#------------------------------------------------------------------------------
#$Date: 2021-05-05 11:36:27 +0300 (Wed, 05 May 2021) $
#$Revision: 264897 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/68/7706869.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7706869
loop_
_publ_author_name
'Adhikari, Suman'
'Bhattacharjee, Tirtha'
'Bhattacharjee, Sharmila'
'Daniliuc, Constantin Gabriel'
'Frontera, Antonio'
'Lopato, Eric M.'
'Bernhard, Stefan'
_publ_section_title
;
 Nickel(II) complexes based on dithiolate-polyamine binary ligand systems:
 crystal structures, hirshfeld surface analysis, theoretical study, and
 catalytic activity study on photocatalytic hydrogen generation.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5632
_journal_page_last               5643
_journal_paper_doi               10.1039/d1dt00352f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_sum            'C16 H26 N10 Ni2 S4'
_chemical_formula_weight         604.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           'APEX3 v2016.1-0'
_audit_update_record
;
2021-01-06 deposited with the CCDC.	2021-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.143(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3199(6)
_cell_length_b                   9.1021(3)
_cell_length_c                   18.1332(7)
_cell_measurement_reflns_used    2872
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     2457.99(16)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection
;

Collect (Nonius B.V., 1998)
;
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'rotating anode Nonius FR591'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10388
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         4.37
_diffrn_source                   'Mo rotating anode'
_diffrn_source_type              'Mo rotating anode'
_exptl_absorpt_coefficient_mu    1.898
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.430
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0495
_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)+(0.0342P)²+12.9855P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1148
_reflns_number_gt                2344
_reflns_number_total             2999
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00352f2.cif
_cod_data_source_block           dan9415
_cod_depositor_comments
'Adding full bibliography for 7706868--7706870.cif.'
_cod_database_code               7706869
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'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni2 0.5 0.85978(7) 0.25 0.02073(16) Uani d T P S 1 . .
Ni Ni1 0.5 0.5 0 0.02568(18) Uani d . P S 1 . .
S S1 0.47903(6) 0.37137(10) 0.09440(6) 0.0291(2) Uani d . . . 1 . .
S S2 0.36043(6) 0.56121(12) -0.02367(6) 0.0331(2) Uani d . . . 1 . .
N N1 0.3242(2) 0.2014(4) 0.1817(2) 0.0418(9) Uani d . . . 1 . .
N N2 0.1408(2) 0.4883(4) -0.01320(19) 0.0364(8) Uani d . . . 1 . .
N N3 0.5310(2) 1.0182(4) 0.1823(2) 0.0255(6) Uani d . . . 1 . .
H H3A 0.481(3) 1.042(5) 0.142(3) 0.040(13) Uiso d . . . 1 . .
H H3B 0.552(4) 1.089(6) 0.212(3) 0.063(17) Uiso d . . . 1 . .
N N4 0.5505(2) 0.7135(4) 0.18644(18) 0.0273(7) Uani d . . . 1 . .
H H4 0.513(3) 0.647(4) 0.159(2) 0.026(10) Uiso d . . . 1 . .
N N5 0.6360(2) 0.8362(4) 0.3388(2) 0.0281(7) Uani d . . . 1 . .
H H5A 0.630(3) 0.806(6) 0.382(3) 0.051(15) Uiso d . . . 1 . .
H H5B 0.662(3) 0.912(5) 0.350(2) 0.026(11) Uiso d . . . 1 . .
C C1 0.3700(2) 0.4338(4) 0.0501(2) 0.0259(7) Uani d . . . 1 . .
C C2 0.3001(2) 0.3897(4) 0.0692(2) 0.0261(7) Uani d . . . 1 . .
C C3 0.3133(2) 0.2844(4) 0.1314(2) 0.0303(8) Uani d . . . 1 . .
C C4 0.2115(2) 0.4445(4) 0.0240(2) 0.0258(8) Uani d . . . 1 . .
C C11 0.5936(3) 0.9585(4) 0.1506(2) 0.0334(9) Uani d . . . 1 . .
