# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Richard Layfield' _publ_contact_author_email RICHARD.LAYFIELD@MANCHESTER.AC.UK _publ_section_title ; s-Block metal complexes of a bulky, donor-functionalized allyl ligand ; loop_ _publ_author_name 'Richard Layfield' 'Christopher A Muryn' 'Sophia A Solomon' # Attachment '1.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 678934' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H58 Li2 O2 Si4' _chemical_formula_weight 552.98 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' Li Li -0.0003 0.0001 '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 10.1331(8) _cell_length_b 10.8060(9) _cell_length_c 18.5116(14) _cell_angle_alpha 77.614(7) _cell_angle_beta 89.490(6) _cell_angle_gamma 65.099(8) _cell_volume 1788.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6589 _cell_measurement_theta_min 2.7113 _cell_measurement_theta_max 28.2264 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8805 _exptl_absorpt_correction_T_max 0.9125 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14428 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7253 _reflns_number_gt 4607 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The structure was solved by direct methods. Data was processed to a resolution of 0.80 angstroms. All non hydrogen atoms were refined anisotropically Hydrogen atoms H1, H2, H15 and H16 were refined from the data and all other hydrogen atoms were included in calculated positions using the riding model. Alert Level A - Large non-solvent H, the four allylic H's were refined freely, and the rest were H-fixed. One of the four allyic H's is on the border of being refined freely, but the bond length fits in with the other three allyic H's. C7 and C21 have been split and modelled represent one of the two directions in which the THF moiety kinked. 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^)+(0.0959P)^2^+0.2496P] 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 7253 _refine_ls_number_parameters 373 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1659 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 H2 H 0.308(3) 0.936(3) 0.1342(14) 0.019(7) Uiso 1 1 d . . . H15 H 0.074(3) 0.891(3) 0.3626(14) 0.023(7) Uiso 1 1 d . . . Si4 Si 0.16332(8) 1.23000(8) 0.43235(4) 0.02043(19) Uani 1 1 d . . . Si3 Si 0.31508(7) 0.70911(8) 0.37442(4) 0.01994(19) Uani 1 1 d . . . Si2 Si 0.32699(7) 0.70918(8) 0.07578(4) 0.02033(19) Uani 1 1 d . . . Si1 Si 0.16497(8) 1.22249(8) 0.13594(4) 0.0230(2) Uani 1 1 d . . . O1 O -0.02878(18) 0.8512(2) 0.21725(10) 0.0233(4) Uani 1 1 d . E . O2 O -0.13048(18) 1.1772(2) 0.28430(10) 0.0252(4) Uani 1 1 d . F . C14 C 0.3179(4) 0.7393(4) -0.02797(17) 0.0448(9) Uani 1 1 d . . . H14A H 0.2204 0.7569 -0.0473 0.067 Uiso 1 1 calc R . . H14B H 0.3912 0.6561 -0.0419 0.067 Uiso 1 1 calc R . . H14C H 0.3375 0.8206 -0.0489 0.067 Uiso 1 1 calc R . . C3 C 0.1771(3) 0.8556(3) 0.10485(13) 0.0170(5) Uani 1 1 d . E . C15 C 0.1688(3) 0.8871(3) 0.35518(14) 0.0179(5) Uani 1 1 d . E . C25 C 0.3069(3) 0.5979(3) 0.46553(15) 0.0247(6) Uani 1 1 d . . . H25A H 0.3255 0.6353 0.5061 0.037 Uiso 1 1 calc R . . H25B H 0.3811 0.5014 0.4705 0.037 Uiso 1 1 calc R . . H25C H 0.2098 0.5988 0.4676 0.037 Uiso 1 1 calc R . . C28 C 0.3475(3) 1.2018(4) 0.40251(19) 0.0383(8) Uani 1 1 d . . . H28A H 0.4179 1.1054 0.4250 0.057 Uiso 1 1 calc R . . H28B H 0.3775 1.2676 0.4185 0.057 Uiso 1 1 calc R . . H28C H 0.3443 1.2174 0.3483 0.057 Uiso 1 1 calc R . . C27 C 0.1750(3) 1.1993(3) 0.53592(15) 0.0306(7) Uani 1 1 d . . . H27A H 0.0807 1.2076 0.5533 0.046 Uiso 1 1 calc R . . H27B H 0.1997 1.2691 0.5510 0.046 Uiso 1 1 calc R . . H27C H 0.2508 1.1050 0.5577 0.046 Uiso 1 1 calc R . . C4 C 0.0204(3) 0.8762(3) 0.08929(14) 0.0200(6) Uani 1 1 d . . . H4A H -0.0449 0.9778 0.0790 0.024 Uiso 1 1 calc R . . H4B H 0.0146 0.8435 0.0439 0.024 Uiso 1 1 calc R . . C17 C 0.0983(2) 1.1128(3) 0.40076(13) 0.0174(5) Uani 1 1 d . E . C11 C 0.1553(4) 1.3046(4) 0.03583(16) 0.0457(9) Uani 1 1 d . . . H11A H 0.2155 1.2328 0.0099 0.068 Uiso 1 1 calc R . . H11B H 0.1915 1.3768 0.0306 0.068 Uiso 1 1 calc R . . H11C H 0.0537 1.3476 0.0142 0.068 Uiso 1 1 calc R . . C13 C 0.3117(3) 0.5401(3) 0.10942(17) 0.0320(7) Uani 1 1 d . . . H13A H 0.3203 0.5159 0.1638 0.048 Uiso 1 1 calc R . . H13B H 0.3901 0.4656 0.0915 0.048 Uiso 1 1 calc R . . H13C H 0.2168 0.5502 0.0905 0.048 Uiso 1 1 calc R . . C1 C 0.1091(3) 1.0788(3) 0.15260(14) 0.0209(6) Uani 1 1 d . E . C2 C 0.2035(3) 0.9555(3) 0.12917(14) 0.0191(6) Uani 1 1 d . E . C18 C -0.0589(2) 1.1351(3) 0.41377(14) 0.0183(5) Uani 1 1 d . . . H18A H -0.0624 1.0428 0.4239 0.022 Uiso 1 1 calc R . . H18B H -0.0858 1.1729 0.4586 0.022 Uiso 1 1 calc R . . C12 C 0.5107(3) 0.6852(4) 0.1109(2) 0.0423(8) Uani 1 1 d . . . H12A H 0.5232 0.7708 0.0909 0.063 Uiso 1 1 calc R . . H12B H 0.5869 0.6062 0.0950 0.063 Uiso 1 1 calc R . . H12C H 0.5182 0.6659 0.1653 0.063 Uiso 1 1 calc R . . C10 C 0.3582(4) 1.1554(4) 0.1751(2) 0.0516(10) Uani 1 1 d . . . H10A H 0.3679 1.1094 0.2278 0.077 Uiso 1 1 calc R . . H10B H 0.3851 1.2338 0.1699 0.077 Uiso 1 1 calc R . . H10C H 0.4230 1.0876 0.1482 0.077 Uiso 1 1 calc R . . C26 C 0.0356(3) 1.4195(3) 0.39651(17) 0.0343(7) Uani 1 1 d . . . H26A H 0.0258 1.4420 0.3421 0.051 Uiso 1 1 calc R . . H26B H 0.0746 1.4780 0.4139 0.051 Uiso 1 1 calc R . . H26C H -0.0603 1.4375 0.4148 0.051 Uiso 1 1 calc R . . C5 C -0.0358(3) 0.8008(3) 0.15132(14) 0.0207(6) Uani 1 1 d . E . H5 H 0.0283 0.6977 0.1615 0.025 Uiso 1 1 calc R . . C20 C -0.3259(3) 1.2452(3) 0.35829(16) 0.0293(7) Uani 1 1 d . . . H20A H -0.3256 1.1714 0.4007 0.035 Uiso 1 1 calc R A 1 H20B H -0.3905 1.3379 0.3674 0.035 Uiso 1 1 calc R A 1 C16 C 0.1928(3) 0.9933(3) 0.37971(13) 0.0180(6) Uani 1 1 d . E . C19 C -0.1719(3) 1.2330(3) 0.34981(14) 0.0203(6) Uani 1 1 d . F . H19 H -0.1737 1.3283 0.3407 0.024 Uiso 1 1 calc R . . C24 C 0.4975(3) 0.7139(3) 0.37058(19) 0.0395(8) Uani 1 1 d . . . H24A H 0.4997 0.7744 0.3233 0.059 Uiso 1 1 calc R . . H24B H 0.5742 0.6188 0.3747 0.059 Uiso 1 1 calc R . . H24C H 0.5143 0.7510 0.4117 0.059 Uiso 1 1 calc R . . C22 C -0.2615(3) 1.2361(3) 0.23459(16) 0.0326(7) Uani 1 1 d . . . H22A H -0.2519 1.1800 0.1974 0.039 Uiso 1 1 calc R B 1 H22B H -0.2857 1.3342 0.2086 0.039 Uiso 1 1 calc R B 1 C8 C -0.1316(3) 0.8266(3) 0.26574(16) 0.0314(7) Uani 1 1 d . . . H8A H -0.1893 0.9114 0.2844 0.038 Uiso 1 1 calc R C 1 H8B H -0.0789 0.7479 0.3089 0.038 Uiso 1 1 calc R C 1 C6 C -0.1939(3) 0.8255(3) 0.14160(16) 0.0306(7) Uani 1 1 d . . . H6A H -0.2048 0.7620 0.1132 0.037 Uiso 1 1 calc R D 1 H6B H -0.2569 0.9239 0.1160 0.037 Uiso 1 1 calc R D 1 C23 C 0.3005(3) 0.6116(3) 0.30442(16) 0.0365(8) Uani 1 1 d . . . H23A H 0.2024 0.6151 0.3020 0.055 Uiso 1 1 calc R . . H23B H 0.3732 0.5136 0.3192 0.055 Uiso 1 1 calc R . . H23C H 0.3184 0.6552 0.2555 0.055 Uiso 1 1 calc R . . C7 C -0.2308(7) 0.7919(11) 0.2228(3) 0.0395(18) Uani 0.760(15) 1 d PU E 1 H7A H -0.3346 0.8505 0.2280 0.047 Uiso 0.760(15) 1 calc PR E 1 H7B H -0.2106 0.6917 0.2396 0.047 Uiso 0.760(15) 1 calc PR E 1 C7A C -0.2652(17) 0.874(3) 0.2057(11) 0.032(4) Uani 0.240(15) 1 d PU E 2 H7A1 H -0.3305 0.8292 0.2235 0.039 Uiso 0.240(15) 1 calc PR E 2 H7A2 H -0.3226 0.9772 0.1934 0.039 Uiso 0.240(15) 1 calc PR E 2 C21 C -0.3781(6) 1.2282(9) 0.2883(4) 0.0254(15) Uani 0.72(2) 1 d PU F 1 H21A H -0.4760 1.3043 0.2692 0.030 Uiso 0.72(2) 1 calc PR F 1 H21B H -0.3828 1.1367 0.2956 0.030 Uiso 0.72(2) 1 calc PR F 1 C21A C -0.3851(17) 1.290(3) 0.2682(10) 0.036(4) Uani 0.28(2) 1 d PU F 2 H21C H -0.4524 1.2485 0.2594 0.043 Uiso 0.28(2) 1 calc PR F 2 H21D H -0.4360 1.3930 0.2502 0.043 Uiso 0.28(2) 1 calc PR F 2 C9 C 0.0446(4) 1.3637(4) 0.1814(2) 0.0548(11) Uani 1 1 d . . . H9A H -0.0569 1.3994 0.1611 0.082 Uiso 1 1 calc R . . H9B H 0.0749 1.4403 0.1720 0.082 Uiso 1 1 calc R . . H9C H 0.0528 1.3255 0.2351 0.082 Uiso 1 1 calc R . . Li2 Li 0.0687(5) 1.1012(5) 0.2704(3) 0.0254(10) Uani 1 1 d . . . Li1 Li 0.1399(5) 0.8738(5) 0.2360(2) 0.0252(10) Uani 1 1 d . . . H16 H 0.286(3) 0.984(2) 0.3776(12) 0.006(6) Uiso 1 1 d . . . H1 H 0.006(3) 1.112(3) 0.1426(15) 0.024(7) 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 Si4 0.0211(4) 0.0260(4) 0.0230(4) -0.0104(3) 0.0050(3) -0.0162(3) Si3 0.0165(4) 0.0204(4) 0.0195(4) -0.0045(3) 0.0012(3) -0.0046(3) Si2 0.0174(4) 0.0233(4) 0.0230(4) -0.0084(3) 0.0054(3) -0.0100(3) Si1 0.0332(4) 0.0246(4) 0.0206(4) -0.0082(3) 0.0064(3) -0.0200(4) O1 0.0215(9) 0.0372(12) 0.0193(9) -0.0098(8) 0.0058(7) -0.0189(9) O2 0.0165(9) 0.0363(12) 0.0191(10) -0.0059(8) -0.0011(7) -0.0080(8) C14 0.0413(19) 0.049(2) 0.0283(17) -0.0101(15) 0.0123(14) -0.0038(17) C3 0.0160(12) 0.0174(14) 0.0185(13) -0.0044(10) 0.0051(10) -0.0079(11) C15 0.0123(12) 0.0188(14) 0.0246(14) -0.0053(11) -0.0001(10) -0.0085(11) C25 0.0241(14) 0.0240(16) 0.0247(14) -0.0059(11) 0.0004(11) -0.0088(12) C28 0.0311(16) 0.054(2) 