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_7038311
_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 Bi2 Cl6 N8 S4, C2 N'
_chemical_formula_sum            'C28 H40 Bi2 Cl6 N9 S4'
_chemical_formula_weight         1261.63
_space_group_crystal_system      tetragonal
_space_group_IT_number           138
_space_group_name_Hall           '-P 4ac 2ac'
_space_group_name_H-M_alt        'P 42/n c m'
_symmetry_Int_Tables_number      138
_symmetry_space_group_name_Hall  '-P 4ac 2ac'
_symmetry_space_group_name_H-M   'P 42/n c m :2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.00307(17)
_cell_length_b                   19.00307(17)
_cell_length_c                   12.04528(15)
_cell_measurement_reflns_used    3505
_cell_measurement_temperature    293
_cell_measurement_theta_max      70.8880
_cell_measurement_theta_min      4.3330
_cell_volume                     4349.75(8)
_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 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_details
;
  1 omega   -8.00   35.00   1.0000    1.8200
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   12.0000  -90.0000 43

  2 omega -103.00  -61.00   1.0000    1.8200
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   12.0000  -90.0000 42

  3 omega    1.00   86.00   1.0000    1.8200
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000    0.0000 85

  4 omega   67.00  103.00   1.0000    1.8200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -150.0000 36

  5 omega   45.00   91.00   1.0000    1.8200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -180.0000 46

  6 omega   56.00  115.00   1.0000    1.8200
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 59

  7 omega   36.00   92.00   1.0000    1.8200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  120.0000 56

  8 omega   53.00   79.00   1.0000    1.8200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -30.0000 26

  9 omega  117.00  176.00   1.0000    1.8200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   90.0000 59

 10 omega   47.00   93.00   1.0000    1.8200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   60.0000 46
;
_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      -0.0005058000
_diffrn_orient_matrix_UB_12      -0.0513386000
_diffrn_orient_matrix_UB_13      -0.0989644000
_diffrn_orient_matrix_UB_21      -0.0064902000
_diffrn_orient_matrix_UB_22      0.0625582000
_diffrn_orient_matrix_UB_23      -0.0806790000
_diffrn_orient_matrix_UB_31      0.0808244000
_diffrn_orient_matrix_UB_32      0.0047060000
_diffrn_orient_matrix_UB_33      -0.0070736000
_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  0.0381
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9430
_diffrn_reflns_theta_full        70.8761
_diffrn_reflns_theta_max         70.88
_diffrn_reflns_theta_min         3.29
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.151
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59528
_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    1.9264
_exptl_crystal_description       needle
_exptl_crystal_F_000             2401.5888
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.1306
_refine_diff_density_min         -1.5809
_refine_diff_density_rms         0.1557
_refine_ls_d_res_high            0.8160
_refine_ls_d_res_low             13.4372
_refine_ls_goodness_of_fit_ref   1.0142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    17
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0142
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0526P)^2^+4.9723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              23
_reflns_limit_h_min              0
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                1773
_reflns_number_total             2182
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04738b2.cif
_cod_data_source_block           9
_cod_database_code               7038311
_reflns_odcompleteness_completeness 99.96
_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:
 C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
2.d Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C6(H6a,H6b,H6c)
;
_olex2_submission_special_instructions 'No special instructions were received'