# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1956983'
loop_
_audit_author_name
_audit_author_address
'Mitu Sharma and Biraj Borah'
;Tezpur University
India
;
_audit_update_record             
;
2021-04-08 deposited with the CCDC.	2021-04-29 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         ?
_chemical_formula_sum            'C25 H42 Cl2 N6 Ni2 O17'
_chemical_formula_weight         886.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   22.909(10)
_cell_length_b                   14.148(6)
_cell_length_c                   12.037(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.433(6)
_cell_angle_gamma                90
_cell_volume                     3824(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    25799
_cell_measurement_theta_min      2.292
_cell_measurement_theta_max      28.789

_exptl_crystal_description       needls
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_F_000             1840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.054
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.033
_exptl_absorpt_coefficient_mu    1.201
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.5134
_exptl_absorpt_correction_T_max  0.7174
_exptl_absorpt_process_details   ?
_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  Bruker
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25799
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.292
_diffrn_reflns_theta_max         28.789
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4906
_reflns_number_gt                3095
_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    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (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)+(0.1148P)²+4.7615P] 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     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0007(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4906
_refine_ls_number_parameters     315
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0629
_refine_ls_wR_factor_ref         0.2037
_refine_ls_wR_factor_gt          0.1710
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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 0.02764(2) 0.16797(3) 0.44087(4) 0.0311(2) Uani 1 1 d . . . . .
O1 O 0.000000 0.1787(2) 0.250000 0.0330(9) Uani 1 2 d S T P . .
O2 O 0.00836(13) 0.04433(18) 0.3460(2) 0.0359(7) Uani 1 1 d . . . . .
N1 N 0.11444(16) 0.1768(2) 0.4172(3) 0.0385(8) Uani 1 1 d . . . . .
C13 C 0.000000 0.0865(4) 0.250000 0.0296(11) Uani 1 2 d S T P . .
O3 O 0.0530(2) 0.1066(2) 0.5995(3) 0.0425(8) Uani 1 1 d . . . . .
N3 N -0.05527(17) 0.2092(3) 0.4757(3) 0.0403(8) Uani 1 1 d . . . . .
N2 N 0.04431(18) 0.3055(2) 0.5004(3) 0.0389(8) Uani 1 1 d . . . . .
C1 C 0.1429(2) 0.1162(4) 0.3582(4) 0.0472(11) Uani 1 1 d . . . . .
C11 C -0.0400(2) 0.2547(4) 0.5902(4) 0.0454(11) Uani 1 1 d . . . . .
C6 C 0.1102(2) 0.3205(3) 0.5238(4) 0.0481(12) Uani 1 1 d . . . . .
C5 C 0.1389(2) 0.2624(3) 0.4443(4) 0.0417(10) Uani 1 1 d . . . . .
C9 C -0.0841(2) 0.2791(3) 0.3895(4) 0.0456(11) Uani 1 1 d . . . . .
C7 C 0.0139(3) 0.3711(3) 0.4091(4) 0.0463(12) Uani 1 1 d . . . . .
C10 C 0.0170(3) 0.3133(4) 0.6038(4) 0.0485(12) Uani 1 1 d . . . . .
C8 C -0.0526(3) 0.3750(3) 0.3988(5) 0.0498(12) Uani 1 1 d . . . . .
C4 C 0.1891(2) 0.2930(4) 0.4063(5) 0.0537(13) Uani 1 1 d . . . . .
C12 C -0.0978(2) 0.1287(4) 0.4786(5) 0.0518(12) Uani 1 1 d . . . . .
H12A H -0.079665 0.083067 0.533902 0.078 Uiso 1 1 calc R U . . .
H12B H -0.133617 0.152232 0.498574 0.078 Uiso 1 1 calc R U . . .
H12C H -0.107119 0.099356 0.405344 0.078 Uiso 1 1 calc R U . . .
C3 C 0.2172(2) 0.2307(5) 0.3449(5) 0.0616(15) Uani 1 1 d . . . . .
O8 O 0.1744(2) 0.0805(4) 0.6724(6) 0.113(2) Uani 1 1 d G . . . .
