# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'ProfD Christoph Marschner' _publ_contact_author_address ; Institut fur Anorganische Chemie Technische Universitat Graz Stremayrgasse 16 Graz A-8010 AUSTRIA ; _publ_contact_author_phone '+43 316 873 8209' _publ_contact_author_fax '+43 316 873 8701' _publ_contact_author_email marschner@anorg.tu-graz.ac.at _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; _publ_section_title ; Preparation and Structural Characterisation of Methoxy-bis(trimethylsilyl)silyl Potassium and its Condensation Product ; loop_ _publ_author_name 'Christoph Marschner' 'Judith Baumgartner' 'Pravin R. Likhar' 'Michaela Zirngast' data_147j _database_code_depnum_ccdc_archive 'CCDC 232700' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H45 K O7 Si3' _chemical_formula_weight 508.92 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.6523(19) _cell_length_b 18.092(4) _cell_length_c 34.297(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5989(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour 'slight yellow' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.328 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details XPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40265 _diffrn_reflns_av_R_equivalents 0.0938 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5291 _reflns_number_gt 4350 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (1998)' _computing_cell_refinement 'Bruker SAINT (1998)' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+6.5766P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5291 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.1593 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.184 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 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 K1 K 0.28693(8) 0.04524(4) 0.13441(2) 0.0312(2) Uani 1 1 d . . . Si1 Si 0.02958(11) 0.18728(6) 0.12833(3) 0.0330(3) Uani 1 1 d . . . Si2 Si -0.00374(12) 0.29121(6) 0.16914(3) 0.0346(3) Uani 1 1 d . . . Si3 Si -0.04862(12) 0.23697(6) 0.06836(3) 0.0392(3) Uani 1 1 d . . . O1 O 0.0683(3) -0.05888(15) 0.14160(8) 0.0441(7) Uani 1 1 d . . . O2 O 0.1499(3) -0.00377(15) 0.06815(8) 0.0427(7) Uani 1 1 d . . . O3 O 0.4295(3) 0.03647(15) 0.06032(7) 0.0408(7) Uani 1 1 d . . . O4 O 0.5592(3) 0.09842(15) 0.12716(7) 0.0385(6) Uani 1 1 d . . . O5 O 0.4599(3) 0.06579(14) 0.20293(7) 0.0372(6) Uani 1 1 d . . . O6 O 0.1885(3) 0.00878(15) 0.20930(8) 0.0411(7) Uani 1 1 d . . . O7 O 0.2103(3) 0.18187(15) 0.12372(9) 0.0470(7) Uani 1 1 d . . . C1 C -0.0257(5) -0.0479(3) 0.11029(13) 0.0521(12) Uani 1 1 d . . . H1A H -0.0629 0.0019 0.1113 0.063 Uiso 1 1 calc R . . H1B H -0.1021 -0.0824 0.1124 0.063 Uiso 1 1 calc R . . C2 C 0.0487(5) -0.0594(3) 0.07252(13) 0.0514(12) Uani 1 1 d . . . H2A H 0.0924 -0.1077 0.0723 0.062 Uiso 1 1 calc R . . H2B H -0.0166 -0.0572 0.0510 0.062 Uiso 1 1 calc R . . C3 C 0.2218(5) -0.0076(3) 0.03213(11) 0.0480(11) Uani 1 1 d . . . H3A H 0.1573 -0.0008 0.0108 0.058 Uiso 1 1 calc R . . H3B H 0.2647 -0.0558 0.0293 0.058 Uiso 1 1 calc R . . C4 C 0.3307(5) 0.0514(2) 0.03084(11) 0.0477(11) Uani 1 1 d . . . H4A H 0.3753 0.0517 0.0055 0.057 Uiso 1 1 calc R . . H4B H 0.2889 0.0994 0.0351 0.057 Uiso 1 1 calc R . . C5 C 0.5445(4) 0.0855(2) 0.05873(11) 0.0443(10) Uani 1 1 d . . . H5A H 0.5120 0.1362 0.0581 0.053 Uiso 1 1 calc R . . H5B H 0.5977 0.0764 0.0352 0.053 Uiso 1 1 calc R . . C6 C 0.6337(4) 0.0737(2) 0.09385(12) 0.0432(10) Uani 1 1 d . . . H6A H 0.6562 0.0217 0.0965 0.052 Uiso 1 1 calc R . . H6B H 0.7194 0.1012 0.0913 0.052 Uiso 1 1 calc R . . C7 C 0.6423(4) 0.1008(2) 0.16129(12) 0.0438(10) Uani 1 1 d . . . H7A H 0.7177 0.1356 0.1578 0.053 Uiso 1 1 calc R . . H7B H 0.6817 0.0524 0.1664 0.053 Uiso 1 1 calc R . . C8 C 0.5538(4) 0.1241(2) 0.19472(12) 0.0432(10) Uani 1 1 d . . . H8A H 0.6108 0.1342 0.2174 0.052 Uiso 1 1 calc R . . H8B H 0.5033 0.1687 0.1881 0.052 Uiso 1 1 calc R . . C9 C 0.3731(5) 0.0788(2) 0.23566(11) 0.0440(10) Uani 1 1 d . . . H9A H 0.3166 0.1224 