# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_1
_database_code_depnum_ccdc_archive 'CCDC 1944919'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh'
;University of Calcutta
India
;
_audit_update_record             
;
2019-09-30 deposited with the CCDC.	2019-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H46 N8 Ni2 O2, 2(Cl O4), 2(C2 H3 N)'
_chemical_formula_sum            ' C34 H52 Cl2 N10 Ni2 O10'
_chemical_formula_weight         949.14

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           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.1525(5)
_cell_length_b                   8.4556(4)
_cell_length_c                   21.0201(9)
_cell_angle_alpha                90
_cell_angle_beta                 107.942(2)
_cell_angle_gamma                90
_cell_volume                     2224.01(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    44701
_cell_measurement_theta_min      2.181
_cell_measurement_theta_max      25.074

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_F_000             992
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    1.029
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44701
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.181
_diffrn_reflns_theta_max         25.074
_diffrn_reflns_theta_full        25.074
_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             3930
_reflns_number_gt                3359
_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-II'
_computing_cell_refinement       'BRUKER APEX-II'
_computing_data_reduction        'BRUKER APEX-II'
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep-3 for Windows'
_computing_publication_material  PLATON-97
_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)+(0.0771P)²+2.7602P] 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         3930
_refine_ls_number_parameters     266
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1404
_refine_ls_wR_factor_gt          0.1327
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.008
_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 0.37260(3) 0.48929(4) 0.46838(2) 0.02769(17) Uani 1 1 d . . . . .
Cl1 Cl 0.10729(10) 0.53793(17) 0.66649(7) 0.0725(4) Uani 1 1 d . . . . .
O10 O 0.49623(16) 0.4072(2) 0.54784(10) 0.0276(5) Uani 1 1 d . . . . .
N22 N 0.6100(2) 0.7034(3) 0.59024(14) 0.0329(6) Uani 1 1 d . . . . .
H21 H 0.5458 0.6797 0.6027 0.039 Uiso 1 1 calc R U . . .
N18 N 0.7319(2) 0.3823(3) 0.61016(13) 0.0332(6) Uani 1 1 d . . . . .
H17 H 0.7896 0.3493 0.5927 0.040 Uiso 1 1 calc R U . . .
N1 N 0.3488(2) 0.6813(4) 0.53354(15) 0.0406(7) Uani 1 1 d . . . . .
N2 N 0.2400(3) 0.3791(4) 0.48474(15) 0.0415(7) Uani 1 1 d . . . . .
C11 C 0.4971(3) 0.3436(3) 0.60692(15) 0.0280(7) Uani 1 1 d . . . . .
C12 C 0.4109(3) 0.3630(4) 0.63179(16) 0.0348(7) Uani 1 1 d . . . . .
H11 H 0.3520 0.4222 0.6078 0.042 Uiso 1 1 calc R U . . .
C13 C 0.4128(3) 0.2944(5) 0.69202(18) 0.0460(9) Uani 1 1 d . . . . .
H12 H 0.3550 0.3082 0.7081 0.055 Uiso 1 1 calc R U . . .
C16 C 0.5857(3) 0.2556(4) 0.64434(16) 0.0335(7) Uani 1 1 d . . . . .
C18 C 0.6799(3) 0.2326(4) 0.61944(18) 0.0393(8) Uani 1 1 d . . . . .
H16A H 0.7321 0.1667 0.6510 0.047 Uiso 1 1 calc R U . . .
H16B H 0.6567 0.1768 0.5771 0.047 Uiso 1 1 calc R U . . .
C3 C 0.1640(3) 0.3349(5) 0.49202(19) 0.0460(9) Uani 1 1 d . . . . .
C1 C 0.3281(3) 0.7730(5) 0.5661(2) 0.0476(9) Uani 1 1 d . . . . .
C14 C 0.4987(3) 0.2067(5) 0.72816(19) 0.0512(10) Uani 1 1 d . . . . .
H13 H 0.4988 0.1597 0.7682 0.061 Uiso 1 1 calc R U . . .
C21 C 0.6948(3) 0.7293(4) 0.65429(18) 0.0452(9) Uani 1 1 d . . . . .
H20A H 0.6719 0.8113 0.6791 0.054 Uiso 1 1 calc R U . . .
H20B H 0.7587 0.7665 0.6452 0.054 Uiso 1 1 calc R U . . .
C15 C 0.5848(3) 0.1885(4) 0.70484(18) 0.0447(9) Uani 1 1 d . . . . .
H14 H 0.6435 0.1304 0.7298 0.054 Uiso 1 1 calc R U . . .
C20 C 0.7216(3) 0.5822(5) 0.69685(18) 0.0450(9) Uani 1 1 d . . . . .
H19A H 0.7598 0.6131 0.7424 0.054 Uiso 1 1 calc R U . . .
H19B H 0.6555 0.5321 0.6973 0.054 Uiso 1 1 calc R U . . .
C19 C 0.7877(3) 0.4632(5) 0.67430(19) 0.0455(9) Uani 1 1 d . . . . .
