Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Keith Izod' 'Lyndsey J. Bowman' W.Clegg 'Ross Harrington' _publ_contact_author_name 'Keith Izod ' _publ_contact_author_address ; Department of Chemistry University of Newcastle, Bedson Building Newcastle Upon Tyne NE1 7RU UNITED KINGDOM ; _publ_contact_author_email K.J.IZOD@NCL.AC.UK _publ_section_title ; Alkali Metal Complexes of Sterically Hindered Mono- and Di-Carbanions Containing Si-O Bonds ; data_ki205_compound5 _database_code_depnum_ccdc_archive 'CCDC 279576' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H58 K2 O2 Si6' _chemical_formula_sum 'C22 H58 K2 O2 Si6' _chemical_formula_weight 601.42 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 'C 2/c' 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' _cell_length_a 15.3506(7) _cell_length_b 11.8073(5) _cell_length_c 20.1478(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.5763(7) _cell_angle_gamma 90.00 _cell_volume 3610.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10926 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.69 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.825 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16058 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.94 _reflns_number_total 4477 _reflns_number_gt 3486 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR97 _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0673P)^2^+4.1663P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4477 _refine_ls_number_parameters 195 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1368 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _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 0.5000 0.19167(5) 0.7500 0.04393(19) Uani 1 2 d S . . K2 K 0.5000 0.5000 0.5000 0.0612(2) Uani 1 2 d S . . Si1 Si 0.40781(5) 0.28294(7) 0.58683(3) 0.0400(2) Uani 0.7907(13) 1 d P A 1 Si1A Si 0.4650(2) 0.2267(3) 0.56027(14) 0.0431(8) Uani 0.2093(13) 1 d P A 2 Si2 Si 0.61379(5) 0.26453(6) 0.59867(4) 0.03730(19) Uani 0.7907(13) 1 d P A 1 Si2A Si 0.63073(17) 0.3573(2) 0.63291(13) 0.0355(7) Uani 0.2093(13) 1 d P A 2 Si3 Si 0.53010(4) 0.45290(5) 0.67771(3) 0.02704(17) Uani 0.7907(13) 1 d P A 1 Si3A Si 0.44412(15) 0.4292(2) 0.65909(11) 0.0265(6) Uani 0.2093(13) 1 d P A 2 O1 O 0.5000 0.41223(18) 0.7500 0.0569(7) Uani 1 2 d S . . O2 O 0.5000 -0.0341(2) 0.7500 0.0658(8) Uani 1 2 d S . . C1 C 0.51560(12) 0.33884(16) 0.61714(9) 0.0296(4) Uani 1 1 d . A . C2 C 0.3178(2) 0.3646(6) 0.6237(2) 0.132(2) Uani 0.7907(13) 1 d PU A 1 H2A H 0.2600 0.3325 0.6064 0.197 Uiso 0.7907(13) 1 calc PR A 1 H2B H 0.3193 0.4445 0.6108 0.197 Uiso 0.7907(13) 1 calc PR A 1 H2C H 0.3283 0.3584 0.6728 0.197 Uiso 0.7907(13) 1 calc PR A 1 C2A C 0.3178(2) 0.3646(6) 0.6237(2) 0.132(2) Uani 0.2093(13) 1 d PU A 2 H2A1 H 0.2735 0.4077 0.6435 0.197 Uiso 0.2093(13) 1 calc PR A 2 H2A2 H 0.3151 0.2847 0.6365 0.197 Uiso 0.2093(13) 1 calc PR A 2 H2A3 H 0.3061 0.3712 0.5747 0.197 Uiso 0.2093(13) 1 calc PR A 2 C3 C 0.3901(3) 0.1267(3) 0.60529(19) 0.0965(13) Uani 0.7907(13) 1 d PU A 1 H3A H 0.3297 0.1050 0.5869 0.145 Uiso 0.7907(13) 1 calc PR A 1 H3B H 0.3998 0.1144 0.6539 0.145 Uiso 0.7907(13) 1 calc PR A 1 H3C H 0.4318 0.0806 0.5845 0.145 Uiso 0.7907(13) 1 calc PR A 1 C3A C 0.3901(3) 0.1267(3) 0.60529(19) 0.0965(13) Uani 0.2093(13) 1 d PU A 2 H3A1 H 0.3645 0.0681 0.5739 0.145 Uiso 0.2093(13) 1 calc PR A 2 H3A2 H 0.3429 0.1712 0.6204 0.145 Uiso 0.2093(13) 1 calc PR A 2 H3A3 H 0.4257 0.0910 0.6441 0.145 Uiso 0.2093(13) 1 calc PR A 2 C4 C 0.3774(2) 0.2862(3) 0.49137(13) 0.0825(11) Uani 0.7907(13) 1 d PU A 1 H4A H 0.3182 0.2548 0.4787 0.124 Uiso 0.7907(13) 1 calc PR A 1 H4B H 0.4199 0.2408 0.4710 0.124 Uiso 0.7907(13) 1 calc PR A 1 H4C H 0.3786 0.3645 0.4755 0.124 Uiso 0.7907(13) 1 calc PR A 1 C4A C 0.3774(2) 0.2862(3) 0.49137(13) 0.0825(11) Uani 0.2093(13) 1 d PU A 2 H4A1 H 0.3521 0.2243 0.4623 0.124 Uiso 0.2093(13) 1 calc PR A 2 H4A2 H 0.4045 0.3417 0.4647 0.124 Uiso 0.2093(13) 1 calc PR A 2 H4A3 H 0.3308 0.3228 0.5120 0.124 Uiso 0.2093(13) 1 calc PR A 2 C5 C 0.5851(3) 0.1424(3) 0.5360(2) 0.0992(13) Uani 0.7907(13) 1 d PU A 1 H5A H 0.6394 0.1051 0.5275 0.149 Uiso 0.7907(13) 1 calc PR A 1 H5B H 0.5537 0.1725 0.4937 0.149 Uiso 0.7907(13) 1 calc PR A 1 H5C H 0.5475 0.0875 0.5547 0.149 Uiso 0.7907(13) 1 calc PR A 1 C5A C 0.5851(3) 0.1424(3) 0.5360(2) 0.0992(13) Uani 0.2093(13) 1 d PU A 2 H5A1 H 0.5683 0.0791 0.5053 0.149 Uiso 0.2093(13) 1 calc PR A 2 H5A2 H 0.6199 0.1140 0.5773 0.149 Uiso 0.2093(13) 1 calc PR A 2 H5A3 H 0.6202 0.1969 0.5145 0.149 Uiso 0.2093(13) 1 calc PR A 2 C6 C 0.6855(2) 0.2065(3) 0.67517(18) 0.0828(11) Uani 0.7907(13) 1 d PU A 1 H6A H 0.7366 0.1682 0.6615 0.124 Uiso 0.7907(13) 1 calc PR A 1 H6B H 0.6516 0.1524 0.6979 0.124 Uiso 0.7907(13) 1 calc PR A 1 H6C H 0.7056 0.2688 0.7058 0.124 Uiso 0.7907(13) 1 calc PR A 1 C6A C 0.6855(2) 0.2065(3) 0.67517(18) 0.0828(11) Uani 0.2093(13) 1 d PU A 2 H6A1 H 0.7498 0.2140 0.6846 0.124 Uiso 0.2093(13) 1 calc PR A 2 H6A2 H 0.6700 0.1439 0.6436 0.124 Uiso 0.2093(13) 1 calc PR A 2 H6A3 H 0.6624 0.1910 0.7170 0.124 Uiso 0.2093(13) 1 calc PR A 2 C7 C 0.69168(18) 0.3581(3) 