0.052(2) -0.0286(17) 0.0168(15) -0.0317(16) C27 0.0353(16) 0.0428(19) 0.0258(15) -0.0127(13) 0.0056(12) -0.0261(15) C4 0.0197(13) 0.0259(15) 0.0184(13) -0.0081(11) 0.0022(10) -0.0122(12) C17 0.0111(12) 0.0250(15) 0.0187(13) -0.0046(11) 0.0023(10) -0.0103(11) C11 0.084(3) 0.054(2) 0.0230(16) -0.0055(15) 0.0062(16) -0.054(2) C13 0.0323(16) 0.0267(17) 0.0442(18) -0.0157(14) 0.0123(14) -0.0160(14) C1 0.0214(14) 0.0220(15) 0.0230(14) -0.0061(11) 0.0017(11) -0.0123(12) C2 0.0188(13) 0.0276(15) 0.0169(13) -0.0029(11) 0.0024(10) -0.0167(12) C18 0.0160(12) 0.0239(15) 0.0197(13) -0.0076(11) 0.0034(10) -0.0119(11) C12 0.0220(15) 0.044(2) 0.065(2) -0.0207(17) 0.0068(15) -0.0150(15) C10 0.055(2) 0.045(2) 0.067(3) -0.0044(18) -0.0095(19) -0.0374(19) C26 0.0444(18) 0.0289(17) 0.0368(17) -0.0113(13) 0.0000(14) -0.0207(15) C5 0.0205(13) 0.0274(15) 0.0221(14) -0.0125(11) 0.0055(11) -0.0147(12) C20 0.0140(13) 0.0397(18) 0.0357(17) -0.0148(14) 0.0032(11) -0.0100(13) C16 0.0108(12) 0.0262(15) 0.0188(13) -0.0035(11) 0.0020(10) -0.0103(11) C19 0.0146(12) 0.0227(15) 0.0254(14) -0.0107(11) 0.0021(10) -0.0072(11) C24 0.0203(15) 0.0330(19) 0.055(2) -0.0007(15) 0.0088(14) -0.0066(14) C22 0.0183(14) 0.047(2) 0.0253(15) -0.0021(13) -0.0090(11) -0.0094(14) C8 0.0306(16) 0.047(2) 0.0266(16) -0.0130(14) 0.0141(12) -0.0246(15) C6 0.0232(15) 0.049(2) 0.0321(16) -0.0152(14) 0.0064(12) -0.0247(15) C23 0.0434(18) 0.0213(16) 0.0286(16) -0.0072(13) -0.0050(13) 0.0022(14) C7 0.031(3) 0.074(5) 0.029(3) -0.012(3) 0.012(2) -0.037(4) C7A 0.017(6) 0.056(8) 0.038(7) -0.027(7) 0.010(5) -0.022(7) C21 0.015(2) 0.023(4) 0.036(3) -0.011(3) 0.004(2) -0.005(3) C21A 0.022(5) 0.043(8) 0.034(7) -0.004(6) -0.012(5) -0.008(7) C9 0.086(3) 0.036(2) 0.070(3) -0.0346(19) 0.048(2) -0.042(2) Li2 0.022(2) 0.030(3) 0.027(2) -0.006(2) 0.0004(18) -0.013(2) Li1 0.022(2) 0.035(3) 0.022(2) -0.003(2) 0.0004(18) -0.017(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 Si4 C17 1.846(3) . ? Si4 C28 1.859(3) . ? Si4 C27 1.870(3) . ? Si4 C26 1.873(3) . ? Si3 C15 1.827(3) . ? Si3 C24 1.872(3) . ? Si3 C25 1.873(3) . ? Si3 C23 1.879(3) . ? Si2 C3 1.851(3) . ? Si2 C13 1.870(3) . ? Si2 C12 1.870(3) . ? Si2 C14 1.874(3) . ? Si1 C1 1.832(3) . ? Si1 C11 1.859(3) . ? Si1 C9 1.868(3) . ? Si1 C10 1.868(3) . ? O1 C8 1.440(3) . ? O1 C5 1.453(3) . ? O1 Li1 1.870(5) . ? O2 C22 1.440(3) . ? O2 C19 1.450(3) . ? O2 Li2 1.871(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C3 C2 1.376(4) . ? C3 C4 1.529(3) . ? C3 Li1 2.489(5) . ? C15 C16 1.428(4) . ? C15 Li1 2.272(5) . ? C15 Li2 2.310(5) . ? C15 H15 0.95(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C4 C5 1.511(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C17 C16 1.380(4) . ? C17 C18 1.533(3) . ? C17 Li2 2.470(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C1 C2 1.431(4) . ? C1 Li2 2.260(5) . ? C1 Li1 2.313(5) . ? C1 H1 0.96(3) . ? C2 Li1 2.194(5) . ? C2 H2 0.99(3) . ? C18 C19 1.516(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C5 C6 1.515(3) . ? C5 H5 1.0000 . ? C20 C21 1.479(7) . ? C20 C19 1.520(3) . ? C20 C21A 1.674(17) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C16 Li2 2.198(5) . ? C16 H16 0.91(2) . ? C19 H19 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C22 C21A 1.350(17) . ? C22 C21 1.556(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C8 C7 1.498(6) . ? C8 C7A 1.591(17) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C6 C7A 1.462(16) . ? C6 C7 1.549(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? 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 C17 Si4 C28 111.35(13) . . ? C17 Si4 C27 111.06(12) . . ? C28 Si4 C27 107.88(14) . . ? C17 Si4 C26 112.03(12) . . ? C28 Si4 C26 108.45(15) . . ? C27 Si4 C26 105.83(15) . . ? C15 Si3 C24 110.33(13) . . ? C15 Si3 C25 113.07(12) . . ? C24 Si3 C25 110.16(13) . . ? C15 Si3 C23 111.27(12) . . ? C24 Si3 C23 107.85(15) . . ? C25 Si3 C23 103.88(13) . . ? C3 Si2 C13 111.43(12) . . ? C3 Si2 C12 111.87(14) . . ? C13 Si2 C12 108.39(15) . . ? C3 Si2 C14 110.89(13) . . ? C13 Si2 C14 105.35(16) . . ? C12 Si2 C14 108.65(16) . . ? C1 Si1 C11 113.46(13) . . ? C1 Si1 C9 110.03(13) . . ? C11 Si1 C9 107.28(18) . . ? C1 Si1 C10 109.70(14) . . ? C11 Si1 C10 107.17(17) . . ? C9 Si1 C10 109.07(19) . . ? C8 O1 C5 108.25(18) . . ? C8 O1 Li1 131.8(2) . . ? C5 O1 Li1 116.2(2) . . ? C22 O2 C19 106.40(19) . . ? C22 O2 Li2 133.4(2) . . ? C19 O2 Li2 116.7(2) . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C2 C3 C4 120.4(2) . . ? C2 C3 Si2 120.80(18) . . ? C4 C3 Si2 118.07(18) . . ? C2 C3 Li1 61.42(17) . . ? C4 C3 Li1 92.29(17) . . ? Si2 C3 Li1 124.71(16) . . ? C16 C15 Si3 118.83(18) . . ? C16 C15 Li1 127.1(2) . . ? Si3 C15 Li1 88.97(16) . . ? C16 C15 Li2 67.32(18) . . ? Si3 C15 Li2 144.73(18) . . ? Li1 C15 Li2 65.46(18) . . ? C16 C15 H15 113.8(16) . . ? Si3 C15 H15 113.8(16) . . ? Li1 C15 H15 89.4(16) . . ? Li2 C15 H15 90.9(16) . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si4 C27 H27A 109.5 . . ? Si4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C5 C4 C3 114.9(2) . . ? C5 C4 H4A 108.5 . . ? C3 C4 H4A 108.5 . . ? C5 C4 H4B 108.5 . . ? C3 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C16 C17 C18 119.6(2) . . ? C16 C17 Si4 121.91(17) . . ? C18 C17 Si4 117.31(18) . . ? C16 C17 Li2 62.24(18) . . ? C18 C17 Li2 92.68(17) . . ? Si4 C17 Li2 125.53(16) . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C2 C1 Si1 115.93(18) . . ? C2 C1 Li2 127.3(2) . . ? Si1 C1 Li2 90.24(16) . . ? C2 C1 Li1 67.02(18) . . ? Si1 C1 Li1 143.27(18) . . ? Li2 C1 Li1 65.59(18) . . ? C2 C1 H1 117.9(17) . . ? Si1 C1 H1 112.3(16) . . ? Li2 C1 H1 87.9(16) . . ? Li1 C1 H1 94.8(16) . . ? C3 C2 C1 132.1(2) . . ? C3 C2 Li1 85.17(19) . . ? C1 C2 Li1 76.1(2) . . ? C3 C2 H2 114.6(15) . . ? C1 C2 H2 113.3(15) . . ? Li1 C2 H2 110.0(15) . . ? C19 C18 C17 114.8(2) . . ? C19 C18 H18A 108.6 . . ? C17 C18 H18A 108.6 . . ? C19 C18 H18B 108.6 . . ? C17 C18 H18B 108.6 . . ? H18A C18 H18B 107.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1 C5 C4 108.0(2) . . ? O1 C5 C6 103.6(2) . . ? C4 C5 C6 117.4(2) . . ? O1 C5 H5 109.2 . . ? C4 C5 H5 109.2 . . ? C6 C5 H5 109.2 . . ? C21 C20 C19 107.2(3) . . ? C21 C20 C21A 23.3(8) . . ? C19 C20 C21A 98.6(7) . . ? C21 C20 H20A 110.3 . . ? C19 C20 H20A 110.3 . . ? C21A C20 H20A 133.0 . . ? C21 C20 H20B 110.3 . . ? C19 C20 H20B 110.3 . . ? C21A C20 H20B 94.3 . . ? H20A C20 H20B 108.5 . . ? C17 C16 C15 131.8(2) . . ? C17 C16 Li2 84.0(2) . . ? C15 C16 Li2 75.84(19) . . ? C17 C16 H16 113.8(15) . . ? C15 C16 H16 114.2(15) . . ? Li2 C16 H16 110.3(14) . . ? O2 C19 C18 108.1(2) . . ? O2 C19 C20 104.3(2) . . ? C18 C19 C20 115.7(2) . . ? O2 C19 H19 109.5 . . ? C18 C19 H19 109.5 . . ? C20 C19 H19 109.5 . . ? Si3 C24 H24A 109.5 . . ? Si3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21A C22 O2 113.4(7) . . ? C21A C22 C21 25.2(10) . . ? O2 C22 C21 102.4(3) . . ? C21A C22 H22A 122.5 . . ? O2 C22 H22A 111.3 . . ? C21 C22 H22A 111.3 . . ? C21A C22 H22B 86.1 . . ? O2 C22 H22B 111.3 . . ? C21 C22 H22B 111.3 . . ? H22A C22 H22B 109.2 . . ? O1 C8 C7 108.4(3) . . ? O1 C8 C7A 99.1(7) . . ? C7 C8 C7A 29.6(7) . . ? O1 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? C7A C8 H8A 88.1 . . ? O1 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? C7A C8 H8B 138.0 . . ? H8A C8 H8B 108.4 . . ? C7A C6 C5 107.9(6) . . ? C7A C6 C7 30.4(8) . . ? C5 C6 C7 102.7(3) . . ? C7A C6 H6A 131.1 . . ? C5 C6 H6A 111.2 . . ? C7 C6 H6A 111.2 . . ? C7A C6 H6B 81.8 . . ? C5 C6 H6B 111.2 . . ? C7 C6 H6B 111.2 . . ? H6A C6 H6B 109.1 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 C7 C6 103.4(3) . . ? C8 C7 H7A 111.1 . . ? C6 C7 H7A 111.1 . . ? C8 C7 H7B 111.1 . . ? C6 C7 H7B 111.1 . . ? H7A C7 H7B 109.0 . . ? C6 C7A C8 103.1(9) . . ? C6 C7A H7A1 111.1 . . ? C8 C7A H7A1 111.1 . . ? C6 C7A H7A2 111.1 . . ? C8 C7A H7A2 111.1 . . ? H7A1 C7A H7A2 109.1 . . ? C20 C21 C22 103.7(4) . . ? C20 C21 H21A 111.0 . . ? C22 C21 H21A 111.0 . . ? C20 C21 H21B 111.0 . . ? C22 C21 H21B 111.0 . . ? H21A C21 H21B 109.0 . . ? C22 C21A C20 103.7(9) . . ? C22 C21A H21C 111.0 . . ? C20 C21A H21C 111.0 . . ? C22 C21A H21D 111.0 . . ? C20 C21A H21D 111.0 . . ? H21C C21A H21D 109.0 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 Li2 C16 108.3(2) . . ? O2 Li2 C1 112.2(2) . . ? C16 Li2 C1 135.1(2) . . ? O2 Li2 C15 104.8(2) . . ? C16 Li2 C15 36.84(12) . . ? C1 Li2 C15 112.1(2) . . ? O2 Li2 C17 83.74(19) . . ? C16 Li2 C17 33.76(11) . . ? C1 Li2 C17 163.7(2) . . ? C15 Li2 C17 64.77(14) . . ? O1 Li1 C2 108.0(2) . . ? O1 Li1 C15 112.1(2) . . ? C2 Li1 C15 135.2(2) . . ? O1 Li1 C1 104.7(2) . . ? C2 Li1 C1 36.90(12) . . ? C15 Li1 C1 111.6(2) . . ? O1 Li1 C3 83.55(18) . . ? C2 Li1 C3 33.41(11) . . ? C15 Li1 C3 164.2(2) . . ? C1 Li1 C3 64.44(14) . . ? 