H18A H 0.8505 0.5160 0.6696 0.055 Uiso 1 1 calc R U . . .
H18B H 0.8120 0.3836 0.7089 0.055 Uiso 1 1 calc R U . . .
C23 C 0.5860(4) 0.8536(4) 0.5530(2) 0.0526(10) Uani 1 1 d . . . . .
H22A H 0.5621 0.9301 0.5790 0.079 Uiso 1 1 calc R U . . .
H22B H 0.5310 0.8366 0.5114 0.079 Uiso 1 1 calc R U . . .
H22C H 0.6493 0.8919 0.5445 0.079 Uiso 1 1 calc R U . . .
C5 C 0.0753(4) 0.9332(7) 0.3941(3) 0.0713(13) Uani 1 1 d . . . . .
C4 C 0.0675(4) 0.2746(7) 0.5038(3) 0.0794(16) Uani 1 1 d . . . . .
H4A H 0.0789 0.1672 0.5191 0.119 Uiso 1 1 calc R U . . .
H4B H 0.0092 0.2789 0.4630 0.119 Uiso 1 1 calc R U . . .
H4C H 0.0510 0.3382 0.5372 0.119 Uiso 1 1 calc R U . . .
N3 N 0.1326(4) 0.9242(7) 0.4446(3) 0.0994(16) Uani 1 1 d . . . . .
O1 O 0.0110(4) 0.4672(8) 0.6298(3) 0.134(2) Uani 1 1 d . . . . .
O2 O 0.1703(4) 0.5545(9) 0.6246(3) 0.156(2) Uani 1 1 d . . . . .
C2 C 0.3029(5) 0.8927(7) 0.6087(3) 0.0925(19) Uani 1 1 d . . . . .
H2A H 0.3548 0.8887 0.6523 0.139 Uiso 1 1 calc R U . . .
H2B H 0.2331 0.8730 0.6124 0.139 Uiso 1 1 calc R U . . .
H2C H 0.3043 0.9954 0.5895 0.139 Uiso 1 1 calc R U . . .
O3 O 0.1584(6) 0.4555(11) 0.7226(4) 0.199(4) Uani 1 1 d . . . . .
O4 O 0.0814(8) 0.6795(8) 0.6857(4) 0.222(4) Uani 1 1 d . . . . .
C6 C 0.0022(7) 0.9420(10) 0.3284(4) 0.122(3) Uani 1 1 d . . . . .
H6A H 0.0406 0.9630 0.2972 0.184 Uiso 1 1 calc R U . . .
H6B H -0.0481 1.0257 0.3263 0.184 Uiso 1 1 calc R U . . .
H6C H -0.0353 0.8434 0.3173 0.184 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 O10 2.055(2) 3_666 ?
Ni1 O10 2.060(2) . ?
Ni1 N18 2.096(3) 3_666 ?
Ni1 N22 2.098(3) 3_666 ?
Ni1 N2 2.097(3) . ?
Ni1 N1 2.208(3) . ?
Cl1 O4 1.341(6) . ?
Cl1 O3 1.357(6) . ?
Cl1 O2 1.391(5) . ?
Cl1 O1 1.397(5) . ?
O10 C11 1.350(4) . ?
O10 Ni1 2.055(2) 3_666 ?
N22 C23 1.473(5) . ?
N22 C21 1.476(4) . ?
N22 Ni1 2.097(3) 3_666 ?
N22 H21 0.9800 . ?
N18 C18 1.480(4) . ?
N18 C19 1.488(5) . ?
N18 Ni1 2.097(3) 3_666 ?
N18 H17 0.9800 . ?
N1 C1 1.122(5) . ?
N2 C3 1.120(5) . ?
C11 C12 1.397(4) . ?
C11 C16 1.402(5) . ?
C12 C13 1.386(5) . ?
C12 H11 0.9300 . ?
C13 C14 1.369(6) . ?
C13 H12 0.9300 . ?
C16 C15 1.396(5) . ?
C16 C18 1.499(5) . ?
C18 H16A 0.9700 . ?
C18 H16B 0.9700 . ?
C3 C4 1.458(6) . ?
C1 C2 1.455(6) . ?
C14 C15 1.373(6) . ?
C14 H13 0.9300 . ?
C21 C20 1.509(5) . ?
C21 H20A 0.9700 . ?
C21 H20B 0.9700 . ?
C15 H14 0.9300 . ?
C20 C19 1.499(5) . ?
C20 H19A 0.9700 . ?
C20 H19B 0.9700 . ?
C19 H18A 0.9700 . ?
C19 H18B 0.9700 . ?
C23 H22A 0.9600 . ?
C23 H22B 0.9600 . ?
C23 H22C 0.9600 . ?
C5 N3 1.099(7) . ?
C5 C6 1.421(9) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?

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
O10 Ni1 O10 77.56(9) 3_666 . ?
O10 Ni1 N18 91.66(9) 3_666 3_666 ?
O10 Ni1 N18 167.27(10) . 3_666 ?
O10 Ni1 N22 89.11(10) 3_666 3_666 ?
O10 Ni1 N22 90.74(10) . 3_666 ?
