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_7062584
_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
'2(C24 H33 Bi Cl3 N9 S6), 0.5(C H4 O), 0.25[CH4O]'
_chemical_formula_sum            'C48.5 H68 Bi2 Cl6 N18 O0.5 S12'
_chemical_formula_weight         1926.58
_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
_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                96.771(2)
_cell_angle_beta                 96.425(2)
_cell_angle_gamma                95.962(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0476(4)
_cell_length_b                   14.9502(4)
_cell_length_c                   18.4873(6)
_cell_measurement_reflns_used    12754
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.9550
_cell_measurement_theta_min      4.2570
_cell_volume                     3804.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.73a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.73a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.73a (Rigaku OD, 2020)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.902
_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    -38.00  40.00   1.00   12.50    --    0.23  57.00   0.00   78
  2  \w     54.00  84.00   1.00   12.50    --    0.23  57.00   0.00   30
  3  \w     80.00 117.00   1.00   40.00    --   30.40 125.00 120.00   37
  4  \w     78.00 109.00   1.00   40.00    --   30.40 125.00-150.00   31
  5  \w    -24.00  17.00   1.00   12.50    --    0.23 -99.00  60.00   41
  6  \w    -47.00 -22.00   1.00   40.00    --   30.40 125.00   0.00   25
  7  \w    -67.00 115.00   1.00   40.00    --   30.40  19.00 -60.00  182
  8  \w    -25.00  30.00   1.00   40.00    --  -29.93 -99.00  60.00   55
  9  \w    -25.00  30.00   1.00   40.00    --  -29.93 -99.00 -60.00   55
 10  \w    -25.00  28.00   1.00   40.00    --  -29.93 -99.00-180.00   53
 11  \w    -67.00 -35.00   1.00   12.50    --    0.23-178.00  90.00   32
 12  \w   -104.00 -77.00   1.00   12.50    --    0.23-178.00  90.00   27
 13  \w   -118.00 -93.00   1.00   40.00    --  -29.93-125.00  90.00   25
 14  \w   -118.00 -93.00   1.00   40.00    --  -29.93-125.00 150.00   25
 15  \w   -118.00 -93.00   1.00   40.00    --  -29.93-125.00  30.00   25
 16  \w   -116.00 -86.00   1.00   40.00    --  -29.93-125.00   0.00   30
 17  \w   -117.00 -74.00   1.00   40.00    --  -29.93-125.00 -90.00   43
 18  \w   -110.00 -85.00   1.00   40.00    --  -29.93-125.00-180.00   25
;
_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  0.0185
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31133
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.166
_diffrn_reflns_theta_min         3.096
_exptl_absorpt_coefficient_mu    5.206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.73a (Rigaku Oxford Diffraction, 2020)
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    1.682
_exptl_crystal_description       plate
_exptl_crystal_F_000             1898
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         15243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+4.3107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0453
_refine_ls_wR_factor_ref         0.0479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13218
_reflns_number_total             15243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01411h2.cif
_cod_data_source_block           ibo_82_lt2
_cod_original_cell_volume        3804.25(19)
_cod_original_formula_sum        'C48.50 H68 Bi2 Cl6 N18 O0.50 S12'
_cod_database_code               7062584
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.781
_shelx_estimated_absorpt_t_min   0.230
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: O3R(0.5) H3R(0.5) C4R(0.5) H4RA(0.5) H4RB(0.5) H4RC(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), N8(H8), N10(H10), C22(H22), C23(H23), C24(H24),
 N28(H28), N30(H30), C42(H42), C43(H43), C44(H44), N48(H48), N50(H50), C62(H62),
  C63(H63), C64(H64), N68(H68), N70(H70), C82(H82), C83(H83), C84(H84),
 N88(H88), N90(H90), C102(H102), C103(H103), C104(H104), N108(H108), N110(H110)
3.b Idealised Me refined as rotating group:
 C6'(H6'A,H6'B,H6'C), C11(H11A,H11B,H11C), C26'(H26A,H26B,H26C), C31(H31A,H31B,
 H31C), C46'(H46A,H46B,H46C), C51(H51A,H51B,H51C), C1(H1A,H1B,H1C), C66'(H66A,
 H66B,H66C), C71(H71A,H71B,H71C), C86'(H86A,H86B,H86C), C92(H92A,H92B,H92C),
 C111(H11D,H11E,H11F), C4R(H4RA,H4RB,H4RC)
3.c Idealised tetrahedral OH refined as rotating group:
 O3R(H3R)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 10 electrons were 
found in a volume of 289\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.25[CH4O] per Unit Cell 
which account for 9 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95723
_shelx_hkl_checksum              27006
_shelx_fab_checksum              47313
_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
;