0.2313 0.053 Uiso 1 1 calc R . . H9B H 0.4288 0.0868 0.2588 0.053 Uiso 1 1 calc R . . C10 C 0.2830(5) 0.0125(2) 0.24085(11) 0.0444(10) Uani 1 1 d . . . H10A H 0.3394 -0.0319 0.2415 0.053 Uiso 1 1 calc R . . H10B H 0.2327 0.0161 0.2653 0.053 Uiso 1 1 calc R . . C11 C 0.1068(5) -0.0563(3) 0.21002(13) 0.0496(11) Uani 1 1 d . . . H11A H 0.0611 -0.0609 0.2351 0.059 Uiso 1 1 calc R . . H11B H 0.1653 -0.0993 0.2063 0.059 Uiso 1 1 calc R . . C12 C 0.0012(5) -0.0523(3) 0.17834(13) 0.0540(12) Uani 1 1 d . . . H12A H -0.0657 -0.0918 0.1815 0.065 Uiso 1 1 calc R . . H12B H -0.0477 -0.0055 0.1797 0.065 Uiso 1 1 calc R . . C13 C 0.2968(5) 0.2427(3) 0.11591(17) 0.0665(15) Uani 1 1 d . . . H13A H 0.2745 0.2628 0.0908 0.100 Uiso 1 1 calc R . . H13B H 0.3918 0.2270 0.1161 0.100 Uiso 1 1 calc R . . H13C H 0.2832 0.2799 0.1355 0.100 Uiso 1 1 calc R . . C14 C 0.1001(6) 0.2772(3) 0.21530(13) 0.0606(14) Uani 1 1 d . . . H14A H 0.1971 0.2764 0.2091 0.091 Uiso 1 1 calc R . . H14B H 0.0744 0.2311 0.2271 0.091 Uiso 1 1 calc R . . H14C H 0.0816 0.3169 0.2331 0.091 Uiso 1 1 calc R . . C15 C -0.1902(5) 0.2966(3) 0.18559(14) 0.0593(13) Uani 1 1 d . . . H15A H -0.2130 0.2531 0.2003 0.089 Uiso 1 1 calc R . . H15B H -0.2496 0.2997 0.1632 0.089 Uiso 1 1 calc R . . H15C H -0.2028 0.3396 0.2016 0.089 Uiso 1 1 calc R . . C16 C 0.0420(6) 0.3878(2) 0.15209(15) 0.0478(11) Uani 1 1 d . . . C17 C -0.2319(5) 0.2735(3) 0.07367(15) 0.0643(14) Uani 1 1 d . . . H17A H -0.2754 0.2753 0.0485 0.096 Uiso 1 1 calc R . . H17B H -0.2293 0.3223 0.0846 0.096 Uiso 1 1 calc R . . H17C H -0.2837 0.2414 0.0905 0.096 Uiso 1 1 calc R . . C18 C 0.0498(6) 0.3137(3) 0.04313(15) 0.0743(17) Uani 1 1 d . . . H18A H 0.1420 0.2973 0.0373 0.111 Uiso 1 1 calc R . . H18B H 0.0540 0.3561 0.0599 0.111 Uiso 1 1 calc R . . H18C H 0.0032 0.3267 0.0194 0.111 Uiso 1 1 calc R . . C19 C -0.0564(5) 0.1621(3) 0.02978(13) 0.0554(12) Uani 1 1 d . . . H19A H -0.1057 0.1802 0.0074 0.083 Uiso 1 1 calc R . . H19B H -0.1033 0.1196 0.0401 0.083 Uiso 1 1 calc R . . H19C H 0.0360 0.1486 0.0223 0.083 Uiso 1 1 calc R . . H1 H -0.015(5) 0.402(3) 0.1318(14) 0.058(15) Uiso 1 1 d . . . H2 H 0.014(5) 0.422(3) 0.1721(15) 0.063(14) Uiso 1 1 d . . . H3 H 0.138(5) 0.392(3) 0.1441(14) 0.061(15) 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 0.0347(4) 0.0297(4) 0.0292(4) 0.0010(3) -0.0017(3) -0.0006(3) Si1 0.0362(6) 0.0235(5) 0.0393(6) 0.0002(4) 0.0003(5) 0.0003(4) Si2 0.0433(6) 0.0276(5) 0.0328(6) -0.0001(4) -0.0026(5) -0.0003(5) Si3 0.0466(7) 0.0372(6) 0.0339(6) -0.0018(5) -0.0014(5) 0.0041(5) O1 0.0375(15) 0.0460(17) 0.0488(17) -0.0024(13) -0.0002(13) -0.0020(13) O2 0.0468(17) 0.0420(16) 0.0392(16) -0.0102(12) -0.0085(13) 0.0017(14) O3 0.0485(17) 0.0455(16) 0.0285(14) 0.0038(12) -0.0042(12) -0.0004(14) O4 0.0339(14) 0.0489(16) 0.0325(14) 0.0004(12) -0.0007(12) 0.0011(13) O5 0.0428(16) 0.0393(15) 0.0295(14) -0.0059(11) 0.0009(12) -0.0012(13) O6 0.0406(16) 0.0480(17) 0.0348(15) 0.0073(12) 0.0043(12) 0.0040(13) O7 0.0407(17) 0.0305(15) 0.070(2) 0.0006(13) 0.0017(15) 0.0017(13) C1 0.040(2) 0.051(3) 0.065(3) -0.007(2) -0.011(2) -0.005(2) C2 0.052(3) 0.050(3) 0.053(3) -0.009(2) -0.019(2) -0.006(2) C3 0.060(3) 0.053(3) 0.031(2) -0.0050(19) -0.015(2) 0.008(2) C4 0.064(3) 0.050(3) 0.029(2) 0.0015(18) -0.006(2) 0.006(2) C5 0.048(3) 0.054(3) 0.031(2) 0.0028(18) 0.0100(19) -0.001(2) C6 0.038(2) 0.046(2) 0.045(2) 0.0002(19) 0.0082(19) -0.0007(19) C7 0.035(2) 0.053(3) 0.044(2) 0.002(2) -0.0066(19) -0.012(2) C8 0.050(3) 0.042(2) 0.038(2) -0.0060(18) -0.009(2) -0.006(2) C9 0.057(3) 0.048(3) 0.028(2) -0.0045(18) -0.0002(19) 0.007(2) C10 0.055(3) 0.052(3) 0.026(2) 0.0011(18) 0.0064(19) 0.006(2) C11 0.045(3) 0.055(3) 0.048(3) 0.011(2) 0.013(2) -0.001(2) C12 0.037(2) 0.066(3) 0.059(3) 0.000(2) 0.008(2) -0.011(2) C13 0.044(3) 0.045(3) 0.111(4) 0.013(3) 0.004(3) 0.002(2) C14 0.091(4) 0.045(3) 0.045(3) 0.006(2) -0.025(3) -0.009(3) C15 0.061(3) 0.057(3) 0.059(3) -0.019(2) 0.014(2) 0.000(2) C16 0.068(4) 0.031(2) 0.044(3) -0.001(2) -0.001(3) 0.003(2) C17 