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#$Date: 2024-07-05 19:33:47 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293083 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/59/7715941.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_7715941
loop_
_publ_author_name
'Plyuta, Nataliya'
'Barra, Anne-Laure'
'Novitchi, Ghenadie'
'Avarvari, Narcis'
_publ_section_title
;
 Six-coordinated nickel(II) complexes with benzothiadiazole Schiff-base
 ligands: synthesis, crystal structure, magnetic and HFEPR study.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8835
_journal_page_last               8842
_journal_paper_doi               10.1039/d4dt01143k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C26 H16 N6 Ni O2 S2'
_chemical_formula_sum            'C26 H16 N6 Ni O2 S2'
_chemical_formula_weight         567.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2023-12-08 deposited with the CCDC.	2024-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7879(7)
_cell_length_b                   8.8858(3)
_cell_length_c                   13.6750(5)
_cell_measurement_reflns_used    3461
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.2340
_cell_measurement_theta_min      5.4720
_cell_volume                     2282.98(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, V2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.1990
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova(Cu)micro-focus sealed X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5551
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         72.463
_diffrn_reflns_theta_min         4.707
_exptl_absorpt_coefficient_mu    3.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       prism
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0502P)²+1.2046P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2066
_reflns_number_total             2214
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01143k2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7715941--7715942.cif.'
_cod_database_code               7715941
_shelx_shelxl_version_number     2019/3
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, 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
C1 C 0.55582(9) 0.31671(19) 0.40817(13) 0.0265(4) Uani 1 1 d . . . . .
C2 C 0.60103(10) 0.4181(2) 0.45989(14) 0.0299(4) Uani 1 1 d . . . . .
C3 C 0.59410(11) 0.4326(2) 0.56218(14) 0.0338(4) Uani 1 1 d . . . . .
H3 H 0.623322 0.499698 0.598423 0.041 Uiso 1 1 calc R U . . .
C4 C 0.54347(11) 0.3460(2) 0.60693(14) 0.0341(4) Uani 1 1 d . . . . .
H4 H 0.538289 0.353622 0.675857 0.041 Uiso 1 1 calc R U . . .
C5 C 0.49814(10) 0.2449(2) 0.55536(14) 0.0307(4) Uani 1 1 d . . . . .
H5 H 0.464235 0.186906 0.590537 0.037 Uiso 1 1 calc R U . . .
C6 C 0.50268(9) 0.22986(19) 0.45561(14) 0.0266(4) Uani 1 1 d . . . . .
C7 C 0.40688(10) 0.06808(19) 0.42396(14) 0.0297(4) Uani 1 1 d . . . . .
H7 H 0.394573 0.084346 0.490509 0.036 Uiso 1 1 calc R U . . .
C8 C 0.63745(10) -0.0316(2) 0.13015(15) 0.0310(4) Uani 1 1 d . . . . .
C9 C 0.69385(11) -0.0995(2) 0.07731(16) 0.0371(4) Uani 1 1 d . . . . .
H9 H 0.701734 -0.070545 0.011320 0.045 Uiso 1 1 calc R U . . .
C10 C 0.73725(10) -0.2056(2) 0.11851(18) 0.0417(5) Uani 1 1 d . . . . .
H10 H 0.774456 -0.250642 0.081704 0.050 Uiso 1 1 calc R U . . .
C11 C 0.72563(11) -0.2463(2) 0.21624(17) 0.0395(5) Uani 1 1 d . . . . .
H11 H 0.754794 -0.321327 0.245239 0.047 Uiso 1 1 calc R U . . .
C12 C 0.67301(11) -0.1800(2) 0.27093(16) 0.0357(4) Uani 1 1 d . . . . .
H12 H 0.667984 -0.207547 0.337688 0.043 Uiso 1 1 calc R U . . .
C13 C 0.62558(10) -0.07083(19) 0.23058(16) 0.0306(4) Uani 1 1 d . . . . .
N2 N 0.64693(9) 0.49057(19) 0.40133(12) 0.0353(4) Uani 1 1 d . . . . .
N1 N 0.56790(8) 0.31283(17) 0.31167(11) 0.0287(3) Uani 1 1 d . . . . .
N3 N 0.46254(8) 0.13904(16) 0.39139(11) 0.0268(3) Uani 1 1 d . . . . .