H H11A 0.6557 0.9631 0.1928 0.04 Uiso calc U . R 1 . .
H H11B 0.5907 1.0174 0.1037 0.04 Uiso calc U . R 1 . .
C C12 0.5681(3) 0.7997(5) 0.1250(2) 0.0343(9) Uani d . . . 1 . .
H H12A 0.5137 0.7983 0.0736 0.041 Uiso calc U . R 1 . .
H H12B 0.6174 0.7525 0.1152 0.041 Uiso calc U . R 1 . .
C C13 0.6903(2) 0.7426(5) 0.3097(2) 0.0341(9) Uani d . . . 1 . .
H H13A 0.7348 0.6869 0.3554 0.041 Uiso calc U . R 1 . .
H H13B 0.7232 0.8047 0.2861 0.041 Uiso calc U . R 1 . .
C C14 0.6296(3) 0.6370(5) 0.2465(2) 0.0371(9) Uani d . . . 1 . .
H H14A 0.6637 0.5897 0.2186 0.045 Uiso calc U . R 1 . .
H H14B 0.6092 0.559 0.2732 0.045 Uiso calc U . R 1 . .
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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3 Ni2 N3 . 2_655 92.57(19) ?
N3 Ni2 N4 . 2_655 171.53(13) ?
N3 Ni2 N4 2_655 2_655 82.70(13) ?
N3 Ni2 N4 . . 82.70(13) ?
N3 Ni2 N4 2_655 . 171.53(13) ?
N4 Ni2 N4 2_655 . 102.83(18) ?
N3 Ni2 N5 . 2_655 93.00(13) ?
N3 Ni2 N5 2_655 2_655 94.91(14) ?
N4 Ni2 N5 2_655 2_655 80.46(12) ?
N4 Ni2 N5 . 2_655 92.36(14) ?
N3 Ni2 N5 . . 94.91(14) ?
N3 Ni2 N5 2_655 . 93.00(13) ?
N4 Ni2 N5 2_655 . 92.36(14) ?
N4 Ni2 N5 . . 80.46(12) ?
N5 Ni2 N5 2_655 . 168.5(2) ?
S2 Ni1 S2 5_665 . 180.0 ?
S2 Ni1 S1 5_665 5_665 79.07(4) ?
S2 Ni1 S1 . 5_665 100.93(4) ?
S2 Ni1 S1 5_665 . 100.93(4) ?
S2 Ni1 S1 . . 79.07(4) ?
S1 Ni1 S1 5_665 . 180.0 ?
C1 S1 Ni1 . . 85.53(13) ?
C1 S2 Ni1 . . 85.44(13) ?
C11 N3 Ni2 . . 110.5(2) ?
C11 N3 H3A . . 109.(3) ?
Ni2 N3 H3A . . 107.(3) ?
C11 N3 H3B . . 112.(4) ?
Ni2 N3 H3B . . 108.(4) ?
H3A N3 H3B . . 111.(5) ?
C14 N4 C12 . . 115.1(3) ?
C14 N4 Ni2 . . 108.0(2) ?
C12 N4 Ni2 . . 108.1(2) ?
C14 N4 H4 . . 107.(3) ?
C12 N4 H4 . . 104.(3) ?
Ni2 N4 H4 . . 115.(3) ?
C13 N5 Ni2 . . 112.1(2) ?
C13 N5 H5A . . 117.(3) ?
Ni2 N5 H5A . . 104.(3) ?
C13 N5 H5B . . 105.(3) ?
Ni2 N5 H5B . . 113.(3) ?
H5A N5 H5B . . 107.(4) ?
C2 C1 S1 . . 126.2(3) ?
C2 C1 S2 . . 124.5(3) ?
S1 C1 S2 . . 109.4(2) ?
C1 C2 C4 . . 120.1(3) ?
C1 C2 C3 . . 121.3(3) ?
C4 C2 C3 . . 118.6(3) ?
N1 C3 C2 . . 179.3(5) ?
N2 C4 C2 . . 179.0(4) ?
N3 C11 C12 . . 108.9(3) ?