N18 Ni1 N22 95.93(11) 3_666 3_666 ?
O10 Ni1 N2 178.85(10) 3_666 . ?
O10 Ni1 N2 101.90(10) . . ?
N18 Ni1 N2 88.99(12) 3_666 . ?
N22 Ni1 N2 89.88(11) 3_666 . ?
O10 Ni1 N1 94.37(10) 3_666 . ?
O10 Ni1 N1 88.40(10) . . ?
N18 Ni1 N1 85.64(11) 3_666 . ?
N22 Ni1 N1 176.14(11) 3_666 . ?
N2 Ni1 N1 86.62(12) . . ?
O4 Cl1 O3 107.5(6) . . ?
O4 Cl1 O2 111.0(5) . . ?
O3 Cl1 O2 111.7(5) . . ?
O4 Cl1 O1 106.1(5) . . ?
O3 Cl1 O1 112.4(5) . . ?
O2 Cl1 O1 108.0(4) . . ?
C11 O10 Ni1 123.55(18) . 3_666 ?
C11 O10 Ni1 131.39(19) . . ?
Ni1 O10 Ni1 102.44(9) 3_666 . ?
C23 N22 C21 109.5(3) . . ?
C23 N22 Ni1 113.7(2) . 3_666 ?
C21 N22 Ni1 117.6(2) . 3_666 ?
C23 N22 H21 104.9 . . ?
C21 N22 H21 104.9 . . ?
Ni1 N22 H21 104.9 3_666 . ?
C18 N18 C19 113.1(3) . . ?
C18 N18 Ni1 109.2(2) . 3_666 ?
C19 N18 Ni1 119.8(2) . 3_666 ?
C18 N18 H17 104.4 . . ?
C19 N18 H17 104.4 . . ?
Ni1 N18 H17 104.4 3_666 . ?
C1 N1 Ni1 173.8(3) . . ?
C3 N2 Ni1 172.9(3) . . ?
O10 C11 C12 121.3(3) . . ?
O10 C11 C16 119.9(3) . . ?
C12 C11 C16 118.9(3) . . ?
C13 C12 C11 120.3(3) . . ?
C13 C12 H11 119.9 . . ?
C11 C12 H11 119.9 . . ?
C14 C13 C12 120.9(3) . . ?
C14 C13 H12 119.6 . . ?
C12 C13 H12 119.6 . . ?
C15 C16 C11 119.2(3) . . ?
C15 C16 C18 120.4(3) . . ?
C11 C16 C18 120.4(3) . . ?
N18 C18 C16 113.6(3) . . ?
N18 C18 H16A 108.8 . . ?
C16 C18 H16A 108.8 . . ?
N18 C18 H16B 108.8 . . ?
C16 C18 H16B 108.8 . . ?
H16A C18 H16B 107.7 . . ?
N2 C3 C4 177.9(5) . . ?
N1 C1 C2 179.1(5) . . ?
C13 C14 C15 119.5(3) . . ?
C13 C14 H13 120.3 . . ?
C15 C14 H13 120.3 . . ?
N22 C21 C20 113.1(3) . . ?
N22 C21 H20A 109.0 . . ?
C20 C21 H20A 109.0 . . ?
N22 C21 H20B 109.0 . . ?
C20 C21 H20B 109.0 . . ?
H20A C21 H20B 107.8 . . ?
C14 C15 C16 121.3(4) . . ?
C14 C15 H14 119.4 . . ?
C16 C15 H14 119.4 . . ?
C19 C20 C21 114.7(3) . . ?
C19 C20 H19A 108.6 . . ?
C21 C20 H19A 108.6 . . ?
C19 C20 H19B 108.6 . . ?
C21 C20 H19B 108.6 . . ?
H19A C20 H19B 107.6 . . ?
N18 C19 C20 115.0(3) . . ?
N18 C19 H18A 108.5 . . ?
C20 C19 H18A 108.5 . . ?
N18 C19 H18B 108.5 . . ?
C20 C19 H18B 108.5 . . ?
H18A C19 H18B 107.5 . . ?
N22 C23 H22A 109.5 . . ?
N22 C23 H22B 109.5 . . ?
H22A C23 H22B 109.5 . . ?
N22 C23 H22C 109.5 . . ?
H22A C23 H22C 109.5 . . ?
H22B C23 H22C 109.5 . . ?
N3 C5 C6 178.8(7) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

_refine_diff_density_max         1.340
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.083


####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1944920'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh'
;University of Calcutta
India
;
_audit_update_record             
;
2019-09-30 deposited with the CCDC.	2019-10-24 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         'C21 H26 N4 Ni O2 S'
_chemical_formula_sum            'C21 H26 N4 Ni O2 S'
_chemical_formula_weight         457.21

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'
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      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                   10.976(3)
_cell_length_b                   14.442(4)
_cell_length_c                   14.246(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.399(3)
_cell_angle_gamma                90
_cell_volume                     2196.8(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9755
_cell_measurement_theta_min      2.037
_cell_measurement_theta_max      24.497

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_F_000             960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    1.002
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_T_max  0.818
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9755
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.037
_diffrn_reflns_theta_max         24.497
_diffrn_reflns_theta_full        24.497
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.969
_reflns_number_total             3544
_reflns_number_gt                2288
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WINGX V1.80.03'
_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)+(0.1175P)²+4.1900P] 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         3544
_refine_ls_number_parameters     268
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0706
_refine_ls_wR_factor_ref         0.2318
_refine_ls_wR_factor_gt          0.1994
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.056
_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
C1 C 0.6613(6) 0.2952(5) 0.4107(5) 0.0626(18) Uani 1 1 d . . . . .