0.062(3) 0.071(3) 0.060(3) -0.015(3) -0.013(3) 0.024(3) C18 0.113(5) 0.062(3) 0.048(3) 0.014(2) 0.003(3) -0.018(3) C19 0.060(3) 0.063(3) 0.043(3) -0.014(2) -0.003(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 K1 O7 2.606(3) . ? K1 O2 2.775(3) . ? K1 O4 2.809(3) . ? K1 O6 2.817(3) . ? K1 O1 2.839(3) . ? K1 O3 2.894(3) . ? K1 O5 2.906(3) . ? K1 C16 3.349(5) 8_655 ? K1 Si1 3.5802(14) . ? Si1 O7 1.754(3) . ? Si1 Si2 2.3661(15) . ? Si1 Si3 2.3682(16) . ? Si2 C15 1.889(5) . ? Si2 C14 1.891(4) . ? Si2 C16 1.894(5) . ? Si3 C18 1.892(5) . ? Si3 C19 1.895(4) . ? Si3 C17 1.897(5) . ? O1 C1 1.420(5) . ? O1 C12 1.422(5) . ? O2 C2 1.411(5) . ? O2 C3 1.419(5) . ? O3 C4 1.416(5) . ? O3 C5 1.422(5) . ? O4 C7 1.420(5) . ? O4 C6 1.422(5) . ? O5 C8 1.419(5) . ? O5 C9 1.420(5) . ? O6 C10 1.416(5) . ? O6 C11 1.417(5) . ? O7 C13 1.408(5) . ? C1 C2 1.496(6) . ? C3 C4 1.498(6) . ? C5 C6 1.496(6) . ? C7 C8 1.491(6) . ? C9 C10 1.492(6) . ? C11 C12 1.491(6) . ? C16 K1 3.349(5) 8_665 ? 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 O7 K1 O2 93.02(9) . . ? O7 K1 O4 85.89(9) . . ? O2 K1 O4 118.86(8) . . ? O7 K1 O6 104.75(9) . . ? O2 K1 O6 120.74(9) . . ? O4 K1 O6 118.45(8) . . ? O7 K1 O1 115.50(9) . . ? O2 K1 O1 60.32(8) . . ? O4 K1 O1 158.44(9) . . ? O6 K1 O1 60.98(8) . . ? O7 K1 O3 93.64(9) . . ? O2 K1 O3 59.33(8) . . ? O4 K1 O3 59.75(8) . . ? O6 K1 O3 161.46(8) . . ? O1 K1 O3 113.16(8) . . ? O7 K1 O5 98.95(9) . . ? O2 K1 O5 167.63(8) . . ? O4 K1 O5 59.38(7) . . ? O6 K1 O5 59.10(8) . . ? O1 K1 O5 116.20(8) . . ? O3 K1 O5 116.35(8) . . ? O7 K1 C16 166.54(12) . 8_655 ? O2 K1 C16 96.39(11) . 8_655 ? O4 K1 C16 81.15(11) . 8_655 ? O6 K1 C16 78.58(11) . 8_655 ? O1 K1 C16 77.66(12) . 8_655 ? O3 K1 C16 82.98(11) . 8_655 ? O5 K1 C16 71.29(10) . 8_655 ? O7 K1 Si1 27.63(6) . . ? O2 K1 Si1 81.43(6) . . ? O4 K1 Si1 113.45(6) . . ? O6 K1 Si1 89.27(6) . . ? O1 K1 Si1 88.03(6) . . ? O3 K1 Si1 108.55(6) . . ? O5 K1 Si1 110.72(6) . . ? C16 K1 Si1 164.47(10) 8_655 . ? O7 Si1 Si2 103.46(11) . . ? O7 Si1 Si3 105.06(11) . . ? Si2 Si1 Si3 99.72(5) . . ? O7 Si1 K1 43.55(9) . . ? Si2 Si1 K1 129.06(5) . . ? Si3 Si1 K1 122.97(5) . . ? C15 Si2 C14 105.2(2) . . ? C15 Si2 C16 105.5(2) . . ? C14 Si2 C16 105.0(2) . . ? C15 Si2 Si1 110.31(15) . . ? C14 Si2 Si1 108.45(16) . . ? C16 Si2 Si1 121.23(17) . . ? C18 Si3 C19 103.0(2) . . ? C18 Si3 C17 104.8(3) . . ? C19 Si3 C17 106.2(2) . . ? C18 Si3 Si1 121.05(18) . . ? C19 Si3 Si1 110.34(16) . . ? C17 Si3 Si1 110.24(17) . . ? C1 O1 C12 111.6(3) . . ? C1 O1 K1 108.4(2) . . ? C12 O1 K1 111.1(2) . . ? C2 O2 C3 113.4(3) . . ? C2 O2 K1 118.1(2) . . ? C3 O2 K1 119.7(2) . . ? C4 O3 C5 112.3(3) . . ? C4 O3 K1 107.2(2) . . ? C5 O3 K1 111.7(2) . . ? C7 O4 C6 112.7(3) . . ? C7 O4 K1 117.8(2) . . ? C6 O4 K1 115.9(2) . . ? C8 O5 C9 114.2(3) . . ? C8 O5 K1 107.6(2) . . ? C9 O5 K1 108.8(2) . . ? C10 O6 C11 112.6(3) . . ? C10 O6 K1 117.9(2) . . ? C11 O6 K1 113.5(2) . . ? C13 O7 Si1 124.3(3) . . ? C13 O7 K1 126.9(2) . . ? Si1 O7 K1 108.82(13) . . ? O1 C1 C2 109.2(4) . . ? O2 C2 C1 108.9(3) . . ? O2 C3 C4 109.5(3) . . ? O3 C4 C3 108.4(3) . . ? O3 C5 C6 109.2(3) . . ? O4 C6 C5 108.1(3) . . ? O4 C7 C8 108.6(3) . . ? O5 C8 C7 108.0(3) . . ? O5 C9 C10 107.7(3) . . ? O6 C10 C9 108.8(3) . . ? O6 C11 C12 109.1(4) . . ? O1 C12 C11 109.3(4) . . ? Si2 C16 K1 162.8(3) . 8_665 ? 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 O2 K1 Si1 O7 -113.74(16) . . . . ? O4 K1 Si1 O7 4.08(16) . . . . ? O6 K1 Si1 O7 125.00(16) . . . . ? O1 K1 Si1 O7 -174.01(16) . . . . ? O3 K1 Si1 O7 -60.22(16) . . . . ? O5 K1 Si1 O7 68.64(16) . . . . ? C16 K1 Si1 O7 163.2(4) 8_655 . . . ? O7 K1 Si1 Si2 -65.26(16) . . . . ? O2 K1 Si1 Si2 -178.99(9) . . . . ? O4 K1 Si1 Si2 -61.17(9) . . . . ? O6 K1 Si1 Si2 59.75(9) . . . . ? O1 K1 Si1 Si2 120.73(8) . . . . ? O3 K1 Si1 Si2 -125.47(8) . . . . ? O5 K1 Si1 Si2 3.39(9) . . . . ? C16 K1 Si1 Si2 98.0(4) 8_655 . . . ? O7 K1 Si1 Si3 76.54(16) . . . . ? O2 K1 Si1 Si3 -37.20(8) . . . . ? O4 K1 Si1 Si3 80.62(8) . . . . ? O6 K1 Si1 Si3 -158.46(8) . . . . ? O1 