0.55749(15) 0.0625(7) Uani 0.7907(13) 1 d PU A 1 H7A H 0.7427 0.3135 0.5490 0.094 Uiso 0.7907(13) 1 calc PR A 1 H7B H 0.7116 0.4215 0.5874 0.094 Uiso 0.7907(13) 1 calc PR A 1 H7C H 0.6608 0.3875 0.5149 0.094 Uiso 0.7907(13) 1 calc PR A 1 C7A C 0.69168(18) 0.3581(3) 0.55749(15) 0.0625(7) Uani 0.2093(13) 1 d PU A 2 H7A1 H 0.7548 0.3687 0.5727 0.094 Uiso 0.2093(13) 1 calc PR A 2 H7A2 H 0.6696 0.4202 0.5273 0.094 Uiso 0.2093(13) 1 calc PR A 2 H7A3 H 0.6821 0.2859 0.5336 0.094 Uiso 0.2093(13) 1 calc PR A 2 C8 C 0.64693(18) 0.5105(2) 0.69237(13) 0.0586(7) Uani 0.7907(13) 1 d PU A 1 H8A H 0.6510 0.5718 0.7255 0.088 Uiso 0.7907(13) 1 calc PR A 1 H8B H 0.6622 0.5397 0.6500 0.088 Uiso 0.7907(13) 1 calc PR A 1 H8C H 0.6879 0.4497 0.7092 0.088 Uiso 0.7907(13) 1 calc PR A 1 C8A C 0.64693(18) 0.5105(2) 0.69237(13) 0.0586(7) Uani 0.2093(13) 1 d PU A 2 H8A1 H 0.7098 0.5278 0.7039 0.088 Uiso 0.2093(13) 1 calc PR A 2 H8A2 H 0.6212 0.4997 0.7336 0.088 Uiso 0.2093(13) 1 calc PR A 2 H8A3 H 0.6171 0.5734 0.6665 0.088 Uiso 0.2093(13) 1 calc PR A 2 C9 C 0.45754(18) 0.5824(2) 0.65174(13) 0.0523(6) Uani 0.7907(13) 1 d PU A 1 H9A H 0.4686 0.6407 0.6866 0.079 Uiso 0.7907(13) 1 calc PR A 1 H9B H 0.3954 0.5601 0.6461 0.079 Uiso 0.7907(13) 1 calc PR A 1 H9C H 0.4716 0.6126 0.6093 0.079 Uiso 0.7907(13) 1 calc PR A 1 C9A C 0.45754(18) 0.5824(2) 0.65174(13) 0.0523(6) Uani 0.2093(13) 1 d PU A 2 H9A1 H 0.4157 0.6214 0.6762 0.079 Uiso 0.2093(13) 1 calc PR A 2 H9A2 H 0.4463 0.6042 0.6043 0.079 Uiso 0.2093(13) 1 calc PR A 2 H9A3 H 0.5178 0.6037 0.6708 0.079 Uiso 0.2093(13) 1 calc PR A 2 C10 C 0.4218(3) -0.0997(3) 0.7472(3) 0.0811(16) Uani 0.876(9) 1 d PU B 1 H10A H 0.4270 -0.1674 0.7191 0.097 Uiso 0.876(9) 1 calc PR B 1 H10B H 0.3714 -0.0544 0.7251 0.097 Uiso 0.876(9) 1 calc PR B 1 C10A C 0.475(2) -0.106(4) 0.801(3) 0.128(12) Uani 0.124(9) 1 d PU B -2 H10C H 0.5036 -0.0828 0.8467 0.154 Uiso 0.124(9) 1 calc PR B -2 H10D H 0.4893 -0.1866 0.7938 0.154 Uiso 0.124(9) 1 calc PR B -2 C11 C 0.4031(4) -0.1366(4) 0.8136(4) 0.112(2) Uani 0.876(9) 1 d PU B 1 H11A H 0.3479 -0.1798 0.8081 0.169 Uiso 0.876(9) 1 calc PR B 1 H11B H 0.3975 -0.0701 0.8417 0.169 Uiso 0.876(9) 1 calc PR B 1 H11C H 0.4514 -0.1845 0.8350 0.169 Uiso 0.876(9) 1 calc PR B 1 C11A C 0.380(2) -0.086(4) 0.792(3) 0.114(13) Uani 0.124(9) 1 d PU B -2 H11D H 0.3496 -0.1506 0.7678 0.171 Uiso 0.124(9) 1 calc PR B -2 H11E H 0.3665 -0.0171 0.7655 0.171 Uiso 0.124(9) 1 calc PR B -2 H11F H 0.3603 -0.0779 0.8356 0.171 Uiso 0.124(9) 1 calc PR B -2 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 0.0694(5) 0.0268(3) 0.0364(3) 0.000 0.0106(3) 0.000 K2 0.0893(6) 0.0682(5) 0.0281(3) 0.0128(3) 0.0149(3) -0.0083(4) Si1 0.0363(4) 0.0592(5) 0.0247(3) -0.0098(3) 0.0052(3) -0.0135(3) Si1A 0.0515(17) 0.0489(16) 0.0313(13) -0.0166(12) 0.0136(12) -0.0174(13) Si2 0.0402(4) 0.0364(4) 0.0385(4) -0.0068(3) 0.0164(3) 0.0011(3) Si2A 0.0333(13) 0.0410(15) 0.0334(13) -0.0038(11) 0.0086(10) -0.0006(10) Si3 0.0373(4) 0.0265(3) 0.0190(3) 0.0009(2) 0.0095(2) -0.0005(2) Si3A 0.0302(12) 0.0301(12) 0.0192(10) 0.0004(8) 0.0040(8) -0.0003(9) O1 0.121(2) 0.0292(10) 0.0294(10) 0.000 0.0400(12) 0.000 O2 0.0678(17) 0.0294(11) 0.108(2) 0.000 0.0390(16) 0.000 C1 0.0333(9) 0.0347(9) 0.0222(8) -0.0047(7) 0.0084(7) -0.0040(7) C2 0.0314(15) 0.230(6) 0.136(4) -0.069(4) 0.0191(19) -0.011(2) C2A 0.0314(15) 0.230(6) 0.136(4) -0.069(4) 0.0191(19) -0.011(2) C3 0.103(3) 0.091(2) 0.087(2) 0.019(2) -0.015(2) -0.065(2) C3A 0.103(3) 0.091(2) 0.087(2) 0.019(2) -0.015(2) -0.065(2) C4 0.093(2) 0.110(3) 0.0370(13) 0.0011(15) -0.0147(14) -0.050(2) C4A 0.093(2) 0.110(3) 0.0370(13) 0.0011(15) -0.0147(14) -0.050(2) C5 0.138(3) 0.066(2) 0.108(3) -0.044(2) 0.063(3) -0.003(2) C5A 0.138(3) 0.066(2) 0.108(3) -0.044(2) 0.063(3) -0.003(2) C6 0.0622(18) 0.108(3) 0.080(2) 0.0284(19) 0.0168(16) 0.0388(18) C6A 0.0622(18) 0.108(3) 0.080(2) 0.0284(19) 0.0168(16) 0.0388(18) C7 0.0540(15) 0.0732(18) 0.0688(17) -0.0086(14) 0.0376(13) -0.0065(13) C7A 0.0540(15) 0.0732(18) 0.0688(17) -0.0086(14) 0.0376(13) -0.0065(13) C8 0.0659(16) 0.0628(16) 0.0428(13) -0.0007(11) -0.0058(11) -0.0303(13) C8A 0.0659(16) 0.0628(16) 0.0428(13) -0.0007(11) -0.0058(11) -0.0303(13) C9 0.0692(16) 0.0384(12) 0.0540(14) 0.0048(10) 0.0241(12) 0.0120(11) C9A 0.0692(16) 0.0384(12) 0.0540(14) 0.0048(10) 0.0241(12) 0.0120(11) C10 0.072(3) 0.0472(18) 0.133(4) -0.012(2) 0.044(3) -0.0151(17) C10A 0.054(14) 0.11(2) 0.21(3) 0.02(2) 0.00(2) -0.005(15) C11 0.107(4) 0.065(3) 0.189(6) 0.035(3) 0.096(4) 0.017(3) C11A 0.054(14) 0.11(3) 0.19(3) 0.00(3) 0.05(2) -0.005(18) _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 2.604(2) . ? K1 O2 2.665(2) . ? K1 C1 3.2302(18) . ? K1 C1 3.2302(18) 2_656 ? K1 C3 3.235(3) 2_656 ? K1 C3A 3.235(3) 2_656 ? K1 C6 3.420(3) 2_656 ? K1 C6A 3.420(3) 2_656 ? K2 C1 3.0132(18) . ? K2 C1 3.0132(18) 5_666 ? K2 C4 3.138(3) 5_666 ? K2 C4A 3.138(3) 5_666 ? K2 C7 3.433(3) 5_666 ? K2 C7A 3.433(3) 5_666 ? K2 C9 3.363(2) 5_666 ? K2 C9A 3.363(2) 5_666 ? Si1 C1 1.8014(19) . ? Si1 C2 1.923(4) . ? Si1 C3 1.909(4) . ? Si1 C4 1.911(3) . ? Si1A C1 1.845(3) . ? Si2 C1 1.8296(19) . ? Si2 C5 1.924(3) . ? Si2 C6 1.885(3) . ? Si2 C7 1.907(3) . ? Si2A C1 1.762(3) . ? Si3 O1 1.6631(8) . ? Si3 C1 1.8087(19) . ? Si3 C8 1.900(3) . ? Si3 C9 1.918(2) . ? Si3A O1 1.914(2) . ? Si3A C1 1.826(3) . ? O1 Si3 1.6631(8) 2_656 ? O1 Si3A 1.914(2) 2_656 ? O2 C10 1.423(4) . ? O2 C10 1.423(4) 2_656 ? O2 C10A 1.44(4) . ? O2 C10A 1.44(4) 2_656 ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C10 C11 1.475(8) . ? C10A H10C 0.990 . ? C10A H10D 0.990 . ? C10A C11A 1.46(5) . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C11A H11D 0.980 . ? C11A H11E 0.980 . ? C11A H11F 0.980 . ? 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 O2 180.0 . . ? O1 K1 C1 57.45(3) . . ? O1 K1 C1 57.45(3) . 2_656 ? O1 K1 C3 103.71(7) . 2_656 ? O1 K1 C3A 103.71(7) . 2_656 ? O1 K1 C6 87.07(7) . 2_656 ? O1 K1 C6A 87.07(7) . 2_656 ? O2 K1 C1 122.55(3) . . ? O2 K1 C1 122.55(3) . 2_656 ? O2 K1 C3 76.29(7) . 2_656 ? O2 K1 C3A 76.29(7) . 2_656 ? O2 K1 C6 92.93(7) . 2_656 ? O2 K1 C6A 92.93(7) . 2_656 ? C1 K1 C1 114.91(7) . 2_656 ? C1 K1 C3 58.25(6) 2_656 2_656 ? C1 K1 C3 141.38(10) . 2_656 ? C1 K1 C6 55.78(6) 2_656 2_656 ? C1 K1 C6 120.49(8) . 2_656 ? C3 K1 C6 88.35(10) 2_656 2_656 ? C3A K1 C6A 88.35(10) 2_656 2_656 ? C1 K2 C1 180.0 . 5_666 ? C1 K2 C4 119.19(6) . 5_666 ? C1 K2 C4 60.81(6) 5_666 5_666 ? C1 K2 C7 122.43(5) . 5_666 ? C1 K2 C7 57.57(5) 5_666 5_666 ? C1 K2 C9 121.71(5) . 5_666 ? C1 K2 C9 58.29(5) 5_666 5_666 ? C4 K2 C7 95.90(9) 5_666 5_666 ? C4 K2 C9 95.00(8) 5_666 5_666 ? C4A K2 C7A 95.90(9) 5_666 5_666 ? C4A K2 C9A 95.00(8) 5_666 5_666 ? C7 K2 C9 96.14(6) 5_666 5_666 ? C7A K2 C9A 96.14(6) 5_666 5_666 ? C1 Si1 C2 111.22(15) . . ? C1 Si1 C3 115.97(14) . . ? C1 Si1 C4 114.09(12) . . ? C2 Si1 C3 106.1(2) . . ? C2 Si1 C4 107.3(2) . . ? C3 Si1 C4 101.24(16) . . ? C1 Si2 C5 112.21(15) . . ? C1 Si2 C6 113.99(12) . . ? C1 Si2 C7 113.55(11) . . ? C5 Si2 C6 108.24(19) . . ? C5 Si2 C7 104.23(15) . . ? C6 Si2 C7 103.82(16) . . ? O1 Si3 C1 110.71(9) . . ? O1 Si3 C8 110.27(9) . . ? O1 Si3 C9 104.08(10) . . ? C1 Si3 C8 112.94(11) . . ? C1 Si3 C9 113.67(11) . . ? C8 Si3 C9 104.67(13) . . ? O1 Si3A C1 99.63(13) . . ? K1 O1 Si3 106.78(7) . . ? K1 O1 Si3 106.78(7) . 2_656 ? K1 O1 Si3A 96.02(9) . . ? K1 O1 Si3A 96.02(9) . 2_656 ? Si3 O1 Si3 146.44(14) . 2_656 ? Si3A O1 Si3A 167.96(19) . 2_656 ? K1 O2 C10 122.98(18) . . ? K1 O2 C10 122.98(19) . 2_656 ? K1 O2 C10A 126(2) . . ? K1 O2 C10A 126(2) . 2_656 ? C10 O2 C10 114.0(4) . 2_656 ? C10A O2 C10A 107(4) . 2_656 ? K1 C1 K2 169.04(7) . . ? K1 C1 Si1 84.60(7) . . ? K1 C1 Si1A 93.00(12) . . ? K1 C1 Si2 94.34(7) . . ? K1 C1 Si2A 96.51(11) . . ? K1 C1 Si3 81.85(6) . . ? K1 C1 Si3A 78.87(9) . . ? K2 C1 Si1 90.24(7) . . ? K2 C1 Si1A 89.42(12) . . ? K2 C1 Si2 96.62(7) . . ? K2 C1 Si2A 91.35(11) . . ? K2 C1 Si3 92.62(7) . . ? K2 C1 Si3A 90.60(10) . . ? Si1 C1 Si2 119.88(10) . . ? Si1 C1 Si3 121.06(10) . . ? Si1A C1 Si2A 121.25(16) . . ? Si1A C1 Si3A 118.72(16) . . ? Si2 C1 Si3 118.17(10) . . ? Si2A C1 Si3A 120.01(15) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si3 C9 H9A 109.5 . . ? Si3 C9 H9B 109.5 . . ? Si3 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C10 H10A 108.8 . . ? O2 C10 H10B 108.8 . . ? O2 C10 C11 113.7(5) . . ? H10A C10 H10B 107.7 . . ? H10A C10 C11 108.8 . . ? H10B C10 C11 108.8 . . ? O2 C10A H10C 111.7 . . ? O2 C10A H10D 111.7 . . ? O2 C10A C11A 100(4) . . ? H10C C10A H10D 109.5 . . ? H10C C10A C11A 111.7 . . ? H10D C10A C11A 111.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10A C11A H11D 109.5 . . ? C10A C11A H11E 109.5 . . ? C10A C11A H11F 109.5 . . ? H11D C11A H11E 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.775 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.058 #===END data_ki206_compound7 _database_code_depnum_ccdc_archive 'CCDC 279577' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H30 O6 Li +,C20 H52 O2 Si6 Li -' _chemical_formula_sum 'C32 H82 Li2 O8 Si6' _chemical_formula_weight 777.40 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'A b a 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/2, y+1, z+1/2' 'x+1/2, -y+1, z+1/2' _cell_length_a 22.008(3) _cell_length_b 23.186(2) _cell_length_c 19.182(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9788(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 746 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.055 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 0.