S1 S 0.63202(3) 0.43162(6) 0.29181(3) 0.03566(16) Uani 1 1 d . . . . .
Ni1 Ni 0.500000 0.13161(5) 0.250000 0.02665(15) Uani 1 2 d S T P . .
O1 O 0.57585(7) -0.01643(15) 0.28504(10) 0.0337(3) 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
N1 C1 C6 123.76(16) . . ?
N1 C1 C2 113.83(16) . . ?
C6 C1 C2 122.41(16) . . ?
N2 C2 C3 127.37(18) . . ?
N2 C2 C1 112.98(17) . . ?
C3 C2 C1 119.65(17) . . ?
C4 C3 C2 117.14(18) . . ?
C4 C3 H3 121.4 . . ?
C2 C3 H3 121.4 . . ?
C3 C4 C5 123.30(18) . . ?
C3 C4 H4 118.4 . . ?
C5 C4 H4 118.4 . . ?
C6 C5 C4 121.05(17) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 N3 129.83(16) . . ?
C5 C6 C1 116.43(16) . . ?
N3 C6 C1 113.74(15) . . ?
N3 C7 C8 126.48(18) . 4_655 ?
N3 C7 H7 116.8 . . ?
C8 C7 H7 116.8 4_655 . ?
C9 C8 C7 115.94(18) . 4_655 ?
C9 C8 C13 120.05(18) . . ?
C7 C8 C13 123.93(17) 4_655 . ?
C10 C9 C8 121.9(2) . . ?
C10 C9 H9 119.0 . . ?
C8 C9 H9 119.0 . . ?
C9 C10 C11 118.54(19) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
C12 C11 C10 121.40(19) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C11 C12 C13 122.0(2) . . ?
C11 C12 H12 119.0 . . ?
C13 C12 H12 119.0 . . ?
O1 C13 C12 118.94(18) . . ?
O1 C13 C8 125.08(17) . . ?
C12 C13 C8 115.98(18) . . ?
C2 N2 S1 106.67(13) . . ?
C1 N1 S1 105.88(13) . . ?
C1 N1 Ni1 107.19(12) . . ?
S1 N1 Ni1 146.47(9) . . ?
C7 N3 C6 119.61(16) . . ?
C7 N3 Ni1 125.54(13) . . ?
C6 N3 Ni1 114.84(11) . . ?
N2 S1 N1 100.65(8) . . ?
O1 Ni1 O1 97.64(8) . 4_655 ?
O1 Ni1 N3 90.14(6) . 4_655 ?
O1 Ni1 N3 92.28(6) 4_655 4_655 ?
O1 Ni1 N3 92.28(6) . . ?
O1 Ni1 N3 90.14(6) 4_655 . ?
N3 Ni1 N3 176.32(8) 4_655 . ?
O1 Ni1 N1 88.66(6) . . ?
O1 Ni1 N1 168.05(5) 4_655 . ?
N3 Ni1 N1 97.87(6) 4_655 . ?
N3 Ni1 N1 79.42(6) . . ?
O1 Ni1 N1 168.05(5) . 4_655 ?
O1 Ni1 N1 88.66(6) 4_655 4_655 ?
N3 Ni1 N1 79.42(6) 4_655 4_655 ?
N3 Ni1 N1 97.88(6) . 4_655 ?
N1 Ni1 N1 87.04(8) . 4_655 ?
C13 O1 Ni1 128.72(13) . . ?
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 1.339(2) . ?
C1 C6 1.419(2) . ?
C1 C2 1.426(3) . ?
C2 N2 1.342(3) . ?
C2 C3 1.411(3) . ?
C3 C4 1.368(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.425(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.373(3) . ?
C5 H5 0.9500 . ?
C6 N3 1.411(2) . ?
C7 N3 1.300(2) . ?
C7 C8 1.423(3) 4_655 ?
C7 H7 0.9500 . ?
C8 C9 1.418(3) . ?
C8 C13 1.434(3) . ?
C9 C10 1.367(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.402(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.372(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.428(3) . ?
C12 H12 0.9500 . ?
C13 O1 1.289(2) . ?
N2 S1 1.6112(17) . ?
N1 S1 1.6247(15) . ?
N1 Ni1 2.2207(16) . ?
N3 Ni1 2.0587(15) . ?
Ni1 O1 1.9977(13) . ?
Ni1 O1 1.9977(13) 4_655 ?
