Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jonathan Steed' _publ_contact_author_address ; Department of Chemistry University of Durham University Science Laboratories South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email JON.STEED@DUR.AC.UK _publ_section_title ; Hypervalent hydridosilicates: synthesis, structure and unconventional hydrogen bonding ; loop_ _publ_author_name 'Jonathan Steed' 'Mike Bearpark' 'G. Sean McGrady' 'Paul D. Prince' data_12.CIF _database_code_depnum_ccdc_archive 'CCDC 659284' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70.5 H91 F6.5 K2 O14 Si2' _chemical_formula_weight 1420.32 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' O O 0.0106 0.0060 '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' F F 0.0171 0.0103 '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 C2/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 43.5927(18) _cell_length_b 9.6984(5) _cell_length_c 40.2731(18) _cell_angle_alpha 90.00 _cell_angle_beta 120.188(2) _cell_angle_gamma 90.00 _cell_volume 14717.5(12) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6004 _exptl_absorpt_coefficient_mu 0.238 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9320 _exptl_absorpt_correction_T_max 0.9540 _exptl_absorpt_process_details scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 KappaCCD _diffrn_measurement_method "'0.7o phi + omega scans 85s/o'" _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 27159 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_sigmaI/netI 0.1007 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 24.99 _reflns_number_total 12445 _reflns_number_gt 8745 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed interface to POVRay' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0001P)^2^+89.4194P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12445 _refine_ls_number_parameters 840 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1389 _refine_ls_R_factor_gt 0.0935 _refine_ls_wR_factor_ref 0.1655 _refine_ls_wR_factor_gt 0.1490 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.001 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 0.11592(3) 0.35291(10) 0.67089(3) 0.0269(2) Uani 1 1 d . . . K2 K -0.14726(3) 0.55647(10) 0.54808(3) 0.0256(2) Uani 1 1 d . . . Si1 Si -0.17397(4) 0.87570(15) 0.66009(4) 0.0351(3) Uani 1 1 d . . . Si2 Si -0.06872(3) 0.34461(13) 0.52942(4) 0.0255(3) Uani 1 1 d . . . F1 F -0.27635(10) 1.2945(4) 0.66270(12) 0.0896(13) Uani 1 1 d . . . F2 F -0.25693(9) 0.5292(3) 0.51600(10) 0.0676(10) Uani 1 1 d . A . F3 F -0.01732(8) 0.7816(4) 0.77629(9) 0.0564(9) Uani 1 1 d . . . F4 F -0.01739(9) 0.0368(3) 0.67985(9) 0.0564(9) Uani 1 1 d . A . F5 F -0.17599(9) -0.0034(3) 0.39547(9) 0.0632(10) Uani 1 1 d . A . F6 F -0.00482(8) 0.9089(3) 0.53498(9) 0.0482(8) Uani 1 1 d . A . F7 F -0.10363(12) 0.4217(5) 0.53310(13) 0.0247(11) Uani 0.50 1 d P A 1 O1 O -0.18231(8) 0.3198(3) 0.55177(9) 0.0317(8) Uani 1 1 d . A . O2 O -0.19900(8) 0.4344(3) 0.48037(9) 0.0314(8) Uani 1 1 d . A . O3 O -0.18320(8) 0.7106(3) 0.47876(9) 0.0341(8) Uani 1 1 d . A . O4 O -0.12512(8) 0.8247(3) 0.54466(9) 0.0300(8) Uani 1 1 d . A . O5 O -0.10633(8) 0.7055(3) 0.61510(9) 0.0331(8) Uani 1 1 d . A . O6 O -0.12578(8) 0.4353(3) 0.61980(9) 0.0318(8) Uani 1 1 d . A . O7 O 0.07359(10) 0.1129(4) 0.65236(11) 0.0316(10) Uiso 0.825(4) 1 d P B 1 O8 O 0.08583(12) 0.2326(4) 0.59623(13) 0.0310(10) Uiso 0.825(4) 1 d P B 1 O9 O 0.11448(11) 0.5026(4) 0.61154(12) 0.0336(10) Uiso 0.825(4) 1 d P B 1 O10 O 0.16092(11) 0.5851(4) 0.68762(14) 0.0357(11) Uiso 0.825(4) 1 d P B 1 O11 O 0.14745(11) 0.4675(4) 0.74359(12) 0.0344(10) Uiso 0.825(4) 1 d P B 1 O12 O 0.11517(11) 0.2039(4) 0.72884(12) 0.0352(11) Uiso 0.825(4) 1 d P B 1 O2SA O 0.1847(5) 0.2555(19) 0.7040(5) 0.018(4) Uiso 0.175(4) 1 d P B 2 C1 C -0.20490(13) 1.0121(5) 0.66289(13) 0.0371(12) Uani 1 1 d . . . C2 C -0.22792(16) 0.9791(7) 0.67630(18) 0.0607(18) Uani 1 1 d . . . H2 H -0.2270 0.8890 0.6860 0.073 Uiso 1 1 calc R . . C3 C -0.25208(18) 1.0727(8) 0.6761(2) 0.073(2) Uani 1 1 d . . . H3 H -0.2675 1.0476 0.6853 0.087 Uiso 1 1 calc R . . C4 C -0.25294(16) 1.2019(7) 0.66224(18) 0.0595(17) Uani 1 1 d . . . C5 C -0.23203(15) 1.2406(6) 0.64808(17) 0.0532(15) Uani 1 1 d . . . H5 H -0.2333 1.3309 0.6383 0.064 Uiso 1 1 calc R . . C6 C -0.20850(14) 1.1434(6) 0.64832(15) 0.0437(13) Uani 1 1 d . . . H6 H -0.1941 1.1689 0.6378 0.052 Uiso 1 1 calc R . . C7 C -0.19759(12) 0.7583(5) 0.61556(14) 0.0326(11) Uani 1 1 d . A . C8 C -0.22007(13) 0.6512(5) 0.61322(16) 0.0426(13) Uani 1 1 d . . . H8 H -0.2220 0.6312 0.6352 0.051 Uiso 1 1 calc R . . C9 C -0.23959(14) 0.5734(5) 0.58061(18) 0.0501(15) Uani 1 1 d . A . H9 H -0.2546 0.5013 0.5800 0.060 Uiso 1 1 calc R . . C10 C -0.23674(14) 0.6030(6) 0.54884(17) 0.0462(15) Uani 1 1 d . . . C11 C -0.21503(12) 0.7047(5) 0.54901(15) 0.0368(12) Uani 1 1 d . A . H11 H -0.2131 0.7226 0.5269 0.044 Uiso 1 1 calc R . . C8SA C 0.2058(8) 0.189(3) 0.7334(8) 0.035(7) Uiso 0.175(4) 1 d P B 2 H8S1 H 0.1914 0.1294 0.7404 0.042 Uiso 0.175(4) 1 calc PR B 2 H8S2 H 0.2184 0.2556 0.7546 0.042 Uiso 0.175(4) 1 calc PR B 2 C12 C -0.19577(12) 0.7813(5) 0.58238(14) 0.0329(12) Uani 1 1 d . . . H12 H -0.1807 0.8525 0.5826 0.039 Uiso 1 1 calc R A . C13 C -0.12405(13) 0.8507(5) 0.69729(13) 0.0342(12) Uani 1 1 d . . . C14 C -0.11274(13) 0.7502(6) 0.72612(14) 0.0409(13) Uani 1 1 d . . . H14 H -0.1302 0.6959 0.7275 0.049 Uiso 1 1 calc R . . C7SA C 0.2298(10) 0.110(4) 0.7322(11) 0.053(10) Uiso 0.175(4) 1 d P B 2 H7S1 H 0.2524 0.1037 0.7569 0.064 Uiso 0.175(4) 1 calc PR B 2 H7S2 H 0.2210 0.0176 0.7210 0.064 Uiso 0.175(4) 1 calc PR B 2 C15 C -0.07711(14) 0.7262(6) 0.75283(15) 0.0435(13) Uani 1 1 d . . . H15 H -0.0703 0.6578 0.7722 0.052 Uiso 1 1 calc R . . C16 C -0.05239(14) 0.8045(6) 0.75021(15) 0.0412(14) Uani 1 1 d . . . C17 C -0.06129(14) 0.9036(6) 0.72273(16) 0.0412(14) Uani 1 1 d . . . H17 H -0.0435 0.9566 0.7217 0.049 Uiso 1 1 calc R . . C18 C -0.09716(14) 0.9252(5) 0.69627(14) 0.0356(12) Uani 1 1 d . . . H18 H -0.1035 0.9930 0.6769 0.043 Uiso 1 1 calc R . . C19 C -0.19168(14) 0.2383(5) 0.51864(15) 0.0378(13) Uani 1 1 d . A . H19A H -0.2029 0.1513 0.5200 0.045 Uiso 1 1 calc R . . H19B H -0.1701 0.2149 0.5175 0.045 Uiso 1 1 calc R . . C20 C -0.21705(13) 0.3174(5) 0.48336(16) 0.0396(13) Uani 1 1 d . . . H20A H -0.2255 0.2584 0.4603 0.048 Uiso 1 1 calc R A . H20B H -0.2379 0.3469 0.4852 0.048 Uiso 1 1 calc R . . C21 C -0.22091(14) 0.5182(5) 0.44784(15) 0.0430(13) Uani 1 1 d . . . H21A H -0.2400 0.5612 0.4508 0.052 Uiso 1 1 calc R A . H21B H -0.2320 0.4614 0.4242 0.052 Uiso 1 1 calc R . . C22 C -0.19799(15) 0.6270(5) 0.44509(15) 0.0439(14) Uani 1 1 d . A . H22A H -0.1787 0.5835 0.4426 0.053 Uiso 1 1 calc R . . H22B H -0.2123 0.6848 0.4221 0.053 Uiso 1 1 calc R . . C23 C -0.16252(14) 0.8212(5) 0.47675(15) 0.0431(14) Uani 1 1 d . . . H23A H -0.1774 0.8790 0.4539 0.052 Uiso 1 1 calc R A . H23B H -0.1426 0.7838 0.4744 0.052 Uiso 1 1 calc R . . C24 C -0.14853(14) 0.9061(5) 0.51230(17) 0.0456(14) Uani 1 1 d . A . H24A H -0.1357 0.9872 0.5104 0.055 Uiso 1 1 calc R . . H24B H -0.1684 0.9396 0.5153 0.055 Uiso 1 1 calc R . . C25 C -0.10841(14) 0.9025(5) 0.57954(16) 0.0395(13) Uani 1 1 d . . . H25A H -0.1266 0.9430 0.5844 0.047 Uiso 1 1 calc R A . H25B H -0.0944 0.9786 0.5774 0.047 Uiso 1 1 calc R . . C26 C -0.08467(13) 0.8092(5) 0.61194(15) 0.0383(13) Uani 1 1 d . A . H26A H -0.0669 0.7662 0.6068 0.046 Uiso 1 1 calc R . . H26B H -0.0720 0.8623 0.6362 0.046 Uiso 1 1 calc R . . C27 C -0.08729(13) 0.6250(5) 0.64904(14) 0.0364(12) Uani 1 1 d . . . H27A H -0.0762 0.6857 0.6719 0.044 Uiso 1 1 calc R A . H27B H -0.0683 0.5722 0.6481 0.044 Uiso 1 1 calc R . . C28 C -0.11289(13) 0.5279(5) 0.65156(13) 0.0345(12) Uani 1 1 d . A . H28A H -0.1008 0.4760 0.6760 0.041 Uiso 1 1 calc R . . H28B H -0.1328 0.5801 0.6506 0.041 Uiso 1 1 calc R . . C29 C -0.14978(14) 0.3363(5) 0.61983(14) 0.0379(13) Uani 1 1 d . . . H29A H -0.1707 0.3833 0.6182 0.046 Uiso 1 1 calc R A . H29B H -0.1380 0.2821 0.6439 0.046 Uiso 1 1 calc R . . C30 C -0.16126(15) 0.2431(5) 0.58609(15) 0.0404(13) Uani 1 1 d . A . H30A H -0.1402 0.2048 0.5861 0.048 Uiso 1 1 calc R . . H30B H -0.1752 0.1654 0.5876 0.048 Uiso 1 1 calc R . . C31 C -0.05358(11) 0.2476(5) 0.57683(13) 0.0240(10) Uani 1 1 d . A . C32 C -0.06498(13) 0.2817(5) 0.60265(14) 0.0329(12) Uani 1 1 d . . . H32 H -0.0815 0.3549 0.5964 0.039 Uiso 1 1 calc R A . C33 C -0.05299(14) 0.2123(5) 0.63712(14) 0.0384(13) Uani 1 1 d . A . H33 H -0.0610 0.2380 0.6543 0.046 Uiso 1 1 calc R . . C34 C -0.02944(13) 0.1063(5) 0.64601(14) 0.0352(12) Uani 1 1 d . . . C37 C -0.10320(12) 0.2432(4) 0.48471(13) 0.0258(11) Uani 1 1 d . A . C38 C -0.09230(14) 0.1337(5) 0.47051(14) 0.0381(13) Uani 1 1 d . . . H38 H -0.0677 0.1152 0.4815 0.046 Uiso 1 1 calc R A . C39 C -0.11676(16) 0.0511(6) 0.44059(15) 0.0449(14) Uani 1 1 d . A . H39 H -0.1089 -0.0236 0.4315 0.054 Uiso 1 1 calc R . . C40 C -0.15218(15) 0.0787(5) 0.42440(14) 0.0414(13) Uani 1 1 d . . . C5SA C 0.1998(11) 0.288(4) 0.6959(13) 0.067(11) Uiso 0.175(4) 1 d P B 2 H5S1 H 0.2085 0.3815 0.7061 0.081 Uiso 0.175(4) 1 calc PR B 2 H5S2 H 0.1876 0.2912 0.6675 0.081 Uiso 0.175(4) 1 calc PR B 2 C41 C -0.16401(14) 0.1859(5) 0.43688(14) 0.0370(13) Uani 1 1 d . A . H41 H -0.1887 0.2050 0.4251 0.044 Uiso 1 1 calc R . . C42 C -0.13963(13) 0.2667(5) 0.46699(13) 0.0303(11) Uani 1 1 d . . . H42 H -0.1480 0.3404 0.4759 0.036 Uiso 1 1 calc R A . C43 C -0.04966(12) 0.5256(5) 0.53027(12) 0.0251(10) Uani 1 1 d . A . C44 C -0.01746(12) 0.5402(5) 0.53123(13) 0.0307(11) Uani 1 1 d . . . H44 H -0.0054 0.4591 0.5308 0.037 Uiso 1 1 calc R A . C45 C -0.00201(14) 0.6669(5) 0.53271(14) 0.0371(12) Uani 1 1 d . A . H45 H 0.0200 0.6729 0.5332 0.045 Uiso 1 1 calc R . . C46 C -0.01958(13) 0.7833(5) 0.53342(13) 0.0323(12) Uani 1 1 d . . . C47 C -0.05138(13) 0.7785(5) 0.53259(13) 0.0335(12) Uani 1 1 d . A . H47 H -0.0630 0.8605 0.5331 0.040 Uiso 1 1 calc R . . C48 C -0.06602(12) 0.6493(5) 0.53094(12) 0.0268(10) Uani 1 1 d . . . H48 H -0.0881 0.6448 0.5302 0.032 Uiso 1 1 calc R A . C49 C 0.0675(3) 0.0445(12) 0.6187(3) 0.042(3) Uiso 0.825(4) 1 d P B 1 H49A H 0.0486 -0.0251 0.6115 0.051 Uiso 0.825(4) 1 calc PR B 1 H49B H 0.0894 -0.0043 0.6238 0.051 Uiso 0.825(4) 1 calc PR B 1 C50 C 0.05708(16) 0.1406(7) 0.58702(18) 0.0361(15) Uiso 0.825(4) 1 d P B 1 H50A H 0.0510 0.0893 0.5632 0.043 Uiso 0.825(4) 1 calc PR B 1 H50B H 0.0359 0.1935 0.5826 0.043 Uiso 0.825(4) 1 calc PR B 1 C51 C 0.0786(2) 0.3303(8) 0.5682(2) 0.042(2) Uiso 0.825(4) 1 d P B 1 H51A H 0.0569 0.3810 0.5629 0.051 Uiso 0.825(4) 1 calc PR B 1 H51B H 0.0735 0.2821 0.5443 0.051 Uiso 0.825(4) 1 calc PR B 1 C52 C 0.10632(17) 0.4276(7) 0.57770(18) 0.0385(15) Uiso 0.825(4) 1 d P B 1 H52A H 0.1278 0.3786 0.5816 0.046 Uiso 0.825(4) 1 calc PR B 1 H52B H 0.0990 0.4927 0.5561 0.046 Uiso 0.825(4) 1 calc PR B 1 C53 C 0.1417(2) 0.6018(8) 0.6211(2) 0.0430(17) Uiso 0.825(4) 1 d P B 1 H53A H 0.1346 0.6659 0.5993 0.052 Uiso 0.825(4) 1 calc PR B 1 H53B H 0.1639 0.5550 0.6264 0.052 Uiso 0.825(4) 1 calc PR B 1 C54 C 0.14765(19) 0.6799(8) 0.6556(2) 0.0425(17) Uiso 0.825(4) 1 d P B 1 H54A H 0.1651 0.7548 0.6613 0.051 Uiso 0.825(4) 1 calc PR B 1 H54B H 0.1251 0.7218 0.6510 0.051 Uiso 0.825(4) 1 calc PR B 1 C55 C 0.16921(19) 0.6557(8) 0.7218(2) 0.0365(18) Uiso 0.825(4) 1 d P B 1 H55A H 0.1487 0.7112 0.7181 0.044 Uiso 0.825(4) 1 calc PR B 1 H55B H 0.1897 0.7181 0.7294 0.044 Uiso 0.825(4) 1 calc PR B 1 C56 C 0.17858(17) 0.5431(7) 0.7533(2) 0.0371(15) Uiso 0.825(4) 1 d P B 1 H56A H 0.1971 0.4807 0.7547 0.045 Uiso 0.825(4) 1 calc PR B 1 H56B H 0.1877 0.5873 0.7787 0.045 Uiso 0.825(4) 1 calc PR B 1 C57 C 0.1545(2) 0.3707(8) 0.7734(2) 0.047(2) Uiso 0.825(4) 1 d P B 1 H57A H 0.1609 0.4199 0.7976 0.056 Uiso 0.825(4) 1 calc PR B 1 H57B H 0.1745 0.3098 0.7780 0.056 Uiso 0.825(4) 1 calc PR B 1 C58 C 0.12118(19) 0.2865(8) 0.7606(2) 0.0481(18) Uiso 0.825(4) 1 d P B 1 H58A H 0.1240 0.2271 0.7820 0.058 Uiso 0.825(4) 1 calc PR B 1 H58B H 0.1007 0.3485 0.7532 0.058 Uiso 0.825(4) 1 calc PR B 1 C59 C 0.08615(18) 0.1109(7) 0.71688(19) 0.0403(16) Uiso 0.825(4) 1 d P B 1 H59A H 0.0639 0.1631 0.7084 0.048 Uiso 0.825(4) 1 calc PR B 1 H59B H 0.0902 0.0506 0.7386 0.048 Uiso 0.825(4) 1 calc PR B 1 C60 C 0.08323(18) 0.0260(7) 0.68464(18) 0.0401(16) Uiso 0.825(4) 1 d P B 1 H60A H 0.1062 -0.0194 0.6924 0.048 Uiso 0.825(4) 1 calc PR B 1 H60B H 0.0650 -0.0466 0.6778 0.048 Uiso 0.825(4) 1 calc PR B 1 O10A O 0.1478(7) 0.601(3) 0.6633(9) 0.063(7) Uiso 0.175(4) 1 d P B 2 C56A C 0.1768(9) 0.614(4) 0.7344(10) 0.037(8) Uiso 0.175(4) 1 d P B 2 H56C H 0.1870 0.6798 0.7555 0.044 Uiso 0.175(4) 1 d PR B 2 H56D H 0.1951 0.5508 0.7371 0.044 Uiso 0.175(4) 1 d PR B 2 C2X C -0.0213(4) 0.2737(18) 0.7423(5) 0.062(5) Uiso 0.50 1 d P . 1 C53A C 0.1179(14) 0.530(6) 0.5933(17) 0.103(16) Uiso 0.175(4) 1 d P B 2 H53C H 0.1055 0.5642 0.5665 0.124 Uiso 0.175(4) 1 calc PR B 2 H53D H 0.1398 0.4826 0.5978 0.124 Uiso 0.175(4) 1 calc PR B 2 O1SA O 0.0567(5) 0.4896(19) 0.6474(6) 0.020(4) Uiso 0.175(4) 1 d P B 2 C3SA C 0.0107(10) 0.654(4) 0.6381(11) 0.036(10) Uiso 0.175(4) 1 d P B 2 H3S1 H 0.0095 0.7319 0.6532 0.043 Uiso 0.175(4) 1 calc PR B 2 H3S2 H -0.0079 0.6664 0.6108 0.043 Uiso 0.175(4) 1 calc PR B 2 C54A C 0.1273(10) 0.645(4) 0.6191(10) 0.051(9) Uiso 0.175(4) 1 d P B 2 H54C H 0.1054 0.6956 0.6134 0.062 Uiso 0.175(4) 1 calc PR B 2 H54D H 0.1425 0.7090 0.6145 0.062 Uiso 0.175(4) 1 calc PR B 2 C1SA C 0.0297(10) 0.432(4) 0.6580(12) 0.054(10) Uiso 0.175(4) 1 d P B 2 H1S1 H 0.0184 0.3495 0.6421 0.065 Uiso 0.175(4) 1 calc PR B 2 H1S2 H 0.0428 0.4026 0.6852 0.065 Uiso 0.175(4) 1 calc PR B 2 C4SA C 0.0484(10) 0.645(4) 0.6422(11) 0.019(9) Uiso 0.175(4) 1 d P B 2 H4S1 H 0.0479 0.6805 0.6188 0.022 Uiso 0.175(4) 1 calc PR B 2 H4S2 H 0.0661 0.6981 0.6647 0.022 Uiso 0.175(4) 1 calc PR B 2 C50A C 0.0740(10) 0.033(4) 0.6257(12) 0.022(11) Uiso 0.175(4) 1 d P B 2 H50C H 0.0484 0.0456 0.6166 0.026 Uiso 0.175(4) 1 calc PR B 2 H50D H 0.0763 -0.0483 0.6123 0.026 Uiso 0.175(4) 1 calc PR B 2 C58A C 0.1426(8) 0.394(3) 0.7717(7) 0.016(6) Uiso 0.175(4) 1 d P B 2 H58C H 0.1508 0.3647 0.7985 0.019 Uiso 0.175(4) 1 calc PR B 2 H58D H 0.1197 0.4436 0.7619 0.019 Uiso 0.175(4) 1 calc PR B 2 C2SA C 0.0053(9) 0.517(3) 0.6535(10) 0.036(8) Uiso 0.175(4) 1 d P B 2 H2S1 H 0.0064 0.5320 0.6783 0.043 Uiso 0.175(4) 1 calc PR B 2 H2S2 H -0.0183 0.4779 0.6351 0.043 Uiso 0.175(4) 1 calc PR B 2 C3X C -0.0377(3) 0.3802(12) 0.7324(3) 0.042(3) Uiso 0.50 1 d P C 1 O9A O 0.0961(7) 0.436(3) 0.5978(7) 0.062(7) Uiso 0.175(4) 1 d P B 2 O7A O 0.0946(6) 0.118(3) 0.6870(7) 0.055(6) Uiso 0.175(4) 1 d P B 2 O11A O 0.1529(6) 0.557(2) 0.7327(6) 0.049(6) Uiso 0.175(4) 1 d P B 2 O12A O 0.1384(6) 0.280(2) 0.7487(6) 0.048(6) Uiso 0.175(4) 1 d P B 2 C49A C 0.0910(10) 0.006(4) 0.6637(11) 0.060(10) Uiso 0.175(4) 1 d P B 2 H49C H 0.1150 -0.0294 0.6715 0.072 Uiso 0.175(4) 1 calc PR B 2 H49D H 0.0780 -0.0678 0.6684 0.072 Uiso 0.175(4) 1 calc PR B 2 O1S O 0.05847(13) 0.4946(5) 0.66183(15) 0.0404(13) Uiso 0.825(4) 1 d P B 1 O2S O 0.1738(2) 0.2049(9) 0.6923(2) 0.107(3) Uiso 0.825(4) 1 d P B 1 C4S C 0.0551(3) 0.6269(11) 0.6471(3) 0.049(4) Uiso 0.825(4) 1 d P B 1 H4S3 H 0.0564 0.6245 0.6233 0.059 Uiso 0.825(4) 1 calc PR B 1 H4S4 H 0.0745 0.6866 0.6660 0.059 Uiso 0.825(4) 1 calc PR B 1 C5S C 0.1938(2) 0.2351(10) 0.6738(3) 0.079(3) Uiso 0.825(4) 1 d P B 1 H5S3 H 0.2009 0.3333 0.6775 0.095 Uiso 0.825(4) 1 calc PR B 1 H5S4 H 0.1793 0.2170 0.6458 0.095 Uiso 0.825(4) 1 calc PR B 1 C6S C 0.2254(2) 0.1468(10) 0.6907(3) 0.076(3) Uiso 0.825(4) 1 d P B 1 H6S1 H 0.2473 0.2023 0.7052 0.092 Uiso 0.825(4) 1 calc PR B 1 H6S2 H 0.2269 0.0934 0.6707 0.092 Uiso 0.825(4) 1 calc PR B 1 C7S C 0.2202(3) 0.0533(12) 0.7171(3) 0.090(3) Uiso 0.825(4) 1 d P B 1 H7S3 H 0.2199 -0.0440 0.7095 0.108 Uiso 0.825(4) 1 calc PR B 1 H7S4 H 0.2399 0.0650 0.7438 0.108 Uiso 0.825(4) 1 calc PR B 1 C8S C 0.1869(3) 0.0869(13) 0.7148(4) 0.124(4) Uiso 0.825(4) 1 d P B 1 H8S3 H 0.1699 0.0098 0.7031 0.149 Uiso 0.825(4) 1 calc PR B 1 H8S4 H 0.1906 0.1042 0.7408 0.149 Uiso 0.825(4) 1 calc PR B 1 C1S C 0.02294(17) 0.4358(7) 0.6383(2) 0.0390(17) Uiso 0.825(4) 1 d P B 1 H1S3 H 0.0201 0.3496 0.6497 0.047 Uiso 0.825(4) 1 calc PR B 1 H1S4 H 0.0177 0.4171 0.6118 0.047 Uiso 0.825(4) 1 calc PR B 1 C2S C -0.00060(18) 0.5513(7) 0.6392(2) 0.0335(16) Uiso 0.825(4) 1 d P B 1 H2S3 H -0.0023 0.5461 0.6628 0.040 Uiso 0.825(4) 1 calc PR B 1 H2S4 H -0.0248 0.5468 0.6165 0.040 Uiso 0.825(4) 1 calc PR B 1 C3S C 0.0188(2) 0.6831(8) 0.6388(2) 0.035(2) Uiso 0.825(4) 1 d P B 1 H3S3 H 0.0214 0.7488 0.6589 0.042 Uiso 0.825(4) 1 calc PR B 1 H3S4 H 0.0061 0.7292 0.6134 0.042 Uiso 0.825(4) 1 calc PR B 1 C4SI C -0.03022(12) 0.1373(4) 0.58720(14) 0.0280(11) Uani 1 1 d . . . H4SI H -0.0222 0.1097 0.5702 0.034 Uiso 1 1 calc R A . C5SI C -0.01821(12) 0.0661(5) 0.62133(14) 0.0345(12) Uani 1 1 d . A . H5SI H -0.0024 -0.0096 0.6275 0.041 Uiso 1 1 calc R . . H1SI H -0.1855(12) 0.773(5) 0.6831(14) 0.050 Uiso 1 1 d . . . H2SI H -0.1631(12) 0.983(5) 0.6367(14) 0.050 Uiso 1 1 d . . . H3SI H -0.0382(12) 0.274(5) 0.5254(14) 0.050 Uiso 1 1 d . . . C1X C -0.0144(5) 0.2684(19) 0.7574(5) 0.073(6) Uiso 0.50 1 d P . 1 C5X C -0.0251(4) 0.4190(18) 0.7525(5) 0.081(5) Uiso 0.50 1 d P . 1 C6X C -0.0141(3) 0.4853(14) 0.7374(4) 0.069(4) Uiso 0.50 1 d P . 