .
C00T C 0.63172(19) 0.49189(16) 0.91619(11) 0.0215(5) Uani 1 1 d . . . . .
H00T H 0.571468 0.505517 0.881195 0.026 Uiso 1 1 calc R . . . .
C00U C -0.03570(19) 0.36450(16) 0.83807(11) 0.0221(5) Uani 1 1 d . . . . .
H00F H -0.041548 0.429552 0.822120 0.027 Uiso 1 1 calc R . . . .
H00G H -0.015380 0.379857 0.890602 0.027 Uiso 1 1 calc R . . . .
C00V C 0.0993(2) 0.27458(16) 0.35724(12) 0.0233(5) Uani 1 1 d . . . . .
H00V H 0.135573 0.283954 0.318529 0.028 Uiso 1 1 calc R . . . .
C00W C 1.1378(2) 0.79369(16) 0.97033(12) 0.0256(5) Uani 1 1 d . . . . .
H00W H 1.188349 0.829262 1.015835 0.031 Uiso 1 1 calc R . . . .
C00X C -0.08360(19) 0.20827(15) 0.39912(11) 0.0173(4) Uani 1 1 d . . . . .
C00Y C 0.93376(19) 0.69464(15) 0.89684(11) 0.0186(5) Uani 1 1 d . . . . .
C00Z C -0.40324(19) 0.13363(17) 0.26904(11) 0.0228(5) Uani 1 1 d . . . . .
H00Z H -0.432626 0.184610 0.293823 0.027 Uiso 1 1 calc R . . . .
C010 C 0.61710(19) 0.81793(17) 0.99935(11) 0.0225(5) Uani 1 1 d . . . . .
H010 H 0.563286 0.808100 1.029954 0.027 Uiso 1 1 calc R . . . .
C011 C -0.05170(19) 0.39231(17) 0.62162(11) 0.0234(5) Uani 1 1 d . . . . .
C012 C -0.33508(19) 0.26041(17) 0.47713(11) 0.0222(5) Uani 1 1 d . . . . .
H012 H -0.345193 0.203969 0.500898 0.027 Uiso 1 1 calc R . . . .
C013 C 0.71644(18) 0.60861(16) 0.80411(11) 0.0182(5) Uani 1 1 d . . . . .
C014 C 0.03100(19) -0.01332(16) 0.86425(11) 0.0201(5) Uani 1 1 d . . . . .
H014 H 0.039651 -0.060486 0.894889 0.024 Uiso 1 1 calc R . . . .
C015 C 0.77239(19) 0.84377(16) 0.91146(11) 0.0201(5) Uani 1 1 d . . . . .
H015 H 0.826619 0.854815 0.881182 0.024 Uiso 1 1 calc R . . . .
C016 C 0.73641(18) 0.74386(16) 0.92554(10) 0.0170(4) Uani 1 1 d . . . . .
C017 C 0.6550(2) 0.91470(18) 0.98335(11) 0.0259(5) Uani 1 1 d . . . . .
H017 H 0.627687 0.971483 1.002338 0.031 Uiso 1 1 calc R . . . .
C018 C -0.03365(19) -0.05049(16) 0.79412(11) 0.0203(5) Uani 1 1 d . . . . .
H018 H -0.071319 -0.122795 0.776448 0.024 Uiso 1 1 calc R . . . .
C019 C -0.40738(19) -0.07290(16) 0.46309(11) 0.0231(5) Uani 1 1 d . . . . .
H019 H -0.489497 -0.100633 0.465478 0.028 Uiso 1 1 calc R . . . .
C01A C 0.11534(19) 0.29737(15) 0.48151(12) 0.0220(5) Uani 1 1 d . . . . .
H01J H 0.162844 0.322537 0.529053 0.026 Uiso 1 1 calc R . . . .
C01B C 0.6811(2) 0.39227(16) 1.00331(11) 0.0235(5) Uani 1 1 d . . . . .
H01G H 0.656494 0.340334 1.029088 0.028 Uiso 1 1 calc R . . . .
C01C C -0.3701(2) 0.12882(17) 0.74823(12) 0.0275(5) Uani 1 1 d . . . . .
H01C H -0.442898 0.074454 0.726664 0.033 Uiso 1 1 calc R . . . .
C01D C -0.4627(2) 0.08897(18) 0.19872(12) 0.0293(5) Uani 1 1 d . . . . .
H01M H -0.531049 0.109719 0.176325 0.035 Uiso 1 1 calc R . . . .
C01E C 0.60850(19) 0.63042(18) 0.68944(11) 0.0245(5) Uani 1 1 d . . . . .
H01H H 0.571527 0.672521 0.662587 0.029 Uiso 1 1 calc R . . . .
C01F C -0.3176(2) -0.11856(16) 0.48993(11) 0.0234(5) Uani 1 1 d . . . . .
H01P H -0.337356 -0.177469 0.510649 0.028 Uiso 1 1 calc R . . . .
C01G C 0.83778(19) 0.52359(15) 0.97879(10) 0.0171(4) Uani 1 1 d . . . . .
H01I H 0.922174 0.559350 0.987979 0.021 Uiso 1 1 calc R . . . .
C01H C -0.26642(19) 0.34273(16) 0.38881(11) 0.0215(5) Uani 1 1 d . . . . .
H01Q H -0.228223 0.343532 0.350291 0.026 Uiso 1 1 calc R . . . .
C01I C 0.16992(19) 0.31027(16) 0.42568(12) 0.0218(5) Uani 1 1 d . . . . .
H01S H 0.255028 0.343346 0.434532 0.026 Uiso 1 1 calc R . . . .
C01J C -0.3055(2) 0.42770(17) 0.41165(11) 0.0258(5) Uani 1 1 d . . . . .
H01T H -0.294236 0.485261 0.388967 0.031 Uiso 1 1 calc R . . . .
C01K C 0.5949(2) 0.41481(16) 0.95255(12) 0.0236(5) Uani 1 1 d . . . . .
H01K H 0.510951 0.377487 0.942772 0.028 Uiso 1 1 calc R . . . .
C01L C 0.9895(2) 0.68563(18) 0.83981(12) 0.0249(5) Uani 1 1 d . . . . .
H01L H 0.940827 0.647133 0.794522 0.030 Uiso 1 1 calc R . . . .
C01M C -0.4228(2) 0.01460(18) 0.16133(12) 0.0288(6) Uani 1 1 d . . . . .
H01U H -0.462257 -0.015378 0.112881 0.035 Uiso 1 1 calc R . . . .
C01N C -0.3589(2) 0.19576(18) 0.81185(12) 0.0283(5) Uani 1 1 d . . . . .
H01N H -0.425560 0.187449 0.833862 0.034 Uiso 1 1 calc R . . . .
C01O C 0.7340(2) 0.92636(17) 0.93873(11) 0.0233(5) Uani 1 1 d . . . . .
H01O H 0.761748 0.992045 0.927006 0.028 Uiso 1 1 calc R . . . .
C01P C -0.3616(2) 0.42900(18) 0.46821(12) 0.0276(5) Uani 1 1 d . . . . .
H01W H -0.389884 0.486814 0.484007 0.033 Uiso 1 1 calc R . . . .
C01Q C -0.2682(2) 0.08014(18) 0.64857(11) 0.0261(5) Uani 1 1 d . . . . .
H01A H -0.319081 0.007992 0.642722 0.031 Uiso 1 1 calc R . . . .
H01B H -0.303843 0.109208 0.608706 0.031 Uiso 1 1 calc R . . . .
C01R C 0.6081(2) 0.53262(18) 0.65702(11) 0.0260(5) Uani 1 1 d . . . . .
H01R H 0.571172 0.506924 0.607818 0.031 Uiso 1 1 calc R . . . .
C01S C -0.3752(2) 0.34550(17) 0.50068(12) 0.0266(5) Uani 1 1 d . . . . .
H01Z H -0.412424 0.345889 0.539607 0.032 Uiso 1 1 calc R . . . .
C01T C -0.3245(2) -0.01593(18) 0.19525(12) 0.0290(5) Uani 1 1 d . . . . .
H01 H -0.296543 -0.067794 0.170316 0.035 Uiso 1 1 calc R . . . .
C01U C -0.2671(2) 0.02937(17) 0.26566(11) 0.0242(5) Uani 1 1 d . . . . .
H0AA H -0.200645 0.006442 0.288187 0.029 Uiso 1 1 calc R . . . .
C01V C 0.7138(2) 0.50971(17) 0.76885(11) 0.0252(5) Uani 1 1 d . . . . .
H01V H 0.749111 0.466463 0.795426 0.030 Uiso 1 1 calc R . . . .
C01W C 0.2430(2) 0.23417(19) 0.68465(12) 0.0320(6) Uani 1 1 d . . . . .
C01X C 0.6620(2) 0.47217(18) 0.69686(12) 0.0283(5) Uani 1 1 d . . . . .
H01X H 0.663539 0.405003 0.674919 0.034 Uiso 1 1 calc R . . . .
C01Y C 1.1138(2) 0.73125(19) 0.84735(13) 0.0300(6) Uani 1 1 d . . . . .
H01Y H 1.147488 0.724870 0.807141 0.036 Uiso 1 1 calc R . . . .
C01Z C -0.0603(2) 0.47162(18) 0.58028(13) 0.0344(6) Uani 1 1 d . . . . .
H01D H -0.104699 0.438428 0.531166 0.052 Uiso 1 1 calc GR . . . .
H01E H 0.022286 0.512319 0.581113 0.052 Uiso 1 1 calc GR . . . .
H01F H -0.104123 0.517691 0.600631 0.052 Uiso 1 1 calc GR . . . .
C020 C 0.3969(2) 0.65099(19) 0.81594(13) 0.0329(6) Uani 1 1 d . . . . .
H02D H 0.407981 0.672397 0.771693 0.049 Uiso 1 1 calc GR . . . .
H02E H 0.476524 0.669075 0.850132 0.049 Uiso 1 1 calc GR . . . .
H02F H 0.342739 0.686865 0.835626 0.049 Uiso 1 1 calc GR . . . .
C021 C 1.1879(2) 0.78524(18) 0.91221(13) 0.0291(6) Uani 1 1 d . . . . .
H021 H 1.272517 0.816388 0.917096 0.035 Uiso 1 1 calc R . . . .
C022 C 0.3431(2) 0.5406(2) 0.80181(13) 0.0380(6) Uani 1 1 d . . . . .
B1 B -0.2308(2) 0.15756(19) 0.38866(12) 0.0180(5) Uani 1 1 d . . . . .
N7 N 0.3015(3) 0.4527(2) 0.79088(15) 0.0687(8) Uani 1 1 d . . . . .
C025 C 0.3733(2) 0.2501(3) 0.68844(16) 0.0563(9) Uani 1 1 d . . . . .
H02A H 0.397988 0.296672 0.657135 0.084 Uiso 1 1 calc GR . . . .
H02B H 0.388997 0.183023 0.673363 0.084 Uiso 1 1 calc GR . . . .
H02C H 0.420456 0.281245 0.737365 0.084 Uiso 1 1 calc GR . . . .
B2 B 0.7860(2) 0.64891(19) 0.88911(12) 0.0185(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.9973(17) . ?
Ni1 N3 2.0033(17) . ?
Ni1 N1S 2.0479(18) . ?
Ni1 N4 2.1509(17) . ?
Ni1 N2S 2.053(2) . ?
Ni1 N2 2.1667(18) . ?
N1 C008 1.338(3) . ?
N1 C00B 1.338(3) . ?
N3 C00A 1.335(3) . ?
N3 C00F 1.339(3) . ?
N1S C011 1.137(3) . ?
N4 H4 1.0000 . ?
N4 C00O 1.481(2) . ?
N4 C00U 1.479(3) . ?
N2S C01W 1.138(3) . ?
N2 H2 1.0000 . ?
N2 C00R 1.483(3) . ?
N2 C01Q 1.490(3) . ?
C008 C00E 1.387(3) . ?
C008 C00O 1.513(3) . ?
C009 H009 0.9500 . ?
C009 C00W 1.387(3) . ?
C009 C00Y 1.403(3) . ?
C00A C00N 1.386(3) . ?
C00A C00U 1.506(3) . ?
C00B C00R 1.514(3) . ?
C00B C018 1.377(3) . ?
C00C H00H 0.9500 . ?
C00C C00V 1.397(3) . ?
C00C C00X 1.397(3) . ?
C00D C00T 1.405(3) . ?
C00D C01G 1.395(3) . ?
C00D B2 1.642(3) . ?
C00E H00E 0.9500 . ?
C00E C014 1.388(3) . ?
C00F C01C 1.379(3) . ?
C00F C01Q 1.508(3) . ?
C00G H00J 0.9500 . ?
C00G C00H 1.397(3) . ?
C00G C00Q 1.397(3) . ?
C00H C00P 1.406(3) . ?
C00H B1 1.644(3) . ?
C00I H00I 0.9500 . ?
C00I C01B 1.382(3) . ?
C00I C01G 1.394(3) . ?
C00J H00K 0.9500 . ?
C00J C00X 1.407(3) . ?
C00J C01A 1.382(3) . ?
C00K C012 1.399(3) . ?
C00K C01H 1.411(3) . ?
C00K B1 1.635(3) . ?
C00L C00Z 1.397(3) . ?
C00L C01U 1.395(3) . ?
C00L B1 1.643(3) . ?
C00M H00M 0.9500 . ?
C00M C010 1.398(3) . ?
C00M C016 1.404(3) . ?
C00N H00N 0.9500 . ?
C00N C01N 1.372(3) . ?
C00O H00A 0.9900 . ?
C00O H00B 0.9900 . ?
C00P H00P 0.9500 . ?
C00P C019 1.391(3) . ?
C00Q H00Q 0.9500 . ?
C00Q C01F 1.384(3) . ?
C00R H00C 0.9900 . ?
C00R H00D 0.9900 . ?
C00S H00S 0.9500 . ?
C00S C013 1.398(3) . ?
C00S C01E 1.392(3) . ?
C00T H00T 0.9500 . ?
C00T C01K 1.385(3) . ?
C00U H00F 0.9900 . ?
C00U H00G 0.9900 . ?
C00V H00V 0.9500 . ?
C00V C01I 1.375(3) . ?
C00W H00W 0.9500 . ?
C00W C021 1.382(3) . ?
C00X B1 1.639(3) . ?
C00Y C01L 1.404(3) . ?
C00Y B2 1.645(3) . ?
C00Z H00Z 0.9500 . ?
C00Z C01D 1.386(3) . ?
C010 H010 0.9500 . ?
C010 C017 1.383(3) . ?
C011 C01Z 1.450(3) . ?
C012 H012 0.9500 . ?
C012 C01S 1.389(3) . ?
C013 C01V 1.400(3) . ?
C013 B2 1.649(3) . ?
C014 H014 0.9500 . ?
C014 C018 1.384(3) . ?
C015 H015 0.9500 . ?
C015 C016 1.404(3) . ?
C015 C01O 1.370(3) . ?
C016 B2 1.650(3) . ?
C017 H017 0.9500 . ?
C017 C01O 1.388(3) . ?
C018 H018 0.9500 . ?
C019 H019 0.9500 . ?
C019 C01F 1.387(3) . ?
C01A H01J 0.9500 . ?
C01A C01I 1.385(3) . ?
C01B H01G 0.9500 . ?
C01B C01K 1.387(3) . ?
C01C H01C 0.9500 . ?
C01C C01N 1.391(3) . ?
C01D H01M 0.9500 . ?
C01D C01M 1.376(3) . ?
C01E H01H 0.9500 . ?
C01E C01R 1.376(3) . ?
C01F H01P 0.9500 . ?
C01G H01I 0.9500 . ?
C01H H01Q 0.9500 . ?
C01H C01J 1.376(3) . ?
C01I H01S 0.9500 . ?
C01J H01T 0.9500 . ?
C01J C01P 1.395(3) . ?
C01K H01K 0.9500 . ?
C01L H01L 0.9500 . ?
C01L C01Y 1.394(3) . ?
C01M H01U 0.9500 . ?
C01M C01T 1.384(3) . ?
C01N H01N 0.9500 . ?
C01O H01O 0.9500 . ?
C01P H01W 0.9500 . ?
C01P C01S 1.372(3) . ?
C01Q H01A 0.9900 . ?
C01Q H01B 0.9900 . ?
C01R H01R 0.9500 . ?
C01R C01X 1.383(3) . ?
C01S H01Z 0.9500 . ?
C01T H01 0.9500 . ?
C01T C01U 1.385(3) . ?
C01U H0AA 0.9500 . ?
C01V H01V 0.9500 . ?
C01V C01X 1.386(3) . ?
C01W C025 1.458(4) . ?
C01X H01X 0.9500 . ?
C01Y H01Y 0.9500 . ?
C01Y C021 1.372(3) . ?
C01Z H01D 0.9800 . ?
C01Z H01E 0.9800 . ?
C01Z H01F 0.9800 . ?
C020 H02D 0.9800 . ?
C020 H02E 0.9800 . ?
C020 H02F 0.9800 . ?
C020 C022 1.436(4) . ?
C021 H021 0.9500 . ?
C022 N7 1.141(3) . ?
C025 H02A 0.9800 . ?
C025 H02B 0.9800 . ?
C025 H02C 0.9800 . ?

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
N1 Ni1 N3 86.72(7) . . ?
N1 Ni1 N1S 177.64(7) . . ?
N1 Ni1 N4 80.56(7) . . ?
N1 Ni1 N2S 90.43(7) . . ?
N1 Ni1 N2 80.10(7) . . ?
N3 Ni1 N1S 93.19(7) . . ?
N3 Ni1 N4 80.57(7) . . ?
N3 Ni1 N2S 176.46(7) . . ?
N3 Ni1 N2 80.30(7) . . ?
N1S Ni1 N4 97.10(7) . . ?
N1S Ni1 N2S 89.57(7) . . ?
N1S Ni1 N2 102.21(7) . . ?
N4 Ni1 N2 153.43(7) . . ?
N2S Ni1 N4 96.90(7) . . ?
N2S Ni1 N2 101.29(7) . . ?
C008 N1 Ni1 118.69(14) . . ?
C008 N1 C00B 121.23(17) . . ?
C00B N1 Ni1 119.55(13) . . ?
C00A N3 Ni1 118.12(14) . . ?
C00A N3 C00F 121.49(18) . . ?
C00F N3 Ni1 119.08(14) . . ?
C011 N1S Ni1 175.72(18) . . ?
Ni1 N4 H4 109.0 . . ?
C00O N4 Ni1 107.67(12) . . ?
C00O N4 H4 109.0 . . ?
C00U N4 Ni1 107.72(12) . . ?
C00U N4 H4 109.0 . . ?
C00U N4 C00O 114.38(16) . . ?
C01W N2S Ni1 162.01(19) . . ?
Ni1 N2 H2 109.4 . . ?
C00R N2 Ni1 107.68(12) . . ?
C00R N2 H2 109.4 . . ?
C00R N2 C01Q 113.53(17) . . ?
C01Q N2 Ni1 107.40(12) . . ?
C01Q N2 H2 109.4 . . ?
N1 C008 C00E 120.86(19) . . ?
N1 C008 C00O 114.51(17) . . ?
C00E C008 C00O 124.58(18) . . ?
C00W C009 H009 118.3 . . ?
C00W C009 C00Y 123.3(2) . . ?
C00Y C009 H009 118.3 . . ?
N3 C00A C00N 120.62(19) . . ?
N3 C00A C00U 114.84(18) . . ?
C00N C00A C00U 124.54(19) . . ?
N1 C00B C00R 114.12(17) . . ?
N1 C00B C018 120.84(19) . . ?
C018 C00B C00R 124.96(19) . . ?
C00V C00C H00H 118.8 . . ?
C00V C00C C00X 122.4(2) . . ?
C00X C00C H00H 118.8 . . ?
C00T C00D B2 119.20(18) . . ?
C01G C00D C00T 115.10(19) . . ?
C01G C00D B2 125.55(19) . . ?
C008 C00E H00E 120.9 . . ?
C008 C00E C014 118.17(19) . . ?
C014 C00E H00E 120.9 . . ?
N3 C00F C01C 120.9(2) . . ?
N3 C00F C01Q 114.18(19) . . ?
C01C C00F C01Q 124.9(2) . . ?
C00H C00G H00J 118.6 . . ?
C00Q C00G H00J 118.6 . . ?
C00Q C00G C00H 122.90(19) . . ?
C00G C00H C00P 115.09(18) . . ?
C00G C00H B1 124.62(18) . . ?
C00P C00H B1 120.09(18) . . ?
C01B C00I H00I 120.1 . . ?
C01B C00I C01G 119.8(2) . . ?
C01G C00I H00I 120.1 . . ?
C00X C00J H00K 118.6 . . ?
C01A C00J H00K 118.6 . . ?
C01A C00J C00X 122.9(2) . . ?
C012 C00K C01H 114.83(19) . . ?
C012 C00K B1 125.82(18) . . ?
C01H C00K B1 119.33(18) . . ?
C00Z C00L B1 124.03(19) . . ?
C01U C00L C00Z 114.94(19) . . ?
C01U C00L B1 120.97(18) . . ?
C010 C00M H00M 118.8 . . ?
C010 C00M C016 122.3(2) . . ?
C016 C00M H00M 118.8 . . ?
C00A C00N H00N 120.9 . . ?
C01N C00N C00A 118.2(2) . . ?
C01N C00N H00N 120.9 . . ?
N4 C00O C008 111.80(16) . . ?
N4 C00O H00A 109.3 . . ?
N4 C00O H00B 109.3 . . ?
C008 C00O H00A 109.3 . . ?
C008 C00O H00B 109.3 . . ?
H00A C00O H00B 107.9 . . ?
C00H C00P H00P 118.6 . . ?
C019 C00P C00H 122.7(2) . . ?
C019 C00P H00P 118.6 . . ?
C00G C00Q H00Q 119.9 . . ?
C01F C00Q C00G 120.2(2) . . ?
C01F C00Q H00Q 119.9 . . ?
N2 C00R C00B 112.10(17) . . ?
N2 C00R H00C 109.2 . . ?
N2 C00R H00D 109.2 . . ?
C00B C00R H00C 109.2 . . ?
C00B C00R H00D 109.2 . . ?
H00C C00R H00D 107.9 . . ?
C013 C00S H00S 118.7 . . ?
C01E C00S H00S 118.7 . . ?
C01E C00S C013 122.6(2) . . ?
C00D C00T H00T 118.5 . . ?
C01K C00T C00D 123.0(2) . . ?
C01K C00T H00T 118.5 . . ?
N4 C00U C00A 111.60(17) . . ?
N4 C00U H00F 109.3 . . ?
N4 C00U H00G 109.3 . . ?
C00A C00U H00F 109.3 . . ?
C00A C00U H00G 109.3 . . ?
H00F C00U H00G 108.0 . . ?
C00C C00V H00V 119.9 . . ?
C01I C00V C00C 120.3(2) . . ?
C01I C00V H00V 119.9 . . ?
C009 C00W H00W 120.1 . . ?
C021 C00W C009 119.8(2) . . ?
C021 C00W H00W 120.1 . . ?
C00C C00X C00J 115.18(19) . . ?
C00C C00X B1 125.35(18) . . ?
C00J C00X B1 119.23(18) . . ?
C009 C00Y C01L 114.77(19) . . ?
C009 C00Y B2 121.39(18) . . ?
C01L C00Y B2 123.80(19) . . ?
C00L C00Z H00Z 118.5 . . ?
C01D C00Z C00L 122.9(2) . . ?
C01D C00Z H00Z 118.5 . . ?
C00M C010 H010 119.6 . . ?
C017 C010 C00M 120.9(2) . . ?
C017 C010 H010 119.6 . . ?
N1S C011 C01Z 178.9(2) . . ?
C00K C012 H012 118.7 . . ?
C01S C012 C00K 122.6(2) . . ?
C01S C012 H012 118.7 . . ?
C00S C013 C01V 115.29(19) . . ?
C00S C013 B2 125.17(19) . . ?
C01V C013 B2 119.46(18) . . ?
C00E C014 H014 119.9 . . ?
C018 C014 C00E 120.15(19) . . ?
C018 C014 H014 119.9 . . ?
C016 C015 H015 118.0 . . ?
C01O C015 H015 118.0 . . ?
C01O C015 C016 124.0(2) . . ?
C00M C016 B2 125.30(18) . . ?
C015 C016 C00M 114.36(19) . . ?
C015 C016 B2 120.34(18) . . ?
C010 C017 H017 121.0 . . ?
C010 C017 C01O 118.0(2) . . ?
C01O C017 H017 121.0 . . ?
C00B C018 C014 118.7(2) . . ?
C00B C018 H018 120.6 . . ?
C014 C018 H018 120.6 . . ?
C00P C019 H019 119.8 . . ?
C01F C019 C00P 120.42(19) . . ?
C01F C019 H019 119.8 . . ?
C00J C01A H01J 120.0 . . ?
C00J C01A C01I 120.1(2) . . ?
C01I C01A H01J 120.0 . . ?
C00I C01B H01G 120.4 . . ?
C00I C01B C01K 119.30(19) . . ?
C01K C01B H01G 120.4 . . ?
C00F C01C H01C 121.2 . . ?
C00F C01C C01N 117.7(2) . . ?
C01N C01C H01C 121.2 . . ?
C00Z C01D H01M 120.0 . . ?
C01M C01D C00Z 120.0(2) . . ?
C01M C01D H01M 120.0 . . ?
C00S C01E H01H 119.9 . . ?
C01R C01E C00S 120.1(2) . . ?
C01R C01E H01H 119.9 . . ?
C00Q C01F C019 118.62(19) . . ?
C00Q C01F H01P 120.7 . . ?
C019 C01F H01P 120.7 . . ?
C00D C01G H01I 118.5 . . ?
C00I C01G C00D 122.9(2) . . ?
C00I C01G H01I 118.5 . . ?
C00K C01H H01Q 118.4 . . ?
C01J C01H C00K 123.2(2) . . ?
C01J C01H H01Q 118.4 . . ?
C00V C01I C01A 119.1(2) . . ?
C00V C01I H01S 120.4 . . ?
C01A C01I H01S 120.4 . . ?
C01H C01J H01T 120.1 . . ?
C01H C01J C01P 119.8(2) . . ?
C01P C01J H01T 120.1 . . ?
C00T C01K C01B 119.8(2) . . ?
C00T C01K H01K 120.1 . . ?
C01B C01K H01K 120.1 . . ?
C00Y C01L H01L 118.9 . . ?
C01Y C01L C00Y 122.3(2) . . ?
C01Y C01L H01L 118.9 . . ?
C01D C01M H01U 120.4 . . ?
C01D C01M C01T 119.1(2) . . ?
C01T C01M H01U 120.4 . . ?
C00N C01N C01C 121.1(2) . . ?
C00N C01N H01N 119.5 . . ?
C01C C01N H01N 119.5 . . ?
C015 C01O C017 120.5(2) . . ?
C015 C01O H01O 119.8 . . ?
C017 C01O H01O 119.8 . . ?
C01J C01P H01W 120.5 . . ?
C01S C01P C01J 119.0(2) . . ?
C01S C01P H01W 120.5 . . ?
N2 C01Q C00F 111.99(17) . . ?
N2 C01Q H01A 109.2 . . ?
N2 C01Q H01B 109.2 . . ?
C00F C01Q H01A 109.2 . . ?
C00F C01Q H01B 109.2 . . ?
H01A C01Q H01B 107.9 . . ?
C01E C01R H01R 120.4 . . ?
C01E C01R C01X 119.3(2) . . ?
C01X C01R H01R 120.4 . . ?
C012 C01S H01Z 119.7 . . ?
C01P C01S C012 120.6(2) . . ?
C01P C01S H01Z 119.7 . . ?
C01M C01T H01 120.1 . . ?
C01M C01T C01U 119.8(2) . . ?
C01U C01T H01 120.1 . . ?
C00L C01U H0AA 118.4 . . ?
C01T C01U C00L 123.1(2) . . ?
C01T C01U H0AA 118.4 . . ?
C013 C01V H01V 118.6 . . ?
C01X C01V C013 122.9(2) . . ?
C01X C01V H01V 118.6 . . ?
N2S C01W C025 178.7(3) . . ?
C01R C01X C01V 119.9(2) . . ?
C01R C01X H01X 120.0 . . ?
C01V C01X H01X 120.0 . . ?
C01L C01Y H01Y 119.6 . . ?
C021 C01Y C01L 120.7(2) . . ?
C021 C01Y H01Y 119.6 . . ?
C011 C01Z H01D 109.5 . . ?
C011 C01Z H01E 109.5 . . ?
C011 C01Z H01F 109.5 . . ?
H01D C01Z H01E 109.5 . . ?
H01D C01Z H01F 109.5 . . ?
H01E C01Z H01F 109.5 . . ?
H02D C020 H02E 109.5 . . ?
H02D C020 H02F 109.5 . . ?
H02E C020 H02F 109.5 . . ?
C022 C020 H02D 109.5 . . ?
C022 C020 H02E 109.5 . . ?
C022 C020 H02F 109.5 . . ?
C00W C021 H021 120.5 . . ?
C01Y C021 C00W 119.1(2) . . ?
C01Y C021 H021 120.5 . . ?
N7 C022 C020 179.3(3) . . ?
C00K B1 C00H 113.14(17) . . ?
C00K B1 C00L 110.96(17) . . ?
C00K B1 C00X 104.63(16) . . ?
C00L B1 C00H 104.35(16) . . ?
C00X B1 C00H 111.66(17) . . ?
C00X B1 C00L 112.31(17) . . ?
C01W C025 H02A 109.5 . . ?
C01W C025 H02B 109.5 . . ?
C01W C025 H02C 109.5 . . ?
H02A C025 H02B 109.5 . . ?
H02A C025 H02C 109.5 . . ?
H02B C025 H02C 109.5 . . ?
C00D B2 C00Y 112.72(17) . . ?
C00D B2 C013 108.27(17) . . ?
C00D B2 C016 108.65(16) . . ?
C00Y B2 C013 108.70(17) . . ?
C00Y B2 C016 107.97(17) . . ?
C013 B2 C016 110.54(17) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[(LH)Ni(BH4)](BPh4)
_database_code_depnum_ccdc_archive 'CCDC 1878194'
loop_
_audit_author_name
_audit_author_address
'Ray J. Butcher'
;Howard University
United States of America
;
_audit_update_record             
;
2019-03-21 deposited with the CCDC.	2019-04-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
'Olex2 1.2(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H20 B N4 Ni, C24 H20 B'
_chemical_formula_sum            'C38 H40 B2 N4 Ni'
_chemical_formula_weight         633.07