C2 C 0.5037(7) 0.7129(5) 0.3246(6) 0.0662(19) Uani 1 1 d . . . . .
C3 C 0.4525(10) 0.8007(6) 0.3433(8) 0.116(4) Uani 1 1 d . . . . .
H3A H 0.382659 0.790832 0.372054 0.174 Uiso 1 1 calc R U . . .
H3B H 0.425019 0.833917 0.283735 0.174 Uiso 1 1 calc R U . . .
H3C H 0.515546 0.836072 0.386505 0.174 Uiso 1 1 calc R U . . .
C11 C 0.7396(5) 0.6098(5) 0.5031(4) 0.0485(15) Uani 1 1 d . . . . .
C12 C 0.7252(6) 0.6824(5) 0.5633(5) 0.0593(17) Uani 1 1 d . . . . .
H12 H 0.653780 0.686301 0.587700 0.071 Uiso 1 1 calc R U . . .
C13 C 0.8168(7) 0.7482(5) 0.5865(5) 0.070(2) Uani 1 1 d . . . . .
H13 H 0.806845 0.797323 0.626292 0.085 Uiso 1 1 calc R U . . .
C14 C 0.9245(7) 0.7427(6) 0.5514(5) 0.071(2) Uani 1 1 d . . . . .
H14 H 0.987217 0.786949 0.568616 0.085 Uiso 1 1 calc R U . . .
C15 C 0.9374(6) 0.6719(5) 0.4917(5) 0.0620(18) Uani 1 1 d . . . . .
H15 H 1.009009 0.668689 0.467465 0.074 Uiso 1 1 calc R U . . .
C16 C 0.8456(5) 0.6039(5) 0.4658(4) 0.0503(15) Uani 1 1 d . . . . .
C17 C 0.8627(6) 0.5226(5) 0.4042(5) 0.0597(18) Uani 1 1 d . . . . .
H17A H 0.944793 0.526625 0.390047 0.072 Uiso 1 1 calc R U . . .
H17B H 0.860135 0.466108 0.440517 0.072 Uiso 1 1 calc R U . . .
C19 C 0.8041(7) 0.4391(6) 0.2564(6) 0.083(2) Uani 1 1 d . . . . .
H19A H 0.807706 0.382803 0.294015 0.100 Uiso 1 1 calc R U . . .
H19B H 0.887679 0.451211 0.247574 0.100 Uiso 1 1 calc R U . . .
C20 C 0.7166(8) 0.4239(7) 0.1584(6) 0.097(3) Uani 1 1 d . . . . .
H20A H 0.755230 0.379554 0.123037 0.116 Uiso 1 1 calc R U . . .
H20B H 0.708469 0.481828 0.123074 0.116 Uiso 1 1 calc R U . . .
C21 C 0.5849(7) 0.3890(6) 0.1595(5) 0.074(2) Uani 1 1 d . . . . .
H21A H 0.542000 0.371510 0.094472 0.089 Uiso 1 1 calc R U . . .
H21B H 0.592165 0.334043 0.199594 0.089 Uiso 1 1 calc R U . . .
C23 C 0.4914(12) 0.5331(9) 0.1272(9) 0.138(4) Uani 1 1 d . U . . .
H23A H 0.566622 0.569270 0.137018 0.206 Uiso 1 1 calc R U . . .
H23B H 0.423261 0.571733 0.135038 0.206 Uiso 1 1 calc R U . . .
H23C H 0.472758 0.507675 0.063154 0.206 Uiso 1 1 calc R U . . .
C24 C 0.3824(7) 0.4193(5) 0.1904(5) 0.069(2) Uani 1 1 d . . . . .
H24A H 0.390171 0.367988 0.235330 0.083 Uiso 1 1 calc R U . . .
H24B H 0.350794 0.394733 0.125947 0.083 Uiso 1 1 calc R U . . .
C25 C 0.2889(6) 0.4871(4) 0.2121(5) 0.0534(17) Uani 1 1 d . . . . .
C26 C 0.1851(7) 0.5141(6) 0.1420(5) 0.074(2) Uani 1 1 d . . . . .
H26 H 0.172042 0.490504 0.079696 0.088 Uiso 1 1 calc R U . . .
C27 C 0.1016(7) 0.5761(7) 0.1651(7) 0.087(3) Uani 1 1 d . . . . .
H27 H 0.031044 0.593682 0.118546 0.104 Uiso 1 1 calc R U . . .