1 C59A C 0.1150(11) 0.196(4) 0.7530(13) 0.070(11) Uiso 0.175(4) 1 d P B 2 H59C H 0.0924 0.2448 0.7451 0.084 Uiso 0.175(4) 1 calc PR B 2 H59D H 0.1254 0.1656 0.7800 0.084 Uiso 0.175(4) 1 calc PR B 2 C51A C 0.0661(10) 0.233(4) 0.5810(11) 0.051(9) Uiso 0.175(4) 1 d P B 2 H51C H 0.0617 0.1661 0.5605 0.062 Uiso 0.175(4) 1 calc PR B 2 H51D H 0.0431 0.2396 0.5805 0.062 Uiso 0.175(4) 1 calc PR B 2 C60A C 0.1094(9) 0.075(3) 0.7267(9) 0.042(8) Uiso 0.175(4) 1 d P B 2 H60C H 0.1324 0.0285 0.7354 0.050 Uiso 0.175(4) 1 calc PR B 2 H60D H 0.0932 0.0081 0.7285 0.050 Uiso 0.175(4) 1 calc PR B 2 O8A O 0.0870(6) 0.157(2) 0.6145(6) 0.049(6) Uiso 0.175(4) 1 d P B 2 C55A C 0.1553(11) 0.705(4) 0.6864(12) 0.073(12) Uiso 0.175(4) 1 d P B 2 H55C H 0.1337 0.7554 0.6815 0.088 Uiso 0.175(4) 1 calc PR B 2 H55D H 0.1719 0.7698 0.6845 0.088 Uiso 0.175(4) 1 calc PR B 2 C52A C 0.0681(7) 0.352(3) 0.5663(7) 0.012(6) Uiso 0.175(4) 1 d P B 2 H52C H 0.0450 0.4009 0.5549 0.014 Uiso 0.175(4) 1 calc PR B 2 H52D H 0.0741 0.3368 0.5460 0.014 Uiso 0.175(4) 1 calc PR B 2 C57A C 0.1710(12) 0.491(5) 0.7703(13) 0.077(12) Uiso 0.175(4) 1 d P B 2 H57C H 0.1798 0.5604 0.7910 0.093 Uiso 0.175(4) 1 calc PR B 2 H57D H 0.1914 0.4358 0.7733 0.093 Uiso 0.175(4) 1 calc PR B 2 C6SA C 0.2303(9) 0.186(3) 0.7116(10) 0.045(8) Uiso 0.175(4) 1 d P B 2 H6S3 H 0.2295 0.1358 0.6898 0.054 Uiso 0.175(4) 1 calc PR B 2 H6S4 H 0.2529 0.2382 0.7247 0.054 Uiso 0.175(4) 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 0.0331(6) 0.0261(6) 0.0240(5) 0.0042(5) 0.0162(5) 0.0027(5) K2 0.0294(5) 0.0186(5) 0.0300(6) -0.0003(4) 0.0159(5) -0.0010(4) Si1 0.0383(8) 0.0381(9) 0.0259(7) 0.0032(6) 0.0138(7) -0.0096(7) Si2 0.0296(7) 0.0238(7) 0.0294(7) 0.0030(6) 0.0194(6) 0.0046(6) F1 0.075(3) 0.094(3) 0.094(3) -0.005(3) 0.039(3) 0.024(2) F2 0.054(2) 0.052(2) 0.074(3) -0.0351(19) 0.015(2) -0.0053(17) F3 0.0390(18) 0.078(2) 0.045(2) -0.0136(18) 0.0154(17) -0.0033(17) F4 0.067(2) 0.050(2) 0.0391(19) 0.0209(16) 0.0164(18) -0.0021(17) F5 0.076(2) 0.055(2) 0.043(2) -0.0123(17) 0.0180(19) -0.0209(19) F6 0.061(2) 0.0320(17) 0.064(2) -0.0132(15) 0.0408(19) -0.0183(15) F7 0.027(3) 0.024(3) 0.028(3) 0.002(2) 0.017(2) 0.004(2) O1 0.043(2) 0.0202(17) 0.039(2) -0.0037(15) 0.0253(18) -0.0041(15) O2 0.0263(17) 0.0303(19) 0.0328(19) -0.0020(16) 0.0112(16) 0.0006(15) O3 0.039(2) 0.0268(19) 0.033(2) 0.0036(16) 0.0158(17) 0.0000(16) O4 0.0300(18) 0.0175(17) 0.041(2) -0.0004(15) 0.0165(17) 0.0000(14) O5 0.0352(19) 0.0305(19) 0.036(2) -0.0033(16) 0.0195(17) -0.0051(16) O6 0.041(2) 0.0276(18) 0.0348(19) -0.0020(16) 0.0245(17) -0.0042(16) C1 0.038(3) 0.044(3) 0.019(3) 0.001(2) 0.006(2) -0.006(3) C2 0.066(4) 0.066(4) 0.061(4) 0.022(3) 0.040(4) 0.009(4) C3 0.069(5) 0.091(6) 0.081(5) 0.020(4) 0.055(4) 0.016(4) C4 0.046(4) 0.070(5) 0.052(4) -0.005(4) 0.017(3) 0.013(3) C5 0.053(4) 0.043(4) 0.049(4) -0.004(3) 0.015(3) -0.007(3) C6 0.044(3) 0.044(3) 0.036(3) -0.003(3) 0.015(3) -0.005(3) C7 0.028(3) 0.026(3) 0.040(3) 0.003(2) 0.014(2) -0.001(2) C8 0.037(3) 0.034(3) 0.048(3) 0.006(3) 0.014(3) -0.002(3) C9 0.039(3) 0.024(3) 0.070(4) -0.006(3) 0.015(3) -0.008(3) C10 0.032(3) 0.038(3) 0.049(4) -0.016(3) 0.006(3) 0.007(3) C11 0.027(3) 0.039(3) 0.039(3) -0.013(3) 0.013(3) 0.005(2) C12 0.021(2) 0.033(3) 0.039(3) -0.003(2) 0.011(2) 0.002(2) C13 0.039(3) 0.041(3) 0.025(3) -0.008(2) 0.017(2) -0.009(3) C14 0.036(3) 0.057(4) 0.028(3) -0.004(3) 0.014(3) -0.011(3) C15 0.042(3) 0.052(4) 0.027(3) -0.001(3) 0.011(3) -0.002(3) C16 0.038(3) 0.051(4) 0.035(3) -0.018(3) 0.019(3) -0.005(3) C17 0.044(3) 0.047(3) 0.048(3) -0.025(3) 0.034(3) -0.018(3) C18 0.051(3) 0.033(3) 0.030(3) -0.013(2) 0.026(3) -0.012(3) C19 0.045(3) 0.025(3) 0.056(4) -0.015(3) 0.034(3) -0.013(2) C20 0.037(3) 0.033(3) 0.053(4) -0.020(3) 0.025(3) -0.016(2) C21 0.040(3) 0.038(3) 0.036(3) -0.009(3) 0.009(3) 0.006(3) C22 0.052(3) 0.039(3) 0.033(3) 0.008(3) 0.016(3) 0.015(3) C23 0.042(3) 0.037(3) 0.043(3) 0.015(3) 0.017(3) 0.001(3) C24 0.042(3) 0.024(3) 0.068(4) 0.014(3) 0.026(3) 0.005(3) C25 0.045(3) 0.028(3) 0.059(4) -0.016(3) 0.036(3) -0.014(3) C26 0.037(3) 0.041(3) 0.041(3) -0.017(3) 0.023(3) -0.020(3) C27 0.032(3) 0.040(3) 0.035(3) -0.017(3) 0.016(3) -0.006(2) C28 0.041(3) 0.041(3) 0.023(3) 0.000(2) 0.017(2) 0.008(2) C29 0.053(3) 0.034(3) 0.039(3) 0.004(2) 0.032(3) -0.002(3) C30 0.055(3) 0.022(3) 0.055(4) 0.003(3) 0.035(3) -0.004(3) C31 0.023(2) 0.024(3) 0.026(3) -0.002(2) 0.012(2) -0.004(2) C32 0.035(3) 0.033(3) 0.036(3) -0.002(2) 0.022(3) 0.000(2) C33 0.049(3) 0.043(3) 0.029(3) 0.004(3) 0.024(3) 0.002(3) C34 0.039(3) 0.030(3) 0.029(3) 0.010(2) 0.011(3) -0.007(2) C37 0.038(3) 0.021(2) 0.027(3) 0.007(2) 0.023(2) 0.003(2) C38 0.046(3) 0.034(3) 0.041(3) -0.006(3) 0.027(3) 0.005(3) C39 0.066(4) 0.036(3) 0.038(3) -0.008(3) 0.030(3) 0.002(3) C40 0.056(4) 0.035(3) 0.025(3) -0.005(2) 0.014(3) -0.014(3) C41 0.043(3) 0.038(3) 0.034(3) 0.010(2) 0.022(3) -0.005(3) C42 0.039(3) 0.028(3) 0.032(3) 0.004(2) 0.023(3) 0.002(2) C43 0.031(3) 0.028(3) 0.020(2) 0.004(2) 0.016(2) 0.006(2) C44 0.038(3) 0.030(3) 0.030(3) 0.001(2) 0.021(2) 0.009(2) C45 0.041(3) 0.037(3) 0.039(3) -0.005(2) 0.024(3) -0.005(3) C46 0.044(3) 0.026(3) 0.028(3) -0.004(2) 0.018(3) -0.010(2) C47 0.041(3) 0.031(3) 0.031(3) -0.002(2) 0.020(3) 0.002(2) C48 0.031(3) 0.026(3) 0.025(2) 0.002(2) 0.016(2) 0.002(2) C4SI 0.026(3) 0.019(2) 0.038(3) 0.000(2) 0.015(2) -0.001(2) C5SI 0.027(3) 0.024(3) 0.043(3) 0.010(2) 0.011(3) 0.003(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 O1SA 2.620(18) . ? K1 O2S 2.644(8) . ? K1 O7A 2.67(2) . ? K1 O1S 2.716(5) . ? K1 O8A 2.73(2) . ? K1 O9A 2.74(2) . ? K1 O12 2.759(4) . ? K1 O11 2.766(4) . ? K1 O2SA 2.764(17) . ? K1 O9 2.770(5) . ? K1 O7 2.827(4) . ? K1 O10 2.836(4) . ? K2 F7 2.616(4) . ? K2 O5 2.777(3) . ? K2 O2 2.782(3) . ? K2 O4 2.802(3) . ? K2 O1 2.802(3) . ? K2 O6 2.808(3) . ? K2 O3 2.843(3) . ? K2 C11 3.303(4) . ? K2 C19 3.517(5) . ? Si1 C7 1.928(5) . ? Si1 C1 1.933(5) . ? Si1 C13 1.939(5) . ? Si2 F7 1.767(4) . ? Si2 C31 1.923(4) . ? Si2 C43 1.935(5) . ? Si2 C37 1.936(5) . ? F1 C4 1.366(7) . ? F2 C10 1.366(6) . ? F3 C16 1.369(6) . ? F4 C34 1.366(5) . ? F5 C40 1.361(6) . ? F6 C46 1.364(5) . ? O1 C19 1.422(5) . ? O1 C30 1.425(6) . ? O2 C20 1.420(5) . ? O2 C21 1.425(6) . ? O3 C22 1.426(6) . ? O3 C23 1.429(6) . ? O4 C24 1.423(6) . ? O4 C25 1.429(6) . ? O5 C27 1.424(6) . ? O5 C26 1.429(5) . ? O6 C29 1.421(5) . ? O6 C28 1.427(5) . ? O7 C49 1.409(11) . ? O7 C60 1.424(7) . ? O8 C51 1.382(9) . ? O8 C50 1.427(8) . ? O9 C53 1.423(8) . ? O9 C52 1.423(8) . ? O10 C55 1.410(8) . ? O10 C54 1.446(9) . ? O11 C56 1.413(8) . ? O11 C57 1.432(8) . ? O12 C58 1.419(8) . ? O12 C59 1.426(7) . ? O2SA C5SA 0.93(4) . ? O2SA C8SA 1.25(3) . ? C1 C6 1.377(7) . ? C1 C2 1.395(7) . ? C2 C3 1.387(8) . ? C3 C4 1.364(9) . ? C4 C5 1.349(8) . ? C5 C6 1.390(8) . ? C7 C12 1.396(6) . ? C7 C8 1.398(7) . ? C8 C9 1.377(7) . ? C9 C10 1.376(8) . ? C10 C11 1.364(7) . ? C11 C12 1.389(7) . ? C8SA C7SA 1.32(4) . ? C13 C18 1.395(6) . ? C13 C14 1.402(7) . ? C14 C15 1.394(7) . ? C7SA C6SA 1.12(4) . ? C15 C16 1.365(7) . ? C16 C17 1.367(7) . ? C17 C18 1.396(7) . ? C19 C20 1.500(7) . ? C21 C22 1.495(7) . ? C23 C24 1.490(7) . ? C25 C26 1.494(7) . ? C27 C28 1.502(7) . ? C29 C30 1.493(7) . ? C31 C4SI 1.388(6) . ? C31 C32 1.399(6) . ? C32 C33 1.387(6) . ? C33 C34 1.367(7) . ? C34 C5SI 1.367(7) . ? C37 C42 1.394(6) . ? C37 C38 1.398(6) . ? C38 C39 1.392(7) . ? C39 C40 1.367(7) . ? C40 C41 1.364(7) . ? C5SA C6SA 1.51(5) . ? C41 C42 1.385(7) . ? C43 C44 1.392(6) . ? C43 C48 1.403(6) . ? C44 C45 1.388(7) . ? C45 C46 1.373(7) . ? C46 C47 1.370(6) . ? C47 C48 1.392(6) . ? C49 C50 1.456(12) . ? C51 C52 1.425(10) . ? C53 C54 1.488(10) . ? C55 C56 1.566(9) . ? C57 C58 1.512(10) . ? C59 C60 1.488(9) . ? O10A C55A 1.30(5) . ? O10A C54A 1.60(4) . ? C56A O11A 1.15(4) . ? C56A C55A 1.89(5) . ? C56A C57A 1.99(5) . ? C2X C1X 0.53(2) . ? C2X C3X 1.204(18) . ? C2X C5X 1.50(2) . ? C2X C1X 1.553(13) 2_556 ? C2X C2X 1.64(3) 2_556 ? C53A O9A 1.40(6) . ? C53A C54A 1.44(6) . ? O1SA C1SA 1.54(4) . ? O1SA C4SA 1.54(4) . ? C3SA C2SA 1.53(5) . ? C3SA C4SA 1.57(5) . ? C1SA C2SA 1.28(4) . ? C50A C49A 1.35(5) . ? C50A O8A 1.50(5) . ? C58A O12A 1.40(3) . ? C58A C57A 1.58(5) . ? C3X C5X 0.807(17) . ? C3X C6X 1.389(17) . ? C3X C1X 1.48(2) . ? O9A C52A 1.48(4) . ? O7A C49A 1.39(4) . ? O7A C60A 1.45(4) . ? O11A C57A 1.46(5) . ? O12A C59A 1.38(5) . ? O1S C4S 1.389(11) . ? O1S C1S 1.465(8) . ? O2S C8S 1.392(12) . ? O2S C5S 1.434(10) . ? C4S C3S 1.545(11) . ? C5S C6S 1.465(12) . ? C6S C7S 1.498(13) . ? C7S C8S 1.444(13) . ? C1S C2S 1.532(9) . ? C2S C3S 1.538(10) . ? C4SI C5SI 1.384(6) . ? C1X C5X 1.52(2) . ? C1X C2X 1.553(13) 2_556 ? C1X C1X 1.64(3) 2_556 ? C5X C6X 1.141(18) . ? C5X C6X 1.67(2) 2_556 ? C6X C6X 1.13(2) 2_556 ? C6X C5X 1.67(2) 2_556 ? C59A C60A 1.52(5) . ? C51A C52A 1.33(4) . ? C51A O8A 1.40(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1SA K1 O2S 177.1(5) . . ? O1SA K1 O7A 96.9(6) . . ? O2S K1 O7A 81.3(5) . . ? O1SA K1 O1S 11.6(4) . . ? O2S K1 O1S 169.6(2) . . ? O7A K1 O1S 93.1(5) . . ? O1SA K1 O8A 95.3(6) . . ? O2S K1 O8A 81.9(5) . . ? O7A K1 O8A 62.3(7) . . ? O1S K1 O8A 103.4(5) . . ? O1SA K1 O9A 75.1(7) . . ? O2S K1 O9A 104.0(5) . . ? O7A K1 O9A 123.5(8) . . ? O1S K1 O9A 86.3(5) . . ? O8A K1 O9A 63.0(8) . . ? O1SA K1 O12 98.1(4) . . ? O2S K1 O12 81.70(19) . . ? O7A K1 O12 36.1(5) . . ? O1S K1 O12 88.64(14) . . ? O8A K1 O12 98.2(5) . . ? O9A K1 O12 158.6(6) . . ? O1SA K1 O11 93.1(4) . . ? O2S K1 O11 89.4(2) . . ? O7A K1 O11 97.8(5) . . ? O1S K1 O11 82.68(14) . . ? O8A K1 O11 159.2(5) . . ? O9A K1 O11 137.8(6) . . ? O12 K1 O11 61.71(13) . . ? O1SA K1 O2SA 168.6(6) . . ? O2S K1 O2SA 14.2(4) . . ? O7A K1 O2SA 91.0(6) . . ? O1S K1 O2SA 160.2(4) . . ? O8A K1 O2SA 95.6(6) . . ? O9A K1 O2SA 107.4(6) . . ? O12 K1 O2SA 83.3(4) . . ? O11 K1 O2SA 77.6(4) . . ? O1SA K1 O9 80.4(4) . . ? O2S K1 O9 99.74(19) . . ? O7A K1 O9 143.1(5) . . ? O1S K1 O9 89.98(14) . . ? O8A K1 O9 81.1(5) . . ? O9A K1 O9 20.1(6) . . ? O12 K1 O9 178.29(13) . . ? O11 K1 O9 119.11(13) . . ? O2SA K1 O9 98.3(4) . . ? O1SA K1 O7 85.8(4) . . ? O2S K1 O7 91.6(2) . . ? O7A K1 O7 25.5(5) . . ? O1S K1 O7 86.89(13) . . ? O8A K1 O7 40.7(5) . . ? O9A K1 O7 98.4(6) . . ? O12 K1 O7 60.55(12) . . ? O11 K1 O7 121.41(12) . . ? O2SA K1 O7 104.6(4) . . ? O9 K1 O7 118.36(13) . . ? O1SA K1 O10 97.0(4) . . ? O2S K1 O10 85.5(2) . . ? O7A K1 O10 155.1(5) . . ? O1S K1 O10 96.37(14) . . ? O8A K1 O10 136.3(5) . . ? O9A K1 O10 80.2(6) . . ? O12 K1 O10 121.05(13) . . ? O11 K1 O10 60.87(13) . . ? O2SA K1 O10 72.8(4) . . ? O9 K1 O10 60.13(13) . . ? O7 K1 O10 176.33(11) . . ? F7 K2 O5 107.33(13) . . ? F7 K2 O2 83.48(12) . . ? O5 K2 O2 169.11(10) . . ? F7 K2 O4 98.30(12) . . ? O5 K2 O4 59.73(9) . . ? O2 K2 O4 118.45(10) . . ? F7 K2 O1 94.71(12) . . ? O5 K2 O1 118.39(10) . . ? O2 K2 O1 60.56(9) . . ? O4 K2 O1 166.76(9) . . ? F7 K2 O6 97.07(12) . . ? O5 K2 O6 59.93(9) . . ? O2 K2 O6 121.12(10) . . ? O4 K2 O6 119.62(10) . . ? O1 K2 O6 60.74(10) . . ? F7 K2 O3 98.16(12) . . ? O5 K2 O3 116.62(10) . . ? O2 K2 O3 59.10(10) . . ? O4 K2 O3 59.80(10) . . ? O1 K2 O3 115.90(10) . . ? O6 K2 O3 164.65(9) . . ? F7 K2 C11 168.05(14) . . ? O5 K2 C11 84.47(11) . . ? O2 K2 C11 84.68(11) . . ? O4 K2 C11 85.90(11) . . ? O1 K2 C11 80.86(12) . . ? O6 K2 C11 90.46(12) . . ? O3 K2 C11 74.21(12) . . ? F7 K2 C19 79.91(13) . . ? O5 K2 C19 139.45(11) . . ? O2 K2 C19 42.15(11) . . ? O4 K2 C19 160.55(12) . . ? O1 K2 C19 22.60(10) . . ? O6 K2 C19 79.73(11) . . ? O3 K2 C19 101.08(12) . . ? C11 K2 C19 92.38(12) . . ? C7 Si1 C1 113.4(2) . . ? C7 Si1 C13 120.8(2) . . ? C1 Si1 C13 125.8(2) . . ? F7 Si2 C31 90.2(2) . . ? F7 Si2 C43 89.7(2) . . ? C31 Si2 C43 119.76(19) . . ? F7 Si2 C37 89.7(2) . . ? C31 Si2 C37 113.16(19) . . ? C43 Si2 C37 127.08(19) . . ? Si2 F7 K2 170.8(3) . . ? C19 O1 C30 111.1(4) . . ? C19 O1 K2 108.2(2) . . ? C30 O1 K2 112.1(3) . . ? C20 O2 C21 113.0(4) . . ? C20 O2 K2 117.9(3) . . ? C21 O2 K2 119.8(3) . . ? C22 O3 C23 111.7(4) . . ? C22 O3 K2 113.4(3) . . ? C23 O3 K2 113.5(3) . . ? C24 O4 C25 112.6(4) . . ? C24 O4 K2 117.0(3) . . ? C25 O4 K2 117.4(3) . . ? C27 O5 C26 112.3(4) . . ? C27 O5 K2 115.3(3) . . ? C26 O5 K2 114.2(3) . . ? C29 O6 C28 112.5(3) . . ? C29 O6 K2 114.8(3) . . ? C28 O6 K2 115.8(3) . . ? C49 O7 C60 115.2(6) . . ? C49 O7 K1 115.0(5) . . ? C60 O7 K1 113.1(4) . . ? C51 O8 C50 114.0(5) . . ? C51 O8 K1 112.0(4) . . ? C50 O8 K1 114.1(3) . . ? C53 O9 C52 112.2(5) . . ? C53 O9 K1 117.9(4) . . ? C52 O9 K1 116.4(4) . . ? C55 O10 C54 110.6(5) . . ? C55 O10 K1 115.1(4) . . ? C54 O10 K1 112.0(4) . . ? C56 O11 C57 109.7(5) . . ? C56 O11 K1 113.5(3) . . ? C57 O11 K1 114.1(4) . . ? C58 O12 C59 113.1(5) . . ? C58 O12 K1 113.1(4) . . ? C59 O12 K1 115.6(4) . . ? C5SA O2SA C8SA 101(3) . . ? C5SA O2SA K1 120(3) . . ? C8SA O2SA K1 137.3(16) . . ? C6 C1 C2 115.3(5) . . ? C6 C1 Si1 122.8(4) . . ? C2 C1 Si1 121.6(4) . . ? C3 C2 C1 122.6(6) . . ? C4 C3 C2 117.9(6) . . ? C5 C4 C3 122.9(6) . . ? C5 C4 F1 119.4(6) . . ? C3 C4 F1 117.7(6) . . ? C4 C5 C6 117.5(6) . . ? C1 C6 C5 123.7(5) . . ? C12 C7 C8 115.5(5) . . ? C12 C7 Si1 122.3(4) . . ? C8 C7 Si1 122.0(4) . . ? C9 C8 C7 123.2(5) . . ? C10 C9 C8 118.1(5) . . ? C11 C10 F2 119.4(5) . . ? C11 C10 C9 122.2(5) . . ? F2 C10 C9 118.4(5) . . ? C10 C11 C12 118.2(5) . . ? C10 C11 K2 107.9(3) . . ? C12 C11 K2 97.7(3) . . ? O2SA C8SA C7SA 119(3) . . ? C11 C12 C7 122.9(5) . . ? C18 C13 C14 115.7(5) . . ? C18 C13 Si1 123.1(4) . . ? C14 C13 Si1 121.2(4) . . ? C15 C14 C13 123.1(5) . . ? C6SA C7SA C8SA 87(3) . . ? C16 C15 C14 117.7(5) . . ? C15 C16 C17 122.7(5) . . ? C15 C16 F3 118.1(5) . . ? C17 C16 F3 119.2(5) . . ? C16 C17 C18 118.4(5) . . ? C13 C18 C17 122.4(5) . . ? O1 C19 C20 109.4(4) . . ? O1 C19 K2 49.20(19) . . ? C20 C19 K2 83.7(3) . . ? O2 C20 C19 108.2(4) . . ? O2 C21 C22 107.9(4) . . ? O3 C22 C21 109.3(4) . . ? O3 C23 C24 109.0(4) . . ? O4 C24 C23 109.4(4) . . ? O4 C25 C26 109.0(4) . . ? O5 C26 C25 107.8(4) . . ? O5 C27 C28 108.3(4) . . ? O6 C28 C27 107.8(3) . . ? O6 C29 C30 108.6(4) . . ? O1 C30 C29 108.9(4) . . ? C4SI C31 C32 116.1(4) . . ? C4SI C31 Si2 120.6(3) . . ? C32 C31 Si2 123.3(3) . . ? C33 C32 C31 122.2(5) . . ? C34 C33 C32 118.9(4) . . ? F4 C34 C5SI 119.0(4) . . ? F4 C34 C33 119.6(4) . . ? C5SI C34 C33 121.3(4) . . ? C42 C37 C38 116.6(4) . . ? C42 C37 Si2 123.0(3) . . ? C38 C37 Si2 120.1(4) . . ? C39 C38 C37 121.4(5) . . ? C40 C39 C38 119.3(5) . . ? F5 C40 C41 119.6(5) . . ? F5 C40 C39 119.1(5) . . ? C41 C40 C39 121.3(5) . . ? O2SA C5SA C6SA 105(4) . . ? C40 C41 C42 119.2(5) . . ? C41 C42 C37 122.1(4) . . ? C44 C43 C48 115.3(4) . . ? C44 C43 Si2 120.7(3) . . ? C48 C43 Si2 123.9(3) . . ? C45 C44 C43 123.5(4) . . ? C46 C45 C44 117.7(4) . . ? F6 C46 C47 118.7(4) . . ? F6 C46 C45 118.7(4) . . ? C47 C46 C45 122.7(5) . . ? C46 C47 C48 117.8(4) . . ? C47 C48 C43 123.0(4) . . ? O7 C49 C50 111.5(8) . . ? O8 C50 C49 109.0(6) . . ? O8 C51 C52 114.9(7) . . ? O9 C52 C51 111.4(6) . . ? O9 C53 C54 109.1(5) . . ? O10 C54 C53 108.2(6) . . ? O10 C55 C56 106.7(5) . . ? O11 C56 C55 108.3(5) . . ? O11 C57 C58 107.7(6) . . ? O12 C58 C57 108.8(6) . . ? O12 C59 C60 108.5(5) . . ? O7 C60 C59 109.0(5) . . ? C55A O10A C54A 113(3) . . ? C55A O10A K1 122(3) . . ? C54A O10A K1 108.3(18) . . ? O11A C56A C55A 101(3) . . ? O11A C56A C57A 47(2) . . ? C55A C56A C57A 148(3) . . ? C1X C2X C3X 112(4) . . ? C1X C2X C5X 82(3) . . ? C3X C2X C5X 32.5(9) . . ? C1X C2X C1X 90(3) . 2_556 ? C3X C2X C1X 117.1(18) . 2_556 ? C5X C2X C1X 106.0(16) . 2_556 ? C1X C2X C2X 71(3) . 2_556 ? C3X C2X C2X 119.8(10) . 2_556 ? C5X C2X C2X 99.0(10) . 2_556 ? C1X C2X C2X 18.8(8) 2_556 2_556 ? O9A C53A C54A 112(4) . . ? C1SA O1SA C4SA 103(2) . . ? C1SA O1SA K1 117.9(17) . . ? C4SA O1SA K1 131.7(17) . . ? C2SA C3SA C4SA 106(3) . . ? C53A C54A O10A 113(4) . . ? C2SA C1SA O1SA 115(3) . . ? O1SA C4SA C3SA 103(3) . . ? C49A C50A O8A 115(3) . . ? O12A C58A C57A 107(2) . . ? C1SA C2SA C3SA 109(3) . . ? C5X C3X C2X 94.2(19) . . ? C5X C3X C6X 55.2(15) . . ? C2X C3X C6X 108.0(13) . . ? C5X C3X C1X 76.7(17) . . ? C2X C3X C1X 19.3(11) . . ? C6X C3X C1X 103.5(12) . . ? C53A O9A C52A 124(3) . . ? C53A O9A K1 118(3) . . ? C52A O9A K1 116.1(16) . . ? C49A O7A C60A 111(3) . . ? C49A O7A K1 116(2) . . ? C60A O7A K1 119.6(19) . . ? C56A O11A C57A 99(3) . . ? C56A O11A K1 118(2) . . ? C57A O11A K1 111(2) . . ? C59A O12A C58A 104(3) . . ? C59A O12A K1 115(2) . . ? C58A O12A K1 113.1(15) . . ? C50A C49A O7A 115(3) . . ? C50A C49A K1 83(2) . . ? O7A C49A K1 43.2(15) . . ? C4S O1S C1S 103.6(6) . . ? C4S O1S K1 114.6(5) . . ? C1S O1S K1 119.5(4) . . ? C8S O2S C5S 110.6(8) . . ? C8S O2S K1 132.0(7) . . ? C5S O2S K1 116.8(6) . . ? O1S C4S C3S 107.2(8) . . ? O2S C5S C6S 108.1(8) . . ? C5S C6S C7S 104.1(8) . . ? C8S C7S C6S 108.9(9) . . ? O2S C8S C7S 107.1(10) . . ? O1S C1S C2S 101.7(5) . . ? C1S C2S C3S 103.2(5) . . ? C2S C3S C4S 102.3(6) . . ? C5SI C4SI C31 122.5(4) . . ? C34 C5SI C4SI 119.0(4) . . ? C2X C1X C3X 49(3) . . ? C2X C1X C5X 78(3) . . ? C3X C1X C5X 31.2(8) . . ? C2X C1X C2X 90(3) . 2_556 ? C3X C1X C2X 108.8(15) . 2_556 ? C5X C1X C2X 102.1(16) . 2_556 ? C2X C1X C1X 71(3) . 2_556 ? C3X C1X C1X 98.1(12) . 2_556 ? C5X C1X C1X 101.1(9) . 2_556 ? C2X C1X C1X 18.8(9) 2_556 2_556 ? C3X C5X C6X 89.3(19) . . ? C3X C5X C2X 53.3(15) . . ? C6X C5X C2X 104.7(15) . . ? C3X C5X C1X 72.1(17) . . ? C6X C5X C1X 115.5(16) . . ? C2X C5X C1X 20.1(9) . . ? C3X C5X C6X 122(2) . 2_556 ? C6X C5X C6X 42.6(12) . 2_556 ? C2X C5X C6X 101.0(12) . 2_556 ? C1X C5X C6X 97.5(12) . 2_556 ? C6X C6X C5X 94.5(17) 2_556 . ? C6X C6X C3X 121.3(12) 2_556 . ? C5X C6X C3X 35.5(10) . . ? C6X C6X C5X 42.9(10) 2_556 2_556 ? C5X C6X C5X 107.6(16) . 2_556 ? C3X C6X C5X 110.1(11) . 2_556 ? O12A C59A C60A 104(3) . . ? C52A C51A O8A 137(4) . . ? C52A C51A K1 91(2) . . ? O8A C51A K1 52.2(16) . . ? O7A C60A C59A 112(3) . . ? C51A O8A C50A 123(3) . . ? C51A O8A K1 104(2) . . ? C50A O8A K1 113.3(19) . . ? O10A C55A C56A 101(3) . . ? C51A C52A O9A 108(3) . . ? O11A C57A C58A 106(3) . . ? O11A C57A C56A 34.9(16) . . ? C58A C57A C56A 141(3) . . ? C7SA C6SA C5SA 114(4) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.517 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.072 # Attachment '1a.CIF' data_ppsilyl1 _database_code_depnum_ccdc_archive 'CCDC 169646' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H41 K O6 Si' _chemical_formula_weight 564.82 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 P21/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 9.3861(5) _cell_length_b 20.2252(10) _cell_length_c 16.5969(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.540(3) _cell_angle_gamma 90.00 _cell_volume 3063.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.251 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7871 _exptl_absorpt_correction_T_max 0.8846 _exptl_absorpt_process_details Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 KappaCCD _diffrn_measurement_method '1.6 phi + omega scans 6s/o' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16817 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.0999 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6802 _reflns_number_gt 4249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _computing_publication_material ? _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^)+(0.0451P)^2^+0.9529P] 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 SHELXL _refine_ls_extinction_coef 0.0013(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6802 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1095 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Si1 Si 0.83492(7) 0.13943(3) 0.17855(4) 0.02705(17) Uani 1 1 d . . . C1 C 0.6534(2) 0.16788(11) 0.20232(13) 0.0288(5) Uani 1 1 d . . . C2 C 0.5281(3) 0.12871(14) 0.18700(16) 0.0448(7) Uani 1 1 d . . . H2 H 0.5305 0.0868 0.1616 0.054 Uiso 1 1 calc R . . C3 C 0.3999(3) 0.14878(17) 0.20753(18) 0.0593(9) Uani 1 1 d . . . H3 H 0.3172 0.1203 0.1977 0.071 Uiso 1 1 calc R . . C4 C 0.3928(3) 0.21007(16) 0.24221(16) 0.0521(8) Uani 1 1 d . . . H4 H 0.3049 0.2243 0.2558 0.063 Uiso 1 1 calc R . . C5 C 0.5140(3) 0.25075(13) 0.25719(16) 0.0459(7) Uani 1 1 d . . . H5 H 0.5097 0.2933 0.2807 0.055 Uiso 1 1 calc R . . C6 C 0.6424(3) 0.22925(11) 0.23781(15) 0.0371(6) Uani 1 1 d . . . H6 H 0.7256 0.2575 0.2492 0.045 Uiso 1 1 calc R . . C7 C 0.8894(2) 0.18809(10) 0.09109(14) 0.0268(5) Uani 1 1 d . . . C8 C 1.0069(2) 0.23214(11) 0.10558(16) 0.0336(6) Uani 1 1 d . . . H8 H 1.0677 0.2356 0.1599 0.040 Uiso 1 1 calc R . . C9 C 1.0376(3) 0.27098(12) 0.04313(18) 0.0417(6) Uani 1 1 d . . . H9 H 1.1200 0.2997 0.0544 0.050 Uiso 1 1 calc R . . C10 C 0.9484(3) 0.26783(13) -0.03551(18) 0.0478(7) Uani 1 1 d . . . H10 H 0.9679 0.2951 -0.0783 0.057 Uiso 1 1 calc R . . C11 C 0.8309(3) 0.22521(13) -0.05196(17) 0.0451(7) Uani 1 1 d . . . H11 H 0.7684 0.2234 -0.1060 0.054 Uiso 1 1 calc R . . C12 C 0.8039(3) 0.18493(11) 0.01030(14) 0.0331(5) Uani 1 1 d . . . H12 H 0.7249 0.1544 -0.0024 0.040 Uiso 1 1 calc R . . C13 C 0.9514(2) 0.06863(11) 0.23955(14) 0.0291(5) Uani 1 1 d . . . C14 C 0.9127(3) 0.00236(11) 0.22502(16) 0.0369(6) Uani 1 1 d . . . H14 H 0.8277 -0.0083 0.1834 0.044 Uiso 1 1 calc R . . C15 C 0.9939(4) -0.04837(14) 0.26926(19) 0.0521(8) Uani 1 1 d . . . H15 H 0.9626 -0.0928 0.2586 0.062 Uiso 1 1 calc R . . C16 C 1.1190(4) -0.03509(16) 0.32829(19) 0.0581(9) Uani 1 1 d . . . H16 H 1.1749 -0.0701 0.3583 0.070 Uiso 1 1 calc R . . C17 C 1.1630(3) 0.02967(16) 0.34386(17) 0.0539(8) Uani 1 1 d . . . H17 H 1.2508 0.0394 0.3839 0.065 Uiso 1 1 calc R . . C18 C 1.0782(3) 0.08114(13) 0.30064(15) 0.0378(6) Uani 1 1 d . . . H18 