C2 C 0.1942(2) 0.1393(5) 0.3223(5) 0.0592(14) Uani 1 1 d . . . . .
Cl1 Cl 0.17629(8) 0.56879(12) 0.34795(17) 0.0771(5) Uani 1 1 d . . . . .
O6 O 0.1782(3) 0.6638(4) 0.3273(8) 0.142(3) Uani 1 1 d . . . . .
O7 O 0.2290(4) 0.5359(6) 0.4155(7) 0.190(4) Uani 1 1 d . . . . .
O9 O 0.2270(4) 0.1467(6) 0.8751(7) 0.158(3) Uani 1 1 d G . . . .
O4 O 0.1282(5) 0.5382(5) 0.3809(12) 0.249(7) Uani 1 1 d . . . . .
O5 O 0.1837(5) 0.5224(8) 0.2452(10) 0.226(5) Uani 1 1 d . . . . .
H4 H 0.2053(17) 0.353(3) 0.430(3) 0.019(9) Uiso 1 1 d . . . . .
H1 H 0.1254(18) 0.057(3) 0.349(3) 0.026(10) Uiso 1 1 d . . . . .
H6A H 0.126(2) 0.309(4) 0.604(5) 0.050(14) Uiso 1 1 d . . . . .
H3 H 0.256(3) 0.257(4) 0.325(5) 0.067(17) Uiso 1 1 d . . . . .
H2 H 0.211(3) 0.085(5) 0.281(6) 0.10(2) Uiso 1 1 d . . . . .
H6B H 0.122(2) 0.396(4) 0.519(4) 0.054(14) Uiso 1 1 d . . . . .
H10A H 0.007(2) 0.380(4) 0.617(5) 0.056(15) Uiso 1 1 d . . . . .
H10B H 0.048(2) 0.283(3) 0.663(4) 0.046(13) Uiso 1 1 d . . . . .
H7A H 0.020(2) 0.348(3) 0.332(4) 0.040(13) Uiso 1 1 d . . . . .
H7B H 0.021(4) 0.423(6) 0.403(7) 0.12(3) Uiso 1 1 d . . . . .
H9A H -0.087(2) 0.254(3) 0.321(4) 0.038(12) Uiso 1 1 d . . . . .
H8A H -0.066(2) 0.402(3) 0.329(4) 0.037(12) Uiso 1 1 d . . . . .
H9B H -0.123(2) 0.285(3) 0.396(4) 0.043(13) Uiso 1 1 d . . . . .
H8B H -0.065(2) 0.407(4) 0.476(5) 0.055(14) Uiso 1 1 d . . . . .
H11A H -0.0334(19) 0.207(3) 0.642(4) 0.030(11) Uiso 1 1 d . . . . .
H11B H -0.069(2) 0.290(3) 0.605(4) 0.032(11) Uiso 1 1 d . . . . .
H3A H 0.0803(17) 0.097(3) 0.608(3) 0.005(11) Uiso 1 1 d . . . . .
H3B H 0.031(3) 0.058(5) 0.619(6) 0.10(2) 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 2.068(4) . ?
Ni1 O3 2.073(4) . ?
Ni1 N2 2.082(4) . ?
Ni1 O2 2.088(3) . ?
Ni1 N3 2.107(4) . ?
Ni1 O1 2.2641(11) . ?
O1 C13 1.305(6) . ?
O2 C13 1.280(4) . ?
N1 C5 1.347(5) . ?
N1 C1 1.360(6) . ?
O3 H3A 0.63(4) . ?
O3 H3B 0.91(8) . ?
N3 C9 1.490(6) . ?
N3 C11 1.499(6) . ?
N3 C12 1.503(6) . ?
N2 C6 1.494(6) . ?
N2 C7 1.500(6) . ?
N2 C10 1.504(6) . ?
C1 C2 1.370(7) . ?
C1 H1 0.93(4) . ?
C11 C10 1.528(8) . ?
C11 H11A 0.91(5) . ?
C11 H11B 0.88(5) . ?
C6 C5 1.508(7) . ?
C6 H6A 0.97(5) . ?
C6 H6B 1.11(5) . ?
C5 C4 1.390(7) . ?
