Synthesis and Structural Characterization of Novel Neutral Hexacoordinate Silicon(IV) Complexes with SiO2N4 Skeletons Containing Cyanato-N or Thiocyanato-N Ligands
Oliver Seiler; Christian Burschka; Markus Fischer; Martin Penka; Reinhold Tacke; Inorganic Chemistry 44 (2005) 2337–2346; doi:10.1021/ic0485211

data_4308978
_publ_contact_author_address
;
Institut f\"ur Anorganische Chemie
Universit\"at W\"urzburg
Am Hubland
97074 W\"urzburg
Bundesrepublik Deutschland
;
_publ_contact_author_email       r.tacke@mail.uni-wuerzburg.de
_publ_contact_author_fax         '049 931 888-4609'
_publ_contact_author_name        'Professor Dr. Reinhold Tacke'
_publ_contact_author_phone       '049 931 888-5250'
_publ_section_title
;
Synthesis and Structural Characterization of Novel Neutral Hexacoordinate
Silicon(IV) Complexes with SiO2N4 Skeletons Containing Cyanato-N or
Thiocyanato-N Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2337
_journal_page_last               2346
_journal_paper_doi               10.1021/ic0485211
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C24 H24 N4 O4 Si'
_chemical_formula_sum            'C24 H24 N4 O4 Si'
_chemical_formula_weight         460.56
_chemical_name_common
;(OC-6-12)-Di(cyanato-N)bis(4-(phenylimino)pent-2-en-2-olato(1-
)-N,O)silicon(IV)
;
_chemical_name_systematic
;
(OC-6-12)-Di(cyanato-N)bis[4-(phenylimino)pent-2-en-2-olato(1-)-N,O]silicon(IV)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.584(17)
_cell_angle_beta                 89.652(17)
_cell_angle_gamma                64.888(16)
_cell_formula_units_Z            1
_cell_length_a                   7.8647(11)
_cell_length_b                   8.9206(13)
_cell_length_c                   9.0668(13)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      2.55
_cell_volume                     566.79(16)
_computing_cell_refinement       'Stoe-IPDS cell'
_computing_data_collection       'Stoe-IPDS expose'
_computing_data_reduction        'Stoe-IPDS integrate'
_computing_molecular_graphics    ORTEP-POVRAY
_computing_publication_material  'Bruker Shelxtl'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997), Version 6.10'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       Phi-Scans
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6024
_diffrn_reflns_theta_full        27.07
_diffrn_reflns_theta_max         27.07
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             242
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0489P)^2^+0.1959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                2038
_reflns_number_total             2277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0485211si20041027_112104_3.cif
_cod_data_source_block           4
_cod_original_cell_volume        566.79(14)
_cod_database_code               4308978