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 C13 Si2 C3 C2 139.3(2) . . . . ? C12 Si2 C3 C2 17.7(3) . . . . ? C14 Si2 C3 C2 -103.7(2) . . . . ? C13 Si2 C3 C4 -50.5(2) . . . . ? C12 Si2 C3 C4 -172.0(2) . . . . ? C14 Si2 C3 C4 66.5(2) . . . . ? C13 Si2 C3 Li1 64.6(2) . . . . ? C12 Si2 C3 Li1 -56.9(2) . . . . ? C14 Si2 C3 Li1 -178.38(19) . . . . ? C24 Si3 C15 C16 -34.2(2) . . . . ? C25 Si3 C15 C16 89.7(2) . . . . ? C23 Si3 C15 C16 -153.8(2) . . . . ? C24 Si3 C15 Li1 98.60(17) . . . . ? C25 Si3 C15 Li1 -137.53(15) . . . . ? C23 Si3 C15 Li1 -21.07(18) . . . . ? C24 Si3 C15 Li2 56.8(3) . . . . ? C25 Si3 C15 Li2 -179.4(3) . . . . ? C23 Si3 C15 Li2 -62.9(3) . . . . ? C2 C3 C4 C5 -98.3(3) . . . . ? Si2 C3 C4 C5 91.5(2) . . . . ? Li1 C3 C4 C5 -40.4(2) . . . . ? C28 Si4 C17 C16 19.0(3) . . . . ? C27 Si4 C17 C16 -101.3(2) . . . . ? C26 Si4 C17 C16 140.6(2) . . . . ? C28 Si4 C17 C18 -173.46(19) . . . . ? C27 Si4 C17 C18 66.3(2) . . . . ? C26 Si4 C17 C18 -51.8(2) . . . . ? C28 Si4 C17 Li2 -57.8(2) . . . . ? C27 Si4 C17 Li2 -178.02(19) . . . . ? C26 Si4 C17 Li2 63.9(2) . . . . ? C11 Si1 C1 C2 67.6(2) . . . . ? C9 Si1 C1 C2 -172.2(2) . . . . ? C10 Si1 C1 C2 -52.2(3) . . . . ? C11 Si1 C1 Li2 -159.88(18) . . . . ? C9 Si1 C1 Li2 -39.7(2) . . . . ? C10 Si1 C1 Li2 80.3(2) . . . . ? C11 Si1 C1 Li1 153.4(3) . . . . ? C9 Si1 C1 Li1 -86.4(3) . . . . ? C10 Si1 C1 Li1 33.6(3) . . . . ? C4 C3 C2 C1 8.2(4) . . . . ? Si2 C3 C2 C1 178.2(2) . . . . ? Li1 C3 C2 C1 -66.3(3) . . . . ? C4 C3 C2 Li1 74.5(2) . . . . ? Si2 C3 C2 Li1 -115.5(2) . . . . ? Si1 C1 C2 C3 -150.3(2) . . . . ? Li2 C1 C2 C3 97.6(3) . . . . ? Li1 C1 C2 C3 70.1(3) . . . . ? Si1 C1 C2 Li1 139.6(2) . . . . ? Li2 C1 C2 Li1 27.5(3) . . . . ? C16 C17 C18 C19 -99.9(3) . . . . ? Si4 C17 C18 C19 92.2(2) . . . . ? Li2 C17 C18 C19 -40.6(2) . . . . ? C8 O1 C5 C4 157.2(2) . . . . ? Li1 O1 C5 C4 -42.2(3) . . . . ? C8 O1 C5 C6 32.0(3) . . . . ? Li1 O1 C5 C6 -167.4(2) . . . . ? C3 C4 C5 O1 59.1(3) . . . . ? C3 C4 C5 C6 175.6(2) . . . . ? C18 C17 C16 C15 11.3(4) . . . . ? Si4 C17 C16 C15 178.6(2) . . . . ? Li2 C17 C16 C15 -64.9(3) . . . . ? C18 C17 C16 Li2 76.2(2) . . . . ? Si4 C17 C16 Li2 -116.5(2) . . . . ? Si3 C15 C16 C17 -150.5(2) . . . . ? Li1 C15 C16 C17 96.5(3) . . . . ? Li2 C15 C16 C17 68.3(3) . . . . ? Si3 C15 C16 Li2 141.3(2) . . . . ? Li1 C15 C16 Li2 28.3(3) . . . . ? C22 O2 C19 C18 158.0(2) . . . . ? Li2 O2 C19 C18 -40.0(3) . . . . ? C22 O2 C19 C20 34.4(3) . . . . ? Li2 O2 C19 C20 -163.6(2) . . . . ? C17 C18 C19 O2 57.7(3) . . . . ? C17 C18 C19 C20 174.1(2) . . . . ? C21 C20 C19 O2 -13.1(5) . . . . ? C21A C20 C19 O2 -35.4(10) . . . . ? C21 C20 C19 C18 -131.6(4) . . . . ? C21A C20 C19 C18 -153.9(10) . . . . ? C19 O2 C22 C21A -17.2(14) . . . . ? Li2 O2 C22 C21A -174.9(14) . . . . ? C19 O2 C22 C21 -41.1(4) . . . . ? Li2 O2 C22 C21 161.3(4) . . . . ? C5 O1 C8 C7 -13.6(5) . . . . ? Li1 O1 C8 C7 -170.1(5) . . . . ? C5 O1 C8 C7A -42.6(9) . . . . ? Li1 O1 C8 C7A 160.9(9) . . . . ? O1 C5 C6 C7A -5.9(12) . . . . ? C4 C5 C6 C7A -124.7(12) . . . . ? O1 C5 C6 C7 -36.9(4) . . . . ? C4 C5 C6 C7 -155.8(4) . . . . ? O1 C8 C7 C6 -10.0(7) . . . . ? C7A C8 C7 C6 65.6(13) . . . . ? C7A C6 C7 C8 -75.3(13) . . . . ? C5 C6 C7 C8 28.6(6) . . . . ? C5 C6 C7A C8 -19.0(16) . . . . ? C7 C6 C7A C8 65.5(14) . . . . ? O1 C8 C7A C6 36.8(15) . . . . ? C7 C8 C7A C6 -74.6(14) . . . . ? C19 C20 C21 C22 -11.0(6) . . . . ? C21A C20 C21 C22 60.2(17) . . . . ? C21A C22 C21 C20 -87.9(19) . . . . ? O2 C22 C21 C20 31.4(6) . . . . ? O2 C22 C21A C20 -6.2(19) . . . . ? C21 C22 C21A C20 62.0(15) . . . . ? C21 C20 C21A C22 -88(2) . . . . ? C19 C20 C21A C22 25.6(17) . . . . ? C22 O2 Li2 C16 -167.3(3) . . . . ? C19 O2 Li2 C16 36.8(3) . . . . ? C22 O2 Li2 C1 -7.1(4) . . . . ? C19 O2 Li2 C1 -163.0(2) . . . . ? C22 O2 Li2 C15 -129.0(3) . . . . ? C19 O2 Li2 C15 75.1(3) . . . . ? C22 O2 Li2 C17 169.2(3) . . . . ? C19 O2 Li2 C17 13.3(2) . . . . ? C17 C16 Li2 O2 -45.4(2) . . . . ? C15 C16 Li2 O2 90.4(2) . . . . ? C17 C16 Li2 C1 161.0(3) . . . . ? C15 C16 Li2 C1 -63.1(3) . . . . ? C17 C16 Li2 C15 -135.9(2) . . . . ? C15 C16 Li2 C17 135.9(2) . . . . ? C2 C1 Li2 O2 -127.6(3) . . . . ? Si1 C1 Li2 O2 108.9(2) . . . . ? Li1 C1 Li2 O2 -99.7(3) . . . . ? C2 C1 Li2 C16 25.3(5) . . . . ? Si1 C1 Li2 C16 -98.3(3) . . . . ? Li1 C1 Li2 C16 53.2(3) . . . . ? C2 C1 Li2 C15 -10.0(3) . . . . ? Si1 C1 Li2 C15 -133.53(18) . . . . ? Li1 C1 Li2 C15 17.90(18) . . . . ? C2 C1 Li2 C17 65.5(9) . . . . ? Si1 C1 Li2 C17 -58.0(9) . . . . ? Li1 C1 Li2 C17 93.4(9) . . . . ? C16 C15 Li2 O2 -100.9(2) . . . . ? Si3 C15 Li2 O2 150.8(2) . . . . ? Li1 C15 Li2 O2 103.7(2) . . . . ? Si3 C15 Li2 C16 -108.3(3) . . . . ? Li1 C15 Li2 C16 -155.5(2) . . . . ? C16 C15 Li2 C1 137.2(2) . . . . ? Si3 C15 Li2 C1 28.9(4) . . . . ? Li1 C15 Li2 C1 -18.25(19) . . . . ? C16 C15 Li2 C17 -25.32(14) . . . . ? Si3 C15 Li2 C17 -133.6(3) . . . . ? Li1 C15 Li2 C17 179.21(18) . . . . ? C16 C17 Li2 O2 137.1(2) . . . . ? C18 C17 Li2 O2 14.8(2) . . . . ? Si4 C17 Li2 O2 -111.90(19) . . . . ? C18 C17 Li2 C16 -122.3(2) . . . . ? Si4 C17 Li2 C16 111.0(2) . . . . ? C16 C17 Li2 C1 -55.1(9) . . . . ? C18 C17 Li2 C1 -177.4(8) . . . . ? Si4 C17 Li2 C1 55.9(9) . . . . ? C16 C17 Li2 C15 27.48(15) . . . . ? C18 C17 Li2 C15 -94.82(17) . . . . ? Si4 C17 Li2 C15 138.46(17) . . . . ? C8 O1 Li1 C2 -166.9(2) . . . . ? C5 O1 Li1 C2 38.1(3) . . . . ? C8 O1 Li1 C15 -7.5(4) . . . . ? C5 O1 Li1 C15 -162.5(2) . . . . ? C8 O1 Li1 C1 -128.5(3) . . . . ? C5 O1 Li1 C1 76.4(3) . . . . ? C8 O1 Li1 C3 170.1(2) . . . . ? C5 O1 Li1 C3 15.0(2) . . . . ? C3 C2 Li1 O1 -45.0(3) . . . . ? C1 C2 Li1 O1 90.6(3) . . . . ? C3 C2 Li1 C15 162.6(3) . . . . ? C1 C2 Li1 C15 -61.9(3) . . . . ? C3 C2 Li1 C1 -135.5(2) . . . . ? C1 C2 Li1 C3 135.5(2) . . . . ? C16 C15 Li1 O1 -127.9(3) . . . . ? Si3 C15 Li1 O1 105.8(2) . . . . ? Li2 C15 Li1 O1 -99.2(3) . . . . ? C16 C15 Li1 C2 23.8(5) . . . . ? Si3 C15 Li1 C2 -102.5(3) . . . . ? Li2 C15 Li1 C2 52.5(3) . . . . ? C16 C15 Li1 C1 -11.0(3) . . . . ? Si3 C15 Li1 C1 -137.19(18) . . . . ? Li2 C15 Li1 C1 17.76(19) . . . . ? C16 C15 Li1 C3 61.1(10) . . . . ? Si3 C15 Li1 C3 -65.1(9) . . . . ? Li2 C15 Li1 C3 89.8(9) . . . . ? C2 C1 Li1 O1 -100.6(2) . . . . ? Si1 C1 Li1 O1 156.3(2) . . . . ? Li2 C1 Li1 O1 103.2(2) . . . . ? Si1 C1 Li1 C2 -103.1(3) . . . . ? Li2 C1 Li1 C2 -156.2(2) . . . . ? C2 C1 Li1 C15 138.0(2) . . . . ? Si1 C1 Li1 C15 35.0(4) . . . . ? Li2 C1 Li1 C15 -18.14(19) . . . . ? C2 C1 Li1 C3 -25.31(14) . . . . ? Si1 C1 Li1 C3 -128.4(3) . . . . ? Li2 C1 Li1 C3 178.53(19) . . . . ? C2 C3 Li1 O1 137.5(2) . . . . ? C4 C3 Li1 O1 13.8(2) . . . . ? Si2 C3 Li1 O1 -113.16(19) . . . . ? C4 C3 Li1 C2 -123.7(2) . . . . ? Si2 C3 Li1 C2 109.4(2) . . . . ? C2 C3 Li1 C15 -51.0(9) . . . . ? C4 C3 Li1 C15 -174.7(9) . . . . ? Si2 C3 Li1 C15 58.4(10) . . . . ? C2 C3 Li1 C1 27.79(16) . . . . ? C4 C3 Li1 C1 -95.91(17) . . . . ? Si2 C3 Li1 C1 137.18(17) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.624 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.081 # Attachment '2_thf.cif' data_compound[2(thf)]2 _database_code_depnum_ccdc_archive 'CCDC 678935' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H74 K2 O4 Si4' _chemical_formula_weight 761.51 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' Si Si 0.0817 0.0704 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.9205(18) _cell_length_b 18.729(3) _cell_length_c 11.2860(18) _cell_angle_alpha 90.00 _cell_angle_beta 97.988(3) _cell_angle_gamma 90.00 _cell_volume 2285.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3567 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 24.44 _exptl_crystal_description Needle _exptl_crystal_colour Pink _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7249 _exptl_absorpt_correction_T_max 0.9344 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14374 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 28.30 _reflns_number_total 8085 _reflns_number_gt 6906 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. Data was processed to a resolution of 0.75 angstroms. All non hydrogen atoms were refined anisotropically Hydrogen atoms H1, H2, H15 and H16 were refined from the data and all other hydrogen atoms were included in calculated positions using the riding model. Atoms O4, C35 and C36 of the THF molecule O4C33-C36 are partially disordered over 2 sites. Geometrical and displacement restraints were applied to O4, C35 and C36 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^)+(0.0716P)^2^+0.1503P] 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 0.04(4) _refine_ls_number_reflns 8085 _refine_ls_number_parameters 471 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.009 _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 0.44891(7) 0.66767(4) 0.85598(6) 0.02815(17) Uani 1 1 d . . . K2 K 0.92802(7) 0.72007(4) 0.70892(7) 0.03351(19) Uani 1 1 d . . . Si1 Si 0.18779(9) 0.59393(6) 0.58418(9) 0.0309(2) Uani 1 1 d . . . Si2 Si 0.13709(9) 0.66630(7) 1.05814(9) 0.0352(2) Uani 1 1 d . . . Si3 Si 0.71260(9) 