C28 C 0.1219(7) 0.6122(6) 0.2564(7) 0.080(2) Uani 1 1 d . . . . .
H28 H 0.066519 0.655630 0.271136 0.096 Uiso 1 1 calc R U . . .
C29 C 0.2239(6) 0.5843(5) 0.3264(6) 0.0671(19) Uani 1 1 d . . . . .
H29 H 0.235738 0.607416 0.388805 0.080 Uiso 1 1 calc R U . . .
C30 C 0.3079(6) 0.5230(5) 0.3047(5) 0.0514(16) Uani 1 1 d . . . . .
N1 N 0.6220(6) 0.3658(4) 0.3835(4) 0.0668(16) Uani 1 1 d . . . . .
N2 N 0.5430(6) 0.6433(4) 0.3121(4) 0.0607(14) Uani 1 1 d . . . . .
N18 N 0.7661(5) 0.5170(4) 0.3116(4) 0.0582(15) Uani 1 1 d . . . . .
H18 H 0.766871 0.574621 0.275479 0.070 Uiso 1 1 calc R U . . .
N22 N 0.5084(5) 0.4592(4) 0.1964(4) 0.0533(13) Uani 1 1 d . U . . .
Ni1 Ni 0.58610(7) 0.49905(5) 0.34088(5) 0.0450(3) Uani 1 1 d . . . . .
O10 O 0.6520(4) 0.5420(3) 0.4801(3) 0.0525(11) Uani 1 1 d D . . . .
O31 O 0.4114(4) 0.4953(3) 0.3720(3) 0.0514(11) Uani 1 1 d . . . . .
S1 S 0.7210(2) 0.1961(2) 0.4502(3) 0.1516(16) Uani 1 1 d . . . . .
H10 H 0.634(8) 0.526(6) 0.541(3) 0.10(3) Uiso 1 1 d 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
C1 N1 1.139(8) . ?
C1 S1 1.619(8) . ?
C2 N2 1.124(8) . ?
C2 C3 1.437(11) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C11 O10 1.358(7) . ?
C11 C12 1.387(9) . ?
C11 C16 1.389(8) . ?
C12 C13 1.367(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.389(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.358(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.394(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.502(9) . ?
C17 N18 1.491(9) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C19 N18 1.486(9) . ?
C19 C20 1.517(11) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.535(11) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 N22 1.488(9) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C23 N22 1.435(12) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 N22 1.482(9) . ?
C24 C25 1.503(10) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.386(10) . ?
C25 C30 1.388(10) . ?
C26 C27 1.375(12) . ?
C26 H26 0.9300 . ?
C27 C28 1.372(12) . ?
C27 H27 0.9300 . ?
C28 C29 1.376(10) . ?
C28 H28 0.9300 . ?
C29 C30 1.364(10) . ?
C29 H29 0.9300 . ?
C30 O31 1.366(7) . ?
N1 Ni1 2.029(6) . ?
N2 Ni1 2.154(6) . ?
N18 Ni1 2.128(5) . ?
N18 H18 0.9800 . ?
N22 Ni1 2.117(5) . ?
Ni1 O10 2.043(4) . ?
Ni1 O31 2.066(4) . ?
O10 H10 0.96(2) . ?

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 C1 S1 178.4(7) . . ?
N2 C2 C3 178.2(9) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O10 C11 C12 121.2(5) . . ?
O10 C11 C16 118.2(6) . . ?
C12 C11 C16 120.6(6) . . ?
C13 C12 C11 119.5(6) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 120.8(7) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C15 C14 C13 119.3(7) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 121.5(7) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C11 C16 C15 118.3(6) . . ?
C11 C16 C17 120.0(6) . . ?
C15 C16 C17 121.6(6) . . ?
N18 C17 C16 113.6(5) . . ?
N18 C17 H17A 108.8 . . ?
C16 C17 H17A 108.8 . . ?
N18 C17 H17B 108.8 . . ?
C16 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
N18 C19 C20 113.7(7) . . ?
N18 C19 H19A 108.8 . . ?
C20 C19 H19A 108.8 . . ?
N18 C19 H19B 108.8 . . ?
C20 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 C21 115.8(7) . . ?
C19 C20 H20A 108.3 . . ?
C21 C20 H20A 108.3 . . ?
C19 C20 H20B 108.3 . . ?
C21 C20 H20B 108.3 . . ?
H20A C20 H20B 107.4 . . ?
N22 C21 C20 112.9(6) . . ?
N22 C21 H21A 109.0 . . ?
C20 C21 H21A 109.0 . . ?
N22 C21 H21B 109.0 . . ?
C20 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
N22 C23 H23A 109.5 . . ?
N22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N22 C24 C25 114.1(6) . . ?
N22 C24 H24A 108.7 . . ?
C25 C24 H24A 108.7 . . ?
N22 C24 H24B 108.7 . . ?
C25 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
C26 C25 C30 119.8(7) . . ?
C26 C25 C24 121.5(7) . . ?
C30 C25 C24 118.7(6) . . ?
C27 C26 C25 119.5(8) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C28 C27 C26 120.3(8) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 120.1(8) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C30 C29 C28 120.4(8) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C29 C30 O31 121.8(6) . . ?
