#------------------------------------------------------------------------------ #$Date: 2014-07-12 01:16:09 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120081 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/30/89/4308980.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_4308980 loop_ _publ_author_name 'Oliver Seiler' 'Christian Burschka' 'Markus Fischer' 'Martin Penka' 'Reinhold Tacke' _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_volume 44 _journal_year 2005 _chemical_formula_moiety 'C18 H28 N4 O2 S2 Si' _chemical_formula_sum 'C18 H28 N4 O2 S2 Si' _chemical_formula_weight 424.65 _chemical_name_common ; (OC-6-12)-Bis(4-(isopropylimino)pent-2-en-2-olato(1-)-N,O)- di(thiocyanato-N)silicon(IV) ; _chemical_name_systematic ; (OC-6-12)-Bis[4-(isopropylimino)pent-2-en-2-olato(1-)-N,O]- di(thiocyanato-N)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 76.053(15) _cell_angle_beta 84.672(15) _cell_angle_gamma 82.245(14) _cell_formula_units_Z 1 _cell_length_a 7.0217(9) _cell_length_b 8.6194(11) _cell_length_c 9.3688(13) _cell_measurement_reflns_used 5000 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.95 _cell_measurement_theta_min 5.85 _cell_volume 544.20(13) _computing_cell_refinement Stoe-IPDS _computing_data_collection Stoe-IPDS _computing_data_reduction Stoe-IPDS _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 0.905 _diffrn_measured_fraction_theta_max 0.905 _diffrn_measurement_device_type Stoe-IPDS _diffrn_measurement_method Stoe-IPDS _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 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0203 _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 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 6999 _diffrn_reflns_theta_full 27.93 _diffrn_reflns_theta_max 27.93 _diffrn_reflns_theta_min 3.69 _exptl_absorpt_coefficient_mu 0.320 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_description platelet _exptl_crystal_F_000 226 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.315 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.047 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 128 _refine_ls_number_reflns 2373 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.064 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0312 _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^)+(0.0543P)^2^+0.1193P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0860 _refine_ls_wR_factor_ref 0.0877 _reflns_number_gt 2150 _reflns_number_total 2373 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic0485211si20041027_112104_5.cif _[local]_cod_data_source_block 6 _cod_original_cell_volume 544.20(12) _cod_database_code 4308980 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 0.5000 1.0000 1.0000 0.01537(12) Uani 1 2 d S . . S S 0.21776(6) 1.43858(4) 0.66798(4) 0.03521(13) Uani 1 1 d . . . O O 0.31002(12) 0.89619(9) 0.98470(9) 0.01912(18) Uani 1 1 d . . . N1 N 0.37068(15) 1.18369(12) 0.88478(11) 0.0201(2) Uani 1 1 d . . . C3 C 0.32993(19) 0.75484(14) 0.94795(13) 0.0215(2) Uani 1 1 d . . . C1 C 0.30676(18) 1.29057(13) 0.79384(13) 0.0200(2) Uani 1 1 d . . . C4 C 0.48451(19) 0.70581(14) 0.86656(14) 0.0240(3) Uani 1 1 d . . . H4 H 0.5015 0.5974 0.8573 0.029 Uiso 1 1 calc R . . C2 C 0.1634(2) 0.65978(16) 1.00164(16) 0.0306(3) Uani 1 1 d . . . H2A H 0.1547 0.6308 1.1096 0.046 Uiso 1 1 calc R . . H2B H 0.1825 0.5617 0.9642 0.046 Uiso 1 1 calc R . . H2C H 0.0441 0.7247 0.9663 0.046 Uiso 1 1 calc R . . N2 N 0.63182(15) 0.95004(11) 0.82433(10) 0.0179(2) Uani 1 1 d . . . C5 C 0.62508(18) 0.81005(14) 0.79302(12) 0.0204(2) Uani 1 1 d . . . C8 C 0.6735(2) 1.12442(17) 0.56755(14) 0.0319(3) Uani 1 1 d . . . H8A H 0.7179 1.0380 0.5166 0.048 Uiso 1 1 calc R . . H8B H 0.7258 1.2234 0.5137 0.048 Uiso 1 1 calc R . . H8C H 0.5325 1.1426 0.5722 0.048 Uiso 1 1 calc R . . C6 C 0.7562(2) 0.74412(15) 0.67930(14) 0.0270(3) Uani 1 1 d . . . H6A H 0.8178 0.8318 0.6124 0.041 Uiso 1 1 calc