0.54395(5) 0.74208(9) 0.0298(2) Uani 1 1 d . . . Si4 Si 0.56671(9) 0.82377(5) 0.60495(9) 0.0293(2) Uani 1 1 d . . . O1 O 0.0407(3) 0.83424(16) 0.8133(3) 0.0481(7) Uani 1 1 d . . . O2 O 0.5577(3) 0.78080(16) 0.9686(2) 0.0394(7) Uani 1 1 d . A . O3 O 0.5372(3) 0.60501(17) 1.0693(2) 0.0422(7) Uani 1 1 d . . . O4X O 0.9680(7) 0.7884(4) 0.5099(7) 0.0495(14) Uani 0.518(7) 1 d PDU A 1 C35X C 1.0804(8) 0.8673(6) 0.4070(7) 0.0482(14) Uani 0.518(7) 1 d PDU A 1 H35A H 1.1653 0.8531 0.3957 0.058 Uiso 0.518(7) 1 calc PR A 1 H35B H 1.0716 0.9193 0.3921 0.058 Uiso 0.518(7) 1 calc PR A 1 C36X C 1.0595(8) 0.8514(5) 0.5281(7) 0.0479(13) Uani 0.518(7) 1 d PDU A 1 H36A H 1.0230 0.8927 0.5651 0.058 Uiso 0.518(7) 1 calc PR A 1 H36B H 1.1373 0.8374 0.5785 0.058 Uiso 0.518(7) 1 calc PR A 1 O4Y O 0.9482(6) 0.8164(5) 0.5252(6) 0.0480(14) Uani 0.482(7) 1 d PDU A 2 C35Y C 1.1128(7) 0.8306(7) 0.4063(7) 0.0475(14) Uani 0.482(7) 1 d PDU A 2 H35C H 1.1745 0.7983 0.3783 0.057 Uiso 0.482(7) 1 calc PR A 2 H35D H 1.1465 0.8797 0.4121 0.057 Uiso 0.482(7) 1 calc PR A 2 C36Y C 1.0827(7) 0.8085(6) 0.5136(8) 0.0497(13) Uani 0.482(7) 1 d PDU A 2 H36C H 1.1318 0.8362 0.5782 0.060 Uiso 0.482(7) 1 calc PR A 2 H36D H 1.1061 0.7576 0.5254 0.060 Uiso 0.482(7) 1 calc PR A 2 C1 C 0.1911(3) 0.6629(2) 0.6977(3) 0.0279(7) Uani 1 1 d . . . C2 C 0.1673(3) 0.6520(2) 0.8161(3) 0.0289(8) Uani 1 1 d . . . C3 C 0.1762(3) 0.6983(2) 0.9137(3) 0.0290(8) Uani 1 1 d . . . C4 C 0.2251(3) 0.7735(2) 0.9042(3) 0.0343(8) Uani 1 1 d . . . H4A H 0.2954 0.7797 0.9689 0.041 Uiso 1 1 calc R . . H4B H 0.2587 0.7771 0.8274 0.041 Uiso 1 1 calc R . . C5 C 0.1383(4) 0.8357(2) 0.9107(4) 0.0390(9) Uani 1 1 d . . . H5 H 0.1027 0.8334 0.9876 0.047 Uiso 1 1 calc R . . C6 C 0.2007(4) 0.9090(2) 0.9006(4) 0.0455(10) Uani 1 1 d . . . H6A H 0.2150 0.9328 0.9797 0.055 Uiso 1 1 calc R . . H6B H 0.2811 0.9032 0.8706 0.055 Uiso 1 1 calc R . . C7 C 0.1124(5) 0.9524(3) 0.8133(6) 0.0662(15) Uani 1 1 d . . . H7A H 0.0950 0.9994 0.8474 0.079 Uiso 1 1 calc R . . H7B H 0.1454 0.9596 0.7369 0.079 Uiso 1 1 calc R . . C8 C -0.0010(5) 0.9059(3) 0.7968(7) 0.080(2) Uani 1 1 d . . . H8A H -0.0563 0.9184 0.8561 0.096 Uiso 1 1 calc R . . H8B H -0.0470 0.9123 0.7155 0.096 Uiso 1 1 calc R . . C9 C 0.2396(4) 0.7086(3) 1.1850(4) 0.0526(12) Uani 1 1 d . . . H9A H 0.3259 0.6962 1.1799 0.079 Uiso 1 1 calc R . . H9B H 0.2171 0.6911 1.2610 0.079 Uiso 1 1 calc R . . H9C H 0.2296 0.7605 1.1809 0.079 Uiso 1 1 calc R . . C10 C 0.1524(5) 0.5664(3) 1.0715(4) 0.0550(12) Uani 1 1 d . . . H10A H 0.0835 0.5436 1.0203 0.083 Uiso 1 1 calc R . . H10B H 0.1508 0.5522 1.1548 0.083 Uiso 1 1 calc R . . H10C H 0.2307 0.5514 1.0462 0.083 Uiso 1 1 calc R . . C11 C -0.0275(4) 0.6841(3) 1.0809(3) 0.0454(11) Uani 1 1 d . . . H11A H -0.0455 0.7351 1.0698 0.068 Uiso 1 1 calc R . . H11B H -0.0394 0.6699 1.1621 0.068 Uiso 1 1 calc R . . H11C H -0.0834 0.6565 1.0227 0.068 Uiso 1 1 calc R . . C12 C 0.3224(4) 0.6055(2) 0.4986(4) 0.0394(9) Uani 1 1 d . . . H12A H 0.3254 0.6551 0.4714 0.059 Uiso 1 1 calc R . . H12B H 0.3125 0.5735 0.4291 0.059 Uiso 1 1 calc R . . H12C H 0.3993 0.5939 0.5505 0.059 Uiso 1 1 calc R . . C13 C 0.0468(4) 0.5951(3) 0.4695(4) 0.0611(14) Uani 1 1 d . . . H13A H -0.0268 0.5881 0.5088 0.092 Uiso 1 1 calc R . . H13B H 0.0523 0.5567 0.4115 0.092 Uiso 1 1 calc R . . H13C H 0.0411 0.6412 0.4280 0.092 Uiso 1 1 calc R . . C14 C 0.1959(5) 0.5028(2) 0.6536(5) 0.0524(12) Uani 1 1 d . . . H14A H 0.2705 0.4992 0.7125 0.079 Uiso 1 1 calc R . . H14B H 0.1985 0.4667 0.5913 0.079 Uiso 1 1 calc R . . H14C H 0.1227 0.4950 0.6934 0.079 Uiso 1 1 calc R . . C15 C 0.7065(3) 0.63728(19) 0.7805(3) 0.0277(7) Uani 1 1 d . A . C16 C 0.6525(3) 0.69243(19) 0.7056(3) 0.0247(7) Uani 1 1 d . A . C17 C 0.6466(3) 0.76614(19) 0.7232(3) 0.0271(7) Uani 1 1 d . A . C18 C 0.7114(4) 0.8003(2) 0.8360(3) 0.0350(9) Uani 1 1 d . . . H18A H 0.7679 0.8374 0.8124 0.042 Uiso 1 1 calc R A . H18B H 0.7634 0.7633 0.8812 0.042 Uiso 1 1 calc R . . C19 C 0.6315(4) 0.8345(2) 0.9211(3) 0.0378(9) Uani 1 1 d . A . H19 H 0.5756 0.8706 0.8762 0.045 Uiso 1 1 calc R . . C20 C 0.7055(5) 0.8708(3) 1.0319(4) 0.0522(12) Uani 1 1 d . . . H20A H 0.7956 0.8648 1.0315 0.063 Uiso 1 1 calc R A . H20B H 0.6864 0.9224 1.0334 0.063 Uiso 1 1 calc R . . C21 C 0.6647(4) 0.8333(3) 1.1387(4) 0.0472(10) Uani 1 1 d . A . H21A H 0.7248 0.7960 1.1703 0.057 Uiso 1 1 calc R . . H21B H 0.6549 0.8676 1.2034 0.057 Uiso 1 1 calc R . . C22 C 0.5428(4) 0.8009(3) 1.0882(4) 0.0452(10) Uani 1 1 d . . . H22A H 0.5242 0.7587 1.1354 0.054 Uiso 1 1 calc R A . H22B H 0.4751 0.8361 1.0880 0.054 Uiso 1 1 calc R . . C23 C 0.5887(4) 0.4881(3) 0.7942(5) 0.0512(11) Uani 1 1 d . A . H23A H 0.5911 0.4937 0.8808 0.077 Uiso 1 1 calc R . . H23B H 0.6022 0.4378 0.7756 0.077 Uiso 1 1 calc R . . H23C H 0.5078 0.5034 0.7535 0.077 Uiso 1 1 calc R . . C24 C 0.6964(5) 0.5314(2) 0.5757(4) 0.0470(11) Uani 1 1 d . A . H24A H 0.6189 0.5532 0.5384 0.071 Uiso 1 1 calc R . . H24B H 0.6957 0.4803 0.5570 0.071 Uiso 1 1 calc R . . H24C H 0.7662 0.5543 0.5446 0.071 Uiso 1 1 calc R . . C25 C 0.8638(4) 0.5049(2) 0.8142(4) 0.0443(10) Uani 1 1 d . A . H25A H 0.9321 0.5273 0.7801 0.066 Uiso 1 1 calc R . . H25B H 0.8641 0.4533 0.7994 0.066 Uiso 1 1 calc R . . H25C H 0.8737 0.5137 0.9006 0.066 Uiso 1 1 calc R . . C26 C 0.4036(4) 0.8467(3) 0.6283(4) 0.0471(11) Uani 1 1 d . A . H26A H 0.3525 0.8035 0.6194 0.071 Uiso 1 1 calc R . . H26B H 0.3696 0.8822 0.5689 0.071 Uiso 1 1 calc R . . H26C H 0.4039 0.8663 0.7089 0.071 Uiso 1 1 calc R . . C27 C 0.5505(4) 0.7805(2) 0.4537(4) 0.0423(10) Uani 1 1 d . A . H27A H 0.6325 0.7676 0.4346 0.063 Uiso 1 1 calc R . . H27B H 0.5108 0.8139 0.3934 0.063 Uiso 1 1 calc R . . H27C H 0.4997 0.7374 0.4542 0.063 Uiso 1 1 calc R . . C28 C 0.6509(4) 0.9105(2) 0.5988(4) 0.0438(10) Uani 1 1 d . A . H28A H 0.6502 0.9363 0.6741 0.066 Uiso 1 1 calc R . . H28B H 0.6101 0.9393 0.5324 0.066 Uiso 1 1 calc R . . H28C H 0.7366 0.9011 0.5866 0.066 Uiso 1 1 calc R . . C29 C 0.6644(4) 0.6182(3) 1.1079(4) 0.0425(10) Uani 1 1 d . . . H29A H 0.6889 0.6657 1.0806 0.051 Uiso 1 1 calc R . . H29B H 0.7165 0.5812 1.0770 0.051 Uiso 1 1 calc R . . C30 C 0.6766(4) 0.6153(3) 1.2452(4) 0.0486(11) Uani 1 1 d . . . H30A H 0.7603 0.5997 1.2807 0.058 Uiso 1 1 calc R . . H30B H 0.6583 0.6622 1.2792 0.058 Uiso 1 1 calc R . . C31 C 0.5799(5) 0.5603(3) 1.2644(5) 0.0616(14) Uani 1 1 d . . . H31A H 0.6195 0.5151 1.2949 0.074 Uiso 1 1 calc R . . H31B H 0.5270 0.5779 1.3227 0.074 Uiso 1 1 calc R . . C32 C 0.5062(5) 0.5492(3) 1.1464(5) 0.0625(14) Uani 1 1 d . . . H32A H 0.5253 0.5021 1.1137 0.075 Uiso 1 1 calc R . . H32B H 0.4169 0.5509 1.1533 0.075 Uiso 1 1 calc R . . C33 C 0.8978(4) 0.8006(2) 0.3978(4) 0.0490(11) Uani 1 1 d D . . H33A H 0.8323 0.8364 0.4040 0.059 Uiso 1 1 calc R A 1 H33B H 0.8589 0.7558 0.3646 0.059 Uiso 1 1 calc R A 1 C34 C 0.9891(4) 0.8279(3) 0.3213(4) 0.0607(13) Uani 1 1 d D A . H34A H 1.0291 0.7881 0.2835 0.073 Uiso 1 1 calc R B 1 H34B H 0.9488 0.8600 0.2579 0.073 Uiso 1 1 calc R B 1 H1 H 0.214(3) 0.717(2) 0.663(3) 0.021(9) Uiso 1 1 d . . . H2 H 0.155(3) 0.6069(19) 0.832(3) 0.010(8) Uiso 1 1 d . . . H15 H 0.749(3) 0.6483(19) 0.865(3) 0.021(9) Uiso 1 1 d . . . H16 H 0.617(3) 0.675(2) 0.623(3) 0.020(8) 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 0.0194(3) 0.0359(4) 0.0294(3) -0.0012(3) 0.0041(3) 0.0001(3) K2 0.0193(4) 0.0375(4) 0.0439(5) 0.0053(4) 0.0051(3) -0.0025(3) Si1 0.0252(5) 0.0318(5) 0.0375(6) -0.0058(4) 0.0105(4) -0.0030(4) Si2 0.0236(5) 0.0522(7) 0.0298(5) 0.0068(5) 0.0039(4) -0.0008(5) Si3 0.0253(5) 0.0289(5) 0.0345(5) 0.0031(4) 0.0022(4) -0.0003(4) Si4 0.0265(5) 0.0289(5) 0.0339(5) 0.0067(4) 0.0090(4) -0.0016(4) O1 0.0321(15) 0.0367(16) 0.072(2) 0.0037(14) -0.0063(14) -0.0048(13) O2 0.0333(15) 0.0505(18) 0.0363(15) -0.0126(12) 0.0113(12) -0.0148(13) O3 0.0324(15) 0.059(2) 0.0344(15) 0.0058(13) 0.0016(11) 0.0011(13) O4X 0.032(2) 0.061(4) 0.054(2) 0.012(3) 0.000(2) -0.002(2) C35X 0.033(3) 0.056(4) 0.056(2) 0.004(3) 0.008(2) -0.001(3) C36X 0.034(2) 0.055(3) 0.054(2) 0.006(3) 0.002(2) 0.001(2) O4Y 0.032(2) 0.059(4) 0.053(3) 0.018(3) 0.0045(19) -0.001(3) C35Y 0.033(3) 0.056(4) 0.055(3) -0.004(3) 0.009(2) 0.003(3) C36Y 0.032(2) 0.059(3) 0.057(2) 0.008(3) 0.002(2) 0.002(2) C1 0.0243(17) 0.0312(18) 0.0291(16) -0.0008(16) 0.0065(13) -0.0002(15) C2 0.0174(16) 0.029(2) 0.041(2) 0.0050(16) 0.0061(14) 0.0015(14) C3 0.0224(17) 0.035(2) 0.0298(18) 0.0029(15) 0.0047(14) 0.0025(14) C4 0.0254(19) 0.044(2) 0.0341(19) -0.0045(17) 0.0051(15) -0.0041(16) C5 0.035(2) 0.042(2) 0.041(2) -0.0045(18) 0.0106(17) -0.0029(18) C6 0.039(2) 0.036(2) 0.063(3) -0.014(2) 0.012(2) -0.0072(18) C7 0.045(3) 0.040(3) 0.109(5) 0.010(3) -0.007(3) -0.010(2) C8 0.039(3) 0.038(3) 0.157(6) 0.012(3) -0.010(3) -0.002(2) C9 0.036(2) 0.089(4) 0.033(2) 0.004(2) 0.0033(17) -0.008(2) C10 0.060(3) 0.058(3) 0.047(3) 0.023(2) 0.006(2) -0.005(2) C11 0.026(2) 0.080(3) 