#------------------------------------------------------------------------------ #$Date: 2016-03-22 11:58:54 +0200 (Tue, 22 Mar 2016) $ #$Revision: 178927 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/11/56/4115646.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_4115646 loop_ _publ_author_name 'Michael J. Bearpark' 'G. Sean McGrady' 'Paul D. Prince' 'Jonathan W. Steed' _publ_section_title ; The First Structurally Characterized Hypervalent Silicon Hydride: Unexpected Molecular Geometry and Si-H...K Interactions ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 7736 _journal_page_last 7737 _journal_paper_doi 10.1021/ja0162616 _journal_volume 123 _journal_year 2001 _chemical_formula_sum 'C30 H41 K O6 Si' _chemical_formula_weight 564.82 _chemical_name_systematic ; ? ; _space_group_IT_number 146 _symmetry_cell_setting rhombohedral _symmetry_space_group_name_Hall 'P 3*' _symmetry_space_group_name_H-M 'R 3 :R' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 97.930(10) _cell_angle_beta 97.930(10) _cell_angle_gamma 97.930(10) _cell_formula_units_Z 1 _cell_length_a 9.4424(15) _cell_length_b 9.4424(15) _cell_length_c 9.4424(15) _cell_measurement_temperature 393(2) _cell_volume 815.2(2) _computing_cell_refinement DENZO-SMN _computing_data_collection 'Nonius Collect' _computing_data_reduction DENZO-SMN _computing_molecular_graphics 'XSeed (Barbour, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 393(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi scans 6s/o' _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 0.0800 _diffrn_reflns_av_sigmaI/netI 0.1117 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 4386 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 2.21 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 0.236 _exptl_absorpt_correction_T_max 0.9543 _exptl_absorpt_correction_T_min 0.9543 _exptl_absorpt_correction_type Scalepack _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.151 _exptl_crystal_description prism _exptl_crystal_F_000 302 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.394 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.075 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(7) _refine_ls_extinction_coef 0.041(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 171 _refine_ls_number_reflns 2257 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0462 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.0933 _reflns_number_gt 1650 _reflns_number_total 2257 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ja0162616_s1.cif _cod_data_source_block ppbypa(trigonal_K[Ph3SiH2]18C6) _cod_original_sg_symbol_H-M 'R 3' _cod_database_code 4115646 