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'
B B 0.0013 0.0007 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   11.1094(7)
_cell_length_b                   15.0969(9)
_cell_length_c                   18.9302(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3174.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6403
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      24.91

_exptl_crystal_description       needle
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_F_000             1336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.646
_shelx_estimated_absorpt_T_min   0.871
_shelx_estimated_absorpt_T_max   0.893
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25414
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_av_R_equivalents  0.0967
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.126
_diffrn_reflns_theta_max         25.087
_diffrn_reflns_theta_full        25.087
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5621
_reflns_number_gt                4494
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.996

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0434P)²+0.0634P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1589 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(11)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         5621
_refine_ls_number_parameters     422
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0508
_refine_ls_wR_factor_ref         0.1005
_refine_ls_wR_factor_gt          0.0918
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.57528(6) 0.35686(4) 0.61745(3) 0.01464(19) Uani 1 1 d . . . . .
N2 N 0.7610(4) 0.3169(3) 0.6151(2) 0.0161(10) Uani 1 1 d . . . . .
H2 H 0.766806 0.251744 0.623897 0.019 Uiso 1 1 calc R U . . .
N3 N 0.6396(4) 0.4344(3) 0.6932(2) 0.0151(11) Uani 1 1 d . . . . .
N4 N 0.4350(4) 0.4553(3) 0.6210(2) 0.0204(10) Uani 1 1 d . . . . .
H4 H 0.355366 0.427080 0.610917 0.024 Uiso 1 1 calc R U . . .
N1 N 0.6374(4) 0.4390(3) 0.5453(2) 0.0174(11) Uani 1 1 d . . . . .
C32 C 0.2423(5) 0.6973(3) 0.6549(3) 0.0141(12) Uani 1 1 d . . . . .
C2 C 0.7558(5) 0.4343(4) 0.7081(3) 0.0138(12) Uani 1 1 d . . . . .
C4 C 0.7264(6) 0.5571(4) 0.7846(3) 0.0245(15) Uani 1 1 d . . . . .
H4A H 0.757014 0.599238 0.817220 0.029 Uiso 1 1 calc R U . . .
C38 C 0.1105(4) 0.6408(3) 0.7698(3) 0.0143(12) Uani 1 1 d . . . . .
C20 C 0.1410(5) 0.4726(4) 0.6818(3) 0.0189(13) Uani 1 1 d . . . . .
H20 H 0.154945 0.475313 0.731229 0.023 Uiso 1 1 calc R U . . .
C9 C 0.5771(6) 0.5132(3) 0.5303(3) 0.0178(12) Uani 1 1 d . . . . .
C33 C 0.2623(5) 0.7093(3) 0.5820(3) 0.0155(12) Uani 1 1 d . . . . .
H33 H 0.201436 0.690593 0.550026 0.019 Uiso 1 1 calc R U . . .
C31 C 0.2033(5) 0.6046(3) 0.8105(3) 0.0181(13) Uani 1 1 d . . . . .
H31 H 0.274605 0.585744 0.787256 0.022 Uiso 1 1 calc R U . . .
C27 C 0.0094(5) 0.6665(3) 0.8089(3) 0.0155(13) Uani 1 1 d . . . . .
H27 H -0.057101 0.691321 0.784380 0.019 Uiso 1 1 calc R U . . .
C30 C 0.1962(5) 0.5947(3) 0.8835(3) 0.0205(12) Uani 1 1 d . . . . .
H30 H 0.261788 0.569323 0.908571 0.025 Uiso 1 1 calc R U . . .
C13 C 0.7449(5) 0.4215(3) 0.5159(3) 0.0161(13) Uani 1 1 d . . . . .
C14 C 0.8013(5) 0.3367(3) 0.5423(3) 0.0182(13) Uani 1 1 d . . . . .
H14A H 0.778590 0.287193 0.510655 0.022 Uiso 1 1 calc R U . . .
H14B H 0.890091 0.342376 0.541461 0.022 Uiso 1 1 calc R U . . .
C15 C 0.1110(5) 0.5504(3) 0.6460(3) 0.0151(13) Uani 1 1 d . . . . .
C28 C 0.0012(5) 0.6574(3) 0.8816(3) 0.0204(12) Uani 1 1 d . . . . .
H28 H -0.069541 0.676248 0.905433 0.024 Uiso 1 1 calc R U . . .
C7 C 0.4374(6) 0.4884(4) 0.6945(3) 0.0235(14) Uani 1 1 d . . . . .
H7A H 0.392495 0.447204 0.725447 0.028 Uiso 1 1 calc R U . . .
H7B H 0.397673 0.547061 0.696777 0.028 Uiso 1 1 calc R U . . .
C16 C 0.0842(6) 0.5399(4) 0.5739(3) 0.0228(14) Uani 1 1 d . . . . .
H16 H 0.057866 0.589915 0.547649 0.027 Uiso 1 1 calc R U . . .
C3 C 0.8037(5) 0.4943(4) 0.7551(3) 0.0191(14) Uani 1 1 d . . . . .
H3 H 0.886692 0.492948 0.767099 0.023 Uiso 1 1 calc R U . . .
B1 B 0.4769(7) 0.2326(4) 0.6097(4) 0.0215(16) Uani 1 1 d . . . . .
C1 C 0.8302(5) 0.3656(4) 0.6702(3) 0.0215(13) Uani 1 1 d . . . . .
H1E H 0.900143 0.394946 0.647831 0.026 Uiso 1 1 calc R U . . .
H1F H 0.861408 0.322540 0.705190 0.026 Uiso 1 1 calc R U . . .
C5 C 0.6070(5) 0.5584(4) 0.7669(3) 0.0211(14) Uani 1 1 d . . . . .
H5 H 0.554437 0.601348 0.786759 0.025 Uiso 1 1 calc R U . . .
C6 C 0.5644(5) 0.4963(3) 0.7197(3) 0.0174(12) Uani 1 1 d . . . . .
C18 C 0.1319(5) 0.3852(4) 0.5757(3) 0.0307(17) Uani 1 1 d . . . . .
H18 H 0.143906 0.330882 0.551340 0.037 Uiso 1 1 calc R U . . .
C26 C 0.0093(5) 0.8033(3) 0.6574(3) 0.0195(14) Uani 1 1 d . . . . .
H26 H 0.085391 0.830311 0.665369 0.023 Uiso 1 1 calc R U . . .
C29 C 0.0953(5) 0.6213(3) 0.9194(3) 0.0226(14) Uani 1 1 d . . . . .
H29 H 0.090220 0.614963 0.969283 0.027 Uiso 1 1 calc R U . . .
C36 C 0.4380(5) 0.7688(4) 0.6712(3) 0.0230(13) Uani 1 1 d . . . . .
H36 H 0.497765 0.789937 0.702859 0.028 Uiso 1 1 calc R U . . .
C21 C 0.0015(5) 0.7110(4) 0.6577(3) 0.0156(13) Uani 1 1 d . . . . .
C35 C 0.4558(5) 0.7771(3) 0.5993(3) 0.0210(14) Uani 1 1 d . . . . .
H35 H 0.527482 0.802761 0.581113 0.025 Uiso 1 1 calc R U . . .
C25 C -0.0909(5) 0.8575(4) 0.6456(3) 0.0251(13) Uani 1 1 d . . . . .
H25 H -0.081857 0.920055 0.645176 0.030 Uiso 1 1 calc R U . . .
C17 C 0.0949(5) 0.4593(4) 0.5400(3) 0.0301(16) Uani 1 1 d . . . . .
H17 H 0.076365 0.455234 0.491083 0.036 Uiso 1 1 calc R U . . .
C24 C -0.2021(5) 0.8206(4) 0.6347(3) 0.0257(15) Uani 1 1 d . . . . .
H24 H -0.270690 0.857193 0.627693 0.031 Uiso 1 1 calc R U . . .
C8 C 0.4593(5) 0.5264(4) 0.5682(3) 0.0246(15) Uani 1 1 d . . . . .
H8A H 0.460477 0.584432 0.592524 0.030 Uiso 1 1 calc R U . . .
H8B H 0.393203 0.527532 0.533124 0.030 Uiso 1 1 calc R U . . .
C37 C 0.3349(5) 0.7304(3) 0.6977(3) 0.0193(13) Uani 1 1 d . . . . .
H37 H 0.326150 0.726213 0.747504 0.023 Uiso 1 1 calc R U . . .
C34 C 0.3661(5) 0.7469(3) 0.5545(3) 0.0186(13) Uani 1 1 d . . . . .
H34 H 0.375725 0.751893 0.504762 0.022 Uiso 1 1 calc R U . . .
C12 C 0.7938(5) 0.4776(4) 0.4666(3) 0.0224(14) Uani 1 1 d . . . . .
H12 H 0.868826 0.464495 0.444907 0.027 Uiso 1 1 calc R U . . .
C10 C 0.6241(6) 0.5733(4) 0.4819(3) 0.0238(15) Uani 1 1 d . . . . .
H10 H 0.582997 0.626925 0.471592 0.029 Uiso 1 1 calc R U . . .
C23 C -0.2130(5) 0.7291(4) 0.6340(3) 0.0269(15) Uani 1 1 d . . . . .
H23 H -0.289361 0.702528 0.626304 0.032 Uiso 1 1 calc R U . . .
C19 C 0.1514(5) 0.3908(4) 0.6477(3) 0.0271(15) Uani 1 1 d . . . . .
H19 H 0.171876 0.339312 0.673846 0.033 Uiso 1 1 calc R U . . .
C11 C 0.7313(6) 0.5533(4) 0.4493(3) 0.0254(15) Uani 1 1 d . . . . .
H11 H 0.762742 0.592285 0.414510 0.030 Uiso 1 1 calc R U . . .
C22 C -0.1130(5) 0.6769(4) 0.6446(3) 0.0221(14) Uani 1 1 d . . . . .
H22 H -0.122512 0.614376 0.642895 0.026 Uiso 1 1 calc R U . . .
B2 B 0.1164(5) 0.6508(4) 0.6825(3) 0.0155(13) Uani 1 1 d . . . . .
H1A H 0.381(4) 0.232(3) 0.609(3) 0.016(13) Uiso 1 1 d . . . . .
H1B H 0.518(4) 0.171(3) 0.606(3) 0.020(14) Uiso 1 1 d . . . . .
H1C H 0.505(5) 0.285(3) 0.559(3) 0.023(15) Uiso 1 1 d . . . . .
H1D H 0.506(4) 0.275(3) 0.662(3) 0.020(14) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.970(4) . ?
Ni1 N3 1.983(4) . ?
Ni1 N2 2.150(4) . ?
Ni1 N4 2.155(4) . ?
Ni1 B1 2.176(7) . ?
N2 C14 1.479(6) . ?
N2 C1 1.490(6) . ?
N3 C2 1.321(7) . ?
N3 C6 1.351(6) . ?
N4 C7 1.478(6) . ?
N4 C8 1.491(7) . ?
N1 C9 1.336(7) . ?
N1 C13 1.343(7) . ?
C32 C37 1.402(7) . ?
C32 C33 1.409(6) . ?
C32 B2 1.650(8) . ?
C2 C3 1.377(7) . ?
C2 C1 1.508(7) . ?
C4 C5 1.369(8) . ?
C4 C3 1.395(8) . ?
C38 C31 1.399(7) . ?
C38 C27 1.401(7) . ?
C38 B2 1.661(7) . ?
C20 C15 1.396(7) . ?
C20 C19 1.398(7) . ?
C9 C10 1.390(7) . ?
C9 C8 1.506(8) . ?
C33 C34 1.387(7) . ?
C31 C30 1.391(7) . ?
C27 C28 1.384(7) . ?
C30 C29 1.372(7) . ?
C13 C12 1.373(7) . ?
C13 C14 1.511(7) . ?
C15 C16 1.407(7) . ?
C15 B2 1.665(8) . ?
C28 C29 1.380(7) . ?
C7 C6 1.494(8) . ?
C16 C17 1.381(7) . ?
C5 C6 1.379(7) . ?
C18 C17 1.370(8) . ?
C18 C19 1.383(7) . ?
C26 C21 1.397(7) . ?
C26 C25 1.400(7) . ?
C36 C37 1.378(8) . ?
C36 C35 1.380(7) . ?
C21 C22 1.394(7) . ?
C21 B2 1.635(8) . ?
C35 C34 1.387(7) . ?
C25 C24 1.371(7) . ?
C24 C23 1.386(8) . ?
C12 C11 1.377(8) . ?
C10 C11 1.375(8) . ?
C23 C22 1.377(7) . ?

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
N1 Ni1 N3 90.21(16) . . ?
N1 Ni1 N2 79.97(18) . . ?
N3 Ni1 N2 80.50(17) . . ?
N1 Ni1 N4 80.83(18) . . ?
N3 Ni1 N4 80.29(17) . . ?
N2 Ni1 N4 152.66(16) . . ?
N1 Ni1 B1 132.2(2) . . ?
N3 Ni1 B1 137.6(2) . . ?
N2 Ni1 B1 103.8(2) . . ?
N4 Ni1 B1 103.5(2) . . ?
C14 N2 C1 113.4(4) . . ?
C14 N2 Ni1 104.7(3) . . ?
C1 N2 Ni1 110.0(3) . . ?
C2 N3 C6 121.7(5) . . ?
C2 N3 Ni1 120.4(4) . . ?
C6 N3 Ni1 117.0(4) . . ?
C7 N4 C8 112.6(4) . . ?
C7 N4 Ni1 104.4(3) . . ?
C8 N4 Ni1 110.1(3) . . ?
C9 N1 C13 121.5(5) . . ?
C9 N1 Ni1 120.0(4) . . ?
C13 N1 Ni1 118.3(4) . . ?
C37 C32 C33 113.9(5) . . ?
C37 C32 B2 126.2(5) . . ?
C33 C32 B2 119.9(5) . . ?
N3 C2 C3 121.0(5) . . ?
N3 C2 C1 115.8(5) . . ?
C3 C2 C1 123.2(5) . . ?
C5 C4 C3 120.6(5) . . ?
C31 C38 C27 114.0(5) . . ?
C31 C38 B2 123.8(5) . . ?
C27 C38 B2 122.2(4) . . ?
C15 C20 C19 122.6(5) . . ?
N1 C9 C10 119.9(6) . . ?
N1 C9 C8 116.4(5) . . ?
C10 C9 C8 123.7(5) . . ?
C34 C33 C32 123.5(5) . . ?
C30 C31 C38 123.2(5) . . ?
C28 C27 C38 123.4(5) . . ?
C29 C30 C31 120.5(5) . . ?
N1 C13 C12 120.8(5) . . ?
N1 C13 C14 113.5(5) . . ?
C12 C13 C14 125.7(5) . . ?
N2 C14 C13 110.7(4) . . ?
C20 C15 C16 115.2(5) . . ?
C20 C15 B2 123.8(5) . . ?
C16 C15 B2 120.8(5) . . ?
C29 C28 C27 120.3(5) . . ?
N4 C7 C6 110.2(5) . . ?
C17 C16 C15 122.2(6) . . ?
C2 C3 C4 117.9(5) . . ?
N2 C1 C2 112.9(4) . . ?
C4 C5 C6 118.8(5) . . ?
N3 C6 C5 120.0(5) . . ?
N3 C6 C7 114.2(5) . . ?
C5 C6 C7 125.8(5) . . ?
C17 C18 C19 118.9(6) . . ?
C21 C26 C25 122.3(5) . . ?
C30 C29 C28 118.5(5) . . ?
C37 C36 C35 121.1(5) . . ?
C22 C21 C26 115.1(5) . . ?
C22 C21 B2 123.9(5) . . ?
C26 C21 B2 120.5(5) . . ?
C36 C35 C34 118.1(5) . . ?
C24 C25 C26 120.3(5) . . ?
C18 C17 C16 121.1(6) . . ?
C25 C24 C23 119.0(5) . . ?
N4 C8 C9 112.5(4) . . ?
C36 C37 C32 123.3(5) . . ?
C33 C34 C35 120.2(5) . . ?
C13 C12 C11 118.3(6) . . ?
C11 C10 C9 118.5(6) . . ?
C22 C23 C24 119.9(5) . . ?
C18 C19 C20 119.8(6) . . ?
C10 C11 C12 120.8(6) . . ?
C23 C22 C21 123.4(5) . . ?
C21 B2 C32 109.5(4) . . ?
C21 B2 C38 107.7(4) . . ?
C32 B2 C38 112.7(4) . . ?
C21 B2 C15 111.1(4) . . ?
C32 B2 C15 106.6(4) . . ?
C38 B2 C15 109.2(4) . . ?

_refine_diff_density_max         0.651
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.073

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[(LH)Ni(mu-OMe)2Ni(LH)](BPh4)2
_database_code_depnum_ccdc_archive 'CCDC 1878196'
loop_
_audit_author_name
_audit_author_address
'Sakthi Raje'
;Indian Institute of Technology Kanpur
India
;
_audit_update_record             
;
2018-11-09 deposited with the CCDC.	2019-04-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C30 H38 N8 Ni2 O2, 2(C24 H20 B), 4(C2 H3 N), 2(C H O)
;
_chemical_formula_sum            'C88 H92 B2 N12 Ni2 O4'
_chemical_formula_weight         1520.77

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'
B B 0.0013 0.0007 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   16.7786(13)
_cell_length_b                   11.9023(9)
_cell_length_c                   21.2510(19)
_cell_angle_alpha                90
_cell_angle_beta                 105.676(2)
_cell_angle_gamma                90
_cell_volume                     4086.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9570
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      28.02

