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_7219396
_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         'C27 H36 N2 S'
_chemical_formula_sum            'C27 H36 N2 S'
_chemical_formula_weight         420.67
_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             2014-01-20
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_audit_update_record
;
2014-05-01 deposited with the CCDC.
2015-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.338(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2174(14)
_cell_length_b                   6.8155(4)
_cell_length_c                   20.0755(17)
_cell_measurement_reflns_used    2162
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.6964
_cell_measurement_theta_min      4.6381
_cell_volume                     2578.1(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)
;
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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)
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 16.1293
_diffrn_measured_fraction_theta_full 0.972217
_diffrn_measured_fraction_theta_max 0.972217
_diffrn_measurement_details
;
  1 omega -102.00  -75.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000    0.0000 27

  2 omega  -62.00  -34.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000    0.0000 28

  3 omega  -34.00   37.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   38.0000 -120.0000 71

  4 omega   26.00  120.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 94

  5 omega   28.00   73.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  150.0000 45

  6 omega   -9.00   90.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -19.0000  -30.0000 99

  7 omega   41.00   84.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000    0.0000 43

  8 omega   37.00   92.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 55

  9 omega   41.00   68.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -82.0000  105.0000 27

 10 omega   39.00   85.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   60.0000 46

 11 omega   94.00  174.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -120.0000 80

 12 omega   64.00   93.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -120.0000 29

 13 omega   56.00  103.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000   90.0000 47

 14 omega   61.00   88.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000 -150.0000 27

 15 omega   54.00   90.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -30.0000 36

 16 omega   44.00   90.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  150.0000 46

 17 omega   92.00  128.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -82.0000  105.0000 36

 18 omega   78.00  178.00   1.0000    1.6400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000 -150.0000 100
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0185700000
_diffrn_orient_matrix_UB_12      0.0698933000
_diffrn_orient_matrix_UB_13      -0.0673389000
_diffrn_orient_matrix_UB_21      0.0583244000
_diffrn_orient_matrix_UB_22      0.1340303000
_diffrn_orient_matrix_UB_23      0.0397595000
_diffrn_orient_matrix_UB_31      0.0541348000
_diffrn_orient_matrix_UB_32      -0.1681676000
_diffrn_orient_matrix_UB_33      0.0033816000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9769
_diffrn_reflns_theta_full        70.832564
_diffrn_reflns_theta_max         70.83
_diffrn_reflns_theta_min         4.64
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72964
_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    1.0837
_exptl_crystal_description       plate
_exptl_crystal_F_000             915.5451
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.453638
_refine_diff_density_min         -0.360232
_refine_diff_density_rms         0.078292
_refine_ls_d_res_high            0.816166
_refine_ls_d_res_low             9.421175
_refine_ls_goodness_of_fit_ref   1.064470
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    56
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064470
_refine_ls_R_factor_all          0.083202
_refine_ls_R_factor_gt           0.062640
_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^)+(0.0668P)^2^+2.7025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.178639
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -23
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              -14
_reflns_number_gt                3670
_reflns_number_total             4829
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c4ra17144f2.cif
_cod_data_source_block           3
_cod_database_code               7219396
_chemical_oxdiff_formula         'C27 H36 N2 S'
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97