H 1.1079 0.1256 0.3133 0.045 Uiso 1 1 calc R . . K1A K 1.0000 0.0000 0.5000 0.03169(19) Uani 1 2 d S . . O1A O 0.79958(17) 0.10626(7) 0.46317(10) 0.0345(4) Uani 1 1 d . . . C1A C 0.6872(3) 0.09080(12) 0.39181(15) 0.0356(6) Uani 1 1 d . . . H1A1 H 0.7296 0.0868 0.3427 0.043 Uiso 1 1 calc R . . H1A2 H 0.6131 0.1265 0.3812 0.043 Uiso 1 1 calc R . . O2A O 1.10051(17) 0.12968(7) 0.52583(10) 0.0363(4) Uani 1 1 d . . . C2A C 0.8666(3) 0.16772(11) 0.45236(17) 0.0389(6) Uani 1 1 d . . . H2A1 H 0.7945 0.2040 0.4481 0.047 Uiso 1 1 calc R . . H2A2 H 0.9022 0.1668 0.4008 0.047 Uiso 1 1 calc R . . O3A O 1.28190(17) 0.02527(8) 0.59221(10) 0.0361(4) Uani 1 1 d . . . C3A C 0.9927(3) 0.17886(11) 0.52580(17) 0.0392(6) Uani 1 1 d . . . H3A1 H 1.0351 0.2233 0.5225 0.047 Uiso 1 1 calc R . . H3A2 H 0.9582 0.1762 0.5777 0.047 Uiso 1 1 calc R . . C4A C 1.2276(3) 0.13971(12) 0.59077(16) 0.0369(6) Uani 1 1 d . . . H4A1 H 1.2026 0.1352 0.6453 0.044 Uiso 1 1 calc R . . H4A2 H 1.2672 0.1847 0.5869 0.044 Uiso 1 1 calc R . . C5A C 1.3391(3) 0.08887(11) 0.58227(17) 0.0376(6) Uani 1 1 d . . . H5A1 H 1.3614 0.0924 0.5270 0.045 Uiso 1 1 calc R . . H5A2 H 1.4309 0.0961 0.6249 0.045 Uiso 1 1 calc R . . C6A C 1.3836(2) -0.02660(12) 0.59362(16) 0.0371(6) Uani 1 1 d . . . H6A1 H 1.4723 -0.0189 0.6384 0.044 Uiso 1 1 calc R . . H6A2 H 1.4132 -0.0283 0.5402 0.044 Uiso 1 1 calc R . . K1B K 0.5000 0.0000 0.0000 0.0412(2) Uani 1 2 d S . . O1B O 0.30284(17) 0.09833(7) -0.06732(10) 0.0360(4) Uani 1 1 d . . . C1B C 0.3635(3) 0.15075(13) -0.10494(19) 0.0504(7) Uani 1 1 d . . . H1B1 H 0.4338 0.1760 -0.0622 0.060 Uiso 1 1 calc R . . H1B2 H 0.2848 0.1812 -0.1329 0.060 Uiso 1 1 calc R . . O2B O 0.27445(16) 0.02889(8) 0.07584(10) 0.0352(4) Uani 1 1 d . . . C2B C 0.2143(3) 0.12122(13) -0.01389(19) 0.0492(7) Uani 1 1 d . . . H2B1 H 0.1320 0.1481 -0.0458 0.059 Uiso 1 1 calc R . . H2B2 H 0.2735 0.1493 0.0304 0.059 Uiso 1 1 calc R . . O3B O 0.44095(17) -0.08404(8) 0.12266(10) 0.0376(4) Uani 1 1 d . . . C3B C 0.1567(3) 0.06325(14) 0.02326(17) 0.0447(7) Uani 1 1 d . . . H3B1 H 0.0864 0.0782 0.0556 0.054 Uiso 1 1 calc R . . H3B2 H 0.1044 0.0334 -0.0212 0.054 Uiso 1 1 calc R . . C4B C 0.2247(3) -0.02393(14) 0.11897(18) 0.0465(7) Uani 1 1 d . . . H4B1 H 0.1693 -0.0563 0.0789 0.056 Uiso 1 1 calc R . . H4B2 H 0.1588 -0.0066 0.1527 0.056 Uiso 1 1 calc R . . C5B C 0.3546(3) -0.05663(15) 0.17372(17) 0.0483(7) Uani 1 1 d . . . H5B1 H 0.4125 -0.0239 0.2123 0.058 Uiso 1 1 calc R . . H5B2 H 0.3222 -0.0919 0.2068 0.058 Uiso 1 1 calc R . . C6B C 0.5599(3) -0.12289(14) 0.16660(18) 0.0482(7) Uani 1 1 d . . . H6B1 H 0.5235 -0.1591 0.1966 0.058 Uiso 1 1 calc R . . H6B2 H 0.6282 -0.0953 0.2075 0.058 Uiso 1 1 calc R . . H1S H 0.922(2) 0.1903(10) 0.2403(14) 0.036(6) Uiso 1 1 d . . . H2S H 0.752(2) 0.0885(10) 0.1144(14) 0.035(6) 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 Si1 0.0275(3) 0.0257(3) 0.0266(3) -0.0021(3) 0.0038(3) -0.0009(3) C1 0.0325(12) 0.0337(12) 0.0180(11) 0.0000(10) 0.0015(10) 0.0028(10) C2 0.0322(13) 0.0642(18) 0.0371(15) -0.0233(13) 0.0065(11) -0.0056(13) C3 0.0309(14) 0.100(3) 0.0449(17) -0.0350(17) 0.0047(13) -0.0065(15) C4 0.0333(14) 0.090(2) 0.0297(14) -0.0097(15) 0.0003(12) 0.0228(15) C5 0.0634(19) 0.0412(14) 0.0361(15) 0.0016(12) 0.0173(14) 0.0178(14) C6 0.0499(15) 0.0315(13) 0.0331(14) 0.0045(11) 0.0161(12) 0.0032(11) C7 0.0235(11) 0.0246(11) 0.0332(13) -0.0048(10) 0.0084(10) 0.0035(9) C8 0.0255(12) 0.0346(13) 0.0419(15) -0.0047(11) 0.0101(11) 0.0017(10) C9 0.0362(14) 0.0363(14) 0.0607(19) -0.0081(13) 0.0275(14) -0.0056(11) C10 0.0648(19) 0.0434(15) 0.0464(17) 0.0015(13) 0.0358(15) -0.0047(14) C11 0.0564(17) 0.0488(16) 0.0319(14) -0.0001(12) 0.0143(13) -0.0041(14) C12 0.0367(13) 0.0342(13) 0.0298(13) -0.0035(11) 0.0106(11) -0.0024(11) C13 0.0292(12) 0.0331(12) 0.0293(13) 0.0026(10) 0.0156(10) 0.0028(10) C14 0.0411(13) 0.0332(13) 0.0423(14) 0.0051(11) 0.0217(12) 0.0053(11) C15 0.071(2) 0.0385(15) 0.0575(19) 0.0107(14) 0.0379(17) 0.0131(15) C16 0.074(2) 0.062(2) 0.0497(19) 0.0294(16) 0.0369(17) 0.0369(18) C17 0.0422(16) 0.086(2) 0.0332(15) 0.0118(15) 0.0085(13) 0.0253(16) C18 0.0354(13) 0.0480(15) 0.0322(13) 0.0037(12) 0.0120(11) 0.0058(12) K1A 0.0240(3) 0.0267(4) 0.0442(4) 0.0024(3) 0.0075(3) 0.0013(3) O1A 0.0346(9) 0.0336(9) 0.0353(10) 0.0092(7) 0.0080(8) 0.0024(7) C1A 0.0304(12) 0.0415(14) 0.0339(14) 0.0068(11) 0.0054(11) 0.0084(11) O2A 0.0336(9) 0.0326(9) 0.0425(10) 0.0025(8) 0.0084(8) 0.0022(7) C2A 0.0401(14) 0.0295(12) 0.0507(16) 0.0145(12) 0.0180(13) 0.0072(11) O3A 0.0287(8) 0.0351(9) 0.0458(10) 0.0050(8) 0.0110(8) 0.0015(7) C3A 0.0414(14) 0.0261(12) 0.0506(16) 0.0051(11) 0.0116(13) 0.0048(11) C4A 0.0355(13) 0.0347(13) 0.0389(14) 0.0025(11) 0.0055(11) -0.0084(11) C5A 0.0306(13) 0.0368(14) 0.0445(15) 0.0014(12) 0.0070(11) -0.0068(11) C6A 0.0265(12) 0.0450(14) 0.0383(14) 0.0005(12) 0.0049(11) 0.0078(11) K1B 0.0403(4) 0.0451(4) 0.0438(5) 0.0112(4) 0.0209(4) 0.0207(4) O1B 0.0343(9) 0.0315(9) 0.0389(10) -0.0041(7) 0.0022(8) 0.0061(7) C1B 0.0432(15) 0.0331(14) 0.069(2) 0.0092(14) 0.0008(15) 0.0084(12) O2B 0.0235(8) 0.0442(10) 0.0375(10) -0.0090(8) 0.0063(7) 0.0016(7) C2B 0.0409(15) 0.0481(16) 0.0551(18) -0.0098(14) 0.0039(13) 0.0236(13) O3B 0.0311(9) 0.0446(10) 0.0350(9) -0.0005(8) 0.0034(8) 0.0012(8) C3B 0.0250(12) 0.0594(17) 0.0492(17) -0.0138(14) 0.0078(12) 0.0098(12) C4B 0.0349(14) 0.0592(17) 0.0507(17) -0.0050(14) 0.0207(13) -0.0044(13) C5B 0.0450(16) 0.0644(18) 0.0383(15) 0.0015(14) 0.0155(13) -0.0043(14) C6B 0.0390(15) 0.0506(17) 0.0503(17) 0.0164(14) 0.0009(13) 0.0007(13) _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 C7 1.919(2) . ? Si1 C1 1.925(2) . ? Si1 C13 1.937(2) . ? C1 C6 1.388(3) . ? C1 C2 1.391(3) . ? C2 C3 1.386(4) . ? C3 C4 1.375(4) . ? C4 C5 1.379(4) . ? C5 C6 1.388(4) . ? C7 C12 1.394(3) . ? C7 C8 1.395(3) . ? C8 C9 1.383(4) . ? C9 C10 1.377(4) . ? C10 C11 1.376(4) . ? C11 C12 1.385(3) . ? C13 C18 1.394(3) . ? C13 C14 1.395(3) . ? C14 C15 1.382(4) . ? C15 C16 1.368(4) . ? C16 C17 1.380(4) . ? C16 K1A 3.371(3) . ? C17 C18 1.401(4) . ? C17 K1A 3.358(3) . ? K1A O3A 2.7764(16) 3_756 ? K1A O3A 2.7764(16) . ? K1A O2A 2.7863(15) 3_756 ? K1A O2A 2.7863(15) . ? K1A O1A 2.8272(15) . ? K1A O1A 2.8272(15) 3_756 ? K1A C17 3.358(3) 3_756 ? K1A C16 3.371(3) 3_756 ? O1A C2A 1.423(3) . ? O1A C1A 1.424(3) . ? C1A C6A 1.504(3) 3_756 ? O2A C3A 1.419(3) . ? O2A C4A 1.423(3) . ? C2A C3A 1.504(3) . ? O3A C6A 1.415(3) . ? O3A C5A 1.418(3) . ? C4A C5A 1.497(3) . ? C6A C1A 1.504(3) 3_756 ? K1B O2B 2.7669(15) 3_655 ? K1B O2B 2.7669(15) . ? K1B O1B 2.7677(15) . ? K1B O1B 2.7677(15) 3_655 ? K1B O3B 2.8051(17) 3_655 ? K1B O3B 2.8051(17) . ? O1B C1B 1.416(3) . ? O1B C2B 1.427(3) . ? C1B C6B 1.492(4) 3_655 ? O2B C3B 1.419(3) . ? O2B C4B 1.424(3) . ? C2B C3B 1.484(4) . ? O3B C5B 1.416(3) . ? O3B C6B 1.420(3) . ? C4B C5B 1.494(4) . ? C6B C1B 1.492(4) 3_655 ? 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 C7 Si1 C1 114.03(9) . . ? C7 Si1 C13 123.81(9) . . ? C1 Si1 C13 122.16(10) . . ? C6 C1 C2 116.3(2) . . ? C6 C1 Si1 120.75(18) . . ? C2 C1 Si1 122.91(17) . . ? C3 C2 C1 122.3(2) . . ? C4 C3 C2 119.8(3) . . ? C3 C4 C5 119.7(3) . . ? C4 C5 C6 119.7(2) . . ? C5 C6 C1 122.2(2) . . ? C12 C7 C8 116.7(2) . . ? C12 C7 Si1 120.57(17) . . ? C8 C7 Si1 122.50(18) . . ? C9 C8 C7 121.9(2) . . ? C10 C9 C8 119.8(2) . . ? C11 C10 C9 119.9(2) . . ? C10 C11 C12 119.9(3) . . ? C11 C12 C7 121.7(2) . . ? C18 C13 C14 116.4(2) . . ? C18 C13 Si1 121.82(18) . . ? C14 C13 Si1 121.83(18) . . ? C15 C14 C13 122.2(3) . . ? C16 C15 C14 120.6(3) . . ? C15 C16 C17 119.3(3) . . ? C15 C16 K1A 104.38(18) . . ? C17 C16 K1A 77.63(17) . . ? C16 C17 C18 120.0(3) . . ? C16 C17 K1A 78.71(17) . . ? C18 C17 K1A 102.78(16) . . ? C13 C18 C17 121.5(3) . . ? O3A K1A O3A 180.00(7) 3_756 . ? O3A K1A O2A 59.82(4) 3_756 3_756 ? O3A K1A O2A 120.18(4) . 3_756 ? O3A K1A O2A 120.18(4) 3_756 . ? O3A K1A O2A 59.82(4) . . ? O2A K1A O2A 180.00(2) 3_756 . ? O3A K1A O1A 61.36(4) 3_756 . ? O3A K1A O1A 118.64(4) . . ? O2A K1A O1A 119.88(4) 3_756 . ? O2A K1A O1A 60.12(4) . . ? O3A K1A O1A 118.64(4) 3_756 3_756 ? O3A K1A O1A 61.36(4) . 3_756 ? O2A K1A O1A 60.12(4) 3_756 3_756 ? O2A K1A O1A 119.88(4) . 3_756 ? O1A K1A O1A 180.0 . 3_756 ? O3A K1A C17 98.92(6) 3_756 . ? O3A K1A C17 81.08(6) . . ? O2A K1A C17 104.39(7) 3_756 . ? O2A K1A C17 75.61(7) . . ? O1A K1A C17 95.60(6) . . ? O1A K1A C17 84.40(6) 3_756 . ? O3A K1A C17 81.08(6) 3_756 3_756 ? O3A K1A C17 98.92(6) . 3_756 ? O2A K1A C17 75.61(7) 3_756 3_756 ? O2A K1A C17 104.39(7) . 3_756 ? O1A K1A C17 84.40(6) . 3_756 ? O1A K1A C17 95.60(6) 3_756 3_756 ? C17 K1A C17 180.0 . 3_756 ? O3A K1A C16 87.52(7) 3_756 . ? O3A K1A C16 92.48(7) . . ? O2A K1A C16 80.73(7) 3_756 . ? O2A K1A C16 99.27(7) . . ? O1A K1A C16 108.22(6) . . ? O1A K1A C16 71.78(6) 3_756 . ? C17 K1A C16 23.66(7) . . ? C17 K1A C16 156.34(7) 3_756 . ? O3A K1A C16 92.48(7) 3_756 3_756 ? O3A K1A C16 87.52(7) . 3_756 ? O2A K1A C16 99.27(7) 3_756 3_756 ? O2A K1A C16 80.73(7) . 3_756 ? O1A K1A C16 71.78(6) . 3_756 ? O1A K1A C16 108.22(6) 3_756 3_756 ? C17 K1A C16 156.34(7) . 3_756 ? C17 K1A C16 23.66(7) 3_756 3_756 ? C16 K1A C16 180.0 . 3_756 ? C2A O1A C1A 110.49(18) . . ? C2A O1A K1A 113.57(13) . . ? C1A O1A K1A 109.79(12) . . ? O1A C1A C6A 108.97(19) . 3_756 ? C3A O2A C4A 111.82(18) . . ? C3A O2A K1A 116.37(13) . . ? C4A O2A K1A 116.39(13) . . ? O1A C2A C3A 108.41(19) . . ? C6A O3A C5A 113.71(18) . . ? C6A O3A K1A 115.13(13) . . ? C5A O3A K1A 116.15(13) . . ? O2A C3A C2A 108.7(2) . . ? O2A C4A C5A 108.1(2) . . ? O3A C5A C4A 108.65(19) . . ? O3A C6A C1A 108.73(19) . 3_756 ? O2B K1B O2B 180.00(6) 3_655 . ? O2B K1B O1B 118.59(5) 3_655 . ? O2B K1B O1B 61.41(5) . . ? O2B K1B O1B 61.41(5) 3_655 3_655 ? O2B K1B O1B 118.59(5) . 3_655 ? O1B K1B O1B 180.00(4) . 3_655 ? O2B K1B O3B 59.71(5) 3_655 3_655 ? O2B K1B O3B 120.29(5) . 3_655 ? O1B K1B O3B 59.91(5) . 3_655 ? O1B K1B O3B 120.09(5) 3_655 3_655 ? O2B K1B O3B 120.29(5) 3_655 . ? O2B K1B O3B 59.71(5) . . ? O1B K1B O3B 120.09(5) . . ? O1B K1B O3B 59.91(5) 3_655 . ? O3B K1B O3B 180.00(9) 3_655 . ? C1B O1B C2B 112.6(2) . . ? C1B O1B K1B 114.59(14) . . ? C2B O1B K1B 114.44(14) . . ? O1B C1B C6B 109.1(2) . 3_655 ? C3B O2B C4B 112.12(18) . . ? C3B O2B K1B 113.09(14) . . ? C4B O2B K1B 116.50(13) . . ? O1B C2B C3B 108.9(2) . . ? C5B O3B C6B 113.6(2) . . ? C5B O3B K1B 115.81(14) . . ? C6B O3B K1B 116.29(14) . . ? O2B C3B C2B 109.6(2) . . ? O2B C4B C5B 108.7(2) . . ? O3B C5B C4B 108.0(2) . . ? O3B C6B C1B 107.7(2) . 3_655 ? 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 C7 Si1 C1 C6 -68.6(2) . . . . ? C13 Si1 C1 C6 110.6(2) . . . . ? C7 Si1 C1 C2 112.7(2) . . . . ? C13 Si1 C1 C2 -68.1(2) . . . . ? C6 C1 C2 C3 -1.4(4) . . . . ? Si1 C1 C2 C3 177.3(2) . . . . ? C1 C2 C3 C4 1.8(5) . . . . ? C2 C3 C4 C5 -0.8(4) . . . . ? C3 C4 C5 C6 -0.6(4) . . . . ? C4 C5 C6 C1 0.9(4) . . . . ? C2 C1 C6 C5 0.0(4) . . . . ? Si1 C1 C6 C5 -178.75(19) . . . . ? C1 Si1 C7 C12 -64.8(2) . . . . ? C13 Si1 C7 C12 115.99(18) . . . . ? C1 Si1 C7 C8 109.53(18) . . . . ? C13 Si1 C7 C8 -69.6(2) . . . . ? C12 C7 C8 C9 0.1(3) . . . . ? Si1 C7 C8 C9 -174.51(18) . . . . ? C7 C8 C9 C10 1.7(4) . . . . ? C8 C9 C10 C11 -1.3(4) . . . . ? C9 C10 C11 C12 -0.9(4) . . . . ? C10 C11 C12 C7 2.7(4) . . . . ? C8 C7 C12 C11 -2.2(3) . . . . ? Si1 C7 C12 C11 172.46(19) . . . . ? C7 Si1 C13 C18 76.1(2) . . . . ? C1 Si1 C13 C18 -103.0(2) . . . . ? C7 Si1 C13 C14 -104.2(2) . . . . ? C1 Si1 C13 C14 76.7(2) . . . . ? C18 C13 C14 C15 0.8(3) . . . . ? Si1 C13 C14 C15 -178.89(19) . . . . ? C13 C14 C15 C16 -1.6(4) . . . . ? C14 C15 C16 C17 0.5(4) . . . . ? C14 C15 C16 K1A 84.2(3) . . . . ? C15 C16 C17 C18 1.3(4) . . . . ? K1A C16 C17 C18 -98.3(2) . . . . ? C15 C16 C17 K1A 99.7(2) . . . . ? C14 C13 C18 C17 1.1(3) . . . . ? Si1 C13 C18 C17 -179.23(19) . . . . ? C16 C17 C18 C13 -2.2(4) . . . . ? K1A C17 C18 C13 -86.4(2) . . . . ? C16 C17 K1A O3A -62.13(17) . . . 3_756 ? C18 C17 K1A O3A 56.4(2) . . . 3_756 ? C16 C17 K1A O3A 117.87(17) . . . . ? C18 C17 K1A O3A -123.6(2) . . . . ? C16 C17 K1A O2A -1.15(18) . . . 3_756 ? C18 C17 K1A O2A 117.37(19) . . . 3_756 ? C16 C17 K1A O2A 178.85(18) . . . . ? C18 C17 K1A O2A -62.63(19) . . . . ? C16 C17 K1A O1A -123.97(17) . . . . ? C18 C17 K1A O1A -5.4(2) . . . . ? C16 C17 K1A O1A 56.03(17) . . . 3_756 ? C18 C17 K1A O1A 174.6(2) . . . 3_756 ? C16 C17 K1A C17 -91(100) . . . 3_756 ? C18 C17 K1A C17 27(100) . . . 3_756 ? C18 C17 K1A C16 118.5(3) . . . . ? C16 C17 K1A C16 180.0 . . . 3_756 ? C18 C17 K1A C16 -61.5(3) . . . 3_756 ? C15 C16 K1A O3A 1.57(19) . . . 3_756 ? C17 C16 K1A O3A 119.06(17) . . . 3_756 ? C15 C16 K1A O3A -178.43(19) . . . . ? C17 C16 K1A O3A -60.94(17) . . . . ? C15 C16 K1A O2A 61.39(19) . . . 3_756 ? C17 C16 K1A O2A 178.87(18) . . . 3_756 ? C15 C16 K1A O2A -118.61(19) . . . . ? C17 C16 K1A O2A -1.13(18) . . . . ? C15 C16 K1A O1A -57.1(2) . . . . ? C17 C16 K1A O1A 60.34(18) . . . . ? C15 C16 K1A O1A 122.9(2) . . . 3_756 ? C17 C16 K1A O1A -119.66(18) . . . 3_756 ? C15 C16 K1A C17 -117.5(3) . . . . ? C15 C16 K1A C17 62.5(3) . . . 3_756 ? C17 C16 K1A C17 180.0 . . . 3_756 ? C15 C16 K1A C16 73(100) . . . 3_756 ? C17 C16 K1A C16 -170(100) . . . 3_756 ? O3A K1A O1A C2A -147.06(16) 3_756 . . . ? O3A K1A O1A C2A 32.94(16) . . . . ? O2A K1A O1A C2A -160.08(14) 3_756 . . . ? O2A K1A O1A C2A 19.92(14) . . . . ? O1A K1A O1A C2A 162(100) 3_756 . . . ? C17 K1A O1A C2A -49.94(16) . . . . ? C17 K1A O1A C2A 130.06(16) 3_756 . . . ? C16 K1A O1A C2A -70.45(16) . . . . ? C16 K1A O1A C2A 109.55(16) 3_756 . . . ? O3A K1A O1A C1A -22.81(13) 3_756 . . . ? O3A K1A O1A C1A 157.19(13) . . . . ? O2A K1A O1A C1A -35.83(15) 3_756 . . . ? O2A K1A O1A C1A 144.17(15) . . . . ? O1A K1A O1A C1A -73(100) 3_756 . . . ? C17 K1A O1A C1A 74.32(14) . . . . ? C17 K1A O1A C1A -105.68(14) 3_756 . . . ? C16 K1A O1A C1A 53.80(15) . . . . ? C16 K1A O1A C1A -126.20(15) 3_756 . . . ? C2A O1A C1A C6A -178.51(19) . . . 3_756 ? K1A O1A C1A C6A 55.5(2) . . . 3_756 ? O3A K1A O2A C3A 28.30(17) 3_756 . . . ? O3A K1A O2A C3A -151.70(17) . . . . ? O2A K1A O2A C3A -54(100) 3_756 . . . ? O1A K1A O2A C3A 15.08(15) . . . . ? O1A K1A O2A C3A -164.92(15) 3_756 . . . ? C17 K1A O2A C3A 120.36(16) . . . . ? C17 K1A O2A C3A -59.64(16) 3_756 . . . ? C16 K1A O2A C3A 120.83(16) . . . . ? C16 K1A O2A C3A -59.17(16) 3_756 . . . ? O3A K1A O2A C4A 163.45(14) 3_756 . . . ? O3A K1A O2A C4A -16.55(14) . . . . ? O2A K1A O2A C4A 81(100) 3_756 . . . ? O1A K1A O2A C4A 150.23(16) . . . . ? O1A K1A O2A C4A -29.77(16) 3_756 . . . ? C17 K1A O2A C4A -104.48(16) . . . . ? C17 K1A O2A C4A 75.52(16) 3_756 . . . ? C16 K1A O2A C4A -104.02(16) . . . . ? C16 K1A O2A C4A 75.98(16) 3_756 . . . ? C1A O1A C2A C3A -175.04(19) . . . . ? K1A O1A C2A C3A -51.2(2) . . . . ? O3A K1A O3A C6A 119(50) 3_756 . . . ? O2A K1A O3A C6A 25.52(16) 3_756 . . . ? O2A K1A O3A C6A -154.48(16) . . . . ? O1A K1A O3A C6A -167.54(14) . . . . ? O1A K1A O3A C6A 12.46(14) 3_756 . . . ? C17 K1A O3A C6A -76.00(15) . . . . ? C17 K1A O3A C6A 104.00(15) 3_756 . . . ? C16 K1A O3A C6A -55.20(15) . . . . ? C16 K1A O3A C6A 124.80(15) 3_756 . . . ? O3A K1A O3A C5A -105(50) 3_756 . . . ? O2A K1A O3A C5A 162.00(14) 3_756 . . . ? O2A K1A O3A C5A -18.00(14) . . . . ? O1A K1A O3A C5A -31.06(16) . . . . ? O1A K1A O3A C5A 148.94(16) 3_756 . . . ? C17 K1A O3A C5A 60.48(16) . . . . ? C17 K1A O3A C5A -119.52(16) 3_756 . . . ? C16 K1A O3A C5A 81.28(16) . . . . ? C16 K1A O3A C5A -98.72(16) 3_756 . . . ? C4A O2A C3A C2A 176.21(19) . . . . ? K1A O2A C3A C2A -46.7(2) . . . . ? O1A C2A C3A O2A 65.1(2) . . . . ? C3A O2A C4A C5A -175.86(19) . . . . ? K1A O2A C4A C5A 47.0(2) . . . . ? C6A O3A C5A C4A -174.1(2) . . . . ? K1A O3A C5A C4A 48.9(2) . . . . ? O2A C4A C5A O3A -62.6(2) . . . . ? C5A O3A C6A C1A 177.5(2) . . . 3_756 ? K1A O3A C6A C1A -45.0(2) . . . 3_756 ? O2B K1B O1B C1B -32.78(18) 3_655 . . . ? O2B K1B O1B C1B 147.22(18) . . . . ? O1B K1B O1B C1B 125(100) 3_655 . . . ? O3B K1B O1B C1B -21.24(16) 3_655 . . . ? O3B K1B O1B C1B 158.76(16) . . . . ? O2B K1B O1B C2B -165.00(15) 3_655 . . . ? O2B K1B O1B C2B 15.00(15) . . . . ? O1B K1B O1B C2B -8(100) 3_655 . . . ? O3B K1B O1B C2B -153.45(17) 3_655 . . . ? O3B K1B O1B C2B 26.55(17) . . . . ? C2B O1B C1B C6B -173.7(2) . . . 3_655 ? K1B O1B C1B C6B 53.2(2) . . . 3_655 ? O2B K1B O2B C3B 74(100) 3_655 . . . ? O1B K1B O2B C3B 19.12(14) . . . . ? O1B K1B O2B C3B -160.88(14) 3_655 . . . ? O3B K1B O2B C3B 30.68(16) 3_655 . . . ? O3B K1B O2B C3B -149.32(16) . . . . ? O2B K1B O2B C4B -154(100) 3_655 . . . ? O1B K1B O2B C4B 151.18(16) . . . . ? O1B K1B O2B C4B -28.82(16) 3_655 . . . ? O3B K1B O2B C4B 162.74(15) 3_655 . . . ? O3B K1B O2B C4B -17.26(15) . . . . ? C1B O1B C2B C3B -179.5(2) . . . . ? K1B O1B C2B C3B -46.3(2) . . . . ? O2B K1B O3B C5B 162.60(15) 3_655 . . . ? O2B K1B O3B C5B -17.40(15) . . . . ? O1B K1B O3B C5B -29.14(16) . . . . ? O1B K1B O3B C5B 150.86(16) 3_655 . . . ? O3B K1B O3B C5B 42(33) 3_655 . . . ? O2B K1B O3B C6B 25.23(17) 3_655 . . . ? O2B K1B O3B C6B -154.77(17) . . . . ? O1B K1B O3B C6B -166.51(16) . . . . ? O1B K1B O3B C6B 13.49(16) 3_655 . . . ? O3B K1B O3B C6B -96(33) 3_655 . . . ? C4B O2B C3B C2B 174.8(2) . . . . ? K1B O2B C3B C2B -51.0(2) . . . . ? O1B C2B C3B O2B 65.6(3) . . . . ? C3B O2B C4B C5B -179.1(2) . . . . ? K1B O2B C4B C5B 48.4(2) . . . . ? C6B O3B C5B C4B -173.5(2) . . . . ? K1B O3B C5B C4B 48.0(2) . . . . ? O2B C4B C5B O3B -63.1(3) . . . . ? C5B O3B C6B C1B 177.5(2) . . . 3_655 ? K1B O3B C6B C1B -44.2(2) . . . 3_655 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.399 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.077 # Attachment '1b.CIF' data_R3M1.CIF _database_code_depnum_ccdc_archive 'CCDC 659285' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H41 K O6 Si' _chemical_formula_weight 564.82 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 trigonal _symmetry_space_group_name_H-M R3mr loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' 'y, x, z' 'x, z, y' 'z, y, x' _cell_length_a 9.4377(12) _cell_length_b 9.4377(12) _cell_length_c 9.4377(12) _cell_angle_alpha 97.956(6) _cell_angle_beta 97.956(6) _cell_angle_gamma 97.956(6) _cell_volume 813.80(18) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 302 _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9432 _exptl_absorpt_correction_T_max 0.9432 _exptl_absorpt_process_details scalepack _exptl_special_details ; refined as racemic twin. ; _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 KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4637 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 24.96 _reflns_number_total 1043 _reflns_number_gt 1000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material ? _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^)+(0.0230P)^2^+0.2182P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.54(7) _refine_ls_number_reflns 1043 _refine_ls_number_parameters 77 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.131 _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 0.09938(7) 0.09938(7) 0.09938(7) 0.0196(3) Uani 1 6 d S . . Si1 Si -0.21127(10) -0.21127(10) -0.21127(10) 0.0306(4) Uani 1 6 d S . . O1 O 0.0059(2) 0.0059(2) 0.3441(2) 0.0305(4) Uani 1 2 d S . . C1 C 0.0984(3) -0.0676(3) 0.4304(3) 0.0428(6) Uani 1 1 d . . . H1A H 0.0419 -0.1243 0.4904 0.051 Uiso 1 1 calc R . . H1B H 0.1751 0.0033 0.4957 0.051 Uiso 1 1 calc R . . O2 O 0.25246(17) -0.0804(2) 0.25246(17) 0.0304(6) Uani 1 2 d S . . C2 C 0.1645(3) -0.1658(2) 0.3310(3) 0.0438(7) Uani 1 1 d . . . H2A H 0.2245 -0.2233 0.3875 0.053 Uiso 1 1 calc R . . H2B H 0.0875 -0.2337 0.2628 0.053 Uiso 1 1 calc R . . H1S H -0.327(3) -0.327(3) -0.327(3) 0.024(13) Uiso 1 6 d S . . C3 C -0.2885(2) -0.2885(2) -0.0527(3) 0.0291(7) Uani 1 2 d S . . C4 C -0.2312(3) -0.2312(3) 0.0924(3) 0.0301(7) Uani 1 2 d S . . H4 H -0.1527 -0.1527 0.1127 0.036 Uiso 1 2 calc SR . . C5 C -0.2854(3) -0.2854(3) 0.2080(4) 0.0356(8) Uani 1 2 d S . . H5 H -0.2439 -0.2439 0.3049 0.043 Uiso 1 2 calc SR . . C6 C -0.3989(3) -0.3989(3) 0.1813(4) 0.0375(8) Uani 1 2 d S . . H6 H -0.4363 -0.4363 0.2594 0.045 Uiso 1 2 calc SR . . C7 C -0.4580(3) -0.4580(3) 0.0401(4) 0.0441(9) Uani 1 2 d S . . H7 H -0.5364 -0.5364 0.0210 0.053 Uiso 1 2 calc SR . . C8 C -0.4031(3) -0.4031(3) -0.0755(4) 0.0378(9) Uani 1 2 d S . . H8 H -0.4454 -0.4454 -0.1720 0.045 Uiso 1 2 calc SR . . H2S H -0.104(3) -0.104(3) -0.104(3) 0.005(10) Uiso 1 6 d S . . 