_exptl_crystal_description       prismatic
_exptl_crystal_colour            green-brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_F_000             1604
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    0.518
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5573
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32612
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.198
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_full        25.249
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7398
_reflns_number_gt                5516
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0667P)²+5.0385P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7398
_refine_ls_number_parameters     490
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1483
_refine_ls_wR_factor_gt          0.1350
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Ni Ni 0.97864(2) 0.48619(3) 0.56691(2) 0.01989(14) Uani 1 1 d . . . . .
O1 O 0.92225(14) 0.4956(2) 0.47007(11) 0.0275(6) Uani 1 1 d . . . . .
N1 N 1.03879(16) 0.4906(2) 0.66376(12) 0.0187(6) Uani 1 1 d . . . . .
N2 N 0.99207(17) 0.3040(2) 0.59003(14) 0.0247(6) Uani 1 1 d . . . . .
H2B H 1.0110 0.2640 0.5552 0.030 Uiso 1 1 calc R U . . .
N3 N 0.87630(16) 0.4565(2) 0.59832(12) 0.0185(6) Uani 1 1 d . . . . .
N4 N 0.94826(16) 0.6578(2) 0.59255(13) 0.0217(6) Uani 1 1 d . . . . .
H4B H 0.9520 0.7113 0.5572 0.026 Uiso 1 1 calc R U . . .
C1 C 1.03754(19) 0.5867(3) 0.69667(15) 0.0197(7) Uani 1 1 d . . . . .
C2 C 1.0606(2) 0.5900(3) 0.76397(16) 0.0259(8) Uani 1 1 d . . . . .
H2A H 1.0590 0.6584 0.7866 0.031 Uiso 1 1 calc R U . . .
C3 C 1.0861(2) 0.4912(3) 0.79779(17) 0.0310(8) Uani 1 1 d . . . . .
H3A H 1.1042 0.4915 0.8442 0.037 Uiso 1 1 calc R U . . .
C4 C 1.0849(2) 0.3921(3) 0.76366(17) 0.0288(8) Uani 1 1 d . . . . .
H4A H 1.1009 0.3234 0.7864 0.035 Uiso 1 1 calc R U . . .
C5 C 1.0604(2) 0.3940(3) 0.69643(16) 0.0230(7) Uani 1 1 d . . . . .
C6 C 1.0555(2) 0.2914(3) 0.65381(16) 0.0282(8) Uani 1 1 d . . . . .
H6A H 1.1102 0.2782 0.6459 0.034 Uiso 1 1 calc R U . . .
H6B H 1.0418 0.2251 0.6770 0.034 Uiso 1 1 calc R U . . .
C7 C 0.9096(2) 0.2614(3) 0.59121(17) 0.0281(8) Uani 1 1 d . . . . .
H7A H 0.9165 0.1968 0.6215 0.034 Uiso 1 1 calc R U . . .
H7B H 0.8796 0.2348 0.5470 0.034 Uiso 1 1 calc R U . . .
C8 C 0.85925(19) 0.3510(3) 0.61262(15) 0.0207(7) Uani 1 1 d . . . . .
C9 C 0.7987(2) 0.3289(3) 0.64408(16) 0.0281(8) Uani 1 1 d . . . . .
H9A H 0.7864 0.2540 0.6536 0.034 Uiso 1 1 calc R U . . .
C10 C 0.7566(2) 0.4183(3) 0.66137(18) 0.0351(9) Uani 1 1 d . . . . .
H10A H 0.7140 0.4048 0.6821 0.042 Uiso 1 1 calc R U . . .
C11 C 0.7759(2) 0.5261(3) 0.64875(17) 0.0300(8) Uani 1 1 d . . . . .
H11A H 0.7481 0.5879 0.6615 0.036 Uiso 1 1 calc R U . . .
C12 C 0.8370(2) 0.5434(3) 0.61694(15) 0.0217(7) Uani 1 1 d . . . . .
C13 C 0.8628(2) 0.6580(3) 0.59986(17) 0.0275(8) Uani 1 1 d . . . . .
H13A H 0.8240 0.6834 0.5585 0.033 Uiso 1 1 calc R U . . .
H13B H 0.8594 0.7118 0.6346 0.033 Uiso 1 1 calc R U . . .
C14 C 1.0100(2) 0.6883(3) 0.65413(15) 0.0231(7) Uani 1 1 d . . . . .
H14A H 0.9855 0.7440 0.6781 0.028 Uiso 1 1 calc R U . . .
H14B H 1.0585 0.7234 0.6440 0.028 Uiso 1 1 calc R U . . .
C16 C 0.8581(2) 0.4207(4) 0.44173(18) 0.0380(10) Uani 1 1 d . . . . .
H16A H 0.8377 0.4363 0.3948 0.057 Uiso 1 1 calc R U . . .
H16B H 0.8790 0.3434 0.4481 0.057 Uiso 1 1 calc R U . . .
H16C H 0.8129 0.4299 0.4624 0.057 Uiso 1 1 calc R U . . .
B1 B 0.5303(2) 0.4762(3) 0.71451(18) 0.0219(8) Uani 1 1 d . . . . .
C111 C 0.5899(2) 0.4834(3) 0.79022(15) 0.0213(7) Uani 1 1 d . . . . .
C112 C 0.5622(2) 0.4618(3) 0.84591(15) 0.0225(7) Uani 1 1 d . . . . .
H11B H 0.5048 0.4497 0.8404 0.027 Uiso 1 1 calc R U . . .
C113 C 0.6154(2) 0.4576(3) 0.90871(16) 0.0262(8) Uani 1 1 d . . . . .
H11C H 0.5937 0.4414 0.9446 0.031 Uiso 1 1 calc R U . . .
C114 C 0.6985(2) 0.4763(3) 0.91944(16) 0.0281(8) Uani 1 1 d . . . . .
H11D H 0.7346 0.4730 0.9624 0.034 Uiso 1 1 calc R U . . .
C115 C 0.7289(2) 0.5004(3) 0.86593(17) 0.0312(8) Uani 1 1 d . . . . .
H11E H 0.7862 0.5146 0.8722 0.037 Uiso 1 1 calc R U . . .
C116 C 0.6755(2) 0.5036(3) 0.80382(17) 0.0286(8) Uani 1 1 d . . . . .
H11F H 0.6978 0.5204 0.7683 0.034 Uiso 1 1 calc R U . . .
C21 C 0.5382(2) 0.3501(3) 0.68486(15) 0.0216(7) Uani 1 1 d . . . . .
C22 C 0.6016(2) 0.2736(3) 0.71282(16) 0.0244(8) Uani 1 1 d . . . . .
H22A H 0.6412 0.2933 0.7524 0.029 Uiso 1 1 calc R U . . .
C23 C 0.6083(2) 0.1697(3) 0.68437(18) 0.0311(8) Uani 1 1 d . . . . .
H23A H 0.6518 0.1198 0.7049 0.037 Uiso 1 1 calc R U . . .
C24 C 0.5522(2) 0.1388(3) 0.62663(18) 0.0334(9) Uani 1 1 d . . . . .
H24A H 0.5574 0.0685 0.6069 0.040 Uiso 1 1 calc R U . . .
C25 C 0.4884(2) 0.2114(3) 0.59771(17) 0.0333(9) Uani 1 1 d . . . . .
H25A H 0.4492 0.1910 0.5580 0.040 Uiso 1 1 calc R U . . .
C26 C 0.4818(2) 0.3139(3) 0.62684(16) 0.0273(8) Uani 1 1 d . . . . .
H26A H 0.4370 0.3620 0.6066 0.033 Uiso 1 1 calc R U . . .
C31 C 0.4332(2) 0.4967(3) 0.71356(15) 0.0226(7) Uani 1 1 d . . . . .
C32 C 0.3873(2) 0.4150(3) 0.73561(16) 0.0274(8) Uani 1 1 d . . . . .
H32A H 0.4119 0.3433 0.7469 0.033 Uiso 1 1 calc R U . . .
C33 C 0.3082(2) 0.4322(3) 0.74204(17) 0.0344(9) Uani 1 1 d . . . . .
H33A H 0.2805 0.3736 0.7580 0.041 Uiso 1 1 calc R U . . .
C34 C 0.2700(2) 0.5341(3) 0.72521(19) 0.0373(10) Uani 1 1 d . . . . .
H34A H 0.2164 0.5479 0.7305 0.045 Uiso 1 1 calc R U . . .
C35 C 0.3113(2) 0.6163(3) 0.7004(2) 0.0397(10) Uani 1 1 d . . . . .
H35A H 0.2853 0.6866 0.6874 0.048 Uiso 1 1 calc R U . . .
C36 C 0.3910(2) 0.5968(3) 0.69421(18) 0.0317(9) Uani 1 1 d . . . . .
H36A H 0.4173 0.6542 0.6761 0.038 Uiso 1 1 calc R U . . .
C41 C 0.56061(19) 0.5729(3) 0.66949(15) 0.0218(7) Uani 1 1 d . . . . .
C42 C 0.5646(2) 0.5563(3) 0.60553(16) 0.0269(8) Uani 1 1 d . . . . .
H42A H 0.5502 0.4848 0.5860 0.032 Uiso 1 1 calc R U . . .
C43 C 0.5887(2) 0.6404(3) 0.56927(18) 0.0387(10) Uani 1 1 d . . . . .
H43A H 0.5905 0.6254 0.5258 0.046 Uiso 1 1 calc R U . . .
C44 C 0.6099(3) 0.7445(4) 0.59554(19) 0.0429(10) Uani 1 1 d . . . . .
H44A H 0.6270 0.8017 0.5708 0.052 Uiso 1 1 calc R U . . .
C45 C 0.6060(2) 0.7652(3) 0.65860(19) 0.0403(10) Uani 1 1 d . . . . .
H45A H 0.6199 0.8374 0.6774 0.048 Uiso 1 1 calc R U . . .
C46 C 0.5818(2) 0.6806(3) 0.69445(18) 0.0323(9) Uani 1 1 d . . . . .
H46A H 0.5796 0.6966 0.7377 0.039 Uiso 1 1 calc R U . . .
O1S O 0.84643(15) 0.6990(2) 0.45229(13) 0.0399(7) Uani 1 1 d . . . . .
H1S H 0.8670 0.6351 0.4629 0.060 Uiso 1 1 calc R U . . .
C1S C 0.7577(3) 0.6888(5) 0.4256(2) 0.0605(14) Uani 1 1 d . . . . .
N1S N 0.7065(3) 0.1617(4) 0.4361(2) 0.0827(15) Uani 1 1 d . . . . .
C11S C 0.6740(3) 0.2289(5) 0.4579(2) 0.0577(13) Uani 1 1 d . . . . .
C12S C 0.6339(3) 0.3158(5) 0.4869(3) 0.0745(16) Uani 1 1 d . . . . .
H12A H 0.6162 0.2839 0.5235 0.112 Uiso 1 1 calc R U . . .
H12B H 0.5854 0.3445 0.4539 0.112 Uiso 1 1 calc R U . . .
H12C H 0.6729 0.3774 0.5028 0.112 Uiso 1 1 calc R U . . .
N2S N 0.9577(2) 0.1427(3) 0.46597(17) 0.0411(8) Uani 1 1 d . . . . .
C21S C 0.9141(3) 0.0710(3) 0.44196(18) 0.0355(9) Uani 1 1 d . . . . .
C22S C 0.8587(3) -0.0192(3) 0.41124(19) 0.0456(11) Uani 1 1 d . . . . .
H22B H 0.8016 0.0011 0.4097 0.068 Uiso 1 1 calc R U . . .
H22C H 0.8740 -0.0884 0.4366 0.068 Uiso 1 1 calc R U . . .
H22D H 0.8632 -0.0310 0.3667 0.068 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O1 2.023(2) . ?
Ni N1 2.033(3) . ?
Ni O1 2.034(2) 3_766 ?
Ni N3 2.034(3) . ?
Ni N4 2.209(3) . ?
Ni N2 2.222(3) . ?
O1 C16 1.401(4) . ?
O1 Ni 2.034(2) 3_766 ?
N1 C5 1.342(4) . ?
N1 C1 1.344(4) . ?
N2 C7 1.481(4) . ?
N2 C6 1.487(4) . ?
N2 H2B 1.0000 . ?
N3 C8 1.341(4) . ?
N3 C12 1.342(4) . ?
N4 C14 1.478(4) . ?
N4 C13 1.484(4) . ?
N4 H4B 1.0000 . ?
C1 C2 1.377(4) . ?
C1 C14 1.507(4) . ?
C2 C3 1.384(5) . ?
C2 H2A 0.9500 . ?
C3 C4 1.383(5) . ?
C3 H3A 0.9500 . ?
C4 C5 1.376(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.508(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.505(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.384(4) . ?
C9 C10 1.380(5) . ?
C9 H9A 0.9500 . ?
C10 C11 1.368(5) . ?
C10 H10A 0.9500 . ?
C11 C12 1.387(5) . ?
C11 H11A 0.9500 . ?
C12 C13 1.504(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
B1 C31 1.642(5) . ?
B1 C21 1.647(5) . ?
B1 C111 1.651(5) . ?
B1 C41 1.662(5) . ?
C111 C112 1.406(4) . ?
C111 C116 1.408(5) . ?
C112 C113 1.392(5) . ?
C112 H11B 0.9500 . ?
C113 C114 1.368(5) . ?
C113 H11C 0.9500 . ?
C114 C115 1.396(5) . ?
C114 H11D 0.9500 . ?
C115 C116 1.381(5) . ?
C115 H11E 0.9500 . ?
C116 H11F 0.9500 . ?
C21 C26 1.404(5) . ?
C21 C22 1.404(5) . ?
C22 C23 1.395(5) . ?
C22 H22A 0.9500 . ?
C23 C24 1.379(5) . ?
C23 H23A 0.9500 . ?
C24 C25 1.384(5) . ?
C24 H24A 0.9500 . ?
C25 C26 1.387(5) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C31 C36 1.390(5) . ?
C31 C32 1.397(5) . ?
C32 C33 1.386(5) . ?
C32 H32A 0.9500 . ?
C33 C34 1.374(6) . ?
C33 H33A 0.9500 . ?
C34 C35 1.383(6) . ?
C34 H34A 0.9500 . ?
C35 C36 1.398(5) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C41 C42 1.392(5) . ?
C41 C46 1.396(5) . ?
C42 C43 1.389(5) . ?
C42 H42A 0.9500 . ?
C43 C44 1.366(6) . ?
C43 H43A 0.9500 . ?
C44 C45 1.381(6) . ?
C44 H44A 0.9500 . ?
C45 C46 1.388(5) . ?
C45 H45A 0.9500 . ?
C46 H46A 0.9500 . ?
O1S C1S 1.447(5) . ?
O1S H1S 0.8400 . ?
N1S C11S 1.135(6) . ?
C11S C12S 1.459(7) . ?
C12S H12A 0.9800 . ?
C12S H12B 0.9800 . ?
C12S H12C 0.9800 . ?
N2S C21S 1.150(5) . ?
C21S C22S 1.454(6) . ?
C22S H22B 0.9800 . ?
C22S H22C 0.9800 . ?
C22S H22D 0.9800 . ?

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
O1 Ni N1 175.05(10) . . ?
O1 Ni O1 78.90(10) . 3_766 ?
N1 Ni O1 98.88(10) . 3_766 ?
O1 Ni N3 98.00(10) . . ?
N1 Ni N3 84.52(10) . . ?
O1 Ni N3 174.96(10) 3_766 . ?
O1 Ni N4 97.14(10) . . ?
N1 Ni N4 79.12(10) . . ?
O1 Ni N4 105.30(10) 3_766 . ?
N3 Ni N4 78.94(10) . . ?
O1 Ni N2 105.69(10) . . ?
N1 Ni N2 78.94(10) . . ?
O1 Ni N2 98.33(10) 3_766 . ?
N3 Ni N2 78.59(10) . . ?
N4 Ni N2 149.83(10) . . ?
C16 O1 Ni 119.7(2) . . ?
C16 O1 Ni 121.0(2) . 3_766 ?
Ni O1 Ni 101.10(10) . 3_766 ?
C5 N1 C1 120.0(3) . . ?
C5 N1 Ni 119.5(2) . . ?
C1 N1 Ni 118.4(2) . . ?
C7 N2 C6 113.1(3) . . ?
C7 N2 Ni 107.4(2) . . ?
C6 N2 Ni 107.72(19) . . ?
C7 N2 H2B 109.5 . . ?
C6 N2 H2B 109.5 . . ?
Ni N2 H2B 109.5 . . ?
C8 N3 C12 120.2(3) . . ?
C8 N3 Ni 119.2(2) . . ?
C12 N3 Ni 119.2(2) . . ?
C14 N4 C13 111.9(3) . . ?
C14 N4 Ni 107.02(19) . . ?
C13 N4 Ni 108.72(19) . . ?
C14 N4 H4B 109.7 . . ?
C13 N4 H4B 109.7 . . ?
Ni N4 H4B 109.7 . . ?
N1 C1 C2 121.7(3) . . ?
N1 C1 C14 114.6(3) . . ?
C2 C1 C14 123.7(3) . . ?
C1 C2 C3 118.4(3) . . ?
C1 C2 H2A 120.8 . . ?
C3 C2 H2A 120.8 . . ?
C4 C3 C2 119.6(3) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4A 120.4 . . ?
C3 C4 H4A 120.4 . . ?
N1 C5 C4 121.0(3) . . ?
N1 C5 C6 114.8(3) . . ?
C4 C5 C6 124.2(3) . . ?
N2 C6 C5 112.1(3) . . ?
N2 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
N2 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
N2 C7 C8 111.5(3) . . ?
N2 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
N2 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
N3 C8 C9 121.1(3) . . ?
N3 C8 C7 115.1(3) . . ?
C9 C8 C7 123.8(3) . . ?
C10 C9 C8 118.6(3) . . ?
C10 C9 H9A 120.7 . . ?
C8 C9 H9A 120.7 . . ?
C11 C10 C9 120.3(3) . . ?
C11 C10 H10A 119.8 . . ?
C9 C10 H10A 119.8 . . ?
C10 C11 C12 118.7(3) . . ?
C10 C11 H11A 120.7 . . ?
C12 C11 H11A 120.7 . . ?
N3 C12 C11 121.1(3) . . ?
N3 C12 C13 115.6(3) . . ?
C11 C12 C13 123.4(3) . . ?
N4 C13 C12 111.9(3) . . ?
N4 C13 H13A 109.2 . . ?
C12 C13 H13A 109.2 . . ?
N4 C13 H13B 109.2 . . ?
C12 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
N4 C14 C1 111.2(3) . . ?
N4 C14 H14A 109.4 . . ?
C1 C14 H14A 109.4 . . ?
N4 C14 H14B 109.4 . . ?
C1 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
O1 C16 H16A 109.5 . . ?
O1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C31 B1 C21 108.2(3) . . ?
C31 B1 C111 110.0(3) . . ?
C21 B1 C111 109.3(3) . . ?
C31 B1 C41 110.3(3) . . ?
C21 B1 C41 110.0(3) . . ?
C111 B1 C41 109.1(3) . . ?
C112 C111 C116 114.1(3) . . ?
C112 C111 B1 124.1(3) . . ?
C116 C111 B1 121.6(3) . . ?
C113 C112 C111 122.8(3) . . ?
C113 C112 H11B 118.6 . . ?
C111 C112 H11B 118.6 . . ?
C114 C113 C112 120.9(3) . . ?
C114 C113 H11C 119.5 . . ?
C112 C113 H11C 119.5 . . ?
C113 C114 C115 118.5(3) . . ?
C113 C114 H11D 120.7 . . ?
C115 C114 H11D 120.7 . . ?
C116 C115 C114 119.9(3) . . ?
C116 C115 H11E 120.0 . . ?
C114 C115 H11E 120.0 . . ?
C115 C116 C111 123.6(3) . . ?
C115 C116 H11F 118.2 . . ?
C111 C116 H11F 118.2 . . ?
C26 C21 C22 115.2(3) . . ?
C26 C21 B1 120.7(3) . . ?
C22 C21 B1 124.0(3) . . ?
C23 C22 C21 122.2(3) . . ?
C23 C22 H22A 118.9 . . ?
C21 C22 H22A 118.9 . . ?
C24 C23 C22 120.5(3) . . ?
C24 C23 H23A 119.8 . . ?
C22 C23 H23A 119.8 . . ?
C23 C24 C25 119.3(3) . . ?
C23 C24 H24A 120.4 . . ?
C25 C24 H24A 120.4 . . ?
C24 C25 C26 119.8(3) . . ?
C24 C25 H25A 120.1 . . ?
C26 C25 H25A 120.1 . . ?
C25 C26 C21 123.1(3) . . ?
C25 C26 H26A 118.5 . . ?
C21 C26 H26A 118.5 . . ?
C36 C31 C32 114.4(3) . . ?
C36 C31 B1 123.7(3) . . ?
C32 C31 B1 121.8(3) . . ?
C33 C32 C31 124.0(3) . . ?
C33 C32 H32A 118.0 . . ?
C31 C32 H32A 118.0 . . ?
C34 C33 C32 119.8(4) . . ?
C34 C33 H33A 120.1 . . ?
C32 C33 H33A 120.1 . . ?
C33 C34 C35 118.5(4) . . ?
C33 C34 H34A 120.8 . . ?
C35 C34 H34A 120.8 . . ?
C34 C35 C36 120.7(4) . . ?
C34 C35 H35A 119.7 . . ?
C36 C35 H35A 119.7 . . ?
C31 C36 C35 122.5(4) . . ?
C31 C36 H36A 118.7 . . ?
C35 C36 H36A 118.7 . . ?
C42 C41 C46 115.2(3) . . ?
C42 C41 B1 124.5(3) . . ?
C46 C41 B1 120.2(3) . . ?
C43 C42 C41 122.5(4) . . ?
C43 C42 H42A 118.7 . . ?
C41 C42 H42A 118.7 . . ?
C44 C43 C42 120.6(4) . . ?
C44 C43 H43A 119.7 . . ?
C42 C43 H43A 119.7 . . ?
C43 C44 C45 118.9(4) . . ?
C43 C44 H44A 120.5 . . ?
C45 C44 H44A 120.5 . . ?
C44 C45 C46 120.0(4) . . ?
C44 C45 H45A 120.0 . . ?
C46 C45 H45A 120.0 . . ?
C45 C46 C41 122.7(3) . . ?
C45 C46 H46A 118.7 . . ?
C41 C46 H46A 118.7 . . ?
C1S O1S H1S 109.5 . . ?
N1S C11S C12S 178.8(6) . . ?
C11S C12S H12A 109.5 . . ?
C11S C12S H12B 109.5 . . ?
H12A C12S H12B 109.5 . . ?
C11S C12S H12C 109.5 . . ?
H12A C12S H12C 109.5 . . ?
H12B C12S H12C 109.5 . . ?
N2S C21S C22S 179.6(5) . . ?
C21S C22S H22B 109.5 . . ?
C21S C22S H22C 109.5 . . ?
H22B C22S H22C 109.5 . . ?
C21S C22S H22D 109.5 . . ?
H22B C22S H22D 109.5 . . ?
H22C C22S H22D 109.5 . . ?

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
C5 N1 C1 C2 2.1(5) . . . . ?
Ni N1 C1 C2 165.6(2) . . . . ?
C5 N1 C1 C14 -178.4(3) . . . . ?
Ni N1 C1 C14 -14.9(4) . . . . ?
N1 C1 C2 C3 0.5(5) . . . . ?
C14 C1 C2 C3 -179.0(3) . . . . ?
C1 C2 C3 C4 -2.3(5) . . . . ?
C2 C3 C4 C5 1.7(5) . . . . ?
C1 N1 C5 C4 -2.8(5) . . . . ?
Ni N1 C5 C4 -166.1(2) . . . . ?
C1 N1 C5 C6 177.3(3) . . . . ?
Ni N1 C5 C6 14.0(4) . . . . ?
C3 C4 C5 N1 0.9(5) . . . . ?
C3 C4 C5 C6 -179.2(3) . . . . ?
C7 N2 C6 C5 -91.3(3) . . . . ?
Ni N2 C6 C5 27.2(3) . . . . ?
N1 C5 C6 N2 -28.1(4) . . . . ?
C4 C5 C6 N2 151.9(3) . . . . ?
C6 N2 C7 C8 88.2(3) . . . . ?
Ni N2 C7 C8 -30.4(3) . . . . ?
C12 N3 C8 C9 2.9(5) . . . . ?
Ni N3 C8 C9 169.3(2) . . . . ?
C12 N3 C8 C7 -177.9(3) . . . . ?
Ni N3 C8 C7 -11.5(4) . . . . ?
N2 C7 C8 N3 29.0(4) . . . . ?
N2 C7 C8 C9 -151.7(3) . . . . ?
N3 C8 C9 C10 -0.8(5) . . . . ?
C7 C8 C9 C10 180.0(3) . . . . ?
C8 C9 C10 C11 -1.4(5) . . . . ?
C9 C10 C11 C12 1.6(5) . . . . ?
C8 N3 C12 C11 -2.7(5) . . . . ?
Ni N3 C12 C11 -169.1(2) . . . . ?
C8 N3 C12 C13 178.4(3) . . . . ?
Ni N3 C12 C13 12.0(4) . . . . ?
C10 C11 C12 N3 0.5(5) . . . . ?
C10 C11 C12 C13 179.3(3) . . . . ?
C14 N4 C13 C12 -93.2(3) . . . . ?
Ni N4 C13 C12 24.8(3) . . . . ?
N3 C12 C13 N4 -25.1(4) . . . . ?
C11 C12 C13 N4 156.0(3) . . . . ?
C13 N4 C14 C1 86.8(3) . . . . ?
Ni N4 C14 C1 -32.2(3) . . . . ?
N1 C1 C14 N4 32.4(4) . . . . ?
C2 C1 C14 N4 -148.1(3) . . . . ?
C31 B1 C111 C112 25.0(4) . . . . ?
C21 B1 C111 C112 -93.7(4) . . . . ?
C41 B1 C111 C112 146.0(3) . . . . ?
C31 B1 C111 C116 -160.1(3) . . . . ?
C21 B1 C111 C116 81.3(4) . . . . ?
C41 B1 C111 C116 -39.0(4) . . . . ?
C116 C111 C112 C113 -1.9(5) . . . . ?
B1 C111 C112 C113 173.4(3) . . . . ?
C111 C112 C113 C114 1.1(5) . . . . ?
C112 C113 C114 C115 0.3(5) . . . . ?
C113 C114 C115 C116 -0.7(5) . . . . ?
C114 C115 C116 C111 -0.1(5) . . . . ?
C112 C111 C116 C115 1.4(5) . . . . ?
B1 C111 C116 C115 -174.0(3) . . . . ?
C31 B1 C21 C26 47.1(4) . . . . ?
C111 B1 C21 C26 166.8(3) . . . . ?
C41 B1 C21 C26 -73.5(4) . . . . ?
C31 B1 C21 C22 -135.5(3) . . . . ?
C111 B1 C21 C22 -15.8(4) . . . . ?
C41 B1 C21 C22 103.9(3) . . . . ?
C26 C21 C22 C23 0.7(5) . . . . ?
B1 C21 C22 C23 -176.8(3) . . . . ?
C21 C22 C23 C24 0.5(5) . . . . ?
C22 C23 C24 C25 -1.0(5) . . . . ?
C23 C24 C25 C26 0.3(5) . . . . ?
C24 C25 C26 C21 1.0(5) . . . . ?
C22 C21 C26 C25 -1.5(5) . . . . ?
B1 C21 C26 C25 176.2(3) . . . . ?
C21 B1 C31 C36 -137.4(3) . . . . ?
C111 B1 C31 C36 103.3(4) . . . . ?
C41 B1 C31 C36 -17.0(4) . . . . ?
C21 B1 C31 C32 45.9(4) . . . . ?
C111 B1 C31 C32 -73.5(4) . . . . ?
C41 B1 C31 C32 166.2(3) . . . . ?
C36 C31 C32 C33 -3.8(5) . . . . ?
B1 C31 C32 C33 173.2(3) . . . . ?
C31 C32 C33 C34 1.1(5) . . . . ?
C32 C33 C34 C35 1.8(5) . . . . ?
C33 C34 C35 C36 -1.6(6) . . . . ?
C32 C31 C36 C35 4.0(5) . . . . ?
B1 C31 C36 C35 -173.0(3) . . . . ?
C34 C35 C36 C31 -1.4(6) . . . . ?
C31 B1 C41 C42 -99.0(4) . . . . ?
C21 B1 C41 C42 20.3(4) . . . . ?
C111 B1 C41 C42 140.1(3) . . . . ?
C31 B1 C41 C46 78.9(4) . . . . ?
C21 B1 C41 C46 -161.8(3) . . . . ?
C111 B1 C41 C46 -41.9(4) . . . . ?
C46 C41 C42 C43 0.6(5) . . . . ?
B1 C41 C42 C43 178.7(3) . . . . ?
C41 C42 C43 C44 0.0(6) . . . . ?
C42 C43 C44 C45 -0.7(6) . . . . ?
C43 C44 C45 C46 0.7(6) . . . . ?
C44 C45 C46 C41 0.0(6) . . . . ?
C42 C41 C46 C45 -0.6(5) . . . . ?
B1 C41 C46 C45 -178.7(3) . . . . ?

