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_7038305
_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
'3(C27 H36 Bi N12 S6), Bi6 C12 F36 O44 S12, 3(C F3 O3 S)'
_chemical_formula_sum            'C96 H108 Bi9 F45 N36 O53 S33'
_chemical_formula_weight         6408.07
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_Int_Tables_number      167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   30.7421(7)
_cell_length_b                   30.7421(7)
_cell_length_c                   70.888(2)
_cell_measurement_reflns_used    10175
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.0800
_cell_measurement_theta_min      4.1510
_cell_volume                     58019(2)
_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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1293
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9903
_diffrn_measured_fraction_theta_max 0.9903
_diffrn_measurement_details
;
  1 omega  -39.00    6.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  116.0000   89.0000 45

  2 omega  -28.00    0.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000  -30.0000 28

  3 omega   65.00  130.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       55.1553  167.0000  144.0000 65

  4 omega   51.00  120.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       55.1553   57.0000 -150.0000 69

  5 omega   39.00   75.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      110.3105  -38.0000   90.0000 36

  6 omega   52.00   88.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      110.3105  -25.0000 -180.0000 36

  7 omega   62.00   99.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      110.3105  -50.0000 -180.0000 37

  8 omega  116.00  167.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      110.3105  111.0000    0.0000 51

  9 omega   40.00   89.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      110.3105  -38.0000 -120.0000 49

 10 omega  108.00  178.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      110.3105  -12.0000  -30.0000 70

 11 omega   37.00   63.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      110.3105  -12.0000  -30.0000 26
;
_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      -0.0428667000
_diffrn_orient_matrix_UB_12      -0.0402036000
_diffrn_orient_matrix_UB_13      0.0121212000
_diffrn_orient_matrix_UB_21      -0.0098272000
_diffrn_orient_matrix_UB_22      0.0405409000
_diffrn_orient_matrix_UB_23      0.0083686000
_diffrn_orient_matrix_UB_31      -0.0376352000
_diffrn_orient_matrix_UB_32      -0.0093045000
_diffrn_orient_matrix_UB_33      -0.0159685000
_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  0.0549
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_number            42164
_diffrn_reflns_theta_full        71.2234
_diffrn_reflns_theta_max         71.22
_diffrn_reflns_theta_min         4.15
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.189
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53444
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.2006
_exptl_crystal_F_000             36339.3471
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.6938
_refine_diff_density_min         -1.7320
_refine_diff_density_rms         0.2300
_refine_ls_d_res_high            0.8143
_refine_ls_d_res_low             10.6436
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0456
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    57
_refine_ls_number_parameters     823
_refine_ls_number_reflns         12404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0456
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+111.0811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              32
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              85
_reflns_limit_l_min              -85
_reflns_number_gt                10295
_reflns_number_total             12404
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04738b2.cif
_cod_data_source_block           1
_cod_database_code               7038305
_reflns_odcompleteness_completeness 99.87
_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:
 C4(H4a,H4b), C14(H14a,H14b), C23(H23a,H23b)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C12(H12), C13(H13), C16(H16), C17(H17),
 C21(H21), C22(H22), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C18(H18a,H18b,H18c),
 C20(H20a,H20b,H20c), C27(H27a,H27b,H27c)
;
_olex2_submission_special_instructions 'No special instructions were received'