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_7061464
_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 H12 Cl N S'
_chemical_formula_sum            'C19 H12 Cl N S'
_chemical_formula_weight         321.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-12 deposited with the CCDC.	2022-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.162(11)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   25.360(3)
_cell_length_b                   7.5833(5)
_cell_length_c                   33.138(3)
_cell_measurement_reflns_used    802
_cell_measurement_temperature    293
_cell_measurement_theta_max      18.8360
_cell_measurement_theta_min      2.6110
_cell_volume                     5982.3(11)
_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
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1293
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.8494
_diffrn_measured_fraction_theta_max 0.8494
_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     67.00  95.00   1.00   10.94    --   19.48 178.00-180.00   28
  2  \w    -20.00  84.00   1.00   10.94    --   19.48   0.00-180.00  104
  3  \w     12.00  92.00   1.00   10.94    --   19.48  38.00-150.00   80
;
_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      -0.0149489000
_diffrn_orient_matrix_UB_12      0.0137148000
_diffrn_orient_matrix_UB_13      0.0142964000
_diffrn_orient_matrix_UB_21      0.0233233000
_diffrn_orient_matrix_UB_22      0.0465019000
_diffrn_orient_matrix_UB_23      0.0141878000
_diffrn_orient_matrix_UB_31      -0.0109898000
_diffrn_orient_matrix_UB_32      0.0799776000
_diffrn_orient_matrix_UB_33      -0.0106936000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1147
_diffrn_reflns_av_unetI/netI     0.3028
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            12375
_diffrn_reflns_theta_full        29.0862
_diffrn_reflns_theta_max         29.09
_diffrn_reflns_theta_min         2.49
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79921
_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    1.4292
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2661.1969
_exptl_crystal_size_max          0.077
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.062
_refine_diff_density_max         2.0951
_refine_diff_density_min         -1.2456
_refine_diff_density_rms         0.3136
_refine_ls_d_res_high            0.7310
_refine_ls_d_res_low             8.1881
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.9540
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    48
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9540
_refine_ls_R_factor_all          0.3443
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          2.0818
_refine_ls_shift/su_mean         0.4192
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.1791
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              31
_reflns_limit_h_min              -33
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              42
_reflns_limit_l_min              0
_reflns_number_gt                1409
_reflns_number_total             6817
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj01151d2.cif
_cod_data_source_block           V
_cod_depositor_comments
'Adding full bibliography for 7061460--7061465.cif.'
_cod_original_cell_volume        5982.3(10)
_cod_original_sg_symbol_Hall     '-C 2yc (x,y,-x+z)'
_cod_database_code               7061464
_chemical_oxdiff_formula         C16H20N3S
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C38(H38), C37(H37), C35(H35), C34(H34), C23(H23), C22(H22), C21(H21),
 C20(H20), C24(H24), C25(H25), C26(H26), C27(H27), C15(H15), C16(H16), C18(H18),
  C19(H19), C4(H4), C3(H3), C2(H2), C1(H1), C5(H5), C6(H6), C7(H7), C8(H8)
;
_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 1.386
_oxdiff_exptl_absorpt_empirical_full_min 0.676