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
N2 H2B O1S 1.00 2.48 3.077(4) 117.9 3_766
N2 H2B N2S 1.00 2.36 3.185(4) 139.4 .
N4 H4B O1S 1.00 2.45 3.048(4) 118.0 .
N4 H4B N2S 1.00 2.44 3.276(4) 140.7 3_766
C6 H6A O1S 0.99 2.40 3.132(4) 129.9 3_766
C7 H7B N2S 0.99 2.67 3.301(5) 122.1 .
C13 H13A O1S 0.99 2.39 3.112(4) 128.9 .
O1S H1S O1 0.84 1.89 2.714(4) 167.0 .
C22S H22B N1S 0.98 2.65 3.488(7) 144.2 .
C22S H22C O1S 0.98 2.61 3.486(5) 148.9 1_545

_refine_diff_density_max         1.196
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.072

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[(LH)Ni(H2O)2](HSO4)(SO4)
_database_code_depnum_ccdc_archive 'CCDC 1878200'
loop_
_audit_author_name
_audit_author_address
'Ray J. Butcher'
;Howard University
United States of America
;
_audit_update_record             
;
2019-03-21 deposited with the CCDC.	2019-04-18 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_3augc_0m            
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......       O1AA Check 
RESPONSE: H-atoms on the free water molecules could not be placed 
satisfactorily because it is hydrogen-bonded to coordinated water 
and two oxygen atoms from bisulfate ions.
;
_vrf_PLAT430_3augc_0m            
;
PROBLEM: Short Inter D...A Contact  O1AA     ..O4       .       2.80 Ang.  
RESPONSE: It is hydrogen-bonded to coordinated water and two oxygen atoms 
from bisulfate ions.
;
# end Validation Reply Form
_audit_creation_date             2018-11-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H20 N4 Ni O2, H O4 S, O2 S0.5, O'
_chemical_formula_sum            'C14 H21 N4 Ni O9 S1.50'
_chemical_formula_weight         496.15
_chemical_melting_point          ?
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_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'

_cell_length_a                   21.7139(16)
_cell_length_b                   11.0715(8)
_cell_length_c                   16.0808(12)
_cell_angle_alpha                90
_cell_angle_beta                 100.803(2)
_cell_angle_gamma                90
_cell_volume                     3797.4(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5465
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.817
_cell_measurement_theta_min      2.345
_shelx_estimated_absorpt_T_max   0.976
_shelx_estimated_absorpt_T_min   0.940
_exptl_absorpt_coefficient_mu    1.246
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1033 before and 0.0683 after correction. The Ratio of minimum to maximum transmission is 0.8499. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light violet'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22394
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.095
_diffrn_reflns_theta_max         25.095
_diffrn_reflns_theta_min         2.904
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2380
_reflns_number_total             3386
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.719
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3386
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0592
_refine_ls_restrained_S_all      1.086
_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)+(0.0443P)²+42.6219P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1367
_refine_special_details          
;
H-atoms on the free water molecules could not be placed 
satisfactorily because it is hydrogen-bonded to coordinated water 
and two oxygen atoms from bisulfate ions.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O2W-H2WA = O2W-H2WB
 0.87 with sigma of 0.02
 H2WA-H2WB
 1.38 with sigma of 0.04
 Ni1-H2WA \\sim Ni1-H2WB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S1A \\sim O3A \\sim O3A \\sim O1A \\sim O1A \\sim O2A \\sim O2A: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008
4. Others
 Fixed Sof: O3A(0.5) O1A(0.5)
5.a Rotating group:
 O1W(H1WA,H1WB)
5.b Ternary CH refined with riding coordinates:
 N2(H2), N4(H4)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C14(H14A,H14B), C7(H7A,H7B), C8(H8A,H8B)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C12(H12), C4(H4A), C10(H10), C11(H11)
5.e Idealised tetrahedral OH refined as rotating group:
 O2(H2A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.37693(3) 0.73218(6) 0.32716(4) 0.0177(2) Uani 1 1 d D . . . .
S1 S 0.31941(6) 0.31104(13) 0.35262(9) 0.0210(3) Uani 1 1 d . . . . .
S1A S 0.500000 0.4017(2) 0.250000 0.0263(5) Uani 1 2 d S TU P . .
O1 O 0.27922(17) 0.4147(3) 0.3575(2) 0.0219(9) Uani 1 1 d . . . . .
O1W O 0.30256(18) 0.6229(4) 0.2814(2) 0.0263(10) Uani 1 1 d . . . . .
H1WA H 0.263626 0.659819 0.274211 0.039 Uiso 1 1 d GR . . . .
H1WB H 0.296075 0.561879 0.318002 0.039 Uiso 1 1 d GR . . . .
O3 O 0.30431(17) 0.2512(4) 0.2711(2) 0.0271(10) Uani 1 1 d . . . . .
O4 O 0.3169(2) 0.2277(4) 0.4225(3) 0.0366(11) Uani 1 1 d . . . . .
N2 N 0.3347(2) 0.9016(4) 0.2833(3) 0.0175(10) Uani 1 1 d . . . . .
H2 H 0.310283 0.891037 0.235976 0.021 Uiso 1 1 calc R . . . .
O2 O 0.38616(19) 0.3563(5) 0.3642(3) 0.0487(14) Uani 1 1 d . . . . .
H2A H 0.394154 0.377378 0.316468 0.073 Uiso 1 1 calc GR . . . .
N3 N 0.4499(2) 0.8404(4) 0.3635(3) 0.0189(10) Uani 1 1 d . . . . .
N1 N 0.34340(19) 0.7805(4) 0.4298(3) 0.0183(10) Uani 1 1 d . . . . .
N4 N 0.4325(2) 0.6176(4) 0.4216(3) 0.0291(12) Uani 1 1 d . . . . .
H4 H 0.437319 0.549124 0.399718 0.035 Uiso 1 1 calc R . . . .
C1 C 0.3875(2) 0.9800(5) 0.2711(3) 0.0194(12) Uani 1 1 d . . . . .
H1A H 0.377190 1.053577 0.274973 0.023 Uiso 1 1 calc R . . . .
H1B H 0.395149 0.968884 0.221704 0.023 Uiso 1 1 calc R . . . .
C2 C 0.4455(3) 0.9543(5) 0.3352(3) 0.0187(12) Uani 1 1 d . . . . .
C14 C 0.2982(2) 0.9471(5) 0.3455(3) 0.0189(12) Uani 1 1 d . . . . .
H14A H 0.259414 0.940429 0.324579 0.023 Uiso 1 1 calc R . . . .
H14B H 0.306132 1.021777 0.353797 0.023 Uiso 1 1 calc R . . . .
C13 C 0.3113(2) 0.8832(5) 0.4288(3) 0.0185(12) Uani 1 1 d . . . . .
C5 C 0.5471(2) 0.8803(5) 0.4512(3) 0.0226(13) Uani 1 1 d . . . . .
H5 H 0.578574 0.856197 0.486919 0.027 Uiso 1 1 calc R . . . .
C3 C 0.4926(3) 1.0356(5) 0.3623(3) 0.0223(13) Uani 1 1 d . . . . .
H3 H 0.490453 1.107488 0.343454 0.027 Uiso 1 1 calc R . . . .
C6 C 0.4978(2) 0.8034(5) 0.4218(3) 0.0187(12) Uani 1 1 d . . . . .
O3A O 0.4836(4) 0.4336(8) 0.1635(5) 0.0317(16) Uani 0.5 1 d . U . . .
C9 C 0.3592(3) 0.7146(5) 0.5006(4) 0.0253(14) Uani 1 1 d . . . . .
C12 C 0.2921(3) 0.9228(5) 0.5013(3) 0.0231(13) Uani 1 1 d . . . . .
H12 H 0.271598 0.988223 0.501125 0.028 Uiso 1 1 calc R . . . .
C4 C 0.5440(3) 0.9973(6) 0.4212(4) 0.0253(14) Uani 1 1 d . . . . .
H4A H 0.573715 1.046180 0.438997 0.030 Uiso 1 1 calc R . . . .
C10 C 0.3418(3) 0.7498(6) 0.5747(4) 0.0329(16) Uani 1 1 d . . . . .
H10 H 0.352160 0.708476 0.619748 0.039 Uiso 1 1 calc R . . . .
C11 C 0.3068(3) 0.8549(6) 0.5740(4) 0.0318(16) Uani 1 1 d . . . . .
H11 H 0.294431 0.877358 0.618614 0.038 Uiso 1 1 calc R . . . .
C7 C 0.4948(3) 0.6737(5) 0.4504(4) 0.0332(16) Uani 1 1 d . . . . .
H7A H 0.522307 0.632681 0.431485 0.040 Uiso 1 1 calc R . . . .
H7B H 0.503739 0.671197 0.504138 0.040 Uiso 1 1 calc R . . . .
C8 C 0.3955(3) 0.6025(5) 0.4889(4) 0.0340(16) Uani 1 1 d . . . . .
H8A H 0.420011 0.585531 0.535125 0.041 Uiso 1 1 calc R . . . .
H8B H 0.370239 0.543864 0.476397 0.041 Uiso 1 1 calc R . . . .
O1A O 0.5033(4) 0.5066(9) 0.3040(6) 0.0363(17) Uani 0.5 1 d . U . . .
O2A O 0.4470(3) 0.3238(6) 0.2570(4) 0.094(2) Uani 1 1 d . U . . .
O2W O 0.40945(19) 0.6886(4) 0.2168(3) 0.0274(10) Uani 1 1 d D . . . .
H2WA H 0.3780(16) 0.671(5) 0.170(2) 0.041 Uiso 1 1 d DR . . . .
H2WB H 0.432(2) 0.625(4) 0.216(3) 0.041 Uiso 1 1 d DR . . . .
O1AA O 0.3190(3) 0.6702(6) 0.0820(4) 0.0827(19) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1W 2.041(4) . ?
Ni1 N2 2.148(4) . ?
Ni1 N3 1.986(4) . ?
Ni1 N1 1.998(5) . ?
Ni1 N4 2.164(5) . ?
Ni1 O2W 2.086(4) . ?
S1 O1 1.453(4) . ?
S1 O3 1.451(4) . ?
S1 O4 1.463(4) . ?
S1 O2 1.512(4) . ?
S1A O3A 1.414(8) . ?
S1A O3A 1.414(8) 2_655 ?
S1A O1A 1.444(9) . ?
S1A O1A 1.444(9) 2_655 ?
S1A O2A 1.459(6) . ?
S1A O2A 1.459(6) 2_655 ?
N2 C1 1.481(6) . ?
N2 C14 1.475(7) . ?
N3 C2 1.338(7) . ?
N3 C6 1.328(6) . ?
N1 C13 1.332(7) . ?
N1 C9 1.341(7) . ?
N4 C7 1.481(7) . ?
N4 C8 1.474(8) . ?
C1 C2 1.497(7) . ?
C2 C3 1.371(7) . ?
C14 C13 1.494(7) . ?
C13 C12 1.381(8) . ?
C5 C6 1.379(8) . ?
C5 C4 1.378(8) . ?
C3 C4 1.388(8) . ?
C6 C7 1.513(8) . ?
O3A O1A 0.976(10) 2_655 ?
C9 C10 1.373(8) . ?
C9 C8 1.501(9) . ?
C12 C11 1.375(8) . ?
C10 C11 1.388(9) . ?
O1A O3A 0.976(10) 2_655 ?
O1A O1A 1.716(18) 2_655 ?

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
O1W Ni1 N2 97.99(16) . . ?
O1W Ni1 N4 101.83(17) . . ?
O1W Ni1 O2W 85.85(16) . . ?
N2 Ni1 N4 152.85(18) . . ?
N3 Ni1 O1W 176.06(17) . . ?
N3 Ni1 N2 80.68(17) . . ?
N3 Ni1 N1 89.43(17) . . ?
N3 Ni1 N4 80.66(18) . . ?
N3 Ni1 O2W 90.61(17) . . ?
N1 Ni1 O1W 94.02(16) . . ?
N1 Ni1 N2 80.68(17) . . ?
N1 Ni1 N4 79.59(19) . . ?
N1 Ni1 O2W 177.20(17) . . ?
O2W Ni1 N2 96.57(16) . . ?
O2W Ni1 N4 103.17(18) . . ?
O1 S1 O4 110.3(2) . . ?
O1 S1 O2 107.7(3) . . ?
O3 S1 O1 111.9(2) . . ?
O3 S1 O4 111.8(2) . . ?
O3 S1 O2 108.1(2) . . ?
O4 S1 O2 106.7(3) . . ?
O3A S1A O3A 151.1(8) 2_655 . ?
O3A S1A O1A 111.5(7) . . ?
O3A S1A O1A 39.9(4) 2_655 . ?
O3A S1A O1A 111.5(7) 2_655 2_655 ?
O3A S1A O1A 39.9(4) . 2_655 ?
O3A S1A O2A 99.6(5) . . ?
O3A S1A O2A 97.4(5) . 2_655 ?
O3A S1A O2A 97.4(5) 2_655 . ?
O3A S1A O2A 99.6(5) 2_655 2_655 ?
O1A S1A O1A 72.9(8) 2_655 . ?
O1A S1A O2A 112.3(4) 2_655 2_655 ?
O1A S1A O2A 124.8(5) 2_655 . ?
O1A S1A O2A 112.3(4) . . ?
O1A S1A O2A 124.8(5) . 2_655 ?
O2A S1A O2A 107.5(6) 2_655 . ?
C1 N2 Ni1 105.2(3) . . ?
C14 N2 Ni1 109.0(3) . . ?
C14 N2 C1 114.7(4) . . ?
C2 N3 Ni1 117.8(4) . . ?
C6 N3 Ni1 119.9(4) . . ?
C6 N3 C2 121.9(5) . . ?
C13 N1 Ni1 119.3(4) . . ?
C13 N1 C9 121.6(5) . . ?
C9 N1 Ni1 118.7(4) . . ?
C7 N4 Ni1 109.3(3) . . ?
C8 N4 Ni1 105.8(3) . . ?
C8 N4 C7 114.1(5) . . ?
N2 C1 C2 111.6(4) . . ?
N3 C2 C1 114.3(5) . . ?
N3 C2 C3 120.6(5) . . ?
C3 C2 C1 125.1(5) . . ?
N2 C14 C13 114.2(4) . . ?
N1 C13 C14 115.2(5) . . ?
N1 C13 C12 120.0(5) . . ?
C12 C13 C14 124.8(5) . . ?
C4 C5 C6 118.5(5) . . ?
C2 C3 C4 118.2(5) . . ?
N3 C6 C5 120.3(5) . . ?
N3 C6 C7 115.8(5) . . ?
C5 C6 C7 123.8(5) . . ?
O1A O3A S1A 71.7(7) 2_655 . ?
N1 C9 C10 121.0(6) . . ?
N1 C9 C8 113.6(5) . . ?
C10 C9 C8 125.4(5) . . ?
C11 C12 C13 119.0(6) . . ?
C5 C4 C3 120.4(5) . . ?
C9 C10 C11 118.0(5) . . ?
C12 C11 C10 120.4(6) . . ?
N4 C7 C6 113.0(4) . . ?
N4 C8 C9 111.7(5) . . ?
S1A O1A O1A 53.5(4) . 2_655 ?
O3A O1A S1A 68.4(7) 2_655 . ?
O3A O1A O1A 120.2(8) 2_655 2_655 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[(LH)Ni(mu-SPh)2Ni(LH)](BPh4)2
_database_code_depnum_ccdc_archive 'CCDC 1878198'
loop_
_audit_author_name
_audit_author_address
'Ray J. Butcher'
;Howard University
United States of America
;
_audit_update_record             
;
2019-03-21 deposited with the CCDC.	2019-04-18 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT232_shelx               
;
PROBLEM: Hirshfeld Test Diff (M-X)  Ni       --S1_a     .       10.7 s.u.  
RESPONSE: S1 is bridging between two Nickel atoms.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H42 N8 Ni2 S2, 2(C24 H20 B), 4(C2 H3 N)'
_chemical_formula_sum            'C96 H94 B2 N12 Ni2 S2'
_chemical_formula_weight         1618.99

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'
B B 0.0013 0.0007 '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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8252(14)
_cell_length_b                   11.8798(16)
_cell_length_c                   17.529(3)
_cell_angle_alpha                70.982(4)
_cell_angle_beta                 72.243(3)
_cell_angle_gamma                78.092(3)
_cell_volume                     2015.3(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3642
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      23.44

_exptl_crystal_description       prism
_exptl_crystal_colour            brown-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_F_000             852
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.576
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6136
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19037
_diffrn_reflns_av_unetI/netI     0.1998
_diffrn_reflns_av_R_equivalents  0.1178
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.680
_diffrn_reflns_theta_max         25.252
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7257
_reflns_number_gt                3646
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0751P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7257
_refine_ls_number_parameters     524
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1780
_refine_ls_R_factor_gt           0.0791
_refine_ls_wR_factor_ref         0.1849
_refine_ls_wR_factor_gt          0.1532
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Ni Ni 0.58650(8) 0.44373(6) 0.58121(5) 0.0241(3) Uani 1 1 d . . . . .
S1 S 0.36302(16) 0.48615(13) 0.57054(10) 0.0318(5) Uani 1 1 d . . . . .
N1 N 0.7755(4) 0.3994(4) 0.5883(3) 0.0205(12) Uani 1 1 d . . . . .
C1 C 0.8241(6) 0.2841(5) 0.6074(4) 0.0260(15) Uani 1 1 d . . . . .
N3 N 0.5462(4) 0.4032(4) 0.7082(3) 0.0220(12) Uani 1 1 d . . . . .
N2 N 0.6257(5) 0.6084(4) 0.5973(3) 0.0233(13) Uani 1 1 d . . . . .
H2N H 0.586(5) 0.667(5) 0.568(3) 0.024(17) Uiso 1 1 d . . . . .
C2 C 0.9396(6) 0.2470(5) 0.6301(4) 0.0321(16) Uani 1 1 d . . . . .
H2A H 0.972966 0.164426 0.643396 0.039 Uiso 1 1 calc R U . . .
C3 C 1.0065(6) 0.3318(6) 0.6333(4) 0.0345(17) Uani 1 1 d . . . . .
H3A H 1.086797 0.308279 0.648771 0.041 Uiso 1 1 calc R U . . .
N4 N 0.6013(5) 0.2480(4) 0.6165(3) 0.0274(13) Uani 1 1 d . . . . .
H4N H 0.561(5) 0.220(4) 0.588(3) 0.023(17) Uiso 1 1 d . . . . .
C4 C 0.9551(6) 0.4526(5) 0.6135(4) 0.0315(16) Uani 1 1 d . . . . .
H4A H 0.999666 0.512619 0.614958 0.038 Uiso 1 1 calc R U . . .
C5 C 0.8376(6) 0.4821(5) 0.5918(3) 0.0204(14) Uani 1 1 d . . . . .
C6 C 0.7689(6) 0.6084(4) 0.5696(4) 0.0261(15) Uani 1 1 d . . . . .
H6A H 0.795117 0.657862 0.596507 0.031 Uiso 1 1 calc R U . . .
H6B H 0.795549 0.644380 0.508399 0.031 Uiso 1 1 calc R U . . .
C7 C 0.5710(6) 0.6082(4) 0.6857(3) 0.0255(15) Uani 1 1 d . . . . .
H7A H 0.483597 0.655458 0.692267 0.031 Uiso 1 1 calc R U . . .
H7B H 0.628031 0.647015 0.701699 0.031 Uiso 1 1 calc R U . . .
C8 C 0.5593(5) 0.4823(5) 0.7432(4) 0.0201(14) Uani 1 1 d . . . . .
C9 C 0.5637(5) 0.4491(5) 0.8257(4) 0.0240(15) Uani 1 1 d . . . . .
H9A H 0.573277 0.506415 0.850078 0.029 Uiso 1 1 calc R U . . .
C10 C 0.5539(5) 0.3318(5) 0.8716(4) 0.0279(16) Uani 1 1 d . . . . .
H10A H 0.556147 0.307239 0.928525 0.034 Uiso 1 1 calc R U . . .
C11 C 0.5406(6) 0.2487(5) 0.8350(4) 0.0280(16) Uani 1 1 d . . . . .
H11A H 0.533355 0.167224 0.866133 0.034 Uiso 1 1 calc R U . . .
C12 C 0.5381(5) 0.2875(5) 0.7530(4) 0.0230(14) Uani 1 1 d . . . . .
C13 C 0.5231(6) 0.2101(5) 0.7049(3) 0.0270(15) Uani 1 1 d . . . . .
H13A H 0.552679 0.125371 0.730910 0.032 Uiso 1 1 calc R U . . .
H13B H 0.429831 0.216063 0.706400 0.032 Uiso 1 1 calc R U . . .
C14 C 0.7431(6) 0.1998(5) 0.6008(4) 0.0300(16) Uani 1 1 d . . . . .
H14A H 0.774197 0.187963 0.544356 0.036 Uiso 1 1 calc R U . . .
H14B H 0.754370 0.120857 0.641942 0.036 Uiso 1 1 calc R U . . .
C15 C 0.2906(6) 0.5961(5) 0.6230(4) 0.0334(17) Uani 1 1 d . . . . .
C16 C 0.3244(6) 0.7130(5) 0.5936(4) 0.0363(17) Uani 1 1 d . . . . .
H16A H 0.383641 0.736879 0.540226 0.044 Uiso 1 1 calc R U . . .
C17 C 0.2746(7) 0.7954(6) 0.6393(4) 0.0408(18) Uani 1 1 d . . . . .
H17A H 0.300379 0.873851 0.617876 0.049 Uiso 1 1 calc R U . . .
C18 C 0.1854(6) 0.7615(6) 0.7178(4) 0.0416(18) Uani 1 1 d . . . . .
H18A H 0.149183 0.817226 0.749606 0.050 Uiso 1 1 calc R U . . .
C19 C 0.1511(6) 0.6472(6) 0.7480(4) 0.0429(19) Uani 1 1 d . . . . .
H19A H 0.092322 0.623429 0.801535 0.051 Uiso 1 1 calc R U . . .
C20 C 0.2018(6) 0.5651(6) 0.7009(4) 0.0411(18) Uani 1 1 d . . . . .
H20A H 0.175225 0.486954 0.722465 0.049 Uiso 1 1 calc R U . . .
B1 B 0.2890(6) 0.1903(6) 1.1859(4) 0.0222(17) Uani 1 1 d . . . . .
C111 C 0.4450(5) 0.1565(4) 1.1405(3) 0.0188(14) Uani 1 1 d . . . . .
C112 C 0.5412(5) 0.2101(5) 1.1496(4) 0.0230(15) Uani 1 1 d . . . . .
H11B H 0.515595 0.264867 1.182374 0.028 Uiso 1 1 calc R U . . .
C113 C 0.6714(6) 0.1863(5) 1.1126(4) 0.0238(15) Uani 1 1 d . . . . .
H11C H 0.733998 0.223010 1.121459 0.029 Uiso 1 1 calc R U . . .
C114 C 0.7129(6) 0.1087(5) 1.0623(4) 0.0256(15) Uani 1 1 d . . . . .
H11D H 0.802853 0.093322 1.035928 0.031 Uiso 1 1 calc R U . . .
C115 C 0.6211(6) 0.0555(5) 1.0519(4) 0.0240(15) Uani 1 1 d . . . . .
H11E H 0.647623 0.001035 1.018916 0.029 Uiso 1 1 calc R U . . .
C116 C 0.4894(6) 0.0802(5) 1.0892(3) 0.0227(15) Uani 1 1 d . . . . .
H11F H 0.427411 0.044014 1.079335 0.027 Uiso 1 1 calc R U . . .
C211 C 0.1950(5) 0.1252(5) 1.1578(3) 0.0189(14) Uani 1 1 d . . . . .
C212 C 0.1958(6) 0.0021(5) 1.1823(4) 0.0265(15) Uani 1 1 d . . . . .
H21A H 0.250324 -0.045529 1.217345 0.032 Uiso 1 1 calc R U . . .
C213 C 0.1214(6) -0.0553(5) 1.1583(4) 0.0289(16) Uani 1 1 d . . . . .
H21B H 0.126167 -0.140253 1.177005 0.035 Uiso 1 1 calc R U . . .
C214 C 0.0411(6) 0.0084(5) 1.1082(4) 0.0299(16) Uani 1 1 d . . . . .
H21C H -0.008845 -0.030912 1.090718 0.036 Uiso 1 1 calc R U . . .
C215 C 0.0347(6) 0.1325(5) 1.0836(4) 0.0330(17) Uani 1 1 d . . . . .
H21D H -0.021649 0.179435 1.049625 0.040 Uiso 1 1 calc R U . . .
C216 C 0.1106(6) 0.1885(5) 1.1084(4) 0.0286(16) Uani 1 1 d . . . . .
H21E H 0.104411 0.273529 1.090682 0.034 Uiso 1 1 calc R U . . .
C311 C 0.2543(5) 0.3383(5) 1.1533(4) 0.0223(14) Uani 1 1 d . . . . .
C312 C 0.3041(6) 0.3994(5) 1.0699(4) 0.0271(15) Uani 1 1 d . . . . .
H31A H 0.364112 0.355434 1.034625 0.033 Uiso 1 1 calc R U . . .
C313 C 0.2709(6) 0.5209(5) 1.0354(4) 0.0313(16) Uani 1 1 d . . . . .
H31B H 0.306761 0.558398 0.978043 0.038 Uiso 1 1 calc R U . . .
C314 C 0.1847(6) 0.5865(5) 1.0862(4) 0.0290(16) Uani 1 1 d . . . . .
H31C H 0.161430 0.669869 1.063962 0.035 Uiso 1 1 calc R U . . .
C315 C 0.1330(5) 0.5305(5) 1.1689(4) 0.0280(15) Uani 1 1 d . . . . .
H31D H 0.073300 0.575265 1.203746 0.034 Uiso 1 1 calc R U . . .
C316 C 0.1676(5) 0.4079(5) 1.2020(4) 0.0227(15) Uani 1 1 d . . . . .
H31E H 0.131136 0.370963 1.259439 0.027 Uiso 1 1 calc R U . . .
C411 C 0.2595(6) 0.1431(4) 1.2877(4) 0.0211(14) Uani 1 1 d . . . . .
C412 C 0.1294(6) 0.1440(4) 1.3367(4) 0.0257(15) Uani 1 1 d . . . . .
H41A H 0.060739 0.168992 1.309345 0.031 Uiso 1 1 calc R U . . .
C413 C 0.0975(6) 0.1097(5) 1.4231(4) 0.0267(16) Uani 1 1 d . . . . .
H41B H 0.008261 0.112872 1.453402 0.032 Uiso 1 1 calc R U . . .
C414 C 0.1930(6) 0.0712(5) 1.4659(4) 0.0273(16) Uani 1 1 d . . . . .
H41C H 0.170524 0.048467 1.525240 0.033 Uiso 1 1 calc R U . . .
C415 C 0.3218(6) 0.0665(5) 1.4209(4) 0.0254(15) Uani 1 1 d . . . . .
H41D H 0.389244 0.039874 1.449194 0.031 Uiso 1 1 calc R U . . .
C416 C 0.3533(6) 0.1005(4) 1.3342(4) 0.0243(15) Uani 1 1 d . . . . .
H41E H 0.442964 0.094600 1.304766 0.029 Uiso 1 1 calc R U . . .
N1S N 0.1614(8) 0.2424(6) 0.8153(5) 0.081(2) Uani 1 1 d . . . . .
C11S C 0.1786(8) 0.2941(7) 0.8553(5) 0.056(2) Uani 1 1 d . . . . .
C12S C 0.1992(8) 0.3661(7) 0.9032(5) 0.066(2) Uani 1 1 d . . . . .
H12A H 0.116698 0.413118 0.922850 0.099 Uiso 1 1 calc R U . . .
H12B H 0.264418 0.420361 0.867550 0.099 Uiso 1 1 calc R U . . .
H12C H 0.230359 0.312967 0.951268 0.099 Uiso 1 1 calc R U . . .
N2S N 0.3846(6) 0.1624(5) 0.5672(4) 0.0431(16) Uani 1 1 d . . . . .
C21S C 0.3224(7) 0.1117(6) 0.6296(4) 0.0346(17) Uani 1 1 d . . . . .
C22S C 0.2425(7) 0.0506(6) 0.7111(4) 0.053(2) Uani 1 1 d . . . . .
H22A H 0.293182 -0.023021 0.736478 0.079 Uiso 1 1 calc R U . . .
H22B H 0.164204 0.030469 0.703970 0.079 Uiso 1 1 calc R U . . .
H22C H 0.216780 0.103546 0.747517 0.079 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N1 2.036(5) . ?
Ni N3 2.043(5) . ?
Ni N4 2.188(5) . ?
Ni N2 2.205(5) . ?
Ni S1 2.4193(18) . ?
Ni S1 2.4342(19) 2_666 ?
S1 C15 1.757(6) . ?
N1 C5 1.326(6) . ?
N1 C1 1.333(7) . ?
C1 C2 1.371(8) . ?
C1 C14 1.512(8) . ?
N3 C8 1.327(6) . ?
N3 C12 1.348(6) . ?
N2 C6 1.476(7) . ?
N2 C7 1.481(7) . ?
N2 H2N 0.84(5) . ?
C2 C3 1.381(8) . ?
C2 H2A 0.9500 . ?
C3 C4 1.397(8) . ?
C3 H3A 0.9500 . ?
N4 C13 1.490(7) . ?
N4 C14 1.497(7) . ?
N4 H4N 0.93(5) . ?
C4 C5 1.382(7) . ?
C4 H4A 0.9500 . ?
C5 C6 1.513(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.512(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.382(7) . ?
C9 C10 1.371(7) . ?
C9 H9A 0.9500 . ?
C10 C11 1.392(7) . ?
C10 H10A 0.9500 . ?
C11 C12 1.365(7) . ?
C11 H11A 0.9500 . ?
C12 C13 1.496(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.394(8) . ?
C15 C16 1.399(8) . ?
C16 C17 1.386(8) . ?
C16 H16A 0.9500 . ?
C17 C18 1.406(8) . ?
C17 H17A 0.9500 . ?
C18 C19 1.372(8) . ?
C18 H18A 0.9500 . ?
C19 C20 1.400(8) . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9500 . ?
B1 C411 1.634(8) . ?
B1 C111 1.660(8) . ?
B1 C211 1.661(9) . ?
B1 C311 1.662(8) . ?
C111 C116 1.397(7) . ?
C111 C112 1.399(7) . ?
C112 C113 1.373(7) . ?
C112 H11B 0.9500 . ?
C113 C114 1.395(7) . ?
C113 H11C 0.9500 . ?
C114 C115 1.366(7) . ?
C114 H11D 0.9500 . ?
C115 C116 1.389(7) . ?
C115 H11E 0.9500 . ?
C116 H11F 0.9500 . ?
C211 C212 1.383(7) . ?
C211 C216 1.387(7) . ?
C212 C213 1.382(7) . ?
C212 H21A 0.9500 . ?
C213 C214 1.364(8) . ?
C213 H21B 0.9500 . ?
C214 C215 1.388(8) . ?
C214 H21C 0.9500 . ?
C215 C216 1.392(8) . ?
C215 H21D 0.9500 . ?
C216 H21E 0.9500 . ?
C311 C312 1.394(7) . ?
C311 C316 1.395(7) . ?
C312 C313 1.388(7) . ?
C312 H31A 0.9500 . ?
C313 C314 1.383(7) . ?
C313 H31B 0.9500 . ?
C314 C315 1.374(7) . ?
C314 H31C 0.9500 . ?
C315 C316 1.398(7) . ?
C315 H31D 0.9500 . ?
C316 H31E 0.9500 . ?
C411 C416 1.406(7) . ?
C411 C412 1.408(7) . ?
C412 C413 1.385(7) . ?
C412 H41A 0.9500 . ?
C413 C414 1.377(8) . ?
C413 H41B 0.9500 . ?
C414 C415 1.376(8) . ?
C414 H41C 0.9500 . ?
C415 C416 1.390(7) . ?
C415 H41D 0.9500 . ?
C416 H41E 0.9500 . ?
N1S C11S 1.145(9) . ?
C11S C12S 1.465(10) . ?
C12S H12A 0.9800 . ?
C12S H12B 0.9800 . ?
C12S H12C 0.9800 . ?
N2S C21S 1.141(7) . ?
C21S C22S 1.465(8) . ?
C22S H22A 0.9800 . ?
C22S H22B 0.9800 . ?
C22S H22C 0.9800 . ?