C9 C8 1.530(7) . ?
C9 H9A 0.89(5) . ?
C9 H9B 0.90(5) . ?
C7 C8 1.504(8) . ?
C7 H7A 1.03(5) . ?
C7 H7B 0.76(9) . ?
C10 H10A 0.99(6) . ?
C10 H10B 1.00(5) . ?
C8 H8A 0.92(5) . ?
C8 H8B 1.12(5) . ?
C4 C3 1.388(8) . ?
C4 H4 0.94(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C3 C2 1.401(9) . ?
C3 H3 1.04(6) . ?
C2 H2 1.04(7) . ?
Cl1 O4 1.315(7) . ?
Cl1 O6 1.370(5) . ?
Cl1 O7 1.395(8) . ?
Cl1 O5 1.440(9) . ?

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 O3 92.90(16) . . ?
N1 Ni1 N2 82.83(15) . . ?
O3 Ni1 N2 94.35(14) . . ?
N1 Ni1 O2 94.60(13) . . ?
O3 Ni1 O2 98.24(12) . . ?
N2 Ni1 O2 167.27(12) . . ?
N1 Ni1 N3 160.09(15) . . ?
O3 Ni1 N3 91.82(16) . . ?
N2 Ni1 N3 77.53(15) . . ?
O2 Ni1 N3 103.85(13) . . ?
N1 Ni1 O1 86.53(11) . . ?
O3 Ni1 O1 159.04(13) . . ?
N2 Ni1 O1 106.34(13) . . ?
O2 Ni1 O1 60.98(11) . . ?
N3 Ni1 O1 95.81(11) . . ?
C13 O1 Ni1 86.14(9) . 2 ?
C13 O1 Ni1 86.14(9) . . ?
Ni1 O1 Ni1 172.28(17) 2 . ?
C13 O2 Ni1 94.6(2) . . ?
C5 N1 C1 118.3(4) . . ?
C5 N1 Ni1 112.7(3) . . ?
C1 N1 Ni1 127.5(3) . . ?
O2 C13 O2 124.5(5) 2 . ?
O2 C13 O1 117.8(2) 2 . ?
O2 C13 O1 117.8(2) . . ?
Ni1 O3 H3A 109(4) . . ?
Ni1 O3 H3B 119(5) . . ?
H3A O3 H3B 112(6) . . ?
C9 N3 C11 110.2(4) . . ?
C9 N3 C12 108.7(4) . . ?
C11 N3 C12 109.7(4) . . ?
C9 N3 Ni1 109.8(3) . . ?
C11 N3 Ni1 104.3(3) . . ?
C12 N3 Ni1 114.1(3) . . ?
C6 N2 C7 110.8(4) . . ?
C6 N2 C10 113.8(4) . . ?
C7 N2 C10 110.6(4) . . ?
C6 N2 Ni1 107.9(3) . . ?
C7 N2 Ni1 107.4(3) . . ?
C10 N2 Ni1 106.0(3) . . ?
N1 C1 C2 123.0(5) . . ?
N1 C1 H1 113(3) . . ?
C2 C1 H1 124(3) . . ?
N3 C11 C10 111.7(4) . . ?
N3 C11 H11A 107(3) . . ?
C10 C11 H11A 108(3) . . ?
N3 C11 H11B 112(3) . . ?
C10 C11 H11B 109(3) . . ?
H11A C11 H11B 109(4) . . ?
N2 C6 C5 110.7(4) . . ?
N2 C6 H6A 109(3) . . ?
C5 C6 H6A 114(3) . . ?
N2 C6 H6B 112(3) . . ?
C5 C6 H6B 111(3) . . ?
H6A C6 H6B 100(4) . . ?
N1 C5 C4 122.1(5) . . ?
N1 C5 C6 115.6(4) . . ?
C4 C5 C6 122.2(4) . . ?
N3 C9 C8 113.6(4) . . ?
N3 C9 H9A 109(3) . . ?
C8 C9 H9A 111(3) . . ?
N3 C9 H9B 108(3) . . ?
C8 C9 H9B 112(3) . . ?
H9A C9 H9B 103(4) . . ?