0.0318(19) -0.001(2) 0.0073(15) -0.006(2) C12 0.041(2) 0.036(2) 0.044(2) 0.0017(18) 0.0179(18) -0.0025(18) C13 0.043(3) 0.083(4) 0.055(3) -0.031(3) -0.001(2) -0.005(3) C14 0.061(3) 0.034(2) 0.071(3) -0.002(2) 0.041(3) -0.006(2) C15 0.0233(18) 0.0305(18) 0.0294(18) 0.0031(15) 0.0041(15) -0.0015(15) C16 0.0176(16) 0.0308(18) 0.0262(17) 0.0033(14) 0.0052(13) -0.0047(13) C17 0.0249(18) 0.0293(18) 0.0282(17) -0.0018(14) 0.0079(14) -0.0023(14) C18 0.029(2) 0.041(2) 0.036(2) -0.0035(17) 0.0073(16) -0.0088(16) C19 0.047(2) 0.0281(19) 0.037(2) -0.0016(16) 0.0019(17) 0.0001(18) C20 0.062(3) 0.046(3) 0.047(3) -0.009(2) 0.002(2) -0.021(2) C21 0.048(3) 0.047(3) 0.045(2) -0.006(2) 0.0018(19) -0.006(2) C22 0.041(2) 0.050(3) 0.047(2) -0.015(2) 0.0116(19) -0.002(2) C23 0.044(3) 0.039(2) 0.072(3) 0.008(2) 0.012(2) -0.010(2) C24 0.055(3) 0.042(2) 0.042(2) -0.0022(19) -0.001(2) 0.008(2) C25 0.039(2) 0.044(2) 0.048(2) 0.005(2) -0.0003(19) 0.0084(19) C26 0.035(2) 0.049(3) 0.060(3) 0.022(2) 0.014(2) 0.0087(19) C27 0.040(2) 0.050(3) 0.036(2) 0.0054(18) 0.0034(17) -0.006(2) C28 0.047(3) 0.035(2) 0.051(2) 0.0115(19) 0.0105(19) -0.0083(19) C29 0.036(2) 0.049(2) 0.044(2) -0.0015(19) 0.0091(18) 0.0011(19) C30 0.049(3) 0.054(3) 0.040(2) 0.000(2) -0.002(2) 0.005(2) C31 0.054(3) 0.079(4) 0.052(3) 0.019(3) 0.008(2) -0.001(3) C32 0.054(3) 0.070(3) 0.061(3) 0.020(3) -0.001(2) -0.012(3) C33 0.037(2) 0.039(2) 0.070(3) -0.002(2) 0.003(2) -0.0054(19) C34 0.050(3) 0.081(4) 0.052(3) -0.020(3) 0.012(2) -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 O2 2.664(3) . ? K1 O3 2.731(3) . ? K1 C16 3.015(3) . ? K1 C2 3.059(4) . ? K1 C15 3.103(4) . ? K1 C1 3.119(4) . ? K1 C3 3.188(4) . ? K1 C17 3.348(4) . ? K2 O1 2.659(3) 1_655 ? K2 O4X 2.673(8) . ? K2 O4Y 2.780(8) . ? K2 C2 3.007(4) 1_655 ? K2 C16 3.048(3) . ? K2 C15 3.074(3) . ? K2 C1 3.085(4) 1_655 ? K2 C17 3.218(4) . ? K2 C3 3.333(4) 1_655 ? Si1 C1 1.816(4) . ? Si1 C13 1.869(5) . ? Si1 C14 1.875(5) . ? Si1 C12 1.880(4) . ? Si2 C3 1.842(4) . ? Si2 C9 1.867(5) . ? Si2 C11 1.881(4) . ? Si2 C10 1.882(5) . ? Si3 C15 1.804(4) . ? Si3 C23 1.869(4) . ? Si3 C24 1.877(4) . ? Si3 C25 1.884(4) . ? Si4 C17 1.839(4) . ? Si4 C28 1.872(4) . ? Si4 C27 1.876(4) . ? Si4 C26 1.887(4) . ? O1 C5 1.421(5) . ? O1 C8 1.421(6) . ? O1 K2 2.659(3) 1_455 ? O2 C22 1.433(5) . ? O2 C19 1.439(5) . ? O3 C29 1.418(5) . ? O3 C32 1.430(6) . ? O4X C33 1.404(7) . ? O4X C36X 1.541(8) . ? C35X C36X 1.448(8) . ? C35X C34 1.485(8) . ? C35X H35A 0.9900 . ? C35X H35B 0.9900 . ? C36X H36A 0.9900 . ? C36X H36B 0.9900 . ? O4Y C36Y 1.500(8) . ? O4Y C33 1.495(8) . ? C35Y C36Y 1.363(8) . ? C35Y C34 1.545(8) . ? C35Y H35C 0.9900 . ? C35Y H35D 0.9900 . ? C36Y H36C 0.9900 . ? C36Y H36D 0.9900 . ? C1 C2 1.411(5) . ? C1 K2 3.085(4) 1_455 ? C1 H1 1.12(4) . ? C2 C3 1.395(5) . ? C2 K2 3.007(4) 1_455 ? C2 H2 0.88(3) . ? C3 C4 1.516(5) . ? C3 K2 3.333(4) 1_455 ? C4 C5 1.509(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.543(6) . ? C5 H5 1.0000 . ? C6 C7 1.516(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.504(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.411(5) . ? C15 H15 1.02(3) . ? C16 C17 1.397(5) . ? C16 H16 1.02(3) . ? C17 C18 1.510(5) . ? C18 C19 1.526(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.548(6) . ? C19 H19 1.0000 . ? C20 C21 1.514(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.501(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.538(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.513(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.472(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.497(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? 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 O2 K1 O3 80.90(9) . . ? O2 K1 C16 80.29(9) . . ? O3 K1 C16 111.38(9) . . ? O2 K1 C2 121.27(10) . . ? O3 K1 C2 108.26(9) . . ? C16 K1 C2 137.45(10) . . ? O2 K1 C15 85.16(9) . . ? O3 K1 C15 86.59(9) . . ? C16 K1 C15 26.62(9) . . ? C2 K1 C15 150.80(10) . . ? O2 K1 C1 127.11(10) . . ? O3 K1 C1 132.29(9) . . ? C16 K1 C1 111.07(9) . . ? C2 K1 C1 26.39(9) . . ? C15 K1 C1 128.17(10) . . ? O2 K1 C3 97.29(9) . . ? O3 K1 C3 97.06(9) . . ? C16 K1 C3 150.50(10) . . ? C2 K1 C3 25.69(10) . . ? C15 K1 C3 175.87(10) . . ? C1 K1 C3 47.75(9) . . ? O2 K1 C17 60.18(8) . . ? O3 K1 C17 117.43(9) . . ? C16 K1 C17 24.67(9) . . ? C2 K1 C17 133.19(10) . . ? C15 K1 C17 46.57(9) . . ? C1 K1 C17 110.26(9) . . ? C3 K1 C17 132.16(9) . . ? O1 K2 O4X 82.39(17) 1_655 . ? O1 K2 O4Y 74.28(18) 1_655 . ? O4X K2 O4Y 12.5(2) . . ? O1 K2 C2 80.79(10) 1_655 1_655 ? O4X K2 C2 107.86(18) . 1_655 ? O4Y K2 C2 114.87(16) . 1_655 ? O1 K2 C16 122.50(10) 1_655 . ? O4X K2 C16 110.31(17) . . ? O4Y K2 C16 106.34(16) . . ? C2 K2 C16 137.25(10) 1_655 . ? O1 K2 C15 128.45(10) 1_655 . ? O4X K2 C15 133.52(16) . . ? O4Y K2 C15 132.07(16) . . ? C2 K2 C15 110.62(10) 1_655 . ? C16 K2 C15 26.64(9) . . ? O1 K2 C1 85.47(10) 1_655 1_655 ? O4X K2 C1 82.52(19) . 1_655 ? O4Y K2 C1 91.36(17) . 1_655 ? C2 K2 C1 26.75(9) 1_655 1_655 ? C16 K2 C1 149.75(10) . 1_655 ? C15 K2 C1 127.37(10) . 1_655 ? O1 K2 C17 98.55(9) 1_655 . ? O4X K2 C17 100.51(18) . . ? O4Y K2 C17 92.21(16) . . ? C2 K2 C17 151.22(10) 1_655 . ? C16 K2 C17 25.59(9) . . ? C15 K2 C17 47.95(10) . . ? C1 K2 C17 175.22(10) 1_655 . ? O1 K2 C3 60.63(9) 1_655 1_655 ? O4X K2 C3 115.41(16) . 1_655 ? O4Y K2 C3 117.09(16) . 1_655 ? C2 K2 C3 24.73(9) 1_655 1_655 ? C16 K2 C3 133.94(9) . 1_655 ? C15 K2 C3 110.47(10) . 1_655 ? C1 K2 C3 46.68(9) 1_655 1_655 ? C17 K2 C3 133.50(9) . 1_655 ? C1 Si1 C13 114.4(2) . . ? C1 Si1 C14 110.9(2) . . ? C13 Si1 C14 106.7(3) . . ? C1 Si1 C12 109.89(18) . . ? C13 Si1 C12 105.7(2) . . ? C14 Si1 C12 109.0(2) . . ? C3 Si2 C9 110.68(19) . . ? C3 Si2 C11 114.00(18) . . ? C9 Si2 C11 107.6(2) . . ? C3 Si2 C10 111.4(2) . . ? C9 Si2 C10 108.9(2) . . ? C11 Si2 C10 103.9(2) . . ? C15 Si3 C23 114.5(2) . . ? C15 Si3 C24 111.10(19) . . ? C23 Si3 C24 105.9(2) . . ? C15 Si3 C25 109.37(19) . . ? C23 Si3 C25 106.0(2) . . ? C24 Si3 C25 109.8(2) . . ? C17 Si4 C28 110.50(19) . . ? C17 Si4 C27 112.46(18) . . ? C28 Si4 C27 109.0(2) . . ? C17 Si4 C26 113.19(17) . . ? C28 Si4 C26 106.6(2) . . ? C27 Si4 C26 104.7(2) . . ? C5 O1 C8 106.0(4) . . ? C5 O1 K2 127.6(2) . 1_455 ? C8 O1 K2 125.5(3) . 1_455 ? C22 O2 C19 108.0(3) . . ? C22 O2 K1 123.9(2) . . ? C19 O2 K1 127.9(2) . . ? C29 O3 C32 104.2(3) . . ? C29 O3 K1 114.0(2) . . ? C32 O3 K1 140.0(3) . . ? C33 O4X C36X 104.9(6) . . ? C33 O4X K2 134.7(5) . . ? C36X O4X K2 115.7(5) . . ? C36X C35X C34 109.4(6) . . ? C36X C35X H35A 109.8 . . ? C34 C35X H35A 109.8 . . ? C36X C35X H35B 109.8 . . ? C34 C35X H35B 109.8 . . ? H35A C35X H35B 108.2 . . ? C35X C36X O4X 102.5(7) . . ? C35X C36X H36A 111.3 . . ? O4X C36X H36A 111.3 . . ? C35X C36X H36B 111.3 . . ? O4X C36X H36B 111.3 . . ? H36A C36X H36B 109.2 . . ? C36Y O4Y C33 97.5(6) . . ? C36Y O4Y K2 100.4(5) . . ? C33 O4Y K2 122.2(5) . . ? C36Y C35Y C34 104.1(7) . . ? C36Y C35Y H35C 110.9 . . ? C34 C35Y H35C 110.9 . . ? C36Y C35Y H35D 110.9 . . ? C34 C35Y H35D 110.9 . . ? H35C C35Y H35D 108.9 . . ? C35Y C36Y O4Y 114.0(8) . . ? C35Y C36Y H36C 108.8 . . ? O4Y C36Y H36C 108.8 . . ? C35Y C36Y H36D 108.7 . . ? O4Y C36Y H36D 108.8 . . ? H36C C36Y H36D 107.6 . . ? C2 C1 Si1 125.2(3) . . ? C2 C1 K2 73.52(19) . 1_455 ? Si1 C1 K2 110.40(15) . 1_455 ? C2 C1 K1 74.4(2) . . ? Si1 C1 K1 110.64(15) . . ? K2 C1 K1 137.56(12) 1_455 . ? C2 C1 H1 122.5(17) . . ? Si1 C1 H1 112.3(17) . . ? K2 C1 H1 87.6(18) 1_455 . ? K1 C1 H1 86.7(18) . . ? C3 C2 C1 131.0(3) . . ? C3 C2 K2 90.9(2) . 1_455 ? C1 C2 K2 79.7(2) . 1_455 ? C3 C2 K1 82.3(2) . . ? C1 C2 K1 79.2(2) . . ? K2 C2 K1 144.91(13) 1_455 . ? C3 C2 H2 116(2) . . ? C1 C2 H2 113(2) . . ? K2 C2 H2 110(2) 1_455 . ? K1 C2 H2 104(2) . . ? C2 C3 C4 120.6(3) . . ? C2 C3 Si2 119.8(3) . . ? C4 C3 Si2 119.4(3) . . ? C2 C3 K1 72.01(19) . . ? C4 C3 K1 78.8(2) . . ? Si2 C3 K1 117.40(15) . . ? C2 C3 K2 64.42(19) . 1_455 ? C4 C3 K2 95.6(2) . 1_455 ? Si2 C3 K2 112.78(15) . 1_455 ? K1 C3 K2 124.97(11) . 