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 0.0202(3) 0.0202(3) 0.0202(3) 0.0052(3) 0.0052(3) 0.0052(3) Si1 0.0289(4) 0.0289(4) 0.0289(4) -0.0010(5) -0.0010(5) -0.0010(5) O1 0.0364(8) 0.0364(8) 0.0183(11) 0.0066(6) 0.0066(6) 0.0000(10) C1 0.0506(15) 0.0509(15) 0.0279(12) 0.0218(11) 0.0025(10) -0.0001(11) O2 0.0338(8) 0.0239(12) 0.0338(8) 0.0087(8) -0.0019(10) 0.0087(8) C2 0.0538(15) 0.0346(14) 0.0468(16) 0.0267(12) 0.0016(12) 0.0070(12) C3 0.0231(10) 0.0231(10) 0.0413(19) 0.0035(11) 0.0035(11) 0.0074(12) C4 0.0264(11) 0.0264(11) 0.0360(18) 0.0033(11) 0.0033(11) 0.0031(13) C5 0.0354(12) 0.0354(12) 0.0391(19) 0.0081(12) 0.0081(12) 0.0124(15) C6 0.0318(12) 0.0318(12) 0.057(2) 0.0161(14) 0.0161(14) 0.0138(15) C7 0.0283(12) 0.0283(12) 0.077(3) 0.0129(14) 0.0129(14) 0.0018(14) C8 0.0288(12) 0.0288(12) 0.050(2) -0.0020(12) -0.0020(12) 0.0012(14) _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 2.7937(18) 3 ? K1 O1 2.7937(18) 2 ? K1 O1 2.7937(18) . ? K1 O2 2.799(2) 3 ? K1 O2 2.799(2) . ? K1 O2 2.799(2) 2 ? Si1 C3 1.938(3) . ? Si1 C3 1.938(3) 3 ? Si1 C3 1.938(3) 2 ? O1 C1 1.426(3) . ? O1 C1 1.426(3) 4 ? C1 C2 1.486(4) . ? O2 C2 1.428(3) . ? O2 C2 1.428(3) 6 ? C3 C8 1.391(4) . ? C3 C4 1.404(4) . ? C4 C5 1.396(4) . ? C5 C6 1.376(5) . ? C6 C7 1.378(5) . ? C7 C8 1.402(5) . ? 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 O1 119.097(18) 3 2 ? O1 K1 O1 119.097(18) 3 . ? O1 K1 O1 119.097(18) 2 . ? O1 K1 O2 59.556(10) 3 3 ? O1 K1 O2 162.44(8) 2 3 ? O1 K1 O2 59.556(10) . 3 ? O1 K1 O2 162.44(8) 3 . ? O1 K1 O2 59.556(10) 2 . ? O1 K1 O2 59.556(10) . . ? O2 K1 O2 115.74(3) 3 . ? O1 K1 O2 59.556(10) 3 2 ? O1 K1 O2 59.556(10) 2 2 ? O1 K1 O2 162.44(8) . 2 ? O2 K1 O2 115.74(3) 3 2 ? O2 K1 O2 115.74(3) . 2 ? C3 Si1 C3 119.990(3) . 3 ? C3 Si1 C3 119.990(3) . 2 ? C3 Si1 C3 119.990(3) 3 2 ? C1 O1 C1 112.0(3) . 4 ? C1 O1 K1 118.23(12) . . ? C1 O1 K1 118.23(12) 4 . ? O1 C1 C2 107.96(19) . . ? C2 O2 C2 112.3(2) . 6 ? C2 O2 K1 112.97(12) . . ? C2 O2 K1 112.97(12) 6 . ? O2 C2 C1 108.81(18) . . ? C8 C3 C4 116.1(3) . . ? C8 C3 Si1 122.3(2) . . ? C4 C3 Si1 121.5(2) . . ? C5 C4 C3 122.3(3) . . ? C6 C5 C4 119.9(3) . . ? C5 C6 C7 119.4(3) . . ? C6 C7 C8 120.4(3) . . ? C3 C8 C7 121.8(3) . . ? 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 O1 K1 O1 C1 -150.80(14) 3 . . . ? O1 K1 O1 C1 10.4(3) 2 . . . ? O2 K1 O1 C1 -149.4(2) 3 . . . ? O2 K1 O1 C1 9.01(18) . . . . ? O2 K1 O1 C1 -70.20(18) 2 . . . ? O1 K1 O1 C1 -10.4(3) 3 . . 4 ? O1 K1 O1 C1 150.80(14) 2 . . 4 ? O2 K1 O1 C1 -9.01(18) 3 . . 4 ? O2 K1 O1 C1 149.4(2) . . . 4 ? O2 K1 O1 C1 70.20(18) 2 . . 4 ? C1 O1 C1 C2 177.47(15) 4 . . . ? K1 O1 C1 C2 -39.8(2) . . . . ? O1 K1 O2 C2 115.61(15) 3 . . . ? O1 K1 O2 C2 -153.69(17) 2 . . . ? O1 K1 O2 C2 24.90(14) . . . . ? O2 K1 O2 C2 45.52(19) 3 . . . ? O2 K1 O2 C2 -174.31(12) 2 . . . ? O1 K1 O2 C2 -115.61(15) 3 . . 6 ? O1 K1 O2 C2 -24.90(14) 2 . . 6 ? O1 K1 O2 C2 153.69(17) . . . 6 ? O2 K1 O2 C2 174.31(12) 3 . . 6 ? O2 K1 O2 C2 -45.52(19) 2 . . 6 ? C2 O2 C2 C1 174.37(15) 6 . . . ? K1 O2 C2 C1 -56.5(2) . . . . ? O1 C1 C2 O2 63.3(2) . . . . ? C3 Si1 C3 C8 90.99(16) 3 . . . ? C3 Si1 C3 C8 -90.99(16) 2 . . . ? C3 Si1 C3 C4 -89.01(16) 3 . . . ? C3 Si1 C3 C4 89.01(16) 2 . . . ? C8 C3 C4 C5 0.0 . . . . ? Si1 C3 C4 C5 180.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C8 0.000(1) . . . . ? C4 C3 C8 C7 0.0 . . . . ? Si1 C3 C8 C7 180.0 . . . . ? C6 C7 C8 C3 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.364 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.033 # Attachment '5.CIF' data_pp2063o _database_code_depnum_ccdc_archive 'CCDC 659286' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H17 K O10 Si' _chemical_formula_weight 724.73 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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 37.820(8) _cell_length_b 12.712(3) _cell_length_c 17.536(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8431(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 0.205 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8701 _exptl_absorpt_correction_T_max 0.9227 _exptl_absorpt_process_details scalepack _exptl_special_details ; large residual shifts associated with disordered atoms ; _diffrn_ambient_temperature 120(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 35476 _diffrn_reflns_av_R_equivalents 0.1724 _diffrn_reflns_av_sigmaI/netI 0.1653 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7703 _reflns_number_gt 4149 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.2000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0052(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7703 _refine_ls_number_parameters 541 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2264 _refine_ls_R_factor_gt 0.1319 _refine_ls_wR_factor_ref 0.3894 _refine_ls_wR_factor_gt 0.3374 _refine_ls_goodness_of_fit_ref 1.262 _refine_ls_restrained_S_all 1.262 _refine_ls_shift/su_max 0.100 _refine_ls_shift/su_mean 0.005 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 0.13095(5) 0.7500 0.57105(9) 0.0339(6) Uani 1 2 d S . . Si1 Si 0.18992(7) 0.2500 0.89799(16) 0.0491(8) Uani 1 2 d SD . . C1 C 0.21699(17) 0.3789(5) 0.8939(4) 0.0464(17) Uani 1 1 d . . . K2 K 0.11705(5) 0.7500 0.07004(9) 0.0343(6) Uani 1 2 d S . . Si2 Si 0.05152(7) 0.2500 0.26294(15) 0.0398(7) Uani 1 2 d SD . . O2 O 0.20204(18) 0.7500 0.6277(4) 0.0565(18) Uani 1 2 d S . . C2 C 0.22688(18) 0.4354(5) 0.9589(4) 0.0504(18) Uani 1 1 d . . . H2 H 0.2193 0.4103 1.0072 0.060 Uiso 1 1 calc R . . C3 C 0.24670(19) 0.5237(6) 0.9566(5) 0.060(2) Uani 1 1 d . . . H3 H 0.2525 0.5589 1.0027 0.073 Uiso 1 1 calc R . . C4 C 0.25875(19) 0.5640(5) 0.8868(5) 0.062(2) Uani 1 1 d . . . H4 H 0.2723 0.6269 0.8853 0.074 Uiso 1 1 calc R . . C5 C 0.25076(19) 0.5111(6) 0.8210(5) 0.063(2) Uani 1 1 d . . . H5 H 0.2595 0.5355 0.7734 0.076 Uiso 1 1 calc R . . C6 C 0.22943(19) 0.4203(6) 0.8243(4) 0.0575(19) Uani 1 1 d . . . H6 H 0.2232 0.3858 0.7782 0.069 Uiso 1 1 calc R . . C7 C 0.1376(3) 0.2500 0.9068(7) 0.062(3) Uani 1 2 d S . . C8 C 0.1204(3) 0.2500 0.9784(8) 0.098(5) Uani 1 2 d S . . H8 H 0.1338 0.2500 1.0242 0.118 Uiso 1 2 calc SR . . C9 C 0.0845(4) 0.2500 0.9808(9) 0.125(6) Uani 1 2 d S . . H9 H 0.0736 0.2500 1.0296 0.150 Uiso 1 2 calc SR . . C10 C 0.0640(4) 0.2500 0.9220(8) 0.085(4) Uani 1 2 d S . . H10 H 0.0390 0.2500 0.9279 0.102 Uiso 1 2 calc SR . . C11 C 0.0784(3) 0.2500 0.8533(8) 0.069(4) Uani 1 2 d S . . H11 H 0.0635 0.2500 0.8097 0.083 Uiso 1 2 calc SR . . C12 C 0.1163(3) 0.2500 0.8426(6) 0.060(3) Uani 1 2 d S . . H12 H 0.1263 0.2500 0.7929 0.072 Uiso 1 2 calc SR . . C13 C 0.1030(2) 0.2500 0.2599(6) 0.041(2) Uani 1 2 d S . . C14 C 0.1230(3) 0.2500 0.3270(6) 0.051(3) Uani 1 2 d S . . H14 H 0.1113 0.2500 0.3750 0.061 Uiso 1 2 calc SR . . C15 C 0.1593(3) 0.2500 0.3238(8) 0.066(3) Uani 1 2 d S . . H15 H 0.1721 0.2500 0.3704 0.079 Uiso 1 2 calc SR . . C16 C 0.1782(3) 0.2500 0.2558(9) 0.076(4) Uani 1 2 d S . . H16 H 0.2034 0.2500 0.2541 0.091 Uiso 1 2 calc SR . . C17 C 0.1577(4) 0.2500 0.1919(7) 0.074(3) Uani 1 2 d S . . H17 H 0.1695 0.2500 0.1441 0.089 Uiso 1 2 calc SR . . C18 C 0.1219(3) 0.2500 0.1909(6) 0.055(3) Uani 1 2 d S . . H18 H 0.1096 0.2500 0.1437 0.066 Uiso 1 2 calc SR . . C19 C 0.02397(17) 0.1231(4) 0.2657(4) 0.0409(16) Uani 1 1 d . . . C20 C 0.01164(17) 0.0791(5) 0.3339(4) 0.0483(17) Uani 1 1 d . . . H20 H 0.0183 0.1117 0.3805 0.058 Uiso 1 1 calc R . . C21 C -0.00982(18) -0.0096(5) 0.3375(4) 0.0541(19) Uani 1 1 d . . . H21 H -0.0179 -0.0360 0.3851 0.065 Uiso 1 1 calc R . . C22 C -0.01899(19) -0.0578(5) 0.2701(5) 0.063(2) Uani 1 1 d . . . H22 H -0.0335 -0.1189 0.2714 0.075 Uiso 1 1 calc R . . C23 C -0.00765(18) -0.0197(5) 0.2009(5) 0.0537(19) Uani 1 1 d . . . H23 H -0.0141 -0.0541 0.1548 0.064 Uiso 1 1 calc R . . C24 C 0.01361(16) 0.0710(5) 0.1994(4) 0.0457(17) Uani 1 1 d . . . H24 H 0.0212 0.0978 0.1516 0.055 Uiso 1 1 calc R . . H25 H 0.197(4) 0.2500 0.994(5) 0.17(6) Uiso 1 2 d SD . . H26 H 0.1917(17) 0.2500 0.817(4) 0.023(18) Uiso 1 2 d S . . H28 H 0.053(2) 0.2500 0.185(4) 0.04(2) Uiso 1 2 d S . . C1A C 0.07629(18) 0.8088(5) 0.7405(4) 0.057(2) Uani 1 1 d . . . O2A O 0.1112(2) 0.8475(6) 0.7224(6) 0.043(2) Uani 0.50 1 d P . 1 C2A C 0.1135(5) 0.9591(15) 0.7091(11) 0.029(5) Uiso 0.50 1 d P . 1 C3A C 0.1484(2) 0.9691(8) 0.7086(4) 0.082(3) Uani 1 1 d . . 1 O1B O 0.0906(3) 0.8580(7) 0.6834(5) 0.042(2) Uani 0.50 1 d P . 2 C1B C 0.1029(5) 0.9607(19) 0.7013(15) 0.067(8) Uani 0.50 1 d P . 2 O2B O 0.16083(12) 0.9370(3) 0.6347(3) 0.0569(13) Uani 1 1 d . . . C4B C 0.1990(2) 0.9371(6) 0.6254(5) 0.078(3) Uani 1 1 d . . 2 C5B C 0.2163(2) 0.8414(5) 0.6636(5) 0.073(2) Uani 1 1 d . . 2 O1C O 0.1756(3) 0.6664(9) 0.4585(7) 0.059(3) Uani 0.50 1 d P . 1 C1C C 0.1983(3) 0.7500 0.4251(6) 0.066(3) Uani 1 2 d S . 1 C2C C 0.1598(5) 0.5945(14) 0.4070(11) 0.070(5) Uiso 0.50 1 d P . 1 O3C O 0.0636(6) 0.7500 0.4897(13) 0.246(8) Uiso 1 2 d S . 2 C3C C 0.1348(5) 0.5047(15) 0.4644(12) 0.082(6) Uiso 0.50 1 d P . 1 C4C C 0.0564(5) 0.6011(15) 0.4778(9) 0.058(4) Uiso 0.50 1 d P . 1 C5C C 0.0507(5) 0.7059(11) 0.5420(11) 0.075(5) Uiso 0.50 1 d P . 1 O1D O 0.1615(4) 0.6185(10) 0.4588(8) 0.068(4) Uiso 0.50 1 d P . 2 C1D C 0.1770(4) 0.6687(11) 0.3939(10) 0.058(4) Uiso 0.50 1 d P . 2 O2D O 0.0957(3) 0.5684(8) 0.5076(7) 0.073(3) Uiso 0.50 1 d P . 1 C2D C 0.1389(4) 0.5336(12) 0.4292(9) 0.049(4) Uiso 0.50 1 d P . 2 O3D O 0.1049(5) 0.5935(14) 0.4446(11) 0.147(6) Uiso 0.50 1 d P . 2 C3D C 0.0739(4) 0.5579(10) 0.4703(8) 0.045(3) Uiso 0.50 1 d P . 2 C4D C 0.0463(4) 0.6512(12) 0.4893(8) 0.045(4) Uiso 0.50 1 d P . 2 O1E O 0.1588(3) 0.5906(9) 0.1401(6) 0.060(3) Uani 0.50 1 d P . 1 O2E O 0.0860(3) 0.6070(8) 0.1674(5) 0.057(3) Uani 0.50 1 d P . 1 C2E C 0.1985(2) 0.6263(7) 0.1616(5) 0.016(2) Uiso 0.50 1 d P . 2 C3E C 0.1437(5) 0.5356(14) 0.1989(9) 0.058(4) Uiso 0.50 1 d P . 1 C4E C 0.1042(4) 0.5107(12) 0.1752(9) 0.052(4) Uiso 0.50 1 d P . 1 C5E C 0.0728(5) 0.6441(14) 0.2421(11) 0.047(4) Uiso 0.50 1 d P . 1 C6E C 0.0489(3) 0.7500 0.2172(6) 0.060(3) Uiso 1 2 d S . 1 O1F O 0.1951(3) 0.7038(6) 0.1054(5) 0.060(3) Uiso 0.50 1 d P . 2 O2F O 0.1403(3) 0.6075(8) 0.2001(6) 0.061(3) Uani 0.50 1 d P . 2 O3F O 0.0697(3) 0.6732(7) 0.1901(7) 0.055(3) Uani 0.50 1 d P . 2 C3F C 0.1746(6) 0.5578(15) 0.1724(12) 0.086(6) Uiso 0.50 1 d P . 2 C4F C 0.1109(4) 0.5386(9) 0.2159(8) 0.045(4) Uani 0.50 1 d P . 2 C5F C 0.0845(6) 0.6067(15) 0.2495(10) 0.068(6) Uiso 0.50 1 d P . 2 O1G O 0.1581(3) 0.6465(8) -0.0412(6) 0.056(3) Uani 0.50 1 d P . 1 C1G C 0.1697(4) 0.7010(10) -0.1044(8) 0.030(3) Uiso 0.50 1 d P . 1 O2G O 0.0856(5) 0.5621(14) 0.0070(10) 0.032(4) Uani 0.50 1 d P . 1 C2G C 0.1452(7) 0.550(2) -0.0618(16) 0.092(10) Uiso 0.50 1 d P . 1 O3G O 0.04381(18) 0.7500 0.0121(4) 0.0585(18) Uani 1 2 d S . . C3G C 0.1040(4) 0.5559(13) -0.0761(9) 0.058(4) Uiso 0.50 1 d P . 1 C4G C 0.0482(4) 0.5764(13) -0.0055(11) 0.057(5) Uiso 0.50 1 d P . 2 C5G C 0.0338(6) 0.6695(15) -0.0417(12) 0.069(7) Uiso 0.50 1 d P . 2 O1H O 0.1371(3) 0.6449(6) -0.0794(6) 0.048(2) Uani 0.50 1 d P . 2 C1H C 0.1720(8) 0.662(2) -0.0974(18) 0.106(9) Uiso 0.50 1 d P . 2 O2H O 0.0894(9) 0.577(2) 0.004(2) 0.141(13) Uani 0.50 1 d P . 2 C2H C 0.1363(4) 0.5347(12) -0.0620(8) 0.025(4) Uiso 0.50 1 d P . 2 C3H C 0.0980(4) 0.5094(12) -0.0539(9) 0.053(4) Uiso 0.50 1 d P . 2 C4H C 0.0485(4) 0.5555(11) 0.0284(10) 0.054(4) Uiso 0.50 1 d P . 1 C5H C 0.0318(4) 0.6461(13) -0.0198(10) 0.042(5) Uiso 0.50 1 d P . 1 C1S C 0.0474(8) 0.2500 0.5566(14) 0.169(9) Uiso 1 2 d S . . C2S C 0.0725(12) 0.2500 0.567(2) 0.239(16) Uiso 1 2 d S . . C3S C 0.1020(6) 0.2500 0.5497(12) 0.131(6) Uiso 1 2 d S . . C4S C 0.1127(11) 0.2500 0.625(2) 0.266(15) Uiso 1 2 d S . . C5S C 0.1492(9) 0.2500 0.6109(17) 0.220(12) Uiso 1 2 d S . . C6S C 0.1673(7) 0.2500 0.5412(13) 0.160(8) Uiso 1 2 d S . . C7S C 0.1947(8) 0.2500 0.5749(14) 0.185(9) Uiso 1 2 d S . . H27 H 0.039(4) 0.2500 0.352(5) 0.17(6) Uiso 1 2 d SD . . 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 0.0323(11) 0.0428(11) 0.0265(11) 0.000 -0.0005(8) 0.000 Si1 0.0495(18) 0.0560(17) 0.0417(17) 0.000 -0.0137(13) 0.000 C1 0.037(4) 0.052(4) 0.050(4) 0.004(3) -0.006(3) 0.013(3) K2 0.0469(13) 0.0297(10) 0.0263(11) 0.000 0.0000(9) 0.000 Si2 0.0359(16) 0.0388(14) 0.0446(17) 0.000 -0.0086(12) 0.000 O2 0.053(4) 0.049(4) 0.067(5) 0.000 -0.015(4) 0.000 C2 0.051(5) 0.051(4) 0.049(4) -0.003(3) -0.016(3) 0.007(3) C3 0.048(5) 0.052(4) 0.082(6) -0.012(4) -0.019(4) 0.015(4) C4 0.044(5) 0.044(4) 0.097(7) 0.007(5) -0.005(5) 0.007(3) C5 0.057(5) 0.055(5) 0.078(6) 0.014(4) -0.004(4) 0.019(4) C6 0.052(5) 0.061(5) 0.059(5) 0.003(4) -0.010(4) 0.020(4) C7 0.047(7) 0.049(6) 0.089(9) 0.000 -0.040(6) 0.000 C8 0.046(8) 0.193(15) 0.057(9) 0.000 -0.009(6) 0.000 C9 0.043(9) 0.25(2) 0.087(12) 0.000 -0.012(8) 0.000 C10 0.073(10) 0.122(11) 0.061(9) 0.000 0.006(8) 0.000 C11 0.053(8) 0.044(6) 0.111(11) 0.000 -0.059(7) 0.000 C12 0.084(9) 0.029(5) 0.068(7) 0.000 -0.031(6) 0.000 C13 0.030(5) 0.030(4) 0.063(7) 0.000 -0.011(5) 0.000 C14 0.044(7) 0.043(5) 0.066(7) 0.000 -0.011(5) 0.000 C15 0.035(7) 0.063(7) 0.100(10) 0.000 -0.036(7) 0.000 C16 0.034(7) 0.069(7) 0.124(12) 0.000 -0.012(8) 0.000 C17 0.075(10) 0.078(8) 0.071(9) 0.000 0.022(7) 0.000 C18 0.031(6) 0.080(7) 0.055(7) 0.000 -0.003(5) 0.000 C19 0.040(4) 0.040(3) 0.042(4) -0.002(3) -0.014(3) 0.007(3) C20 0.044(4) 0.049(4) 0.052(5) 0.006(3) -0.008(3) -0.001(3) C21 0.054(5) 0.047(4) 0.061(5) 0.009(4) -0.005(4) 0.001(3) C22 0.043(5) 0.042(4) 0.103(7) 0.008(4) -0.009(5) 0.000(3) C23 0.043(4) 0.043(4) 0.074(6) -0.015(4) -0.024(4) 0.006(3) C24 0.041(4) 0.046(4) 0.050(4) 0.001(3) -0.008(3) 0.009(3) C1A 0.036(4) 0.065(4) 0.071(5) 0.002(4) 0.008(4) 0.008(3) O2A 0.035(6) 0.036(5) 0.057(7) 0.002(4) 0.006(5) 0.002(4) C3A 0.065(6) 0.126(7) 0.056(5) -0.036(5) -0.006(4) 0.033(5) O1B 0.046(6) 0.044(5) 0.035(6) 0.006(4) 0.006(5) 0.007(5) C1B 0.013(10) 0.083(14) 0.104(17) -0.022(10) 0.005(10) 0.006(10) O2B 0.049(3) 0.060(3) 0.061(3) -0.012(2) -0.002(2) 0.000(2) C4B 0.057(6) 0.062(5) 0.114(7) -0.006(5) 0.000(5) -0.016(4) C5B 0.072(6) 0.053(5) 0.094(6) -0.008(4) -0.030(5) -0.004(4) O1C 0.041(7) 0.073(7) 0.063(8) -0.018(6) -0.004(5) -0.001(6) C1C 0.039(7) 0.079(7) 0.081(8) 0.000 0.023(6) 0.000 O1E 0.052(7) 0.087(7) 0.041(6) -0.002(6) -0.004(5) 0.011(6) O2E 0.074(8) 0.045(6) 0.051(7) 0.016(5) 0.017(5) 0.007(5) O2F 0.076(8) 0.046(6) 0.061(7) -0.003(5) -0.013(6) -0.005(5) O3F 0.062(7) 0.044(6) 0.058(8) -0.002(5) -0.004(5) -0.012(5) C4F 0.072(11) 0.023(6) 0.040(9) 0.002(6) 0.008(8) -0.011(7) O1G 0.054(7) 0.061(7) 0.054(7) -0.027(5) -0.024(6) 0.032(5) O2G 0.024(7) 0.029(6) 0.044(8) -0.017(6) 0.008(6) -0.007(5) O3G 0.055(5) 0.062(4) 0.058(5) 0.000 -0.010(3) 0.000 O1H 0.054(7) 0.029(5) 0.061(7) 0.011(4) 0.018(6) -0.002(4) O2H 0.10(2) 0.13(2) 0.19(3) -0.120(18) -0.040(18) 0.031(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 K1 O1C 2.806(11) 8_575 ? K1 O1C 2.806(11) . ? K1 O1D 2.829(14) . ? K1 O1D 2.829(14) 8_575 ? K1 O1B 2.845(9) . ? K1 O1B 2.845(9) 8_575 ? K1 O2B 2.859(4) . ? K1 O2B 2.859(4) 8_575 ? K1 O2 2.866(7) . ? K1 O2D 2.889(11) . ? K1 O2D 2.889(11) 8_575 ? K1 O3C 2.92(2) . ? Si1 C1 1.934(7) . ? Si1 C1 1.934(7) 8_565 ? Si1 C7 1.986(11) . ? C1 C2 1.397(9) . ? C1 C6 1.409(9) . ? K2 O2H 2.70(3) . ? K2 O2H 2.70(3) 8_575 ? K2 O2E 2.757(9) . ? K2 O2E 2.757(9) 8_575 ? K2 O1G 2.819(10) . ? K2 O1G 2.819(10) 8_575 ? K2 O1E 2.847(11) 8_575 ? K2 O1E 2.847(11) . ? K2 O2G 2.888(19) . ? K2 O2G 2.888(19) 8_575 ? K2 O3F 2.931(11) 8_575 ? K2 O3F 2.931(11) . ? Si2 C19 1.921(6) . ? Si2 C19 1.921(6) 8_565 ? Si2 C13 1.949(9) . ? O2 C5B 1.428(8) . ? O2 C5B 1.428(8) 8_575 ? C2 C3 1.351(9) . ? C3 C4 1.402(10) . ? C4 C5 1.370(10) . ? C5 C6 1.410(10) . ? C7 C12 1.385(13) . ? C7 C8 1.412(16) . ? C8 C9 1.359(16) . ? C9 C10 1.291(17) . ? C10 C11 1.323(16) . ? C11 C12 1.443(15) . ? C13 C14 1.396(12) . ? C13 C18 1.405(13) . ? C14 C15 1.376(14) . ? C15 C16 1.391(17) . ? C16 C17 1.363(16) . ? C17 C18 1.355(15) . ? C19 C24 1.393(8) . ? C19 C20 1.401(9) . ? C20 C21 1.390(9) . ? C21 C22 1.376(10) . ? C22 C23 1.376(10) . ? C23 C24 1.406(9) . ? C1A O1B 1.298(10) . ? C1A O2A 1.442(11) . ? C1A C1A 1.496(14) 8_575 ? O2A C2A 1.44(2) . ? C2A C3A 1.324(19) . ? C3A O2B 1.438(8) . ? O1B C1B 1.42(2) . ? O2B C4B 1.453(9) . ? C4B C5B 1.535(11) . ? O1C C2C 1.42(2) . ? O1C C1C 1.485(15) . ? C1C O1C 1.485(15) 8_575 ? C2C C3C 1.79(3) . ? O3C C4D 1.417(16) . ? O3C C4D 1.417(16) 8_575 ? C3C O2D 1.85(2) . ? C4C O2D 1.63(2) . ? C4C C5C 1.76(2) . ? C5C C5C 1.12(3) 8_575 ? O1D C1D 1.43(2) . ? O1D C2D 1.47(2) . ? C2D O3D 1.52(2) . ? O3D C3D 1.34(2) . ? C3D C4D 1.616(19) . ? O1E C3E 1.37(2) . ? O2E C4E 1.411(18) . ? O2E C5E 1.479(19) . ? C2E C3F 1.27(2) . ? C2E O1F 1.399(12) . ? C3E C4E 1.58(2) . ? C5E C6E 1.68(2) . ? C6E C5E 1.68(2) 8_575 ? O1F O1F 1.174(15) 8_575 ? O2F C4F 1.445(16) . ? O2F C3F 1.52(2) . ? O3F C5F 1.45(2) . ? C4F C5F 1.45(2) . ? O1G C1G 1.379(19) . ? O1G C2G 1.37(3) . ? C1G C1G 1.24(3) 8_575 ? O2G C4H 1.46(3) . ? O2G C3G 1.62(3) . ? C2G C3G 1.58(3) . ? O3G C5G 1.44(2) . ? O3G C5G 1.44(2) 8_575 ? O3G C5H 1.504(16) . ? O3G C5H 1.504(16) 8_575 ? C4G C5G 1.45(3) . ? C4G O2H 1.57(4) . ? O1H C1H 1.37(3) . ? O1H C2H 1.434(18) . ? O2H C3H 1.36(3) . ? C2H C3H 1.49(2) . ? C4H C5H 1.56(2) . ? C1S C2S 0.97(4) . ? C1S C3S 2.07(4) . ? C2S C3S 1.16(4) . ? C2S C4S 1.82(5) . ? C3S C4S 1.37(4) . ? C4S C5S 1.40(4) . ? C5S C6S 1.40(3) . ? C5S C7S 1.83(4) . ? C6S C7S 1.19(3) . ? 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 O1C K1 O1C 44.5(5) 8_575 . ? O1C K1 O1D 59.2(4) 8_575 . ? O1C K1 O1D 16.5(2) . . ? O1C K1 O1D 16.5(2) 8_575 8_575 ? O1C K1 O1D 59.2(4) . 8_575 ? O1D K1 O1D 72.4(5) . 8_575 ? O1C K1 O1B 128.8(3) 8_575 . ? O1C K1 O1B 172.9(3) . . ? O1D K1 O1B 170.4(3) . . ? O1D K1 O1B 114.6(3) 8_575 . ? O1C K1 O1B 172.9(3) 8_575 8_575 ? O1C K1 O1B 128.8(3) . 8_575 ? O1D K1 O1B 114.6(3) . 8_575 ? O1D K1 O1B 170.4(3) 8_575 8_575 ? O1B K1 O1B 57.7(4) . 8_575 ? O1C K1 O2B 73.8(3) 8_575 . ? O1C K1 O2B 110.6(3) . . ? O1D K1 O2B 127.0(3) . . ? O1D K1 O2B 67.6(3) 8_575 . ? O1B K1 O2B 62.6(2) . . ? O1B K1 O2B 110.0(2) 8_575 . ? O1C K1 O2B 110.6(3) 8_575 8_575 ? O1C K1 O2B 73.8(3) . 8_575 ? O1D K1 O2B 67.6(3) . 8_575 ? O1D K1 O2B 127.0(3) 8_575 8_575 ? O1B K1 O2B 110.0(2) . 8_575 ? O1B K1 O2B 62.6(2) 8_575 8_575 ? O2B K1 O2B 112.5(2) . 