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_7061462
_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 H15 Bi Br3 N2 O Se'
_chemical_formula_sum            'C12 H15 Bi Br3 N2 O Se'
_chemical_formula_weight         730.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_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                77.900(4)
_cell_angle_beta                 78.288(4)
_cell_angle_gamma                84.332(4)
_cell_formula_units_Z            2
_cell_length_a                   7.6380(4)
_cell_length_b                   11.3080(4)
_cell_length_c                   13.1866(7)
_cell_measurement_reflns_used    2168
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.9010
_cell_measurement_theta_min      3.6750
_cell_volume                     1088.56(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_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 16.0309
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.8161
_diffrn_measured_fraction_theta_max 0.8161
_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    -13.00  84.00   1.00   22.00    --   16.95  77.00 -60.00   97
  2  \w    -20.00  59.00   1.00   22.00    --   16.95 -99.00-180.00   79
  3  \w    -75.00 -47.00   1.00   22.00    --  -18.98 124.00  16.00   28
  4  \w    -46.00  46.00   1.00   22.00    --  -18.98  77.00  60.00   92
  5  \w    -88.00 -16.00   1.00   22.00    --  -18.98 -57.00-180.00   72
  6  \w     -6.00  50.00   1.00   22.00    --  -18.98  57.00 -30.00   56
;
_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      -0.0215779000
_diffrn_orient_matrix_UB_12      0.0134207000
_diffrn_orient_matrix_UB_13      0.0514381000
_diffrn_orient_matrix_UB_21      0.0133443000
_diffrn_orient_matrix_UB_22      0.0620757000
_diffrn_orient_matrix_UB_23      -0.0217056000
_diffrn_orient_matrix_UB_31      -0.0915529000
_diffrn_orient_matrix_UB_32      0.0097999000
_diffrn_orient_matrix_UB_33      -0.0043996000
_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  0.0798
_diffrn_reflns_av_unetI/netI     0.1136
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8154
_diffrn_reflns_theta_full        29.1034
_diffrn_reflns_theta_max         29.10
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.271
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
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    2.2298
_exptl_crystal_description       plate
_exptl_crystal_F_000             653.4063
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.4867
_refine_diff_density_min         -3.9716
_refine_diff_density_rms         0.4034
_refine_ls_d_res_high            0.7306
_refine_ls_d_res_low             7.0340
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.9272
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    25
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9272
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          2.3081
_refine_ls_shift/su_mean         0.0125
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0566P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -9
_reflns_limit_k_max              14
_reflns_limit_k_min              -13
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                3210
_reflns_number_total             4770
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj01151d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7061460--7061465.cif.'
_cod_database_code               7061462
_reflns_odcompleteness_completeness 96.78
_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.a Ternary CH refined with riding coordinates:
 C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b)
2.c Aromatic/amide H refined with riding coordinates:
 C1aa(H1aa), C6(H6), C12(H12), C4(H4), C3(H3)
2.d Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C9(H9a,H9b,H9c)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_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 4.643
_oxdiff_exptl_absorpt_empirical_full_min 0.535