C29 C30 C25 119.8(6) . . ?
O31 C30 C25 118.4(6) . . ?
C1 N1 Ni1 169.3(6) . . ?
C2 N2 Ni1 155.5(6) . . ?
C19 N18 C17 106.3(5) . . ?
C19 N18 Ni1 113.5(5) . . ?
C17 N18 Ni1 109.6(4) . . ?
C19 N18 H18 109.1 . . ?
C17 N18 H18 109.1 . . ?
Ni1 N18 H18 109.1 . . ?
C23 N22 C24 106.1(7) . . ?
C23 N22 C21 105.0(7) . . ?
C24 N22 C21 108.0(6) . . ?
C23 N22 Ni1 115.1(7) . . ?
C24 N22 Ni1 108.8(4) . . ?
C21 N22 Ni1 113.3(4) . . ?
N1 Ni1 O10 89.8(2) . . ?
N1 Ni1 O31 92.1(2) . . ?
O10 Ni1 O31 86.39(16) . . ?
N1 Ni1 N22 92.3(2) . . ?
O10 Ni1 N22 176.68(19) . . ?
O31 Ni1 N22 90.96(19) . . ?
N1 Ni1 N18 92.8(2) . . ?
O10 Ni1 N18 91.01(19) . . ?
O31 Ni1 N18 174.42(19) . . ?
N22 Ni1 N18 91.5(2) . . ?
N1 Ni1 N2 173.2(2) . . ?
O10 Ni1 N2 84.5(2) . . ?
O31 Ni1 N2 83.81(19) . . ?
N22 Ni1 N2 93.2(2) . . ?
N18 Ni1 N2 91.0(2) . . ?
C11 O10 Ni1 121.6(3) . . ?
C11 O10 H10 103(5) . . ?
Ni1 O10 H10 135(5) . . ?
C30 O31 Ni1 120.4(4) . . ?

_refine_diff_density_max         1.826
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.099


####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1944921'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh'
;University of Calcutta
India
;
_audit_update_record             
;
2019-09-30 deposited with the CCDC.	2019-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H52 N6 Ni3 O8 S2, O'
_chemical_formula_sum            'C38 H54 N6 Ni3 O8 S2'
_chemical_formula_weight         977.05

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'
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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+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                   19.913(5)
_cell_length_b                   11.258(5)
_cell_length_c                   19.410(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 92.010(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     4349(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    30552
_cell_measurement_theta_min      2.047
_cell_measurement_theta_max      26.789

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_F_000             2040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    1.440
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30552
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.047
_diffrn_reflns_theta_max         26.789
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4642
_reflns_number_gt                3784
_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-II'
_computing_cell_refinement       'BRUKER APEX-II'
_computing_data_reduction        'BRUKER APEX-II'
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep-3 for Windows'
_computing_publication_material  PLATON-97
_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)+(0.0778P)²+10.7049P] 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         4642
_refine_ls_number_parameters     284
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1459
_refine_ls_wR_factor_gt          0.1374
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.069
_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
Ni2 Ni 0.0000 0.00612(5) 0.2500 0.03128(17) Uani 1 2 d S T P . .
Ni1 Ni 0.07479(2) 0.17604(4) 0.14490(2) 0.03275(15) Uani 1 1 d . . . . .
O31 O 0.09292(11) 0.0367(2) 0.21094(11) 0.0351(5) Uani 1 1 d . . . . .
O2 O 0.08203(14) 0.2886(2) 0.23317(13) 0.0416(6) Uani 1 1 d D . . . .
O10 O -0.02390(11) 0.1463(2) 0.17559(11) 0.0312(5) Uani 1 1 d . . . . .
N18 N 0.04594(17) 0.3176(3) 0.08062(16) 0.0441(7) Uani 1 1 d D . . . .
O1 O 0.05765(18) 0.0467(4) 0.06590(17) 0.0690(9) Uani 1 1 d D . . . .
N22 N 0.17864(16) 0.2061(3) 0.12782(16) 0.0463(8) Uani 1 1 d . . . . .
C16 C -0.07244(18) 0.2436(3) 0.07687(18) 0.0400(8) Uani 1 1 d . . . . .
N1 N -0.02637(17) -0.1230(3) 0.17864(17) 0.0457(7) Uani 1 1 d . . . . .
C11 C -0.07235(16) 0.1492(3) 0.12474(16) 0.0324(7) Uani 1 1 d . . . . .
C29 C 0.1360(2) -0.1601(4) 0.1960(2) 0.0515(10) Uani 1 1 d . . . . .
H29 H 0.0949 -0.1938 0.2064 0.062 Uiso 1 1 calc R U . . .
C12 C -0.12296(17) 0.0648(3) 0.11904(18) 0.0391(8) Uani 1 1 d . . . . .
H12 H -0.1257 0.0054 0.1521 0.047 Uiso 1 1 calc R U . . .
C15 C -0.1200(2) 0.2441(4) 0.0224(2) 0.0521(10) Uani 1 1 d . . . . .
