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_7062583
_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         'C28 H36 Bi2 Br6 N12 S8'
_chemical_formula_sum            'C28 H36 Bi2 Br6 N12 S8'
_chemical_formula_weight         1694.59
_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     iterative
_audit_creation_date             2023-05-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-31 deposited with the CCDC.	2023-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                96.698(6)
_cell_angle_beta                 114.671(7)
_cell_angle_gamma                100.972(6)
_cell_formula_units_Z            1
_cell_length_a                   10.3573(7)
_cell_length_b                   11.2631(8)
_cell_length_c                   11.6777(8)
_cell_measurement_reflns_used    4017
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.2350
_cell_measurement_theta_min      3.5500
_cell_volume                     1185.57(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.821
_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    -52.00  38.00   1.00    9.50    --   16.56 -57.00 -90.00   90
  2  \w    -44.00  41.00   1.00    9.50    --   16.56 -37.00   0.00   85
  3  \w    -49.00  21.00   1.00    9.50    --   16.56 -57.00 150.00   70
  4  \w     -5.00  26.00   1.00    9.50    --   16.56  57.00  60.00   31
  5  \w    -39.00  12.00   1.00    9.50    --  -17.42 -77.00-180.00   51
  6  \w    -39.00   8.00   1.00    9.50    --  -17.42 -77.00  60.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8697
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.585
_diffrn_reflns_theta_min         3.294
_exptl_absorpt_coefficient_mu    12.858
_exptl_absorpt_correction_T_max  0.258
_exptl_absorpt_correction_T_min  0.082
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    2.373
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.675
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.303
_refine_diff_density_max         1.289
_refine_diff_density_min         -1.961
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4968
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0245
_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/[\s^2^(Fo^2^)+(0.0217P)^2^+0.6544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4731
_reflns_number_total             4968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01411h2.cif
_cod_data_source_block           ibo91_lt_sm_f
_cod_original_cell_volume        1185.57(16)
_cod_database_code               7062583
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.112
_shelx_estimated_absorpt_t_min   0.042
_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. Restrained distances
 C25-C24
 1.36 with sigma of 0.001
 C25-S21
 1.72 with sigma of 0.001
 S21-C25 \\sim S21A-C25A
 with sigma of 0.02
 S21-C22 \\sim S21A-C22A
 with sigma of 0.02
 C24-C23 \\sim C24A-C23A
 with sigma of 0.02
 C24-C25 \\sim C24A-C25A
 with sigma of 0.02
 C26-C25 \\sim C26-C25A
 with sigma of 0.02
 C23-C22 \\sim C23A-C22A
 with sigma of 0.02
 S21-C24 \\sim S21A-C24A
 with sigma of 0.04
 S21-C26 \\sim S21A-C26
 with sigma of 0.04
 S21-C23 \\sim S21A-C23A
 with sigma of 0.04
 C24-C26 \\sim C24A-C26
 with sigma of 0.04
 C24-C22 \\sim C24A-C22A
 with sigma of 0.04
 C23-C25 \\sim C23A-C25A
 with sigma of 0.04
 C25-C22 \\sim C25A-C22A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(S21) = Uanis(S21A)
Uanis(C25) = Uanis(C25A)
Uanis(C24A) = Uanis(C24)
Uanis(C22A) = Uanis(C23)
Uanis(C23A) = Uanis(C22)
4. Others
 Fixed Sof: S21(0.92) C24(0.92) H24(0.92) C23(0.92) H23(0.92) C25(0.92)
 C22(0.92) H22(0.92) C25A(0.08) S21A(0.08) C22A(0.08) H22A(0.08) C23A(0.08)
 H23A(0.08) C24A(0.08) H24A(0.08)
5.a Aromatic/amide H refined with riding coordinates:
 N8(H8), N28(H28), C24(H24), C4(H4), C3(H3), C23(H23), C22(H22), C2(H2),
 C22A(H22A), C23A(H23A), C24A(H24A)
5.b X=CH2 refined with riding coordinates:
 N10(H10A,H10B), N30(H30A,H30B)
5.c Idealised Me refined as rotating group:
 C6'(H6'A,H6'B,H6'C), C26'(H26A,H26B,H26C)
;
_shelx_res_checksum              4228
_shelx_hkl_checksum              62526
_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
;