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 0.916 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34805 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 27.51 _reflns_number_total 9070 _reflns_number_gt 6398 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _computing_structure_solution SIR97 _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.1021P)^2^+0.0000P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0031(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.73(14) _refine_ls_number_reflns 9070 _refine_ls_number_parameters 458 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1695 _refine_ls_wR_factor_gt 0.1459 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.002 _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 Si1 Si 0.43743(5) 0.57356(5) 0.76380(7) 0.0275(3) Uani 1 1 d . . . Si2 Si 0.37011(5) 0.56700(5) 0.61939(7) 0.0300(3) Uani 1 1 d . . . Si3 Si 0.49876(5) 0.61589(4) 0.62715(7) 0.0285(3) Uani 1 1 d . . . O1 O 0.52715(13) 0.57053(12) 0.56544(16) 0.0328(7) Uani 1 1 d . . . Li1 Li 0.5000 0.5000 0.6171(5) 0.026(2) Uani 1 2 d S . . C1 C 0.50164(18) 0.53362(17) 0.8100(2) 0.0302(10) Uani 1 1 d . . . H1A H 0.5405 0.5452 0.7881 0.036 Uiso 1 1 calc R . . H1B H 0.5028 0.5468 0.8591 0.036 Uiso 1 1 calc R . . C2 C 0.4378(2) 0.6492(2) 0.8030(3) 0.0474(13) Uani 1 1 d . . . H2A H 0.4778 0.6669 0.7958 0.071 Uiso 1 1 calc R . . H2B H 0.4293 0.6468 0.8531 0.071 Uiso 1 1 calc R . . H2C H 0.4066 0.6727 0.7803 0.071 Uiso 1 1 calc R . . C3 C 0.3654(2) 0.5407(2) 0.8019(3) 0.0421(12) Uani 1 1 d . . . H3A H 0.3299 0.5617 0.7843 0.063 Uiso 1 1 calc R . . H3B H 0.3667 0.5435 0.8529 0.063 Uiso 1 1 calc R . . H3C H 0.3626 0.5001 0.7882 0.063 Uiso 1 1 calc R . . C4 C 0.44104(18) 0.57290(17) 0.6684(2) 0.0256(9) Uani 1 1 d . . . C5 C 0.3147(2) 0.6283(2) 0.6368(3) 0.0423(12) Uani 1 1 d . . . H5A H 0.3043 0.6290 0.6864 0.063 Uiso 1 1 calc R . . H5B H 0.2778 0.6224 0.6091 0.063 Uiso 1 1 calc R . . H5C H 0.3336 0.6650 0.6237 0.063 Uiso 1 1 calc R . . C6 C 0.3817(2) 0.5667(2) 0.5214(3) 0.0447(12) Uani 1 1 d . . . H6A H 0.3957 0.6049 0.5062 0.067 Uiso 1 1 calc R . . H6B H 0.3433 0.5574 0.4982 0.067 Uiso 1 1 calc R . . H6C H 0.4123 0.5377 0.5091 0.067 Uiso 1 1 calc R . . C7 C 0.3261(2) 0.4984(2) 0.6351(3) 0.0427(12) Uani 1 1 d . . . H7A H 0.3515 0.4652 0.6231 0.064 Uiso 1 1 calc R . . H7B H 0.2895 0.4983 0.6061 0.064 Uiso 1 1 calc R . . H7C H 0.3145 0.4962 0.6844 0.064 Uiso 1 1 calc R . . C8 C 0.4765(2) 0.6845(2) 0.5822(3) 0.0495(14) Uani 1 1 d . . . H8A H 0.5128 0.7029 0.5625 0.074 Uiso 1 1 calc R . . H8B H 0.4575 0.7107 0.6159 0.074 Uiso 1 1 calc R . . H8C H 0.4477 0.6759 0.5447 0.074 Uiso 1 1 calc R . . C9 C 0.5676(2) 0.6363(2) 0.6818(3) 0.0440(12) Uani 1 1 d . . . H9A H 0.5833 0.6019 0.7054 0.066 Uiso 1 1 calc R . . H9B H 0.5558 0.6651 0.7166 0.066 Uiso 1 1 calc R . . H9C H 0.5993 0.6523 0.6515 0.066 Uiso 1 1 calc R . . C10 C 0.5618(3) 0.5887(3) 0.5063(4) 0.0694(19) Uani 1 1 d . . . H10A H 0.5367 0.6136 0.4767 0.104 Uiso 1 1 calc R . . H10B H 0.5749 0.5549 0.4797 0.104 Uiso 1 1 calc R . . H10C H 0.5976 0.6102 0.5222 0.104 Uiso 1 1 calc R . . Si4 Si 0.06259(5) 0.57232(5) 0.56563(7) 0.0321(3) Uani 1 1 d . . . Si5 Si 0.04467(5) 0.63392(5) 0.70956(8) 0.0350(3) Uani 1 1 d . . . Si6 Si 0.11792(5) 0.52160(5) 0.70163(7) 0.0299(3) Uani 1 1 d . . . O2 O 0.07669(12) 0.48666(13) 0.76345(16) 0.0329(7) Uani 1 1 d . . . Li2 Li 0.0000 0.5000 0.7108(6) 0.031(2) Uani 1 2 d S . . C11 C 0.0349(2) 0.50516(19) 0.5183(2) 0.0337(10) Uani 1 1 d . . . H11A H 0.0488 0.5073 0.4693 0.040 Uiso 1 1 calc R . . H11B H 0.0548 0.4712 0.5397 0.040 Uiso 1 1 calc R . . C12 C 0.0142(3) 0.6340(2) 0.5288(3) 0.0506(14) Uani 1 1 d . . . H12A H -0.0283 0.6286 0.5428 0.076 Uiso 1 1 calc R . . H12B H 0.0169 0.6340 0.4778 0.076 Uiso 1 1 calc R . . H12C H 0.0291 0.6709 0.5469 0.076 Uiso 1 1 calc R . . C13 C 0.1412(2) 0.5873(3) 0.5272(3) 0.0517(14) Uani 1 1 d . . . H13A H 0.1581 0.6223 0.5483 0.077 Uiso 1 1 calc R . . H13B H 0.1377 0.5926 0.4767 0.077 Uiso 1 1 calc R . . H13C H 0.1681 0.5546 0.5369 0.077 Uiso 1 1 calc R . . C14 C 0.06241(18) 0.56794(17) 0.6617(2) 0.0270(10) Uani 1 1 d . . . C15 C 0.0975(2) 0.69677(19) 0.6856(3) 0.0491(13) Uani 1 1 d . . . H15A H 0.1399 0.6846 0.6908 0.074 Uiso 1 1 calc R . . H15B H 0.0895 0.7295 0.7167 0.074 Uiso 1 1 calc R . . H15C H 0.0901 0.7084 0.6373 0.074 Uiso 1 1 calc R . . C16 C -0.0357(2) 0.6631(2) 0.6971(3) 0.0505(13) Uani 1 1 d . . . H16A H -0.0436 0.6688 0.6473 0.076 Uiso 1 1 calc R . . H16B H -0.0397 0.7001 0.7216 0.076 Uiso 1 1 calc R . . H16C H -0.0651 0.6356 0.7161 0.076 Uiso 1 1 calc R . . C17 C 0.0513(2) 0.6249(2) 0.8093(3) 0.0480(13) Uani 1 1 d . . . H17A H 0.0343 0.5875 0.8230 0.072 Uiso 1 1 calc R . . H17B H 0.0289 0.6559 0.8325 0.072 Uiso 1 1 calc R . . H17C H 0.0942 0.6266 0.8229 0.072 Uiso 1 1 calc R . . C18 C 0.1499(2) 0.4625(2) 0.6447(3) 0.0427(12) Uani 1 1 d . . . H18A H 0.1738 0.4358 0.6734 0.064 Uiso 1 1 calc R . . H18B H 0.1761 0.4794 0.6088 0.064 Uiso 1 1 calc R . . H18C H 0.1165 0.4415 0.6224 0.064 Uiso 1 1 calc R . . C19 C 0.1855(2) 0.5533(2) 0.7479(3) 0.0429(12) Uani 1 1 d . . . H19A H 0.1718 0.5738 0.7898 0.064 Uiso 1 1 calc R . . H19B H 0.2064 0.5804 0.7168 0.064 Uiso 1 1 calc R . . H19C H 0.2135 0.5223 0.7613 0.064 Uiso 1 1 calc R . . C20 C 0.1017(2) 0.4571(3) 0.8231(3) 0.0594(16) Uani 1 1 d . . . H20A H 0.1386 0.4363 0.8092 0.089 Uiso 1 1 calc R . . H20B H 0.0718 0.4296 0.8413 0.089 Uiso 1 1 calc R . . H20C H 0.1119 0.4853 0.8594 0.089 Uiso 1 1 calc R . . Li3 Li 0.2680(3) 0.8019(3) 0.4180(4) 0.0287(15) Uani 1 1 d . . . O3 O 0.16980(14) 0.80479(14) 0.44381(18) 0.0388(8) Uani 1 1 d . . . O4 O 0.26811(13) 0.78404(13) 0.52568(16) 0.0355(7) Uani 1 1 d . . . O5 O 0.27937(13) 0.89312(12) 0.42180(17) 0.0377(7) Uani 1 1 d . . . O6 O 0.36559(13) 0.81088(13) 0.41730(18) 0.0386(7) Uani 1 1 d . . . O7 O 0.25765(18) 