Bismuth(III)dichalcogenones as Highly Active Catalysts in Multiple C-C Bond Formation Reactions
Katam, Srinivas; Arruri, Sathyanarayana; Chatla, Naga Babu; Ganesan, Prabusankar; Dalton Trans.  (2016) –; doi:10.1039/C5DT04738B

data_7038310
_publ_section_title
;
 Bismuth(III)dichalcogenones as Highly Active Catalysts in Multiple C-C
 Bond Formation Reactions
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C5DT04738B
_journal_year                    2016
_chemical_formula_moiety         'C18 H24 Bi2 Br6 N8 S4'
_chemical_formula_sum            'C18 H24 Bi2 Br6 N8 S4'
_chemical_formula_weight         1378.09
_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
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-12-03 deposited with the CCDC.
2016-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.29(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.393(2)
_cell_length_b                   17.461(2)
_cell_length_c                   11.491(2)
_cell_measurement_reflns_used    781
_cell_measurement_temperature    293
_cell_measurement_theta_max      69.1650
_cell_measurement_theta_min      5.1860
_cell_volume                     1731.1(6)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1293
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.00000
_diffrn_measured_fraction_theta_max 1.00000
_diffrn_measurement_details
;
  1 omega   32.00   58.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -120.0000 26

  2 omega  -45.00    9.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000 -150.0000 54

  3 omega -117.00  -92.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000  120.0000 25

  4 omega -111.00  -11.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -90.0000 100

  5 omega   55.00  104.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -      110.3105 -111.0000    0.0000 49

  6 omega   41.00   71.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -      110.3105  -38.0000   30.0000 30

  7 omega   40.00   79.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -      110.3105  -38.0000 -120.0000 39

  8 omega   39.00   92.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -      110.3105  -25.0000  -30.0000 53

  9 omega   41.00  104.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -      110.3105  -50.0000 -180.0000 63

 10 omega   45.00   87.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -      110.3105  -38.0000   60.0000 42
;
_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      0.1702170000
_diffrn_orient_matrix_UB_12      -0.0112855000
_diffrn_orient_matrix_UB_13      0.0914364000
_diffrn_orient_matrix_UB_21      -0.0428460000
_diffrn_orient_matrix_UB_22      0.0187260000
_diffrn_orient_matrix_UB_23      0.1130578000
_diffrn_orient_matrix_UB_31      -0.0318171000
_diffrn_orient_matrix_UB_32      -0.0856214000
_diffrn_orient_matrix_UB_33      0.0125394000
_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  0.0284
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3383
_diffrn_reflns_theta_full        70.9917
_diffrn_reflns_theta_max         70.99
_diffrn_reflns_theta_min         4.90
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    30.304
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65388
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.6438
_exptl_crystal_description       needle
_exptl_crystal_F_000             1238.0679
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.1527
_refine_diff_density_min         -2.4895
_refine_diff_density_rms         0.2723
_refine_ls_d_res_high            0.8154
_refine_ls_d_res_low             9.0324
_refine_ls_goodness_of_fit_ref   0.9962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    19
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9962
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0643P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -11
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                2016
_reflns_number_total             2520
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04738b2.cif
_cod_data_source_block           6
_cod_original_cell_volume        1731.0(7)
_cod_database_code               7038310
_chemical_oxdiff_formula         'C21 H24 N2 S Bi Br3'
_reflns_odcompleteness_completeness 99.33
_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
2.a Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8)
2.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C9(H9a,H9b,H9c)
;
_olex2_submission_special_instructions 'No special instructions were received'