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_7219402
_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         '0.5(C38 H40 N4 Se2)'
_chemical_formula_sum            'C19 H20 N2 Se'
_chemical_formula_weight         355.34
_chemical_name_systematic        4a
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 98.462(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3877(14)
_cell_length_b                   7.4849(14)
_cell_length_c                   13.728(2)
_cell_measurement_reflns_used    1621
_cell_measurement_temperature    150
_cell_measurement_theta_max      71.4592
_cell_measurement_theta_min      3.2544
_cell_volume                     852.5(2)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
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)
;
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 16.1293
_diffrn_measured_fraction_theta_full 0.944344
_diffrn_measured_fraction_theta_max 0.944344
_diffrn_measurement_details
;
  1 omega   27.00   52.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 25

  2 omega  -18.00   10.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 28

  3 omega  -86.00  -41.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000  120.0000 45

  4 omega  -11.00   82.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000  120.0000 93

  5 omega  -12.00   49.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000    0.0000 61

  6 omega    4.00   72.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000 -150.0000 68

  7 omega   60.00  104.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000  -30.0000 44

  8 omega   44.00   79.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  150.0000 35

  9 omega   36.00   93.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   90.0000 57

 10 omega   37.00   88.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -90.0000 51

 11 omega   93.00  178.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -90.0000 85

 12 omega   48.00   93.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000    0.0000 45

 13 omega   47.00   88.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -30.0000 41

 14 omega   85.00  174.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000   30.0000 89

 15 omega  -68.00   19.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 87

 16 omega -102.00  -15.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -57.0000  -30.0000 87
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0236369000
_diffrn_orient_matrix_UB_12      -0.1133015000
_diffrn_orient_matrix_UB_13      -0.0906325000
_diffrn_orient_matrix_UB_21      0.1639466000
_diffrn_orient_matrix_UB_22      -0.0655946000
_diffrn_orient_matrix_UB_23      0.0546920000
_diffrn_orient_matrix_UB_31      -0.0854125000
_diffrn_orient_matrix_UB_32      -0.1582294000
_diffrn_orient_matrix_UB_33      0.0419707000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3047
_diffrn_reflns_theta_full        71.126047
_diffrn_reflns_theta_max         71.13
_diffrn_reflns_theta_min         3.25
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    2.948
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79938
_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    1.3843
_exptl_crystal_description       needle
_exptl_crystal_F_000             363.2098
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.465417
_refine_diff_density_min         -0.873706
_refine_diff_density_rms         0.114703
_refine_ls_d_res_high            0.814726
_refine_ls_d_res_low             7.594127
_refine_ls_goodness_of_fit_ref   1.036298
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    16
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036298
_refine_ls_R_factor_all          0.061601
_refine_ls_R_factor_gt           0.045226
_refine_ls_shift/su_max          0.0018
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+2.1041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.146383
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -10
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              -7
_reflns_number_gt                1287
_reflns_number_total             1561
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c4ra17144f2.cif
_cod_data_source_block           4a
_cod_original_cell_volume        852.5(3)
_cod_database_code               7219402
_chemical_oxdiff_formula         'C25 H25 N2 Se'
_reflns_odcompleteness_completeness 97.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97