8_575 ? O1C K1 O2 71.3(2) 8_575 . ? O1C K1 O2 71.3(2) . . ? O1D K1 O2 81.8(3) . . ? O1D K1 O2 81.8(3) 8_575 . ? O1B K1 O2 105.2(3) . . ? O1B K1 O2 105.2(3) 8_575 . ? O2B K1 O2 59.60(10) . . ? O2B K1 O2 59.60(10) 8_575 . ? O1C K1 O2D 108.1(3) 8_575 . ? O1C K1 O2D 72.8(3) . . ? O1D K1 O2D 56.6(4) . . ? O1D K1 O2D 113.1(4) 8_575 . ? O1B K1 O2D 113.9(3) . . ? O1B K1 O2D 68.5(3) 8_575 . ? O2B K1 O2D 175.7(2) . . ? O2B K1 O2D 70.6(2) 8_575 . ? O2 K1 O2D 124.5(2) . . ? O1C K1 O2D 72.8(3) 8_575 8_575 ? O1C K1 O2D 108.1(3) . 8_575 ? O1D K1 O2D 113.1(4) . 8_575 ? O1D K1 O2D 56.6(4) 8_575 8_575 ? O1B K1 O2D 68.5(3) . 8_575 ? O1B K1 O2D 113.9(3) 8_575 8_575 ? O2B K1 O2D 70.6(2) . 8_575 ? O2B K1 O2D 175.7(2) 8_575 8_575 ? O2 K1 O2D 124.5(2) . 8_575 ? O2D K1 O2D 106.1(4) . 8_575 ? O1C K1 O3C 100.5(5) 8_575 . ? O1C K1 O3C 100.5(5) . . ? O1D K1 O3C 90.9(5) . . ? O1D K1 O3C 90.9(5) 8_575 . ? O1B K1 O3C 82.6(4) . . ? O1B K1 O3C 82.6(4) 8_575 . ? O2B K1 O3C 122.39(13) . . ? O2B K1 O3C 122.39(13) 8_575 . ? O2 K1 O3C 171.0(5) . . ? O2D K1 O3C 53.8(2) . . ? O2D K1 O3C 53.8(2) 8_575 . ? C1 Si1 C1 115.9(4) . 8_565 ? C1 Si1 C7 122.05(19) . . ? C1 Si1 C7 122.05(19) 8_565 . ? C2 C1 C6 115.2(6) . . ? C2 C1 Si1 123.1(5) . . ? C6 C1 Si1 121.6(5) . . ? O2H K2 O2H 109.3(15) . 8_575 ? O2H K2 O2E 64.1(8) . . ? O2H K2 O2E 129.7(7) 8_575 . ? O2H K2 O2E 129.7(7) . 8_575 ? O2H K2 O2E 64.1(8) 8_575 8_575 ? O2E K2 O2E 82.5(4) . 8_575 ? O2H K2 O1G 62.2(8) . . ? O2H K2 O1G 107.2(8) 8_575 . ? O2E K2 O1G 110.8(3) . . ? O2E K2 O1G 166.2(3) 8_575 . ? O2H K2 O1G 107.2(8) . 8_575 ? O2H K2 O1G 62.2(8) 8_575 8_575 ? O2E K2 O1G 166.2(3) . 8_575 ? O2E K2 O1G 110.8(3) 8_575 8_575 ? O1G K2 O1G 55.7(5) . 8_575 ? O2H K2 O1E 168.7(7) . 8_575 ? O2H K2 O1E 79.6(8) 8_575 8_575 ? O2E K2 O1E 116.0(3) . 8_575 ? O2E K2 O1E 60.0(3) 8_575 8_575 ? O1G K2 O1E 109.0(3) . 8_575 ? O1G K2 O1E 70.2(3) 8_575 8_575 ? O2H K2 O1E 79.6(8) . . ? O2H K2 O1E 168.7(7) 8_575 . ? O2E K2 O1E 60.0(3) . . ? O2E K2 O1E 116.0(3) 8_575 . ? O1G K2 O1E 70.2(3) . . ? O1G K2 O1E 109.0(3) 8_575 . ? O1E K2 O1E 90.7(4) 8_575 . ? O2H K2 O2G 3.1(10) . . ? O2H K2 O2G 110.5(5) 8_575 . ? O2E K2 O2G 61.1(4) . . ? O2E K2 O2G 127.4(4) 8_575 . ? O1G K2 O2G 64.9(4) . . ? O1G K2 O2G 110.3(4) 8_575 . ? O1E K2 O2G 169.1(5) 8_575 . ? O1E K2 O2G 78.7(4) . . ? O2H K2 O2G 110.5(5) . 8_575 ? O2H K2 O2G 3.1(10) 8_575 8_575 ? O2E K2 O2G 127.4(4) . 8_575 ? O2E K2 O2G 61.1(4) 8_575 8_575 ? O1G K2 O2G 110.3(4) . 8_575 ? O1G K2 O2G 64.9(4) 8_575 8_575 ? O1E K2 O2G 78.7(4) 8_575 8_575 ? O1E K2 O2G 169.1(5) . 8_575 ? O2G K2 O2G 111.6(8) . 8_575 ? O2H K2 O3F 110.2(7) . 8_575 ? O2H K2 O3F 78.6(8) 8_575 8_575 ? O2E K2 O3F 60.9(4) . 8_575 ? O2E K2 O3F 22.4(2) 8_575 8_575 ? O1G K2 O3F 171.4(3) . 8_575 ? O1G K2 O3F 132.7(3) 8_575 8_575 ? O1E K2 O3F 78.0(3) 8_575 8_575 ? O1E K2 O3F 105.4(3) . 8_575 ? O2G K2 O3F 107.4(4) . 8_575 ? O2G K2 O3F 75.4(4) 8_575 8_575 ? O2H K2 O3F 78.6(8) . . ? O2H K2 O3F 110.2(7) 8_575 . ? O2E K2 O3F 22.4(2) . . ? O2E K2 O3F 60.9(4) 8_575 . ? O1G K2 O3F 132.7(3) . . ? O1G K2 O3F 171.4(3) 8_575 . ? O1E K2 O3F 105.4(3) 8_575 . ? O1E K2 O3F 78.0(3) . . ? O2G K2 O3F 75.4(4) . . ? O2G K2 O3F 107.4(4) 8_575 . ? O3F K2 O3F 38.9(4) 8_575 . ? C19 Si2 C19 114.2(4) . 8_565 ? C19 Si2 C13 122.89(19) . . ? C19 Si2 C13 122.89(19) 8_565 . ? C5B O2 C5B 109.0(7) . 8_575 ? C5B O2 K1 120.5(4) . . ? C5B O2 K1 120.5(4) 8_575 . ? C3 C2 C1 123.4(7) . . ? C2 C3 C4 120.7(7) . . ? C5 C4 C3 119.0(7) . . ? C4 C5 C6 119.5(8) . . ? C1 C6 C5 122.2(7) . . ? C12 C7 C8 117.1(11) . . ? C12 C7 Si1 121.1(10) . . ? C8 C7 Si1 121.8(8) . . ? C9 C8 C7 119.1(12) . . ? C10 C9 C8 125.1(15) . . ? C9 C10 C11 118.7(15) . . ? C10 C11 C12 121.8(11) . . ? C7 C12 C11 118.1(11) . . ? C14 C13 C18 116.9(9) . . ? C14 C13 Si2 121.0(8) . . ? C18 C13 Si2 122.1(7) . . ? C15 C14 C13 120.3(10) . . ? C14 C15 C16 123.3(11) . . ? C17 C16 C15 114.4(11) . . ? C18 C17 C16 125.4(11) . . ? C17 C18 C13 119.8(10) . . ? C24 C19 C20 115.4(6) . . ? C24 C19 Si2 122.1(5) . . ? C20 C19 Si2 122.5(5) . . ? C21 C20 C19 123.8(6) . . ? C22 C21 C20 118.0(7) . . ? C23 C22 C21 121.5(7) . . ? C22 C23 C24 118.9(6) . . ? C19 C24 C23 122.4(6) . . ? O1B C1A O2A 44.4(5) . . ? O1B C1A C1A 118.8(5) . 8_575 ? O2A C1A C1A 109.9(4) . 8_575 ? C2A O2A C1A 115.3(10) . . ? C2A O2A K1 104.2(9) . . ? C1A O2A K1 106.2(6) . . ? C3A C2A O2A 99.0(14) . . ? C2A C3A O2B 107.7(11) . . ? C1A O1B C1B 114.1(12) . . ? C1A O1B K1 121.7(6) . . ? C1B O1B K1 114.9(10) . . ? C3A O2B C4B 115.3(6) . . ? C3A O2B K1 117.3(5) . . ? C4B O2B K1 110.5(4) . . ? O2B C4B C5B 111.9(6) . . ? O2 C5B C4B 107.0(6) . . ? C2C O1C C1C 117.0(13) . . ? C2C O1C K1 116.0(10) . . ? C1C O1C K1 110.7(6) . . ? O1C C1C O1C 91.4(9) . 8_575 ? O1C C2C C3C 106.0(15) . . ? C4D O3C C4D 125(2) . 8_575 ? C4D O3C K1 114.0(11) . . ? C4D O3C K1 114.0(11) 8_575 . ? C2C C3C O2D 112.0(12) . . ? O2D C4C C5C 95.7(11) . . ? C5C C5C C4C 139.3(8) 8_575 . ? C5C C5C K1 79.7(3) 8_575 . ? C4C C5C K1 97.0(9) . . ? C1D O1D C2D 106.5(14) . . ? C1D O1D K1 117.2(10) . . ? C2D O1D K1 116.1(9) . . ? C4C O2D C3C 135.3(12) . . ? C4C O2D K1 109.9(8) . . ? C3C O2D K1 97.9(8) . . ? O1D C2D O3D 93.5(12) . . ? C3D O3D C2D 129.3(16) . . ? C3D O3D K1 104.6(11) . . ? C2D O3D K1 100.3(10) . . ? O3D C3D C4D 112.9(12) . . ? O3C C4D C3D 110.6(13) . . ? C3E O1E K2 117.2(10) . . ? C4E O2E C5E 110.7(12) . . ? C4E O2E K2 115.1(8) . . ? C5E O2E K2 118.8(9) . . ? C3F C2E O1F 121.7(13) . . ? O1E C3E C4E 107.4(12) . . ? O2E C4E C3E 108.2(12) . . ? O2E C5E C6E 101.9(14) . . ? C5E C6E C5E 106.6(12) 8_575 . ? O1F O1F C2E 134.8(5) 8_575 . ? O1F O1F K2 78.99(14) 8_575 . ? C2E O1F K2 111.3(6) . . ? C4F O2F C3F 117.9(12) . . ? C4F O2F K2 106.3(8) . . ? C3F O2F K2 104.7(11) . . ? C5F O3F K2 118.3(10) . . ? C2E C3F O2F 111.7(15) . . ? C5F C4F O2F 104.3(11) . . ? C4F C5F O3F 108.7(15) . . ? C1G O1G C2G 110.7(14) . . ? C1G O1G K2 119.8(7) . . ? C2G O1G K2 113.9(14) . . ? C1G C1G O1G 120.2(7) 8_575 . ? C4H O2G C3G 130.1(16) . . ? C4H O2G K2 110.2(11) . . ? C3G O2G K2 102.1(9) . . ? O1G C2G C3G 110(2) . . ? C5G O3G C5G 90.4(17) . 8_575 ? C5G O3G C5H 19.1(10) . . ? C5G O3G C5H 107.5(11) 8_575 . ? C5G O3G C5H 107.5(11) . 8_575 ? C5G O3G C5H 19.1(10) 8_575 8_575 ? C5H O3G C5H 122.8(14) . 8_575 ? C5G O3G K2 118.1(9) . . ? C5G O3G K2 118.1(9) 8_575 . ? C5H O3G K2 114.3(7) . . ? C5H O3G K2 114.3(7) 8_575 . ? C2G C3G O2G 106.5(16) . . ? C5G C4G O2H 114.8(18) . . ? O3G C5G C4G 101.2(14) . . ? C1H O1H C2H 103.1(14) . . ? C1H O1H K2 111.5(14) . . ? C2H O1H K2 103.9(7) . . ? C3H O2H C4G 99(2) . . ? C3H O2H K2 138(2) . . ? C4G O2H K2 115.4(16) . . ? O1H C2H C3H 104.5(12) . . ? O2H C3H C2H 99.7(17) . . ? O2G C4H C5H 102.0(13) . . ? O3G C5H C4H 109.0(11) . . ? C2S C1S C3S 14(3) . . ? C1S C2S C3S 154(5) . . ? C1S C2S C4S 157(5) . . ? C3S C2S C4S 49(2) . . ? C2S C3S C4S 92(2) . . ? C2S C3S C1S 12(2) . . ? C4S C3S C1S 104(2) . . ? C5S C4S C3S 97(3) . . ? C5S C4S C2S 137(4) . . ? C3S C4S C2S 39.4(17) . . ? C6S C5S C4S 129(3) . . ? C6S C5S C7S 40.6(14) . . ? C4S C5S C7S 170(3) . . ? C7S C6S C5S 90(2) . . ? C6S C7S C5S 49.8(17) . . ? 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 C1 Si1 C1 C2 -96.4(6) 8_565 . . . ? C7 Si1 C1 C2 83.0(7) . . . . ? C1 Si1 C1 C6 80.8(6) 8_565 . . . ? C7 Si1 C1 C6 -99.7(7) . . . . ? O1C K1 O2 C5B 85.6(6) 8_575 . . . ? O1C K1 O2 C5B 132.7(6) . . . . ? O1D K1 O2 C5B 145.8(6) . . . . ? O1D K1 O2 C5B 72.5(6) 8_575 . . . ? O1B K1 O2 C5B -40.8(6) . . . . ? O1B K1 O2 C5B -100.8(6) 8_575 . . . ? O2B K1 O2 C5B 3.8(5) . . . . ? O2B K1 O2 C5B -145.4(6) 8_575 . . . ? O2D K1 O2 C5B -174.9(6) . . . . ? O2D K1 O2 C5B 33.3(7) 8_575 . . . ? O3C K1 O2 C5B 109.2(6) . . . . ? O1C K1 O2 C5B -132.7(6) 8_575 . . 8_575 ? O1C K1 O2 C5B -85.6(6) . . . 8_575 ? O1D K1 O2 C5B -72.5(6) . . . 8_575 ? O1D K1 O2 C5B -145.8(6) 8_575 . . 8_575 ? O1B K1 O2 C5B 100.8(6) . . . 8_575 ? O1B K1 O2 C5B 40.8(6) 8_575 . . 8_575 ? O2B K1 O2 C5B 145.4(6) . . . 8_575 ? O2B K1 O2 C5B -3.8(5) 8_575 . . 8_575 ? O2D K1 O2 C5B -33.3(7) . . . 8_575 ? O2D K1 O2 C5B 174.9(6) 8_575 . . 8_575 ? O3C K1 O2 C5B -109.2(6) . . . 8_575 ? C6 C1 C2 C3 0.4(9) . . . . ? Si1 C1 C2 C3 177.9(5) . . . . ? C1 C2 C3 C4 -0.2(10) . . . . ? C2 C3 C4 C5 -1.4(10) . . . . ? C3 C4 C5 C6 2.7(10) . . . . ? C2 C1 C6 C5 0.9(9) . . . . ? Si1 C1 C6 C5 -176.6(5) . . . . ? C4 C5 C6 C1 -2.5(10) . . . . ? C1 Si1 C7 C12 90.3(4) . . . . ? C1 Si1 C7 C12 -90.3(4) 8_565 . . . ? C1 Si1 C7 C8 -89.7(4) . . . . ? C1 Si1 C7 C8 89.7(4) 8_565 . . . ? C12 C7 C8 C9 0.000(4) . . . . ? Si1 C7 C8 C9 180.000(3) . . . . ? C7 C8 C9 C10 0.000(5) . . . . ? C8 C9 C10 C11 0.000(5) . . . . ? C9 C10 C11 C12 0.000(4) . . . . ? C8 C7 C12 C11 0.000(3) . . . . ? Si1 C7 C12 C11 180.000(2) . . . . ? C10 C11 C12 C7 0.000(3) . . . . ? C19 Si2 C13 C14 -89.3(3) . . . . ? C19 Si2 C13 C14 89.3(3) 8_565 . . . ? C19 Si2 C13 C18 90.7(3) . . . . ? C19 Si2 C13 C18 -90.7(3) 8_565 . . . ? C18 C13 C14 C15 0.000(1) . . . . ? Si2 C13 C14 C15 180.0 . . . . ? C13 C14 C15 C16 0.000(1) . . . . ? C14 C15 C16 C17 0.000(1) . . . . ? C15 C16 C17 C18 0.000(1) . . . . ? C16 C17 C18 C13 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? Si2 C13 C18 C17 180.0 . . . . ? C19 Si2 C19 C24 93.7(6) 8_565 . . . ? C13 Si2 C19 C24 -87.6(6) . . . . ? C19 Si2 C19 C20 -83.5(6) 8_565 . . . ? C13 Si2 C19 C20 95.2(6) . . . . ? C24 C19 C20 C21 -0.7(9) . . . . ? Si2 C19 C20 C21 176.7(5) . . . . ? C19 C20 C21 C22 1.1(10) . . . . ? C20 C21 C22 C23 -0.5(10) . . . . ? C21 C22 C23 C24 -0.4(10) . . . . ? C20 C19 C24 C23 -0.2(9) . . . . ? Si2 C19 C24 C23 -177.6(5) . . . . ? C22 C23 C24 C19 0.8(9) . . . . ? O1B C1A O2A C2A 59.6(12) . . . . ? C1A C1A O2A C2A 170.8(10) 8_575 . . . ? O1B C1A O2A K1 -55.2(7) . . . . ? C1A C1A O2A K1 56.0(5) 8_575 . . . ? O1C K1 O2A C2A 28.5(11) 8_575 . . . ? O1C K1 O2A C2A 89.2(12) . . . . ? O1D K1 O2A C2A 136.0(13) . . . . ? O1D K1 O2A C2A 12.5(10) 8_575 . . . ? O1B K1 O2A C2A -72.8(11) . . . . ? O1B K1 O2A C2A -157.9(10) 8_575 . . . ? O2B K1 O2A C2A 36.0(9) . . . . ? O2B K1 O2A C2A 149.8(9) 8_575 . . . ? O2 K1 O2A C2A 90.9(9) . . . . ? O2D K1 O2A C2A -139.8(9) . . . . ? O2D K1 O2A C2A -34.4(9) 8_575 . . . ? O3C K1 O2A C2A -85.3(9) . . . . ? O1C K1 O2A C1A 150.7(5) 8_575 . . . ? O1C K1 O2A C1A -148.5(8) . . . . ? O1D K1 O2A C1A -101.8(12) . . . . ? O1D K1 O2A C1A 134.7(6) 8_575 . . . ? O1B K1 O2A C1A 49.4(7) . . . . ? O1B K1 O2A C1A -35.7(6) 8_575 . . . ? O2B K1 O2A C1A 158.2(7) . . . . ? O2B K1 O2A C1A -88.0(6) 8_575 . . . ? O2 K1 O2A C1A -146.8(6) . . . . ? O2D K1 O2A C1A -17.6(7) . . . . ? O2D K1 O2A C1A 87.8(6) 8_575 . . . ? O3C K1 O2A C1A 36.9(6) . . . . ? C1A O2A C2A C3A 169.2(10) . . . . ? K1 O2A C2A C3A -74.8(12) . . . . ? O2A C2A C3A O2B 80.2(12) . . . . ? O2A C1A O1B C1B -64.8(12) . . . . ? C1A C1A O1B C1B -154.5(10) 8_575 . . . ? O2A C1A O1B K1 80.2(8) . . . . ? C1A C1A O1B K1 -9.5(9) 8_575 . . . ? O1C K1 O1B C1A -167.1(7) 8_575 . . . ? O1C K1 O1B C1A -149(2) . . . . ? O1D K1 O1B C1A 48(2) . . . . ? O1D K1 O1B C1A -176.9(8) 8_575 . . . ? O1B K1 O1B C1A 9.5(9) 8_575 . . . ? O2B K1 O1B C1A -132.1(9) . . . . ? O2B K1 O1B C1A -26.4(9) 8_575 . . . ? O2 K1 O1B C1A -89.1(8) . . . . ? O2D K1 O1B C1A 50.6(9) . . . . ? O2D K1 O1B C1A 149.3(9) 8_575 . . . ? O3C K1 O1B C1A 95.4(8) . . . . ? O1C K1 O1B C1B -22.4(13) 8_575 . . . ? O1C K1 O1B C1B -4(3) . . . . ? O1D K1 O1B C1B -168(2) . . . . ? O1D K1 O1B C1B -32.2(13) 8_575 . . . ? O1B K1 O1B C1B 154.3(12) 8_575 . . . ? O2B K1 O1B C1B 12.7(12) . . . . ? O2B K1 O1B C1B 118.3(12) 8_575 . . . ? O2 K1 O1B C1B 55.6(12) . . . . ? O2D K1 O1B C1B -164.7(12) . . . . ? O2D K1 O1B C1B -66.0(12) 8_575 . . . ? O3C K1 O1B C1B -119.8(12) . . . . ? C2A C3A O2B C4B -176.6(10) . . . . ? C2A C3A O2B K1 -43.9(12) . . . . ? O1C K1 O2B C3A 175.3(5) 8_575 . . . ? O1C K1 O2B C3A -159.1(5) . . . . ? O1D K1 O2B C3A -156.8(5) . . . . ? O1D K1 O2B C3A 159.1(6) 8_575 . . . ? O1B K1 O2B C3A 23.1(5) . . . . ? O1B K1 O2B C3A -10.9(5) 8_575 . . . ? O2B K1 O2B C3A -78.6(5) 8_575 . . . ? O2 K1 O2B C3A -107.2(5) . . . . ? O2D K1 O2B C3A 58(4) . . . . ? O2D K1 O2B C3A 98.3(5) 8_575 . . . ? O3C K1 O2B C3A 83.1(7) . . . . ? O1C K1 O2B C4B -49.9(5) 8_575 . . . ? O1C K1 O2B C4B -24.3(5) . . . . ? O1D K1 O2B C4B -22.0(6) . . . . ? O1D K1 O2B C4B -66.0(5) 8_575 . . . ? O1B K1 O2B C4B 157.9(5) . . . . ? O1B K1 O2B C4B 123.9(5) 8_575 . . . ? O2B K1 O2B C4B 56.2(5) 8_575 . . . ? O2 K1 O2B C4B 27.6(5) . . . . ? O2D K1 O2B C4B -167(3) . . . . ? O2D K1 O2B C4B -126.9(5) 8_575 . . . ? O3C K1 O2B C4B -142.1(7) . . . . ? C3A O2B C4B C5B 77.0(8) . . . . ? K1 O2B C4B C5B -58.8(7) . . . . ? C5B O2 C5B C4B -177.6(5) 8_575 . . . ? K1 O2 C5B C4B -32.1(8) . . . . ? O2B C4B C5B O2 60.6(9) . . . . ? O1C K1 O1C C2C -125.2(11) 8_575 . . . ? O1D K1 O1C C2C 24.8(13) . . . . ? O1D K1 O1C C2C -115.7(13) 8_575 . . . ? O1B K1 O1C C2C -146(2) . . . . ? O1B K1 O1C C2C 58.0(12) 8_575 . . . ? O2B K1 O1C C2C -161.5(10) . . . . ? O2B K1 O1C C2C 90.1(11) 8_575 . . . ? O2 K1 O1C C2C 152.8(12) . . . . ? O2D K1 O1C C2C 15.8(11) . . . . ? O2D K1 O1C C2C -86.0(11) 8_575 . . . ? O3C K1 O1C C2C -30.8(11) . . . . ? O1C K1 O1C C1C 11.2(8) 8_575 . . . ? O1D K1 O1C C1C 161.2(19) . . . . ? O1D K1 O1C C1C 20.7(7) 8_575 . . . ? O1B K1 O1C C1C -9(3) . . . . ? O1B K1 O1C C1C -165.6(7) 8_575 . . . ? O2B K1 O1C C1C -25.1(8) . . . . ? O2B K1 O1C C1C -133.6(7) 8_575 . . . ? O2 K1 O1C C1C -70.8(7) . . . . ? O2D K1 O1C C1C 152.2(8) . . . . ? O2D K1 O1C C1C 50.4(8) 8_575 . . . ? O3C K1 O1C C1C 105.5(7) . . . . ? C2C O1C C1C O1C 121.0(10) . . . 8_575 ? K1 O1C C1C O1C -14.9(10) . . . 8_575 ? C1C O1C C2C C3C 179.8(10) . . . . ? K1 O1C C2C C3C -46.6(13) . . . . ? O1C K1 O3C C4D 126.7(14) 8_575 . . . ? O1C K1 O3C C4D 81.4(15) . . . . ? O1D K1 O3C C4D 67.8(15) . . . . ? O1D K1 O3C C4D 140.3(14) 8_575 . . . ? O1B K1 O3C C4D -105.1(15) . . . . ? O1B K1 O3C C4D -46.8(14) 8_575 . . . ? O2B K1 O3C C4D -155.9(12) . . . . ? O2B K1 O3C C4D 4.0(17) 8_575 . . . ? O2 K1 O3C C4D 104.0(14) . . . . ? O2D K1 O3C C4D 21.9(12) . . . . ? O2D K1 O3C C4D -173.8(17) 8_575 . . . ? O1C K1 O3C C4D -81.4(15) 8_575 . . 8_575 ? O1C K1 O3C C4D -126.7(14) . . . 8_575 ? O1D K1 O3C C4D -140.3(14) . . . 8_575 ? O1D K1 O3C C4D -67.8(15) 8_575 . . 8_575 ? O1B K1 O3C C4D 46.8(14) . . . 8_575 ? O1B K1 O3C C4D 105.1(15) 8_575 . . 8_575 ? O2B K1 O3C C4D -4.0(17) . . . 8_575 ? O2B K1 O3C C4D 155.9(12) 8_575 . . 8_575 ? O2 K1 O3C C4D -104.0(14) . . . 8_575 ? O2D K1 O3C C4D 173.8(17) . . . 8_575 ? O2D K1 O3C C4D -21.9(12) 8_575 . . 8_575 ? O1C C2C C3C O2D 69.6(15) . . . . ? O2D C4C C5C C5C 106.1(11) . . . 8_575 ? O2D C4C C5C K1 23.8(9) . . . . ? O1C K1 C5C C5C -70.1(4) 8_575 . . 8_575 ? O1C K1 C5C C5C -120.0(3) . . . 8_575 ? O1D K1 C5C C5C -130.0(3) . . . 8_575 ? O1D K1 C5C C5C -54.9(3) 8_575 . . 8_575 ? O1B K1 C5C C5C 54.6(2) . . . 8_575 ? O1B K1 C5C C5C 117.4(2) 8_575 . . 8_575 ? O2B K1 C5C C5C 23.5(2) . . . 8_575 ? O2B K1 C5C C5C 160.4(2) 8_575 . . 8_575 ? O2 K1 C5C C5C 133.4(12) . . . 8_575 ? O2D K1 C5C C5C -156.4(4) . . . 8_575 ? O2D K1 C5C C5C -19.0(3) 8_575 . . 8_575 ? O3C K1 C5C C5C -63.4(9) . . . 8_575 ? O1C K1 C5C C4C 68.8(9) 8_575 . . . ? O1C K1 C5C C4C 18.9(9) . . . . ? O1D K1 C5C C4C 8.9(9) . . . . ? O1D K1 C5C C4C 84.0(8) 8_575 . . . ? O1B K1 C5C C4C -166.5(9) . . . . ? O1B K1 C5C C4C -103.6(8) 8_575 . . . ? O2B K1 C5C C4C 162.4(7) . . . . ? O2B K1 C5C C4C -60.6(9) 8_575 . . . ? O2 K1 C5C C4C -87.7(16) . . . . ? O2D K1 C5C C4C -17.4(7) . . . . ? O2D K1 C5C C4C 119.9(9) 8_575 . . . ? O3C K1 C5C C4C 75.5(11) . . . . ? O1C K1 O1D C1D -14.2(11) 8_575 . . . ? O1C K1 O1D C1D -38.2(12) . . . . ? O1D K1 O1D C1D -3.2(13) 8_575 . . . ? O1B K1 O1D C1D 134.8(18) . . . . ? O1B K1 O1D C1D 169.7(11) 8_575 . . . ? O2B K1 O1D C1D -45.6(13) . . . . ? O2B K1 O1D C1D -147.6(12) 8_575 . . . ? O2 K1 O1D C1D -87.2(12) . . . . ? O2D K1 O1D C1D 131.5(13) . . . . ? O2D K1 O1D C1D 36.9(13) 8_575 . . . ? O3C K1 O1D C1D 87.5(12) . . . . ? O1C K1 O1D C2D -141.6(11) 8_575 . . . ? O1C K1 O1D C2D -166(2) . . . . ? O1D K1 O1D C2D -130.7(9) 8_575 . . . ? O1B K1 O1D C2D 7(3) . . . . ? O1B K1 O1D C2D 42.3(11) 8_575 . . . ? O2B K1 O1D C2D -173.1(9) . . . . ? O2B K1 O1D C2D 84.9(10) 8_575 . . . ? O2 K1 O1D C2D 145.3(10) . . . . ? O2D K1 O1D C2D 4.0(9) . . . . ? O2D K1 O1D C2D -90.5(10) 8_575 . . . ? O3C K1 O1D C2D -40.0(10) . . . . ? C5C C4C O2D C3C -152.6(14) . . . . ? C5C C4C O2D K1 -27.5(10) . . . . ? C2C C3C O2D C4C 78.9(19) . . . . ? C2C C3C O2D K1 -50.2(13) . . . . ? O1C K1 O2D C4C -97.8(8) 8_575 . . . ? O1C K1 O2D C4C -125.5(9) . . . . ? O1D K1 O2D C4C -128.5(9) . . . . ? O1D K1 O2D C4C -81.0(9) 8_575 . . . ? O1B K1 O2D C4C 52.1(9) . . . . ? O1B K1 O2D C4C 88.8(8) 8_575 . . . ? O2B K1 O2D C4C 18(4) . . . . ? O2B K1 O2D C4C 156.1(9) 8_575 . . . ? O2 K1 O2D C4C -177.1(7) . . . . ? O2D K1 O2D C4C -21.1(10) 8_575 . . . ? O3C K1 O2D C4C -8.0(9) . . . . ? O1C K1 O2D C3C 46.6(8) 8_575 . . . ? O1C K1 O2D C3C 19.0(8) . . . . ? O1D K1 O2D C3C 15.9(8) . . . . ? O1D K1 O2D C3C 63.4(9) 8_575 . . . ? O1B K1 O2D C3C -163.5(8) . . . . ? O1B K1 O2D C3C -126.8(8) 8_575 . . . ? O2B K1 O2D C3C 163(3) . . . . ? O2B K1 O2D C3C -59.5(8) 8_575 . . . ? O2 K1 O2D C3C -32.7(9) . . . . ? O2D K1 O2D C3C 123.4(7) 8_575 . . . ? O3C K1 O2D C3C 136.5(10) . . . . ? C1D O1D C2D O3D -104.9(13) . . . . ? K1 O1D C2D O3D 27.7(14) . . . . ? O1D C2D O3D C3D -141.1(19) . . . . ? O1D C2D O3D K1 -22.5(11) . . . . ? O1C K1 O3D C3D -160.7(12) 8_575 . . . ? O1C K1 O3D C3D 163.4(14) . . . . ? O1D K1 O3D C3D 152.5(15) . . . . ? O1D K1 O3D C3D -144.9(12) 8_575 . . . ? O1B K1 O3D C3D -22.0(14) . . . . ? O1B K1 O3D C3D 25.7(12) 8_575 . . . ? O2B K1 O3D C3D -136.7(10) . . . . ? O2B K1 O3D C3D 87.9(12) 8_575 . . . ? O2 K1 O3D C3D 134.5(11) . . . . ? O2D K1 O3D C3D 32.2(10) . . . . ? O2D K1 O3D C3D -88.4(12) 8_575 . . . ? O3C K1 O3D C3D -54.2(11) . . . . ? O1C K1 O3D C2D 63.9(11) 8_575 . . . ? O1C K1 O3D C2D 28.0(10) . . . . ? O1D K1 O3D C2D 17.1(9) . . . . ? O1D K1 O3D C2D 79.8(11) 8_575 . . . ? O1B K1 O3D C2D -157.4(9) . . . . ? O1B K1 O3D C2D -109.7(11) 8_575 . . . ? O2B K1 O3D C2D 87.9(14) . . . . ? O2B K1 O3D C2D -47.5(10) 8_575 . . . ? O2 K1 O3D C2D -0.9(12) . . . . ? O2D K1 O3D C2D -103.2(16) . . . . ? O2D K1 O3D C2D 136.2(10) 8_575 . . . ? O3C K1 O3D C2D 170.5(14) . . . . ? C2D O3D C3D C4D 172.3(15) . . . . ? K1 O3D C3D C4D 55.5(14) . . . . ? C4D O3C C4D C3D 166.9(16) 8_575 . . . ? K1 O3C C4D C3D -44.8(16) . . . . ? O3D C3D C4D O3C -12(2) . . . . ? O2H K2 O1E C3E -78.7(13) . . . . ? O2H K2 O1E C3E 139(4) 8_575 . . . ? O2E K2 O1E C3E -12.7(10) . . . . ? O2E K2 O1E C3E 50.6(11) 8_575 . . . ? O1G K2 O1E C3E -142.8(11) . . . . ? O1G K2 O1E C3E 176.5(10) 8_575 . . . ? O1E K2 O1E C3E 107.2(10) 8_575 . . . ? O2G K2 O1E C3E -75.6(11) . . . . ? O2G K2 O1E C3E 122(2) 8_575 . . . ? O3F K2 O1E C3E 29.5(11) 8_575 . . . ? O3F K2 O1E C3E 1.7(10) . . . . ? O2H K2 O2E C4E 69.0(12) . . . . ? O2H K2 O2E C4E 163.3(13) 8_575 . . . ? O2E K2 O2E C4E -149.7(9) 8_575 . . . ? O1G K2 O2E C4E 26.6(10) . . . . ? O1G K2 O2E C4E 15.7(19) 8_575 . . . ? O1E K2 O2E C4E -98.4(10) 8_575 . . . ? O1E K2 O2E C4E -23.7(9) . . . . ? O2G K2 O2E C4E 69.8(10) . . . . ? O2G K2 O2E C4E 165.9(10) 8_575 . . . ? O3F K2 O2E C4E -155.9(11) 8_575 . . . ? O3F K2 O2E C4E -164.2(15) . . . . ? O2H K2 O2E C5E -156.3(14) . . . . ? O2H K2 O2E C5E -62.0(15) 8_575 . . . ? O2E K2 O2E C5E -15.0(12) 8_575 . . . ? O1G K2 O2E C5E 161.3(11) . . . . ? O1G K2 O2E C5E 150.4(14) 8_575 . . . ? O1E K2 O2E C5E 36.3(12) 8_575 . . . ? O1E K2 O2E C5E 111.0(11) . . . . ? O2G K2 O2E C5E -155.5(13) . . . . ? O2G K2 O2E C5E -59.4(12) 8_575 . . . ? O3F K2 O2E C5E -21.2(10) 8_575 . . . ? O3F K2 O2E C5E -29.5(10) . . . . ? K2 O1E C3E C4E 42.1(15) . . . . ? C5E O2E C4E C3E -84.2(14) . . . . ? K2 O2E C4E C3E 54.1(14) . . . . ? O1E C3E C4E O2E -63.4(16) . . . . ? C4E O2E C5E C6E -174.2(10) . . . . ? K2 O2E C5E C6E 49.3(12) . . . . ? O2E C5E C6E C5E -105.2(11) . . . 