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
N1 Ni N3 83.74(18) . . ?
N1 Ni N4 79.38(19) . . ?
N3 Ni N4 78.89(18) . . ?
N1 Ni N2 78.75(18) . . ?
N3 Ni N2 78.37(18) . . ?
N4 Ni N2 149.9(2) . . ?
N1 Ni S1 176.76(13) . . ?
N3 Ni S1 97.36(13) . . ?
N4 Ni S1 97.81(15) . . ?
N2 Ni S1 104.45(14) . . ?
N1 Ni S1 95.88(13) . 2_666 ?
N3 Ni S1 173.77(13) . 2_666 ?
N4 Ni S1 107.18(14) . 2_666 ?
N2 Ni S1 95.45(14) . 2_666 ?
S1 Ni S1 83.37(6) . 2_666 ?
C15 S1 Ni 104.8(2) . . ?
C15 S1 Ni 115.9(2) . 2_666 ?
Ni S1 Ni 96.64(6) . 2_666 ?
C5 N1 C1 120.5(5) . . ?
C5 N1 Ni 118.8(4) . . ?
C1 N1 Ni 119.1(4) . . ?
N1 C1 C2 121.7(6) . . ?
N1 C1 C14 114.8(5) . . ?
C2 C1 C14 123.5(5) . . ?
C8 N3 C12 120.1(5) . . ?
C8 N3 Ni 119.9(4) . . ?
C12 N3 Ni 118.0(4) . . ?
C6 N2 C7 112.9(5) . . ?
C6 N2 Ni 106.2(3) . . ?
C7 N2 Ni 109.3(3) . . ?
C6 N2 H2N 113(4) . . ?
C7 N2 H2N 108(4) . . ?
Ni N2 H2N 108(4) . . ?
C1 C2 C3 118.7(6) . . ?
C1 C2 H2A 120.7 . . ?
C3 C2 H2A 120.7 . . ?
C2 C3 C4 119.5(6) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C13 N4 C14 115.6(5) . . ?
C13 N4 Ni 106.3(3) . . ?
C14 N4 Ni 108.1(3) . . ?
C13 N4 H4N 104(3) . . ?
C14 N4 H4N 110(3) . . ?
Ni N4 H4N 113(3) . . ?
C5 C4 C3 118.0(6) . . ?
C5 C4 H4A 121.0 . . ?
C3 C4 H4A 121.0 . . ?
N1 C5 C4 121.6(5) . . ?
N1 C5 C6 114.0(5) . . ?
C4 C5 C6 124.4(5) . . ?
N2 C6 C5 110.9(4) . . ?
N2 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.0 . . ?
N2 C7 C8 111.7(5) . . ?
N2 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
N2 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
N3 C8 C9 121.4(5) . . ?
N3 C8 C7 114.8(5) . . ?
C9 C8 C7 123.8(5) . . ?
C10 C9 C8 118.7(6) . . ?
C10 C9 H9A 120.7 . . ?
C8 C9 H9A 120.7 . . ?
C9 C10 C11 120.0(6) . . ?
C9 C10 H10A 120.0 . . ?
C11 C10 H10A 120.0 . . ?
C12 C11 C10 118.2(5) . . ?
C12 C11 H11A 120.9 . . ?
C10 C11 H11A 120.9 . . ?
N3 C12 C11 121.7(5) . . ?
N3 C12 C13 113.6(5) . . ?
C11 C12 C13 124.8(5) . . ?
N4 C13 C12 110.4(5) . . ?
N4 C13 H13A 109.6 . . ?
C12 C13 H13A 109.6 . . ?
N4 C13 H13B 109.6 . . ?
C12 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
N4 C14 C1 111.3(5) . . ?
N4 C14 H14A 109.4 . . ?
C1 C14 H14A 109.4 . . ?
N4 C14 H14B 109.4 . . ?
C1 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C20 C15 C16 117.1(6) . . ?
C20 C15 S1 119.5(5) . . ?
C16 C15 S1 123.3(5) . . ?
C17 C16 C15 122.4(6) . . ?
C17 C16 H16A 118.8 . . ?
C15 C16 H16A 118.8 . . ?
C16 C17 C18 119.2(6) . . ?
C16 C17 H17A 120.4 . . ?
C18 C17 H17A 120.4 . . ?
C19 C18 C17 119.3(6) . . ?
C19 C18 H18A 120.3 . . ?
C17 C18 H18A 120.3 . . ?
C18 C19 C20 120.8(7) . . ?
C18 C19 H19A 119.6 . . ?
C20 C19 H19A 119.6 . . ?
C15 C20 C19 121.1(6) . . ?
C15 C20 H20A 119.5 . . ?
C19 C20 H20A 119.5 . . ?
C411 B1 C111 111.5(5) . . ?
C411 B1 C211 107.5(4) . . ?
C111 B1 C211 110.0(5) . . ?
C411 B1 C311 111.2(5) . . ?
C111 B1 C311 107.5(4) . . ?
C211 B1 C311 109.2(5) . . ?
C116 C111 C112 115.7(5) . . ?
C116 C111 B1 124.4(5) . . ?
C112 C111 B1 119.8(5) . . ?
C113 C112 C111 122.2(6) . . ?
C113 C112 H11B 118.9 . . ?
C111 C112 H11B 118.9 . . ?
C112 C113 C114 120.7(6) . . ?
C112 C113 H11C 119.6 . . ?
C114 C113 H11C 119.6 . . ?
C115 C114 C113 118.4(5) . . ?
C115 C114 H11D 120.8 . . ?
C113 C114 H11D 120.8 . . ?
C114 C115 C116 120.7(6) . . ?
C114 C115 H11E 119.7 . . ?
C116 C115 H11E 119.7 . . ?
C115 C116 C111 122.2(6) . . ?
C115 C116 H11F 118.9 . . ?
C111 C116 H11F 118.9 . . ?
C212 C211 C216 114.9(5) . . ?
C212 C211 B1 121.8(5) . . ?
C216 C211 B1 123.4(5) . . ?
C213 C212 C211 123.3(5) . . ?
C213 C212 H21A 118.4 . . ?
C211 C212 H21A 118.4 . . ?
C214 C213 C212 121.0(6) . . ?
C214 C213 H21B 119.5 . . ?
C212 C213 H21B 119.5 . . ?
C213 C214 C215 117.8(6) . . ?
C213 C214 H21C 121.1 . . ?
C215 C214 H21C 121.1 . . ?
C214 C215 C216 120.3(6) . . ?
C214 C215 H21D 119.8 . . ?
C216 C215 H21D 119.8 . . ?
C211 C216 C215 122.7(5) . . ?
C211 C216 H21E 118.6 . . ?
C215 C216 H21E 118.6 . . ?
C312 C311 C316 115.5(5) . . ?
C312 C311 B1 119.8(5) . . ?
C316 C311 B1 124.5(5) . . ?
C313 C312 C311 123.7(6) . . ?
C313 C312 H31A 118.1 . . ?
C311 C312 H31A 118.1 . . ?
C314 C313 C312 118.8(6) . . ?
C314 C313 H31B 120.6 . . ?
C312 C313 H31B 120.6 . . ?
C315 C314 C313 119.8(5) . . ?
C315 C314 H31C 120.1 . . ?
C313 C314 H31C 120.1 . . ?
C314 C315 C316 120.3(6) . . ?
C314 C315 H31D 119.8 . . ?
C316 C315 H31D 119.8 . . ?
C311 C316 C315 121.9(5) . . ?
C311 C316 H31E 119.0 . . ?
C315 C316 H31E 119.0 . . ?
C416 C411 C412 114.1(5) . . ?
C416 C411 B1 126.2(5) . . ?
C412 C411 B1 119.6(5) . . ?
C413 C412 C411 122.6(6) . . ?
C413 C412 H41A 118.7 . . ?
C411 C412 H41A 118.7 . . ?
C414 C413 C412 121.2(6) . . ?
C414 C413 H41B 119.4 . . ?
C412 C413 H41B 119.4 . . ?
C415 C414 C413 118.5(6) . . ?
C415 C414 H41C 120.7 . . ?
C413 C414 H41C 120.7 . . ?
C414 C415 C416 120.2(6) . . ?
C414 C415 H41D 119.9 . . ?
C416 C415 H41D 119.9 . . ?
C415 C416 C411 123.4(6) . . ?
C415 C416 H41E 118.3 . . ?
C411 C416 H41E 118.3 . . ?
N1S C11S C12S 177.0(9) . . ?
C11S C12S H12A 109.5 . . ?
C11S C12S H12B 109.5 . . ?
H12A C12S H12B 109.5 . . ?
C11S C12S H12C 109.5 . . ?
H12A C12S H12C 109.5 . . ?
H12B C12S H12C 109.5 . . ?
N2S C21S C22S 177.6(7) . . ?
C21S C22S H22A 109.5 . . ?
C21S C22S H22B 109.5 . . ?
H22A C22S H22B 109.5 . . ?
C21S C22S H22C 109.5 . . ?
H22A C22S H22C 109.5 . . ?
H22B C22S H22C 109.5 . . ?

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
C5 N1 C1 C2 -0.8(8) . . . . ?
Ni N1 C1 C2 -166.2(4) . . . . ?
C5 N1 C1 C14 179.9(5) . . . . ?
Ni N1 C1 C14 14.6(6) . . . . ?
N1 C1 C2 C3 0.1(9) . . . . ?
C14 C1 C2 C3 179.3(5) . . . . ?
C1 C2 C3 C4 0.1(9) . . . . ?
C2 C3 C4 C5 0.4(9) . . . . ?
C1 N1 C5 C4 1.3(8) . . . . ?
Ni N1 C5 C4 166.7(4) . . . . ?
C1 N1 C5 C6 -179.1(5) . . . . ?
Ni N1 C5 C6 -13.8(6) . . . . ?
C3 C4 C5 N1 -1.1(8) . . . . ?
C3 C4 C5 C6 179.4(5) . . . . ?
C7 N2 C6 C5 84.5(6) . . . . ?
Ni N2 C6 C5 -35.2(5) . . . . ?
N1 C5 C6 N2 34.0(7) . . . . ?
C4 C5 C6 N2 -146.5(5) . . . . ?
C6 N2 C7 C8 -93.3(5) . . . . ?
Ni N2 C7 C8 24.6(6) . . . . ?
C12 N3 C8 C9 -0.6(8) . . . . ?
Ni N3 C8 C9 -164.4(4) . . . . ?
C12 N3 C8 C7 178.4(5) . . . . ?
Ni N3 C8 C7 14.7(6) . . . . ?
N2 C7 C8 N3 -26.4(7) . . . . ?
N2 C7 C8 C9 152.6(5) . . . . ?
N3 C8 C9 C10 -0.2(8) . . . . ?
C7 C8 C9 C10 -179.1(5) . . . . ?
C8 C9 C10 C11 0.4(8) . . . . ?
C9 C10 C11 C12 0.2(9) . . . . ?
C8 N3 C12 C11 1.2(8) . . . . ?
Ni N3 C12 C11 165.3(4) . . . . ?
C8 N3 C12 C13 179.7(5) . . . . ?
Ni N3 C12 C13 -16.2(6) . . . . ?
C10 C11 C12 N3 -1.0(9) . . . . ?
C10 C11 C12 C13 -179.4(6) . . . . ?
C14 N4 C13 C12 82.7(6) . . . . ?
Ni N4 C13 C12 -37.3(5) . . . . ?
N3 C12 C13 N4 36.6(7) . . . . ?
C11 C12 C13 N4 -144.9(6) . . . . ?
C13 N4 C14 C1 -91.3(5) . . . . ?
Ni N4 C14 C1 27.6(6) . . . . ?
N1 C1 C14 N4 -28.6(7) . . . . ?
C2 C1 C14 N4 152.2(5) . . . . ?
Ni S1 C15 C20 -107.2(5) . . . . ?
Ni S1 C15 C20 147.7(5) 2_666 . . . ?
Ni S1 C15 C16 67.9(5) . . . . ?
Ni S1 C15 C16 -37.2(6) 2_666 . . . ?
C20 C15 C16 C17 1.0(9) . . . . ?
S1 C15 C16 C17 -174.2(5) . . . . ?
C15 C16 C17 C18 -0.9(10) . . . . ?
C16 C17 C18 C19 1.0(10) . . . . ?
C17 C18 C19 C20 -1.3(10) . . . . ?
C16 C15 C20 C19 -1.3(10) . . . . ?
S1 C15 C20 C19 174.2(5) . . . . ?
C18 C19 C20 C15 1.5(10) . . . . ?
C411 B1 C111 C116 116.7(6) . . . . ?
C211 B1 C111 C116 -2.5(7) . . . . ?
C311 B1 C111 C116 -121.2(6) . . . . ?
C411 B1 C111 C112 -66.4(6) . . . . ?
C211 B1 C111 C112 174.4(4) . . . . ?
C311 B1 C111 C112 55.7(7) . . . . ?
C116 C111 C112 C113 -2.1(8) . . . . ?
B1 C111 C112 C113 -179.3(5) . . . . ?
C111 C112 C113 C114 1.6(8) . . . . ?
C112 C113 C114 C115 -1.2(8) . . . . ?
C113 C114 C115 C116 1.4(8) . . . . ?
C114 C115 C116 C111 -2.1(8) . . . . ?
C112 C111 C116 C115 2.4(8) . . . . ?
B1 C111 C116 C115 179.4(5) . . . . ?
C411 B1 C211 C212 -54.3(7) . . . . ?
C111 B1 C211 C212 67.3(7) . . . . ?
C311 B1 C211 C212 -175.0(5) . . . . ?
C411 B1 C211 C216 126.0(6) . . . . ?
C111 B1 C211 C216 -112.4(6) . . . . ?
C311 B1 C211 C216 5.3(8) . . . . ?
C216 C211 C212 C213 1.5(9) . . . . ?
B1 C211 C212 C213 -178.3(5) . . . . ?
C211 C212 C213 C214 -0.2(9) . . . . ?
C212 C213 C214 C215 -1.3(9) . . . . ?
C213 C214 C215 C216 1.3(9) . . . . ?
C212 C211 C216 C215 -1.4(9) . . . . ?
B1 C211 C216 C215 178.4(5) . . . . ?
C214 C215 C216 C211 0.1(9) . . . . ?
C411 B1 C311 C312 162.9(5) . . . . ?
C111 B1 C311 C312 40.6(7) . . . . ?
C211 B1 C311 C312 -78.6(6) . . . . ?
C411 B1 C311 C316 -23.0(8) . . . . ?
C111 B1 C311 C316 -145.3(5) . . . . ?
C211 B1 C311 C316 95.5(6) . . . . ?
C316 C311 C312 C313 -0.6(9) . . . . ?
B1 C311 C312 C313 174.0(5) . . . . ?
C311 C312 C313 C314 0.7(9) . . . . ?
C312 C313 C314 C315 -0.6(9) . . . . ?
C313 C314 C315 C316 0.4(9) . . . . ?
C312 C311 C316 C315 0.4(8) . . . . ?
B1 C311 C316 C315 -173.9(5) . . . . ?
C314 C315 C316 C311 -0.3(9) . . . . ?
C111 B1 C411 C416 11.9(8) . . . . ?
C211 B1 C411 C416 132.6(5) . . . . ?
C311 B1 C411 C416 -108.0(6) . . . . ?
C111 B1 C411 C412 -168.5(5) . . . . ?
C211 B1 C411 C412 -47.9(6) . . . . ?
C311 B1 C411 C412 71.6(6) . . . . ?
C416 C411 C412 C413 2.2(8) . . . . ?
B1 C411 C412 C413 -177.4(5) . . . . ?
C411 C412 C413 C414 -0.8(8) . . . . ?
C412 C413 C414 C415 -0.5(8) . . . . ?
C413 C414 C415 C416 0.2(8) . . . . ?
C414 C415 C416 C411 1.3(8) . . . . ?
C412 C411 C416 C415 -2.5(8) . . . . ?
B1 C411 C416 C415 177.1(5) . . . . ?

