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_7038315
_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         'C26 H40 Bi4 Br12 N8 Se4, 2(C2 H3 N)'
_chemical_formula_sum            'C30 H46 Bi4 Br12 N10 Se4'
_chemical_formula_weight         2657.37
_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             2015-09-24
_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                 107.2678(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.54238(19)
_cell_length_b                   21.6905(3)
_cell_length_c                   12.37785(18)
_cell_measurement_reflns_used    5719
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.5730
_cell_measurement_theta_min      4.2020
_cell_volume                     3215.62(9)
_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      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1293
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9829
_diffrn_measured_fraction_theta_max 0.9829
_diffrn_measurement_details
;
  1 omega  -85.00  -59.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000 -180.0000 26

  2 omega  -23.00   30.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   77.0000   90.0000 53

  3 omega  -54.00  -28.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   77.0000   90.0000 26

  4 omega  -14.00   82.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000   60.0000 96

  5 omega   25.00   93.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000  -30.0000 68

  6 omega   38.00  125.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000 -150.0000 87

  7 omega   95.00  174.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  120.0000 79

  8 omega   37.00   92.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000   90.0000 55

  9 omega   58.00  147.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000    0.0000 89

 10 omega   47.00   84.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 37

 11 omega   45.00   84.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000   30.0000 39

 12 omega   87.00  130.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -30.0000 43

 13 omega   93.00  168.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000 -150.0000 75

 14 omega   38.00   82.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -120.0000 44

 15 omega   63.00   93.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   90.0000 30

 16 omega  110.00  135.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -60.0000 25

 17 omega   39.00   80.00   1.0000    5.3500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -30.0000 41
;
_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      -0.1033016000
_diffrn_orient_matrix_UB_12      0.0423267000
_diffrn_orient_matrix_UB_13      -0.0303592000
_diffrn_orient_matrix_UB_21      -0.0254157000
_diffrn_orient_matrix_UB_22      -0.0195631000
_diffrn_orient_matrix_UB_23      0.1094283000
_diffrn_orient_matrix_UB_31      0.0722527000
_diffrn_orient_matrix_UB_32      0.0535967000
_diffrn_orient_matrix_UB_33      0.0639647000
_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  0.0442
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14054
_diffrn_reflns_theta_full        70.8791
_diffrn_reflns_theta_max         70.88
_diffrn_reflns_theta_min         3.69
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    32.666
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17747
_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    2.7443
_exptl_crystal_description       needle
_exptl_crystal_F_000             2319.9978
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.8519
_refine_diff_density_min         -1.7028
_refine_diff_density_rms         0.3200
_refine_ls_d_res_high            0.8159
_refine_ls_d_res_low             11.9771
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.9831
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    33
_refine_ls_number_parameters     280
_refine_ls_number_reflns         6092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9831
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0840P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                5093
_reflns_number_total             6092
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04738b2.cif
_cod_data_source_block           13
_cod_original_cell_volume        3215.62(8)
_cod_database_code               7038315
_chemical_oxdiff_formula         'C21 H24 N2 Se Bi Br3'
_reflns_odcompleteness_completeness 99.92
_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 Ternary CH refined with riding coordinates:
 C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C9(H9), C10(H10)
2.d Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c),
 C14(H14a,H14b,H14c)
;
_olex2_submission_special_instructions 'No special instructions were received'