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#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/65/1546581.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_1546581
loop_
_publ_author_name
'Xue, Dan'
'Luo, Su-Ping'
'Zhan, Shu-Zhong'
_publ_section_title
;
 A coordinatively saturated nickel complex supported by triazenido
 ligands: a new electrocatalyst for hydrogen generation via
 ligand-centered proton-transfer
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8503
_journal_page_last               8508
_journal_paper_doi               10.1039/C7NJ01705G
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C28 H16 N10 Ni S4'
_chemical_formula_weight         679.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-05-04 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.256(8)
_cell_length_b                   10.256(8)
_cell_length_c                   13.160(10)
_cell_measurement_reflns_used    1221
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.52
_cell_volume                     1384.2(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2740
_diffrn_reflns_av_sigmaI/netI    0.1433
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5830
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    1.044
_exptl_absorpt_correction_T_max  0.9400
_exptl_absorpt_correction_T_min  0.8850
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.365
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0151P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                1108
_reflns_number_total             1221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj01705g2.cif
_cod_data_source_block           m101024e1
_cod_original_sg_symbol_H-M      i_-4
_cod_database_code               1546581
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.0000 1.0000 0.0000 0.0350(4) Uani 1 4 d S
S1 S 0.1424(2) 0.66032(19) 0.18361(13) 0.0493(5) Uani 1 1 d .
N1 N 0.0752(5) 0.8171(5) 0.0388(4) 0.0388(13) Uani 1 1 d .
N2 N 0.0408(6) 0.8999(6) 0.2080(4) 0.0467(14) Uani 1 1 d .
N3 N 0.0000 1.0000 0.1558(5) 0.0375(16) Uani 1 2 d S
C1 C 0.1212(6) 0.7062(6) -0.0080(6) 0.0405(14) Uani 1 1 d .
C2 C 0.1313(7) 0.6896(7) -0.1132(6) 0.0482(17) Uani 1 1 d .
H2 H 0.1033 0.7559 -0.1586 0.058 Uiso 1 1 calc R
C3 C 0.1829(10) 0.5742(8) -0.1491(6) 0.067(2) Uani 1 1 d .
H3 H 0.1908 0.5604 -0.2202 0.080 Uiso 1 1 calc R
C4 C 0.2242(10) 0.4764(9) -0.0804(7) 0.073(3) Uani 1 1 d .
H4 H 0.2590 0.3975 -0.1068 0.088 Uiso 1 1 calc R
C5 C 0.2159(9) 0.4912(8) 0.0222(5) 0.060(2) Uani 1 1 d .
H5 H 0.2448 0.4243 0.0668 0.072 Uiso 1 1 calc R
C6 C 0.1636(7) 0.6078(7) 0.0605(5) 0.0485(17) Uani 1 1 d .
C7 C 0.0788(6) 0.8063(7) 0.1359(5) 0.0428(16) Uani 1 1 d .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N3 Ni1 N3 180.000(1) 2_465 .
N3 Ni1 N1 75.87(14) 2_465 2_465
N3 Ni1 N1 104.13(14) . 2_465
N3 Ni1 N1 75.87(14) 2_465 4_665
N3 Ni1 N1 104.13(14) . 4_665
N1 Ni1 N1 151.7(3) 2_465 4_665
N3 Ni1 N1 104.13(14) 2_465 .
N3 Ni1 N1 75.87(14) . .
N1 Ni1 N1 93.42(7) 2_465 .
N1 Ni1 N1 93.42(7) 4_665 .
N3 Ni1 N1 104.13(14) 2_465 3_575
N3 Ni1 N1 75.87(14) . 3_575
N1 Ni1 N1 93.42(7) 2_465 3_575
N1 Ni1 N1 93.42(7) 4_665 3_575
N1 Ni1 N1 151.7(3) . 3_575
C6 S1 C7 88.7(3) . .
C7 N1 C1 111.4(6) . .
C7 N1 Ni1 109.3(5) . .
C1 N1 Ni1 139.3(4) . .
N3 N2 C7 105.7(5) . .
N2 N3 N2 116.5(6) . 3_575
N2 N3 Ni1 121.8(3) . .
N2 N3 Ni1 121.8(3) 3_575 .
N1 C1 C2 124.7(6) . .
N1 C1 C6 114.0(6) . .
C2 C1 C6 121.3(7) . .
C3 C2 C1 118.2(7) . .
C3 C2 H2 120.9 . .
