Heavier chalcogenone complexes of bismuth(III)trihalides: Potential catalysts for acylative cleavage of cyclic ethers
Katam, Srinivas; Suresh, Paladugu; Chatla, Naga Babu; Arruri, Sathyanarayana; Ganesan, Prabusankar; RSC Adv.  (2015) –; doi:10.1039/C4RA17144F

data_7219403
_publ_section_title
;
 Heavier chalcogenone complexes of bismuth(III)trihalides: Potential
 catalysts for acylative cleavage of cyclic ethers
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA17144F
_journal_year                    2015
_chemical_formula_moiety         'C42 H48 Bi2 Cl6 N4 S2, 4(C H Cl3)'
_chemical_formula_sum            'C46 H52 Bi2 Cl18 N4 S2'
_chemical_formula_weight         1781.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2014-07-02
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_audit_update_record
;
2014-07-03 deposited with the CCDC.
2015-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.117(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2653(8)
_cell_length_b                   17.1990(9)
_cell_length_c                   15.5570(7)
_cell_measurement_reflns_used    4772
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.7293
_cell_measurement_theta_min      3.6470
_cell_volume                     3240.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
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olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 16.1293
_diffrn_measured_fraction_theta_full 0.977251
_diffrn_measured_fraction_theta_max 0.977251
_diffrn_measurement_details
;
  1 omega   38.00   65.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 27

  2 omega  -18.00   29.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 47

  3 omega  -94.00  -33.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -63.0000 -180.0000 61

  4 omega   36.00  124.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000 -120.0000 88

  5 omega   44.00  109.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000   90.0000 65

  6 omega   17.00  105.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -       54.0000   19.0000    0.0000 88

  7 omega   59.00   87.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -180.0000 28

  8 omega   38.00   92.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000    0.0000 54

  9 omega   66.00   93.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000    0.0000 27

 10 omega   43.00  178.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000 -150.0000 135

 11 omega   37.00   91.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 54

 12 omega   37.00   93.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -120.0000 56

 13 omega   40.00   67.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 27

 14 omega   42.00   93.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -180.0000 51

 15 omega   57.00   94.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -30.0000 37

 16 omega   86.00  113.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 27

 17 omega   70.00  134.00   1.0000    5.5700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  150.0000 64
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0970398000
_diffrn_orient_matrix_UB_12      0.0060243000
_diffrn_orient_matrix_UB_13      0.0514543000
_diffrn_orient_matrix_UB_21      0.0798708000
_diffrn_orient_matrix_UB_22      -0.0142413000
_diffrn_orient_matrix_UB_23      0.0855213000
_diffrn_orient_matrix_UB_31      0.0195878000
_diffrn_orient_matrix_UB_32      0.0882251000
_diffrn_orient_matrix_UB_33      0.0102132000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12843
_diffrn_reflns_theta_full        70.883503
_diffrn_reflns_theta_max         70.88
_diffrn_reflns_theta_min         3.65
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.252
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74415
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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    1.8255
_exptl_crystal_description       block
_exptl_crystal_F_000             1722.8694
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         7.072494
_refine_diff_density_min         -3.305245
_refine_diff_density_rms         0.427419
_refine_ls_d_res_high            0.815914
_refine_ls_d_res_low             11.456554
_refine_ls_goodness_of_fit_ref   1.045602
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     330
_refine_ls_number_reflns         6100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045602
_refine_ls_R_factor_all          0.136857
_refine_ls_R_factor_gt           0.119004
_refine_ls_shift/su_max          0.0076
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1746P)^2^+97.2544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.321768
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -14
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              -10
_reflns_number_gt                5119
_reflns_number_total             6100
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c4ra17144f2.cif
_cod_data_source_block           12
_cod_database_code               7219403
_chemical_oxdiff_formula         'C21 H36 N2 S Bi Cl3'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97