# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year 2011 _journal_volume 47 _journal_page_first 11680 _publ_contact_author_name 'James C. Fettinger' _publ_contact_author_email jcfettinger@ucdavis.edu loop_ _publ_author_name 'Gereon M. Yee' 'Kristin Kowolik' 'Shuhei Manabe' 'James C. Fettinger' 'Louise A. Berben' data_gmy1tw51 _database_code_depnum_ccdc_archive 'CCDC 830017' #TrackingRef 'GMY1TW51.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H100 Fe Li2 O2 Si8, C5 H12' _chemical_formula_sum 'C69 H112 Fe Li2 O2 Si8' _chemical_formula_weight 1268.04 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' Fe Fe 0.3463 0.8444 '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' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 12.3933(6) _cell_length_b 13.4814(6) _cell_length_c 14.5801(7) _cell_angle_alpha 93.651(2) _cell_angle_beta 114.647(2) _cell_angle_gamma 114.067(2) _cell_volume 1939.78(16) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9870 _cell_measurement_theta_min 4.25 _cell_measurement_theta_max 67.57 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 686 _exptl_absorpt_coefficient_mu 0.356 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9745 _exptl_absorpt_correction_T_max 0.9891 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II Duo CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11875 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.32 _reflns_number_total 11884 _reflns_number_gt 11820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2010-3) (Bruker, 2010)' _computing_cell_refinement 'SAINT (7.68A) (Bruker, 2009)' _computing_data_reduction 'SAINT (7.68A) (Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.924 Data collected on an APEXII Duo with Cu radiation and detector maximum had been reached. PLAT413_ALERT_2_A Short Inter XH3 .. XHn H40B .. H68C .. 1.82 Ang. C68 is a disordered atom in a solvent pentane molecule with a large amount of thermal motion so such short H...H distances are unreliable. ; _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^)+(0.0840P)^2^+0.3961P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.146(12) _refine_ls_number_reflns 11884 _refine_ls_number_parameters 785 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.039 _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 Fe1 Fe 0.03171(4) 0.05909(3) 0.34725(3) 0.02566(12) Uani 1 1 d . . . C1 C -0.0893(3) 0.0976(3) 0.2253(2) 0.0213(6) Uani 1 1 d . . . C2 C -0.1388(3) 0.1257(2) 0.1476(2) 0.0212(6) Uani 1 1 d . . . C3 C -0.1969(3) 0.1601(2) 0.0547(2) 0.0209(6) Uani 1 1 d . . . C4 C -0.3265(3) 0.1510(2) 0.0205(2) 0.0215(6) Uani 1 1 d . . . C5 C -0.3838(3) 0.1764(3) -0.0741(3) 0.0255(7) Uani 1 1 d . . . H5A H -0.4715 0.1693 -0.1002 0.031 Uiso 1 1 calc R . . C6 C -0.3148(4) 0.2117(3) -0.1306(3) 0.0297(7) Uani 1 1 d . . . H6A H -0.3567 0.2261 -0.1957 0.036 Uiso 1 1 calc R . . C7 C -0.1860(3) 0.2257(3) -0.0921(3) 0.0281(7) Uani 1 1 d . . . H7A H -0.1386 0.2531 -0.1298 0.034 Uiso 1 1 calc R . . C8 C -0.1227(3) 0.2006(2) 0.0012(2) 0.0227(6) Uani 1 1 d . . . Si1 Si -0.41652(9) 0.11360(7) 0.10102(7) 0.02599(19) Uani 1 1 d . . . C9 C -0.5682(4) 0.1366(3) 0.0412(3) 0.0352(8) Uani 1 1 d . . . H9A H -0.6210 0.1101 0.0776 0.053 Uiso 1 1 calc R . . H9B H -0.6243 0.0942 -0.0335 0.053 Uiso 1 1 calc R . . H9C H -0.5383 0.2174 0.0483 0.053 Uiso 1 1 calc R . . C10 C -0.3023(5) 0.2108(4) 0.2387(3) 0.0466(10) Uani 1 1 d . . . H10A H -0.3440 0.1843 0.2826 0.070 Uiso 1 1 calc R . . H10B H -0.2880 0.2877 0.2376 0.070 Uiso 1 1 calc R . . H10C H -0.2151 0.2112 0.2676 0.070 Uiso 1 1 calc R . . C11 C -0.4731(4) -0.0376(3) 0.1020(4) 0.0461(10) Uani 1 1 d . . . H11A H -0.5210 -0.0556 0.1427 0.069 Uiso 1 1 calc R . . H11B H -0.3941 -0.0497 