0.80544(15) 0.30685(17) 0.0497(9) Uani 1 1 d . . . O8 O 0.26222(16) 0.71393(13) 0.38898(18) 0.0467(9) Uani 1 1 d . . . C21 C 0.1238(2) 0.7928(2) 0.3945(3) 0.0511(14) Uani 1 1 d . . . H21A H 0.1251 0.7519 0.3820 0.077 Uiso 1 1 calc R . . H21B H 0.1303 0.8163 0.3527 0.077 Uiso 1 1 calc R . . H21C H 0.0840 0.8020 0.4147 0.077 Uiso 1 1 calc R . . C22 C 0.1634(2) 0.7707(3) 0.5052(3) 0.0512(14) Uani 1 1 d . . . H22A H 0.1696 0.7294 0.4940 0.061 Uiso 1 1 calc R . . H22B H 0.1221 0.7754 0.5248 0.061 Uiso 1 1 calc R . . C23 C 0.2098(2) 0.7901(3) 0.5572(3) 0.0556(15) Uani 1 1 d . . . H23A H 0.2026 0.8308 0.5702 0.067 Uiso 1 1 calc R . . H23B H 0.2073 0.7662 0.5999 0.067 Uiso 1 1 calc R . . C24 C 0.3170(2) 0.7990(2) 0.5736(3) 0.0467(12) Uani 1 1 d . . . H24A H 0.3143 0.8400 0.5856 0.070 Uiso 1 1 calc R . . H24B H 0.3563 0.7914 0.5514 0.070 Uiso 1 1 calc R . . H24C H 0.3134 0.7758 0.6161 0.070 Uiso 1 1 calc R . . C25 C 0.2386(3) 0.9328(2) 0.4530(3) 0.0562(15) Uani 1 1 d . . . H25A H 0.2439 0.9321 0.5037 0.084 Uiso 1 1 calc R . . H25B H 0.1968 0.9221 0.4413 0.084 Uiso 1 1 calc R . . H25C H 0.2471 0.9717 0.4355 0.084 Uiso 1 1 calc R . . C26 C 0.3410(2) 0.9092(2) 0.4326(3) 0.0457(13) Uani 1 1 d . . . H26A H 0.3507 0.9082 0.4829 0.055 Uiso 1 1 calc R . . H26B H 0.3479 0.9489 0.4153 0.055 Uiso 1 1 calc R . . C27 C 0.3805(2) 0.8674(2) 0.3937(3) 0.0454(13) Uani 1 1 d . . . H27A H 0.3731 0.8706 0.3429 0.055 Uiso 1 1 calc R . . H27B H 0.4239 0.8757 0.4028 0.055 Uiso 1 1 calc R . . C28 C 0.4078(2) 0.7680(3) 0.3948(3) 0.0582(15) Uani 1 1 d . . . H28A H 0.4092 0.7674 0.3438 0.087 Uiso 1 1 calc R . . H28B H 0.3949 0.7302 0.4121 0.087 Uiso 1 1 calc R . . H28C H 0.4482 0.7771 0.4132 0.087 Uiso 1 1 calc R . . C29 C 0.2504(3) 0.8543(3) 0.2635(3) 0.0628(16) Uani 1 1 d . . . H29A H 0.2780 0.8514 0.2236 0.094 Uiso 1 1 calc R . . H29B H 0.2599 0.8893 0.2901 0.094 Uiso 1 1 calc R . . H29C H 0.2084 0.8562 0.2469 0.094 Uiso 1 1 calc R . . C30 C 0.2475(3) 0.7518(2) 0.2751(3) 0.0636(17) Uani 1 1 d . . . H30A H 0.2714 0.7499 0.2315 0.076 Uiso 1 1 calc R . . H30B H 0.2040 0.7489 0.2624 0.076 Uiso 1 1 calc R . . C31 C 0.2633(3) 0.7033(2) 0.3180(3) 0.0621(16) Uani 1 1 d . . . H31A H 0.2348 0.6714 0.3077 0.074 Uiso 1 1 calc R . . H31B H 0.3046 0.6902 0.3050 0.074 Uiso 1 1 calc R . . C32 C 0.2746(3) 0.6641(2) 0.4309(3) 0.0528(14) Uani 1 1 d . . . H32A H 0.2443 0.6342 0.4210 0.079 Uiso 1 1 calc R . . H32B H 0.2726 0.6747 0.4803 0.079 Uiso 1 1 calc R . . H32C H 0.3152 0.6495 0.4200 0.079 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 Si1 0.0287(6) 0.0284(6) 0.0255(6) -0.0014(5) 0.0020(5) 0.0036(5) Si2 0.0253(5) 0.0318(6) 0.0329(7) 0.0003(6) -0.0033(5) 0.0025(5) Si3 0.0303(5) 0.0222(5) 0.0330(6) 0.0027(5) 0.0027(5) -0.0021(4) O1 0.0388(16) 0.0296(16) 0.0301(17) 0.0040(13) 0.0127(14) 0.0002(12) Li1 0.025(4) 0.025(4) 0.027(5) 0.000 0.000 -0.014(4) C1 0.035(2) 0.027(2) 0.028(2) -0.0012(19) -0.0058(19) -0.0034(18) C2 0.064(3) 0.037(3) 0.042(3) -0.009(2) 0.001(3) 0.017(2) C3 0.030(2) 0.058(3) 0.038(3) 0.011(2) 0.008(2) 0.008(2) C4 0.025(2) 0.025(2) 0.027(2) 0.0007(17) 0.0021(18) 0.0017(16) C5 0.035(2) 0.043(3) 0.049(3) 0.004(2) -0.004(2) 0.009(2) C6 0.043(3) 0.054(3) 0.037(3) -0.004(2) -0.010(2) 0.005(2) C7 0.030(2) 0.047(3) 0.052(3) -0.006(2) -0.004(2) -0.011(2) C8 0.053(3) 0.030(2) 0.066(4) 0.013(2) 0.011(3) 0.003(2) C9 0.040(3) 0.040(3) 0.052(3) 0.000(2) -0.001(2) -0.013(2) C10 0.086(4) 0.058(4) 0.064(4) 0.018(3) 0.046(4) 0.010(3) Si4 0.0348(7) 0.0296(6) 0.0318(7) 0.0042(5) -0.0034(6) -0.0074(5) Si5 0.0408(6) 0.0246(5) 0.0395(7) -0.0022(6) -0.0021(6) -0.0033(5) Si6 0.0257(5) 0.0313(6) 0.0327(7) 0.0005(5) -0.0030(5) -0.0034(5) O2 0.0299(15) 0.0391(17) 0.0298(17) 0.0075(14) -0.0057(13) 0.0008(12) Li2 0.030(5) 0.031(5) 0.033(6) 0.000 0.000 -0.010(4) C11 0.035(2) 0.037(2) 0.030(2) -0.003(2) 0.002(2) -0.0022(19) C12 0.066(3) 0.034(3) 0.052(3) 0.016(2) -0.020(3) -0.006(2) C13 0.052(3) 0.066(3) 0.037(3) 0.008(3) 0.004(2) -0.027(3) C14 0.024(2) 0.024(2) 0.033(3) -0.0022(18) -0.0031(18) -0.0062(16) C15 0.063(3) 0.027(2) 0.058(4) -0.002(2) -0.007(3) -0.011(2) C16 0.052(3) 0.043(3) 0.057(4) 0.003(3) -0.002(3) 0.011(2) C17 0.057(3) 0.038(3) 0.048(3) -0.012(2) 0.008(3) -0.012(2) C18 0.039(3) 0.044(3) 0.045(3) 0.004(2) -0.002(2) 0.006(2) C19 0.031(2) 0.049(3) 0.049(3) 0.001(2) -0.004(2) -0.009(2) C20 0.058(3) 0.074(4) 0.046(4) 0.024(3) -0.014(3) 0.000(3) Li3 0.023(3) 0.035(4) 0.028(4) 0.000(3) 0.003(3) -0.003(3) O3 0.0329(16) 0.0401(19) 0.043(2) -0.0076(15) 0.0059(14) -0.0031(14) O4 0.0390(17) 0.0421(18) 0.0255(16) -0.0025(14) 0.0068(14) -0.0058(14) O5 0.0411(17) 0.0315(16) 0.0404(19) -0.0036(15) -0.0015(16) -0.0031(13) O6 0.0342(16) 0.0440(18) 0.0376(18) -0.0015(16) 0.0027(15) -0.0031(13) O7 0.080(3) 0.0405(19) 0.0280(19) 0.0031(16) -0.0111(17) 0.0022(18) O8 0.073(2) 0.0323(16) 0.0347(19) -0.0030(15) -0.0066(17) 0.0100(16) C21 0.046(3) 0.050(3) 0.057(4) -0.024(3) 0.000(3) 0.000(2) C22 0.035(3) 0.059(3) 0.060(4) 0.003(3) 0.024(3) -0.009(2) C23 0.053(3) 0.070(4) 0.043(3) 0.009(3) 0.020(3) 0.000(3) C24 0.062(3) 0.051(3) 0.027(3) 0.004(2) -0.003(2) -0.002(2) C25 0.061(3) 