Studies on the Properties of Organoselenium(IV) Fluorides and Azides
Thomas M. Klapötke; Burkhard Krumm; Matthias Scherr; Inorganic Chemistry 47 (2008) 4712–4722; doi:10.1021/ic800051s

data_4304946
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
Ludwig-Maximilian University
Butenandtstr. 5--13 (Haus D)
D-81377 Munich
Germany
;
_publ_contact_author_email       tmk@cup.uni-muenchen.de
_publ_contact_author_fax         +49-89-2180-77492
_publ_contact_author_name        'Thomas M. Klap\"otke'
_publ_contact_author_phone       +49-89-2180-77491
_publ_section_title
;
Studies on the Properties of Organoselenium(IV) Fluorides and Azides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4712
_journal_page_last               4722
_journal_paper_doi               10.1021/ic800051s
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C10 H20 N2 S4 Se, C6 H6'
_chemical_formula_sum            'C16 H26 N2 S4 Se'
_chemical_formula_weight         453.63
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Scherr, Matthias'
_audit_block_code                Se(dtc)2_C6H6_cx156_Scherr
_audit_creation_date
;
'Wed Apr 25 12:37:01 2007'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_cell_angle_alpha                90.0
_cell_angle_beta                 99.053(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   8.2071(2)
_cell_length_b                   12.0351(3)
_cell_length_c                   20.7122(7)
_cell_measurement_reflns_used    463
_cell_measurement_temperature    100(3)
_cell_measurement_theta_max      29.9993
_cell_measurement_theta_min      3.8253
_cell_volume                     2020.33(10)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1996)'
_computing_publication_material
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      100(3)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega -101.00  -49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -28.0744  -45.0000  240.0000    0.0000    0.0000 52

  2 omega -101.00  -50.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -28.0744  -45.0000  120.0000    0.0000    0.0000 51

  3 omega   52.00  103.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.2619   45.0000    0.0000    0.0000    0.0000 51

  4 omega    8.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.2619  -75.0000  120.0000    0.0000    0.0000 54

  5 omega    4.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.2619   45.0000  120.0000    0.0000    0.0000 51

  6 omega    6.00   53.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.2619   45.0000    0.0000    0.0000    0.0000 47

  7 omega   56.00   84.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.2619   15.0000 -104.0000    0.0000    0.0000 28

  8 omega    8.00   36.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.2619  -75.0000  240.0000    0.0000    0.0000 28

  9 omega   16.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.2619  -75.0000    0.0000    0.0000    0.0000 46

;
_diffrn_measurement_device_type  'Oxford Xcalibur3 CCD area-detector'
_diffrn_measurement_method       'omega scan'
_diffrn_orient_matrix_UB_11      -0.0091659183
_diffrn_orient_matrix_UB_12      -0.0120175969
_diffrn_orient_matrix_UB_13      -0.0339784795
_diffrn_orient_matrix_UB_21      -0.0874509401
_diffrn_orient_matrix_UB_22      0.0021651551
_diffrn_orient_matrix_UB_23      -0.0018073904
_diffrn_orient_matrix_UB_31      0.0012129634
_diffrn_orient_matrix_UB_32      0.0576171290
_diffrn_orient_matrix_UB_33      -0.0070633328
_diffrn_radiation_collimation    '0.5 mm collimator'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6527
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.84
_diffrn_source_current           40_mA
_diffrn_source_power             2.00_kW
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50_kV
_exptl_absorpt_coefficient_mu    2.272
_exptl_absorpt_correction_T_max  0.81000
_exptl_absorpt_correction_T_min  0.64827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.49137(14)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0555
_reflns_number_gt                1535
_reflns_number_total             1964
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800051s-file001_2.cif
_cod_data_source_block           cx156
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4304946
_kl_diffrn_measurement_detector_distance 50