C1 C2 H2 120.9 . .
C2 C3 C4 120.2(7) . .
C2 C3 H3 119.9 . .
C4 C3 H3 119.9 . .
C5 C4 C3 122.4(7) . .
C5 C4 H4 118.8 . .
C3 C4 H4 118.8 . .
C4 C5 C6 118.4(7) . .
C4 C5 H5 120.8 . .
C6 C5 H5 120.8 . .
C5 C6 C1 119.6(7) . .
C5 C6 S1 130.8(6) . .
C1 C6 S1 109.6(5) . .
N1 C7 N2 127.3(7) . .
N1 C7 S1 116.2(5) . .
N2 C7 S1 116.5(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N3 2.051(6) 2_465
Ni1 N3 2.051(6) .
Ni1 N1 2.092(6) 2_465
Ni1 N1 2.092(6) 4_665
Ni1 N1 2.092(6) .
Ni1 N1 2.092(6) 3_575
S1 C6 1.721(7) .
S1 C7 1.750(7) .
N1 C7 1.284(8) .
N1 C1 1.377(8) .
N2 N3 1.305(6) .
N2 C7 1.404(9) .
N3 N2 1.305(6) 3_575
C1 C2 1.398(10) .
C1 C6 1.422(10) .
C2 C3 1.380(10) .
C2 H2 0.9500 .
C3 C4 1.416(11) .
C3 H3 0.9500 .
C4 C5 1.361(12) .
C4 H4 0.9500 .
C5 C6 1.404(10) .
C5 H5 0.9500 .
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_4
N3 Ni1 N1 C7 -179.7(4) 2_465 .
N3 Ni1 N1 C7 0.3(4) . .
N1 Ni1 N1 C7 -103.4(4) 2_465 .
N1 Ni1 N1 C7 104.1(4) 4_665 .
N1 Ni1 N1 C7 0.3(4) 3_575 .
N3 Ni1 N1 C1 0.3(7) 2_465 .
N3 Ni1 N1 C1 -179.7(7) . .
N1 Ni1 N1 C1 76.5(7) 2_465 .
N1 Ni1 N1 C1 -76.0(7) 4_665 .
N1 Ni1 N1 C1 -179.7(7) 3_575 .
C7 N2 N3 N2 179.9(6) . 3_575
C7 N2 N3 Ni1 -0.1(6) . .
N3 Ni1 N3 N2 0(100) 2_465 .
N1 Ni1 N3 N2 89.8(4) 2_465 .
N1 Ni1 N3 N2 -90.2(4) 4_665 .
N1 Ni1 N3 N2 -0.2(4) . .
N1 Ni1 N3 N2 179.8(4) 3_575 .
N3 Ni1 N3 N2 0(100) 2_465 3_575
N1 Ni1 N3 N2 -90.2(4) 2_465 3_575
N1 Ni1 N3 N2 89.8(4) 4_665 3_575
N1 Ni1 N3 N2 179.8(4) . 3_575
N1 Ni1 N3 N2 -0.2(4) 3_575 3_575
C7 N1 C1 C2 -178.9(6) . .
Ni1 N1 C1 C2 1.2(11) . .
C7 N1 C1 C6 -1.1(8) . .
Ni1 N1 C1 C6 179.0(5) . .
N1 C1 C2 C3 178.1(7) . .
C6 C1 C2 C3 0.5(12) . .
C1 C2 C3 C4 -0.1(14) . .
C2 C3 C4 C5 -0.4(16) . .
C3 C4 C5 C6 0.4(15) . .
C4 C5 C6 C1 0.0(12) . .
C4 C5 C6 S1 -178.3(7) . .
N1 C1 C6 C5 -178.3(7) . .
C2 C1 C6 C5 -0.5(11) . .
N1 C1 C6 S1 0.3(8) . .
C2 C1 C6 S1 178.2(6) . .
C7 S1 C6 C5 178.8(8) . .
C7 S1 C6 C1 0.3(5) . .
C1 N1 C7 N2 179.5(7) . .
Ni1 N1 C7 N2 -0.6(9) . .
C1 N1 C7 S1 1.3(8) . .
Ni1 N1 C7 S1 -178.7(3) . .
N3 N2 C7 N1 0.5(9) . .
N3 N2 C7 S1 178.6(4) . .
C6 S1 C7 N1 -1.0(6) . .
C6 S1 C7 N2 -179.3(6) . .