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' 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 K1 K 0.61310(7) 0.61310(7) 0.61310(7) 0.0251(3) Uani 1 3 d S Si1 Si 0.92404(11) 0.92404(11) 0.92404(11) 0.0342(4) Uani 1 3 d S O1 O 0.3687(2) 0.7064(2) 0.7066(3) 0.0343(5) Uani 1 1 d . C1 C 0.2821(4) 0.6140(5) 0.7799(5) 0.0489(10) Uani 1 1 d . H1 H 1.042(3) 1.042(3) 1.042(3) 0.038(14) Uiso 1 3 d S H2 H 0.8073 0.8063 0.8063 0.046 Uiso 1 3 d SR O2 O 0.7927(2) 0.4605(2) 0.4602(2) 0.0347(6) Uani 1 1 d . C2 C 0.2824(4) 0.7806(5) 0.6140(5) 0.0488(10) Uani 1 1 d . C3 C 0.8780(4) 0.5481(5) 0.3814(4) 0.0478(10) Uani 1 1 d . C4 C 0.8777(4) 0.3812(4) 0.5478(5) 0.0483(10) Uani 1 1 d . C5 C 1.0006(3) 0.7659(3) 1.0001(3) 0.0334(8) Uani 1 1 d . C6 C 0.9439(3) 0.6202(3) 0.9435(3) 0.0335(7) Uani 1 1 d . H6 H 0.855(3) 0.595(3) 0.859(3) 0.040(8) Uiso 1 1 d . C7 C 0.9981(4) 0.5055(4) 0.9989(4) 0.0401(9) Uani 1 1 d . H7 H 0.956(4) 0.408(4) 0.960(4) 0.048(10) Uiso 1 1 d . C8 C 1.1121(4) 0.5314(4) 1.1115(4) 0.0419(9) Uani 1 1 d . H8 H 1.155(3) 0.442(3) 1.153(3) 0.031(8) Uiso 1 1 d . C9 C 1.1696(4) 0.6730(5) 1.1713(4) 0.0497(10) Uani 1 1 d . H9 H 1.240(4) 0.685(4) 1.239(4) 0.042(10) Uiso 1 1 d . C10 C 1.1157(4) 0.7887(5) 1.1162(4) 0.0409(9) Uani 1 1 d . H10 H 1.154(4) 0.891(5) 1.153(4) 0.077(14) Uiso 1 1 d . H1A H 0.215(4) 0.532(4) 0.708(4) 0.051(10) Uiso 1 1 d . H2A H 0.221(4) 0.841(4) 0.673(4) 0.052(10) Uiso 1 1 d . H3A H 0.943(4) 0.482(4) 0.335(4) 0.070(11) Uiso 1 1 d . H4A H 0.945(4) 0.444(4) 0.622(4) 0.047(11) Uiso 1 1 d . H1B H 0.225(4) 0.667(4) 0.843(4) 0.054(10) Uiso 1 1 d . H2B H 0.217(4) 0.714(4) 0.539(4) 0.053(11) Uiso 1 1 d . H3B H 0.945(4) 0.620(4) 0.450(4) 0.043(10) Uiso 1 1 d . H4B H 0.942(4) 0.330(4) 0.480(4) 0.054(10) Uiso 1 1 d . 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 K1 0.0257(3) 0.0257(3) 0.0257(3) 0.0061(4) 0.0061(4) 0.0061(4) Si1 0.0327(5) 0.0327(5) 0.0327(5) -0.0002(5) -0.0002(5) -0.0002(5) O1 0.0207(11) 0.0394(13) 0.0416(13) 0.0001(11) 0.0056(9) 0.0058(9) C1 0.035(2) 0.056(2) 0.057(2) -0.001(2) 0.0283(19) 0.0000(18) O2 0.0279(12) 0.0380(13) 0.0387(13) 0.0007(11) 0.0092(10) 0.0086(11) C2 0.0310(19) 0.057(2) 0.060(2) 0.002(2) 0.0027(18) 0.0237(19) C3 0.037(2) 0.056(2) 0.054(2) 0.003(2) 0.027(2) 0.004(2) C4 0.038(2) 0.054(3) 0.056(2) 0.004(2) 0.004(2) 0.027(2) C5 0.0242(16) 0.048(2) 0.0244(16) -0.0017(14) 0.0049(13) 0.0007(14) C6 0.0287(17) 0.0384(18) 0.0328(18) 0.0055(15) 0.0051(15) 0.0037(15) C7 0.0388(19) 0.043(2) 0.042(2) 0.0095(18) 0.0135(17) 0.0092(18) C8 0.038(2) 0.064(3) 0.0342(19) 0.017(2) 0.0179(17) 0.022(2) C9 0.033(2) 0.082(3) 0.037(2) 0.015(2) 0.0019(18) 0.016(2) C10 0.0308(19) 0.057(3) 