K1 Si1 Si3 -97.47(8) . . . . ? O3 K1 Si1 Si3 16.32(9) . . . . ? O5 K1 Si1 Si3 145.18(8) . . . . ? C16 K1 Si1 Si3 -120.2(3) 8_655 . . . ? O7 Si1 Si2 C15 -169.4(2) . . . . ? Si3 Si1 Si2 C15 82.39(18) . . . . ? K1 Si1 Si2 C15 -129.38(18) . . . . ? O7 Si1 Si2 C14 -54.7(2) . . . . ? Si3 Si1 Si2 C14 -162.90(18) . . . . ? K1 Si1 Si2 C14 -14.66(19) . . . . ? O7 Si1 Si2 C16 66.7(2) . . . . ? Si3 Si1 Si2 C16 -41.5(2) . . . . ? K1 Si1 Si2 C16 106.8(2) . . . . ? O7 Si1 Si3 C18 -40.0(2) . . . . ? Si2 Si1 Si3 C18 66.9(2) . . . . ? K1 Si1 Si3 C18 -84.0(2) . . . . ? O7 Si1 Si3 C19 80.2(2) . . . . ? Si2 Si1 Si3 C19 -172.89(17) . . . . ? K1 Si1 Si3 C19 36.27(18) . . . . ? O7 Si1 Si3 C17 -162.8(2) . . . . ? Si2 Si1 Si3 C17 -55.87(19) . . . . ? K1 Si1 Si3 C17 153.29(18) . . . . ? O7 K1 O1 C1 49.4(3) . . . . ? O2 K1 O1 C1 -28.8(2) . . . . ? O4 K1 O1 C1 -122.7(3) . . . . ? O6 K1 O1 C1 142.7(3) . . . . ? O3 K1 O1 C1 -56.9(3) . . . . ? O5 K1 O1 C1 164.7(2) . . . . ? C16 K1 O1 C1 -133.6(3) 8_655 . . . ? Si1 K1 O1 C1 52.5(2) . . . . ? O7 K1 O1 C12 -73.5(3) . . . . ? O2 K1 O1 C12 -151.7(3) . . . . ? O4 K1 O1 C12 114.3(3) . . . . ? O6 K1 O1 C12 19.8(3) . . . . ? O3 K1 O1 C12 -179.8(3) . . . . ? O5 K1 O1 C12 41.7(3) . . . . ? C16 K1 O1 C12 103.5(3) 8_655 . . . ? Si1 K1 O1 C12 -70.4(3) . . . . ? O7 K1 O2 C2 -122.3(3) . . . . ? O4 K1 O2 C2 150.8(3) . . . . ? O6 K1 O2 C2 -13.1(3) . . . . ? O1 K1 O2 C2 -4.5(3) . . . . ? O3 K1 O2 C2 145.3(3) . . . . ? O5 K1 O2 C2 72.5(5) . . . . ? C16 K1 O2 C2 67.4(3) 8_655 . . . ? Si1 K1 O2 C2 -97.1(3) . . . . ? O7 K1 O2 C3 92.4(3) . . . . ? O4 K1 O2 C3 5.4(3) . . . . ? O6 K1 O2 C3 -158.5(3) . . . . ? O1 K1 O2 C3 -149.8(3) . . . . ? O3 K1 O2 C3 -0.1(3) . . . . ? O5 K1 O2 C3 -72.9(5) . . . . ? C16 K1 O2 C3 -78.0(3) 8_655 . . . ? Si1 K1 O2 C3 117.5(3) . . . . ? O7 K1 O3 C4 -59.0(2) . . . . ? O2 K1 O3 C4 32.4(2) . . . . ? O4 K1 O3 C4 -142.1(3) . . . . ? O6 K1 O3 C4 128.2(3) . . . . ? O1 K1 O3 C4 60.8(2) . . . . ? O5 K1 O3 C4 -160.9(2) . . . . ? C16 K1 O3 C4 134.1(3) 8_655 . . . ? Si1 K1 O3 C4 -35.2(2) . . . . ? O7 K1 O3 C5 64.5(2) . . . . ? O2 K1 O3 C5 155.8(3) . . . . ? O4 K1 O3 C5 -18.6(2) . . . . ? O6 K1 O3 C5 -108.4(3) . . . . ? O1 K1 O3 C5 -175.8(2) . . . . ? O5 K1 O3 C5 -37.4(3) . . . . ? C16 K1 O3 C5 -102.4(3) 8_655 . . . ? Si1 K1 O3 C5 88.3(2) . . . . ? O7 K1 O4 C7 108.6(3) . . . . ? O2 K1 O4 C7 -160.2(3) . . . . ? O6 K1 O4 C7 4.0(3) . . . . ? O1 K1 O4 C7 -78.5(3) . . . . ? O3 K1 O4 C7 -154.8(3) . . . . ? O5 K1 O4 C7 5.7(2) . . . . ? C16 K1 O4 C7 -67.8(3) 8_655 . . . ? Si1 K1 O4 C7 106.7(3) . . . . ? O7 K1 O4 C6 -113.7(3) . . . . ? O2 K1 O4 C6 -22.5(3) . . . . ? O6 K1 O4 C6 141.8(2) . . . . ? O1 K1 O4 C6 59.2(4) . . . . ? O3 K1 O4 C6 -17.0(2) . . . . ? O5 K1 O4 C6 143.4(3) . . . . ? C16 K1 O4 C6 70.0(3) 8_655 . . . ? Si1 K1 O4 C6 -115.6(2) . . . . ? O7 K1 O5 C8 -50.6(2) . . . . ? O2 K1 O5 C8 114.6(4) . . . . ? O4 K1 O5 C8 29.2(2) . . . . ? O6 K1 O5 C8 -152.5(2) . . . . ? O1 K1 O5 C8 -174.8(2) . . . . ? O3 K1 O5 C8 48.1(2) . . . . ? C16 K1 O5 C8 119.9(2) 8_655 . . . ? Si1 K1 O5 C8 -76.5(2) . . . . ? O7 K1 O5 C9 73.6(2) . . . . ? O2 K1 O5 C9 -121.2(4) . . . . ? O4 K1 O5 C9 153.4(3) . . . . ? O6 K1 O5 C9 -28.3(2) . . . . ? O1 K1 O5 C9 -50.6(2) . . . . ? O3 K1 O5 C9 172.2(2) . . . . ? C16 K1 O5 C9 -115.9(3) 8_655 . . . ? Si1 K1 O5 C9 47.7(2) . . . . ? O7 K1 O6 C10 -98.5(3) . . . . ? O2 K1 O6 C10 158.8(2) . . . . ? O4 K1 O6 C10 -5.1(3) . . . . ? O1 K1 O6 C10 150.2(3) . . . . ? O3 K1 O6 C10 74.1(4) . . . . ? O5 K1 O6 C10 -6.8(2) . . . . ? C16 K1 O6 C10 68.1(3) 8_655 . . . ? Si1 K1 O6 C10 -121.6(3) . . . . ? O7 K1 O6 C11 126.8(2) . . . . ? O2 K1 O6 C11 24.1(3) . . . . ? O4 K1 O6 C11 -139.9(2) . . . . ? O1 K1 O6 C11 15.5(2) . . . . ? O3 K1 O6 C11 -60.6(4) . . . . ? O5 K1 O6 C11 -141.5(3) . . . . ? C16 K1 O6 C11 -66.6(3) 8_655 . . . ? Si1 K1 O6 C11 103.6(2) . . . . ? Si2 Si1 O7 C13 -45.9(4) . . . . ? Si3 Si1 O7 C13 58.3(4) . . . . ? K1 Si1 O7 C13 -179.4(4) . . . . ? Si2 Si1 O7 K1 133.52(10) . . . . ? Si3 Si1 O7 K1 -122.34(10) . . . . ? O2 