0.037(3) 0.070(4) -0.009(3) 0.003(3) 0.011(2) C26 0.050(3) 0.034(3) 0.053(3) 0.009(2) -0.003(2) -0.016(2) C27 0.036(2) 0.055(3) 0.044(3) 0.012(3) 0.006(2) -0.019(2) C28 0.034(3) 0.077(4) 0.064(4) -0.017(3) 0.002(3) 0.011(3) C29 0.091(4) 0.062(4) 0.035(3) 0.017(3) -0.004(3) 0.016(3) C30 0.100(5) 0.061(4) 0.030(3) -0.012(3) -0.012(3) 0.033(3) C31 0.089(4) 0.048(3) 0.049(4) -0.016(3) -0.006(3) 0.008(3) C32 0.069(3) 0.032(3) 0.058(4) 0.008(2) 0.010(3) 0.002(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 Si1 C1 1.908(4) . ? Si1 C2 1.909(5) . ? Si1 C3 1.904(5) . ? Si1 C4 1.831(5) . ? Si2 C4 1.828(4) . ? Si2 C5 1.901(5) . ? Si2 C6 1.897(6) . ? Si2 C7 1.885(5) . ? Si3 O1 1.702(3) . ? Si3 C4 1.799(4) . ? Si3 C8 1.875(5) . ? Si3 C9 1.902(5) . ? O1 Li1 2.003(6) . ? O1 C10 1.430(6) . ? Li1 O1 2.003(6) 2_665 ? Li1 C4 2.347(6) . ? Li1 C4 2.347(6) 2_665 ? C1 C1 1.561(8) 2_665 ? C1 H1A 0.990 . ? C1 H1B 0.990 . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? Si4 C11 1.902(4) . ? Si4 C12 1.919(5) . ? Si4 C13 1.913(5) . ? Si4 C14 1.846(5) . ? Si5 C14 1.826(4) . ? Si5 C15 1.920(5) . ? Si5 C16 1.908(5) . ? Si5 C17 1.929(6) . ? Si6 O2 1.699(3) . ? Si6 C14 1.798(4) . ? Si6 C18 1.889(5) . ? Si6 C19 1.882(5) . ? O2 Li2 1.991(6) . ? O2 C20 1.444(6) . ? Li2 O2 1.991(6) 2_565 ? Li2 C14 2.292(6) . ? Li2 C14 2.292(6) 2_565 ? C11 C11 1.557(9) 2_565 ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 H13A 0.980 . ? C13 H13B 0.980 . ? C13 H13C 0.980 . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C18 H18A 0.980 . ? C18 H18B 0.980 . ? C18 H18C 0.980 . ? C19 H19A 0.980 . ? C19 H19B 0.980 . ? C19 H19C 0.980 . ? C20 H20A 0.980 . ? C20 H20B 0.980 . ? C20 H20C 0.980 . ? Li3 O3 2.218(7) . ? Li3 O4 2.106(8) . ? Li3 O5 2.130(7) . ? Li3 O6 2.158(7) . ? Li3 O7 2.147(8) . ? Li3 O8 2.119(8) . ? O3 C21 1.413(6) . ? O3 C22 1.426(6) . ? O4 C23 1.426(6) . ? O4 C24 1.458(6) . ? O5 C25 1.418(6) . ? O5 C26 1.421(5) . ? O6 C27 1.425(6) . ? O6 C28 1.426(6) . ? O7 C29 1.415(6) . ? O7 C30 1.402(6) . ? O8 C31 1.384(7) . ? O8 C32 1.432(6) . ? C21 H21A 0.980 . ? C21 H21B 0.980 . ? C21 H21C 0.980 . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C22 C23 1.495(8) . ? C23 H23A 0.990 . ? C23 H23B 0.990 . ? C24 H24A 0.980 . ? C24 H24B 0.980 . ? C24 H24C 0.980 . ? C25 H25A 0.980 . ? C25 H25B 0.980 . ? C25 H25C 0.980 . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C26 C27 1.503(7) . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C28 H28A 0.980 . ? C28 H28B 0.980 . ? C28 H28C 0.980 . ? C29 H29A 0.980 . ? C29 H29B 0.980 . ? C29 H29C 0.980 . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? C30 C31 1.436(8) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 H32A 0.980 . ? C32 H32B 0.980 . ? C32 H32C 0.980 . ? 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 C1 Si1 C2 105.1(2) . . ? C1 Si1 C3 104.1(2) . . ? C1 Si1 C4 115.3(2) . . ? C2 Si1 C3 102.7(2) . . ? C2 Si1 C4 113.6(2) . . ? C3 Si1 C4 114.6(2) . . ? C4 Si2 C5 113.7(2) . . ? C4 Si2 C6 113.3(2) . . ? C4 Si2 C7 114.8(2) . . ? C5 Si2 C6 105.2(2) . . ? C5 Si2 C7 105.8(2) . . ? C6 Si2 C7 103.0(2) . . ? O1 Si3 C4 102.88(17) . . ? O1 Si3 C8 107.5(2) . . ? O1 Si3 C9 104.1(2) . . ? C4 Si3 C8 119.2(2) . . ? C4 Si3 C9 117.2(2) . . ? C8 Si3 C9 104.5(2) . . ? Si3 O1 Li1 92.9(3) . . ? Si3 O1 C10 124.4(3) . . ? Li1 O1 C10 142.4(4) . . ? O1 Li1 O1 120.7(5) . 2_665 ? O1 Li1 C4 77.56(13) . . ? O1 Li1 C4 129.08(14) 2_665 . ? O1 Li1 C4 77.56(13) 2_665 2_665 ? O1 Li1 C4 129.08(14) . 2_665 ? C4 Li1 C4 130.4(5) . 2_665 ? Si1 C1 C1 116.8(3) . 2_665 ? Si1 C1 H1A 108.1 . . ? Si1 C1 H1B 108.1 . . ? C1 C1 H1A 108.1 2_665 . ? C1 C1 H1B 108.1 2_665 . ? H1A C1 H1B 107.3 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 Si2 118.5(2) . . ? Si1 C4 Si3 117.8(2) . . ? Si1 C4 Li1 116.7(3) . . ? Si2 C4 Si3 114.7(2) . . ? Si2 C4 Li1 101.7(2) . . ? Si3 C4 Li1 79.86(18) . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si3 C9 H9A 109.5 . . ? Si3 C9 H9B 109.5 . . ? Si3 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 H10A 109.5 . . ? O1 C10 H10B 109.5 . . ? O1 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 Si4 C12 104.9(2) . . ? C11 Si4 C13 104.7(2) . . ? C11 Si4 C14 115.5(2) . . ? C12 Si4 C13 103.0(3) . . ? C12 Si4 C14 114.1(2) . . ? C13 Si4 C14 113.4(2) . . ? C14 Si5 C15 112.7(2) . . ? C14 Si5 C16 115.6(2) . . ? C14 Si5 C17 113.0(2) . . ? C15 Si5 C16 105.2(2) . . ? C15 Si5 C17 105.9(2) . . ? C16 Si5 C17 103.5(3) . . ? O2 Si6 C14 102.66(17) . . ? O2 Si6 C18 104.85(19) . . ? O2 Si6 C19 106.2(2) . . ? C14 Si6 C18 116.2(2) . . ? C14 Si6 C19 120.3(2) . . ? C18 Si6 C19 105.2(2) . . ? Si6 O2 Li2 91.4(3) . . ? Si6 O2 C20 125.2(3) . . ? Li2 O2 C20 143.1(4) . . ? O2 Li2 O2 119.1(6) . 2_565 ? O2 Li2 C14 78.88(14) . . ? O2 Li2 C14 127.55(14) . 2_565 ? O2 Li2 C14 78.88(14) 2_565 2_565 ? O2 Li2 C14 127.55(14) 2_565 . ? C14 Li2 C14 131.5(6) . 2_565 ? Si4 C11 C11 116.2(4) . 