8_575 ? C3F C2E O1F O1F 121.6(13) . . . 8_575 ? C3F C2E O1F K2 26.0(14) . . . . ? O2H K2 O1F O1F 159.0(8) . . . 8_575 ? O2H K2 O1F O1F 25.7(10) 8_575 . . 8_575 ? O2E K2 O1F O1F -135.4(2) . . . 8_575 ? O2E K2 O1F O1F -49.5(3) 8_575 . . 8_575 ? O1G K2 O1F O1F 115.8(3) . . . 8_575 ? O1G K2 O1F O1F 56.0(2) 8_575 . . 8_575 ? O1E K2 O1F O1F -20.6(3) 8_575 . . 8_575 ? O1E K2 O1F O1F -151.9(4) . . . 8_575 ? O2G K2 O1F O1F 162.2(3) . . . 8_575 ? O2G K2 O1F O1F 22.0(4) 8_575 . . 8_575 ? O3F K2 O1F O1F -73.8(2) 8_575 . . 8_575 ? O3F K2 O1F O1F -116.5(2) . . . 8_575 ? O2H K2 O1F C2E -67.1(10) . . . . ? O2H K2 O1F C2E 159.6(11) 8_575 . . . ? O2E K2 O1F C2E -1.4(6) . . . . ? O2E K2 O1F C2E 84.4(6) 8_575 . . . ? O1G K2 O1F C2E -110.2(6) . . . . ? O1G K2 O1F C2E -170.1(7) 8_575 . . . ? O1E K2 O1F C2E 113.3(7) 8_575 . . . ? O1E K2 O1F C2E -17.9(6) . . . . ? O2G K2 O1F C2E -63.8(7) . . . . ? O2G K2 O1F C2E 155.9(6) 8_575 . . . ? O3F K2 O1F C2E 60.2(6) 8_575 . . . ? O3F K2 O1F C2E 17.5(7) . . . . ? O2H K2 O2F C4F -43.4(11) . . . . ? O2H K2 O2F C4F 93(2) 8_575 . . . ? O2E K2 O2F C4F 10.6(7) . . . . ? O2E K2 O2F C4F 86.3(8) 8_575 . . . ? O1G K2 O2F C4F -105.2(8) . . . . ? O1G K2 O2F C4F -153.4(8) 8_575 . . . ? O1E K2 O2F C4F 145.9(8) 8_575 . . . ? O1E K2 O2F C4F -114.8(10) . . . . ? O2G K2 O2F C4F -41.0(8) . . . . ? O2G K2 O2F C4F 90.6(12) 8_575 . . . ? O3F K2 O2F C4F 67.6(8) 8_575 . . . ? O3F K2 O2F C4F 34.7(8) . . . . ? O2H K2 O2F C3F 82.0(12) . . . . ? O2H K2 O2F C3F -142(2) 8_575 . . . ? O2E K2 O2F C3F 136.1(11) . . . . ? O2E K2 O2F C3F -148.3(9) 8_575 . . . ? O1G K2 O2F C3F 20.2(10) . . . . ? O1G K2 O2F C3F -27.9(10) 8_575 . . . ? O1E K2 O2F C3F -88.6(9) 8_575 . . . ? O1E K2 O2F C3F 10.7(10) . . . . ? O2G K2 O2F C3F 84.4(10) . . . . ? O2G K2 O2F C3F -143.9(13) 8_575 . . . ? O3F K2 O2F C3F -167.0(10) 8_575 . . . ? O3F K2 O2F C3F 160.2(10) . . . . ? O2H K2 O3F C5F 95.1(13) . . . . ? O2H K2 O3F C5F -158.4(13) 8_575 . . . ? O2E K2 O3F C5F 47.8(11) . . . . ? O2E K2 O3F C5F -115.7(11) 8_575 . . . ? O1G K2 O3F C5F 61.6(12) . . . . ? O1G K2 O3F C5F -132(2) 8_575 . . . ? O1E K2 O3F C5F -74.0(11) 8_575 . . . ? O1E K2 O3F C5F 13.4(10) . . . . ? O2G K2 O3F C5F 94.8(11) . . . . ? O2G K2 O3F C5F -156.8(11) 8_575 . . . ? O3F K2 O3F C5F -120.7(10) 8_575 . . . ? O1F C2E C3F O2F -64.8(19) . . . . ? C4F O2F C3F C2E -179.2(13) . . . . ? K2 O2F C3F C2E 63.0(17) . . . . ? C3F O2F C4F C5F 173.1(15) . . . . ? K2 O2F C4F C5F -69.9(12) . . . . ? O2F C4F C5F O3F 72.7(15) . . . . ? K2 O3F C5F C4F -36.9(15) . . . . ? O2H K2 O1G C1G 123.1(13) . . . . ? O2H K2 O1G C1G 19.9(12) 8_575 . . . ? O2E K2 O1G C1G 166.4(9) . . . . ? O2E K2 O1G C1G -29.2(18) 8_575 . . . ? O1G K2 O1G C1G -16.8(10) 8_575 . . . ? O1E K2 O1G C1G -64.8(9) 8_575 . . . ? O1E K2 O1G C1G -148.5(10) . . . . ? O2G K2 O1G C1G 125.0(10) . . . . ? O2G K2 O1G C1G 19.9(10) 8_575 . . . ? O3F K2 O1G C1G 151.1(18) 8_575 . . . ? O3F K2 O1G C1G 160.8(8) . . . . ? O2H K2 O1G C2G -11.2(16) . . . . ? O2H K2 O1G C2G -114.4(16) 8_575 . . . ? O2E K2 O1G C2G 32.1(15) . . . . ? O2E K2 O1G C2G -163.5(16) 8_575 . . . ? O1G K2 O1G C2G -151.1(14) 8_575 . . . ? O1E K2 O1G C2G 160.9(14) 8_575 . . . ? O1E K2 O1G C2G 77.2(15) . . . . ? O2G K2 O1G C2G -9.3(15) . . . . ? O2G K2 O1G C2G -114.4(15) 8_575 . . . ? O3F K2 O1G C2G 17(3) 8_575 . . . ? O3F K2 O1G C2G 26.5(16) . . . . ? C2G O1G C1G C1G 152.8(14) . . . 8_575 ? K2 O1G C1G C1G 17.2(10) . . . 8_575 ? O2H K2 O2G C4H -135(21) . . . . ? O2H K2 O2G C4H -67.5(12) 8_575 . . . ? O2E K2 O2G C4H 57.4(10) . . . . ? O2E K2 O2G C4H 5.0(14) 8_575 . . . ? O1G K2 O2G C4H -167.5(13) . . . . ? O1G K2 O2G C4H -134.4(11) 8_575 . . . ? O1E K2 O2G C4H 135(2) 8_575 . . . ? O1E K2 O2G C4H 119.2(11) . . . . ? O2G K2 O2G C4H -64.4(12) 8_575 . . . ? O3F K2 O2G C4H 16.5(12) 8_575 . . . ? O3F K2 O2G C4H 38.9(11) . . . . ? O2H K2 O2G C3G 6(20) . . . . ? O2H K2 O2G C3G 73.8(11) 8_575 . . . ? O2E K2 O2G C3G -161.2(12) . . . . ? O2E K2 O2G C3G 146.4(9) 8_575 . . . ? O1G K2 O2G C3G -26.1(9) . . . . ? O1G K2 O2G C3G 6.9(11) 8_575 . . . ? O1E K2 O2G C3G -84(2) 8_575 . . . ? O1E K2 O2G C3G -99.4(10) . . . . ? O2G K2 O2G C3G 77.0(12) 8_575 . . . ? O3F K2 O2G C3G 157.8(9) 8_575 . . . ? O3F K2 O2G C3G -179.7(11) . . . . ? C1G O1G C2G C3G -92.5(19) . . . . ? K2 O1G C2G C3G 46(2) . . . . ? O2H K2 O3G C5G -18.1(13) . . . . ? O2H K2 O3G C5G 125.2(14) 8_575 . . . ? O2E K2 O3G C5G -84.3(10) . . . . ? O2E K2 O3G C5G -168.6(11) 8_575 . . . ? O1G K2 O3G C5G 24.5(11) . . . . ? O1G K2 O3G C5G 82.6(10) 8_575 . . . ? O1E K2 O3G C5G 160.3(10) 8_575 . . . ? O1E K2 O3G C5G -53.2(11) . . . . ? O2G K2 O3G C5G -21.7(11) . . . . ? O2G K2 O3G C5G 128.8(11) 8_575 . . . ? O3F K2 O3G C5G -147.1(10) 8_575 . . . ? O3F K2 O3G C5G -105.8(10) . . . . ? O2H K2 O3G C5G -125.2(14) . . . 8_575 ? O2H K2 O3G C5G 18.1(13) 8_575 . . 8_575 ? O2E K2 O3G C5G 168.6(11) . . . 8_575 ? O2E K2 O3G C5G 84.3(10) 8_575 . . 8_575 ? O1G K2 O3G C5G -82.6(10) . . . 8_575 ? O1G K2 O3G C5G -24.5(11) 8_575 . . 8_575 ? O1E K2 O3G C5G 53.2(11) 8_575 . . 8_575 ? O1E K2 O3G C5G -160.3(10) . . . 8_575 ? O2G K2 O3G C5G -128.8(11) . . . 8_575 ? O2G K2 O3G C5G 21.7(11) 8_575 . . 8_575 ? O3F K2 O3G C5G 105.8(10) 8_575 . . 8_575 ? O3F K2 O3G C5G 147.1(10) . . . 8_575 ? O2H K2 O3G C5H 2.8(12) . . . . ? O2H K2 O3G C5H 146.0(12) 8_575 . . . ? O2E K2 O3G C5H -63.4(8) . . . . ? O2E K2 O3G C5H -147.7(8) 8_575 . . . ? O1G K2 O3G C5H 45.3(9) . . . . ? O1G K2 O3G C5H 103.5(8) 8_575 . . . ? O1E K2 O3G C5H -178.8(8) 8_575 . . . ? O1E K2 O3G C5H -32.3(9) . . . . ? O2G K2 O3G C5H -0.8(8) . . . . ? O2G K2 O3G C5H 149.7(9) 8_575 . . . ? O3F K2 O3G C5H -126.2(8) 8_575 . . . ? O3F K2 O3G C5H -85.0(8) . . . . ? O2H K2 O3G C5H -146.0(12) . . . 8_575 ? O2H K2 O3G C5H -2.8(12) 8_575 . . 8_575 ? O2E K2 O3G C5H 147.7(8) . . . 8_575 ? O2E K2 O3G C5H 63.4(8) 8_575 . . 8_575 ? O1G K2 O3G C5H -103.5(8) . . . 8_575 ? O1G K2 O3G C5H -45.3(9) 8_575 . . 8_575 ? O1E K2 O3G C5H 32.3(9) 8_575 . . 8_575 ? O1E K2 O3G C5H 178.8(8) . . . 8_575 ? O2G K2 O3G C5H -149.7(9) . . . 8_575 ? O2G K2 O3G C5H 0.8(8) 8_575 . . 8_575 ? O3F K2 O3G C5H 85.0(8) 8_575 . . 8_575 ? O3F K2 O3G C5H 126.2(8) . . . 8_575 ? O1G C2G C3G O2G -75(2) . . . . ? C4H O2G C3G C2G -171.1(18) . . . . ? K2 O2G C3G C2G 58.9(15) . . . . ? C5G O3G C5G C4G 169.0(8) 8_575 . . . ? C5H O3G C5G C4G -37(3) . . . . ? C5H O3G C5G C4G 177.6(14) 8_575 . . . ? K2 O3G C5G C4G 46.5(16) . . . . ? O2H C4G C5G O3G -63(2) . . . . ? O2H K2 O1H C1H -152.1(17) . . . . ? O2H K2 O1H C1H 96.8(15) 8_575 . . . ? O2E K2 O1H C1H -127.4(13) . . . . ? O2E K2 O1H C1H 107.7(16) 8_575 . . . ? O1G K2 O1H C1H -32.8(14) . . . . ? O1G K2 O1H C1H 44.0(13) 8_575 . . . ? O1E K2 O1H C1H 16.1(14) 8_575 . . . ? O1E K2 O1H C1H -71.8(13) . . . . ? O2G K2 O1H C1H -151.2(14) . . . . ? O2G K2 O1H C1H 97.7(14) 8_575 . . . ? O3F K2 O1H C1H 168.9(13) 8_575 . . . ? O3F K2 O1H C1H -142.4(13) . . . . ? O2H K2 O1H C2H -41.7(12) . . . . ? O2H K2 O1H C2H -152.8(11) 8_575 . . . ? O2E K2 O1H C2H -17.0(10) . . . . ? O2E K2 O1H C2H -141.9(10) 8_575 . . . ? O1G K2 O1H C2H 77.6(12) . . . . ? O1G K2 O1H C2H 154.4(9) 8_575 . . . ? O1E K2 O1H C2H 126.5(9) 8_575 . . . ? O1E K2 O1H C2H 38.6(9) . . . . ? O2G K2 O1H C2H -40.8(9) . . . . ? O2G K2 O1H C2H -151.9(9) 8_575 . . . ? O3F K2 O1H C2H -80.8(12) 8_575 . . . ? O3F K2 O1H C2H -32.1(10) . . . . ? C5G C4G O2H C3H -104(2) . . . . ? C5G C4G O2H K2 51(3) . . . . ? O2H K2 O2H C3H 94(3) 8_575 . . . ? O2E K2 O2H C3H -141(4) . . . . ? O2E K2 O2H C3H 166(3) 8_575 . . . ? O1G K2 O2H C3H -6(3) . . . . ? O1G K2 O2H C3H 28(4) 8_575 . . . ? O1E K2 O2H C3H -47(7) 8_575 . . . ? O1E K2 O2H C3H -79(3) . . . . ? O2G K2 O2H C3H -153(23) . . . . ? O2G K2 O2H C3H 97(3) 8_575 . . . ? O3F K2 O2H C3H 178(3) 8_575 . . . ? O3F K2 O2H C3H -159(3) . . . . ? O2H K2 O2H C4G -48(3) 8_575 . . . ? O2E K2 O2H C4G 78(2) . . . . ? O2E K2 O2H C4G 24(3) 8_575 . . . ? O1G K2 O2H C4G -148(2) . . . . ? O1G K2 O2H C4G -114(2) 8_575 . . . ? O1E K2 O2H C4G 171(2) 8_575 . . . ? O1E K2 O2H C4G 139(2) . . . . ? O2G K2 O2H C4G 66(20) . . . . ? O2G K2 O2H C4G -45(2) 8_575 . . . ? O3F K2 O2H C4G 37(2) 8_575 . . . ? O3F K2 O2H C4G 60(2) . . . . ? C1H O1H C2H C3H -171.6(17) . . . . ? K2 O1H C2H C3H 72.0(11) . . . . ? C4G O2H C3H C2H 162.9(17) . . . . ? K2 O2H C3H C2H 17(4) . . . . ? O1H C2H C3H O2H -59(2) . . . . ? C3G O2G C4H C5H -57(2) . . . . ? K2 O2G C4H C5H 70.3(12) . . . . ? C5G O3G C5H C4H 142(5) . . . . ? C5G O3G C5H C4H 168.9(15) 8_575 . . . ? C5H O3G C5H C4H -178.4(8) 8_575 . . . ? K2 O3G C5H C4H 35.7(13) . . . . ? O2G C4H C5H O3G -70.1(15) . . . . ? C3S C1S C2S C4S 180.00(3) . . . . ? C1S C2S C3S C4S 180.000(12) . . . . ? C4S C2S C3S C1S 180.000(13) . . . . ? C2S C1S C3S C4S 0.000(14) . . . . ? C2S C3S C4S C5S 180.000(4) . . . . ? C1S C3S C4S C5S 180.000(3) . . . . ? C1S C3S C4S C2S 0.000(6) . . . . ? C1S C2S C4S C5S 180.000(14) . . . . ? C3S C2S C4S C5S 0.000(7) . . . . ? C1S C2S C4S C3S 180.000(18) . . . . ? C3S C4S C5S C6S 0.000(6) . . . . ? C2S C4S C5S C6S 0.000(9) . . . . ? C3S C4S C5S C7S 0.000(19) . . . . ? C2S C4S C5S C7S 0.00(2) . . . . ? C4S C5S C6S C7S 180.000(5) . . . . ? C4S C5S C7S C6S 0.000(17) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.953 _refine_diff_density_min -0.770 _refine_diff_density_rms 0.182 # Attachment '7.CIF' data_7.CIF _database_code_depnum_ccdc_archive 'CCDC 659287' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H47 K O9 Si' _chemical_formula_weight 510.78 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 P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.2574(9) _cell_length_b 15.1610(12) _cell_length_c 20.5984(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2891.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 145(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.266 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9244 _exptl_absorpt_correction_T_max 0.9487 _exptl_absorpt_process_details scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 145(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10561 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.1030 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4928 _reflns_number_gt 3533 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed interface to POVRay' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0755P)^2^+0.7412P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0037(19) _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 0.00(8) _refine_ls_number_reflns 4928 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1049 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1628 _refine_ls_wR_factor_gt 0.1453 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 -0.70062(11) -0.59522(7) -0.08466(5) 0.0393(3) Uani 1 1 d . . . Si1 Si -0.46168(15) -0.43354(9) -0.16055(7) 0.0411(4) Uani 1 1 d . . . O1 O -0.3713(4) -0.4627(2) -0.22893(16) 0.0469(9) Uani 1 1 d . . . C1 C -0.4851(7) -0.5837(4) -0.2836(3) 0.0662(17) Uani 1 1 d . . . H1A H -0.5180 -0.5399 -0.3153 0.099 Uiso 1 1 calc R . . H1B H -0.5607 -0.5931 -0.2511 0.099 Uiso 1 1 calc R . . H1C H -0.4645 -0.6394 -0.3059 0.099 Uiso 1 1 calc R . . H2S H -0.4936 -0.3467 -0.1920 0.052(15) Uiso 1 1 d R . . O2 O -0.3755(4) -0.3940(2) -0.09065(19) 0.0606(10) Uani 1 1 d . . . C2 C -0.3516(6) -0.5513(3) -0.2511(3) 0.0468(13) Uani 1 1 d . . . H2 H -0.3307 -0.5898 -0.2129 0.056 Uiso 1 1 calc R . . O3 O -0.6457(4) -0.4477(2) -0.16245(18) 0.0546(10) Uani 1 1 d . . . C3 C -0.2206(7) -0.5511(5) -0.2957(3) 0.0728(19) Uani 1 1 d . . . H3A H -0.2424 -0.5170 -0.3349 0.109 Uiso 1 1 calc R . . H3B H -0.1966 -0.6119 -0.3078 0.109 Uiso 1 1 calc R . . H3C H -0.1383 -0.5245 -0.2731 0.109 Uiso 1 1 calc R . . O4 O -0.4469(4) -0.6965(2) -0.05812(16) 0.0465(9) Uani 1 1 d . . . C4 C -0.1987(7) -0.2813(4) -0.1100(4) 0.0746(19) Uani 1 1 d . . . H4A H -0.1224 -0.3053 -0.0821 0.112 Uiso 1 1 calc R . . H4B H -0.1892 -0.2170 -0.1123 0.112 Uiso 1 1 calc R . . H4C H -0.1898 -0.3063 -0.1537 0.112 Uiso 1 1 calc R . . O5 O -0.5458(4) -0.5824(2) 0.04121(16) 0.0501(9) Uani 1 1 d . . . C5 C -0.3435(6) -0.3047(3) -0.0822(3) 0.0555(14) Uani 1 1 d . . . H5 H -0.4195 -0.2685 -0.1041 0.067 Uiso 1 1 calc R . . O6 O -0.8140(4) -0.4948(2) 0.02022(18) 0.0522(10) Uani 1 1 d . . . C6 C -0.3454(11) -0.2852(5) -0.0100(4) 0.102(3) Uani 1 1 d . . . H6A H -0.4429 -0.2949 0.0071 0.153 Uiso 1 1 calc R . . H6B H -0.3171 -0.2238 -0.0026 0.153 Uiso 1 1 calc R . . H6C H -0.2774 -0.3245 0.0123 0.153 Uiso 1 1 calc R . . O7 O -1.0247(4) -0.5748(2) -0.05632(17) 0.0520(10) Uani 1 1 d . . . C7 C -0.7946(8) -0.3182(5) -0.1583(4) 0.088(2) Uani 1 1 d . . . H7A H -0.8473 -0.3434 -0.1215 0.132 Uiso 1 1 calc R . . H7B H -0.8602 -0.2818 -0.1843 0.132 Uiso 1 1 calc R . . H7C H -0.7149 -0.2816 -0.1422 0.132 Uiso 1 1 calc R . . O8 O -0.9264(4) -0.6843(2) -0.15644(16) 0.0468(9) Uani 1 1 d . . . C8 C -0.7364(6) -0.3897(4) -0.1987(3) 0.0607(17) Uani 1 1 d . . . H8 H -0.6757 -0.3621 -0.2333 0.073 Uiso 1 1 calc R . . O9 O -0.6601(4) -0.7705(2) -0.13812(16) 0.0476(9) Uani 1 1 d . . . C9 C -0.8536(8) -0.4427(5) -0.2321(4) 0.087(2) Uani 1 1 d . . . H9A H -0.8107 -0.4947 -0.2527 0.130 Uiso 1 1 calc R . . H9B H -0.9005 -0.4062 -0.2652 0.130 Uiso 1 1 calc R . . H9C H -0.9254 -0.4615 -0.2000 0.130 Uiso 1 1 calc R . . C10 C -0.3710(6) -0.6846(4) 0.0022(3) 0.0501(14) Uani 1 1 d . . . H10A H -0.2661 -0.6939 -0.0042 0.060 Uiso 1 1 calc R . . H10B H -0.4060 -0.7274 0.0349 0.060 Uiso 1 1 calc R . . C11 C -0.3997(6) -0.5918(4) 0.0247(2) 0.0527(14) Uani 1 1 d . . . H11A H -0.3386 -0.5783 0.0629 0.063 Uiso 1 1 calc R . . H11B H -0.3747 -0.5497 -0.0103 0.063 Uiso 1 1 calc R . . C12 C -0.5772(7) -0.4951(4) 0.0633(3) 0.0624(16) Uani 1 1 d . . . H12A H -0.5492 -0.4518 0.0297 0.075 Uiso 1 1 calc R . . H12B H -0.5210 -0.4824 0.1031 0.075 Uiso 1 1 calc R . . C13 C -0.7348(7) -0.4871(4) 0.0774(3) 0.0643(17) Uani 1 1 d . . . H13A H -0.7644 -0.5340 0.1081 0.077 Uiso 1 1 calc R . . H13B H -0.7547 -0.4293 0.0978 0.077 Uiso 1 1 calc R . . C14 C -0.9638(7) -0.4785(4) 0.0289(3) 0.0588(16) Uani 1 1 d . . . H14A H -0.9781 -0.4182 0.0464 0.071 Uiso 1 1 calc R . . H14B H -1.0040 -0.5210 0.0606 0.071 Uiso 1 1 calc R . . C15 C -1.0400(7) -0.4873(3) -0.0335(3) 0.0591(16) Uani 1 1 d . . . H15A H -1.1436 -0.4731 -0.0278 0.071 Uiso 1 1 calc R . . H15B H -0.9988 -0.4456 -0.0656 0.071 Uiso 1 1 calc R . . C16 C -1.1066(6) -0.5890(4) -0.1144(3) 0.0598(15) Uani 1 1 d . . . H16A H -1.0809 -0.5439 -0.1472 0.072 Uiso 1 1 calc R . . H16B H -1.2111 -0.5836 -0.1049 0.072 Uiso 1 1 calc R . . C17 C -1.0746(6) -0.6793(4) -0.1405(3) 0.0585(15) Uani 1 1 d . . . H17A H -1.0985 -0.7244 -0.1074 0.070 Uiso 1 1 calc R . . H17B H -1.1340 -0.6907 -0.1795 0.070 Uiso 1 1 calc R . . C18 C -0.8915(6) -0.7670(4) -0.1863(3) 0.0550(15) Uani 1 1 d . . . H18A H -0.9441 -0.7729 -0.2279 0.066 Uiso 1 1 calc R . . H18B H -0.9214 -0.8161 -0.1575 0.066 Uiso 1 1 calc R . . C19 C -0.7338(6) -0.7718(3) -0.1981(2) 0.0485(14) Uani 1 1 d . . . H19A H -0.7104 -0.8267 -0.2219 0.058 Uiso 1 1 calc R . . H19B H -0.7029 -0.7211 -0.2250 0.058 Uiso 1 1 calc R . . C20 C -0.5084(6) -0.7884(3) -0.1452(3) 0.0494(14) Uani 1 1 d . . . H20A H -0.4639 -0.7442 -0.1743 0.059 Uiso 1 1 calc R . . H20B H -0.4944 -0.8475 -0.1646 0.059 Uiso 1 1 calc R . . C21 C -0.4384(6) -0.7848(3) -0.0803(3) 0.0520(13) Uani 1 1 d . . . H21A H -0.4887 -0.8247 -0.0497 0.062 Uiso 1 1 calc R . . H21B H -0.3362 -0.8036 -0.0835 0.062 Uiso 1 1 calc R . . H1S H -0.475(5) -0.516(3) -0.119(2) 0.050 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 0.0390(6) 0.0410(6) 0.0378(5) -0.0053(5) 0.0054(5) -0.0037(5) Si1 0.0372(8) 0.0437(8) 0.0423(8) 0.0135(6) 0.0015(6) 0.0012(6) O1 0.051(2) 0.045(2) 0.045(2) 0.0080(16) 0.0084(17) -0.0018(17) C1 0.070(4) 0.066(4) 0.063(4) 0.010(3) -0.016(3) -0.004(3) O2 0.067(2) 0.051(2) 0.063(2) -0.0007(19) 0.000(2) 0.0026(19) C2 0.046(3) 0.044(3) 0.050(3) -0.001(2) 0.001(3) -0.001(3) O3 0.047(2) 0.060(2) 0.057(2) 0.0209(19) 0.0036(18) 0.0050(18) C3 0.069(5) 0.075(4) 0.074(4) -0.007(3) 0.025(4) -0.005(4) O4 0.049(2) 0.046(2) 0.0447(19) 0.0044(15) -0.0087(18) 0.0022(17) C4 0.068(4) 0.050(3) 0.106(5) 0.010(3) -0.012(4) -0.005(3) O5 0.045(2) 0.058(2) 0.047(2) -0.0039(17) 0.0013(18) -0.0094(19) C5 0.060(4) 0.040(3) 0.066(4) 0.003(3) -0.009(3) 0.006(3) O6 0.057(2) 0.046(2) 0.054(2) -0.0040(16) 0.008(2) -0.0061(19) C6 0.143(8) 0.060(4) 0.103(6) -0.015(4) 0.013(6) 0.004(5) O7 0.053(2) 0.050(2) 0.053(2) 0.0063(16) -0.0032(19) 0.0113(18) C7 0.062(4) 0.078(5) 0.124(6) -0.006(4) 0.007(5) 0.016(4) O8 0.040(2) 0.057(2) 0.044(2) -0.0004(17) -0.0024(17) -0.0037(16) C8 0.049(3) 0.050(4) 0.084(4) 0.029(3) -0.004(3) 0.007(3) O9 0.049(2) 0.048(2) 0.045(2) -0.0122(15) 0.0048(18) -0.0019(16) C9 0.061(4) 0.093(5) 0.105(6) 0.024(4) -0.031(4) 0.000(4) C10 0.035(3) 0.075(4) 0.040(3) 0.009(3) -0.005(2) 0.001(3) C11 0.051(3) 0.071(4) 0.037(3) 0.001(3) -0.004(2) -0.013(3) C12 0.062(4) 0.058(4) 0.068(4) -0.015(3) -0.002(3) -0.019(3) C13 0.080(4) 0.048(3) 0.065(4) -0.023(3) -0.001(4) -0.011(3) C14 0.060(4) 0.039(3) 0.077(4) -0.005(3) 0.021(4) 0.008(3) C15 0.058(4) 0.044(3) 0.075(4) 0.014(3) 0.019(3) 0.011(3) C16 0.048(3) 0.080(4) 0.052(3) 0.013(3) 0.002(3) 0.017(3) C17 0.043(3) 0.080(4) 0.052(3) 0.004(3) -0.011(3) -0.005(3) C18 0.055(4) 0.066(4) 0.044(3) -0.006(3) -0.004(3) -0.014(3) C19 0.074(4) 0.042(3) 0.030(3) -0.007(2) 0.008(3) -0.009(3) C20 0.050(3) 0.046(3) 0.053(3) -0.006(2) 0.020(3) 0.012(2) C21 0.050(3) 0.047(3) 0.059(3) 0.003(3) 0.010(3) 0.006(3) _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 O3 2.798(4) . ? K1 O6 2.844(4) . ? K1 O4 2.859(4) . ? K1 O8 2.895(3) . ? K1 O9 2.900(3) . ? K1 O5 2.969(3) . ? K1 O7 3.072(4) . ? Si1 O1 1.697(4) . ? Si1 O3 1.717(4) . ? Si1 O2 1.752(4) . ? O1 C2 1.430(6) . ? C1 C2 1.489(8) . ? O2 C5 1.396(6) . ? C2 C3 1.521(8) . ? O3 C8 1.427(6) . ? O4 C21 1.417(6) . ? O4 C10 1.439(6) . ? C4 C5 1.500(9) . ? O5 C11 1.402(6) . ? O5 C12 1.430(6) . ? C5 C6 1.518(9) . ? O6 C13 1.391(7) . ? O6 C14 1.421(7) . ? O7 C15 1.415(6) . ? O7 C16 1.434(6) . ? C7 C8 1.470(9) . ? O8 C17 1.413(6) . ? O8 C18 1.434(7) . ? C8 C9 1.515(9) . ? O9 C19 1.412(6) . ? O9 C20 1.438(6) . ? C10 C11 1.505(8) . ? C12 C13 1.493(8) . ? C14 C15 1.474(8) . ? C16 C17 1.500(8) . ? C18 C19 1.481(8) . ? C20 C21 1.485(8) . ? 