K1 O7 C13 -115.6(4) . . . . ? O4 K1 O7 C13 3.1(4) . . . . ? O6 K1 O7 C13 121.5(4) . . . . ? O1 K1 O7 C13 -174.0(4) . . . . ? O3 K1 O7 C13 -56.2(4) . . . . ? O5 K1 O7 C13 61.2(4) . . . . ? C16 K1 O7 C13 18.7(7) 8_655 . . . ? Si1 K1 O7 C13 179.4(5) . . . . ? O2 K1 O7 Si1 65.02(15) . . . . ? O4 K1 O7 Si1 -176.25(15) . . . . ? O6 K1 O7 Si1 -57.88(16) . . . . ? O1 K1 O7 Si1 6.63(18) . . . . ? O3 K1 O7 Si1 124.46(14) . . . . ? O5 K1 O7 Si1 -118.14(14) . . . . ? C16 K1 O7 Si1 -160.6(4) 8_655 . . . ? C12 O1 C1 C2 -177.0(4) . . . . ? K1 O1 C1 C2 60.4(4) . . . . ? C3 O2 C2 C1 -176.9(3) . . . . ? K1 O2 C2 C1 35.6(4) . . . . ? O1 C1 C2 O2 -65.6(5) . . . . ? C2 O2 C3 C4 -177.6(3) . . . . ? K1 O2 C3 C4 -30.7(4) . . . . ? C5 O3 C4 C3 174.1(3) . . . . ? K1 O3 C4 C3 -62.8(3) . . . . ? O2 C3 C4 O3 64.2(4) . . . . ? C4 O3 C5 C6 172.0(3) . . . . ? K1 O3 C5 C6 51.4(4) . . . . ? C7 O4 C6 C5 -170.5(3) . . . . ? K1 O4 C6 C5 49.7(4) . . . . ? O3 C5 C6 O4 -68.4(4) . . . . ? C6 O4 C7 C8 -177.6(3) . . . . ? K1 O4 C7 C8 -38.6(4) . . . . ? C9 O5 C8 C7 176.9(3) . . . . ? K1 O5 C8 C7 -62.3(3) . . . . ? O4 C7 C8 O5 69.3(4) . . . . ? C8 O5 C9 C10 -179.0(3) . . . . ? K1 O5 C9 C10 60.9(3) . . . . ? C11 O6 C10 C9 174.7(3) . . . . ? K1 O6 C10 C9 39.6(4) . . . . ? O5 C9 C10 O6 -68.5(4) . . . . ? C10 O6 C11 C12 174.4(3) . . . . ? K1 O6 C11 C12 -48.4(4) . . . . ? C1 O1 C12 C11 -174.0(4) . . . . ? K1 O1 C12 C11 -52.9(4) . . . . ? O6 C11 C12 O1 69.8(5) . . . . ? C15 Si2 C16 K1 142.4(8) . . . 8_665 ? C14 Si2 C16 K1 31.5(9) . . . 8_665 ? Si1 Si2 C16 K1 -91.5(8) . . . 8_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.505 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.085 #===END data_150j _database_code_depnum_ccdc_archive 'CCDC 232701' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H39 K O Si6' _chemical_formula_weight 419.08 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.835(2) _cell_length_b 17.659(4) _cell_length_c 14.158(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.94(3) _cell_angle_gamma 90.00 _cell_volume 2562.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour 'slight yellow' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.486 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details XPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17598 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 24.71 _reflns_number_total 4368 _reflns_number_gt 3578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (1998)' _computing_cell_refinement 'Bruker SAINT (1998)' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.2389P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4368 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 K1 K 0.39225(8) 0.09564(4) 0.43562(6) 0.0369(2) Uani 1 1 d . . . O1 O 0.3302(2) 0.14420(13) 0.58640(16) 0.0332(6) Uani 1 1 d . . . Si1 Si 0.71144(9) 0.19429(5) 0.66226(7) 0.0284(2) Uani 1 1 d . . . Si2 Si 0.61604(9) 0.07833(5) 0.67779(7) 0.0246(2) Uani 1 1 d . . . Si3 Si 0.41599(9) 0.10731(5) 0.70084(7) 0.0249(2) Uani 1 1 d . . . Si4 Si 0.29892(9) -0.00442(5) 0.70938(7) 0.0301(2) Uani 1 1 d . . . Si5 Si 0.39097(9) 0.18838(5) 0.82614(7) 0.0313(3) Uani 1 1 d . . . Si6 Si 0.76231(9) 0.02444(5) 0.82207(7) 0.0288(2) Uani 1 1 d . . . C1 C 0.5906(4) 0.2542(2) 0.5657(3) 0.0444(10) Uani 1 1 d . . . H1A H 0.6301 0.3018 0.5594 0.067 Uiso 1 1 calc R . . H1B H 0.5153 0.2630 0.5859 0.067 Uiso 1 1 calc R . . H1C H 0.5647 0.2284 0.5026 0.067 Uiso 1 1 calc R . . C2 C 0.8545(3) 0.1786(2) 0.6172(3) 0.0457(10) Uani 1 1 d . . . H2A H 0.8267 0.1508 0.5557 0.069 Uiso 1 1 calc R . . H2B H 0.9205 0.1504 0.6664 0.069 Uiso 1 1 calc R . . H2C H 0.8894 0.2266 0.6066 0.069 Uiso 1 1 calc R . . C3 C 0.7793(5) 0.2578(3) 0.7753(3) 0.0443(11) Uani 1 1 d . . . C4 C 0.2228(5) 0.1947(3) 0.5706(4) 0.0545(13) Uani 1 1 d . . . C5 C 0.3652(5) -0.0872(2) 0.6582(4) 0.0439(10) Uani 1 1 d . . . C6 C 0.1257(3) 0.0088(2) 0.6257(3) 0.0478(10) Uani 1 1 d . . . H6A H 0.0770 -0.0366 0.6255 0.072 Uiso 1 1 calc R . . H6B H 0.1249 0.0196 0.5590 