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_7061461
_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         'C19 H13 N S'
_chemical_formula_sum            'C19 H13 N S'
_chemical_formula_weight         287.39
_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                 110.628(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4635(8)
_cell_length_b                   22.1889(13)
_cell_length_c                   9.3494(9)
_cell_measurement_reflns_used    1194
_cell_measurement_temperature    293
_cell_measurement_theta_max      68.3190
_cell_measurement_theta_min      3.9900
_cell_volume                     1449.1(3)
_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 0.4750
_diffrn_measured_fraction_theta_max 0.4750
_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    -25.00   2.00   1.00    1.40    --    0.00  77.00  30.00   27
  2  \w    -22.00  37.00   1.00    1.40    --    0.00  57.00-180.00   59
  3  \w     36.00  71.00   1.00    1.40    --    0.00  77.00  30.00   35
  4  \w     30.00 109.00   1.00    5.59    --   54.00  77.00  60.00   79
  5  \w     49.00 112.00   1.00    5.59    --   54.00  57.00-180.00   63
  6  \w     78.00 116.00   1.00    5.59    --   54.00  57.00 -60.00   38
  7  \w    -10.00  17.00   1.00    5.59    --   54.00 -57.00-150.00   27
  8  \w      7.00  85.00   1.00    5.59    --   54.00 -77.00 -60.00   78
  9  \w    116.00 141.00   1.00    5.59    --  108.00 178.00  90.00   25
 10  \w     49.00  74.00   1.00    5.59    --  108.00-111.00  30.00   25
;
_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      -0.1981654000
_diffrn_orient_matrix_UB_12      0.0088504000
_diffrn_orient_matrix_UB_13      -0.1246848000
_diffrn_orient_matrix_UB_21      -0.0914570000
_diffrn_orient_matrix_UB_22      0.0049112000
_diffrn_orient_matrix_UB_23      0.1238570000
_diffrn_orient_matrix_UB_31      0.0321901000
_diffrn_orient_matrix_UB_32      0.0686942000
_diffrn_orient_matrix_UB_33      0.0070021000
_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  0.0148
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2122
_diffrn_reflns_theta_full        69.6717
_diffrn_reflns_theta_max         69.67
_diffrn_reflns_theta_min         3.98
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.894
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67079
_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    1.3172
_exptl_crystal_description       irregular
_exptl_crystal_F_000             602.8531
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.52
_refine_diff_density_max         0.1205
_refine_diff_density_min         -0.1652
_refine_diff_density_rms         0.0309
_refine_ls_d_res_high            0.8221
_refine_ls_d_res_low             11.0945
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     191
_refine_ls_number_reflns         1301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0969
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+0.2326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              0
_reflns_number_gt                1147
_reflns_number_total             1301
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj01151d2.cif
_cod_data_source_block           IV
_cod_depositor_comments
'Adding full bibliography for 7061460--7061465.cif.'
_cod_database_code               7061461
_chemical_oxdiff_formula         C19H12NS
_reflns_odcompleteness_completeness 44.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C1(H1), C4(H4), C8(H8), C5(H5), C16(H16), C19(H19), C6(H6), C3(H3),
 C7(H7), C2(H2), C17(H17), C18(H18)
;
_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 1.649
_oxdiff_exptl_absorpt_empirical_full_min 0.741