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_7219405
_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 Se2, 4(C H2 Cl2)'
_chemical_formula_sum            'C46 H56 Bi2 Cl14 N4 Se2'
_chemical_formula_weight         1737.20
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2014-06-03
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;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
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_audit_update_record
;
2014-07-03 deposited with the CCDC.
2015-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.510(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.9721(6)
_cell_length_b                   10.8271(4)
_cell_length_c                   18.3916(6)
_cell_measurement_reflns_used    6261
_cell_measurement_temperature    150.00(10)
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_cell_measurement_theta_min      3.4467
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_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
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olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 16.1293
_diffrn_measured_fraction_theta_full 0.979071
_diffrn_measured_fraction_theta_max 0.979071
_diffrn_measurement_details
;
  1 omega  -18.00   22.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  150.0000 40

  2 omega   35.00   65.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  150.0000 30

  3 omega -102.00  -53.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -77.0000   60.0000 49

  4 omega   31.00  121.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   66.0000   75.0000 90

  5 omega   17.00  102.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   19.0000 -150.0000 85

  6 omega   70.00  123.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -164.0000   72.0000 53

  7 omega   42.00   68.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -150.0000 26

  8 omega   84.00  118.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -150.0000 34

  9 omega   92.00  178.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   30.0000 86

 10 omega  113.00  140.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000  120.0000 27

 11 omega   55.00  105.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  150.0000 50

 12 omega   41.00   90.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  150.0000 49

 13 omega   37.00   91.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000   30.0000 54

 14 omega   45.00  124.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000  -60.0000 79

 15 omega   36.00   86.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -150.0000 50

 16 omega  100.00  165.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -30.0000 65

 17 omega   69.00  103.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 34

 18 omega   42.00   70.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -90.0000 28

 19 omega  -74.00  -25.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  164.0000  -72.0000 49

 20 omega -101.00  -73.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -63.0000  -60.0000 28

 21 omega  -17.00   76.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000   60.0000 93
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0947544000
_diffrn_orient_matrix_UB_12      0.0101314000
_diffrn_orient_matrix_UB_13      -0.0075437000
_diffrn_orient_matrix_UB_21      0.0221450000
_diffrn_orient_matrix_UB_22      -0.0208636000
_diffrn_orient_matrix_UB_23      0.0831653000
_diffrn_orient_matrix_UB_31      0.0035889000
_diffrn_orient_matrix_UB_32      -0.1402473000
_diffrn_orient_matrix_UB_33      -0.0129944000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14171
_diffrn_reflns_theta_full        70.710824
_diffrn_reflns_theta_max         70.71
_diffrn_reflns_theta_min         3.45
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    17.875
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31219
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.8296
_exptl_crystal_description       block
_exptl_crystal_F_000             1659.2918
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         6.335816
_refine_diff_density_min         -2.269692
_refine_diff_density_rms         0.270022
_refine_ls_d_res_high            0.816771
_refine_ls_d_res_low             9.309559
_refine_ls_goodness_of_fit_ref   1.040703
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    42
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040703
_refine_ls_R_factor_all          0.063470
_refine_ls_R_factor_gt           0.053101
_refine_ls_shift/su_max          3.9901
_refine_ls_shift/su_mean         0.0146
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+33.6989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.161189
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                5031
_reflns_number_total             5941
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c4ra17144f2.cif
_cod_data_source_block           14
_cod_original_cell_volume        3153.19(19)
_cod_database_code               7219405
_chemical_oxdiff_formula         'C21 H36 N2 Se Bi Cl3'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97