0.0309(19) 0.0004(18) 0.0008(15) 0.0032(18) 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' 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' K K 0.2009 0.2494 '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 O1 K1 O1 119.096(19) 3 2 O1 K1 O1 119.096(19) 3 . O1 K1 O1 119.10(2) 2 . O1 K1 O2 59.53(7) 3 . O1 K1 O2 59.58(7) 2 . O1 K1 O2 162.45(8) . . O1 K1 O2 162.45(8) 3 3 O1 K1 O2 59.53(7) 2 3 O1 K1 O2 59.58(7) . 3 O2 K1 O2 115.75(3) . 3 O1 K1 O2 59.58(7) 3 2 O1 K1 O2 162.45(8) 2 2 O1 K1 O2 59.53(7) . 2 O2 K1 O2 115.75(3) . 2 O2 K1 O2 115.75(3) 3 2 C5 Si1 C5 119.983(5) 2 . C5 Si1 C5 119.983(5) 2 3 C5 Si1 C5 119.983(5) . 3 C1 O1 C2 111.9(3) . . C1 O1 K1 118.37(18) . . C2 O1 K1 118.25(18) . . O1 C1 C4 107.8(3) . 3 C3 O2 C4 112.4(3) . . C3 O2 K1 113.13(19) . . C4 O2 K1 113.02(19) . . O1 C2 C3 108.0(3) . 2 O2 C3 C2 108.9(3) . 3 O2 C4 C1 109.1(3) . 2 C10 C5 C6 115.7(3) . . C10 C5 Si1 122.2(3) . . C6 C5 Si1 122.1(2) . . C7 C6 C5 122.3(3) . . C8 C7 C6 120.6(4) . . C7 C8 C9 118.8(4) . . C8 C9 C10 120.9(4) . . C9 C10 C5 121.7(4) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 K1 O1 2.7907(18) 3 K1 O1 2.7907(18) 2 K1 O1 2.7907(18) . K1 O2 2.795(2) . K1 O2 2.795(2) 3 K1 O2 2.795(2) 2 Si1 C5 1.928(3) 2 Si1 C5 1.928(3) . Si1 C5 1.928(3) 3 O1 C1 1.426(4) . O1 C2 1.431(4) . C1 C4 1.484(5) 3 O2 C3 1.428(4) . O2 C4 1.429(4) . C2 C3 1.479(5) 2 C3 C2 1.479(5) 3 C4 C1 1.484(5) 2 C5 C10 1.404(4) . C5 C6 1.407(4) . C6 C7 1.394(4) . C7 C8 1.374(5) . C8 C9 1.381(6) . C9 C10 1.400(5) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C9 H9 O2 0.84(4) 2.72(4) 3.534(5) 166(3) 2_656 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_4 O1 K1 O1 C1 150.7(2) 3 . O1 K1 O1 C1 -10.5(3) 2 . O2 K1 O1 C1 70.2(4) . . O2 K1 O1 C1 -9.1(2) 3 . O2 K1 O1 C1 149.3(3) 2 . O1 K1 O1 C2 10.2(3) 3 . O1 K1 O1 C2 -151.0(2) 2 . O2 K1 O1 C2 -70.3(4) . . O2 K1 O1 C2 -149.6(3) 3 . O2 K1 O1 C2 8.8(3) 2 . C2 O1 C1 C4 -177.4(3) . 3 K1 O1 C1 C4 39.8(4) . 3 O1 K1 O2 C3 24.8(2) 3 . O1 K1 O2 C3 -153.8(2) 2 . O1 K1 O2 C3 115.5(3) . . O2 K1 O2 C3 -174.3(2) 3 . O2 K1 O2 C3 45.4(3) 2 . O1 K1 O2 C4 154.0(2) 3 . O1 K1 O2 C4 -24.6(2) 2 . O1 K1 O2 C4 -115.4(3) . . O2 K1 O2 C4 -45.2(3) 3 . O2 K1 O2 C4 174.6(2) 2 . C1 O1 C2 C3 177.6(3) . 2 K1 O1 C2 C3 -39.6(4) . 2 C4 O2 C3 C2 174.1(3) . 3 K1 O2 C3 C2 -56.4(3) . 3 C3 O2 C4 C1 -174.3(3) . 2 K1 O2 C4 C1 56.2(3) . 2 C5 Si1 C5 C10 91.8(3) 2 . C5 Si1 C5 C10 -90.9(3) 3 . C5 Si1 C5 C6 -88.8(3) 2 . C5 Si1 C5 C6 88.6(3) 3 . C10 C5 C6 C7 0.0(4) . . Si1 C5 C6 C7 -179.4(2) . . C5 C6 C7 C8 -0.9(5) . . C6 C7 C8 C9 1.7(5) . . C7 C8 C9 C10 -1.7(5) . . C8 C9 C10 C5 0.8(5) . . C6 C5 C10 C9 0.0(5) . . Si1 C5 C10 C9 179.5(3) . .