1_455 ? C5 C4 C3 119.0(3) . . ? C5 C4 H4A 107.6 . . ? C3 C4 H4A 107.6 . . ? C5 C4 H4B 107.6 . . ? C3 C4 H4B 107.6 . . ? H4A C4 H4B 107.0 . . ? O1 C5 C4 110.8(3) . . ? O1 C5 C6 104.6(3) . . ? C4 C5 C6 113.3(3) . . ? O1 C5 H5 109.3 . . ? C4 C5 H5 109.3 . . ? C6 C5 H5 109.3 . . ? C7 C6 C5 106.1(4) . . ? C7 C6 H6A 110.5 . . ? C5 C6 H6A 110.5 . . ? C7 C6 H6B 110.5 . . ? C5 C6 H6B 110.5 . . ? H6A C6 H6B 108.7 . . ? C8 C7 C6 102.1(4) . . ? C8 C7 H7A 111.4 . . ? C6 C7 H7A 111.4 . . ? C8 C7 H7B 111.4 . . ? C6 C7 H7B 111.4 . . ? H7A C7 H7B 109.2 . . ? O1 C8 C7 106.7(4) . . ? O1 C8 H8A 110.4 . . ? C7 C8 H8A 110.4 . . ? O1 C8 H8B 110.4 . . ? C7 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 Si3 126.3(3) . . ? C16 C15 K2 75.63(19) . . ? Si3 C15 K2 111.64(15) . . ? C16 C15 K1 73.20(19) . . ? Si3 C15 K1 107.98(14) . . ? K2 C15 K1 139.12(13) . . ? C16 C15 H15 121(2) . . ? Si3 C15 H15 113(2) . . ? K2 C15 H15 83(2) . . ? K1 C15 H15 91(2) . . ? C17 C16 C15 131.4(3) . . ? C17 C16 K1 91.1(2) . . ? C15 C16 K1 80.18(19) . . ? C17 C16 K2 84.0(2) . . ? C15 C16 K2 77.72(19) . . ? K1 C16 K2 145.41(12) . . ? C17 C16 H16 115(2) . . ? C15 C16 H16 113(2) . . ? K1 C16 H16 104(2) . . ? K2 C16 H16 109(2) . . ? C16 C17 C18 120.8(3) . . ? C16 C17 Si4 120.2(3) . . ? C18 C17 Si4 118.9(3) . . ? C16 C17 K2 70.4(2) . . ? C18 C17 K2 79.4(2) . . ? Si4 C17 K2 118.75(15) . . ? C16 C17 K1 64.21(19) . . ? C18 C17 K1 96.4(2) . . ? Si4 C17 K1 112.20(15) . . ? K2 C17 K1 123.68(11) . . ? C17 C18 C19 117.8(3) . . ? C17 C18 H18A 107.9 . . ? C19 C18 H18A 107.9 . . ? C17 C18 H18B 107.9 . . ? C19 C18 H18B 107.9 . . ? H18A C18 H18B 107.2 . . ? O2 C19 C18 109.8(3) . . ? O2 C19 C20 105.2(3) . . ? C18 C19 C20 114.4(4) . . ? O2 C19 H19 109.1 . . ? C18 C19 H19 109.1 . . ? C20 C19 H19 109.1 . . ? C21 C20 C19 105.1(4) . . ? C21 C20 H20A 110.7 . . ? C19 C20 H20A 110.7 . . ? C21 C20 H20B 110.7 . . ? C19 C20 H20B 110.7 . . ? H20A C20 H20B 108.8 . . ? C22 C21 C20 103.2(4) . . ? C22 C21 H21A 111.1 . . ? C20 C21 H21A 111.1 . . ? C22 C21 H21B 111.1 . . ? C20 C21 H21B 111.1 . . ? H21A C21 H21B 109.1 . . ? O2 C22 C21 104.7(3) . . ? O2 C22 H22A 110.8 . . ? C21 C22 H22A 110.8 . . ? O2 C22 H22B 110.8 . . ? C21 C22 H22B 110.8 . . ? H22A C22 H22B 108.9 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C24 H24A 109.5 . . ? Si3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si4 C27 H27A 109.5 . . ? Si4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C30 104.3(3) . . ? O3 C29 H29A 110.9 . . ? C30 C29 H29A 110.9 . . ? O3 C29 H29B 110.9 . . ? C30 C29 H29B 110.9 . . ? H29A C29 H29B 108.9 . . ? C31 C30 C29 101.8(4) . . ? C31 C30 H30A 111.4 . . ? C29 C30 H30A 111.4 . . ? C31 C30 H30B 111.4 . . ? C29 C30 H30B 111.4 . . ? H30A C30 H30B 109.3 . . ? C32 C31 C30 105.7(4) . . ? C32 C31 H31A 110.6 . . ? C30 C31 H31A 110.6 . . ? C32 C31 H31B 110.6 . . ? C30 C31 H31B 110.6 . . ? H31A C31 H31B 108.7 . . ? O3 C32 C31 107.6(4) . . ? O3 C32 H32A 110.2 . . ? C31 C32 H32A 110.2 . . ? O3 C32 H32B 110.2 . . ? C31 C32 H32B 110.2 . . ? H32A C32 H32B 108.5 . . ? O4X C33 C34 104.6(5) . . ? O4X C33 O4Y 23.7(4) . . ? C34 C33 O4Y 107.6(4) . . ? O4X C33 H33A 110.8 . . ? C34 C33 H33A 110.8 . . ? O4Y C33 H33A 88.3 . . ? O4X C33 H33B 110.8 . . ? C34 C33 H33B 110.8 . . ? O4Y C33 H33B 127.8 . . ? H33A C33 H33B 108.9 . . ? C35X C34 C33 103.5(5) . . ? C35X C34 C35Y 29.5(5) . . ? C33 C34 C35Y 104.3(5) . . ? C35X C34 H34A 111.1 . . ? C33 C34 H34A 111.1 . . ? C35Y C34 H34A 83.8 . . ? C35X C34 H34B 111.1 . . ? C33 C34 H34B 111.1 . . ? C35Y C34 H34B 133.8 . . ? H34A C34 H34B 109.0 . . ? 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 O3 K1 O2 C22 -47.2(3) . . . . ? C16 K1 O2 C22 -160.9(3) . . . . ? C2 K1 O2 C22 58.7(3) . . . . ? C15 K1 O2 C22 -134.5(3) . . . . ? C1 K1 O2 C22 90.0(3) . . . . ? C3 K1 O2 C22 48.8(3) . . . . ? C17 K1 O2 C22 -176.2(3) . . . . ? O3 K1 O2 C19 137.9(3) . . . . ? C16 K1 O2 C19 24.2(3) . . . . ? C2 K1 O2 C19 -116.2(3) . . . . ? C15 K1 O2 C19 50.6(3) . . . . ? C1 K1 O2 C19 -84.9(3) . . . . ? C3 K1 O2 C19 -126.0(3) . . . . ? C17 K1 O2 C19 8.9(3) . . . . ? O2 K1 O3 C29 -50.5(3) . . . . ? C16 K1 O3 C29 25.2(3) . . . . ? C2 K1 O3 C29 -170.6(3) . . . . ? C15 K1 O3 C29 35.1(3) . . . . ? C1 K1 O3 C29 176.6(2) . . . . ? C3 K1 O3 C29 -146.8(3) . . . . ? C17 K1 O3 C29 -1.1(3) . . . . ? O2 K1 O3 C32 148.1(5) . . . . ? C16 K1 O3 C32 -136.1(5) . . . . ? C2 K1 O3 C32 28.1(5) . . . . ? C15 K1 O3 C32 -126.2(5) . . . . ? C1 K1 O3 C32 15.3(5) . . . . ? C3 K1 O3 C32 51.9(5) . . . . ? C17 K1 O3 C32 -162.4(5) . . . . ? O1 K2 O4X C33 -137.8(8) 1_655 . . . ? O4Y K2 O4X C33 -89.3(14) . . . . ? C2 K2 O4X C33 144.5(7) 1_655 . . . ? C16 K2 O4X C33 -15.9(8) . . . . ? C15 K2 O4X C33 -0.2(9) . . . . ? C1 K2 O4X C33 135.8(8) 1_655 . . . ? C17 K2 O4X C33 -40.5(8) . . . . ? C3 K2 O4X C33 169.9(7) 1_655 . . . ? O1 K2 O4X C36X 13.5(7) 1_655 . . . ? O4Y K2 O4X C36X 62.0(11) . . . . ? C2 K2 O4X C36X -64.2(7) 1_655 . . . ? C16 K2 O4X C36X 135.4(6) . . . . ? C15 K2 O4X C36X 151.1(6) . . . . ? C1 K2 O4X C36X -72.9(7) 1_655 . . . ? C17 K2 O4X C36X 110.9(7) . . . . ? C3 K2 O4X C36X -38.8(7) 1_655 . . . ? C34 C35X C36X O4X 11.1(10) . . . . ? C33 O4X C36X C35X -31.7(9) . . . . ? K2 O4X C36X C35X 169.0(6) . . . . ? O1 K2 O4Y C36Y 75.8(6) 1_655 . . . ? O4X K2 O4Y C36Y -53.8(11) . . . . ? C2 K2 O4Y C36Y 4.1(7) 1_655 . . . ? C16 K2 O4Y C36Y -164.2(6) . . . . ? C15 K2 O4Y C36Y -156.2(5) . . . . ? C1 K2 O4Y C36Y -9.1(6) 1_655 . . . ? C17 K2 O4Y C36Y 174.1(6) . . . . ? C3 K2 O4Y C36Y 31.6(7) 1_655 . . . ? O1 K2 O4Y C33 -178.4(5) 1_655 . . . ? O4X K2 O4Y C33 52.1(11) . . . . ? C2 K2 O4Y C33 109.9(5) 1_655 . . . ? C16 K2 O4Y C33 -58.4(5) . . . . ? C15 K2 O4Y C33 -50.3(6) . . . . ? C1 K2 O4Y C33 96.7(5) 1_655 . . . ? C17 K2 O4Y C33 -80.1(5) . . . . ? C3 K2 O4Y C33 137.4(4) 1_655 . . . ? C34 C35Y C36Y O4Y -21.5(12) . . . . ? C33 O4Y C36Y C35Y 34.6(11) . . . . ? K2 O4Y C36Y C35Y 159.3(9) . . . . ? C13 Si1 C1 C2 103.8(4) . . . . ? C14 Si1 C1 C2 -17.0(4) . . . . ? C12 Si1 C1 C2 -137.6(3) . . . . ? C13 Si1 C1 K2 20.0(3) . . . 1_455 ? C14 Si1 C1 K2 -100.8(2) . . . 1_455 ? C12 Si1 C1 K2 138.63(17) . . . 1_455 ? C13 Si1 C1 K1 -171.1(2) . . . . ? C14 Si1 C1 K1 68.1(2) . . . . ? C12 Si1 C1 K1 -52.4(2) . . . . ? O2 K1 C1 C2 -86.5(2) . . . . ? O3 K1 C1 C2 28.3(3) . . . . ? C16 K1 C1 C2 179.7(2) . . . . ? C15 K1 C1 C2 156.1(2) . . . . ? C3 K1 C1 C2 -24.7(2) . . . . ? C17 K1 C1 C2 -153.9(2) . . . . ? O2 K1 C1 Si1 151.12(14) . . . . ? O3 K1 C1 Si1 -94.05(18) . . . . ? C16 K1 C1 Si1 57.41(19) . . . . ? C2 K1 C1 Si1 -122.3(3) . . . . ? C15 K1 C1 Si1 33.7(2) . . . . ? C3 K1 C1 Si1 -147.1(2) . . . . ? C17 K1 C1 Si1 83.79(18) . . . . ? O2 K1 C1 K2 -44.3(2) . . . 1_455 ? O3 K1 C1 K2 70.5(2) . . . 1_455 ? C16 K1 C1 K2 -138.06(18) . . . 1_455 ? C2 K1 C1 K2 42.19(19) . . . 1_455 ? C15 K1 C1 K2 -161.74(16) . . . 1_455 ? C3 K1 C1 K2 17.47(15) . . . 1_455 ? C17 K1 C1 K2 -111.68(18) . . . 1_455 ? Si1 C1 C2 C3 174.2(3) . . . . ? K2 C1 C2 C3 -82.1(4) 1_455 . . . ? K1 C1 C2 C3 69.7(4) . . . . ? Si1 C1 C2 K2 -103.7(3) . . . 1_455 ? K1 C1 C2 K2 151.79(11) . . . 1_455 ? Si1 C1 C2 K1 104.6(3) . . . . ? K2 C1 C2 K1 -151.79(11) 1_455 . . . ? O2 K1 C2 C3 -23.1(2) . . . . ? O3 K1 C2 C3 67.2(2) . . . . ? C16 K1 C2 C3 -134.8(2) . . . . ? C15 K1 C2 C3 -175.3(2) . . . . ? C1 K1 C2 C3 -134.4(3) . . . . ? C17 K1 C2 C3 -99.9(2) . . . . ? O2 K1 C2 C1 111.4(2) . . . . ? O3 K1 C2 C1 -158.3(2) . . . . ? C16 K1 C2 C1 -0.3(3) . . . . ? C15 K1 C2 C1 -40.8(3) . . . . ? C3 K1 C2 C1 134.4(3) . . . . ? C17 K1 C2 C1 34.5(3) . . . . ? O2 K1 C2 K2 57.4(3) . . . 1_455 ? O3 K1 C2 K2 147.7(2) . . . 1_455 ? C16 K1 C2 K2 -54.3(3) . . . 1_455 ? C15 K1 C2 K2 -94.8(3) . . . 1_455 ? C1 K1 C2 K2 -54.0(2) . . . 1_455 ? C3 K1 C2 K2 80.4(3) . . . 1_455 ? C17 K1 C2 K2 -19.5(3) . . . 1_455 ? C1 C2 C3 C4 -3.9(6) . . . . ? K2 C2 C3 C4 -81.0(3) 1_455 . . . ? K1 C2 C3 C4 64.5(3) . . . . ? C1 C2 C3 Si2 179.8(3) . . . . ? K2 C2 C3 Si2 102.7(2) 1_455 . . . ? K1 C2 C3 Si2 -111.8(2) . . . . ? C1 C2 C3 K1 -68.4(4) . . . . ? K2 C2 C3 K1 -145.46(12) 1_455 . . . ? C1 C2 C3 K2 77.1(4) . . . 1_455 ? K1 C2 C3 K2 145.46(12) . . . 1_455 ? C9 Si2 C3 C2 144.7(3) . . . . ? C11 Si2 C3 C2 -93.8(3) . . . . ? C10 Si2 C3 C2 23.4(4) . . . . ? C9 Si2 C3 C4 -31.7(4) . . . . ? C11 Si2 C3 C4 89.8(3) . . . . ? C10 Si2 C3 C4 -152.9(3) . . . . ? C9 Si2 C3 K1 60.7(3) . . . . ? C11 Si2 C3 K1 -177.88(19) . . . . ? C10 Si2 C3 K1 -60.6(2) . . . . ? C9 Si2 C3 K2 -142.7(2) . . . 1_455 ? C11 Si2 C3 K2 -21.2(2) . . . 1_455 ? C10 Si2 C3 K2 96.0(2) . . . 1_455 ? O2 K1 C3 C2 160.3(2) . . . . ? O3 K1 C3 C2 -118.1(2) . . . . ? C16 K1 C3 C2 77.1(3) . . . . ? C15 K1 C3 C2 34.1(15) . . . . ? C1 K1 C3 C2 25.4(2) . . . . ? C17 K1 C3 C2 104.3(2) . . . . ? O2 K1 C3 C4 32.6(2) . . . . ? O3 K1 C3 C4 114.3(2) . . . . ? C16 K1 C3 C4 -50.5(3) . . . . ? C2 K1 C3 C4 -127.6(3) . . . . ? C15 K1 C3 C4 -93.6(14) . . . . ? C1 K1 C3 C4 -102.2(2) . . . . ? C17 K1 C3 C4 -23.3(2) . . . . ? O2 K1 C3 Si2 -84.85(19) . . . . ? O3 K1 C3 Si2 -3.18(19) . . . . ? C16 K1 C3 Si2 -168.00(16) . . . . ? C2 K1 C3 Si2 114.9(3) . . . . ? C15 K1 C3 Si2 149.0(13) . . . . ? C1 K1 C3 Si2 140.3(2) . . . . ? C17 K1 C3 Si2 -140.77(15) . . . . ? O2 K1 C3 K2 121.64(14) . . . 1_455 ? O3 K1 C3 K2 -156.68(14) . . . 1_455 ? C16 K1 C3 K2 38.5(3) . . . 1_455 ? C2 K1 C3 K2 -38.62(18) . . . 1_455 ? C15 K1 C3 K2 -4.5(15) . . . 1_455 ? C1 K1 C3 K2 -13.23(12) . . . 1_455 ? C17 K1 C3 K2 65.73(18) . . . 