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
N2 H2N N2S 0.84(5) 2.55(5) 3.269(7) 144(5) 2_666 yes
N4 H4N N2S 0.93(5) 2.31(5) 3.174(8) 154(4) . yes
C16 H16A N4 0.95 2.65 3.414(8) 137.8 2_666 yes
C22S H22C N1S 0.98 2.22 3.195(10) 172.8 . yes

_refine_diff_density_max         0.673
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.092

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[(LH)Ni(CO3)]
_database_code_depnum_ccdc_archive 'CCDC 1878199'
loop_
_audit_author_name
_audit_author_address
'Ray J. Butcher'
;Howard University
United States of America
;
_audit_update_record             
;
2019-03-21 deposited with the CCDC.	2019-04-18 downloaded from the CCDC.
;
_audit_creation_date             2019-03-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C15 H16 N4 Ni O3'
_chemical_formula_sum            'C15 H16 N4 Ni O3'
_chemical_formula_weight         359.03
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   30.9603(10)
_cell_length_b                   30.9603(10)
_cell_length_c                   11.4869(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9535.5(7)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.578
_cell_measurement_theta_min      2.278
_shelx_estimated_absorpt_T_max   0.982
_shelx_estimated_absorpt_T_min   0.929
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1284 before and 0.0507 after correction. The Ratio of minimum to maximum transmission is 0.8570. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light violet'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3348
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            38689
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.979
_diffrn_reflns_theta_max         24.979
_diffrn_reflns_theta_min         2.279
_diffrn_ambient_temperature      100.2
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3079
_reflns_number_total             3723
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3723
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0429
_refine_ls_restrained_S_all      1.139
_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)+(0.0673P)²+21.9961P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1283
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N4(H4), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7A,H7B), C14(H14A,H14B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C5(H5), C12(H12), C10(H10), C11(H11)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.64071(2) 0.57643(2) 0.88805(3) 0.02658(15) Uani 1 1 d . . . . .
O1 O 0.62032(8) 0.63122(8) 0.89467(19) 0.0333(5) Uani 1 1 d . . . . .
O2 O 0.69862(8) 0.64954(8) 0.88068(19) 0.0333(5) Uani 1 1 d . . . . .
O3 O 0.68123(9) 0.71157(8) 0.89100(18) 0.0377(6) Uani 1 1 d . . . . .
N4 N 0.61943(10) 0.55386(10) 0.7082(2) 0.0335(6) Uani 1 1 d . . . . .
H4 H 0.629439 0.584163 0.659357 0.040 Uiso 1 1 calc R . . . .
N1 N 0.57540(9) 0.51539(9) 0.9126(2) 0.0257(5) Uani 1 1 d . . . . .
N3 N 0.67193(9) 0.53434(10) 0.8652(2) 0.0338(6) Uani 1 1 d . . . . .
N2 N 0.64976(9) 0.56131(10) 1.0681(2) 0.0313(6) Uani 1 1 d . . . . .
H2 H 0.660355 0.592081 1.115599 0.038 Uiso 1 1 calc R . . . .
C1C C 0.66727(13) 0.66548(12) 0.8887(2) 0.0326(7) Uani 1 1 d . . . . .
C2 C 0.56289(11) 0.49485(11) 1.0178(3) 0.0259(6) Uani 1 1 d . . . . .
C3 C 0.51653(12) 0.45378(11) 1.0372(3) 0.0294(7) Uani 1 1 d . . . . .
H3 H 0.507373 0.439379 1.112597 0.035 Uiso 1 1 calc R . . . .
C6 C 0.54485(11) 0.49515(12) 0.8213(3) 0.0299(7) Uani 1 1 d . . . . .
C13 C 0.69133(12) 0.52373(13) 0.9576(3) 0.0415(9) Uani 1 1 d . . . . .
C1 C 0.60163(12) 0.52109(12) 1.1120(3) 0.0315(7) Uani 1 1 d . . . . .
H1A H 0.588366 0.535299 1.169541 0.038 Uiso 1 1 calc R . . . .
H1B H 0.607299 0.496203 1.152824 0.038 Uiso 1 1 calc R . . . .
C7 C 0.56475(13) 0.52273(14) 0.7080(3) 0.0410(8) Uani 1 1 d . . . . .
H7A H 0.554426 0.498301 0.643613 0.049 Uiso 1 1 calc R . . . .
H7B H 0.549964 0.544151 0.693703 0.049 Uiso 1 1 calc R . . . .
C9 C 0.66971(12) 0.51435(12) 0.7609(3) 0.0396(8) Uani 1 1 d . . . . .
C4 C 0.48368(12) 0.43395(11) 0.9452(3) 0.0308(7) Uani 1 1 d . . . . .
H4A H 0.451063 0.406554 0.957527 0.037 Uiso 1 1 calc R . . . .
C14 C 0.69011(13) 0.54870(15) 1.0687(3) 0.0455(9) Uani 1 1 d . . . . .
H14A H 0.685069 0.526283 1.135083 0.055 Uiso 1 1 calc R . . . .
H14B H 0.722605 0.579582 1.079524 0.055 Uiso 1 1 calc R . . . .
C5 C 0.49832(12) 0.45403(12) 0.8353(3) 0.0323(7) Uani 1 1 d . . . . .
H5 H 0.476648 0.439693 0.770514 0.039 Uiso 1 1 calc R . . . .
C8 C 0.64551(13) 0.52790(13) 0.6659(3) 0.0427(9) Uani 1 1 d . . . . .
H8A H 0.671333 0.549599 0.609082 0.051 Uiso 1 1 calc R . . . .
H8B H 0.621268 0.497122 0.624755 0.051 Uiso 1 1 calc R . . . .
C12 C 0.71177(14) 0.49329(15) 0.9447(5) 0.0585(12) Uani 1 1 d . . . . .
H12 H 0.725846 0.485746 1.009648 0.070 Uiso 1 1 calc R . . . .
C10 C 0.68990(14) 0.48381(14) 0.7438(5) 0.0569(11) Uani 1 1 d . . . . .
H10 H 0.688836 0.469904 0.669376 0.068 Uiso 1 1 calc R . . . .
C11 C 0.71150(15) 0.47408(15) 0.8369(5) 0.0683(14) Uani 1 1 d . . . . .
H11 H 0.726366 0.453920 0.826588 0.082 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.086(2) . ?
Ni1 O2 2.070(2) . ?
Ni1 N4 2.175(3) . ?
Ni1 N1 1.979(2) . ?
Ni1 N3 1.990(3) . ?
Ni1 N2 2.170(3) . ?
Ni1 C1C 2.452(3) . ?
O1 C1C 1.304(4) . ?
O2 C1C 1.293(4) . ?
O3 C1C 1.268(4) . ?
N4 C7 1.471(4) . ?
N4 C8 1.477(4) . ?
N1 C2 1.330(4) . ?
N1 C6 1.340(4) . ?
N3 C13 1.339(5) . ?
N3 C9 1.335(4) . ?
N2 C1 1.473(4) . ?
N2 C14 1.483(4) . ?
C2 C3 1.379(4) . ?
C2 C1 1.514(4) . ?
C3 C4 1.380(4) . ?
C6 C7 1.509(5) . ?
C6 C5 1.374(4) . ?
C13 C14 1.501(6) . ?
C13 C12 1.381(5) . ?
C9 C8 1.497(5) . ?
C9 C10 1.384(5) . ?
C4 C5 1.380(5) . ?
C12 C11 1.372(7) . ?
C10 C11 1.372(7) . ?