N3 C11 H11A . . 109.9 ?
C12 C11 H11A . . 109.9 ?
N3 C11 H11B . . 109.9 ?
C12 C11 H11B . . 109.9 ?
H11A C11 H11B . . 108.3 ?
N4 C12 C11 . . 112.7(3) ?
N4 C12 H12A . . 109.1 ?
C11 C12 H12A . . 109.1 ?
N4 C12 H12B . . 109.1 ?
C11 C12 H12B . . 109.1 ?
H12A C12 H12B . . 107.8 ?
N5 C13 C14 . . 109.6(3) ?
N5 C13 H13A . . 109.8 ?
C14 C13 H13A . . 109.8 ?
N5 C13 H13B . . 109.8 ?
C14 C13 H13B . . 109.8 ?
H13A C13 H13B . . 108.2 ?
N4 C14 C13 . . 111.3(3) ?
N4 C14 H14A . . 109.4 ?
C13 C14 H14A . . 109.4 ?
N4 C14 H14B . . 109.4 ?
C13 C14 H14B . . 109.4 ?
H14A C14 H14B . . 108.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni2 N3 . 2.086(3) ?
Ni2 N3 2_655 2.086(3) ?
Ni2 N4 2_655 2.135(3) ?
Ni2 N4 . 2.135(3) ?
Ni2 N5 2_655 2.154(3) ?
Ni2 N5 . 2.154(3) ?
Ni1 S2 5_665 2.2098(10) ?
Ni1 S2 . 2.2098(10) ?
Ni1 S1 5_665 2.2129(10) ?
Ni1 S1 . 2.2130(10) ?
S1 C1 . 1.721(4) ?
S2 C1 . 1.729(4) ?
N1 C3 . 1.142(5) ?
N2 C4 . 1.145(5) ?
N3 C11 . 1.464(5) ?
N3 H3A . 0.87(5) ?
N3 H3B . 0.82(6) ?
N4 C14 . 1.478(5) ?
N4 C12 . 1.483(5) ?
N4 H4 . 0.86(4) ?
N5 C13 . 1.474(5) ?
N5 H5A . 0.87(5) ?
N5 H5B . 0.80(4) ?
C1 C2 . 1.381(5) ?
C2 C4 . 1.428(5) ?
C2 C3 . 1.428(5) ?
C11 C12 . 1.523(6) ?
C11 H11A . 0.99 ?
C11 H11B . 0.99 ?
C12 H12A . 0.99 ?
C12 H12B . 0.99 ?
C13 C14 . 1.513(5) ?
C13 H13A . 0.99 ?
C13 H13B . 0.99 ?
C14 H14A . 0.99 ?
C14 H14B . 0.99 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N3 H3A N2 7_565 0.87(5) 2.39(5) 3.198(5) 156.(4) ?
N3 H3B N1 2_665 0.82(6) 2.38(6) 3.111(5) 150.(5) ?
N4 H4 S1 . 0.86(4) 2.72(4) 3.500(3) 151.(3) ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Ni1 S1 C1 C2 . . . . 172.8(3) ?
Ni1 S1 C1 S2 . . . . -6.76(16) ?
Ni1 S2 C1 C2 . . . . -172.8(3) ?
Ni1 S2 C1 S1 . . . . 6.77(16) ?
S1 C1 C2 C4 . . . . -176.3(3) ?
S2 C1 C2 C4 . . . . 3.2(5) ?
S1 C1 C2 C3 . . . . 0.9(6) ?
S2 C1 C2 C3 . . . . -179.6(3) ?
Ni2 N3 C11 C12 . . . . 38.7(4) ?
C14 N4 C12 C11 . . . . -90.8(4) ?
Ni2 N4 C12 C11 . . . . 30.0(4) ?
N3 C11 C12 N4 . . . . -46.3(4) ?
Ni2 N5 C13 C14 . . . . -26.1(4) ?
C12 N4 C14 C13 . . . . 77.0(4) ?
Ni2 N4 C14 C13 . . . . -43.9(4) ?
N5 C13 C14 N4 . . . . 46.9(5) ?