1_455 ? C2 C3 C4 C5 113.2(4) . . . . ? Si2 C3 C4 C5 -70.5(4) . . . . ? K1 C3 C4 C5 174.2(3) . . . . ? K2 C3 C4 C5 49.6(3) 1_455 . . . ? C8 O1 C5 C4 -155.3(4) . . . . ? K2 O1 C5 C4 35.4(4) 1_455 . . . ? C8 O1 C5 C6 -32.8(5) . . . . ? K2 O1 C5 C6 157.9(3) 1_455 . . . ? C3 C4 C5 O1 -63.1(4) . . . . ? C3 C4 C5 C6 179.7(4) . . . . ? O1 C5 C6 C7 13.8(5) . . . . ? C4 C5 C6 C7 134.6(4) . . . . ? C5 C6 C7 C8 9.1(6) . . . . ? C5 O1 C8 C7 40.3(6) . . . . ? K2 O1 C8 C7 -150.2(4) 1_455 . . . ? C6 C7 C8 O1 -29.5(7) . . . . ? C23 Si3 C15 C16 -97.3(3) . . . . ? C24 Si3 C15 C16 22.6(4) . . . . ? C25 Si3 C15 C16 144.0(3) . . . . ? C23 Si3 C15 K2 175.03(19) . . . . ? C24 Si3 C15 K2 -65.1(2) . . . . ? C25 Si3 C15 K2 56.3(2) . . . . ? C23 Si3 C15 K1 -15.2(2) . . . . ? C24 Si3 C15 K1 104.6(2) . . . . ? C25 Si3 C15 K1 -134.03(18) . . . . ? O1 K2 C15 C16 87.0(2) 1_655 . . . ? O4X K2 C15 C16 -34.4(4) . . . . ? O4Y K2 C15 C16 -17.5(3) . . . . ? C2 K2 C15 C16 -178.4(2) 1_655 . . . ? C1 K2 C15 C16 -154.36(19) 1_655 . . . ? C17 K2 C15 C16 24.41(19) . . . . ? C3 K2 C15 C16 155.2(2) 1_655 . . . ? O1 K2 C15 Si3 -149.29(14) 1_655 . . . ? O4X K2 C15 Si3 89.3(3) . . . . ? O4Y K2 C15 Si3 106.2(3) . . . . ? C2 K2 C15 Si3 -54.68(19) 1_655 . . . ? C16 K2 C15 Si3 123.7(3) . . . . ? C1 K2 C15 Si3 -30.6(2) 1_655 . . . ? C17 K2 C15 Si3 148.1(2) . . . . ? C3 K2 C15 Si3 -81.12(18) 1_655 . . . ? O1 K2 C15 K1 45.7(2) 1_655 . . . ? O4X K2 C15 K1 -75.6(3) . . . . ? O4Y K2 C15 K1 -58.8(3) . . . . ? C2 K2 C15 K1 140.35(18) 1_655 . . . ? C16 K2 C15 K1 -41.25(19) . . . . ? C1 K2 C15 K1 164.40(15) 1_655 . . . ? C17 K2 C15 K1 -16.84(15) . . . . ? C3 K2 C15 K1 113.91(19) 1_655 . . . ? O2 K1 C15 C16 -77.9(2) . . . . ? O3 K1 C15 C16 -159.1(2) . . . . ? C2 K1 C15 C16 78.5(3) . . . . ? C1 K1 C15 C16 56.8(2) . . . . ? C3 K1 C15 C16 48.6(14) . . . . ? C17 K1 C15 C16 -25.31(19) . . . . ? O2 K1 C15 Si3 158.59(16) . . . . ? O3 K1 C15 Si3 77.45(16) . . . . ? C16 K1 C15 Si3 -123.5(3) . . . . ? C2 K1 C15 Si3 -45.0(3) . . . . ? C1 K1 C15 Si3 -66.7(2) . . . . ? C3 K1 C15 Si3 -74.9(14) . . . . ? C17 K1 C15 Si3 -148.8(2) . . . . ? O2 K1 C15 K2 -36.09(19) . . . . ? O3 K1 C15 K2 -117.2(2) . . . . ? C16 K1 C15 K2 41.8(2) . . . . ? C2 K1 C15 K2 120.3(2) . . . . ? C1 K1 C15 K2 98.6(2) . . . . ? C3 K1 C15 K2 90.5(14) . . . . ? C17 K1 C15 K2 16.54(15) . . . . ? Si3 C15 C16 C17 -177.0(3) . . . . ? K2 C15 C16 C17 -70.5(4) . . . . ? K1 C15 C16 C17 82.7(4) . . . . ? Si3 C15 C16 K1 100.3(3) . . . . ? K2 C15 C16 K1 -153.21(10) . . . . ? Si3 C15 C16 K2 -106.5(3) . . . . ? K1 C15 C16 K2 153.21(10) . . . . ? O2 K1 C16 C17 -33.3(2) . . . . ? O3 K1 C16 C17 -109.4(2) . . . . ? C2 K1 C16 C17 93.0(2) . . . . ? C15 K1 C16 C17 -131.9(3) . . . . ? C1 K1 C16 C17 92.9(2) . . . . ? C3 K1 C16 C17 54.4(3) . . . . ? O2 K1 C16 C15 98.7(2) . . . . ? O3 K1 C16 C15 22.5(2) . . . . ? C2 K1 C16 C15 -135.0(2) . . . . ? C1 K1 C16 C15 -135.2(2) . . . . ? C3 K1 C16 C15 -173.7(2) . . . . ? C17 K1 C16 C15 131.9(3) . . . . ? O2 K1 C16 K2 47.8(2) . . . . ? O3 K1 C16 K2 -28.4(3) . . . . ? C2 K1 C16 K2 174.10(18) . . . . ? C15 K1 C16 K2 -50.9(2) . . . . ? C1 K1 C16 K2 173.9(2) . . . . ? C3 K1 C16 K2 135.4(2) . . . . ? C17 K1 C16 K2 81.1(3) . . . . ? O1 K2 C16 C17 22.8(2) 1_655 . . . ? O4X K2 C16 C17 -71.2(3) . . . . ? O4Y K2 C16 C17 -58.7(3) . . . . ? C2 K2 C16 C17 136.9(2) 1_655 . . . ? C15 K2 C16 C17 134.7(3) . . . . ? C1 K2 C16 C17 177.8(2) 1_655 . . . ? C3 K2 C16 C17 101.6(2) 1_655 . . . ? O1 K2 C16 C15 -112.0(2) 1_655 . . . ? O4X K2 C16 C15 154.1(3) . . . . ? O4Y K2 C16 C15 166.5(3) . . . . ? C2 K2 C16 C15 2.2(3) 1_655 . . . ? C1 K2 C16 C15 43.1(3) 1_655 . . . ? C17 K2 C16 C15 -134.7(3) . . . . ? C3 K2 C16 C15 -33.1(3) 1_655 . . . ? O1 K2 C16 K1 -60.5(3) 1_655 . . . ? O4X K2 C16 K1 -154.4(3) . . . . ? O4Y K2 C16 K1 -142.0(3) . . . . ? C2 K2 C16 K1 53.7(3) 1_655 . . . ? C15 K2 C16 K1 51.5(2) . . . . ? C1 K2 C16 K1 94.5(3) 1_655 . . . ? C17 K2 C16 K1 -83.3(3) . . . . ? C3 K2 C16 K1 18.3(3) 1_655 . . . ? C15 C16 C17 C18 3.9(6) . . . . ? K1 C16 C17 C18 81.7(3) . . . . ? K2 C16 C17 C18 -63.9(3) . . . . ? C15 C16 C17 Si4 -179.7(3) . . . . ? K1 C16 C17 Si4 -101.8(2) . . . . ? K2 C16 C17 Si4 112.5(2) . . . . ? C15 C16 C17 K2 67.8(4) . . . . ? K1 C16 C17 K2 145.67(11) . . . . ? C15 C16 C17 K1 -77.9(4) . . . . ? K2 C16 C17 K1 -145.67(11) . . . . ? C28 Si4 C17 C16 -142.5(3) . . . . ? C27 Si4 C17 C16 -20.5(4) . . . . ? C26 Si4 C17 C16 97.9(3) . . . . ? C28 Si4 C17 C18 34.0(3) . . . . ? C27 Si4 C17 C18 156.1(3) . . . . ? C26 Si4 C17 C18 -85.5(3) . . . . ? C28 Si4 C17 K2 -59.6(2) . . . . ? C27 Si4 C17 K2 62.4(2) . . . . ? C26 Si4 C17 K2 -179.1(2) . . . . ? C28 Si4 C17 K1 145.29(18) . . . . ? C27 Si4 C17 K1 -92.66(19) . . . . ? C26 Si4 C17 K1 25.8(2) . . . . ? O1 K2 C17 C16 -160.7(2) 1_655 . . . ? O4X K2 C17 C16 115.5(3) . . . . ? O4Y K2 C17 C16 124.8(3) . . . . ? C2 K2 C17 C16 -74.3(3) 1_655 . . . ? C15 K2 C17 C16 -25.41(19) . . . . ? C1 K2 C17 C16 -13.5(12) 1_655 . . . ? C3 K2 C17 C16 -103.5(2) 1_655 . . . ? O1 K2 C17 C18 -32.4(2) 1_655 . . . ? O4X K2 C17 C18 -116.2(3) . . . . ? O4Y K2 C17 C18 -106.9(3) . . . . ? C2 K2 C17 C18 54.0(3) 1_655 . . . ? C16 K2 C17 C18 128.3(3) . . . . ? C15 K2 C17 C18 102.9(2) . . . . ? C1 K2 C17 C18 114.8(11) 1_655 . . . ? C3 K2 C17 C18 24.8(3) 1_655 . . . ? O1 K2 C17 Si4 84.81(18) 1_655 . . . ? O4X K2 C17 Si4 1.0(2) . . . . ? O4Y K2 C17 Si4 10.4(2) . . . . ? C2 K2 C17 Si4 171.23(17) 1_655 . . . ? C16 K2 C17 Si4 -114.5(3) . . . . ? C15 K2 C17 Si4 -139.9(2) . . . . ? C1 K2 C17 Si4 -128.0(10) 1_655 . . . ? C3 K2 C17 Si4 142.07(15) 1_655 . . . ? O1 K2 C17 K1 -123.14(13) 1_655 . . . ? O4X K2 C17 K1 153.1(2) . . . . ? O4Y K2 C17 K1 162.4(2) . . . . ? C2 K2 C17 K1 -36.7(3) 1_655 . . . ? C16 K2 C17 K1 37.60(17) . . . . ? C15 K2 C17 K1 12.19(11) . . . . ? C1 K2 C17 K1 24.1(12) 1_655 . . . ? C3 K2 C17 K1 -65.88(18) 1_655 . . . ? O2 K1 C17 C16 141.4(2) . . . . ? O3 K1 C17 C16 81.6(2) . . . . ? C2 K1 C17 C16 -112.2(2) . . . . ? C15 K1 C17 C16 27.3(2) . . . . ? C1 K1 C17 C16 -96.6(2) . . . . ? C3 K1 C17 C16 -147.3(2) . . . . ? O2 K1 C17 C18 20.2(2) . . . . ? O3 K1 C17 C18 -39.6(2) . . . . ? C16 K1 C17 C18 -121.2(3) . . . . ? C2 K1 C17 C18 126.6(2) . . . . ? C15 K1 C17 C18 -93.9(2) . . . . ? C1 K1 C17 C18 142.2(2) . . . . ? C3 K1 C17 C18 91.5(2) . . . . ? O2 K1 C17 Si4 -104.59(18) . . . . ? O3 K1 C17 Si4 -164.40(14) . . . . ? C16 K1 C17 Si4 114.0(3) . . . . ? C2 K1 C17 Si4 1.8(2) . . . . ? C15 K1 C17 Si4 141.3(2) . . . . ? C1 K1 C17 Si4 17.40(19) . . . . ? C3 K1 C17 Si4 -33.3(2) . . . . ? O2 K1 C17 K2 101.76(15) . . . . ? O3 K1 C17 K2 41.95(16) . . . . ? C16 K1 C17 K2 -39.67(18) . . . . ? C2 K1 C17 K2 -151.82(12) . . . . ? C15 K1 C17 K2 -12.35(11) . . . . ? C1 K1 C17 K2 -136.25(12) . . . . ? C3 K1 C17 K2 173.00(11) . . . . ? C16 C17 C18 C19 -113.9(4) . . . . ? Si4 C17 C18 C19 69.6(4) . . . . ? K2 C17 C18 C19 -173.3(3) . . . . ? K1 C17 C18 C19 -50.2(4) . . . . ? C22 O2 C19 C18 146.8(3) . . . . ? K1 O2 C19 C18 -37.7(4) . . . . ? C22 O2 C19 C20 23.2(4) . . . . ? K1 O2 C19 C20 -161.3(3) . . . . ? C17 C18 C19 O2 64.2(4) . . . . ? C17 C18 C19 C20 -177.7(4) . . . . ? O2 C19 C20 C21 -0.5(5) . . . . ? C18 C19 C20 C21 -121.2(4) . . . . ? C19 C20 C21 C22 -20.7(5) . . . . ? C19 O2 C22 C21 -37.2(5) . . . . ? K1 O2 C22 C21 147.1(3) . . . . ? C20 C21 C22 O2 35.1(5) . . . . ? C32 O3 C29 C30 -41.3(5) . . . . ? K1 O3 C29 C30 150.9(3) . . . . ? O3 C29 C30 C31 32.6(5) . . . . ? C29 C30 C31 C32 -11.9(5) . . . . ? C29 O3 C32 C31 34.1(5) . . . . ? K1 O3 C32 C31 -163.5(3) . . . . ? C30 C31 C32 O3 -12.5(6) . . . . ? C36X O4X C33 C34 39.5(8) . . . . ? K2 O4X C33 C34 -167.1(6) . . . . ? C36X O4X C33 O4Y -61.1(12) . . . . ? K2 O4X C33 O4Y 92.3(16) . . . . ? C36Y O4Y C33 O4X 53.5(12) . . . . ? K2 O4Y C33 O4X -53.8(13) . . . . ? C36Y O4Y C33 C34 -32.8(8) . . . . ? K2 O4Y C33 C34 -140.2(4) . . . . ? C36X C35X C34 C33 11.6(9) . . . . ? C36X C35X C34 C35Y -83.6(12) . . . . ? O4X C33 C34 C35X -32.0(8) . . . . ? O4Y C33 C34 C35X -7.6(8) . . . . ? O4X C33 C34 C35Y -1.6(8) . . . . ? O4Y C33 C34 C35Y 22.9(8) . . . . ? C36Y C35Y C34 C35X 90.9(12) . . . . ? C36Y C35Y C34 C33 -1.3(10) . . . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.633 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.061 # Attachment '3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 678936' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H58 Mg O2 Si4' _chemical_formula_weight 563.41 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' Mg Mg 0.0486 0.0363 '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 orthorhombic _symmetry_space_group_name_H-M 'P c c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 12.0480(10) _cell_length_b 15.1550(10) _cell_length_c 19.4280(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3547.