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
O1 Ni1 N4 97.45(10) . . ?
O1 Ni1 N2 105.36(9) . . ?
O1 Ni1 C1C 32.14(10) . . ?
O2 Ni1 O1 63.98(8) . . ?
O2 Ni1 N4 105.66(10) . . ?
O2 Ni1 N2 98.06(9) . . ?
O2 Ni1 C1C 31.84(10) . . ?
N4 Ni1 C1C 103.97(10) . . ?
N1 Ni1 O1 101.01(9) . . ?
N1 Ni1 O2 164.22(9) . . ?
N1 Ni1 N4 80.10(10) . . ?
N1 Ni1 N3 89.57(10) . . ?
N1 Ni1 N2 80.70(10) . . ?
N1 Ni1 C1C 132.95(11) . . ?
N3 Ni1 O1 168.71(10) . . ?
N3 Ni1 O2 105.78(9) . . ?
N3 Ni1 N4 80.36(11) . . ?
N3 Ni1 N2 80.05(11) . . ?
N3 Ni1 C1C 137.49(11) . . ?
N2 Ni1 N4 152.54(11) . . ?
N2 Ni1 C1C 103.47(10) . . ?
C1C O1 Ni1 89.53(18) . . ?
C1C O2 Ni1 90.54(19) . . ?
C7 N4 Ni1 106.02(18) . . ?
C7 N4 C8 114.0(3) . . ?
C8 N4 Ni1 109.1(2) . . ?
C2 N1 Ni1 120.0(2) . . ?
C2 N1 C6 121.3(3) . . ?
C6 N1 Ni1 118.7(2) . . ?
C13 N3 Ni1 118.7(2) . . ?
C9 N3 Ni1 119.5(2) . . ?
C9 N3 C13 121.6(3) . . ?
C1 N2 Ni1 108.85(18) . . ?
C1 N2 C14 113.9(3) . . ?
C14 N2 Ni1 106.1(2) . . ?
O1 C1C Ni1 58.33(15) . . ?
O2 C1C Ni1 57.62(16) . . ?
O2 C1C O1 115.9(3) . . ?
O3 C1C Ni1 178.9(2) . . ?
O3 C1C O1 121.9(3) . . ?
O3 C1C O2 122.2(3) . . ?
N1 C2 C3 120.5(3) . . ?
N1 C2 C1 115.4(3) . . ?
C3 C2 C1 124.0(3) . . ?
C2 C3 C4 118.9(3) . . ?
N1 C6 C7 114.7(3) . . ?
N1 C6 C5 120.7(3) . . ?
C5 C6 C7 124.6(3) . . ?
N3 C13 C14 114.7(3) . . ?
N3 C13 C12 119.8(4) . . ?
C12 C13 C14 125.5(4) . . ?
N2 C1 C2 113.9(2) . . ?
N4 C7 C6 112.4(3) . . ?
N3 C9 C8 116.2(3) . . ?
N3 C9 C10 120.5(4) . . ?
C10 C9 C8 123.3(4) . . ?
C3 C4 C5 119.8(3) . . ?
N2 C14 C13 111.9(3) . . ?
C6 C5 C4 118.7(3) . . ?
N4 C8 C9 113.6(3) . . ?
C11 C12 C13 119.2(4) . . ?
C11 C10 C9 118.4(4) . . ?
C10 C11 C12 120.4(4) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[(LH)Ni(dbm)](BPh4)
_database_code_depnum_ccdc_archive 'CCDC 1878197'
loop_
_audit_author_name
_audit_author_address
'Sakthi Raje'
;Indian Institute of Technology Kanpur
India
;
_audit_update_record             
;
2018-11-09 deposited with the CCDC.	2019-04-18 downloaded from the CCDC.
;
_audit_creation_date             2018-10-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '3(C29 H27 N4 Ni O2), C4 H10 O, 3(C24 H20 B)'
_chemical_formula_sum            'C163 H151 B3 N12 Ni3 O7'
_chemical_formula_weight         2598.51
_chemical_absolute_configuration unk
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   42.319(3)
_cell_length_b                   22.6000(14)
_cell_length_c                   15.7228(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.976(4)
_cell_angle_gamma                90
_cell_volume                     15001.4(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9171
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.643
_cell_measurement_theta_min      2.385
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1579 before and 0.0558 after correction. The Ratio of minimum to maximum transmission is 0.9095. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            90580
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.757
_diffrn_ambient_temperature      100.2
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_source                   ?
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                22890
_reflns_number_total             26417
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.125
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.551(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1686
_refine_ls_number_reflns         26417
_refine_ls_number_restraints     121
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0531
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0689P)²+28.2146P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1403
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.449(13)
 0.551(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C38 \\sim C43 \\sim C42 \\sim C41 \\sim C40 \\sim C39: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
O7 \\sim C89 \\sim C90 \\sim C91 \\sim C92: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
O1B \\sim C64 \\sim C65 \\sim C63 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim
C62: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Ni1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.05
4.a Ternary CH refined with riding coordinates:
 N2A(H2A), N4A(H4A), N4(H4), N2(H2), N2C(H2C), N2B(H2B)
4.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C51(H51A,H51B), C57(H57A,H57B), C44(H44A,H44B), C7(H7A,H7B),
 C8(H8A,H8B), C0AA(H0AA,H0AB), C1(H1A,H1B), C82(H82A,H82B), C81(H81A,H81B),
 C66(H66A,H66B), C72(H72A,H72B), C89(H89A,H89B), C91(H91A,H91B)
4.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C43(H43),
 C42(H42), C41(H41), C40(H40), C39(H39), C46(H46), C47(H47), C48(H48), C55(H55),
  C54(H54), C53(H53), C21(H21), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C3(H3), C4(H4B),
 C5(H5), C12(H12), C11(H11), C10(H10), C80(H80), C73(H73), C74(H74), C75(H75),
 C76(H76), C77(H77), C2BA(H2BA), C84(H84), C4BA(H4BA), C65(H65), C58(H58),
 C59(H59), C60(H60), C61(H61), C62(H62), C68(H68), C69(H69), C70(H70), C94(H94),
  C95(H95), C96(H96), C97(H97), C98(H98), C100(H100), C101(H101), C102(H102),
 C103(H103), C104(H104), C106(H106), C107(H107), C108(H108), C109(H109),
 C110(H110), C112(H112), C113(H113), C114(H114), C115(H115), C116(H116),
 C118(H118), C119(H119), C120(H120), C121(H121), C122(H122), C124(H124),
 C125(H125), C126(H126), C127(H127), C128(H128), C130(H130), C131(H131),
 C132(H132), C133(H133), C134(H134), C136(H136), C137(H137), C138(H138),
 C139(H139), C140(H140), C142(H142), C143(H143), C144(H144), C145(H145),
 C146(H146), C148(H148), C149(H149), C150(H150), C151(H151), C152(H152),
 C154(H154), C155(H155), C156(H156), C157(H157), C158(H158), C160(H160),
 C161(H161), C162(H162), C163(H163), C164(H164)
4.d Fitted hexagon refined as free rotating group:
 C63(C58,C59,C60,C61,C62)
4.e Idealised Me refined as rotating group:
 C90(H90A,H90B,H90C), C92(H92A,H92B,H92C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Ni1A Ni 0.23907(2) 0.34823(3) 0.50092(4) 0.02749(18) Uani 1 1 d . . . . .
O2A O 0.27017(10) 0.28245(19) 0.5188(3) 0.0357(10) Uani 1 1 d . . . . .
O1A O 0.25474(10) 0.36452(19) 0.3860(3) 0.0327(10) Uani 1 1 d . . . . .
N1A N 0.21894(12) 0.3321(2) 0.6121(3) 0.0271(11) Uani 1 1 d . . . . .
N2A N 0.26306(12) 0.4147(2) 0.5841(3) 0.0293(11) Uani 1 1 d . . . . .
H2A H 0.285954 0.416129 0.572129 0.035 Uiso 1 1 calc R . . . .
N3A N 0.20845(12) 0.4157(2) 0.4851(3) 0.0274(11) Uani 1 1 d . . . . .
N4A N 0.19703(13) 0.3002(2) 0.4527(3) 0.0347(12) Uani 1 1 d . . . . .
H4A H 0.203223 0.268639 0.412455 0.042 Uiso 1 1 calc R . . . .
C37 C 0.29304(15) 0.2695(3) 0.4727(4) 0.0331(14) Uani 1 1 d . . . . .
C36 C 0.29758(16) 0.2959(3) 0.3932(4) 0.0340(15) Uani 1 1 d . . . . .
H36 H 0.314636 0.281647 0.362727 0.041 Uiso 1 1 calc R . . . .
C35 C 0.27916(14) 0.3413(3) 0.3554(4) 0.0300(13) Uani 1 1 d . . . . .
C34 C 0.28774(15) 0.3672(3) 0.2728(4) 0.0304(14) Uani 1 1 d . . . . .
C29 C 0.26354(16) 0.3869(3) 0.2147(4) 0.0348(15) Uani 1 1 d . . . . .
H29 H 0.242053 0.381673 0.226919 0.042 Uiso 1 1 calc R . . . .
C30 C 0.27068(17) 0.4142(3) 0.1390(4) 0.0417(16) Uani 1 1 d . . . . .
H30 H 0.254136 0.426693 0.099130 0.050 Uiso 1 1 calc R . . . .
C31 C 0.30267(17) 0.4232(3) 0.1218(4) 0.0356(15) Uani 1 1 d . . . . .
H31 H 0.307849 0.442256 0.070756 0.043 Uiso 1 1 calc R . . . .
C32 C 0.32624(16) 0.4038(3) 0.1801(4) 0.0334(14) Uani 1 1 d . . . . .
H32 H 0.347773 0.410132 0.169105 0.040 Uiso 1 1 calc R . . . .
C33 C 0.31925(15) 0.3756(3) 0.2539(4) 0.0296(13) Uani 1 1 d . . . . .
H33 H 0.335914 0.361707 0.292329 0.036 Uiso 1 1 calc R . . . .
C38 C 0.31542(18) 0.2233(4) 0.5077(5) 0.0499(15) Uani 1 1 d . U . . .
C43 C 0.30871(19) 0.1918(4) 0.5784(5) 0.0599(17) Uani 1 1 d . U . . .
H43 H 0.288731 0.197423 0.601275 0.072 Uiso 1 1 calc R . . . .
C42 C 0.3296(2) 0.1524(4) 0.6179(6) 0.0642(18) Uani 1 1 d . U . . .
H42 H 0.323952 0.132466 0.667795 0.077 Uiso 1 1 calc R . . . .
C41 C 0.3576(2) 0.1415(4) 0.5876(6) 0.0632(18) Uani 1 1 d . U . . .
H41 H 0.369944 0.108974 0.608697 0.076 Uiso 1 1 calc R . . . .
C40 C 0.3680(2) 0.1759(5) 0.5285(7) 0.080(2) Uani 1 1 d . U . . .
H40 H 0.389332 0.173225 0.513537 0.096 Uiso 1 1 calc R . . . .
C39 C 0.3471(2) 0.2167(4) 0.4878(6) 0.0749(19) Uani 1 1 d . U . . .
H39 H 0.354689 0.241092 0.444543 0.090 Uiso 1 1 calc R . . . .
C49 C 0.23000(13) 0.3601(3) 0.6815(3) 0.0260(12) Uani 1 1 d . . . . .
C50 C 0.26043(14) 0.3947(3) 0.6731(4) 0.0332(14) Uani 1 1 d . . . . .
H50A H 0.260791 0.429492 0.711452 0.040 Uiso 1 1 calc R . . . .
H50B H 0.278819 0.369381 0.690826 0.040 Uiso 1 1 calc R . . . .
C51 C 0.24857(16) 0.4730(3) 0.5635(4) 0.0374(15) Uani 1 1 d . . . . .
H51A H 0.261546 0.494041 0.523083 0.045 Uiso 1 1 calc R . . . .
H51B H 0.248531 0.496938 0.616182 0.045 Uiso 1 1 calc R . . . .
C52 C 0.21503(16) 0.4673(3) 0.5246(4) 0.0318(14) Uani 1 1 d . . . . .
C56 C 0.17980(17) 0.4043(3) 0.4479(4) 0.0387(16) Uani 1 1 d . . . . .
C57 C 0.17698(16) 0.3435(3) 0.4065(4) 0.0409(16) Uani 1 1 d . . . . .
H57A H 0.154654 0.330280 0.404962 0.049 Uiso 1 1 calc R . . . .
H57B H 0.183132 0.346238 0.347030 0.049 Uiso 1 1 calc R . . . .
C44 C 0.18190(17) 0.2724(3) 0.5255(4) 0.0373(16) Uani 1 1 d . . . . .
H44A H 0.187703 0.230012 0.528609 0.045 Uiso 1 1 calc R . . . .
H44B H 0.158595 0.275050 0.515295 0.045 Uiso 1 1 calc R . . . .
C45 C 0.19178(14) 0.3017(2) 0.6093(4) 0.0253(12) Uani 1 1 d . . . . .
C46 C 0.17494(14) 0.2960(3) 0.6812(4) 0.0264(13) Uani 1 1 d . . . . .
H46 H 0.155736 0.274110 0.679660 0.032 Uiso 1 1 calc R . . . .
C47 C 0.18706(15) 0.3234(3) 0.7563(4) 0.0307(13) Uani 1 1 d . . . . .
H47 H 0.176370 0.319591 0.807194 0.037 Uiso 1 1 calc R . . . .
C48 C 0.21448(13) 0.3560(3) 0.7561(4) 0.0285(13) Uani 1 1 d . . . . .
H48 H 0.222712 0.375368 0.806491 0.034 Uiso 1 1 calc R . . . .
C55 C 0.15580(19) 0.4454(3) 0.4472(5) 0.0477(19) Uani 1 1 d . . . . .
H55 H 0.135325 0.437480 0.421074 0.057 Uiso 1 1 calc R . . . .
C54 C 0.1632(2) 0.5001(4) 0.4873(5) 0.053(2) Uani 1 1 d . . . . .
H54 H 0.147309 0.529676 0.487891 0.064 Uiso 1 1 calc R . . . .
C53 C 0.19279(19) 0.5118(3) 0.5257(4) 0.0435(17) Uani 1 1 d . . . . .
H53 H 0.197646 0.548930 0.551685 0.052 Uiso 1 1 calc R . . . .
Ni1 Ni 0.26498(2) 0.22830(3) 0.03521(4) 0.02493(17) Uani 1 1 d . U . . .
O2 O 0.24977(9) 0.20613(17) 0.1489(3) 0.0285(9) Uani 1 1 d . . . . .
O1 O 0.23295(10) 0.29411(18) 0.0245(3) 0.0300(9) Uani 1 1 d . . . . .
N3 N 0.28469(11) 0.2530(2) -0.0725(3) 0.0255(10) Uani 1 1 d . . . . .
N4 N 0.30951(13) 0.2674(2) 0.0882(3) 0.0331(12) Uani 1 1 d . . . . .
H4 H 0.305028 0.297644 0.132097 0.040 Uiso 1 1 calc R . . . .
N1 N 0.29376(12) 0.1574(2) 0.0341(3) 0.0261(11) Uani 1 1 d . . . . .
N2 N 0.23891(12) 0.1736(2) -0.0594(3) 0.0291(11) Uani 1 1 d . . . . .
H2 H 0.216481 0.169990 -0.043801 0.035 Uiso 1 1 calc R . . . .
C22 C 0.22514(13) 0.2257(3) 0.1807(3) 0.0259(12) Uani 1 1 d . . . . .
C21 C 0.20479(14) 0.2699(3) 0.1451(4) 0.0281(13) Uani 1 1 d . . . . .
H21 H 0.186551 0.279478 0.174298 0.034 Uiso 1 1 calc R . . . .
C20 C 0.20952(14) 0.3007(3) 0.0698(4) 0.0251(12) Uani 1 1 d . . . . .
C19 C 0.18533(13) 0.3451(3) 0.0367(3) 0.0271(12) Uani 1 1 d . . . . .
C14 C 0.19319(16) 0.3879(3) -0.0210(4) 0.0336(14) Uani 1 1 d . . . . .
H14 H 0.214428 0.390652 -0.036565 0.040 Uiso 1 1 calc R . . . .
C15 C 0.17083(17) 0.4265(3) -0.0563(4) 0.0417(16) Uani 1 1 d . . . . .
H15 H 0.176772 0.455025 -0.096611 0.050 Uiso 1 1 calc R . . . .
C16 C 0.14039(17) 0.4245(3) -0.0342(5) 0.0443(17) Uani 1 1 d . . . . .
H16 H 0.125419 0.452630 -0.057018 0.053 Uiso 1 1 calc R . . . .
C17 C 0.13101(17) 0.3805(3) 0.0228(5) 0.0511(19) Uani 1 1 d . . . . .
H17 H 0.109536 0.377597 0.036358 0.061 Uiso 1 1 calc R . . . .
C18 C 0.15348(16) 0.3415(3) 0.0587(4) 0.0414(15) Uani 1 1 d . . . . .
H18 H 0.147505 0.312413 0.098146 0.050 Uiso 1 1 calc R . . . .
C23 C 0.21741(15) 0.1981(3) 0.2642(4) 0.0269(13) Uani 1 1 d . . . . .
C24 C 0.24147(15) 0.1787(3) 0.3210(4) 0.0312(14) Uani 1 1 d . . . . .
H24 H 0.262840 0.183904 0.307530 0.037 Uiso 1 1 calc R . . . .
C25 C 0.23524(16) 0.1521(3) 0.3967(4) 0.0318(14) Uani 1 1 d . . . . .
H25 H 0.252147 0.139746 0.435607 0.038 Uiso 1 1 calc R . . . .
C26 C 0.20420(16) 0.1434(3) 0.4157(4) 0.0354(15) Uani 1 1 d . . . . .
H26 H 0.199788 0.124741 0.467740 0.042 Uiso 1 1 calc R . . . .
C27 C 0.17935(16) 0.1617(3) 0.3593(4) 0.0331(14) Uani 1 1 d . . . . .
H27 H 0.158025 0.154846 0.371924 0.040 Uiso 1 1 calc R . . . .
C28 C 0.18605(15) 0.1902(3) 0.2839(4) 0.0295(13) Uani 1 1 d . . . . .
H28 H 0.169261 0.204288 0.245957 0.035 Uiso 1 1 calc R . . . .
C6 C 0.31383(14) 0.2777(2) -0.0678(4) 0.0258(13) Uani 1 1 d . . . . .
C7 C 0.32708(16) 0.2949(3) 0.0205(4) 0.0345(15) Uani 1 1 d . . . . .
H7A H 0.349582 0.282720 0.027737 0.041 Uiso 1 1 calc R . . . .
H7B H 0.326220 0.338456 0.026331 0.041 Uiso 1 1 calc R . . . .
C8 C 0.32665(15) 0.2160(3) 0.1297(4) 0.0361(15) Uani 1 1 d . . . . .
H8A H 0.317971 0.207509 0.185312 0.043 Uiso 1 1 calc R . . . .
H8B H 0.349408 0.225680 0.140171 0.043 Uiso 1 1 calc R . . . .
C9 C 0.32288(14) 0.1628(3) 0.0731(4) 0.0290(13) Uani 1 1 d . . . . .
C13 C 0.28651(14) 0.1133(3) -0.0197(4) 0.0300(13) Uani 1 1 d . . . . .
C0AA C 0.25345(15) 0.1133(3) -0.0593(4) 0.0339(14) Uani 1 1 d . . . . .
H0AA H 0.240398 0.085789 -0.027475 0.041 Uiso 1 1 calc R . . . .
H0AB H 0.253540 0.098782 -0.118684 0.041 Uiso 1 1 calc R . . . .
C1 C 0.23933(15) 0.2050(3) -0.1388(4) 0.0384(15) Uani 1 1 d . . . . .
H1A H 0.222328 0.235138 -0.142139 0.046 Uiso 1 1 calc R . . . .
H1B H 0.235155 0.176965 -0.186709 0.046 Uiso 1 1 calc R . . . .
C2 C 0.27092(14) 0.2348(3) -0.1470(4) 0.0328(14) Uani 1 1 d . . . . .
C3 C 0.28501(17) 0.2440(3) -0.2221(4) 0.0424(17) Uani 1 1 d . . . . .
H3 H 0.274660 0.232736 -0.275247 0.051 Uiso 1 1 calc R . . . .
C4 C 0.31535(17) 0.2706(3) -0.2182(4) 0.0429(17) Uani 1 1 d . . . . .
H4B H 0.325847 0.276900 -0.268916 0.051 Uiso 1 1 calc R . . . .
C5 C 0.32944(15) 0.2870(3) -0.1412(4) 0.0336(14) Uani 1 1 d . . . . .
H5 H 0.349825 0.304829 -0.137891 0.040 Uiso 1 1 calc R . . . .
C12 C 0.30901(16) 0.0714(3) -0.0364(4) 0.0381(15) Uani 1 1 d . . . . .
H12 H 0.303828 0.039670 -0.074458 0.046 Uiso 1 1 calc R . . . .
C11 C 0.33950(18) 0.0764(3) 0.0031(5) 0.0453(18) Uani 1 1 d . . . . .
H11 H 0.355290 0.048060 -0.008026 0.054 Uiso 1 1 calc R . . . .
C10 C 0.34647(15) 0.1225(3) 0.0584(4) 0.0369(15) Uani 1 1 d . . . . .
H10 H 0.367063 0.126548 0.085873 0.044 Uiso 1 1 calc R . . . .
Ni1C Ni 0.500000 0.61108(6) 0.500000 0.0380(3) Uani 1 2 d S T P . .
O1C O 0.50801(13) 0.6728(2) 0.4134(3) 0.0482(13) Uani 1 1 d . . . . .
N1C N 0.51130(13) 0.5475(3) 0.4194(3) 0.0397(14) Uani 1 1 d . . . . .
N2C N 0.54713(13) 0.5866(3) 0.5531(3) 0.0410(14) Uani 1 1 d . . . . .
H2C H 0.559752 0.623478 0.564649 0.049 Uiso 1 1 calc R . . . .
C79 C 0.50491(16) 0.7277(4) 0.4233(4) 0.0443(16) Uani 1 1 d . . . . .
C80 C 0.500000 0.7569(5) 0.500000 0.044(2) Uani 1 2 d S T P . .
H80 H 0.500002 0.798973 0.500001 0.053 Uiso 1 2 calc RS T P . .
C78 C 0.50562(18) 0.7639(3) 0.3430(5) 0.0495(19) Uani 1 1 d . . . . .
C73 C 0.5226(2) 0.7428(4) 0.2780(5) 0.059(2) Uani 1 1 d . . . . .
H73 H 0.533201 0.705823 0.283385 0.070 Uiso 1 1 calc R . . . .
C74 C 0.5239(2) 0.7766(5) 0.2034(6) 0.076(3) Uani 1 1 d . . . . .
H74 H 0.536044 0.762687 0.158879 0.092 Uiso 1 1 calc R . . . .
C75 C 0.5084(2) 0.8284(5) 0.1940(7) 0.083(3) Uani 1 1 d . . . . .
H75 H 0.509374 0.850368 0.142729 0.099 Uiso 1 1 calc R . . . .
C76 C 0.4912(3) 0.8494(5) 0.2580(7) 0.084(3) Uani 1 1 d . . . . .
H76 H 0.480043 0.885818 0.251536 0.100 Uiso 1 1 calc R . . . .
C77 C 0.4902(3) 0.8176(4) 0.3310(7) 0.077(3) Uani 1 1 d . . . . .
H77 H 0.478568 0.832738 0.375630 0.093 Uiso 1 1 calc R . . . .
C83 C 0.54030(15) 0.5207(3) 0.4279(4) 0.0368(16) Uani 1 1 d . . . . .
C82 C 0.56305(16) 0.5504(3) 0.4907(4) 0.0409(17) Uani 1 1 d . . . . .
H82A H 0.576145 0.519875 0.521597 0.049 Uiso 1 1 calc R . . . .
H82B H 0.577388 0.575937 0.459783 0.049 Uiso 1 1 calc R . . . .
C81 C 0.54249(18) 0.5572(4) 0.6346(4) 0.053(2) Uani 1 1 d . . . . .
H81A H 0.543521 0.587191 0.680546 0.064 Uiso 1 1 calc R . . . .
H81B H 0.559996 0.528731 0.647163 0.064 Uiso 1 1 calc R . . . .
C2BA C 0.54622(18) 0.4717(4) 0.3792(5) 0.0477(18) Uani 1 1 d . . . . .
H2BA H 0.566426 0.453294 0.385340 0.057 Uiso 1 1 calc R . . . .
C84 C 0.52377(18) 0.4495(4) 0.3229(5) 0.059(2) Uani 1 1 d . . . . .
H84 H 0.528128 0.416023 0.289079 0.070 Uiso 1 1 calc R . . . .
C4BA C 0.49380(19) 0.4767(4) 0.3152(5) 0.058(2) Uani 1 1 d . . . . .
H4BA H 0.477627 0.461776 0.276069 0.070 Uiso 1 1 calc R . . . .
C85 C 0.48817(16) 0.5251(4) 0.3650(4) 0.0430(17) Uani 1 1 d . . . . .
Ni1B Ni 0.500000 0.46733(4) 0.000000 0.0254(2) Uani 1 2 d S T P . .
O1B O 0.49346(11) 0.4056(2) 0.0885(3) 0.0474(12) Uani 1 1 d . U . . .
N1B N 0.48960(11) 0.5328(2) 0.0806(3) 0.0234(10) Uani 1 1 d . . . . .
N2B N 0.54759(12) 0.4913(2) 0.0517(3) 0.0270(11) Uani 1 1 d . . . . .
H2B H 0.560248 0.454518 0.063805 0.032 Uiso 1 1 calc R . . . .
C64 C 0.49637(16) 0.3503(4) 0.0779(6) 0.0574(15) Uani 1 1 d . U . . .
C65 C 0.500000 0.3221(5) 0.000000 0.059(2) Uani 1 2 d S TU P . .
H65 H 0.499999 0.280037 -0.000001 0.071 Uiso 1 2 calc RS T P . .
C63 C 0.49606(14) 0.3115(2) 0.1542(4) 0.0749(19) Uani 1 1 d . U . . .
C58 C 0.51194(14) 0.2576(3) 0.1598(4) 0.092(2) Uani 1 1 d G U . . .
H58 H 0.523303 0.244166 0.113463 0.110 Uiso 1 1 calc R . . . .
C59 C 0.51119(15) 0.2235(2) 0.2331(5) 0.103(2) Uani 1 1 d G U . . .
H59 H 0.522040 0.186677 0.236960 0.123 Uiso 1 1 calc R . . . .
C60 C 0.49456(16) 0.2432(3) 0.3009(4) 0.099(2) Uani 1 1 d G U . . .
H60 H 0.494044 0.219835 0.351012 0.118 Uiso 1 1 calc R . . . .
C61 C 0.47868(15) 0.2970(3) 0.2953(4) 0.096(2) Uani 1 1 d G U . . .
H61 H 0.467310 0.310481 0.341569 0.115 Uiso 1 1 calc R . . . .
C62 C 0.47943(14) 0.3312(2) 0.2219(4) 0.084(2) Uani 1 1 d G U . . .
H62 H 0.468573 0.367971 0.218073 0.100 Uiso 1 1 calc R . . . .
C67 C 0.51253(14) 0.5558(3) 0.1307(4) 0.0314(14) Uani 1 1 d . . . . .
C66 C 0.54398(14) 0.5234(3) 0.1320(4) 0.0386(16) Uani 1 1 d . . . . .
H66A H 0.561493 0.552168 0.141404 0.046 Uiso 1 1 calc R . . . .
H66B H 0.545385 0.494931 0.180033 0.046 Uiso 1 1 calc R . . . .
C72 C 0.56294(14) 0.5273(3) -0.0118(4) 0.0285(13) Uani 1 1 d . . . . .
H72A H 0.576553 0.501438 -0.044571 0.034 Uiso 1 1 calc R . . . .
H72B H 0.576676 0.557232 0.018146 0.034 Uiso 1 1 calc R . . . .
C68 C 0.50746(17) 0.6046(4) 0.1798(5) 0.051(2) Uani 1 1 d . . . . .
H68 H 0.524065 0.620715 0.216467 0.061 Uiso 1 1 calc R . . . .
C69 C 0.47815(18) 0.6294(4) 0.1748(5) 0.059(2) Uani 1 1 d . . . . .
H69 H 0.473902 0.662270 0.209864 0.070 Uiso 1 1 calc R . . . .
C70 C 0.45435(16) 0.6068(3) 0.1187(5) 0.0453(18) Uani 1 1 d . . . . .
H70 H 0.434104 0.625099 0.112948 0.054 Uiso 1 1 calc R . . . .
C71 C 0.46066(14) 0.5579(3) 0.0723(4) 0.0293(13) Uani 1 1 d . . . . .
O7 O 0.59752(18) 0.8549(4) 0.4195(5) 0.106(2) Uani 1 1 d . U . . .
C89 C 0.5790(3) 0.8769(6) 0.4877(8) 0.101(3) Uani 1 1 d . U . . .
H89A H 0.559272 0.853628 0.489382 0.121 Uiso 1 1 calc R . . . .
H89B H 0.573156 0.918759 0.476473 0.121 Uiso 1 1 calc R . . . .
C90 C 0.5978(3) 0.8723(5) 0.5723(7) 0.093(3) Uani 1 1 d . U . . .
H90A H 0.616859 0.896923 0.571495 0.140 Uiso 1 1 calc GR . . . .
H90B H 0.603994 0.831001 0.582798 0.140 Uiso 1 1 calc GR . . . .
H90C H 0.584852 0.885942 0.617721 0.140 Uiso 1 1 calc GR . . . .
C91 C 0.5800(3) 0.8619(7) 0.3370(8) 0.112(3) Uani 1 1 d . U . . .
H91A H 0.576550 0.904288 0.323522 0.135 Uiso 1 1 calc R . . . .
H91B H 0.559153 0.841930 0.336717 0.135 Uiso 1 1 calc R . . . .
C92 C 0.6000(3) 0.8341(8) 0.2752(9) 0.136(4) Uani 1 1 d . U . . .
H92A H 0.589333 0.836595 0.217940 0.204 Uiso 1 1 calc GR . . . .
H92B H 0.603507 0.792431 0.290453 0.204 Uiso 1 1 calc GR . . . .
H92C H 0.620367 0.854670 0.276085 0.204 Uiso 1 1 calc GR . . . .
C93 C 0.31851(13) 0.4895(2) 0.8199(3) 0.0207(12) Uani 1 1 d . . . . .
C94 C 0.30408(13) 0.4431(2) 0.8622(3) 0.0225(12) Uani 1 1 d . . . . .
H94 H 0.315294 0.406824 0.869490 0.027 Uiso 1 1 calc R . . . .
C95 C 0.27419(13) 0.4472(3) 0.8941(3) 0.0285(13) Uani 1 1 d . . . . .
H95 H 0.265750 0.415080 0.924317 0.034 Uiso 1 1 calc R . . . .
C96 C 0.25699(14) 0.4993(3) 0.8809(4) 0.0300(14) Uani 1 1 d . . . . .
H96 H 0.236471 0.502934 0.901307 0.036 Uiso 1 1 calc R . . . .
C97 C 0.26990(14) 0.5454(3) 0.8381(4) 0.0294(13) Uani 1 1 d . . . . .
H97 H 0.258277 0.581063 0.828932 0.035 Uiso 1 1 calc R . . . .
C98 C 0.29982(13) 0.5400(3) 0.8081(3) 0.0263(13) Uani 1 1 d . . . . .
H98 H 0.307999 0.572446 0.778089 0.032 Uiso 1 1 calc R . . . .
C99 C 0.37285(13) 0.5452(3) 0.7805(3) 0.0224(12) Uani 1 1 d . . . . .
C100 C 0.39161(13) 0.5638(3) 0.7156(3) 0.0238(12) Uani 1 1 d . . . . .
H100 H 0.393264 0.538708 0.667656 0.029 Uiso 1 1 calc R . . . .
C101 C 0.40776(14) 0.6167(3) 0.7178(4) 0.0301(14) Uani 1 1 d . . . . .
H101 H 0.420335 0.627097 0.672323 0.036 Uiso 1 1 calc R . . . .
C102 C 0.40568(14) 0.6552(3) 0.7871(4) 0.0310(14) Uani 1 1 d . . . . .
H102 H 0.415942 0.692600 0.787853 0.037 Uiso 1 1 calc R . . . .
C103 C 0.38852(14) 0.6379(3) 0.8537(4) 0.0307(14) Uani 1 1 d . . . . .
H103 H 0.387470 0.662745 0.902127 0.037 Uiso 1 1 calc R . . . .
C104 C 0.37257(14) 0.5836(3) 0.8505(4) 0.0259(12) Uani 1 1 d . . . . .
H104 H 0.361062 0.572286 0.897632 0.031 Uiso 1 1 calc R . . . .
C105 C 0.37617(13) 0.4367(3) 0.8411(3) 0.0239(12) Uani 1 1 d . . . . .
C106 C 0.40052(14) 0.4027(3) 0.8094(4) 0.0279(13) Uani 1 1 d . . . . .
H106 H 0.404004 0.405338 0.750516 0.034 Uiso 1 1 calc R . . . .
C107 C 0.41960(15) 0.3655(3) 0.8602(4) 0.0347(15) Uani 1 1 d . . . . .
H107 H 0.435680 0.343325 0.835415 0.042 Uiso 1 1 calc R . . . .
C108 C 0.41577(15) 0.3600(3) 0.9454(4) 0.0366(16) Uani 1 1 d . . . . .
H108 H 0.428500 0.333143 0.979381 0.044 Uiso 1 1 calc R . . . .
C109 C 0.39300(15) 0.3942(3) 0.9815(4) 0.0327(15) Uani 1 1 d . . . . .
H109 H 0.390502 0.391854 1.040986 0.039 Uiso 1 1 calc R . . . .
C110 C 0.37369(13) 0.4321(3) 0.9302(4) 0.0250(12) Uani 1 1 d . . . . .
H110 H 0.358396 0.455606 0.956046 0.030 Uiso 1 1 calc R . . . .
C111 C 0.34634(13) 0.4578(2) 0.6839(3) 0.0214(12) Uani 1 1 d . . . . .
C112 C 0.33515(13) 0.4985(3) 0.6198(3) 0.0235(12) Uani 1 1 d . . . . .
H112 H 0.331925 0.538585 0.635408 0.028 Uiso 1 1 calc R . . . .
C113 C 0.32876(15) 0.4822(3) 0.5353(4) 0.0311(14) Uani 1 1 d . . . . .
H113 H 0.321895 0.511044 0.494086 0.037 Uiso 1 1 calc R . . . .
C114 C 0.33243(15) 0.4235(3) 0.5108(4) 0.0368(16) Uani 1 1 d . . . . .
H114 H 0.328318 0.412052 0.452956 0.044 Uiso 1 1 calc R . . . .
C115 C 0.34206(15) 0.3822(3) 0.5715(4) 0.0344(15) Uani 1 1 d . . . . .
H115 H 0.344252 0.341899 0.555795 0.041 Uiso 1 1 calc R . . . .
C116 C 0.34863(14) 0.3994(3) 0.6561(4) 0.0276(13) Uani 1 1 d . . . . .
H116 H 0.354977 0.369943 0.696771 0.033 Uiso 1 1 calc R . . . .
B1 B 0.35379(16) 0.4818(3) 0.7815(4) 0.0237(14) Uani 1 1 d . . . . .
C117 C 0.62467(14) 0.6411(3) 0.6642(4) 0.0301(14) Uani 1 1 d . . . . .
C118 C 0.59898(15) 0.6720(3) 0.6947(4) 0.0364(15) Uani 1 1 d . . . . .
H118 H 0.594468 0.667589 0.752739 0.044 Uiso 1 1 calc R . . . .
C119 C 0.57992(17) 0.7090(3) 0.6419(5) 0.0474(19) Uani 1 1 d . . . . .
H119 H 0.562880 0.729646 0.664743 0.057 Uiso 1 1 calc R . . . .
C120 C 0.58544(18) 0.7162(4) 0.5568(5) 0.052(2) Uani 1 1 d . . . . .
H120 H 0.572753 0.742342 0.521574 0.063 Uiso 1 1 calc R . . . .
C121 C 0.60997(16) 0.6843(4) 0.5237(5) 0.0458(19) Uani 1 1 d . . . . .
H121 H 0.613726 0.687189 0.464958 0.055 Uiso 1 1 calc R . . . .
C122 C 0.62859(15) 0.6487(3) 0.5769(4) 0.0347(15) Uani 1 1 d . . . . .
H122 H 0.645307 0.627692 0.553069 0.042 Uiso 1 1 calc R . . . .
C123 C 0.62665(13) 0.5331(3) 0.7220(3) 0.0231(12) Uani 1 1 d . . . . .
C124 C 0.62571(14) 0.4972(3) 0.6488(4) 0.0281(13) Uani 1 1 d . . . . .
H124 H 0.637525 0.509323 0.602573 0.034 Uiso 1 1 calc R . . . .
C125 C 0.60846(14) 0.4452(3) 0.6405(4) 0.0317(14) Uani 1 1 d . . . . .
H125 H 0.609034 0.422277 0.590040 0.038 Uiso 1 1 calc R . . . .
C126 C 0.59012(15) 0.4263(3) 0.7064(4) 0.0323(14) Uani 1 1 d . . . . .
H126 H 0.578008 0.390965 0.700951 0.039 Uiso 1 1 calc R . . . .
C127 C 0.59013(14) 0.4605(3) 0.7795(4) 0.0315(14) Uani 1 1 d . . . . .
H127 H 0.578119 0.448036 0.825157 0.038 Uiso 1 1 calc R . . . .
C128 C 0.60761(14) 0.5133(3) 0.7873(3) 0.0269(13) Uani 1 1 d . . . . .
H128 H 0.606684 0.536355 0.837608 0.032 Uiso 1 1 calc R . . . .
C129 C 0.68178(14) 0.5882(3) 0.6889(3) 0.0252(13) Uani 1 1 d . . . . .
C130 C 0.69834(14) 0.6380(3) 0.6639(3) 0.0267(13) Uani 1 1 d . . . . .
H130 H 0.688449 0.675708 0.665849 0.032 Uiso 1 1 calc R . . . .
C131 C 0.72867(15) 0.6344(3) 0.6365(4) 0.0313(14) Uani 1 1 d . . . . .
H131 H 0.738909 0.669496 0.619631 0.038 Uiso 1 1 calc R . . . .
C132 C 0.74428(15) 0.5814(3) 0.6332(4) 0.0342(15) Uani 1 1 d . . . . .
H132 H 0.764964 0.579437 0.613437 0.041 Uiso 1 1 calc R . . . .
C133 C 0.72904(15) 0.5301(3) 0.6596(4) 0.0332(14) Uani 1 1 d . . . . .
H133 H 0.739558 0.492976 0.659121 0.040 Uiso 1 1 calc R . . . .
C134 C 0.69846(14) 0.5338(3) 0.6866(4) 0.0300(13) Uani 1 1 d . . . . .
H134 H 0.688408 0.498730 0.704144 0.036 Uiso 1 1 calc R . . . .
C135 C 0.65360(13) 0.6181(3) 0.8236(3) 0.0240(12) Uani 1 1 d . . . . .
C136 C 0.66574(14) 0.5778(3) 0.8853(3) 0.0271(13) Uani 1 1 d . . . . .
H136 H 0.669182 0.538128 0.868343 0.032 Uiso 1 1 calc R . . . .
C137 C 0.67294(14) 0.5930(3) 0.9692(4) 0.0305(14) Uani 1 1 d . . . . .
H137 H 0.680797 0.563958 1.008911 0.037 Uiso 1 1 calc R . . . .
C138 C 0.66868(15) 0.6511(3) 0.9957(4) 0.0341(15) Uani 1 1 d . . . . .
H138 H 0.673210 0.661822 1.053702 0.041 Uiso 1 1 calc R . . . .
C139 C 0.65770(16) 0.6930(3) 0.9363(4) 0.0395(17) Uani 1 1 d . . . . .
H139 H 0.655155 0.732875 0.953517 0.047 Uiso 1 1 calc R . . . .
C140 C 0.65040(15) 0.6771(3) 0.8518(4) 0.0315(14) Uani 1 1 d . . . . .
H140 H 0.643102 0.706601 0.812091 0.038 Uiso 1 1 calc R . . . .
B2 B 0.64657(16) 0.5954(3) 0.7257(4) 0.0241(14) Uani 1 1 d . . . . .
C141 C 0.57541(14) 0.0974(3) 0.6049(4) 0.0357(14) Uani 1 1 d . . . . .
C142 C 0.58422(15) 0.0542(3) 0.5474(4) 0.0384(15) Uani 1 1 d . . . . .
H142 H 0.597568 0.022817 0.567996 0.046 Uiso 1 1 calc R . . . .
C143 C 0.57430(16) 0.0555(3) 0.4619(5) 0.0436(16) Uani 1 1 d . . . . .
H143 H 0.581445 0.025727 0.425073 0.052 Uiso 1 1 calc R . . . .
C144 C 0.55446(17) 0.0985(3) 0.4295(5) 0.0466(18) Uani 1 1 d . . . . .
H144 H 0.547783 0.098975 0.370569 0.056 Uiso 1 1 calc R . . . .
C145 C 0.54409(18) 0.1419(4) 0.4838(5) 0.054(2) Uani 1 1 d . . . . .
H145 H 0.529950 0.172046 0.462877 0.065 Uiso 1 1 calc R . . . .
C146 C 0.55492(16) 0.1403(3) 0.5700(5) 0.0469(17) Uani 1 1 d . . . . .
H146 H 0.547862 0.170284 0.606649 0.056 Uiso 1 1 calc R . . . .
C147 C 0.62295(15) 0.0651(3) 0.7189(4) 0.0328(14) Uani 1 1 d . . . . .
C148 C 0.65091(17) 0.0962(3) 0.7268(4) 0.0405(16) Uani 1 1 d . . . . .
H148 H 0.649876 0.138205 0.726008 0.049 Uiso 1 1 calc R . . . .
C149 C 0.68007(16) 0.0703(3) 0.7358(4) 0.0426(16) Uani 1 1 d . . . . .
H149 H 0.698531 0.094191 0.742522 0.051 Uiso 1 1 calc R . . . .
C150 C 0.68289(17) 0.0086(3) 0.7351(4) 0.0416(16) Uani 1 1 d . . . . .
H150 H 0.703083 -0.009946 0.740560 0.050 Uiso 1 1 calc R . . . .
C151 C 0.65575(18) -0.0243(3) 0.7263(5) 0.0490(18) Uani 1 1 d . . . . .
H151 H 0.656865 -0.066289 0.724559 0.059 Uiso 1 1 calc R . . . .
C152 C 0.62597(17) 0.0045(3) 0.7196(4) 0.0417(16) Uani 1 1 d . . . . .
H152 H 0.607307 -0.018976 0.715551 0.050 Uiso 1 1 calc R . . . .
C153 C 0.58925(14) 0.1646(3) 0.7454(4) 0.0327(14) Uani 1 1 d . . . . .
C154 C 0.60241(16) 0.2112(3) 0.6996(4) 0.0384(15) Uani 1 1 d . . . . .
H154 H 0.609368 0.202943 0.644635 0.046 Uiso 1 1 calc R . . . .
C155 C 0.60568(16) 0.2684(3) 0.7308(5) 0.0429(17) Uani 1 1 d . . . . .
H155 H 0.614525 0.298367 0.697330 0.051 Uiso 1 1 calc R . . . .
C156 C 0.59597(18) 0.2818(3) 0.8114(5) 0.0490(19) Uani 1 1 d . . . . .
H156 H 0.598002 0.320908 0.833328 0.059 Uiso 1 1 calc R . . . .
C157 C 0.58375(17) 0.2389(4) 0.8574(5) 0.051(2) Uani 1 1 d . . . . .
H157 H 0.577534 0.247876 0.912873 0.062 Uiso 1 1 calc R . . . .
C158 C 0.57970(17) 0.1794(3) 0.8254(4) 0.0426(16) Uani 1 1 d . . . . .
H158 H 0.570450 0.150120 0.859285 0.051 Uiso 1 1 calc R . . . .
C159 C 0.56163(16) 0.0596(3) 0.7599(4) 0.0418(16) Uani 1 1 d . . . . .
C160 C 0.5703(2) 0.0304(4) 0.8383(5) 0.057(2) Uani 1 1 d . . . . .
H160 H 0.591883 0.030729 0.859025 0.068 Uiso 1 1 calc R . . . .
C161 C 0.5488(3) 0.0020(4) 0.8853(7) 0.078(3) Uani 1 1 d . . . . .
H161 H 0.555725 -0.016346 0.937645 0.094 Uiso 1 1 calc R . . . .
C162 C 0.5163(3) -0.0004(5) 0.8564(7) 0.077(3) Uani 1 1 d . . . . .
H162 H 0.501286 -0.020707 0.887773 0.092 Uiso 1 1 calc R . . . .
C163 C 0.5076(2) 0.0278(5) 0.7814(7) 0.083(3) Uani 1 1 d . . . . .
H163 H 0.485989 0.027339 0.760076 0.100 Uiso 1 1 calc R . . . .
C164 C 0.52951(19) 0.0567(4) 0.7367(5) 0.062(2) Uani 1 1 d . . . . .
H164 H 0.522118 0.076362 0.685713 0.074 Uiso 1 1 calc R . . . .
B3 B 0.58684(18) 0.0966(3) 0.7077(5) 0.0341(16) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Ni1A O2A 1.993(5) . ?
Ni1A O1A 2.001(4) . ?
Ni1A N1A 2.029(5) . ?
Ni1A N2A 2.195(5) . ?
Ni1A N3A 2.005(5) . ?
Ni1A N4A 2.175(5) . ?
O2A C37 1.282(7) . ?
O1A C35 1.282(7) . ?
N1A C49 1.320(7) . ?
N1A C45 1.338(7) . ?
N2A C50 1.483(8) . ?
N2A C51 1.478(9) . ?
N3A C52 1.343(8) . ?
N3A C56 1.335(8) . ?
N4A C57 1.457(9) . ?
N4A C44 1.487(8) . ?
C37 C36 1.411(9) . ?
C37 C38 1.488(10) . ?
C36 C35 1.396(9) . ?
C35 C34 1.492(8) . ?
C34 C29 1.397(9) . ?
C34 C33 1.399(8) . ?
C29 C30 1.391(9) . ?
C30 C31 1.414(10) . ?
C31 C32 1.379(10) . ?
C32 C33 1.373(9) . ?
C38 C43 1.367(10) . ?
C38 C39 1.404(11) . ?
C43 C42 1.372(11) . ?
C42 C41 1.328(11) . ?
C41 C40 1.311(12) . ?
C40 C39 1.401(12) . ?
C49 C50 1.520(8) . ?
C49 C48 1.386(8) . ?
C51 C52 1.511(9) . ?
C52 C53 1.377(10) . ?
C56 C57 1.521(10) . ?
C56 C55 1.376(10) . ?
C44 C45 1.507(8) . ?
C45 C46 1.384(8) . ?
C46 C47 1.399(8) . ?
C47 C48 1.374(8) . ?
C55 C54 1.412(11) . ?
C54 C53 1.376(11) . ?
Ni1 O2 2.005(4) . ?
Ni1 O1 2.012(4) . ?
Ni1 N3 2.018(5) . ?
Ni1 N4 2.192(5) . ?
Ni1 N1 2.013(5) . ?
Ni1 N2 2.176(5) . ?
O2 C22 1.267(7) . ?
O1 C20 1.269(7) . ?
N3 C6 1.350(8) . ?
N3 C2 1.337(8) . ?
N4 C7 1.477(8) . ?
N4 C8 1.495(8) . ?
N1 C9 1.343(8) . ?
N1 C13 1.330(7) . ?
N2 C0AA 1.495(8) . ?
N2 C1 1.437(8) . ?
C22 C21 1.409(8) . ?
C22 C23 1.510(8) . ?
C21 C20 1.399(8) . ?
C20 C19 1.500(8) . ?
C19 C14 1.383(8) . ?
C19 C18 1.417(8) . ?
C14 C15 1.376(9) . ?
C15 C16 1.358(10) . ?
C16 C17 1.415(10) . ?
C17 C18 1.387(9) . ?
C23 C24 1.378(9) . ?
C23 C28 1.395(9) . ?
C24 C25 1.377(9) . ?
C25 C26 1.381(9) . ?
C26 C27 1.391(9) . ?
C27 C28 1.396(9) . ?
C6 C7 1.510(9) . ?
C6 C5 1.385(8) . ?
C8 C9 1.498(9) . ?
C9 C10 1.383(9) . ?
C13 C0AA 1.491(9) . ?
C13 C12 1.380(9) . ?
C1 C2 1.511(9) . ?
C2 C3 1.375(9) . ?
C3 C4 1.415(10) . ?
C4 C5 1.364(9) . ?
C12 C11 1.398(10) . ?
C11 C10 1.376(10) . ?
Ni1C O1C 1.994(5) . ?
Ni1C O1C 1.995(5) 2_656 ?
Ni1C N1C 1.996(6) . ?
Ni1C N1C 1.996(6) 2_656 ?
Ni1C N2C 2.180(5) 2_656 ?
Ni1C N2C 2.180(5) . ?
O1C C79 1.257(9) . ?
N1C C83 1.367(9) . ?
N1C C85 1.353(9) . ?
N2C C82 1.475(9) . ?
N2C C81 1.469(8) . ?
C79 C80 1.403(9) . ?
C79 C78 1.508(10) . ?
C80 C79 1.403(9) 2_656 ?
C78 C73 1.374(11) . ?
C78 C77 1.383(11) . ?
C73 C74 1.403(12) . ?
C74 C75 1.345(14) . ?
C75 C76 1.369(15) . ?
C76 C77 1.357(13) . ?
C83 C82 1.490(9) . ?
C83 C2BA 1.379(10) . ?
C81 C85 1.487(10) 2_656 ?
C2BA C84 1.349(11) . ?
C84 C4BA 1.407(11) . ?
C4BA C85 1.376(11) . ?
C85 C81 1.486(10) 2_656 ?
Ni1B O1B 2.002(5) . ?
Ni1B O1B 2.002(5) 2_655 ?
Ni1B N1B 2.016(5) . ?
Ni1B N1B 2.017(5) 2_655 ?
Ni1B N2B 2.187(5) . ?
Ni1B N2B 2.187(5) 2_655 ?
O1B C64 1.268(10) . ?
N1B C67 1.314(8) . ?
N1B C71 1.349(8) . ?
N2B C66 1.473(8) . ?
N2B C72 1.472(8) . ?
C64 C65 1.400(11) . ?
C64 C63 1.486(9) . ?
C65 C64 1.400(11) 2_655 ?
C63 C58 1.3900 . ?
C63 C62 1.3900 . ?
C58 C59 1.3900 . ?
C59 C60 1.3900 . ?
C60 C61 1.3900 . ?
C61 C62 1.3900 . ?
C67 C66 1.519(8) . ?
C67 C68 1.371(9) . ?
C72 C71 1.501(9) 2_655 ?
C68 C69 1.358(11) . ?
C69 C70 1.389(10) . ?
C70 C71 1.361(9) . ?
C71 C72 1.500(9) 2_655 ?
O7 C89 1.458(13) . ?
O7 C91 1.457(14) . ?
C89 C90 1.505(15) . ?
C91 C92 1.473(18) . ?
C93 C94 1.405(8) . ?
C93 C98 1.394(8) . ?
C93 B1 1.658(8) . ?
C94 C95 1.396(8) . ?
C95 C96 1.392(9) . ?
C96 C97 1.374(9) . ?
C97 C98 1.386(8) . ?
C99 C100 1.400(8) . ?
C99 C104 1.402(8) . ?
C99 B1 1.645(8) . ?
C100 C101 1.376(8) . ?
C101 C102 1.402(9) . ?
C102 C103 1.373(9) . ?
C103 C104 1.399(8) . ?
C105 C106 1.405(8) . ?
C105 C110 1.414(8) . ?
C105 B1 1.640(8) . ?
C106 C107 1.380(9) . ?
C107 C108 1.367(10) . ?
C108 C109 1.387(10) . ?
C109 C110 1.402(8) . ?
C111 C112 1.422(8) . ?
C111 C116 1.396(8) . ?
C111 B1 1.637(8) . ?
C112 C113 1.387(8) . ?
C113 C114 1.394(9) . ?
C114 C115 1.376(10) . ?
C115 C116 1.395(8) . ?
C117 C118 1.404(9) . ?
C117 C122 1.405(9) . ?
C117 B2 1.655(8) . ?
C118 C119 1.396(9) . ?
C119 C120 1.384(11) . ?
C120 C121 1.394(11) . ?
C121 C122 1.369(9) . ?
C123 C124 1.406(8) . ?
C123 C128 1.421(8) . ?
C123 B2 1.640(9) . ?
C124 C125 1.385(9) . ?
C125 C126 1.403(9) . ?
C126 C127 1.386(9) . ?
C127 C128 1.405(9) . ?
C129 C130 1.397(8) . ?
C129 C134 1.419(9) . ?
C129 B2 1.643(9) . ?
C130 C131 1.385(9) . ?
C131 C132 1.371(9) . ?
C132 C133 1.404(9) . ?
C133 C134 1.392(9) . ?
C135 C136 1.400(8) . ?
C135 C140 1.416(8) . ?
C135 B2 1.630(8) . ?
C136 C137 1.377(8) . ?
C137 C138 1.392(9) . ?
C138 C139 1.388(10) . ?
C139 C140 1.389(9) . ?
C141 C142 1.398(9) . ?
C141 C146 1.389(9) . ?
C141 B3 1.655(9) . ?
C142 C143 1.380(9) . ?
C143 C144 1.362(10) . ?
C144 C145 1.391(11) . ?
C145 C146 1.401(10) . ?
C147 C148 1.374(10) . ?
C147 C152 1.376(9) . ?
C147 B3 1.684(9) . ?
C148 C149 1.365(9) . ?
C149 C150 1.400(10) . ?
C150 C151 1.367(10) . ?
C151 C152 1.416(10) . ?
C153 C154 1.413(9) . ?
C153 C158 1.388(9) . ?
C153 B3 1.647(9) . ?
C154 C155 1.387(9) . ?
C155 C156 1.392(10) . ?
C156 C157 1.335(11) . ?
C157 C158 1.443(10) . ?
C159 C160 1.422(10) . ?
C159 C164 1.384(10) . ?
C159 B3 1.623(10) . ?
C160 C161 1.370(12) . ?
C161 C162 1.418(15) . ?
C162 C163 1.370(14) . ?
C163 C164 1.369(12) . ?