2_565 ? Si4 C11 H11A 108.2 . . ? Si4 C11 H11B 108.2 . . ? C11 C11 H11A 108.2 2_565 . ? C11 C11 H11B 108.2 2_565 . ? H11A C11 H11B 107.4 . . ? Si4 C12 H12A 109.5 . . ? Si4 C12 H12B 109.5 . . ? Si4 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si4 C13 H13A 109.5 . . ? Si4 C13 H13B 109.5 . . ? Si4 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si4 C14 Si5 117.1(2) . . ? Si4 C14 Si6 117.2(2) . . ? Si4 C14 Li2 116.7(3) . . ? Si5 C14 Si6 115.6(2) . . ? Si5 C14 Li2 104.0(3) . . ? Si6 C14 Li2 79.71(19) . . ? Si5 C15 H15A 109.5 . . ? Si5 C15 H15B 109.5 . . ? Si5 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si5 C16 H16A 109.5 . . ? Si5 C16 H16B 109.5 . . ? Si5 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si5 C17 H17A 109.5 . . ? Si5 C17 H17B 109.5 . . ? Si5 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si6 C18 H18A 109.5 . . ? Si6 C18 H18B 109.5 . . ? Si6 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si6 C19 H19A 109.5 . . ? Si6 C19 H19B 109.5 . . ? Si6 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O2 C20 H20A 109.5 . . ? O2 C20 H20B 109.5 . . ? O2 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O3 Li3 O4 77.8(3) . . ? O3 Li3 O5 94.4(3) . . ? O3 Li3 O6 165.6(4) . . ? O3 Li3 O7 96.7(3) . . ? O3 Li3 O8 91.7(3) . . ? O4 Li3 O5 99.3(3) . . ? O4 Li3 O6 91.4(3) . . ? O4 Li3 O7 169.0(4) . . ? O4 Li3 O8 93.9(3) . . ? O5 Li3 O6 77.7(2) . . ? O5 Li3 O7 90.5(3) . . ? O5 Li3 O8 166.3(4) . . ? O6 Li3 O7 95.5(3) . . ? O6 Li3 O8 98.7(3) . . ? O7 Li3 O8 76.6(3) . . ? Li3 O3 C21 122.9(3) . . ? Li3 O3 C22 105.3(3) . . ? C21 O3 C22 111.9(4) . . ? Li3 O4 C23 113.3(3) . . ? Li3 O4 C24 124.9(3) . . ? C23 O4 C24 112.0(4) . . ? Li3 O5 C25 125.8(3) . . ? Li3 O5 C26 112.2(3) . . ? C25 O5 C26 111.8(4) . . ? Li3 O6 C27 108.7(3) . . ? Li3 O6 C28 125.7(3) . . ? C27 O6 C28 113.2(4) . . ? Li3 O7 C29 128.8(4) . . ? Li3 O7 C30 114.5(4) . . ? C29 O7 C30 115.9(4) . . ? Li3 O8 C31 115.4(4) . . ? Li3 O8 C32 128.1(4) . . ? C31 O8 C32 113.9(4) . . ? O3 C21 H21A 109.5 . . ? O3 C21 H21B 109.5 . . ? O3 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O3 C22 H22A 110.0 . . ? O3 C22 H22B 110.0 . . ? O3 C22 C23 108.5(4) . . ? H22A C22 H22B 108.4 . . ? H22A C22 C23 110.0 . . ? H22B C22 C23 110.0 . . ? O4 C23 C22 107.6(4) . . ? O4 C23 H23A 110.2 . . ? O4 C23 H23B 110.2 . . ? C22 C23 H23A 110.2 . . ? C22 C23 H23B 110.2 . . ? H23A C23 H23B 108.5 . . ? O4 C24 H24A 109.5 . . ? O4 C24 H24B 109.5 . . ? O4 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O5 C25 H25A 109.5 . . ? O5 C25 H25B 109.5 . . ? O5 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O5 C26 H26A 110.1 . . ? O5 C26 H26B 110.1 . . ? O5 C26 C27 108.1(4) . . ? H26A C26 H26B 108.4 . . ? H26A C26 C27 110.1 . . ? H26B C26 C27 110.1 . . ? O6 C27 C26 107.6(4) . . ? O6 C27 H27A 110.2 . . ? O6 C27 H27B 110.2 . . ? C26 C27 H27A 110.2 . . ? C26 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? O6 C28 H28A 109.5 . . ? O6 C28 H28B 109.5 . . ? O6 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O7 C29 H29A 109.5 . . ? O7 C29 H29B 109.5 . . ? O7 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O7 C30 H30A 108.7 . . ? O7 C30 H30B 108.7 . . ? O7 C30 C31 114.0(4) . . ? H30A C30 H30B 107.6 . . ? H30A C30 C31 108.7 . . ? H30B C30 C31 108.7 . . ? O8 C31 C30 114.8(4) . . ? O8 C31 H31A 108.6 . . ? O8 C31 H31B 108.6 . . ? C30 C31 H31A 108.6 . . ? C30 C31 H31B 108.6 . . ? H31A C31 H31B 107.5 . . ? O8 C32 H32A 109.5 . . ? O8 C32 H32B 109.5 . . ? O8 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.515 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.100 #===END data_ki136_compound3 _database_code_depnum_ccdc_archive 'CCDC 279578' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H27 K O Si3' _chemical_formula_sum 'C10 H27 K O Si3' _chemical_formula_weight 286.69 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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3569(6) _cell_length_b 15.2079(10) _cell_length_c 12.4082(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.998(1) _cell_angle_gamma 90.00 _cell_volume 1688.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10643 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.62 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_T_max 0.905 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11763 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2958 _reflns_number_gt 2670 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0493P)^2^+2.2458P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2958 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 K K 0.77277(7) 0.25050(5) 0.68205(5) 0.0401(2) Uani 1 1 d . . . Si1 Si 0.61169(8) 0.17272(5) 0.89919(6) 0.0298(2) Uani 1 1 d . . . Si2 Si 0.71275(9) 0.37176(5) 0.91542(7) 0.0318(2) Uani 1 1 d . . . Si3 Si 0.95166(8) 0.22182(5) 0.97593(6) 0.0299(2) Uani 1 1 d . . . O1 O 0.9802(3) 0.17844(18) 1.1054(2) 0.0549(6) Uani 1 1 d . . . C1 C 0.7590(3) 0.25523(17) 0.9256(2) 0.0289(6) Uani 1 1 d . . . C2 C 0.6805(4) 0.0567(2) 0.9238(4) 0.0569(10) Uani 1 1 d . . . H2A H 0.7281 0.0400 0.8662 0.085 Uiso 1 1 calc R . . H2B H 0.5961 0.0173 0.9196 0.085 Uiso 1 1 calc R . . H2C H 0.7534 0.0520 0.9986 0.085 Uiso 1 1 calc R . . C3 C 0.4805(4) 0.1707(3) 0.7512(3) 0.0532(9) Uani 1 1 d . . . H3A H 0.4471 0.2306 0.7278 0.080 Uiso 1 1 calc R . . H3B H 0.3938 0.1339 0.7491 0.080 Uiso 1 1 calc R . . H3C