Homoleptic Selenium Cyanides: Attempted Preparation of Se(CN)4 and Redetermination of the Crystal Structure of Se(CN)2
Thomas M. Klapötke; Burkhard Krumm; Matthias Scherr; Inorganic Chemistry 47 (2008) 7025–7028; doi:10.1021/ic801011g

data_4306092
_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
;
Homoleptic Selenium Cyanides: Attempted Preparation of Se(CN)4 and
Redetermination of the Crystal Structure of Se(CN)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7025
_journal_page_last               7028
_journal_paper_doi               10.1021/ic801011g
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C2 N2 Se'
_chemical_formula_sum            'C2 N2 Se'
_chemical_formula_weight         130.99
_chemical_name_common            'Selenium(II) dicyanide'
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Scherr, Matthias'
_audit_block_code                Se(CN)2_scherr_cx361
_audit_creation_date
;
'Mon Oct 29 08:09:20 2007'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record
;
'Tue Oct 30 10:54:14 2007'
;
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   8.632(5)
_cell_length_b                   6.847(5)
_cell_length_c                   12.8151(7)
_cell_measurement_reflns_used    940
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.9952
_cell_measurement_theta_min      3.7865
_cell_volume                     757.4(7)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_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(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -101.00  -51.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1682  -45.0000  240.0000    0.0000    0.0000 50

  2 omega  -25.00   24.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1682   99.0000   12.0000    0.0000    0.0000 49

  3 omega   50.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.3244 -137.0000  -81.0000    0.0000    0.0000 45

  4 omega    3.00   47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.3244   45.0000    0.0000    0.0000    0.0000 44

  5 omega  -11.00   17.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.3244   99.0000   93.0000    0.0000    0.0000 28

  6 omega  -36.00   -8.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.3244  137.0000  161.0000    0.0000    0.0000 28

  7 omega  -42.00  -14.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.3244  -75.0000  120.0000    0.0000    0.0000 28

;
_diffrn_measurement_device_type  'Oxford Xcalibur3 CCD area-detector'
_diffrn_measurement_method       'omega scan'
_diffrn_orient_matrix_UB_11      -0.0664819746
_diffrn_orient_matrix_UB_12      0.0592385994
_diffrn_orient_matrix_UB_13      -0.0140834281
_diffrn_orient_matrix_UB_21      -0.0791550183
_diffrn_orient_matrix_UB_22      -0.0503222967
_diffrn_orient_matrix_UB_23      0.0107911180
_diffrn_orient_matrix_UB_31      -0.0014935643
_diffrn_orient_matrix_UB_32      0.0263908781
_diffrn_orient_matrix_UB_33      0.0523515409
_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  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2804
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         3.96
_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    9.688
_exptl_absorpt_correction_T_max  0.68000
_exptl_absorpt_correction_T_min  0.26952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.2974(3)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.341
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                421
_reflns_number_total             743
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801011g-file001.cif
_cod_data_source_block           cx361
_cod_database_code               4306092
_kl_diffrn_measurement_detector_distance 50