Crystal structure of S-n-octyl 3-(1-phenylethylidene)dithiocarbazate and of its bis-chelated nickel(II) complex
Khan, Sultana Shakila; Howlader, Md. Belayet Hossain; Sheikh, Md. Chanmiya; Miyatake, Ryuta; Zangrando, Ennio; Ansary, Md. Rezaul Haque; Acta Crystallographica Section E Crystallographic Communications 79 (2023) 1137–1141; doi:10.1107/S2056989023009726

data_2022942
_publ_section_title
;
 Crystal structure of S-n-octyl 3-(1-phenylethylidene)dithiocarbazate and
 of its bis-chelated nickel(II) complex
;
_journal_coeditor_code           ZV2030
_journal_issue                   12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1137
_journal_page_last               1141
_journal_paper_doi               10.1107/S2056989023009726
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          '[Ni (C17 H25 N2 S2)2]'
_chemical_formula_moiety         'C34 H50 N4 Ni S4'
_chemical_formula_sum            'C34 H50 N4 Ni S4'
_chemical_formula_weight         701.73
_chemical_name_systematic
;
Bis[<i>S</i>-<i>n</i>-octyl 3-(1-phenylethylidene)dithiocarbazato]nickel(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/2
_cell_angle_alpha                90
_cell_angle_beta                 114.000(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6399(3)
_cell_length_b                   17.6532(5)
_cell_length_c                   16.7596(3)
_cell_measurement_reflns_used    26150
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      1.76
_cell_volume                     3686.6(3)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2018)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2018)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2018)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
WinGX 2018.3 (Farrugia, 2012)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.464
_diffrn_reflns_theta_min         1.761
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       needle
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         8419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+1.4889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                6674
_reflns_number_total             8419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zv2030sup1.cif
_cod_data_source_block           NiL2
_cod_depositor_comments
'Adding full bibliography for 2022941--2022942.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2022942
_cod_database_fobs_code          2022942
_shelx_estimated_absorpt_t_min   0.817
_shelx_estimated_absorpt_t_max   0.977
_shelx_hkl_checksum              16267
_shelx_res_checksum              62389