R . . H6B H 0.6808 0.6949 0.6229 0.041 Uiso 1 1 calc R . . H6C H 0.8553 0.6629 0.7287 0.041 Uiso 1 1 calc R . . C7 C 0.74295(18) 1.07621(14) 0.72416(13) 0.0215(2) Uani 1 1 d . . . H7 H 0.7074 1.1746 0.7641 0.026 Uiso 1 1 calc R . . C9 C 0.9605(2) 1.03984(18) 0.73341(16) 0.0325(3) Uani 1 1 d . . . H9A H 0.9925 1.0196 0.8364 0.049 Uiso 1 1 calc R . . H9B H 1.0225 1.1321 0.6750 0.049 Uiso 1 1 calc R . . H9C H 1.0065 0.9445 0.6948 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si 0.0142(2) 0.0157(2) 0.0166(2) -0.00441(15) -0.00011(16) -0.00257(15) S 0.0480(3) 0.02389(18) 0.02789(19) 0.00146(13) -0.00628(16) 0.00564(14) O 0.0173(4) 0.0196(4) 0.0222(4) -0.0076(3) -0.0002(3) -0.0041(3) N1 0.0193(5) 0.0202(5) 0.0206(5) -0.0046(4) -0.0006(4) -0.0020(4) C3 0.0243(7) 0.0201(5) 0.0223(5) -0.0059(4) -0.0027(5) -0.0071(4) C1 0.0199(6) 0.0198(5) 0.0215(5) -0.0079(4) 0.0018(4) -0.0033(4) C4 0.0275(7) 0.0196(5) 0.0273(6) -0.0094(5) 0.0002(5) -0.0056(5) C2 0.0286(8) 0.0269(6) 0.0393(7) -0.0105(5) 0.0044(6) -0.0134(5) N2 0.0170(5) 0.0189(4) 0.0180(4) -0.0049(3) 0.0008(4) -0.0031(3) C5 0.0207(6) 0.0213(5) 0.0198(5) -0.0069(4) -0.0019(4) -0.0006(4) C8 0.0400(9) 0.0315(7) 0.0212(6) -0.0014(5) 0.0012(5) -0.0044(6) C6 0.0311(8) 0.0257(6) 0.0254(6) -0.0113(5) 0.0027(5) -0.0007(5) C7 0.0222(6) 0.0213(5) 0.0204(5) -0.0039(4) 0.0044(4) -0.0059(4) C9 0.0224(7) 0.0379(7) 0.0374(7) -0.0091(6) 0.0054(6) -0.0088(5) 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 180.000(1) 2_677 . ? O Si N1 88.27(4) 2_677 2_677 ? O Si N1 91.73(4) . 2_677 ? O Si N1 91.73(4) 2_677 . ? O Si N1 88.27(4) . . ? N1 Si N1 180.00(6) 2_677 . ? O Si N2 91.48(4) 2_677 2_677 ? O Si N2 88.52(4) . 2_677 ? N1 Si N2 89.44(5) 2_677 2_677 ? N1 Si N2 90.56(5) . 2_677 ? O Si N2 88.52(4) 2_677 . ? O Si N2 91.48(4) . . ? N1 Si N2 90.56(5) 2_677 . ? N1 Si N2 89.44(5) . . ? N2 Si N2 180.000(1) 2_677 . ? C3 O Si 124.59(8) . . ? C1 N1 Si 168.99(10) . . ? O C3 C4 122.27(11) . . ? O C3 C2 113.76(11) . . ? C4 C3 C2 123.95(11) . . ? N1 C1 S 179.88(14) . . ? C3 C4 C5 123.07(11) . . ? C5 N2 C7 121.23(10) . . ? C5 N2 Si 120.93(8) . . ? C7 N2 Si 117.84(7) . . ? N2 C5 C4 121.23(11) . . ? N2 C5 C6 124.97(11) . . ? C4 C5 C6 113.79(10) . . ? N2 C7 C9 113.82(10) . . ? N2 C7 C8 112.35(10) . . ? C9 C7 C8 115.04(11) . . ? 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 1.7378(8) 2_677 ? Si O 1.7378(8) . ? Si N1 1.8619(11) 2_677 ? Si N1 1.8619(11) . ? Si N2 1.9241(10) 2_677 ? Si N2 1.9241(10) . ? S C1 1.6140(13) . ? O C3 1.3304(14) . ? N1 C1 1.1649(17) . ? C3 C4 1.3476(19) . ? C3 C2 1.4973(17) . ? C4 C5 1.4390(17) . ? N2 C5 1.3164(14) . ? N2 C7 1.5078(14) . ? C5 C6 1.5081(17) . ? C8 C7 1.5321(17) . ? C7 C9 1.5237(19) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O Si O C3 0(100) 2_677 . . . ? N1 Si O C3 -48.63(9) 2_677 . . . ? N1 Si O C3 131.37(9) . . . . ? N2 Si O C3 -138.03(9) 2_677 . . . ? N2 Si O C3 41.97(9) . . . . ? O Si N1 C1 88.3(5) 2_677 . . . ? O Si N1 C1 -91.7(5) . . . . ? N1 Si N1 C1 103(100) 2_677 . . . ? N2 Si N1 C1 179.8(5) 2_677 . . . ? N2 Si N1 C1 -0.2(5) . . . . ? Si O C3 C4 -25.90(16) . . . . ? Si O C3 C2 155.73(9) . . . . ? Si N1 C1 S 129(100) . . . . ? O C3 C4 C5 -10.20(19) . . . . ? C2 C3 C4 C5 168.01(12) . . . . ? O Si N2 C5 143.65(10) 2_677 . . . ? O Si N2 C5 -36.35(10) . . . . ? N1 Si N2 C5 55.40(10) 2_677 . . . ? N1 Si N2 C5 -124.60(10) . . . . ? N2 Si N2 C5 -116(100) 2_677 . . . ? O Si N2 C7 -36.28(8) 2_677 . . . ? O Si N2 C7 143.72(8) . . . . ? N1 Si N2 C7 -124.53(9) 2_677 . . . ? N1 Si N2 C7 55.47(9) . . . . ? N2 Si N2 C7 64(100) 2_677 . . . ? C7 N2 C5 C4 -164.71(11) . . . . ? Si N2 C5 C4 15.36(16) . . . . ? C7 N2 C5 C6 14.40(18) . . . . ? Si N2 C5 C6 -165.52(9) . . . . ? C3 C4 C5 N2 13.62(19) . . . . ? C3 C4 C5 C6 -165.59(12) . . . . ? C5 N2 C7 C9 -74.90(14) . . . . ? Si N2 C7 C9 105.03(11) . . . . ? C5 N2 C7 C8 58.08(15) . . . . ? Si N2 C7 C8 -121.99(10) . . . . ? _journal_paper_doi 10.1021/ic0485211