0.072 Uiso 1 1 calc R . . H6C H 0.0869 0.0502 0.6498 0.072 Uiso 1 1 calc R . . C7 C 0.2967(4) -0.0305(2) 0.8369(3) 0.0443(10) Uani 1 1 d . . . H7A H 0.2497 -0.0771 0.8333 0.066 Uiso 1 1 calc R . . H7B H 0.2548 0.0089 0.8619 0.066 Uiso 1 1 calc R . . H7C H 0.3846 -0.0368 0.8808 0.066 Uiso 1 1 calc R . . C8 C 0.2201(4) 0.1891(2) 0.8330(3) 0.0489(11) Uani 1 1 d . . . H8A H 0.2192 0.2160 0.8917 0.073 Uiso 1 1 calc R . . H8B H 0.1915 0.1379 0.8360 0.073 Uiso 1 1 calc R . . H8C H 0.1626 0.2136 0.7748 0.073 Uiso 1 1 calc R . . C9 C 0.5008(4) 0.1512(2) 0.9482(3) 0.0427(10) Uani 1 1 d . . . H9A H 0.5895 0.1524 0.9487 0.064 Uiso 1 1 calc R . . H9B H 0.4768 0.1000 0.9571 0.064 Uiso 1 1 calc R . . H9C H 0.4923 0.1821 1.0016 0.064 Uiso 1 1 calc R . . C10 C 0.4342(4) 0.2888(2) 0.8118(3) 0.0501(11) Uani 1 1 d . . . H10A H 0.4370 0.3168 0.8707 0.075 Uiso 1 1 calc R . . H10B H 0.3698 0.3106 0.7548 0.075 Uiso 1 1 calc R . . H10C H 0.5181 0.2909 0.8027 0.075 Uiso 1 1 calc R . . C11 C 0.6849(4) -0.0432(2) 0.8878(3) 0.0426(10) Uani 1 1 d . . . H11A H 0.7510 -0.0656 0.9432 0.064 Uiso 1 1 calc R . . H11B H 0.6402 -0.0822 0.8423 0.064 Uiso 1 1 calc R . . H11C H 0.6236 -0.0165 0.9116 0.064 Uiso 1 1 calc R . . C12 C 0.8629(4) 0.0900(2) 0.9221(3) 0.0597(13) Uani 1 1 d . . . H12A H 0.8064 0.1248 0.9404 0.090 Uiso 1 1 calc R . . H12B H 0.9224 0.1177 0.8975 0.090 Uiso 1 1 calc R . . H12C H 0.9112 0.0610 0.9796 0.090 Uiso 1 1 calc R . . C13 C 0.8863(4) -0.0313(2) 0.7835(3) 0.0494(11) Uani 1 1 d . . . H13A H 0.9514 -0.0509 0.8418 0.074 Uiso 1 1 calc R . . H13B H 0.9270 0.0012 0.7478 0.074 Uiso 1 1 calc R . . H13C H 0.8437 -0.0724 0.7411 0.074 Uiso 1 1 calc R . . H3 H 0.805(4) 0.299(2) 0.753(3) 0.059(14) Uiso 1 1 d . . . H1 H 0.727(5) 0.270(3) 0.822(3) 0.087(16) Uiso 1 1 d . . . H2 H 0.858(5) 0.240(3) 0.814(4) 0.091(19) Uiso 1 1 d . . . H5 H 0.460(4) -0.0982(18) 0.694(2) 0.036(10) Uiso 1 1 d . . . H6 H 0.356(3) -0.0800(18) 0.584(3) 0.032(9) Uiso 1 1 d . . . H4 H 0.309(4) -0.124(2) 0.655(3) 0.070(14) Uiso 1 1 d . . . H9 H 0.158(4) 0.176(2) 0.595(3) 0.061(14) Uiso 1 1 d . . . H8 H 0.187(6) 0.205(3) 0.501(5) 0.13(2) Uiso 1 1 d . . . H7 H 0.258(6) 0.246(4) 0.609(4) 0.13(2) 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 0.0452(5) 0.0364(5) 0.0280(4) -0.0010(4) 0.0106(4) 0.0076(4) O1 0.0304(13) 0.0392(14) 0.0284(13) 0.0058(11) 0.0071(11) 0.0100(11) Si1 0.0268(5) 0.0277(5) 0.0292(5) 0.0021(4) 0.0072(4) -0.0016(4) Si2 0.0232(5) 0.0248(5) 0.0244(5) 0.0000(4) 0.0060(4) 0.0004(4) Si3 0.0244(5) 0.0269(5) 0.0228(5) 0.0012(4) 0.0070(4) 0.0017(4) Si4 0.0269(5) 0.0329(6) 0.0307(6) -0.0016(4) 0.0097(4) -0.0034(4) Si5 0.0324(6) 0.0301(5) 0.0323(6) -0.0037(4) 0.0116(5) 0.0026(4) Si6 0.0262(5) 0.0288(5) 0.0279(5) 0.0031(4) 0.0041(4) 0.0025(4) C1 0.043(2) 0.032(2) 0.053(3) 0.0160(19) 0.008(2) -0.0021(18) C2 0.035(2) 0.050(2) 0.056(3) 0.000(2) 0.021(2) -0.0079(19) C3 0.055(3) 0.031(2) 0.044(3) -0.005(2) 0.011(2) -0.009(2) C4 0.044(3) 0.075(4) 0.041(3) 0.017(3) 0.009(2) 0.031(3) C5 0.043(3) 0.038(2) 0.055(3) -0.011(2) 0.021(2) -0.011(2) C6 0.032(2) 0.055(3) 0.051(3) 0.000(2) 0.0062(19) -0.0084(19) C7 0.053(3) 0.047(2) 0.035(2) 0.0003(19) 0.018(2) -0.014(2) C8 0.047(2) 0.050(2) 0.054(3) -0.014(2) 0.021(2) 0.003(2) C9 0.051(2) 0.044(2) 0.031(2) -0.0076(18) 0.0104(19) -0.0001(19) C10 0.049(2) 0.038(2) 0.066(3) -0.003(2) 0.022(2) 0.0045(19) C11 0.045(2) 0.044(2) 0.040(2) 0.0111(19) 0.0146(19) 0.0063(19) C12 0.057(3) 0.047(3) 0.049(3) 0.001(2) -0.018(2) 0.001(2) C13 0.038(2) 0.056(3) 0.053(3) 0.011(2) 0.014(2) 0.016(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 K1 O1 2.584(2) . ? K1 C5 3.310(5) 3_656 ? K1 C3 3.398(4) 4_565 ? K1 Si2 3.4541(13) 3_656 ? K1 Si2 3.5117(17) . ? K1 C4 3.515(5) . ? K1 Si3 3.6853(14) . ? K1 K1 4.1741(17) 3_656 ? O1 C4 1.424(5) . ? O1 Si3 1.714(2) . ? Si1 C2 1.878(4) . ? Si1 C1 1.882(4) . ? Si1 C3 1.896(4) . ? Si1 Si2 2.3361(13) . ? Si2 Si6 2.3428(15) . ? Si2 Si3 2.3507(13) . ? Si2 K1 3.4541(13) 3_656 ? Si3 Si5 2.3627(14) . ? Si3 Si4 2.3699(13) . ? Si4 C7 1.871(3) . ? Si4 C5 1.876(4) . ? Si4 C6 1.881(4) . ? Si5 C10 1.862(4) . ? Si5 C9 1.871(4) . ? Si5 C8 1.885(4) . ? Si6 C11 1.871(4) . ? Si6 C12 1.879(4) . ? Si6 C13 1.884(4) . ? C3 K1 3.398(4) 4_666 ? C5 K1 3.310(5) 3_656 ? 