N2 C7 C8 113.4(4) . . ?
N2 C7 H7A 110(3) . . ?
C8 C7 H7A 105(3) . . ?
N2 C7 H7B 126(6) . . ?
C8 C7 H7B 101(6) . . ?
H7A C7 H7B 99(7) . . ?
N2 C10 C11 111.0(4) . . ?
N2 C10 H10A 110(3) . . ?
C11 C10 H10A 109(3) . . ?
N2 C10 H10B 102(3) . . ?
C11 C10 H10B 108(3) . . ?
H10A C10 H10B 116(4) . . ?
C7 C8 C9 115.5(4) . . ?
C7 C8 H8A 104(3) . . ?
C9 C8 H8A 104(3) . . ?
C7 C8 H8B 111(3) . . ?
C9 C8 H8B 103(3) . . ?
H8A C8 H8B 120(4) . . ?
C3 C4 C5 118.6(5) . . ?
C3 C4 H4 122(2) . . ?
C5 C4 H4 119(2) . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C4 C3 C2 119.6(5) . . ?
C4 C3 H3 114(3) . . ?
C2 C3 H3 126(3) . . ?
C1 C2 C3 118.1(6) . . ?
C1 C2 H2 114(4) . . ?
C3 C2 H2 128(4) . . ?
O4 Cl1 O6 115.9(4) . . ?
O4 Cl1 O7 113.2(7) . . ?
O6 Cl1 O7 112.2(5) . . ?
O4 Cl1 O5 110.9(7) . . ?
O6 Cl1 O5 106.2(6) . . ?
O7 Cl1 O5 96.5(7) . . ?

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
Ni1 O2 C13 O2 173.04(16) . . . 2 ?
Ni1 O2 C13 O1 -6.96(16) . . . . ?
Ni1 O1 C13 O2 6.41(15) 2 . . 2 ?
Ni1 O1 C13 O2 -173.59(15) . . . 2 ?
Ni1 O1 C13 O2 -173.59(15) 2 . . . ?
Ni1 O1 C13 O2 6.41(15) . . . . ?
C5 N1 C1 C2 -1.9(7) . . . . ?
Ni1 N1 C1 C2 162.6(4) . . . . ?
C9 N3 C11 C10 -79.3(5) . . . . ?
C12 N3 C11 C10 161.1(4) . . . . ?
Ni1 N3 C11 C10 38.5(4) . . . . ?
C7 N2 C6 C5 -86.4(5) . . . . ?
C10 N2 C6 C5 148.3(4) . . . . ?
Ni1 N2 C6 C5 31.0(4) . . . . ?
C1 N1 C5 C4 5.2(7) . . . . ?
Ni1 N1 C5 C4 -161.6(4) . . . . ?
C1 N1 C5 C6 -171.5(4) . . . . ?
Ni1 N1 C5 C6 21.8(5) . . . . ?
N2 C6 C5 N1 -36.1(5) . . . . ?
N2 C6 C5 C4 147.2(4) . . . . ?
C11 N3 C9 C8 45.2(6) . . . . ?
C12 N3 C9 C8 165.4(4) . . . . ?
Ni1 N3 C9 C8 -69.2(5) . . . . ?
C6 N2 C7 C8 -167.4(4) . . . . ?
C10 N2 C7 C8 -40.3(5) . . . . ?
Ni1 N2 C7 C8 74.9(4) . . . . ?
C6 N2 C10 C11 -153.2(4) . . . . ?
C7 N2 C10 C11 81.4(5) . . . . ?
Ni1 N2 C10 C11 -34.8(5) . . . . ?
N3 C11 C10 N2 -3.0(6) . . . . ?
N2 C7 C8 C9 -51.0(6) . . . . ?
N3 C9 C8 C7 47.9(6) . . . . ?
N1 C5 C4 C3 -4.4(7) . . . . ?
C6 C5 C4 C3 172.1(5) . . . . ?
C5 C4 C3 C2 0.3(8) . . . . ?
N1 C1 C2 C3 -2.0(9) . . . . ?
C4 C3 C2 C1 2.7(9) . . . . ?

_refine_diff_density_max         0.959
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.107



