#------------------------------------------------------------------------------
#$Date: 2024-07-05 19:16:04 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293049 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/57/7715757.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_7715757
loop_
_publ_author_name
'Gao, Yan'
'Xu, Lei'
'Feng, Zi-Heng'
'Qian, Yin'
'Tian, Zheng-Fang'
'Ren, Xiao-Ming'
_publ_section_title
;
 Polymorph transformation in a mixed-stacking nickel-dithiolene complex
 with the derivative of 4,4'-bipyridinium.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8202
_journal_page_last               8213
_journal_paper_doi               10.1039/d4dt00324a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C8 N4 Ni S4, C18 H26 N2'
_chemical_formula_sum            'C26 H26 N6 Ni S4'
_chemical_formula_weight         609.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-15 deposited with the CCDC.	2024-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.664(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.864(2)
_cell_length_b                   8.089(2)
_cell_length_c                   20.473(5)
_cell_measurement_reflns_used    1853
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.724
_cell_measurement_theta_min      2.712
_cell_volume                     1451.2(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.00
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.983
_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_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_unetI/netI     0.0822
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12093
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_min         2.324
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1022 before and 0.0689 after correction.
The Ratio of minimum to maximum transmission is 0.6857.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1246
_refine_ls_R_factor_gt           0.0538
_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)+(0.0312P)²+0.3986P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1579
_reflns_number_total             2928
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00324a2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7715756--7715757.cif.'
_cod_original_cell_volume        1451.1(7)
_cod_database_code               7715757
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.695
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
2.b Me refined with riding coordinates:
 C13(H13A,H13B,H13C)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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_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 0.500000 0.000000 0.500000 0.0619(3) Uani 1 2 d S . P . .
S1 S 0.37436(14) 0.23217(13) 0.49582(5) 0.0702(4) Uani 1 1 d . . . . .
S2 S 0.45915(14) -0.05076(13) 0.60015(5) 0.0740(4) Uani 1 1 d . . . . .
N1 N 0.1351(5) 0.4758(5) 0.5942(2) 0.0985(14) Uani 1 1 d . . . . .
N2 N 0.2379(6) 0.1211(5) 0.7257(2) 0.1174(17) Uani 1 1 d . . . . .
N3 N 0.2123(4) 0.2468(4) 0.90669(17) 0.0663(9) Uani 1 1 d . . . . .
C1 C 0.2132(6) 0.3691(6) 0.5845(2) 0.0710(12) Uani 1 1 d . . . . .
C2 C 0.3078(5) 0.2342(5) 0.57107(19) 0.0652(11) Uani 1 1 d . . . . .
C3 C 0.3441(5) 0.1122(5) 0.6160(2) 0.0660(11) Uani 1 1 d . . . . .
C4 C 0.2868(6) 0.1169(5) 0.6777(2) 0.0819(14) Uani 1 1 d . . . . .
C5 C 0.1452(5) 0.1095(6) 0.8807(2) 0.0766(13) Uani 1 1 d . . . . .
H5 H 0.155153 0.079918 0.837690 0.092 Uiso 1 1 calc R U . . .
C6 C 0.0625(5) 0.0119(5) 0.9161(2) 0.0739(12) Uani 1 1 d . . . . .
H6 H 0.017001 -0.083672 0.897078 0.089 Uiso 1 1 calc R U . . .
C7 C 0.0449(5) 0.0529(5) 0.98021(19) 0.0598(11) Uani 1 1 d . . . . .
C8 C 0.1158(5) 0.1937(5) 1.0056(2) 0.0737(12) Uani 1 1 d . . . . .
H8 H 0.106987 0.225875 1.048489 0.088 Uiso 1 1 calc R U . . .
C9 C 0.1996(5) 0.2880(5) 0.9688(2) 0.0755(13) Uani 1 1 d . . . . .
H9 H 0.248547 0.382369 0.987292 0.091 Uiso 1 1 calc R U . . .
C10 C 0.3038(5) 0.3502(6) 0.8681(2) 0.0837(14) Uani 1 1 d . . . . .
H10A H 0.351393 0.280276 0.838592 0.100 Uiso 1 1 calc R U . . .
H10B H 0.384338 0.403975 0.898026 0.100 Uiso 1 1 calc R U . . .
C11 C 0.2097(6) 0.4785(5) 0.8287(2) 0.0891(15) Uani 1 1 d . . . . .
H11A H 0.165377 0.552226 0.857997 0.107 Uiso 1 1 calc R U . . .
H11B H 0.127215 0.426056 0.799439 0.107 Uiso 1 1 calc R U . . .
C12 C 0.3104(8) 0.5771(7) 0.7881(3) 0.135(2) Uani 1 1 d . . . . .
H12A H 0.394610 0.624725 0.817863 0.162 Uiso 1 1 calc R U . . .
H12B H 0.353020 0.501800 0.758801 0.162 Uiso 1 1 calc R U . . .
