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_7061463
_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         'C48 H64 Bi2 Br6 N8 O4 S4'
_chemical_formula_sum            'C48 H64 Bi2 Br6 N8 O4 S4'
_chemical_formula_weight         1842.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 94.9584(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.28018(15)
_cell_length_b                   23.7009(3)
_cell_length_c                   14.4183(3)
_cell_measurement_reflns_used    5425
_cell_measurement_temperature    293
_cell_measurement_theta_max      69.9770
_cell_measurement_theta_min      3.6060
_cell_volume                     3159.42(9)
_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 0.9811
_diffrn_measured_fraction_theta_max 0.9811
_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    -11.00  20.00   1.00    1.00    --    0.00 -57.00 -60.00   31
  2  \w    -63.00 -29.00   1.00    1.00    --    0.00 -57.00  90.00   34
  3  \w    -11.00  16.00   1.00    1.00    --    0.00 -57.00  90.00   27
  4  \w    -17.00  71.00   1.00    1.56    --   54.00 -77.00 -30.00   88
  5  \w     32.00 117.00   1.00    1.56    --   54.00  57.00  90.00   85
  6  \w     42.00 122.00   1.00    1.56    --   54.00  57.00-150.00   80
  7  \w     27.00  52.00   1.00    1.56    --   54.00 -99.00-150.00   25
  8  \w     83.00 108.00   1.00    1.56    --   54.00  57.00 120.00   25
  9  \w     92.00 175.00   1.00    1.56    --  108.00  63.00  60.00   83
 10  \w    110.00 136.00   1.00    1.56    --  108.00  50.00 -30.00   26
 11  \w     37.00 129.00   1.00    1.56    --  108.00 -38.00 -90.00   92
 12  \w     37.00 140.00   1.00    1.56    --  108.00 -77.00 -60.00  103
 13  \w    147.00 173.00   1.00    1.56    --  108.00  50.00 -30.00   26
 14  \w     62.00 143.00   1.00    1.56    --  108.00 178.00-180.00   81
 15  \w     44.00 128.00   1.00    1.56    --  108.00 -50.00 120.00   84
 16  \w     90.00 116.00   1.00    1.56    --  108.00 -25.00  30.00   26
;
_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      -0.0115447000
_diffrn_orient_matrix_UB_12      -0.0601397000
_diffrn_orient_matrix_UB_13      0.0393372000
_diffrn_orient_matrix_UB_21      0.1470428000
_diffrn_orient_matrix_UB_22      -0.0150760000
_diffrn_orient_matrix_UB_23      -0.0355425000
_diffrn_orient_matrix_UB_31      0.0774864000
_diffrn_orient_matrix_UB_32      0.0196152000
_diffrn_orient_matrix_UB_33      0.0931858000
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11869
_diffrn_reflns_theta_full        70.0092
_diffrn_reflns_theta_max         70.01
_diffrn_reflns_theta_min         3.60
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.853
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24211
_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 reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.9369
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1743.2135
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.8415
_refine_diff_density_min         -2.8296
_refine_diff_density_rms         0.2674
_refine_ls_d_res_high            0.8203
_refine_ls_d_res_low             12.2843
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.9798
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    52
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9798
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0764P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1402
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -11
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              -8
_reflns_number_gt                4693
_reflns_number_total             5874
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj01151d2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7061460--7061465.cif.'
_cod_original_cell_volume        3159.41(9)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7061463
_chemical_oxdiff_formula         C28H32BiBr3N2OS
_reflns_odcompleteness_completeness 99.64
_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), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b), C20(H20a,H20b), C21(H21a,H21b)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C15(H15), C16(H16), C17(H17), C5(H5), C4(H4), C18(H18)
2.d Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C23(H23a,H23b,H23c), C12(H12a,H12b,H12c), C24(H24a,H24b,
 H24c)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_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 3.257
_oxdiff_exptl_absorpt_empirical_full_min 0.230