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_7038309
_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
'C9 H12 Bi Cl4 N4 S2, C18 H25 Bi Cl2 N8 S4'
_chemical_formula_sum            'C27 H37 Bi2 Cl6 N12 S6'
_chemical_formula_weight         1352.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-24
_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                 117.194(5)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   27.2866(11)
_cell_length_b                   27.1101(6)
_cell_length_c                   29.9547(11)
_cell_measurement_reflns_used    4120
_cell_measurement_temperature    293
_cell_measurement_theta_max      70.9610
_cell_measurement_theta_min      4.5940
_cell_volume                     19709.4(15)
_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 0.7661
_diffrn_measured_fraction_theta_max 0.7661
_diffrn_measurement_details
;
  1 omega  -33.00   -8.00   1.0000    2.7600
omega____ theta____ kappa____ phi______ frames
    -        0.0000  106.0000  119.0000 25

  2 omega  -37.00   -9.00   1.0000   11.0300
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   50.0000   30.0000 28

  3 omega   31.00   66.00   1.0000   11.0300
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000    0.0000 35

  4 omega  -15.00   72.00   1.0000   11.0300
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -49.0000  106.0000 87

  5 omega   36.00   94.00   1.0000   11.0300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -150.0000 58

  6 omega   88.00  176.00   1.0000   11.0300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -150.0000 88

  7 omega   36.00   64.00   1.0000   11.0300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -90.0000 28

  8 omega   63.00  103.00   1.0000   11.0300
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -106.0000   20.0000 40

  9 omega   37.00   82.00   1.0000   11.0300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  120.0000 45

 10 omega   43.00   78.00   1.0000   11.0300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000   90.0000 35
;
_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      0.0584410000
_diffrn_orient_matrix_UB_12      -0.0107334000
_diffrn_orient_matrix_UB_13      0.0419170000
_diffrn_orient_matrix_UB_21      0.0239022500
_diffrn_orient_matrix_UB_22      0.0369843500
_diffrn_orient_matrix_UB_23      -0.0239495000
_diffrn_orient_matrix_UB_31      -0.0062548500
_diffrn_orient_matrix_UB_32      0.0418090500
_diffrn_orient_matrix_UB_33      0.0318463000
_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  0.0341
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21580
_diffrn_reflns_theta_full        70.8080
_diffrn_reflns_theta_max         70.81
_diffrn_reflns_theta_min         3.26
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.514
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47597
_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    1.8227
_exptl_crystal_description       needle
_exptl_crystal_F_000             10314.2421
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.2874
_refine_diff_density_min         -1.3549
_refine_diff_density_rms         0.1869
_refine_ls_d_res_high            0.8163
_refine_ls_d_res_low             13.5551
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0217
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    115
_refine_ls_number_parameters     967
_refine_ls_number_reflns         14572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0217
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.0028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              29
_reflns_limit_h_min              -33
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                9336
_reflns_number_total             14572
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04738b2.cif
_cod_data_source_block           5
_cod_original_cell_volume        19709.5(15)
_cod_database_code               7038309
_chemical_oxdiff_formula         'C21 H24 N2 Se Bi Cl3'
_reflns_odcompleteness_completeness 78.51
_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:
 C50(H50a,H50b), C23(H23a,H23b), C5(H5a,H5b), C41(H41a,H41b), C32(H32a,H32b),
 C44(H44a,H44b), C14(H14a,H14b)
2.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C13(H13), C2(H2), C53(H53), C25(H25), C35(H35), C52(H52), C17(H17),
 C49(H49), C7(H7), C8(H8), C22(H22), C16(H16), C43(H43), C21(H21), C3(H3),
 C39(H39), C34(H34), C26(H26), C40(H40), C12(H12), C30(H30), C31(H31)
2.c Idealised Me refined as rotating group:
 C45(H45a,H45b,H45c), C54(H54a,H54b,H54c), C18(H18a,H18b,H18c), C27(H27a,H27b,
 H27c), C36(H36a,H36b,H36c), C29(H29a,H29b,H29c), C47(H47a,H47b,H47c), C38(H38a,
 H38b,H38c), C4(H4a,H4b,H4c), C11(H11a,H11b,H11c), C20(H20a,H20b,H20c), C9(H9a,
 H9b,H9c)
;
_olex2_submission_special_instructions 'No special instructions were received'