C13 C 0.2317(9) 0.7068(8) 0.7494(4) 0.188(4) Uani 1 1 d . . . . .
H13A H 0.301365 0.763045 0.725367 0.283 Uiso 1 1 calc R U . . .
H13B H 0.149656 0.660693 0.718868 0.283 Uiso 1 1 calc R U . . .
H13C H 0.191290 0.783750 0.777994 0.283 Uiso 1 1 calc R U . . .
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
_geom_angle_publ_flag
S1 Ni1 S1 180.0 3_656 . ?
S2 Ni1 S1 92.47(4) 3_656 3_656 ?
S2 Ni1 S1 92.47(4) . . ?
S2 Ni1 S1 87.53(4) . 3_656 ?
S2 Ni1 S1 87.53(4) 3_656 . ?
S2 Ni1 S2 180.0 3_656 . ?
C2 S1 Ni1 102.36(15) . . ?
C3 S2 Ni1 102.71(15) . . ?
C5 N3 C9 119.4(4) . . ?
C5 N3 C10 120.5(4) . . ?
C9 N3 C10 120.0(4) . . ?
N1 C1 C2 178.5(5) . . ?
C1 C2 S1 117.9(3) . . ?
C3 C2 S1 121.3(3) . . ?
C3 C2 C1 120.8(4) . . ?
C2 C3 S2 121.0(3) . . ?
C2 C3 C4 120.0(4) . . ?
C4 C3 S2 119.0(3) . . ?
N2 C4 C3 178.3(6) . . ?
N3 C5 H5 119.5 . . ?
N3 C5 C6 121.1(4) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 119.6 . . ?
C5 C6 C7 120.9(4) . . ?
C7 C6 H6 119.6 . . ?
C6 C7 C7 121.6(5) . 3_557 ?
C8 C7 C6 116.7(4) . . ?
C8 C7 C7 121.7(5) . 3_557 ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.8(4) . . ?
C9 C8 H8 119.6 . . ?
N3 C9 C8 121.1(4) . . ?
N3 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
N3 C10 H10A 109.2 . . ?
N3 C10 H10B 109.2 . . ?
N3 C10 C11 112.1(4) . . ?
H10A C10 H10B 107.9 . . ?
C11 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C10 C11 H11A 109.8 . . ?
C10 C11 H11B 109.8 . . ?
C10 C11 C12 109.4(4) . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
C11 C12 H12A 108.8 . . ?
C11 C12 H12B 108.8 . . ?
H12A C12 H12B 107.6 . . ?
C13 C12 C11 114.0(6) . . ?
C13 C12 H12A 108.8 . . ?
C13 C12 H12B 108.8 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
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 S1 2.1785(12) 3_656 ?
Ni1 S1 2.1785(12) . ?
Ni1 S2 2.1743(12) 3_656 ?
Ni1 S2 2.1743(12) . ?
S1 C2 1.731(4) . ?
S2 C3 1.727(4) . ?
N1 C1 1.142(5) . ?
N2 C4 1.133(5) . ?
N3 C5 1.332(5) . ?
N3 C9 1.335(5) . ?
N3 C10 1.475(5) . ?
C1 C2 1.428(6) . ?
C2 C3 1.354(5) . ?
C3 C4 1.430(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.359(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.384(5) . ?
C7 C7 1.489(8) 3_557 ?
C7 C8 1.365(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.368(5) . ?
C9 H9 0.9300 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.490(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.533(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.431(8) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
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 S1 C2 C1 -177.6(3) . . . . ?
Ni1 S1 C2 C3 2.6(4) . . . . ?
Ni1 S2 C3 C2 -2.8(4) . . . . ?
Ni1 S2 C3 C4 177.1(3) . . . . ?
S1 C2 C3 S2 0.2(5) . . . . ?
S1 C2 C3 C4 -179.8(3) . . . . ?
N3 C5 C6 C7 0.3(7) . . . . ?
N3 C10 C11 C12 -178.0(4) . . . . ?
C1 C2 C3 S2 -179.7(3) . . . . ?
C1 C2 C3 C4 0.4(6) . . . . ?
C5 N3 C9 C8 -1.6(6) . . . . ?
C5 N3 C10 C11 89.5(5) . . . . ?
C5 C6 C7 C7 -179.8(4) . . . 3_557 ?
C5 C6 C7 C8 -0.7(6) . . . . ?
C6 C7 C8 C9 0.0(6) . . . . ?
C7 C7 C8 C9 179.1(4) 3_557 . . . ?
C7 C8 C9 N3 1.2(7) . . . . ?
C9 N3 C5 C6 0.9(6) . . . . ?
C9 N3 C10 C11 -92.4(5) . . . . ?
C10 N3 C5 C6 179.0(4) . . . . ?
C10 N3 C9 C8 -179.7(4) . . . . ?
C10 C11 C12 C13 -178.5(5) . . . . ?
