Heteroleptic six-coordinate bismuth(iii) complexes with 2-acetylthiophene thiosemicarbazones: synthesis, characterization, and biological properties
Ozturk, Ibrahim I.; Turk, Kadriye; Grześkiewicz, Anita M.; Kubicki, Maciej; Banti, Christina N.; Hadjikakou, Sotiris K.; New Journal of Chemistry 47 (2023) 12779–12789; doi:10.1039/D3NJ01411H

data_7062581
_publ_section_title
;
 Heteroleptic six-coordinate bismuth(iii) complexes with 2-acetylthiophene
 thiosemicarbazones: synthesis, characterization, and biological
 properties
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12779
_journal_page_last               12789
_journal_paper_doi               10.1039/D3NJ01411H
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C21 H27 Bi Cl3 N9 S6'
_chemical_formula_sum            'C21 H27 Bi Cl3 N9 S6'
_chemical_formula_weight         913.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-22 deposited with the CCDC.	2023-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                70.310(5)
_cell_angle_beta                 84.830(4)
_cell_angle_gamma                88.196(4)
_cell_formula_units_Z            2
_cell_length_a                   7.8136(3)
_cell_length_b                   12.7560(7)
_cell_length_c                   17.6388(11)
_cell_measurement_reflns_used    5450
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.8250
_cell_measurement_theta_min      4.0440
_cell_volume                     1648.53(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -35.00   3.00   1.00    7.50    --  -29.93 -57.00  60.00   38
  2  \w    -20.00   6.00   1.00    7.50    --  -29.93 -99.00 120.00   26
  3  \w    -57.00  81.00   1.00    7.50    --   30.40 -57.00 150.00  138
  4  \w     -4.00 107.00   1.00    7.50    --   30.40  57.00   0.00  111
  5  \w     58.00  83.00   1.00    2.06    --    0.23 -37.00 -90.00   25
  6  \w     12.00  37.00   1.00    2.06    --    0.23 -37.00 -90.00   25
  7  \w    -15.00 131.00   1.00    7.50    --   30.40  77.00  60.00  146
  8  \w     34.00  59.00   1.00    2.06    --    0.23-178.00 -30.00   25
  9  \w     71.00 103.00   1.00    2.06    --    0.23-178.00 -30.00   32
 10  \w    -44.00   1.00   1.00    7.50    --   30.40 125.00-150.00   45
 11  \w    -88.00 -63.00   1.00    2.06    --    0.23 -37.00 -90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0256221000
_diffrn_orient_matrix_UB_12      -0.0301519000
_diffrn_orient_matrix_UB_13      0.0390108000
_diffrn_orient_matrix_UB_21      -0.0086052000
_diffrn_orient_matrix_UB_22      0.0489159000
_diffrn_orient_matrix_UB_23      0.0106418000
_diffrn_orient_matrix_UB_31      -0.0870484000
_diffrn_orient_matrix_UB_32      -0.0136341000
_diffrn_orient_matrix_UB_33      0.0142176000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10860
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.912
_diffrn_reflns_theta_min         3.225
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.001
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.007
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+0.1637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6061
_reflns_number_total             6403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01411h2.cif
_cod_data_source_block           ibo_83_lt_spr
_cod_database_code               7062581
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.380
_shelx_estimated_absorpt_t_min   0.198
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N28(H28), N8(H8), N48(H48), C44(H44), C4(H4), C22(H22), C24(H24), C2(H2),
 C3(H3), C42(H42), C43(H43), C23(H23)
2.b X=CH2 refined with riding coordinates:
 N30(H30A,H30B), N10(H10A,H10B), N50(H50A,H50B)
2.c Idealised Me refined as rotating group:
 C26'(H26A,H26B,H26C), C46'(H46A,H46B,H46C), C6'(H6'A,H6'B,H6'C)
;
_shelx_res_checksum              87830
_shelx_hkl_checksum              37594
_olex2_date_sample_data_collection 2021-04-28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.509
_oxdiff_exptl_absorpt_empirical_full_min 0.778