H15 H -0.1195 0.3052 -0.0098 0.062 Uiso 1 1 calc R U . . .
C24 C 0.21652(19) 0.1430(4) 0.1845(2) 0.0550(11) Uani 1 1 d . . . . .
H24A H 0.2640 0.1604 0.1812 0.066 Uiso 1 1 calc R U . . .
H24B H 0.2022 0.1733 0.2284 0.066 Uiso 1 1 calc R U . . .
C14 C -0.1678(2) 0.1561(4) 0.0151(2) 0.0549(11) Uani 1 1 d . . . . .
H14 H -0.1984 0.1562 -0.0223 0.066 Uiso 1 1 calc R U . . .
C13 C -0.16954(18) 0.0685(4) 0.0642(2) 0.0471(9) Uani 1 1 d . . . . .
H13 H -0.2026 0.0103 0.0606 0.057 Uiso 1 1 calc R U . . .
C25 C 0.20688(19) 0.0116(4) 0.18308(19) 0.0492(10) Uani 1 1 d . . . . .
C21 C 0.1968(2) 0.3346(4) 0.1322(3) 0.0606(12) Uani 1 1 d . . . . .
H21A H 0.2448 0.3425 0.1262 0.073 Uiso 1 1 calc R U . . .
H21B H 0.1874 0.3632 0.1780 0.073 Uiso 1 1 calc R U . . .
C17 C -0.0258(2) 0.3468(3) 0.0881(2) 0.0473(9) Uani 1 1 d . . . . .
H17A H -0.0382 0.4088 0.0553 0.057 Uiso 1 1 calc R U . . .
H17B H -0.0318 0.3782 0.1340 0.057 Uiso 1 1 calc R U . . .
C26 C 0.2596(2) -0.0644(5) 0.1669(2) 0.0652(13) Uani 1 1 d . . . . .
H26 H 0.3014 -0.0324 0.1576 0.078 Uiso 1 1 calc R U . . .
C19 C 0.0857(2) 0.4292(4) 0.0901(2) 0.0592(11) Uani 1 1 d . . . . .
H19A H 0.0795 0.4593 0.1363 0.071 Uiso 1 1 calc R U . . .
H19B H 0.0685 0.4884 0.0577 0.071 Uiso 1 1 calc R U . . .
C20 C 0.1601(2) 0.4126(4) 0.0797(3) 0.0660(13) Uani 1 1 d . . . . .
H20A H 0.1813 0.4901 0.0802 0.079 Uiso 1 1 calc R U . . .
H20B H 0.1657 0.3787 0.0343 0.079 Uiso 1 1 calc R U . . .
C30 C 0.14373(18) -0.0373(4) 0.19725(17) 0.0411(8) Uani 1 1 d . . . . .
C27 C 0.2510(3) -0.1848(5) 0.1644(2) 0.0706(15) Uani 1 1 d . . . . .
H27 H 0.2864 -0.2339 0.1528 0.085 Uiso 1 1 calc R U . . .
C28 C 0.1897(3) -0.2327(4) 0.1793(2) 0.0632(12) Uani 1 1 d . . . . .
H28 H 0.1840 -0.3147 0.1781 0.076 Uiso 1 1 calc R U . . .
C23 C 0.2022(3) 0.1598(5) 0.0618(2) 0.0710(14) Uani 1 1 d . . . . .
H23A H 0.2481 0.1828 0.0563 0.107 Uiso 1 1 calc R U . . .
H23B H 0.1748 0.1919 0.0245 0.107 Uiso 1 1 calc R U . . .
H23C H 0.1988 0.0748 0.0615 0.107 Uiso 1 1 calc R U . . .
S1 S -0.07580(12) -0.30821(17) 0.09691(10) 0.1156(7) Uani 1 1 d . . . . .
C1 C -0.0457(2) -0.1990(4) 0.1452(2) 0.0551(10) Uani 1 1 d . . . . .
O3 O 1.0000 0.5261(9) 0.2500 0.255(8) Uani 1 2 d S T P . .
H H 0.052(2) 0.285(4) 0.0338(14) 0.068(14) Uiso 1 1 d D . . . .
H3 H 0.0630(18) 0.235(3) 0.2626(17) 0.043(10) Uiso 1 1 d D . . . .
H4 H 0.059(3) 0.359(3) 0.235(3) 0.10(2) Uiso 1 1 d D . . . .
H1 H 0.095(8) 0.05(2) 0.036(11) 0.60(18) Uiso 1 1 d D . . . .
H2 H 0.035(9) -0.026(9) 0.055(11) 0.45(12) Uiso 1 1 d 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
Ni2 O31 2.053(2) 2 ?
Ni2 O31 2.053(2) . ?
Ni2 N1 2.063(3) . ?
Ni2 N1 2.063(3) 2 ?
Ni2 O10 2.180(2) . ?
Ni2 O10 2.180(2) 2 ?
Ni1 O31 2.050(2) . ?
Ni1 N18 2.092(3) . ?
Ni1 O10 2.100(2) . ?
Ni1 O2 2.132(3) . ?