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2176 _cell_measurement_theta_min 2.6866 _cell_measurement_theta_max 28.6568 _exptl_crystal_description Needle _exptl_crystal_colour White _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.055 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.206 _exptl_absorpt_correction_T_min 0.8524 _exptl_absorpt_correction_T_max 0.9797 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11765 _diffrn_reflns_av_R_equivalents 0.1090 _diffrn_reflns_av_sigmaI/netI 0.1451 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.20 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3120 _reflns_number_gt 1655 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The structure was solved by direct methods. Data was processed to a resolution of 0.84 angstroms. All non hydrogen atoms were refined anisotropically Hydrogen atoms H1 and H2 were refined from the data and all other hydrogen atoms were included in calculated positions using the riding model. 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^)+(0.0360P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3120 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1348 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _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 Mg1 Mg 0.7500 0.2500 0.45240(7) 0.0197(4) Uani 1 2 d S . . O1 O 0.71838(18) 0.34424(16) 0.52649(10) 0.0212(6) Uani 1 1 d . . . Si1 Si 0.99062(8) 0.22890(7) 0.35472(5) 0.0234(3) Uani 1 1 d . . . Si2 Si 0.79788(8) 0.55615(7) 0.37476(5) 0.0215(3) Uani 1 1 d . . . C1 C 0.9087(3) 0.2961(2) 0.41318(18) 0.0211(10) Uani 1 1 d . . . C2 C 0.8701(3) 0.3818(3) 0.38860(18) 0.0184(9) Uani 1 1 d . . . C3 C 0.8442(3) 0.4573(2) 0.42163(16) 0.0178(9) Uani 1 1 d . . . C4 C 0.8547(3) 0.4602(2) 0.49959(16) 0.0215(9) Uani 1 1 d . . . H4A H 0.9150 0.4196 0.5136 0.026 Uiso 1 1 calc R . . H4B H 0.8770 0.5205 0.5133 0.026 Uiso 1 1 calc R . . C5 C 0.7515(3) 0.4358(2) 0.53856(15) 0.0203(9) Uani 1 1 d . . . H5 H 0.6897 0.4754 0.5235 0.024 Uiso 1 1 calc R . . C6 C 0.7600(3) 0.4392(2) 0.61630(15) 0.0223(9) Uani 1 1 d . . . H6A H 0.7493 0.5002 0.6334 0.027 Uiso 1 1 calc R . . H6B H 0.8330 0.4173 0.6321 0.027 Uiso 1 1 calc R . . C7 C 0.6666(3) 0.3790(3) 0.64087(17) 0.0297(10) Uani 1 1 d . . . H7A H 0.6926 0.3401 0.6785 0.036 Uiso 1 1 calc R . . H7B H 0.6027 0.4141 0.6576 0.036 Uiso 1 1 calc R . . C8 C 0.6346(3) 0.3251(3) 0.57812(17) 0.0308(11) Uani 1 1 d . . . H8A H 0.6338 0.2614 0.5893 0.037 Uiso 1 1 calc R . . H8B H 0.5600 0.3424 0.5614 0.037 Uiso 1 1 calc R . . C9 C 0.9030(3) 0.1793(3) 0.28540(17) 0.0347(11) Uani 1 1 d . . . H9A H 0.8516 0.1364 0.3057 0.052 Uiso 1 1 calc R . . H9B H 0.9507 0.1495 0.2518 0.052 Uiso 1 1 calc R . . H9C H 0.8606 0.2259 0.2623 0.052 Uiso 1 1 calc R . . C10 C 1.1000(3) 0.2957(3) 0.31003(19) 0.0385(11) Uani 1 1 d . . . H10A H 1.0653 0.3459 0.2867 0.058 Uiso 1 1 calc R . . H10B H 1.1382 0.2587 0.2761 0.058 Uiso 1 1 calc R . . H10C H 1.1537 0.3173 0.3439 0.058 Uiso 1 1 calc R . . C11 C 1.0582(3) 0.1380(3) 0.40355(19) 0.0346(11) Uani 1 1 d . . . H11A H 1.1138 0.1627 0.4349 0.052 Uiso 1 1 calc R . . H11B H 1.0944 0.0974 0.3713 0.052 Uiso 1 1 calc R . . H11C H 1.0021 0.1060 0.4301 0.052 Uiso 1 1 calc R . . C12 C 0.8167(3) 0.5415(2) 0.28037(17) 0.0332(11) Uani 1 1 d . . . H12A H 0.8937 0.5249 0.2708 0.050 Uiso 1 1 calc R . . H12B H 0.7994 0.5970 0.2568 0.050 Uiso 1 1 calc R . . H12C H 0.7668 0.4950 0.2639 0.050 Uiso 1 1 calc R . . C13 C 0.8789(3) 0.6549(3) 0.4016(2) 0.0397(11) Uani 1 1 d . . . H13A H 0.8707 0.6637 0.4513 0.060 Uiso 1 1 calc R . . H13B H 0.8512 0.7070 0.3771 0.060 Uiso 1 1 calc R . . H13C H 0.9574 0.6460 0.3905 0.060 Uiso 1 1 calc R . . C14 C 0.6480(3) 0.5813(3) 0.38999(18) 0.0345(11) Uani 1 1 d . . . H14A H 0.6031 0.5297 0.3779 0.052 Uiso 1 1 calc R . . H14B H 0.6258 0.6316 0.3615 0.052 Uiso 1 1 calc R . . H14C H 0.6367 0.5958 0.4386 0.052 Uiso 1 1 calc R . . H1 H 0.943(3) 0.303(2) 0.4557(17) 0.041 Uiso 1 1 d . . . H2 H 0.859(3) 0.381(2) 0.3405(17) 0.041 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 Mg1 0.0187(9) 0.0246(11) 0.0158(8) 0.000 0.000 0.0042(9) O1 0.0206(15) 0.0231(15) 0.0201(12) -0.0027(12) 0.0073(11) 0.0009(13) Si1 0.0208(6) 0.0247(6) 0.0246(5) 0.0033(5) 0.0050(5) 0.0066(6) Si2 0.0227(6) 0.0212(6) 0.0206(5) 0.0004(5) 0.0008(5) 0.0013(6) C1 0.020(2) 0.023(2) 0.021(2) 0.0006(19) -0.0027(17) 0.0009(19) C2 0.012(2) 0.026(2) 0.018(2) 0.0033(19) 0.0033(18) -0.0006(19) C3 0.0122(19) 0.023(3) 0.0187(19) -0.0014(18) 0.0007(16) 0.0009(18) C4 0.024(2) 0.020(2) 0.0204(19) -0.0012(18) -0.0005(18) 0.0012(19) C5 0.025(2) 0.014(2) 0.0211(19) -0.0018(19) -0.0035(18) 0.0068(19) C6 0.025(2) 0.027(2) 0.0151(18) -0.0046(18) 0.0012(17) 0.000(2) C7 0.030(2) 0.037(3) 0.022(2) -0.003(2) -0.0003(19) 0.001(2) C8 0.027(2) 0.035(3) 0.030(2) -0.001(2) 0.007(2) 0.001(2) C9 0.031(2) 0.045(3) 0.028(2) -0.009(2) 0.002(2) 0.006(2) C10 0.029(2) 0.038(3) 0.048(3) 0.000(2) 0.014(2) 0.007(2) C11 0.036(2) 0.031(3) 0.037(2) -0.002(2) 0.006(2) 0.012(2) C12 0.044(3) 0.024(3) 0.031(2) 0.0037(19) 0.005(2) 0.004(2) C13 0.042(3) 0.033(3) 0.044(2) 0.008(2) -0.012(2) 0.000(2) C14 0.036(3) 0.034(3) 0.033(2) 0.007(2) 0.001(2) 0.011(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 Mg1 O1 2.063(2) . ? Mg1 O1 2.063(2) 2_655 ? Mg1 C1 2.173(4) . ? Mg1 C1 2.173(4) 2_655 ? Mg1 C2 2.761(4) 2_655 ? O1 C8 1.452(4) . ? O1 C5 1.462(4) . ? Si1 C1 1.817(4) . ? Si1 C11 1.860(4) . ? Si1 C9 1.869(3) . ? Si1 C10 1.875(4) . ? Si2 C3 1.840(4) . ? Si2 C12 1.861(3) . ? Si2 C13 1.861(4) . ? Si2 C14 1.869(4) . ? C1 C2 1.461(5) . ? C1 H1 0.93(3) . ? C2 C3 1.348(5) . ? C2 H2 0.94(3) . ? C3 C4 1.520(4) . ? C4 C5 1.502(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.515(4) . ? C5 H5 1.0000 . ? C6 C7 1.525(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.517(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? 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 Mg1 O1 91.52(13) . 2_655 ? O1 Mg1 C1 100.65(12) . . ? O1 Mg1 C1 107.73(11) 2_655 . ? O1 Mg1 C1 107.73(11) . 2_655 ? O1 Mg1 C1 100.65(12) 2_655 2_655 ? C1 Mg1 C1 138.9(2) . 2_655 ? O1 Mg1 C2 135.84(10) . 2_655 ? O1 Mg1 C2 84.78(10) 2_655 2_655 ? C1 Mg1 C2 122.42(13) . 2_655 ? C1 Mg1 C2 31.69(11) 2_655 2_655 ? C8 O1 C5 105.5(2) . . ? C8 O1 Mg1 118.2(2) . . ? C5 O1 Mg1 135.92(19) . . ? C1 Si1 C11 109.51(17) . . ? C1 Si1 C9 111.64(16) . . ? C11 Si1 C9 108.47(18) . . ? C1 Si1 C10 111.67(18) . . ? C11 Si1 C10 109.15(18) . . ? C9 Si1 C10 106.28(17) . . ? C3 Si2 C12 110.73(16) . . ? C3 Si2 C13 110.90(17) . . ? C12 Si2 C13 107.93(17) . . ? C3 Si2 C14 112.40(17) . . ? C12 Si2 C14 107.33(17) . . ? C13 Si2 C14 107.34(19) . . ? C2 C1 Si1 117.8(3) . . ? C2 C1 Mg1 96.9(2) . . ? Si1 C1 Mg1 121.16(19) . . ? C2 C1 H1 110(2) . . ? Si1 C1 H1 112(2) . . ? Mg1 C1 H1 97(2) . . ? C3 C2 C1 132.3(3) . . ? C3 C2 H2 116(2) . . ? C1 C2 H2 111(2) . . ? C2 C3 C4 118.6(3) . . ? C2 C3 Si2 121.7(3) . . ? C4 C3 Si2 119.7(3) . . ? C5 C4 C3 115.3(3) . . ? C5 C4 H4A 108.5 . . ? C3 C4 H4A 108.5 . . ? C5 C4 H4B 108.5 . . ? C3 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? O1 C5 C4 112.2(3) . . ? O1 C5 C6 102.2(3) . . ? C4 C5 C6 116.0(3) . . ? O1 C5 H5 108.7 . . ? C4 C5 H5 108.7 . . ? C6 C5 H5 108.7 . . ? C5 C6 C7 104.0(3) . . ? C5 C6 H6A 111.0 . . ? C7 C6 H6A 111.0 . . ? C5 C6 H6B 111.0 . . ? C7 C6 H6B 111.0 . . ? H6A C6 H6B 109.0 . . ? C8 C7 C6 105.0(3) . . ? C8 C7 H7A 110.8 . . ? C6 C7 H7A 110.8 . . ? C8 C7 H7B 110.8 . . ? C6 C7 H7B 110.8 . . ? H7A C7 H7B 108.8 . . ? O1 C8 C7 105.7(3) . . ? O1 C8 H8A 110.6 . . ? C7 C8 H8A 110.6 . . ? O1 C8 H8B 110.6 . . ? C7 C8 H8B 110.6 . . ? H8A C8 H8B 108.7 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? 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 Mg1 O1 C8 -55.1(2) 2_655 . . . ? C1 Mg1 O1 C8 -163.5(2) . . . . ? C1 Mg1 O1 C8 46.6(2) 2_655 . . . ? C2 Mg1 O1 C8 29.0(3) 2_655 . . . ? O1 Mg1 O1 C5 133.1(3) 2_655 . . . ? C1 Mg1 O1 C5 24.8(3) . . . . ? C1 Mg1 O1 C5 -125.2(3) 2_655 . . . ? C2 Mg1 O1 C5 -142.8(3) 2_655 . . . ? C11 Si1 C1 C2 166.1(3) . . . . ? C9 Si1 C1 C2 -73.8(3) . . . . ? C10 Si1 C1 C2 45.1(3) . . . . ? C11 Si1 C1 Mg1 -75.3(2) . . . . ? C9 Si1 C1 Mg1 44.8(3) . . . . ? C10 Si1 C1 Mg1 163.65(19) . . . . ? O1 Mg1 C1 C2 -61.3(2) . . . . ? O1 Mg1 C1 C2 -156.3(2) 2_655 . . . ? C1 Mg1 C1 C2 72.2(2) 2_655 . . . ? C2 Mg1 C1 C2 108.5(3) 2_655 . . . ? O1 Mg1 C1 Si1 170.18(19) . . . . ? O1 Mg1 C1 Si1 75.1(2) 2_655 . . . ? C1 Mg1 C1 Si1 -56.38(18) 2_655 . . . ? C2 Mg1 C1 Si1 -20.1(3) 2_655 . . . ? Si1 C1 C2 C3 -153.3(3) . . . . ? Mg1 C1 C2 C3 75.9(4) . . . . ? C1 C2 C3 C4 0.0(6) . . . . ? C1 C2 C3 Si2 179.7(3) . . . . ? C12 Si2 C3 C2 -9.8(4) . . . . ? C13 Si2 C3 C2 -129.6(3) . . . . ? C14 Si2 C3 C2 110.2(3) . . . . ? C12 Si2 C3 C4 169.8(3) . . . . ? C13 Si2 C3 C4 50.0(3) . . . . ? C14 Si2 C3 C4 -70.2(3) . . . . ? C2 C3 C4 C5 -91.3(4) . . . . ? Si2 C3 C4 C5 89.1(4) . . . . ? C8 O1 C5 C4 167.7(3) . . . . ? Mg1 O1 C5 C4 -19.8(4) . . . . ? C8 O1 C5 C6 42.8(3) . . . . ? Mg1 O1 C5 C6 -144.8(2) . . . . ? C3 C4 C5 O1 63.7(4) . . . . ? C3 C4 C5 C6 -179.3(3) . . . . ? O1 C5 C6 C7 -35.8(3) . . . . ? C4 C5 C6 C7 -158.2(3) . . . . ? C5 C6 C7 C8 16.4(4) . . . . ? C5 O1 C8 C7 -32.6(3) . . . . ? Mg1 O1 C8 C7 153.3(2) . . . . ? C6 C7 C8 O1 9.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.353 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.068