Dinuclear complexes, a one dimensional chain and a two dimensional layer of bismuth(iii) chalcogenones for C–S cross coupling reactions
Mannarsamy, Maruthupandi; Nandeshwar, Muneshwar; Veerapathiran, Sabari; Mandal, Suman; Harijan, Dinesh; Subramaniyam, Kalaivanan; Muduli, Gopendra; Prabusankar, Ganesan; New Journal of Chemistry 46 (2022) 10256–10263; doi:10.1039/D2NJ01151D

data_7061460
_publ_section_title
;
 Dinuclear complexes, a one dimensional chain and a two dimensional layer
 of bismuth(iii) chalcogenones for C--S cross coupling reactions
;
_journal_issue                   21
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10256
_journal_page_last               10263
_journal_paper_doi               10.1039/D2NJ01151D
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C12 H16 Bi Cl3 N2 O S'
_chemical_formula_sum            'C12 H16 Bi Cl3 N2 O S'
_chemical_formula_weight         551.68
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-17 deposited with the CCDC.	2022-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.4866(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6327(2)
_cell_length_b                   10.36708(17)
_cell_length_c                   17.0092(3)
_cell_measurement_reflns_used    3679
_cell_measurement_temperature    293
_cell_measurement_theta_max      69.9710
_cell_measurement_theta_min      4.3650
_cell_volume                     1806.85(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1293
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9854
_diffrn_measured_fraction_theta_max 0.9854
_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     30.00  56.00   1.00    1.00    --    0.00  57.00-180.00   26
  2  \w     25.00  59.00   1.00    1.00    --    0.00  57.00 -90.00   34
  3  \w     -5.00  20.00   1.00    1.00    --    0.00 -87.00 -58.00   25
  4  \w     -6.00  19.00   1.00    1.00    --    0.00  57.00 -90.00   25
  5  \w     34.00  75.00   1.00    1.00    --   54.00 -57.00  90.00   41
  6  \w     39.00 110.00   1.00    1.00    --   54.00  57.00 120.00   71
  7  \w     24.00 106.00   1.00    1.00    --   54.00-125.00  90.00   82
  8  \w    -14.00  12.00   1.00    1.00    --   54.00 -57.00  90.00   26
  9  \w     41.00 118.00   1.00    1.00    --   54.00  77.00 -30.00   77
 10  \w     88.00 125.00   1.00    1.00    --  108.00  50.00 -60.00   37
 11  \w     37.00 129.00   1.00    1.00    --  108.00 -50.00-150.00   92
 12  \w     93.00 174.00   1.00    1.00    --  108.00  63.00  30.00   81
 13  \w    100.00 149.00   1.00    1.00    --  108.00 111.00 -60.00   49
 14  \w    133.00 175.00   1.00    1.00    --  108.00  63.00   0.00   42
 15  \w     85.00 115.00   1.00    1.00    --  108.00  63.00   0.00   30
 16  \w     81.00 112.00   1.00    1.00    --  108.00-111.00 -90.00   31
 17  \w    104.00 138.00   1.00    1.00    --  108.00 111.00-150.00   34
 18  \w     42.00 106.00   1.00    1.00    --  108.00-111.00  30.00   64
 19  \w     42.00  97.00   1.00    1.00    --  108.00 -91.00-150.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0991907000
_diffrn_orient_matrix_UB_12      -0.0104110000
_diffrn_orient_matrix_UB_13      0.0843356000
_diffrn_orient_matrix_UB_21      -0.0220725000
_diffrn_orient_matrix_UB_22      -0.1469097000
_diffrn_orient_matrix_UB_23      -0.0002377000
_diffrn_orient_matrix_UB_31      0.1107649000
_diffrn_orient_matrix_UB_32      -0.0200102000
_diffrn_orient_matrix_UB_33      -0.0414927000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6672
_diffrn_reflns_theta_full        69.9389
_diffrn_reflns_theta_max         69.94
_diffrn_reflns_theta_min         4.31
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.290
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.0279
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1033.3057
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.1878
_refine_diff_density_min         -2.0355
_refine_diff_density_rms         0.2295
_refine_ls_d_res_high            0.8207
_refine_ls_d_res_low             10.2466
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0235
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0235
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0519P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                3031
_reflns_number_total             3365
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj01151d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7061460--7061465.cif.'
_cod_original_cell_volume        1806.84(6)
_cod_database_code               7061460
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         C12H16N2SBiBr3
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3a)
;
_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 3.135
_oxdiff_exptl_absorpt_empirical_full_min 0.522