H 0.5326 0.1465 0.6999 0.080 Uiso 1 1 calc R . . C4 C 0.4800(4) 0.1813(3) 0.9896(3) 0.0550(9) Uani 1 1 d . . . H4A H 0.5290 0.1575 1.0648 0.082 Uiso 1 1 calc R . . H4B H 0.3889 0.1477 0.9546 0.082 Uiso 1 1 calc R . . H4C H 0.4542 0.2431 0.9962 0.082 Uiso 1 1 calc R . . C5 C 0.5077(4) 0.3963(2) 0.8626(4) 0.0630(11) Uani 1 1 d . . . H5A H 0.4664 0.3712 0.7871 0.095 Uiso 1 1 calc R . . H5B H 0.4924 0.4601 0.8592 0.095 Uiso 1 1 calc R . . H5C H 0.4570 0.3704 0.9138 0.095 Uiso 1 1 calc R . . C6 C 0.7760(5) 0.4356(2) 1.0523(3) 0.0545(9) Uani 1 1 d . . . H6A H 0.7122 0.4206 1.0997 0.082 Uiso 1 1 calc R . . H6B H 0.7686 0.4988 1.0360 0.082 Uiso 1 1 calc R . . H6C H 0.8799 0.4205 1.0919 0.082 Uiso 1 1 calc R . . C7 C 0.7913(4) 0.4385(3) 0.8168(3) 0.0560(9) Uani 1 1 d . . . H7A H 0.8977 0.4251 0.8314 0.084 Uiso 1 1 calc R . . H7B H 0.7791 0.5013 0.8295 0.084 Uiso 1 1 calc R . . H7C H 0.7377 0.4237 0.7386 0.084 Uiso 1 1 calc R . . C8 C 1.1173(5) 0.1437(3) 1.1678(4) 0.0751(13) Uani 1 1 d . . . H8A H 1.1698 0.1201 1.1164 0.113 Uiso 1 1 calc R . . H8B H 1.1006 0.0965 1.2165 0.113 Uiso 1 1 calc R . . H8C H 1.1777 0.1902 1.2142 0.113 Uiso 1 1 calc R . . C9 C 1.0930(3) 0.3126(2) 0.9953(3) 0.0478(8) Uani 1 1 d . . . H9A H 1.0701 0.3587 1.0429 0.072 Uiso 1 1 calc R . . H9B H 1.0896 0.3373 0.9217 0.072 Uiso 1 1 calc R . . H9C H 1.1931 0.2891 1.0315 0.072 Uiso 1 1 calc R . . C10 C 1.0167(4) 0.1389(2) 0.8874(3) 0.0518(9) Uani 1 1 d . . . H10A H 1.1084 0.1105 0.9332 0.078 Uiso 1 1 calc R . . H10B H 1.0367 0.1687 0.8233 0.078 Uiso 1 1 calc R . . H10C H 0.9389 0.0943 0.8597 0.078 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 K 0.0424(4) 0.0501(4) 0.0291(3) -0.0014(3) 0.0126(3) -0.0046(3) Si1 0.0274(4) 0.0307(4) 0.0308(4) -0.0026(3) 0.0074(3) -0.0032(3) Si2 0.0290(4) 0.0312(4) 0.0343(4) -0.0021(3) 0.0077(3) -0.0012(3) Si3 0.0258(4) 0.0339(4) 0.0282(4) -0.0014(3) 0.0050(3) -0.0002(3) O1 0.0500(14) 0.0695(17) 0.0436(13) 0.0109(12) 0.0111(11) 0.0055(12) C1 0.0249(13) 0.0269(13) 0.0337(14) -0.0048(11) 0.0065(11) -0.0013(10) C2 0.048(2) 0.0334(17) 0.088(3) 0.0021(17) 0.0172(19) -0.0035(15) C3 0.050(2) 0.063(2) 0.0401(18) -0.0020(16) 0.0024(15) -0.0238(17) C4 0.052(2) 0.062(2) 0.057(2) -0.0100(18) 0.0264(18) -0.0136(17) C5 0.0376(18) 0.0402(19) 0.105(3) 0.004(2) 0.0103(19) 0.0070(15) C6 0.075(2) 0.0390(18) 0.050(2) -0.0063(15) 0.0205(18) -0.0027(17) C7 0.058(2) 0.062(2) 0.051(2) 0.0031(17) 0.0216(17) 0.0033(18) C8 0.068(3) 0.087(3) 0.068(3) 0.021(2) 0.016(2) 0.028(2) C9 0.0287(15) 0.0472(19) 0.063(2) -0.0015(16) 0.0061(15) -0.0030(13) C10 0.0390(18) 0.056(2) 0.057(2) -0.0134(17) 0.0096(16) 0.0100(15) _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 K O1 2.630(3) 4_565 ? K C1 3.063(3) . ? K C1 3.148(3) 4_565 ? K C3 3.326(4) . ? K C4 3.233(4) 4_565 ? K C6 3.261(4) 4_565 ? K C7 3.291(4) . ? K C10 3.344(4) . ? Si1 C1 1.822(3) . ? Si1 C2 1.873(3) . ? Si1 C3 1.887(3) . ? Si1 C4 1.898(3) . ? Si2 C1 1.820(3) . ? Si2 C5 1.875(3) . ? Si2 C6 1.895(3) . ? Si2 C7 1.896(4) . ? Si3 O1 1.685(2) . ? Si3 C1 1.800(3) . ? Si3 C9 1.878(3) . ? Si3 C10 1.887(3) . ? O1 K 2.630(3) 4_566 ? O1 C8 1.394(5) . ? C1 K 3.148(3) 4_566 ? C4 K 3.233(4) 4_566 ? C6 K 3.261(4) 4_566 ? 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 K C1 126.54(7) 4_565 . ? O1 K C1 57.48(7) 4_565 4_565 ? O1 K C3 173.02(9) 4_565 . ? O1 K C4 99.01(9) 4_565 4_565 ? O1 K C6 93.66(9) 4_565 4_565 ? O1 K C7 83.79(8) 4_565 . ? O1 K C10 94.16(9) 4_565 . ? C1 K C1 175.45(10) . 4_565 ? C1 K C3 58.60(8) . . ? C1 K C3 117.20(8) 4_565 . ? C1 K C4 116.75(8) . 4_565 ? C1 K C4 59.14(8) 4_565 4_565 ? C1 K C6 121.11(8) . 4_565 ? C1 K C6 58.69(8) 4_565 4_565 ? C1 K C7 59.31(8) . . ? C1 K C7 121.20(8) 4_565 . ? C1 K C10 58.43(8) . . ? C1 K C10 124.97(8) 4_565 . ? C3 K C4 74.02(9) . 4_565 ? C3 K C6 86.42(10) . 4_565 ? C3 K C7 96.39(9) . . ? C3 K C10 92.74(9) . . ? C4 K C6 92.40(10) 4_565 4_565 ? C4 K C7 90.23(10) 4_565 . ? C4 K C10 165.37(10) 4_565 . ? C6 K C7 176.60(10) 4_565 . ? C6 K C10 80.37(9) 4_565 . ? C7 K C10 97.53(9) . . ? C1 Si1 C2 114.43(14) . . ? C1 Si1 C3 115.42(14) . . ? C1 Si1 C4 115.72(14) . . ? C2 Si1 C3 103.77(18) . . ? C2 Si1 C4 102.72(18) . . ? C3 Si1 C4 103.09(17) . . ? C1 Si2 C5 114.60(15) . . ? C1 Si2 C6 115.54(14) . . ? C1 Si2 C7 115.93(15) . . ? C5 Si2 C6 103.35(19) . . ? C5 Si2 C7 102.60(18) . . ? C6 Si2 C7 103.04(17) . . ? O1 Si3 C1 107.74(13) . . ? O1 Si3 C9 104.86(15) . . ? O1 Si3 C10 107.79(15) . . ? C1 Si3 C9 115.69(14) . . ? C1 Si3 C10 116.59(14) . . ? C9 Si3 C10 103.35(16) . . ? K O1 Si3 104.84(11) 4_566 . ? K O1 C8 127.7(2) 4_566 . ? Si3 O1 C8 122.8(3) . . ? K C1 K 174.59(10) . 4_566 ? K C1 Si1 93.10(10) . . ? K C1 Si1 88.17(10) 4_566 . ? K C1 Si2 91.83(11) . . ? K C1 Si2 92.05(10) 4_566 . ? K C1 Si3 90.51(10) . . ? K C1 Si3 84.30(10) 4_566 . ? Si1 C1 Si2 120.41(14) . . ? Si1 C1 Si3 119.77(15) . . ? Si2 C1 Si3 119.52(14) . . ? K C3 Si1 83.98(11) . . ? K C4 Si1 84.40(12) 4_566 . ? K C6 Si2 87.26(12) 4_566 . ? K C7 Si2 83.67(14) . . ? K C10 Si3 80.78(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.869 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.069 #===END