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 O1 K1 C5 143.11(10) . 3_656 ? O1 K1 C3 99.52(10) . 4_565 ? C5 K1 C3 85.80(13) 3_656 4_565 ? O1 K1 Si2 134.81(6) . 3_656 ? C5 K1 Si2 71.20(8) 3_656 3_656 ? C3 K1 Si2 114.67(9) 4_565 3_656 ? O1 K1 Si2 60.31(5) . . ? C5 K1 Si2 90.08(9) 3_656 . ? C3 K1 Si2 134.71(9) 4_565 . ? Si2 K1 Si2 106.38(3) 3_656 . ? O1 K1 C4 20.60(9) . . ? C5 K1 C4 149.67(13) 3_656 . ? C3 K1 C4 81.14(12) 4_565 . ? Si2 K1 C4 139.09(11) 3_656 . ? Si2 K1 C4 80.18(8) . . ? O1 K1 Si3 24.56(5) . . ? C5 K1 Si3 127.54(9) 3_656 . ? C3 K1 Si3 121.95(9) 4_565 . ? Si2 K1 Si3 120.40(3) 3_656 . ? Si2 K1 Si3 38.03(2) . . ? C4 K1 Si3 45.12(8) . . ? O1 K1 K1 99.58(6) . 3_656 ? C5 K1 K1 74.60(9) 3_656 3_656 ? C3 K1 K1 159.60(9) 4_565 3_656 ? Si2 K1 K1 53.82(3) 3_656 3_656 ? Si2 K1 K1 52.55(2) . 3_656 ? C4 K1 K1 118.81(8) . 3_656 ? Si3 K1 K1 75.88(3) . 3_656 ? C4 O1 Si3 123.5(3) . . ? C4 O1 K1 119.7(2) . . ? Si3 O1 K1 116.62(11) . . ? C2 Si1 C1 107.04(18) . . ? C2 Si1 C3 103.7(2) . . ? C1 Si1 C3 105.6(2) . . ? C2 Si1 Si2 109.98(13) . . ? C1 Si1 Si2 109.66(12) . . ? C3 Si1 Si2 120.10(16) . . ? Si1 Si2 Si6 104.08(5) . . ? Si1 Si2 Si3 106.16(5) . . ? Si6 Si2 Si3 111.15(5) . . ? Si1 Si2 K1 132.95(5) . 3_656 ? Si6 Si2 K1 87.26(4) . 3_656 ? Si3 Si2 K1 111.85(4) . 3_656 ? Si1 Si2 K1 91.04(4) . . ? Si6 Si2 K1 160.74(5) . . ? Si3 Si2 K1 74.99(4) . . ? K1 Si2 K1 73.62(3) 3_656 . ? O1 Si3 Si2 101.15(9) . . ? O1 Si3 Si5 108.68(9) . . ? Si2 Si3 Si5 124.88(5) . . ? O1 Si3 Si4 103.27(9) . . ? Si2 Si3 Si4 111.02(5) . . ? Si5 Si3 Si4 105.81(5) . . ? O1 Si3 K1 38.82(8) . . ? Si2 Si3 K1 66.98(4) . . ? Si5 Si3 K1 144.28(4) . . ? Si4 Si3 K1 98.27(4) . . ? C7 Si4 C5 107.9(2) . . ? C7 Si4 C6 108.42(18) . . ? C5 Si4 C6 106.4(2) . . ? C7 Si4 Si3 115.41(13) . . ? C5 Si4 Si3 110.54(15) . . ? C6 Si4 Si3 107.80(13) . . ? C10 Si5 C9 109.14(19) . . ? C10 Si5 C8 106.58(18) . . ? C9 Si5 C8 107.18(18) . . ? C10 Si5 Si3 113.66(14) . . ? C9 Si5 Si3 106.71(12) . . ? C8 Si5 Si3 113.35(13) . . ? C11 Si6 C12 105.2(2) . . ? C11 Si6 C13 106.74(18) . . ? C12 Si6 C13 104.3(2) . . ? C11 Si6 Si2 114.02(13) . . ? C12 Si6 Si2 118.01(13) . . ? C13 Si6 Si2 107.66(13) . . ? Si1 C3 K1 166.2(2) . 4_666 ? O1 C4 K1 39.67(18) . . ? Si4 C5 K1 130.1(2) . 3_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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 K1 O1 C4 122.8(3) 3_656 . . . ? C3 K1 O1 C4 27.1(3) 4_565 . . . ? Si2 K1 O1 C4 -112.6(3) 3_656 . . . ? Si2 K1 O1 C4 163.6(3) . . . . ? Si3 K1 O1 C4 -175.4(4) . . . . ? K1 K1 O1 C4 -160.1(3) 3_656 . . . ? C5 K1 O1 Si3 -61.8(2) 3_656 . . . ? C3 K1 O1 Si3 -157.48(14) 4_565 . . . ? Si2 K1 O1 Si3 62.77(15) 3_656 . . . ? Si2 K1 O1 Si3 -20.97(9) . . . . ? C4 K1 O1 Si3 175.4(4) . . . . ? K1 K1 O1 Si3 15.32(13) 3_656 . . . ? C2 Si1 Si2 Si6 74.31(14) . . . . ? C1 Si1 Si2 Si6 -168.24(14) . . . . ? C3 Si1 Si2 Si6 -45.8(2) . . . . ? C2 Si1 Si2 Si3 -168.31(14) . . . . ? C1 Si1 Si2 Si3 -50.86(15) . . . . ? C3 Si1 Si2 Si3 71.6(2) . . . . ? C2 Si1 Si2 K1 -25.25(15) . . . 3_656 ? C1 Si1 Si2 K1 92.19(15) . . . 3_656 ? C3 Si1 Si2 K1 -145.38(19) . . . 3_656 ? C2 Si1 Si2 K1 -93.64(14) . . . . ? C1 Si1 Si2 K1 23.80(15) . . . . ? C3 Si1 Si2 K1 146.23(19) . . . . ? O1 K1 Si2 Si1 -92.49(7) . . . . ? C5 K1 Si2 Si1 64.43(8) 3_656 . . . ? C3 K1 Si2 Si1 -19.73(14) 4_565 . . . ? Si2 K1 Si2 Si1 134.83(4) 3_656 . . . ? C4 K1 Si2 Si1 -86.70(11) . . . . ? Si3 K1 Si2 Si1 -106.46(5) . . . . ? K1 K1 Si2 Si1 134.83(4) 3_656 . . . ? O1 K1 Si2 Si6 125.36(15) . . . . ? C5 K1 Si2 Si6 -77.73(15) 3_656 . . . ? C3 K1 Si2 Si6 -161.88(17) 4_565 . . . ? Si2 K1 Si2 Si6 -7.32(13) 3_656 . . . ? C4 K1 Si2 Si6 131.14(17) . . . . ? Si3 K1 Si2 Si6 111.39(14) . . . . ? K1 K1 Si2 Si6 -7.32(13) 3_656 . . . ? O1 K1 Si2 Si3 13.97(7) . . . . ? C5 K1 Si2 Si3 170.89(8) 3_656 . . . ? C3 K1 Si2 Si3 86.73(13) 4_565 . . . ? Si2 K1 Si2 Si3 -118.71(4) 3_656 . . . ? C4 K1 Si2 Si3 19.76(11) . . . . ? K1 K1 Si2 Si3 -118.71(4) 3_656 . . . ? O1 K1 Si2 K1 132.68(7) . . . 