#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:46:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179127 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/89/4308979.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4308979
loop_
_publ_author_name
'Oliver Seiler'
'Christian Burschka'
'Markus Fischer'
'Martin Penka'
'Reinhold Tacke'
_publ_contact_author_address
;
Institut für Anorganische Chemie
Universität Würzburg
Am Hubland
97074 Würzburg
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 O2 S2 Si'
_chemical_formula_sum            'C24 H24 N4 O2 S2 Si'
_chemical_formula_weight         492.68
_chemical_name_common
;
(OC-6-12)-Bis(4-(phenylimino)pent-2-en-2-olato(1-)-N,O)-
di(thiocyanato-N)silicon(IV)
;
_chemical_name_systematic
;
(OC-6-12)-Bis[4-(phenylimino)pent-2-en-2-olato(1-)-N,O]-
di(thiocyanato-N)silicon(IV)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.082(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.299(2)
_cell_length_b                   11.8942(16)
_cell_length_c                   12.1345(16)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.9
_cell_measurement_theta_min      2.1
_cell_volume                     2421.7(6)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10007
_diffrn_reflns_theta_full        26.93
_diffrn_reflns_theta_max         26.93
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0355
_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/[σ²(Fo²)+(0.0560P)²+1.4300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                2294
_reflns_number_total             2603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0485211si20041027_112104_4.cif
_cod_data_source_block           5
_cod_original_cell_volume        2421.7(5)
_cod_database_code               4308979
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si Si 0.2500 0.2500 1.0000 0.02145(14) Uani 1 2 d S . .
O O 0.20384(6) 0.21350(9) 0.86145(8) 0.0269(2) Uani 1 1 d . . .
N2 N 0.25799(7) 0.09351(10) 1.03778(9) 0.0242(2) Uani 1 1 d . . .
N1 N 0.34672(7) 0.24112(10) 0.96260(10) 0.0274(3) Uani 1 1 d . . .
C1 C 0.40331(8) 0.19742(12) 0.94603(11) 0.0258(3) Uani 1 1 d . . .
S S 0.48077(2) 0.13939(4) 0.92272(4) 0.04415(15) Uani 1 1 d . . .
C2 C 0.09674(11) 0.19456(16) 0.69993(14) 0.0438(4) Uani 1 1 d . . .
H2A H 0.1303 0.1680 0.6508 0.066 Uiso 1 1 calc R . .
H2B H 0.0521 0.2383 0.6548 0.066 Uiso 1 1 calc R . .
H2C H 0.0761 0.1299 0.7339 0.066 Uiso 1 1 calc R . .
C3 C 0.14493(8) 0.26668(13) 0.79162(11) 0.0283(3) Uani 1 1 d . . .
C4 C 0.36702(9) 0.12162(13) 1.19986(12) 0.0303(3) Uani 1 1 d . . .
H4 H 0.4129 0.0886 1.2483 0.036 Uiso 1 1 calc R . .
C5 C 0.31383(8) 0.05165(12) 1.12140(11) 0.0275(3) Uani 1 1 d . . .
C6 C 0.32210(10) -0.07256(14) 1.14093(14) 0.0376(4) Uani 1 1 d . . .
H6A H 0.2724 -0.1028 1.1539 0.056 Uiso 1 1 calc R . .
H6B H 0.3659 -0.0874 1.2076 0.056 Uiso 1 1 calc R . .
H6C H 0.3335 -0.1088 1.0741 0.056 Uiso 1 1 calc R . .
C7 C 0.20581(8) 0.01526(11) 0.96466(11) 0.0257(3) Uani 1 1 d . . .
C8 C 0.12954(9) -0.00241(13) 0.97722(13) 0.0322(3) Uani 1 1 d . . .
H8 H 0.1111 0.0368 1.0341 0.039 Uiso 1 1 calc R . .
C9 C 0.08030(9) -0.07773(15) 0.90624(15) 0.0391(4) Uani 1 1 d . . .
H9 H 0.0277 -0.0900 0.9143 0.047 Uiso 1 1 calc R . .
C10 C 0.10692(10) -0.13525(14) 0.82382(15) 0.0386(4) Uani 1 1 d . . .
H10 H 0.0730 -0.1876 0.7760 0.046 Uiso 1 1 calc R . .
C11 C 0.18302(10) -0.11651(14) 0.81098(13) 0.0362(3) Uani 1 1 d . . .
H11 H 0.2013 -0.1556 0.7539 0.043 Uiso 1 1 calc R . .
C12 C 0.23258(9) -0.04128(13) 0.88087(12) 0.0318(3) Uani 1 1 d . . .
H12 H 0.2848 -0.0282 0.8718 0.038 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O Si O 180.0 . 7_557 y
O Si N1 88.76(5) . . y
O Si N1 91.24(5) 7_557 . y
O Si N1 91.24(5) . 7_557 y
O Si N1 88.76(5) 7_557 7_557 y
N1 Si N1 180.0 . 7_557 y
O Si N2 88.74(5) . . y
O Si N2 91.26(5) 7_557 . y
N1 Si N2 89.21(5) . . y
N1 Si N2 90.79(5) 7_557 . y
O Si N2 91.26(5) . 7_557 y
O Si N2 88.74(5) 7_557 7_557 y
N1 Si N2 90.79(5) . 7_557 y
N1 Si N2 89.21(5) 7_557 7_557 y
N2 Si N2 180.0 . 7_557 y
C3 O Si 127.28(9) . . ?
C5 N2 C7 117.53(12) . . ?
C5 N2 Si 123.30(10) . . ?
C7 N2 Si 118.85(9) . . ?
C1 N1 Si 156.68(12) . . y
N1 C1 S 179.22(14) . . y
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O C3 C4 122.08(13) . 7_557 ?
O C3 C2 114.13(13) . . ?
C4 C3 C2 123.70(14) 7_557 . ?
C3 C4 C5 122.72(13) 7_557 . ?
C3 C4 H4 118.6 7_557 . ?
C5 C4 H4 118.6 . . ?
N2 C5 C4 121.93(13) . . ?
N2 C5 C6 121.26(14) . . ?
C4 C5 C6 116.77(13) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C12 120.32(14) . . ?
C8 C7 N2 120.16(12) . . ?
C12 C7 N2 119.51(13) . . ?
C7 C8 C9 119.35(14) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C10 C9 C8 120.59(15) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 119.81(15) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 120.18(14) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C7 119.75(14) . . ?
C11 C12 H12 120.1 . . ?
C7 C12 H12 120.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si O 1.7318(10) . y
Si O 1.7318(10) 7_557 y
Si N1 1.8401(12) . y
Si N1 1.8401(12) 7_557 y
Si N2 1.9138(12) . y
Si N2 1.9138(12) 7_557 y
O C3 1.3178(17) . ?
N2 C5 1.3167(18) . ?
N2 C7 1.4417(18) . ?
N1 C1 1.1684(19) . y
C1 S 1.5925(14) . y
C2 C3 1.489(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.352(2) 7_557 ?
C4 C3 1.352(2) 7_557 ?
C4 C5 1.421(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.498(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.381(2) . ?
C7 C12 1.389(2) . ?
C8 C9 1.383(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.380(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.379(2) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