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 O3 K1 O6 94.25(10) . . ? O3 K1 O4 112.91(11) . . ? O6 K1 O4 116.45(11) . . ? O3 K1 O8 102.22(11) . . ? O6 K1 O8 111.80(11) . . ? O4 K1 O8 116.14(10) . . ? O3 K1 O9 119.43(11) . . ? O6 K1 O9 145.75(10) . . ? O4 K1 O9 58.30(10) . . ? O8 K1 O9 58.14(10) . . ? O3 K1 O5 111.11(11) . . ? O6 K1 O5 58.65(11) . . ? O4 K1 O5 58.08(10) . . ? O8 K1 O5 145.61(10) . . ? O9 K1 O5 109.20(10) . . ? O3 K1 O7 101.89(10) . . ? O6 K1 O7 56.04(10) . . ? O4 K1 O7 145.10(10) . . ? O8 K1 O7 55.86(10) . . ? O9 K1 O7 106.89(10) . . ? O5 K1 O7 107.40(10) . . ? O1 Si1 O3 116.0(2) . . ? O1 Si1 O2 123.1(2) . . ? O3 Si1 O2 120.9(2) . . ? C2 O1 Si1 124.9(3) . . ? C5 O2 Si1 122.0(3) . . ? O1 C2 C1 110.4(5) . . ? O1 C2 C3 107.1(4) . . ? C1 C2 C3 113.0(5) . . ? C8 O3 Si1 121.3(3) . . ? C8 O3 K1 133.2(3) . . ? Si1 O3 K1 105.49(16) . . ? C21 O4 C10 111.7(4) . . ? C21 O4 K1 119.4(3) . . ? C10 O4 K1 119.9(3) . . ? C11 O5 C12 111.5(4) . . ? C11 O5 K1 104.3(3) . . ? C12 O5 K1 103.9(3) . . ? O2 C5 C4 111.8(5) . . ? O2 C5 C6 107.9(5) . . ? C4 C5 C6 109.8(6) . . ? C13 O6 C14 113.1(4) . . ? C13 O6 K1 119.6(3) . . ? C14 O6 K1 123.3(3) . . ? C15 O7 C16 111.4(4) . . ? C15 O7 K1 104.8(3) . . ? C16 O7 K1 110.1(3) . . ? C17 O8 C18 111.4(4) . . ? C17 O8 K1 123.9(3) . . ? C18 O8 K1 117.6(3) . . ? O3 C8 C7 112.0(6) . . ? O3 C8 C9 109.4(5) . . ? C7 C8 C9 112.7(6) . . ? C19 O9 C20 112.4(4) . . ? C19 O9 K1 106.5(3) . . ? C20 O9 K1 109.7(3) . . ? O4 C10 C11 107.3(4) . . ? O5 C11 C10 109.8(4) . . ? O5 C12 C13 109.6(4) . . ? O6 C13 C12 110.1(5) . . ? O6 C14 C15 109.9(5) . . ? O7 C15 C14 109.1(4) . . ? O7 C16 C17 109.3(4) . . ? O8 C17 C16 108.9(5) . . ? O8 C18 C19 109.6(4) . . ? O9 C19 C18 109.3(4) . . ? O9 C20 C21 109.2(4) . . ? O4 C21 C20 107.5(4) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.464 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.058 # Attachment '9.CIF' data_PP3011.CIF _database_code_depnum_ccdc_archive 'CCDC 659288' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H39 F2 K O6 Si' _chemical_formula_weight 600.80 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' F F 0.0171 0.0103 '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 P21/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 9.5474(3) _cell_length_b 37.429(3) _cell_length_c 17.6357(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.016(16) _cell_angle_gamma 90.00 _cell_volume 6140.2(6) _cell_formula_units_Z 8 _cell_measurement_temperature 115(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.264 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8793 _exptl_absorpt_correction_T_max 0.9250 _exptl_absorpt_process_details Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 115(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 KappaCCD _diffrn_measurement_method '0.7o phi + omega scans 70s/o' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24097 _diffrn_reflns_av_R_equivalents 0.1088 _diffrn_reflns_av_sigmaI/netI 0.1735 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11948 _reflns_number_gt 7304 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO_SMN _computing_data_reduction DENZO_SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _computing_publication_material ? _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^)+(0.0000P)^2^+1.2997P] 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 SHELXL _refine_ls_extinction_coef 0.0009(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11948 _refine_ls_number_parameters 722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1600 _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 0.56655(7) 0.02436(2) 0.66290(4) 0.0220(2) Uani 1 1 d . . . Si1 Si 0.37684(8) 0.08074(3) 0.81820(5) 0.0176(2) Uani 1 1 d . . . F1 F 0.40938(16) 0.04988(6) 0.74937(9) 0.0247(5) Uani 1 1 d . . . O1 O 0.3137(2) -0.01558(7) 0.60505(12) 0.0273(6) Uani 1 1 d . . . C1 C 0.2525(3) 0.10706(10) 0.73705(16) 0.0162(8) Uani 1 1 d . . . K2 K 0.55583(6) -0.22326(2) 0.82367(4) 0.0200(2) Uani 1 1 d . . . Si2 Si 0.23753(8) -0.17999(3) 0.64523(5) 0.0193(2) Uani 1 1 d . . . F2 F 0.34692(15) 0.11145(5) 0.88520(9) 0.0220(5) Uani 1 1 d . . . O2 O 0.36511(19) 0.04741(7) 0.52859(11) 0.0235(6) Uani 1 1 d . . . C2 C 0.2619(3) 0.10513(10) 0.65883(17) 0.0228(9) Uani 1 1 d . . . H2 H 0.3283 0.0889 0.6448 0.027 Uiso 1 1 calc R . . F3 F 0.32297(15) -0.20251(5) 0.73049(9) 0.0212(5) Uani 1 1 d . . . O3 O 0.6442(2) 0.07060(7) 0.54857(11) 0.0241(6) Uani 1 1 d . . . C3 C 0.1776(3) 0.12610(11) 0.60131(18) 0.0298(10) Uani 1 1 d . . . H3 H 0.1889 0.1245 0.5493 0.036 Uiso 1 1 calc R . . F4 F 0.15540(16) -0.15754(6) 0.56213(9) 0.0281(5) Uani 1 1 d . . . O4 O 0.8464(2) 0.04653(7) 0.67476(12) 0.0275(6) Uani 1 1 d . . . C4 C 0.0772(3) 0.14931(12) 0.6194(2) 0.0362(11) Uani 1 1 d . . . H4 H 0.0184 0.1634 0.5799 0.043 Uiso 1 1 calc R . . O5 O 0.8007(2) -0.01604(7) 0.75540(12) 0.0317(7) Uani 1 1 d . . . C5 C 0.0633(3) 0.15188(11) 0.6955(2) 0.0305(10) Uani 1 1 d . . . H5 H -0.0053 0.1677 0.7086 0.037 Uiso 1 1 calc R . . O6 O 0.5161(2) -0.03783(7) 0.73608(13) 0.0340(7) Uani 1 1 d . . . C6 C 0.1501(3) 0.13116(10) 0.75278(18) 0.0223(9) Uani 1 1 d . . . H6 H 0.1397 0.1334 0.8049 0.027 Uiso 1 1 calc R . . O7 O 0.7154(2) -0.26898(7) 0.75031(11) 0.0254(6) Uani 1 1 d . . . C7 C 0.5772(3) 0.09178(10) 0.84497(17) 0.0170(8) Uani 1 1 d . . . O8 O 0.8198(2) -0.20069(7) 0.79733(12) 0.0252(6) Uani 1 1 d . . . C8 C 0.6593(3) 0.09766(10) 0.78986(17) 0.0230(9) Uani 1 1 d . . . H8 H 0.6146 0.0951 0.7363 0.028 Uiso 1 1 calc R . . O9 O 0.72592(19) -0.16822(7) 0.91580(11) 0.0228(6) Uani 1 1 d . . . C9 C 0.8035(3) 0.10712(10) 0.81010(19) 0.0258(9) Uani 1 1 d . . . H9 H 0.8549 0.1113 0.7707 0.031 Uiso 1 1 calc R . . O10 O 0.45983(19) -0.18917(7) 0.94305(11) 0.0214(6) Uani 1 1 d . . . C10 C 0.8719(3) 0.11044(11) 0.88715(19) 0.0282(10) Uani 1 1 d . . . H10 H 0.9706 0.1168 0.9014 0.034 Uiso 1 1 calc R . . O11 O 0.35378(19) -0.25794(7) 0.89803(11) 0.0225(6) Uani 1 1 d . . . C11 C 0.7952(3) 0.10441(12) 0.94367(19) 0.0335(11) Uani 1 1 d . . . H11 H 0.8415 0.1064 0.9971 0.040 Uiso 1 1 calc R . . O12 O 0.4507(2) -0.29124(7) 0.77936(11) 0.0245(6) Uani 1 1 d . . . C12 C 0.6499(3) 0.09540(11) 0.92222(18) 0.0273(10) Uani 1 1 d . . . H12 H 0.5987 0.0916 0.9619 0.033 Uiso 1 1 calc R . . C13 C 0.3118(3) 0.04352(11) 0.87543(16) 0.0195(8) Uani 1 1 d . . . C14 C 0.3647(3) 0.00889(12) 0.87756(18) 0.0275(9) Uani 1 1 d . . . H14 H 0.4297 0.0031 0.8458 0.033 Uiso 1 1 calc R . . C15 C 0.3266(4) -0.01767(12) 0.92427(19) 0.0365(10) Uani 1 1 d . . . H15 H 0.3679 -0.0408 0.9254 0.044 Uiso 1 1 calc R . . C16 C 0.2283(4) -0.01028(13) 0.96898(19) 0.0364(11) Uani 1 1 d . . . H16 H 0.2014 -0.0283 1.0010 0.044 Uiso 1 1 calc R . . C17 C 0.1702(4) 0.02326(13) 0.96657(18) 0.0326(10) Uani 1 1 d . . . H17 H 0.0999 0.0282 0.9957 0.039 Uiso 1 1 calc R . . C18 C 0.2124(3) 0.05026(11) 0.92208(17) 0.0245(9) Uani 1 1 d . . . H18 H 0.1736 0.0736 0.9232 0.029 Uiso 1 1 calc R . . C19 C 0.2029(3) 0.00768(11) 0.56736(19) 0.0311(10) Uani 1 1 d . . . H19A H 0.1864 0.0264 0.6041 0.037 Uiso 1 1 calc R . . H19B H 0.1125 -0.0059 0.5495 0.037 Uiso 1 1 calc R . . C20 C 0.2462(3) 0.02469(12) 0.49900(19) 0.0351(11) Uani 1 1 d . . . H20A H 0.2734 0.0061 0.4650 0.042 Uiso 1 1 calc R . . H20B H 0.1652 0.0387 0.4681 0.042 Uiso 1 1 calc R . . C21 C 0.4105(3) 0.06685(11) 0.46934(17) 0.0286(10) Uani 1 1 d . . . H21A H 0.3289 0.0806 0.4382 0.034 Uiso 1 1 calc R . . H21B H 0.4457 0.0502 0.4341 0.034 Uiso 1 1 calc R . . C22 C 0.5280(3) 0.09164(11) 0.50668(18) 0.0283(10) Uani 1 1 d . . . H22A H 0.5598 0.1061 0.4665 0.034 Uiso 1 1 calc R . . H22B H 0.4936 0.1081 0.5425 0.034 Uiso 1 1 calc R . . C23 C 0.7698(3) 0.09118(11) 0.57892(18) 0.0307(10) Uani 1 1 d . . . H23A H 0.7516 0.1080 0.6190 0.037 Uiso 1 1 calc R . . H23B H 0.7968 0.1052 0.5368 0.037 Uiso 1 1 calc R . . C24 C 0.8880(3) 0.06608(11) 0.61383(19) 0.0308(10) Uani 1 1 d . . . H24A H 0.9064 0.0494 0.5736 0.037 Uiso 1 1 calc R . . H24B H 0.9774 0.0796 0.6350 0.037 Uiso 1 1 calc R . . C25 C 0.9610(3) 0.02518(12) 0.7184(2) 0.0355(11) Uani 1 1 d . . . H25A H 1.0467 0.0403 0.7377 0.043 Uiso 1 1 calc R . . H25B H 0.9870 0.0063 0.6846 0.043 Uiso 1 1 calc R . . C26 C 0.9140(4) 0.00855(12) 0.7852(2) 0.0391(11) Uani 1 1 d . . . H26A H 0.9957 -0.0041 0.8191 0.047 Uiso 1 1 calc R . . H26B H 0.8798 0.0272 0.8164 0.047 Uiso 1 1 calc R . . C27 C 0.7495(4) -0.03322(13) 0.8161(2) 0.0441(13) Uani 1 1 d . . . H27A H 0.7132 -0.0152 0.8480 0.053 Uiso 1 1 calc R . . H27B H 0.8288 -0.0466 0.8504 0.053 Uiso 1 1 calc R . . C28 C 0.6309(4) -0.05844(12) 0.7801(2) 0.0441(12) Uani 1 1 d . . . H28A H 0.6655 -0.0757 0.7460 0.053 Uiso 1 1 calc R . . H28B H 0.5980 -0.0719 0.8212 0.053 Uiso 1 1 calc R . . C29 C 0.3921(4) -0.05883(12) 0.7045(2) 0.0414(11) Uani 1 1 d . . . H29A H 0.3638 -0.0729 0.7462 0.050 Uiso 1 1 calc R . . H29B H 0.4127 -0.0756 0.6650 0.050 Uiso 1 1 calc R . . C30 C 0.2744(3) -0.03397(12) 0.6684(2) 0.0362(11) Uani 1 1 d . . . H30A H 0.1844 -0.0475 0.6491 0.043 Uiso 1 1 calc R . . H30B H 0.2576 -0.0165 0.7076 0.043 Uiso 1 1 calc R . . C31 C 0.1740(3) -0.14465(10) 0.70880(17) 0.0183(8) Uani 1 1 d . . . C32 C 0.2414(3) -0.14009(11) 0.78741(18) 0.0252(9) Uani 1 1 d . . . H32 H 0.3161 -0.1561 0.8105 0.030 Uiso 1 1 calc R . . C33 C 0.2032(4) -0.11300(12) 0.8330(2) 0.0333(10) Uani 1 1 d . . . H33 H 0.2541 -0.1102 0.8855 0.040 Uiso 1 1 calc R . . C34 C 0.0913(4) -0.09035(12) 0.8018(2) 0.0386(11) Uani 1 1 d . . . H34 H 0.0634 -0.0722 0.8331 0.046 Uiso 1 1 calc R . . C35 C 0.0201(3) -0.09416(12) 0.7254(2) 0.0360(11) Uani 1 1 d . . . H35 H -0.0576 -0.0787 0.7037 0.043 Uiso 1 1 calc R . . C36 C 0.0622(3) -0.12074(11) 0.6795(2) 0.0299(10) Uani 1 1 d . . . H36 H 0.0130 -0.1227 0.6265 0.036 Uiso 1 1 calc R . . C37 C 0.1343(3) -0.22261(11) 0.60850(16) 0.0172(8) Uani 1 1 d . . . C38 C 0.1844(3) -0.25623(11) 0.63552(17) 0.0235(9) Uani 1 1 d . . . H38 H 0.2717 -0.2577 0.6739 0.028 Uiso 1 1 calc R . . C39 C 0.1123(3) -0.28776(12) 0.60886(18) 0.0289(10) Uani 1 1 d . . . H39 H 0.1510 -0.3101 0.6287 0.035 Uiso 1 1 calc R . . C40 C -0.0157(3) -0.28638(12) 0.55343(18) 0.0308(10) Uani 1 1 d . . . H40 H -0.0664 -0.3077 0.5354 0.037 Uiso 1 1 calc R . . C41 C -0.0688(3) -0.25354(13) 0.52477(18) 0.0311(11) Uani 1 1 d . . . H41 H -0.1563 -0.2524 0.4865 0.037 Uiso 1 1 calc R . . C42 C 0.0042(3) -0.22213(11) 0.55114(16) 0.0249(9) Uani 1 1 d . . . H42 H -0.0343 -0.1999 0.5302 0.030 Uiso 1 1 calc R . . C43 C 0.4209(3) -0.17366(10) 0.62188(17) 0.0184(8) Uani 1 1 d . . . C44 C 0.5322(3) -0.15478(10) 0.67052(17) 0.0205(9) Uani 1 1 d . . . H44 H 0.5160 -0.1447 0.7173 0.025 Uiso 1 1 calc R . . C45 C 0.6656(3) -0.15020(11) 0.65285(17) 0.0235(9) Uani 1 1 d . . . H45 H 0.7380 -0.1367 0.6865 0.028 Uiso 1 1 calc R . . C46 C 0.6926(3) -0.16538(11) 0.58621(18) 0.0268(10) Uani 1 1 d . . . H46 H 0.7844 -0.1627 0.5744 0.032 Uiso 1 1 calc R . . C47 C 0.5862(3) -0.18430(11) 0.53711(19) 0.0319(10) Uani 1 1 d . . . H47 H 0.6045 -0.1949 0.4913 0.038 Uiso 1 1 calc R . . C48 C 0.4515(3) -0.18801(11) 0.55425(17) 0.0257(9) Uani 1 1 d . . . H48 H 0.3784 -0.2007 0.5190 0.031 Uiso 1 1 calc R . . C49 C 0.8010(4) -0.24904(11) 0.70880(19) 0.0365(11) Uani 1 1 d . . . H49A H 0.7385 -0.2342 0.6685 0.044 Uiso 1 1 calc R . . H49B H 0.8563 -0.2655 0.6827 0.044 Uiso 1 1 calc R . . C50 C 0.9012(3) -0.22585(12) 0.7646(2) 0.0365(11) Uani 1 1 d . . . H50A H 0.9604 -0.2406 0.8063 0.044 Uiso 1 1 calc R . . H50B H 0.9664 -0.2131 0.7373 0.044 Uiso 1 1 calc R . . C51 C 0.9090(3) -0.17599(11) 0.84663(18) 0.0299(10) Uani 1 1 d . . . H51A H 0.9724 -0.1636 0.8176 0.036 Uiso 1 1 calc R . . H51B H 0.9703 -0.1887 0.8912 0.036 Uiso 1 1 calc R . . C52 C 0.8163(3) -0.14937(11) 0.87527(18) 0.0266(9) Uani 1 1 d . . . H52A H 0.8767 -0.1320 0.9105 0.032 Uiso 1 1 calc R . . H52B H 0.7571 -0.1361 0.8309 0.032 Uiso 1 1 calc R . . C53 C 0.6406(3) -0.14492(11) 0.95047(18) 0.0287(10) Uani 1 1 d . . . H53A H 0.5734 -0.1313 0.9098 0.034 Uiso 1 1 calc R . . H53B H 0.7028 -0.1278 0.9854 0.034 Uiso 1 1 calc R . . C54 C 0.5582(3) -0.16756(11) 0.99597(18) 0.0319(11) Uani 1 1 d . . . H54A H 0.6253 -0.1828 1.0333 0.038 Uiso 1 1 calc R . . H54B H 0.5056 -0.1521 1.0257 0.038 Uiso 1 1 calc R . . C55 C 0.3653(3) -0.20780(11) 0.98141(18) 0.0292(10) Uani 1 1 d . . . H55A H 0.3072 -0.1905 1.0037 0.035 Uiso 1 1 calc R . . H55B H 0.4217 -0.2224 1.0243 0.035 Uiso 1 1 calc R . . C56 C 0.2693(3) -0.23118(11) 0.92394(17) 0.0247(9) Uani 1 1 d . . . H56A H 0.1968 -0.2425 0.9484 0.030 Uiso 1 1 calc R . . H56B H 0.2183 -0.2168 0.8791 0.030 Uiso 1 1 calc R . . C57 C 0.2673(3) -0.28326(11) 0.84804(19) 0.0304(10) Uani 1 1 d . . . H57A H 0.2074 -0.2709 0.8024 0.036 Uiso 1 1 calc R . . H57B H 0.2027 -0.2957 0.8762 0.036 Uiso 1 1 calc R . . C58 C 0.3630(3) -0.30955(11) 0.82195(19) 0.0329(10) Uani 1 1 d . . . H58A H 0.4240 -0.3216 0.8676 0.039 Uiso 1 1 calc R . . H58B H 0.3047 -0.3279 0.7886 0.039 Uiso 1 1 calc R . . C59 C 0.5427(3) -0.31494(11) 0.7492(2) 0.0321(10) Uani 1 1 d . . . H59A H 0.4849 -0.3336 0.7167 0.039 Uiso 1 1 calc R . . H59B H 0.6113 -0.3267 0.7925 0.039 Uiso 1 1 calc R . . C60 C 0.6224(3) -0.29332(11) 0.70137(18) 0.0315(10) Uani 1 1 d . . . H60A H 0.6793 -0.3093 0.6751 0.038 Uiso 1 1 calc R . . H60B H 0.5534 -0.2800 0.6609 0.038 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 K1 0.0211(3) 0.0210(6) 0.0260(4) 0.0013(4) 0.0099(3) 0.0012(4) Si1 0.0194(4) 0.0159(7) 0.0186(5) -0.0016(4) 0.0068(3) -0.0004(4) F1 0.0321(9) 0.0202(15) 0.0246(10) -0.0043(9) 0.0126(8) 0.0018(10) O1 0.0274(12) 0.0234(19) 0.0359(14) -0.0014(12) 0.0173(10) -0.0051(12) C1 0.0157(15) 0.011(2) 0.0230(18) -0.0025(15) 0.0056(12) -0.0080(15) K2 0.0178(3) 0.0205(6) 0.0215(4) -0.0024(3) 0.0043(3) 0.0004(3) Si2 0.0187(4) 0.0209(7) 0.0173(5) 0.0020(4) 0.0018(3) 0.0005(5) F2 0.0216(9) 0.0226(15) 0.0226(10) -0.0063(9) 0.0067(7) 0.0018(9) O2 0.0235(11) 0.0271(19) 0.0206(12) -0.0019(12) 0.0061(9) -0.0071(12) C2 0.0237(16) 0.023(3) 0.0229(19) -0.0034(17) 0.0073(14) -0.0106(17) F3 0.0252(9) 0.0182(14) 0.0186(9) 0.0024(9) 0.0016(7) -0.0001(9) O3 0.0221(11) 0.0215(19) 0.0278(13) 0.0019(11) 0.0038(9) -0.0055(12) C3 0.0316(18) 0.035(3) 0.0222(19) 0.0061(18) 0.0040(15) -0.012(2) F4 0.0294(9) 0.0285(17) 0.0233(10) 0.0077(9) -0.0002(7) 0.0023(10) O4 0.0201(11) 0.029(2) 0.0330(13) 0.0019(13) 0.0048(10) 0.0024(12) C4 0.0260(18) 0.044(3) 0.034(2) 0.020(2) -0.0038(15) -0.007(2) O5 0.0329(13) 0.032(2) 0.0300(14) 0.0045(13) 0.0075(10) 0.0043(13) C5 0.0203(16) 0.025(3) 0.045(2) 0.009(2) 0.0045(15) 0.0018(18) O6 0.0335(13) 0.024(2) 0.0492(15) 0.0117(14) 0.0188(11) 0.0092(14) C6 0.0193(16) 0.023(3) 0.0261(19) 0.0030(17) 0.0070(14) -0.0054(17) O7 0.0308(12) 0.0240(19) 0.0222(12) -0.0001(12) 0.0076(9) 0.0037(12) C7 0.0211(15) 0.006(2) 0.0251(18) -0.0011(15) 0.0084(13) 0.0047(15) O8 0.0231(11) 0.0266(19) 0.0279(13) 0.0029(12) 0.0100(10) 0.0026(12) C8 0.0269(17) 0.020(3) 0.0224(18) -0.0035(17) 0.0072(14) -0.0013(17) O9 0.0215(11) 0.0264(19) 0.0234(12) -0.0014(11) 0.0108(9) -0.0053(11) C9 0.0276(17) 0.019(3) 0.035(2) -0.0015(18) 0.0150(15) -0.0026(18) O10 0.0224(11) 0.0245(19) 0.0184(12) -0.0032(11) 0.0070(9) -0.0069(12) C10 0.0154(15) 0.023(3) 0.045(2) 0.0038(19) 0.0041(15) 0.0014(17) O11 0.0201(11) 0.0214(18) 0.0247(12) -0.0032(11) 0.0027(9) -0.0037(12) C11 0.0236(17) 0.046(4) 0.029(2) 0.007(2) 0.0010(15) 0.0019(19) O12 0.0253(11) 0.0177(18) 0.0302(13) -0.0044(11) 0.0054(10) 0.0030(12) C12 0.0212(16) 0.037(3) 0.0248(19) 0.0060(18) 0.0073(14) 0.0029(18) C13 0.0168(15) 0.021(3) 0.0193(17) -0.0051(16) 0.0009(12) -0.0045(17) C14 0.0356(19) 0.022(3) 0.027(2) -0.0006(18) 0.0129(15) 0.000(2) C15 0.050(2) 0.021(3) 0.038(2) 0.008(2) 0.0098(18) 0.002(2) C16 0.044(2) 0.035(3) 0.031(2) 0.007(2) 0.0112(17) -0.010(2) C17 0.035(2) 0.039(3) 0.027(2) 0.005(2) 0.0127(15) -0.008(2) C18 0.0255(17) 0.023(3) 0.0252(19) -0.0020(18) 0.0073(14) 0.0010(18) C19 0.0201(17) 0.037(3) 0.036(2) 0.000(2) 0.0057(15) -0.0083(19) C20 0.0267(18) 0.048(4) 0.028(2) -0.004(2) 0.0016(15) -0.014(2) C21 0.0285(17) 0.033(3) 0.0221(19) 0.0061(18) 0.0019(14) 0.0007(19) C22 0.0317(18) 0.024(3) 0.028(2) 0.0041(18) 0.0042(15) -0.0041(19) C23 0.0304(19) 0.031(3) 0.032(2) 0.0009(19) 0.0087(15) -0.006(2) C24 0.0243(17) 0.031(3) 0.039(2) -0.003(2) 0.0122(15) -0.0086(19) C25 0.0178(17) 0.032(3) 0.052(2) -0.006(2) -0.0017(16) 0.0025(19) C26 0.039(2) 0.034(3) 0.036(2) -0.005(2) -0.0078(17) 0.006(2) C27 0.047(2) 0.054(4) 0.034(2) 0.018(2) 0.0130(18) 0.024(2) C28 0.046(2) 0.036(4) 0.058(3) 0.024(2) 0.029(2) 0.016(2) C29 0.047(2) 0.023(3) 0.065(3) 0.007(2) 0.036(2) -0.005(2) C30 0.0316(19) 0.030(3) 0.054(2) 0.001(2) 0.0234(17) -0.004(2) C31 0.0165(15) 0.013(2) 0.0273(19) 0.0034(16) 0.0092(13) -0.0040(16) C32 0.0243(17) 0.027(3) 0.028(2) -0.0025(18) 0.0120(14) -0.0054(18) C33 0.040(2) 0.028(3) 0.038(2) -0.009(2) 0.0226(17) -0.015(2) C34 0.039(2) 0.023(3) 0.065(3) -0.016(2) 0.034(2) -0.008(2) C35 0.0239(18) 0.023(3) 0.067(3) 0.002(2) 0.0214(18) 0.0015(19) C36 0.0225(17) 0.028(3) 0.041(2) -0.003(2) 0.0105(15) -0.0093(19) C37 0.0183(15) 0.020(3) 0.0142(16) 0.0011(16) 0.0056(12) -0.0018(17) C38 0.0252(16) 0.024(3) 0.0212(18) -0.0032(17) 0.0058(13) -0.0047(19) C39 0.0329(19) 0.027(3) 0.030(2) -0.0038(19) 0.0137(16) -0.002(2) C40 0.036(2) 0.031(3) 0.029(2) -0.0142(19) 0.0147(16) -0.019(2) C41 0.0222(17) 0.047(4) 0.0234(19) -0.011(2) 0.0030(14) -0.010(2) C42 0.0224(16) 0.034(3) 0.0191(18) -0.0025(18) 0.0060(13) 0.0045(19) C43 0.0228(16) 0.012(2) 0.0188(17) 0.0051(15) 0.0003(13) 0.0019(16) C44 0.0248(16) 0.020(3) 0.0173(17) 0.0032(16) 0.0053(13) 0.0039(17) C45 0.0202(16) 0.024(3) 0.0246(19) 0.0088(17) 0.0013(13) -0.0001(17) C46 0.0236(17) 0.029(3) 0.030(2) 0.0095(19) 0.0111(15) 0.0086(18) C47 0.0348(19) 0.038(3) 0.026(2) -0.0014(19) 0.0145(16) 0.004(2) C48 0.0283(17) 0.027(3) 0.0214(19) -0.0039(17) 0.0051(14) 0.0007(18) C49 0.050(2) 0.033(3) 0.034(2) 0.001(2) 0.0257(18) 0.009(2) C50 0.0323(19) 0.038(3) 0.046(2) 0.000(2) 0.0231(17) 0.004(2) C51 0.0216(17) 0.037(3) 0.033(2) 0.004(2) 0.0091(15) -0.0095(19) C52 0.0245(17) 0.027(3) 0.030(2) 0.0008(18) 0.0082(14) -0.0105(19) C53 0.0346(18) 0.027(3) 0.0275(19) -0.0145(18) 0.0135(15) -0.0153(19) C54 0.0346(19) 0.041(3) 0.0239(19) -0.0155(19) 0.0157(15) -0.017(2) C55 0.0267(17) 0.037(3) 0.028(2) -0.0052(19) 0.0150(15) -0.0058(19) C56 0.0191(15) 0.028(3) 0.0287(19) -0.0004(18) 0.0097(14) -0.0046(18) C57 0.0276(18) 0.030(3) 0.033(2) -0.0053(19) 0.0058(15) -0.011(2) C58 0.039(2) 0.025(3) 0.034(2) -0.0058(19) 0.0048(16) -0.010(2) C59 0.0348(19) 0.021(3) 0.038(2) -0.0136(19) 0.0040(16) 0.003(2) C60 0.0357(19) 0.033(3) 0.023(2) -0.0107(19) -0.0004(15) 0.010(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 F1 2.5537(17) . ? K1 O6 2.756(3) . ? K1 O4 2.760(2) . ? K1 O1 2.827(2) . ? K1 O2 2.829(2) . ? K1 O3 2.878(2) . ? K1 O5 2.882(2) . ? K1 C8 3.526(4) . ? Si1 F2 1.7179(19) . ? Si1 F1 1.7532(19) . ? Si1 C13 1.904(4) . ? Si1 C7 1.909(3) . ? Si1 C1 1.914(3) . ? O1 C19 1.415(4) . ? O1 C30 1.432(4) . ? C1 C6 1.403(4) . ? C1 C2 1.405(4) . ? K2 F3 2.5691(17) . ? K2 O12 2.782(3) . ? K2 O10 2.787(2) . ? K2 O8 2.794(2) . ? K2 O7 2.795(2) . ? K2 O11 2.875(2) . ? K2 O9 2.887(2) . ? Si2 F4 1.7176(19) . ? Si2 F3 1.7564(18) . ? Si2 C43 1.901(3) . ? Si2 C37 1.910(4) . ? Si2 C31 1.918(3) . ? O2 C21 1.419(4) . ? O2 C20 1.421(4) . ? C2 C3 1.387(4) . ? O3 C22 1.424(4) . ? O3 C23 1.424(4) . ? C3 C4 1.383(5) . ? O4 C24 1.428(4) . ? O4 C25 1.432(4) . ? C4 C5 1.381(4) . ? O5 C27 1.427(4) . ? O5 C26 1.427(4) . ? C5 C6 1.390(4) . ? O6 C28 1.420(4) . ? O6 C29 1.426(4) . ? O7 C60 1.421(4) . ? O7 C49 1.425(4) . ? C7 C12 1.389(4) . ? C7 C8 1.397(4) . ? O8 C51 1.415(4) . ? O8 C50 1.424(4) . ? C8 C9 1.388(4) . ? O9 C53 1.422(4) . ? O9 C52 1.425(3) . ? C9 C10 1.374(4) . ? O10 C54 1.419(4) . ? O10 C55 1.426(3) . ? C10 C11 1.382(4) . ? O11 C56 1.424(4) . ? O11 C57 1.424(4) . ? C11 C12 1.395(4) . ? O12 C58 1.421(4) . ? O12 C59 1.432(4) . ? C13 C14 1.388(5) . ? C13 C18 1.412(4) . ? C14 C15 1.391(5) . ? C15 C16 1.382(4) . ? C16 C17 1.369(5) . ? C17 C18 1.394(5) . ? C19 C20 1.501(4) . ? C21 C22 1.490(5) . ? C23 C24 1.491(5) . ? C25 C26 1.488(5) . ? C27 C28 1.501(5) . ? C29 C30 1.487(5) . ? C31 C36 1.400(5) . ? C31 C32 1.401(4) . ? C32 C33 1.393(5) . ? C33 C34 1.378(5) . ? C34 C35 1.374(5) . ? C35 C36 1.397(5) . ? C37 C38 1.391(5) . ? C37 C42 1.415(4) . ? C38 C39 1.393(5) . ? C39 C40 1.384(4) . ? C40 C41 1.381(5) . ? C41 C42 1.392(5) . ? C43 C44 1.398(4) . ? C43 C48 1.398(4) . ? C44 C45 1.388(4) . ? C45 C46 1.381(4) . ? C46 C47 1.374(5) . ? C47 C48 1.392(4) . ? C49 C50 1.487(5) . ? C51 C52 1.495(5) . ? C53 C54 1.505(4) . ? C55 C56 1.488(4) . ? C57 C58 1.485(5) . ? C59 C60 1.495(5) . ? 