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_4304948
_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         '2(C18 H23 O Se), F6 Si, 2(C H2 Cl2)'
_chemical_formula_sum            'C19 H25 Cl2 F3 O Se Si0.5'
_chemical_formula_weight         490.30
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Scherr, Matthias'
_audit_block_code                (Mes2SeOH)2_SiF6_CH2Cl2_cx025_Scherr
_audit_creation_date
;
'Tue Jan 23 13:54:34 2007'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record
;
'Tue Jan 30 08:37 2007'
;
_cell_angle_alpha                90.0
_cell_angle_beta                 98.4973(14)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   11.34521(16)
_cell_length_b                   14.0128(2)
_cell_length_c                   13.6551(2)
_cell_measurement_reflns_used    1575
_cell_measurement_temperature    100(3)
_cell_measurement_theta_max      28.7073
_cell_measurement_theta_min      3.8476
_cell_volume                     2147.03(5)
_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      200(3)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -92.00  -39.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.9806  -75.0000    0.0000    0.0000    0.0000 53

  2 omega   -2.00   52.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.9806   75.0000  240.0000    0.0000    0.0000 54

  3 omega  -93.00  -42.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.9806  -45.0000    0.0000    0.0000    0.0000 51

  4 omega  -51.00    1.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.9806   75.0000  240.0000    0.0000    0.0000 52

  5 phi   -179.00 -120.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -19.9806    0.0000     -        0.0000    0.0000 59

  6 omega  -46.00    5.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.9806   45.0000    0.0000    0.0000    0.0000 51

  7 omega   -9.00   43.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0119   75.0000  240.0000    0.0000    0.0000 52

  8 omega   43.00   94.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0119   45.0000  240.0000    0.0000    0.0000 51

  9 phi    120.00  180.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   22.0119    0.0000     -        0.0000    0.0000 60

 10 omega    1.00   43.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0119 -129.0000  117.0000    0.0000    0.0000 42

 11 omega   -3.00   47.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0119   45.0000    0.0000    0.0000    0.0000 50

 12 omega   20.00   48.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0119  -45.0000  240.0000    0.0000    0.0000 28

 13 omega  -50.00   -9.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0119  -45.0000    0.0000    0.0000    0.0000 41

 14 omega  -13.00   15.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0119   80.0000  156.0000    0.0000    0.0000 28

;
_diffrn_measurement_device_type  'Oxford Xcalibur3 CCD area-detector'
_diffrn_measurement_method       'omega scan'
_diffrn_orient_matrix_UB_11      0.0380853507
_diffrn_orient_matrix_UB_12      -0.0036649451
_diffrn_orient_matrix_UB_13      0.0459092257
_diffrn_orient_matrix_UB_21      -0.0283707822
_diffrn_orient_matrix_UB_22      -0.0431650107
_diffrn_orient_matrix_UB_23      0.0101251909
_diffrn_orient_matrix_UB_31      0.0416596668
_diffrn_orient_matrix_UB_32      -0.0260693483
_diffrn_orient_matrix_UB_33      -0.0232932595
_diffrn_radiation_collimation    '1.0 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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22731
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.85
_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    2.057
_exptl_absorpt_correction_T_max  0.56350
_exptl_absorpt_correction_T_min  0.31925
_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            colorless
_exptl_crystal_density_diffrn    1.51684(6)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.459
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4186
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+6.7923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                3381
_reflns_number_total             4186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800051s-file001_4.cif
_cod_data_source_block           cx025
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C19 H25 Cl2 F3 O Se Si0.50'
_cod_database_code               4304948
_kl_diffrn_measurement_detector_distance 50