3_656 ? C5 K1 Si2 K1 -70.40(8) 3_656 . . 3_656 ? C3 K1 Si2 K1 -154.56(14) 4_565 . . 3_656 ? Si2 K1 Si2 K1 0.0 3_656 . . 3_656 ? C4 K1 Si2 K1 138.47(11) . . . 3_656 ? Si3 K1 Si2 K1 118.71(4) . . . 3_656 ? C4 O1 Si3 Si2 -156.5(3) . . . . ? K1 O1 Si3 Si2 28.26(12) . . . . ? C4 O1 Si3 Si5 -23.5(4) . . . . ? K1 O1 Si3 Si5 161.25(8) . . . . ? C4 O1 Si3 Si4 88.5(3) . . . . ? K1 O1 Si3 Si4 -86.71(11) . . . . ? C4 O1 Si3 K1 175.2(4) . . . . ? Si1 Si2 Si3 O1 67.86(10) . . . . ? Si6 Si2 Si3 O1 -179.58(9) . . . . ? K1 Si2 Si3 O1 -83.85(9) 3_656 . . . ? K1 Si2 Si3 O1 -18.81(9) . . . . ? Si1 Si2 Si3 Si5 -54.50(7) . . . . ? Si6 Si2 Si3 Si5 58.06(8) . . . . ? K1 Si2 Si3 Si5 153.79(5) 3_656 . . . ? K1 Si2 Si3 Si5 -141.17(6) . . . . ? Si1 Si2 Si3 Si4 176.91(5) . . . . ? Si6 Si2 Si3 Si4 -70.53(6) . . . . ? K1 Si2 Si3 Si4 25.20(6) 3_656 . . . ? K1 Si2 Si3 Si4 90.24(5) . . . . ? Si1 Si2 Si3 K1 86.67(4) . . . . ? Si6 Si2 Si3 K1 -160.77(5) . . . . ? K1 Si2 Si3 K1 -65.04(4) 3_656 . . . ? C5 K1 Si3 O1 138.17(16) 3_656 . . . ? C3 K1 Si3 O1 26.44(17) 4_565 . . . ? Si2 K1 Si3 O1 -132.99(13) 3_656 . . . ? Si2 K1 Si3 O1 149.69(14) . . . . ? C4 K1 Si3 O1 -2.27(19) . . . . ? K1 K1 Si3 O1 -164.42(13) 3_656 . . . ? O1 K1 Si3 Si2 -149.69(14) . . . . ? C5 K1 Si3 Si2 -11.52(10) 3_656 . . . ? C3 K1 Si3 Si2 -123.25(11) 4_565 . . . ? Si2 K1 Si3 Si2 77.32(4) 3_656 . . . ? C4 K1 Si3 Si2 -151.96(15) . . . . ? K1 K1 Si3 Si2 45.89(3) 3_656 . . . ? O1 K1 Si3 Si5 -31.44(14) . . . . ? C5 K1 Si3 Si5 106.73(12) 3_656 . . . ? C3 K1 Si3 Si5 -5.00(14) 4_565 . . . ? Si2 K1 Si3 Si5 -164.43(7) 3_656 . . . ? Si2 K1 Si3 Si5 118.25(8) . . . . ? C4 K1 Si3 Si5 -33.71(16) . . . . ? K1 K1 Si3 Si5 164.14(7) 3_656 . . . ? O1 K1 Si3 Si4 100.91(13) . . . . ? C5 K1 Si3 Si4 -120.92(10) 3_656 . . . ? C3 K1 Si3 Si4 127.35(11) 4_565 . . . ? Si2 K1 Si3 Si4 -32.08(5) 3_656 . . . ? Si2 K1 Si3 Si4 -109.40(5) . . . . ? C4 K1 Si3 Si4 98.64(15) . . . . ? K1 K1 Si3 Si4 -63.51(4) 3_656 . . . ? O1 Si3 Si4 C7 -146.69(17) . . . . ? Si2 Si3 Si4 C7 105.65(15) . . . . ? Si5 Si3 Si4 C7 -32.56(15) . . . . ? K1 Si3 Si4 C7 174.09(15) . . . . ? O1 Si3 Si4 C5 90.56(19) . . . . ? Si2 Si3 Si4 C5 -17.10(18) . . . . ? Si5 Si3 Si4 C5 -155.31(17) . . . . ? K1 Si3 Si4 C5 51.34(17) . . . . ? O1 Si3 Si4 C6 -25.36(16) . . . . ? Si2 Si3 Si4 C6 -133.03(14) . . . . ? Si5 Si3 Si4 C6 88.77(14) . . . . ? K1 Si3 Si4 C6 -64.59(14) . . . . ? O1 Si3 Si5 C10 -53.59(17) . . . . ? Si2 Si3 Si5 C10 65.39(16) . . . . ? Si4 Si3 Si5 C10 -163.93(15) . . . . ? K1 Si3 Si5 C10 -33.40(17) . . . . ? O1 Si3 Si5 C9 -173.94(16) . . . . ? Si2 Si3 Si5 C9 -54.96(15) . . . . ? Si4 Si3 Si5 C9 75.72(14) . . . . ? K1 Si3 Si5 C9 -153.75(14) . . . . ? O1 Si3 Si5 C8 68.32(18) . . . . ? Si2 Si3 Si5 C8 -172.70(15) . . . . ? Si4 Si3 Si5 C8 -42.02(16) . . . . ? K1 Si3 Si5 C8 88.51(17) . . . . ? Si1 Si2 Si6 C11 153.16(14) . . . . ? Si3 Si2 Si6 C11 39.29(15) . . . . ? K1 Si2 Si6 C11 -73.10(14) 3_656 . . . ? K1 Si2 Si6 C11 -66.1(2) . . . . ? Si1 Si2 Si6 C12 28.95(19) . . . . ? Si3 Si2 Si6 C12 -84.92(18) . . . . ? K1 Si2 Si6 C12 162.69(18) 3_656 . . . ? K1 Si2 Si6 C12 169.7(2) . . . . ? Si1 Si2 Si6 C13 -88.62(15) . . . . ? Si3 Si2 Si6 C13 157.51(15) . . . . ? K1 Si2 Si6 C13 45.12(15) 3_656 . . . ? K1 Si2 Si6 C13 52.2(2) . . . . ? C2 Si1 C3 K1 77.9(11) . . . 4_666 ? C1 Si1 C3 K1 -34.5(11) . . . 4_666 ? Si2 Si1 C3 K1 -158.9(10) . . . 4_666 ? Si3 O1 C4 K1 -175.1(4) . . . . ? C5 K1 C4 O1 -87.4(4) 3_656 . . . ? C3 K1 C4 O1 -153.0(3) 4_565 . . . ? Si2 K1 C4 O1 89.3(3) 3_656 . . . ? Si2 K1 C4 O1 -14.4(3) . . . . ? Si3 K1 C4 O1 2.7(2) . . . . ? K1 K1 C4 O1 22.5(4) 3_656 . . . ? C7 Si4 C5 K1 -127.1(3) . . . 3_656 ? C6 Si4 C5 K1 116.8(3) . . . 3_656 ? Si3 Si4 C5 K1 0.0(3) . . . 3_656 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.514 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.076 #===END