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_7061465
_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 Cl6 N8 O4 Se4'
_chemical_formula_sum            'C48 H64 Bi2 Cl6 N8 O4 Se4'
_chemical_formula_weight         1763.61
_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             2022-04-12
_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                90.00(3)
_cell_angle_beta                 95.19(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            2
_cell_length_a                   9.148(2)
_cell_length_b                   23.974(5)
_cell_length_c                   14.150(3)
_cell_measurement_reflns_used    15024
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      28.2980
_cell_measurement_theta_min      3.6930
_cell_volume                     3090.6(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      298.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0309
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.9982
_diffrn_measurement_details
;
  1 omega   -3.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1097   57.0000   90.0000 89

  2 omega   53.00   79.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1097  178.0000   60.0000 26

  3 omega   -9.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1097   77.0000  150.0000 93

  4 omega   -9.00   42.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1097   77.0000  -60.0000 51

  5 omega    9.00   36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9065   77.0000 -150.0000 27

  6 omega  -52.00  -26.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1097  -57.0000 -150.0000 26

  7 omega  -20.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1097  -99.0000    0.0000 73

  8 omega  -16.00   40.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1097  -77.0000 -150.0000 56

  9 omega  -61.00    7.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9065  -19.0000   30.0000 68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0093192000
_diffrn_orient_matrix_UB_12      -0.0289446000
_diffrn_orient_matrix_UB_13      0.0091444000
_diffrn_orient_matrix_UB_21      0.0006423000
_diffrn_orient_matrix_UB_22      0.0051355000
_diffrn_orient_matrix_UB_23      0.0493855000
_diffrn_orient_matrix_UB_31      -0.0772892000
_diffrn_orient_matrix_UB_32      -0.0034434000
_diffrn_orient_matrix_UB_33      -0.0030864000
_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  0.0626
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30790
_diffrn_reflns_theta_full        24.9974
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.347
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.8951
_exptl_crystal_description       block
_exptl_crystal_F_000             1674.4766
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.7354
_refine_diff_density_min         -1.5197
_refine_diff_density_rms         0.3930
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             7.0459
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    52
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5434
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.0156
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1359P)^2^+5.5381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1756
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -10
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              -8
_reflns_number_gt                5000
_reflns_number_total             5434
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj01151d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7061460--7061465.cif.'
_cod_original_cell_volume        3090.5(12)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7061465
_chemical_oxdiff_formula         'C30 N5 H30 O4 Se4 Bi2 Cl10'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 C8-C9
 1.3 with sigma of 0.02
 C9-O1
 1.45 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C10(H10), C22(H22)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b), C20(H20a,H20b), C21(H21a,H21b)
3.c Me refined with riding coordinates:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C23(H23a,H23b,H23c), C24(H24a,H24b,
 H24c)
3.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C15(H15), C16(H16), C17(H17), C18(H18)
3.e Tetrahedral OH refined with riding coordinates:
 O1(H1), O2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'