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
O2A Ni1A O1A 90.42(17) . . ?
O2A Ni1A N1A 93.30(18) . . ?
O2A Ni1A N2A 98.82(19) . . ?
O2A Ni1A N3A 178.5(2) . . ?
O2A Ni1A N4A 101.11(19) . . ?
O1A Ni1A N1A 174.55(19) . . ?
O1A Ni1A N2A 104.07(18) . . ?
O1A Ni1A N3A 90.00(18) . . ?
O1A Ni1A N4A 95.26(18) . . ?
N1A Ni1A N2A 79.30(19) . . ?
N1A Ni1A N4A 80.13(19) . . ?
N3A Ni1A N1A 86.37(19) . . ?
N3A Ni1A N2A 79.7(2) . . ?
N3A Ni1A N4A 80.3(2) . . ?
N4A Ni1A N2A 152.0(2) . . ?
C37 O2A Ni1A 127.4(4) . . ?
C35 O1A Ni1A 126.2(4) . . ?
C49 N1A Ni1A 118.7(4) . . ?
C49 N1A C45 121.9(5) . . ?
C45 N1A Ni1A 118.4(4) . . ?
C50 N2A Ni1A 106.9(4) . . ?
C51 N2A Ni1A 108.2(4) . . ?
C51 N2A C50 114.9(5) . . ?
C52 N3A Ni1A 119.5(4) . . ?
C56 N3A Ni1A 117.9(4) . . ?
C56 N3A C52 121.6(6) . . ?
C57 N4A Ni1A 105.7(4) . . ?
C57 N4A C44 113.6(5) . . ?
C44 N4A Ni1A 109.1(4) . . ?
O2A C37 C36 123.9(6) . . ?
O2A C37 C38 115.9(6) . . ?
C36 C37 C38 120.2(6) . . ?
C35 C36 C37 125.6(6) . . ?
O1A C35 C36 125.5(5) . . ?
O1A C35 C34 114.7(6) . . ?
C36 C35 C34 119.7(5) . . ?
C29 C34 C35 118.9(6) . . ?
C29 C34 C33 119.0(6) . . ?
C33 C34 C35 122.1(6) . . ?
C30 C29 C34 120.5(6) . . ?
C29 C30 C31 119.7(6) . . ?
C32 C31 C30 119.0(6) . . ?
C33 C32 C31 121.4(6) . . ?
C32 C33 C34 120.4(6) . . ?
C43 C38 C37 120.2(6) . . ?
C43 C38 C39 112.3(7) . . ?
C39 C38 C37 125.8(7) . . ?
C38 C43 C42 122.8(7) . . ?
C41 C42 C43 121.3(8) . . ?
C40 C41 C42 119.8(9) . . ?
C41 C40 C39 118.6(9) . . ?
C40 C39 C38 123.5(8) . . ?
N1A C49 C50 115.4(5) . . ?
N1A C49 C48 120.4(5) . . ?
C48 C49 C50 124.2(5) . . ?
N2A C50 C49 111.0(5) . . ?
N2A C51 C52 112.2(5) . . ?
N3A C52 C51 114.8(6) . . ?
N3A C52 C53 121.3(6) . . ?
C53 C52 C51 123.9(6) . . ?
N3A C56 C57 113.8(6) . . ?
N3A C56 C55 121.4(7) . . ?
C55 C56 C57 124.8(7) . . ?
N4A C57 C56 111.7(5) . . ?
N4A C44 C45 112.3(5) . . ?
N1A C45 C44 116.1(5) . . ?
N1A C45 C46 120.7(5) . . ?
C46 C45 C44 123.1(5) . . ?
C45 C46 C47 118.0(5) . . ?
C48 C47 C46 119.7(5) . . ?
C47 C48 C49 119.2(5) . . ?
C56 C55 C54 116.5(7) . . ?
C53 C54 C55 122.1(7) . . ?
C54 C53 C52 117.1(7) . . ?
O2 Ni1 O1 90.21(16) . . ?
O2 Ni1 N3 173.89(18) . . ?
O2 Ni1 N4 94.74(18) . . ?
O2 Ni1 N1 92.35(18) . . ?
O2 Ni1 N2 106.80(18) . . ?
O1 Ni1 N3 92.30(18) . . ?
O1 Ni1 N4 106.90(19) . . ?
O1 Ni1 N1 172.82(18) . . ?
O1 Ni1 N2 93.20(18) . . ?
N3 Ni1 N4 79.20(19) . . ?
N3 Ni1 N2 78.63(19) . . ?
N1 Ni1 N3 85.82(19) . . ?
N1 Ni1 N4 79.6(2) . . ?
N1 Ni1 N2 79.64(19) . . ?
N2 Ni1 N4 150.5(2) . . ?
C22 O2 Ni1 126.0(4) . . ?
C20 O1 Ni1 126.0(4) . . ?
C6 N3 Ni1 119.8(4) . . ?
C2 N3 Ni1 118.0(4) . . ?
C2 N3 C6 121.1(5) . . ?
C7 N4 Ni1 111.0(4) . . ?
C7 N4 C8 112.9(5) . . ?
C8 N4 Ni1 103.4(4) . . ?
C9 N1 Ni1 117.4(4) . . ?
C13 N1 Ni1 119.3(4) . . ?
C13 N1 C9 121.5(5) . . ?
C0AA N2 Ni1 109.1(3) . . ?
C1 N2 Ni1 106.1(4) . . ?
C1 N2 C0AA 114.9(5) . . ?
O2 C22 C21 126.0(5) . . ?
O2 C22 C23 115.6(5) . . ?
C21 C22 C23 118.4(5) . . ?
C20 C21 C22 124.7(6) . . ?
O1 C20 C21 125.5(6) . . ?
O1 C20 C19 115.1(5) . . ?
C21 C20 C19 119.4(5) . . ?
C14 C19 C20 120.4(5) . . ?
C14 C19 C18 118.4(6) . . ?
C18 C19 C20 121.0(5) . . ?
C15 C14 C19 121.3(6) . . ?
C16 C15 C14 120.9(7) . . ?
C15 C16 C17 119.9(7) . . ?
C18 C17 C16 119.3(6) . . ?
C17 C18 C19 120.1(6) . . ?
C24 C23 C22 120.0(5) . . ?
C24 C23 C28 119.2(6) . . ?
C28 C23 C22 120.8(5) . . ?
C25 C24 C23 121.5(6) . . ?
C24 C25 C26 119.4(6) . . ?
C25 C26 C27 120.5(6) . . ?
C26 C27 C28 119.3(6) . . ?
C23 C28 C27 120.0(6) . . ?
N3 C6 C7 115.9(5) . . ?
N3 C6 C5 120.2(5) . . ?
C5 C6 C7 123.9(5) . . ?
N4 C7 C6 112.3(5) . . ?
N4 C8 C9 109.5(5) . . ?
N1 C9 C8 113.6(5) . . ?
N1 C9 C10 120.9(6) . . ?
C10 C9 C8 125.4(6) . . ?
N1 C13 C0AA 115.7(5) . . ?
N1 C13 C12 120.2(6) . . ?
C12 C13 C0AA 124.1(6) . . ?
C13 C0AA N2 112.1(5) . . ?
N2 C1 C2 111.0(5) . . ?
N3 C2 C1 113.4(5) . . ?
N3 C2 C3 121.2(6) . . ?
C3 C2 C1 125.4(6) . . ?
C2 C3 C4 118.2(6) . . ?
C5 C4 C3 119.6(6) . . ?
C4 C5 C6 119.6(6) . . ?
C13 C12 C11 119.2(6) . . ?
C10 C11 C12 119.5(6) . . ?
C11 C10 C9 118.6(6) . . ?
O1C Ni1C O1C 91.2(3) . 2_656 ?
O1C Ni1C N1C 175.2(2) 2_656 . ?
O1C Ni1C N1C 175.2(2) . 2_656 ?
O1C Ni1C N1C 90.6(2) . . ?
O1C Ni1C N1C 90.6(2) 2_656 2_656 ?
O1C Ni1C N2C 104.2(2) 2_656 2_656 ?
O1C Ni1C N2C 96.4(2) . 2_656 ?
O1C Ni1C N2C 104.2(2) . . ?
O1C Ni1C N2C 96.4(2) 2_656 . ?
N1C Ni1C N1C 87.9(3) . 2_656 ?
N1C Ni1C N2C 78.9(2) 2_656 2_656 ?
N1C Ni1C N2C 78.9(2) . . ?
N1C Ni1C N2C 80.0(2) . 2_656 ?
N1C Ni1C N2C 80.0(2) 2_656 . ?
N2C Ni1C N2C 150.6(3) 2_656 . ?
C79 O1C Ni1C 125.5(5) . . ?
C83 N1C Ni1C 120.7(4) . . ?
C85 N1C Ni1C 118.4(5) . . ?
C85 N1C C83 120.1(6) . . ?
C82 N2C Ni1C 109.5(4) . . ?
C81 N2C Ni1C 106.0(4) . . ?
C81 N2C C82 115.0(6) . . ?
O1C C79 C80 126.5(7) . . ?
O1C C79 C78 115.1(7) . . ?
C80 C79 C78 118.4(8) . . ?
C79 C80 C79 123.7(11) 2_656 . ?
C73 C78 C79 118.4(7) . . ?
C73 C78 C77 117.9(8) . . ?
C77 C78 C79 123.6(8) . . ?
C78 C73 C74 119.0(9) . . ?
C75 C74 C73 121.2(10) . . ?
C74 C75 C76 120.1(9) . . ?
C77 C76 C75 119.1(10) . . ?
C76 C77 C78 122.6(10) . . ?
N1C C83 C82 113.6(6) . . ?
N1C C83 C2BA 119.9(6) . . ?
C2BA C83 C82 126.6(6) . . ?
N2C C82 C83 112.7(6) . . ?
N2C C81 C85 113.2(5) . 2_656 ?
C84 C2BA C83 121.1(7) . . ?
C2BA C84 C4BA 118.9(8) . . ?
C85 C4BA C84 119.3(8) . . ?
N1C C85 C81 114.1(6) . 2_656 ?
N1C C85 C4BA 120.7(7) . . ?
C4BA C85 C81 125.1(7) . 2_656 ?
O1B Ni1B O1B 91.7(3) . 2_655 ?
O1B Ni1B N1B 91.6(2) . . ?
O1B Ni1B N1B 173.9(2) 2_655 . ?
O1B Ni1B N1B 173.9(2) . 2_655 ?
O1B Ni1B N1B 91.6(2) 2_655 2_655 ?
O1B Ni1B N2B 105.23(18) 2_655 . ?
O1B Ni1B N2B 94.72(19) . . ?
O1B Ni1B N2B 105.23(18) . 2_655 ?
O1B Ni1B N2B 94.72(19) 2_655 2_655 ?
N1B Ni1B N1B 85.6(3) . 2_655 ?
N1B Ni1B N2B 79.43(18) 2_655 . ?
N1B Ni1B N2B 79.63(18) . . ?
N1B Ni1B N2B 79.63(18) 2_655 2_655 ?
N1B Ni1B N2B 79.43(18) . 2_655 ?
N2B Ni1B N2B 151.3(3) . 2_655 ?
C64 O1B Ni1B 125.2(6) . . ?
C67 N1B Ni1B 118.9(4) . . ?
C67 N1B C71 121.3(5) . . ?
C71 N1B Ni1B 119.0(4) . . ?
C66 N2B Ni1B 107.0(4) . . ?
C72 N2B Ni1B 108.8(3) . . ?
C72 N2B C66 112.7(5) . . ?
O1B C64 C65 125.6(8) . . ?
O1B C64 C63 118.1(8) . . ?
C65 C64 C63 116.3(8) . . ?
C64 C65 C64 125.7(11) . 2_655 ?
C58 C63 C64 122.5(5) . . ?
C58 C63 C62 120.0 . . ?
C62 C63 C64 117.5(5) . . ?
C59 C58 C63 120.0 . . ?
C60 C59 C58 120.0 . . ?
C59 C60 C61 120.0 . . ?
C62 C61 C60 120.0 . . ?
C61 C62 C63 120.0 . . ?
N1B C67 C66 115.2(6) . . ?
N1B C67 C68 121.2(6) . . ?
C68 C67 C66 123.5(6) . . ?
N2B C66 C67 111.7(5) . . ?
N2B C72 C71 112.3(5) . 2_655 ?
C69 C68 C67 118.5(6) . . ?
C68 C69 C70 120.3(7) . . ?
C71 C70 C69 118.6(6) . . ?
N1B C71 C72 115.3(5) . 2_655 ?
N1B C71 C70 120.0(6) . . ?
C70 C71 C72 124.7(6) . 2_655 ?
C91 O7 C89 110.6(10) . . ?
O7 C89 C90 110.4(10) . . ?
O7 C91 C92 105.1(11) . . ?
C94 C93 B1 121.7(5) . . ?
C98 C93 C94 114.4(5) . . ?
C98 C93 B1 123.7(5) . . ?
C95 C94 C93 123.7(5) . . ?
C96 C95 C94 118.7(6) . . ?
C97 C96 C95 119.6(6) . . ?
C96 C97 C98 120.2(6) . . ?
C97 C98 C93 123.4(6) . . ?
C100 C99 C104 115.0(5) . . ?
C100 C99 B1 124.9(5) . . ?
C104 C99 B1 120.0(5) . . ?
C101 C100 C99 123.3(5) . . ?
C100 C101 C102 120.1(6) . . ?
C103 C102 C101 118.7(6) . . ?
C102 C103 C104 120.1(6) . . ?
C103 C104 C99 122.7(5) . . ?
C106 C105 C110 114.7(5) . . ?
C106 C105 B1 123.1(5) . . ?
C110 C105 B1 122.1(5) . . ?
C107 C106 C105 122.8(6) . . ?
C108 C107 C106 121.2(6) . . ?
C107 C108 C109 118.9(6) . . ?
C108 C109 C110 120.0(6) . . ?
C109 C110 C105 122.3(6) . . ?
C112 C111 B1 119.0(5) . . ?
C116 C111 C112 114.6(5) . . ?
C116 C111 B1 126.4(5) . . ?
C113 C112 C111 122.7(6) . . ?
C112 C113 C114 120.0(6) . . ?
C115 C114 C113 119.2(6) . . ?
C114 C115 C116 120.1(6) . . ?
C115 C116 C111 123.3(6) . . ?
C99 B1 C93 111.5(5) . . ?
C105 B1 C93 110.9(4) . . ?
C105 B1 C99 106.4(5) . . ?
C111 B1 C93 104.8(4) . . ?
C111 B1 C99 110.0(4) . . ?
C111 B1 C105 113.4(5) . . ?
C118 C117 C122 114.9(6) . . ?
C118 C117 B2 121.8(5) . . ?
C122 C117 B2 123.2(6) . . ?
C119 C118 C117 121.6(6) . . ?
C120 C119 C118 121.1(7) . . ?
C119 C120 C121 118.7(7) . . ?
C122 C121 C120 119.2(7) . . ?
C121 C122 C117 124.5(7) . . ?
C124 C123 C128 115.2(5) . . ?
C124 C123 B2 120.6(5) . . ?
C128 C123 B2 124.1(5) . . ?
C125 C124 C123 123.4(6) . . ?
C124 C125 C126 120.3(6) . . ?
C127 C126 C125 118.3(6) . . ?
C126 C127 C128 121.0(6) . . ?
C127 C128 C123 121.7(5) . . ?
C130 C129 C134 115.5(5) . . ?
C130 C129 B2 120.3(5) . . ?
C134 C129 B2 124.0(5) . . ?
C131 C130 C129 122.3(6) . . ?
C132 C131 C130 121.5(6) . . ?
C131 C132 C133 118.6(6) . . ?
C134 C133 C132 119.7(6) . . ?
C133 C134 C129 122.3(6) . . ?
C136 C135 C140 115.7(5) . . ?
C136 C135 B2 118.9(5) . . ?
C140 C135 B2 125.2(5) . . ?
C137 C136 C135 123.2(6) . . ?
C136 C137 C138 119.8(6) . . ?
C139 C138 C137 119.1(6) . . ?
C138 C139 C140 120.6(6) . . ?
C139 C140 C135 121.5(6) . . ?
C123 B2 C117 104.5(5) . . ?
C123 B2 C129 112.3(5) . . ?
C129 B2 C117 109.9(5) . . ?
C135 B2 C117 114.4(5) . . ?
C135 B2 C123 111.3(5) . . ?
C135 B2 C129 104.7(5) . . ?
C142 C141 B3 123.4(6) . . ?
C146 C141 C142 114.8(6) . . ?
C146 C141 B3 121.7(6) . . ?
C143 C142 C141 122.6(6) . . ?
C144 C143 C142 121.1(7) . . ?
C143 C144 C145 119.1(7) . . ?
C144 C145 C146 118.7(7) . . ?
C141 C146 C145 123.6(7) . . ?
C148 C147 C152 115.4(6) . . ?
C148 C147 B3 124.3(6) . . ?
C152 C147 B3 120.3(6) . . ?
C149 C148 C147 123.8(7) . . ?
C148 C149 C150 120.3(7) . . ?
C151 C150 C149 118.1(6) . . ?
C150 C151 C152 119.6(7) . . ?
C147 C152 C151 122.7(7) . . ?
C154 C153 B3 121.9(6) . . ?
C158 C153 C154 115.6(6) . . ?
C158 C153 B3 122.4(6) . . ?
C155 C154 C153 123.2(7) . . ?
C154 C155 C156 119.8(7) . . ?
C157 C156 C155 119.0(7) . . ?
C156 C157 C158 122.0(7) . . ?
C153 C158 C157 120.4(7) . . ?
C160 C159 B3 122.6(6) . . ?
C164 C159 C160 113.3(7) . . ?
C164 C159 B3 124.0(6) . . ?
C161 C160 C159 123.0(8) . . ?
C160 C161 C162 120.6(9) . . ?
C163 C162 C161 117.2(9) . . ?
C164 C163 C162 120.7(9) . . ?
C163 C164 C159 125.2(9) . . ?
C141 B3 C147 107.9(5) . . ?
C153 B3 C141 110.4(5) . . ?
C153 B3 C147 108.9(5) . . ?
C159 B3 C141 110.0(5) . . ?
C159 B3 C147 110.7(5) . . ?
C159 B3 C153 109.0(5) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.449(13)
2 0.551(13)

