Crystal structures of 3/4-pyridyl-based thiosemicarbazones and related Cu and Ni coordination compounds
Lobana, Tarlok Singh; Kaushal, Mani; Bhatia, Robin; Bala, Ritu; Butcher, Ray J.; Jasinksi, Jerry P.; Acta Crystallographica Section C 78 (2022) –; doi:10.1107/S205322962101319X

data_2022489
_publ_section_title
;
 Crystal structures of 3/4-pyridyl-based thiosemicarbazones and related Cu
 and Ni coordination compounds
;
_journal_coeditor_code           YD3022
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205322962101319X
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac
'[Cu Cl (C13 H12 N4 S) (C18 H15 P)2], C2 H3 N'
_chemical_formula_moiety         'C49 H42 Cl Cu N4 P2 S, C2 H3 N'
_chemical_formula_sum            'C51 H45 Cl Cu N5 P2 S'
_chemical_formula_weight         920.91
_chemical_name_common
;
Chlorido(3-formylpyridine
4-phenylthiosemicarbazone-\k<i>S</i>)bis(triphenylphosphane-\k<i>P</i>)copper(I)
acetonitrile monosolvate
;
_chemical_name_systematic
;Chlorido[(<i>E</i>)-<i>N</i>-phenyl-2-(pyridin-3-ylmethylidene)hydrazine-1-carbothioamide-\k<i>S</i>]bis(triphenylphosphane-\k<i>P</i>)copper(I)
acetonitrile monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 96.296(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7299(9)
_cell_length_b                   11.1592(2)
_cell_length_c                   21.6646(7)
_cell_measurement_reflns_used    5023
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.3180
_cell_measurement_theta_min      3.7420
_cell_volume                     4500.8(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0416
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'Rigaku OD Gemini Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.1033
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29820
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.872
_diffrn_reflns_theta_min         3.375
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2019)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       prism
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.280
_refine_diff_density_max         1.419
_refine_diff_density_min         -1.029
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         14960
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.1813
_refine_ls_R_factor_gt           0.1150
_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/[\s^2^(Fo^2^)+31.7681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1976
_refine_ls_wR_factor_ref         0.2315
_reflns_number_gt                8988
_reflns_number_total             14960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yd3022sup1.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2022489
_shelx_estimated_absorpt_t_min   0.747
_shelx_estimated_absorpt_t_max   0.827
_shelx_hkl_checksum              39495
_shelx_res_checksum              18524
_cod_database_fobs_code 2022489