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 F1 K1 O6 81.27(7) . . ? F1 K1 O4 122.09(7) . . ? O6 K1 O4 119.12(7) . . ? F1 K1 O1 81.05(6) . . ? O6 K1 O1 59.83(7) . . ? O4 K1 O1 156.86(7) . . ? F1 K1 O2 90.33(6) . . ? O6 K1 O2 119.49(7) . . ? O4 K1 O2 115.83(7) . . ? O1 K1 O2 59.66(7) . . ? F1 K1 O3 118.17(7) . . ? O6 K1 O3 159.34(7) . . ? O4 K1 O3 58.30(6) . . ? O1 K1 O3 113.51(6) . . ? O2 K1 O3 57.58(6) . . ? F1 K1 O5 110.10(6) . . ? O6 K1 O5 59.12(7) . . ? O4 K1 O5 60.04(7) . . ? O1 K1 O5 114.67(8) . . ? O2 K1 O5 158.22(7) . . ? O3 K1 O5 115.00(6) . . ? F1 K1 C8 55.04(6) . . ? O6 K1 C8 113.91(8) . . ? O4 K1 C8 67.51(7) . . ? O1 K1 C8 135.43(7) . . ? O2 K1 C8 108.69(8) . . ? O3 K1 C8 84.80(7) . . ? O5 K1 C8 89.83(8) . . ? F2 Si1 F1 179.05(10) . . ? F2 Si1 C13 90.03(12) . . ? F1 Si1 C13 90.85(13) . . ? F2 Si1 C7 89.86(12) . . ? F1 Si1 C7 89.42(11) . . ? C13 Si1 C7 117.08(14) . . ? F2 Si1 C1 89.92(12) . . ? F1 Si1 C1 89.89(12) . . ? C13 Si1 C1 123.46(13) . . ? C7 Si1 C1 119.45(14) . . ? Si1 F1 K1 151.59(10) . . ? C19 O1 C30 111.3(2) . . ? C19 O1 K1 109.3(2) . . ? C30 O1 K1 108.98(18) . . ? C6 C1 C2 115.4(3) . . ? C6 C1 Si1 121.7(2) . . ? C2 C1 Si1 122.8(2) . . ? F3 K2 O12 83.76(6) . . ? F3 K2 O10 87.73(6) . . ? O12 K2 O10 118.15(7) . . ? F3 K2 O8 119.03(6) . . ? O12 K2 O8 120.77(7) . . ? O10 K2 O8 116.71(7) . . ? F3 K2 O7 111.86(6) . . ? O12 K2 O7 60.63(7) . . ? O10 K2 O7 159.42(6) . . ? O8 K2 O7 60.14(7) . . ? F3 K2 O11 81.68(6) . . ? O12 K2 O11 58.57(6) . . ? O10 K2 O11 59.58(7) . . ? O8 K2 O11 159.27(6) . . ? O7 K2 O11 115.23(8) . . ? F3 K2 O9 116.13(7) . . ? O12 K2 O9 158.82(7) . . ? O10 K2 O9 59.15(6) . . ? O8 K2 O9 57.57(6) . . ? O7 K2 O9 113.66(6) . . ? O11 K2 O9 114.57(6) . . ? F4 Si2 F3 179.32(11) . . ? F4 Si2 C43 91.15(11) . . ? F3 Si2 C43 88.42(11) . . ? F4 Si2 C37 91.01(12) . . ? F3 Si2 C37 89.66(12) . . ? C43 Si2 C37 117.42(15) . . ? F4 Si2 C31 91.02(12) . . ? F3 Si2 C31 88.72(12) . . ? C43 Si2 C31 117.93(15) . . ? C37 Si2 C31 124.55(13) . . ? C21 O2 C20 112.8(2) . . ? C21 O2 K1 120.67(16) . . ? C20 O2 K1 117.5(2) . . ? C3 C2 C1 122.3(3) . . ? Si2 F3 K2 149.41(9) . . ? C22 O3 C23 112.8(3) . . ? C22 O3 K1 113.74(16) . . ? C23 O3 K1 112.95(17) . . ? C4 C3 C2 120.3(3) . . ? C24 O4 C25 112.4(2) . . ? C24 O4 K1 121.71(16) . . ? C25 O4 K1 118.9(2) . . ? C5 C4 C3 119.4(3) . . ? C27 O5 C26 112.0(3) . . ? C27 O5 K1 107.96(18) . . ? C26 O5 K1 107.3(2) . . ? C4 C5 C6 119.7(3) . . ? C28 O6 C29 112.6(3) . . ? C28 O6 K1 121.4(2) . . ? C29 O6 K1 120.0(2) . . ? C5 C6 C1 122.9(3) . . ? C60 O7 C49 112.1(2) . . ? C60 O7 K2 110.05(17) . . ? C49 O7 K2 110.7(2) . . ? C12 C7 C8 115.6(3) . . ? C12 C7 Si1 121.0(2) . . ? C8 C7 Si1 123.4(2) . . ? C51 O8 C50 111.9(2) . . ? C51 O8 K2 122.43(17) . . ? C50 O8 K2 117.6(2) . . ? C9 C8 C7 122.7(3) . . ? C9 C8 K1 117.0(2) . . ? C7 C8 K1 102.7(2) . . ? C53 O9 C52 112.5(3) . . ? C53 O9 K2 112.07(16) . . ? C52 O9 K2 113.48(17) . . ? C10 C9 C8 120.0(3) . . ? C54 O10 C55 111.3(2) . . ? C54 O10 K2 118.44(16) . . ? C55 O10 K2 119.0(2) . . ? C9 C10 C11 119.2(3) . . ? C56 O11 C57 112.1(2) . . ? C56 O11 K2 108.37(19) . . ? C57 O11 K2 111.90(17) . . ? C10 C11 C12 120.0(3) . . ? C58 O12 C59 112.4(3) . . ? C58 O12 K2 120.72(19) . . ? C59 O12 K2 117.27(19) . . ? C7 C12 C11 122.4(3) . . ? C14 C13 C18 116.1(3) . . ? C14 C13 Si1 122.5(2) . . ? C18 C13 Si1 121.3(3) . . ? C13 C14 C15 122.7(3) . . ? C16 C15 C14 119.8(4) . . ? C17 C16 C15 119.2(4) . . ? C16 C17 C18 121.1(3) . . ? C17 C18 C13 121.1(4) . . ? O1 C19 C20 109.1(3) . . ? O2 C20 C19 107.5(2) . . ? O2 C21 C22 108.6(2) . . ? O3 C22 C21 107.8(3) . . ? O3 C23 C24 108.0(3) . . ? O4 C24 C23 108.7(2) . . ? O4 C25 C26 109.2(3) . . ? O5 C26 C25 108.5(3) . . ? O5 C27 C28 108.6(3) . . ? O6 C28 C27 107.8(3) . . ? O6 C29 C30 107.7(3) . . ? O1 C30 C29 109.2(3) . . ? C36 C31 C32 115.4(3) . . ? C36 C31 Si2 122.7(2) . . ? C32 C31 Si2 121.8(3) . . ? C33 C32 C31 122.5(3) . . ? C34 C33 C32 119.9(3) . . ? C35 C34 C33 119.7(4) . . ? C34 C35 C36 119.9(4) . . ? C35 C36 C31 122.5(3) . . ? C38 C37 C42 115.8(3) . . ? C38 C37 Si2 121.9(2) . . ? C42 C37 Si2 122.3(3) . . ? C37 C38 C39 123.0(3) . . ? C40 C39 C38 119.8(4) . . ? C41 C40 C39 119.0(4) . . ? C40 C41 C42 121.0(3) . . ? C41 C42 C37 121.4(4) . . ? C44 C43 C48 116.2(3) . . ? C44 C43 Si2 122.7(2) . . ? C48 C43 Si2 121.1(2) . . ? C45 C44 C43 122.3(3) . . ? C46 C45 C44 119.8(3) . . ? C47 C46 C45 119.6(3) . . ? C46 C47 C48 120.2(3) . . ? C47 C48 C43 121.9(3) . . ? O7 C49 C50 108.9(3) . . ? O8 C50 C49 109.0(3) . . ? O8 C51 C52 108.8(2) . . ? O9 C52 C51 108.1(3) . . ? O9 C53 C54 107.6(3) . . ? O10 C54 C53 108.6(2) . . ? O10 C55 C56 108.8(2) . . ? O11 C56 C55 109.0(2) . . ? O11 C57 C58 108.8(3) . . ? O12 C58 C57 108.8(3) . . ? O12 C59 C60 107.9(3) . . ? O7 C60 C59 109.4(3) . . ? 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 F2 Si1 F1 K1 23(7) . . . . ? C13 Si1 F1 K1 -134.8(2) . . . . ? C7 Si1 F1 K1 -17.7(2) . . . . ? C1 Si1 F1 K1 101.7(2) . . . . ? O6 K1 F1 Si1 127.9(2) . . . . ? O4 K1 F1 Si1 8.9(2) . . . . ? O1 K1 F1 Si1 -171.5(2) . . . . ? O2 K1 F1 Si1 -112.3(2) . . . . ? O3 K1 F1 Si1 -59.6(2) . . . . ? O5 K1 F1 Si1 75.4(2) . . . . ? C8 K1 F1 Si1 0.45(19) . . . . ? F1 K1 O1 C19 66.23(18) . . . . ? O6 K1 O1 C19 151.29(19) . . . . ? O4 K1 O1 C19 -114.6(2) . . . . ? O2 K1 O1 C19 -29.45(17) . . . . ? O3 K1 O1 C19 -50.69(19) . . . . ? O5 K1 O1 C19 174.31(17) . . . . ? C8 K1 O1 C19 56.8(2) . . . . ? F1 K1 O1 C30 -55.6(2) . . . . ? O6 K1 O1 C30 29.5(2) . . . . ? O4 K1 O1 C30 123.6(2) . . . . ? O2 K1 O1 C30 -151.3(2) . . . . ? O3 K1 O1 C30 -172.5(2) . . . . ? O5 K1 O1 C30 52.5(2) . . . . ? C8 K1 O1 C30 -65.0(2) . . . . ? F2 Si1 C1 C6 -20.5(3) . . . . ? F1 Si1 C1 C6 160.4(3) . . . . ? C13 Si1 C1 C6 69.5(3) . . . . ? C7 Si1 C1 C6 -110.3(3) . . . . ? F2 Si1 C1 C2 156.0(3) . . . . ? F1 Si1 C1 C2 -23.0(3) . . . . ? C13 Si1 C1 C2 -114.0(3) . . . . ? C7 Si1 C1 C2 66.3(3) . . . . ? F1 K1 O2 C21 130.9(2) . . . . ? O6 K1 O2 C21 -148.9(2) . . . . ? O4 K1 O2 C21 4.5(3) . . . . ? O1 K1 O2 C21 -149.7(3) . . . . ? O3 K1 O2 C21 7.2(2) . . . . ? O5 K1 O2 C21 -69.0(3) . . . . ? C8 K1 O2 C21 78.0(2) . . . . ? F1 K1 O2 C20 -84.3(2) . . . . ? O6 K1 O2 C20 -4.2(2) . . . . ? O4 K1 O2 C20 149.3(2) . . . . ? O1 K1 O2 C20 -4.9(2) . . . . ? O3 K1 O2 C20 151.9(2) . . . . ? O5 K1 O2 C20 75.8(3) . . . . ? C8 K1 O2 C20 -137.2(2) . . . . ? C6 C1 C2 C3 1.1(5) . . . . ? Si1 C1 C2 C3 -175.7(3) . . . . ? F4 Si2 F3 K2 -45(11) . . . . ? C43 Si2 F3 K2 5.4(2) . . . . ? C37 Si2 F3 K2 122.8(2) . . . . ? C31 Si2 F3 K2 -112.6(2) . . . . ? O12 K2 F3 Si2 -116.2(2) . . . . ? O10 K2 F3 Si2 125.1(2) . . . . ? O8 K2 F3 Si2 5.6(2) . . . . ? O7 K2 F3 Si2 -61.4(2) . . . . ? O11 K2 F3 Si2 -175.3(2) . . . . ? O9 K2 F3 Si2 71.4(2) . . . . ? F1 K1 O3 C22 -43.9(2) . . . . ? O6 K1 O3 C22 114.8(3) . . . . ? O4 K1 O3 C22 -156.1(2) . . . . ? O1 K1 O3 C22 48.4(2) . . . . ? O2 K1 O3 C22 26.64(19) . . . . ? O5 K1 O3 C22 -176.8(2) . . . . ? C8 K1 O3 C22 -89.4(2) . . . . ? F1 K1 O3 C23 86.3(2) . . . . ? O6 K1 O3 C23 -115.0(3) . . . . ? O4 K1 O3 C23 -25.9(2) . . . . ? O1 K1 O3 C23 178.6(2) . . . . ? O2 K1 O3 C23 156.9(2) . . . . ? O5 K1 O3 C23 -46.6(2) . . . . ? C8 K1 O3 C23 40.8(2) . . . . ? C1 C2 C3 C4 -1.7(5) . . . . ? F1 K1 O4 C24 -112.8(2) . . . . ? O6 K1 O4 C24 149.0(2) . . . . ? O1 K1 O4 C24 68.2(3) . . . . ? O2 K1 O4 C24 -4.6(3) . . . . ? O3 K1 O4 C24 -7.2(2) . . . . ? O5 K1 O4 C24 151.1(3) . . . . ? C8 K1 O4 C24 -105.3(3) . . . . ? F1 K1 O4 C25 98.7(2) . . . . ? O6 K1 O4 C25 0.4(2) . . . . ? O1 K1 O4 C25 -80.4(3) . . . . ? O2 K1 O4 C25 -153.2(2) . . . . ? O3 K1 O4 C25 -155.8(2) . . . . ? O5 K1 O4 C25 2.6(2) . . . . ? C8 K1 O4 C25 106.2(2) . . . . ? C2 C3 C4 C5 1.1(5) . . . . ? F1 K1 O5 C27 34.9(3) . . . . ? O6 K1 O5 C27 -31.0(2) . . . . ? O4 K1 O5 C27 151.2(3) . . . . ? O1 K1 O5 C27 -54.2(2) . . . . ? O2 K1 O5 C27 -123.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.847 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.847 _refine_diff_density_max 0.542 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.140 # Attachment 'SiOSi-18c6.CIF' data_ppph3kh _database_code_depnum_ccdc_archive 'CCDC 662558' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H54 O7 Si2' _chemical_formula_weight 799.09 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6423(11) _cell_length_b 9.7626(12) _cell_length_c 12.278(2) _cell_angle_alpha 79.564(8) _cell_angle_beta 72.247(7) _cell_angle_gamma 86.267(10) _cell_volume 1082.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cuboid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 426 _exptl_absorpt_coefficient_mu 0.132 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9489 _exptl_absorpt_correction_T_max 0.9489 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 KappaCCD _diffrn_measurement_method '1o phi + omega scans 30s/o' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7371 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0955 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4925 _reflns_number_gt 3507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _computing_publication_material ? _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^)+(0.0000P)^2^+0.4068P] 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 4925 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Si1 Si 0.33106(6) 0.49829(5) 0.00288(5) 0.02316(15) Uani 1 1 d . . . O1 O 0.76518(15) 0.76468(14) -0.43664(13) 0.0327(4) Uani 1 1 d . . . C1 C 0.8733(2) 0.8388(2) -0.4141(2) 0.0346(5) Uani 1 1 d . . . H1A H 0.939(2) 0.891(2) -0.491(2) 0.033(6) Uiso 1 1 d . . . H1B H 0.935(2) 0.765(2) -0.380(2) 0.041(6) Uiso 1 1 d . . . O2 O 0.52466(16) 0.83186(14) -0.61235(13) 0.0358(4) Uani 1 1 d . . . C2 C 0.6940(2) 0.8444(2) -0.5141(2) 0.0315(5) Uani 1 1 d . . . H2A H 0.770(2) 0.895(2) -0.589(2) 0.036(6) Uiso 1 1 d . . . H2B H 0.632(2) 0.918(2) -0.4803(19) 0.031(6) Uiso 1 1 d . . . O3 O 0.25116(15) 0.94428(14) -0.61836(12) 0.0328(4) Uani 1 1 d . . . C3 C 0.6054(2) 0.7460(2) -0.5460(2) 0.0330(5) Uani 1 1 d . . . H3A H 0.668(2) 0.677(2) -0.5906(19) 0.031(6) Uiso 1 1 d . . . H3B H 0.535(2) 0.692(2) -0.475(2) 0.034(6) Uiso 1 1 d . . . C4 C 0.4237(3) 0.7588(2) -0.6428(2) 0.0336(5) Uani 1 1 d . . . H4A H 0.360(2) 0.703(2) -0.572(2) 0.035(6) Uiso 1 1 d . . . H4B H 0.477(3) 0.694(3) -0.700(2) 0.052(7) Uiso 1 1 d . . . C5 C 0.3382(3) 0.8646(2) -0.7013(2) 0.0332(5) Uani 1 1 d . . . H5A H 0.407(2) 0.925(2) -0.768(2) 0.036(6) Uiso 1 1 d . . . H5B H 0.279(2) 0.818(2) -0.7378(19) 0.031(6) Uiso 1 1 d . . . C6 C 0.1874(3) 1.0636(2) -0.6716(2) 0.0368(5) Uani 1 1 d . . . H6A H 0.105(2) 1.032(2) -0.6971(19) 0.035(6) Uiso 1 1 d . . . H6B H 0.262(2) 1.112(2) -0.7384(18) 0.021(5) Uiso 1 1 d . . . O1S O 0.5000 0.5000 0.0000 0.0292(5) Uani 1 2 d S . . C1S C 0.2140(2) 0.56590(19) 0.13385(18) 0.0249(4) Uani 1 1 d . . . C2S C 0.2284(2) 0.5105(2) 0.24404(18) 0.0284(5) Uani 1 1 d . . . H2S H 0.302(2) 0.440(2) 0.2518(18) 0.027(5) Uiso 1 1 d . . . C3S C 0.1343(2) 0.5512(2) 0.3435(2) 0.0336(5) Uani 1 1 d . . . H3S H 0.149(3) 0.510(3) 0.414(2) 0.047(7) Uiso 1 1 d . . . C4S C 0.0242(2) 0.6474(2) 0.3358(2) 0.0348(5) Uani 1 1 d . . . H4S H -0.042(3) 0.674(3) 0.403(2) 0.047(7) Uiso 1 1 d . . . C5S C 0.0078(2) 0.7040(2) 0.2282(2) 0.0326(5) Uani 1 1 d . . . H5S H -0.066(2) 0.773(2) 0.218(2) 0.038(6) Uiso 1 1 d . . . C6S C 0.1016(2) 0.6630(2) 0.12908(19) 0.0276(4) Uani 1 1 d . . . H6S H 0.091(2) 0.703(2) 0.0540(19) 0.025(5) Uiso 1 1 d . . . C7S C 0.3082(2) 0.6080(2) -0.13195(17) 0.0250(4) Uani 1 1 d . . . C8S C 0.3617(2) 0.7442(2) -0.16781(19) 0.0322(5) Uani 1 1 d . . . H8S H 0.417(2) 0.783(2) -0.123(2) 0.035(6) Uiso 1 1 d . . . C9S C 0.3401(2) 0.8291(2) -0.2654(2) 0.0354(5) Uani 1 1 d . . . H9S H 0.379(3) 0.922(3) -0.285(2) 0.045(7) Uiso 1 1 d . . . C10S C 0.2649(2) 0.7794(2) -0.3289(2) 0.0343(5) Uani 1 1 d . . . H10S H 0.252(2) 0.836(2) -0.396(2) 0.029(5) Uiso 1 1 d . . . C11S C 0.2125(2) 0.6446(2) -0.2965(2) 0.0341(5) Uani 1 1 d . . . H11S H 0.164(3) 0.606(2) -0.340(2) 0.044(7) Uiso 1 1 d . . . C12S C 0.2341(2) 0.5604(2) -0.19882(18) 0.0284(5) Uani 1 1 d . . . H12S H 0.197(2) 0.467(2) -0.1778(19) 0.031(6) Uiso 1 1 d . . . C13S C 0.2767(2) 0.31548(19) 0.01363(17) 0.0247(4) Uani 1 1 d . . . C14S C 0.3757(2) 0.2149(2) -0.0339(2) 0.0337(5) Uani 1 1 d . . . H14S H 0.473(3) 0.237(2) -0.070(2) 0.041(6) Uiso 1 1 d . . . C15S C 0.3315(3) 0.0809(2) -0.0285(2) 0.0421(6) Uani 1 1 d . . . H15S H 0.405(3) 0.010(3) -0.061(2) 0.057(8) Uiso 1 1 d . . . C16S C 0.1868(3) 0.0448(2) 0.0239(2) 0.0392(5) Uani 1 1 d . . . H16S H 0.162(3) -0.049(3) 0.027(2) 0.049(7) Uiso 1 1 d . . . C17S C 0.0878(2) 0.1411(2) 0.0719(2) 0.0333(5) Uani 1 1 d . . . H17S H -0.010(2) 0.117(2) 0.1101(19) 0.031(6) Uiso 1 1 d . . . C18S C 0.1327(2) 0.2750(2) 0.06688(19) 0.0290(5) Uani 1 1 d . . . H18S H 0.061(2) 0.340(2) 0.1042(19) 0.034(6) 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 Si1 0.0229(3) 0.0204(3) 0.0255(3) -0.0017(2) -0.0074(2) -0.0010(2) O1 0.0323(8) 0.0293(7) 0.0365(9) 0.0007(7) -0.0142(7) 0.0016(6) C1 0.0288(11) 0.0356(12) 0.0401(14) -0.0037(11) -0.0131(10) 0.0017(10) O2 0.0397(8) 0.0290(8) 0.0439(10) -0.0009(7) -0.0224(7) -0.0027(6) C2 0.0331(11) 0.0272(11) 0.0347(13) -0.0015(10) -0.0142(10) 0.0043(9) O3 0.0373(8) 0.0310(8) 0.0302(8) -0.0019(6) -0.0129(7) 0.0030(6) C3 0.0326(11) 0.0272(11) 0.0392(14) -0.0041(10) -0.0126(10) 0.0049(9) C4 0.0383(12) 0.0312(11) 0.0345(13) -0.0073(10) -0.0141(10) -0.0024(10) C5 0.0384(12) 0.0344(12) 0.0291(12) -0.0073(10) -0.0119(10) -0.0034(10) C6 0.0391(12) 0.0379(12) 0.0339(13) 0.0001(10) -0.0154(11) 0.0005(10) O1S 0.0221(9) 0.0272(10) 0.0374(12) -0.0024(9) -0.0090(9) -0.0025(8) C1S 0.0256(10) 0.0190(9) 0.0302(11) -0.0030(8) -0.0084(8) -0.0040(8) C2S 0.0308(10) 0.0215(10) 0.0316(12) -0.0013(9) -0.0096(9) 0.0011(8) C3S 0.0421(12) 0.0295(11) 0.0263(12) -0.0016(9) -0.0073(10) -0.0038(10) C4S 0.0347(12) 0.0306(11) 0.0346(13) -0.0093(10) -0.0011(10) -0.0039(9) C5S 0.0286(11) 0.0264(11) 0.0405(13) -0.0062(10) -0.0070(10) 0.0010(9) C6S 0.0276(10) 0.0234(10) 0.0328(12) -0.0020(9) -0.0115(9) -0.0021(8) C7S 0.0212(9) 0.0247(9) 0.0267(11) -0.0038(8) -0.0044(8) 0.0016(8) C8S 0.0380(12) 0.0278(11) 0.0317(12) -0.0022(9) -0.0126(10) -0.0034(9) C9S 0.0438(13) 0.0253(11) 0.0339(13) 0.0007(10) -0.0098(10) -0.0036(10) C10S 0.0396(12) 0.0330(12) 0.0269(12) 0.0024(10) -0.0100(10) 0.0032(10) C11S 0.0346(11) 0.0400(12) 0.0297(12) -0.0043(10) -0.0134(10) -0.0016(10) C12S 0.0291(10) 0.0263(11) 0.0281(12) -0.0004(9) -0.0078(9) -0.0032(9) C13S 0.0288(10) 0.0220(9) 0.0238(11) -0.0005(8) -0.0103(8) -0.0008(8) C14S 0.0313(11) 0.0297(11) 0.0350(13) -0.0068(10) -0.0009(10) -0.0038(9) C15S 0.0475(14) 0.0274(11) 0.0476(15) -0.0117(11) -0.0056(11) -0.0011(10) C16S 0.0533(14) 0.0256(11) 0.0418(14) -0.0033(10) -0.0182(11) -0.0104(10) C17S 0.0322(11) 0.0347(12) 0.0344(12) 0.0046(10) -0.0157(10) -0.0114(10) C18S 0.0270(10) 0.0287(10) 0.0316(12) -0.0021(9) -0.0109(9) -0.0002(9) _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 O1S 1.6196(5) . ? Si1 C13S 1.863(2) . ? Si1 C1S 1.864(2) . ? Si1 C7S 1.867(2) . ? O1 C1 1.426(3) . ? O1 C2 1.429(2) . ? C1 C6 1.507(3) 2_674 ? O2 C4 1.416(3) . ? O2 C3 1.423(2) . ? C2 C3 1.501(3) . ? O3 C5 1.424(3) . ? O3 C6 1.428(2) . ? C4 C5 1.499(3) . ? C6 C1 1.507(3) 2_674 ? O1S Si1 1.6196(5) 2_665 ? C1S C6S 1.401(3) . ? C1S C2S 1.408(3) . ? C2S C3S 1.388(3) . ? C3S C4S 1.385(3) . ? C4S C5S 1.388(3) . ? C5S C6S 1.385(3) . ? C7S C12S 1.392(3) . ? C7S C8S 1.403(3) . ? C8S C9S 1.391(3) . ? C9S C10S 1.378(3) . ? C10S C11S 1.386(3) . ? C11S C12S 1.389(3) . ? C13S C18S 1.391(3) . ? C13S C14S 1.401(3) . ? C14S C15S 1.386(3) . ? C15S C16S 1.385(3) . ? C16S C17S 1.373(3) . ? C17S C18S 1.388(3) . ? 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 O1S Si1 C13S 109.25(6) . . ? O1S Si1 C1S 109.42(7) . . ? C13S Si1 C1S 107.98(9) . . ? O1S Si1 C7S 109.34(6) . . ? C13S Si1 C7S 110.33(9) . . ? C1S Si1 C7S 110.49(9) . . ? C1 O1 C2 114.38(16) . . ? O1 C1 C6 114.13(18) . 2_674 ? C4 O2 C3 114.21(16) . . ? O1 C2 C3 107.70(17) . . ? C5 O3 C6 111.96(16) . . ? O2 C3 C2 105.46(16) . . ? O2 C4 C5 107.48(18) . . ? O3 C5 C4 108.65(18) . . ? O3 C6 C1 109.76(19) . 2_674 ? Si1 O1S Si1 180.00(4) 2_665 . ? C6S C1S C2S 117.39(19) . . ? C6S C1S Si1 122.33(16) . . ? C2S C1S Si1 120.06(14) . . ? C3S C2S C1S 120.83(19) . . ? C4S C3S C2S 120.4(2) . . ? C3S C4S C5S 120.0(2) . . ? C6S C5S C4S 119.59(19) . . ? C5S C6S C1S 121.8(2) . . ? C12S C7S C8S 117.33(19) . . ? C12S C7S Si1 121.86(15) . . ? C8S C7S Si1 120.79(16) . . ? C9S C8S C7S 121.4(2) . . ? C10S C9S C8S 119.9(2) . . ? C9S C10S C11S 120.0(2) . . ? C10S C11S C12S 119.8(2) . . ? C11S C12S C7S 121.56(19) . . ? C18S C13S C14S 117.23(19) . . ? C18S C13S Si1 120.44(15) . . ? C14S C13S Si1 122.30(15) . . ? C15S C14S C13S 121.2(2) . . ? C16S C15S C14S 119.9(2) . . ? C17S C16S C15S 120.0(2) . . ? C16S C17S C18S 119.9(2) . . ? C17S C18S C13S 121.7(2) . . ? 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 C2 O1 C1 C6 78.2(2) . . . 2_674 ? C1 O1 C2 C3 169.67(18) . . . . ? C4 O2 C3 C2 -174.89(19) . . . . ? O1 C2 C3 O2 173.75(17) . . . . ? C3 O2 C4 C5 174.44(19) . . . . ? C6 O3 C5 C4 169.05(18) . . . . ? O2 C4 C5 O3 -66.9(2) . . . . ? C5 O3 C6 C1 -166.78(18) . . . 2_674 ? C13S Si1 O1S Si1 55(100) . . . 2_665 ? C1S Si1 O1S Si1 173(100) . . . 2_665 ? C7S Si1 O1S Si1 -66(100) . . . 2_665 ? O1S Si1 C1S C6S 134.56(15) . . . . ? C13S Si1 C1S C6S -106.62(17) . . . . ? C7S Si1 C1S C6S 14.12(19) . . . . ? O1S Si1 C1S C2S -51.06(17) . . . . ? C13S Si1 C1S C2S 67.75(17) . . . . ? C7S Si1 C1S C2S -171.50(15) . . . . ? C6S C1S C2S C3S 0.0(3) . . . . ? Si1 C1S C2S C3S -174.62(17) . . . . ? C1S C2S C3S C4S 0.0(3) . . . . ? C2S C3S C4S C5S -0.2(3) . . . . ? C3S C4S C5S C6S 0.4(3) . . . . ? C4S C5S C6S C1S -0.3(3) . . . . ? C2S C1S C6S C5S 0.1(3) . . . . ? Si1 C1S C6S C5S 174.64(16) . . . . ? O1S Si1 C7S C12S 131.50(15) . . . . ? C13S Si1 C7S C12S 11.32(19) . . . . ? C1S Si1 C7S C12S -108.01(17) . . . . ? O1S Si1 C7S C8S -50.47(17) . . . . ? C13S Si1 C7S C8S -170.65(16) . . . . ? C1S Si1 C7S C8S 70.02(18) . . . . ? C12S C7S C8S C9S 0.8(3) . . . . ? Si1 C7S C8S C9S -177.29(16) . . . . ? C7S C8S C9S C10S -0.1(3) . . . . ? C8S C9S C10S C11S -0.7(3) . . . . ? C9S C10S C11S C12S 0.9(3) . . . . ? C10S C11S C12S C7S -0.2(3) . . . . ? C8S C7S C12S C11S -0.7(3) . . . . ? Si1 C7S C12S C11S 177.42(16) . . . . ? O1S Si1 C13S C18S 151.65(15) . . . . ? C1S Si1 C13S C18S 32.73(19) . . . . ? C7S Si1 C13S C18S -88.11(18) . . . . ? O1S Si1 C13S C14S -30.47(19) . . . . ? C1S Si1 C13S C14S -149.39(17) . . . . ? C7S Si1 C13S C14S 89.77(18) . . . . ? C18S C13S C14S C15S 0.4(3) . . . . ? Si1 C13S C14S C15S -177.58(18) . . . . ? C13S C14S C15S C16S 0.4(4) . . . . ? C14S C15S C16S C17S -0.9(4) . . . . ? C15S C16S C17S C18S 0.5(3) . . . . ? C16S C17S C18S C13S 0.3(3) . . . . ? C14S C13S C18S C17S -0.7(3) . . . . ? Si1 C13S C18S C17S 177.27(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C9S H9S O2 0.97(3) 2.59(3) 3.533(3) 166(2) 2_674 C4S H4S O1 0.95(3) 2.51(3) 3.448(3) 172(2) 1_456 C2S H2S O1 0.97(2) 2.68(2) 3.253(2) 117.9(15) 2_665 C3S H3S O1 0.93(3) 2.74(2) 3.282(3) 117.5(19) 2_665 C10S H10S O3 0.95(2) 2.74(2) 3.664(3) 165.3(17) . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.302 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.056