Ni1 N22 2.133(3) . ?
Ni1 O1 2.134(3) . ?
O31 C30 1.344(4) . ?
O10 C11 1.356(4) . ?
N18 C17 1.478(5) . ?
N18 C19 1.493(5) . ?
N22 C23 1.475(5) . ?
N22 C24 1.492(5) . ?
N22 C21 1.493(5) . ?
C16 C15 1.396(5) . ?
C16 C11 1.411(5) . ?
C16 C17 1.498(5) . ?
N1 C1 1.134(5) . ?
C11 C12 1.387(5) . ?
C29 C30 1.391(6) . ?
C29 C28 1.395(6) . ?
C12 C13 1.388(5) . ?
C15 C14 1.377(6) . ?
C24 C25 1.492(6) . ?
C14 C13 1.373(6) . ?
C25 C26 1.399(6) . ?
C25 C30 1.409(6) . ?
C21 C20 1.514(7) . ?
C26 C27 1.367(8) . ?
C19 C20 1.513(6) . ?
C27 C28 1.374(7) . ?
S1 C1 1.646(5) . ?

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
O31 Ni2 O31 160.72(14) 2 . ?
O31 Ni2 N1 98.88(11) 2 . ?
O31 Ni2 N1 94.68(11) . . ?
O31 Ni2 N1 94.68(11) 2 2 ?
O31 Ni2 N1 98.88(11) . 2 ?
N1 Ni2 N1 90.42(19) . 2 ?
O31 Ni2 O10 86.84(9) 2 . ?
O31 Ni2 O10 79.21(9) . . ?
N1 Ni2 O10 91.18(11) . . ?
N1 Ni2 O10 177.61(11) 2 . ?
O31 Ni2 O10 79.21(9) 2 2 ?
O31 Ni2 O10 86.84(9) . 2 ?
N1 Ni2 O10 177.61(11) . 2 ?
N1 Ni2 O10 91.18(11) 2 2 ?
O10 Ni2 O10 87.28(12) . 2 ?
O31 Ni1 N18 174.06(11) . . ?
O31 Ni1 O10 81.17(9) . . ?
N18 Ni1 O10 92.90(11) . . ?
O31 Ni1 O2 86.97(10) . . ?
N18 Ni1 O2 92.05(12) . . ?
O10 Ni1 O2 84.52(10) . . ?
O31 Ni1 N22 93.92(11) . . ?
N18 Ni1 N22 91.94(13) . . ?
O10 Ni1 N22 172.46(10) . . ?
O2 Ni1 N22 89.54(11) . . ?
O31 Ni1 O1 86.97(13) . . ?
N18 Ni1 O1 93.31(14) . . ?
O10 Ni1 O1 88.12(11) . . ?
O2 Ni1 O1 171.10(13) . . ?
N22 Ni1 O1 97.37(13) . . ?
C30 O31 Ni1 117.9(2) . . ?
C30 O31 Ni2 131.6(2) . . ?
Ni1 O31 Ni2 102.58(10) . . ?
C11 O10 Ni1 116.01(18) . . ?
C11 O10 Ni2 129.3(2) . . ?
Ni1 O10 Ni2 96.82(9) . . ?
C17 N18 C19 108.2(3) . . ?
C17 N18 Ni1 110.9(2) . . ?
C19 N18 Ni1 115.7(3) . . ?
C23 N22 C24 107.8(4) . . ?
C23 N22 C21 108.0(4) . . ?
C24 N22 C21 107.7(3) . . ?
C23 N22 Ni1 114.7(3) . . ?
C24 N22 Ni1 106.1(2) . . ?
C21 N22 Ni1 112.3(3) . . ?
C15 C16 C11 119.2(3) . . ?
C15 C16 C17 120.5(3) . . ?
C11 C16 C17 120.1(3) . . ?
C1 N1 Ni2 171.9(4) . . ?
O10 C11 C12 122.5(3) . . ?
O10 C11 C16 118.8(3) . . ?
C12 C11 C16 118.6(3) . . ?
C30 C29 C28 120.1(4) . . ?
C11 C12 C13 120.3(3) . . ?
C14 C15 C16 121.6(4) . . ?
C25 C24 N22 113.4(3) . . ?
C13 C14 C15 118.7(4) . . ?
C14 C13 C12 121.5(4) . . ?
C26 C25 C30 119.2(4) . . ?
C26 C25 C24 120.9(4) . . ?
C30 C25 C24 119.9(3) . . ?
N22 C21 C20 114.4(4) . . ?
N18 C17 C16 114.2(3) . . ?
C27 C26 C25 121.3(5) . . ?
N18 C19 C20 113.4(4) . . ?
C19 C20 C21 115.7(4) . . ?
O31 C30 C29 122.4(4) . . ?
O31 C30 C25 118.7(4) . . ?
C29 C30 C25 119.0(4) . . ?
C26 C27 C28 119.6(4) . . ?
C27 C28 C29 120.8(5) . . ?
N1 C1 S1 178.5(4) . . ?

_refine_diff_density_max         1.844
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.098