0.1341 0.069 Uiso 1 1 calc R . . H11C H -0.5337 -0.0869 0.0297 0.069 Uiso 1 1 calc R . . Si2 Si 0.05975(8) 0.23144(7) 0.05586(7) 0.02479(19) Uani 1 1 d . . . C12 C 0.1668(4) 0.3489(3) 0.1815(3) 0.0374(8) Uani 1 1 d . . . H12A H 0.2592 0.3596 0.2149 0.056 Uiso 1 1 calc R . . H12B H 0.1291 0.3294 0.2291 0.056 Uiso 1 1 calc R . . H12C H 0.1680 0.4190 0.1663 0.056 Uiso 1 1 calc R . . C13 C 0.1153(4) 0.2748(4) -0.0424(4) 0.0435(9) Uani 1 1 d . . . H13A H 0.2099 0.2924 -0.0145 0.065 Uiso 1 1 calc R . . H13B H 0.1066 0.3420 -0.0565 0.065 Uiso 1 1 calc R . . H13C H 0.0586 0.2129 -0.1077 0.065 Uiso 1 1 calc R . . C14 C 0.0833(3) 0.1044(3) 0.0802(3) 0.0301(7) Uani 1 1 d . . . H14A H 0.1631 0.1123 0.0758 0.045 Uiso 1 1 calc R . . H14B H 0.0031 0.0358 0.0270 0.045 Uiso 1 1 calc R . . H14C H 0.0959 0.0991 0.1503 0.045 Uiso 1 1 calc R . . C15 C 0.2123(3) 0.2032(2) 0.4130(2) 0.0218(6) Uani 1 1 d . . . C16 C 0.2985(3) 0.3031(3) 0.4505(2) 0.0242(6) Uani 1 1 d . . . C17 C 0.3995(3) 0.4202(3) 0.4848(2) 0.0258(7) Uani 1 1 d . . . C18 C 0.5281(3) 0.4461(3) 0.4944(2) 0.0287(7) Uani 1 1 d . . . C19 C 0.6243(4) 0.5586(3) 0.5288(3) 0.0358(8) Uani 1 1 d . . . H19A H 0.7113 0.5774 0.5375 0.043 Uiso 1 1 calc R . . C20 C 0.5981(4) 0.6448(3) 0.5512(3) 0.0433(10) Uani 1 1 d . . . H20A H 0.6663 0.7215 0.5740 0.052 Uiso 1 1 calc R . . C21 C 0.4714(4) 0.6194(3) 0.5402(3) 0.0343(8) Uani 1 1 d . . . H21A H 0.4538 0.6792 0.5548 0.041 Uiso 1 1 calc R . . C22 C 0.3696(4) 0.5061(3) 0.5079(2) 0.0278(7) Uani 1 1 d . . . Si3 Si 0.56891(9) 0.33075(8) 0.46258(7) 0.0286(2) Uani 1 1 d . . . C23 C 0.7447(4) 0.4008(4) 0.4791(4) 0.0430(9) Uani 1 1 d . . . H23A H 0.7679 0.3426 0.4640 0.064 Uiso 1 1 calc R . . H23B H 0.8094 0.4488 0.5515 0.064 Uiso 1 1 calc R . . H23C H 0.7482 0.4473 0.4304 0.064 Uiso 1 1 calc R . . C24 C 0.4482(4) 0.2389(3) 0.3239(3) 0.0396(9) Uani 1 1 d . . . H24A H 0.4719 0.1806 0.3102 0.059 Uiso 1 1 calc R . . H24B H 0.4535 0.2853 0.2753 0.059 Uiso 1 1 calc R . . H24C H 0.3559 0.2026 0.3136 0.059 Uiso 1 1 calc R . . C25 C 0.5635(5) 0.2407(4) 0.5549(4) 0.0476(10) Uani 1 1 d . . . H25A H 0.5714 0.1755 0.5315 0.071 Uiso 1 1 calc R . . H25B H 0.4776 0.2143 0.5556 0.071 Uiso 1 1 calc R . . H25C H 0.6386 0.2854 0.6258 0.071 Uiso 1 1 calc R . . Si4 Si 0.20155(9) 0.48948(7) 0.49235(6) 0.0259(2) Uani 1 1 d . . . C26 C 0.0712(6) 0.3463(4) 0.4764(6) 0.0710(18) Uani 1 1 d . . . H26A H -0.0107 0.3491 0.4660 0.106 Uiso 1 1 calc R . . H26B H 0.1062 0.3223 0.5395 0.106 Uiso 1 1 calc R . . H26C H 0.0497 0.2922 0.4151 0.106 Uiso 1 1 calc R . . C27 C 0.2370(5) 0.5790(5) 0.6156(4) 0.0595(13) Uani 1 1 d . . . H27A H 0.1518 0.5705 0.6098 0.089 Uiso 1 1 calc R . . H27B H 0.2965 0.6585 0.6257 0.089 Uiso 1 1 calc R . . H27C H 0.2812 0.5547 0.6759 0.089 Uiso 1 1 calc R . . C28 C 0.1254(7) 0.5400(6) 0.3801(5) 0.0765(17) Uani 1 1 d . . . H28A H 0.0403 0.5334 0.3727 0.115 Uiso 1 1 calc R . . H28B H 0.1077 0.4940 0.3156 0.115 Uiso 1 1 calc R . . H28C H 0.1879 0.6194 0.3924 0.115 Uiso 1 1 calc R . . C29 C 0.0025(3) 0.0305(3) 0.4728(2) 0.0218(6) Uani 1 1 d . . . C30 C 0.0066(3) 0.0063(3) 0.5533(2) 0.0227(6) Uani 1 1 d . . . C31 C 0.0039(3) -0.0276(2) 0.6447(2) 0.0233(6) Uani 1 1 d . . . C32 C -0.0880(3) -0.0204(3) 0.6746(3) 0.0278(7) Uani 1 1 d . . . C33 C -0.0797(4) -0.0462(3) 0.7681(3) 0.0369(8) Uani 1 1 d . . . H33A H -0.1389 -0.0405 0.7911 0.044 Uiso 1 1 calc R . . C34 C 0.0124(4) -0.0797(3) 0.8277(3) 0.0405(9) Uani 1 1 d . . . H34A H 0.0166 -0.0960 0.8911 0.049 Uiso 1 1 calc R . . C35 C 0.0990(4) -0.0897(3) 0.7953(3) 0.0355(8) Uani 1 1 d . . . H35A H 0.1605 -0.1144 0.8364 0.043 Uiso 1 1 calc R . . C36 C 0.0979(3) -0.0643(3) 0.7035(2) 0.0264(7) Uani 1 1 d . . . Si5 Si -0.22003(9) 0.02088(8) 0.59391(8) 0.0307(2) Uani 1 1 d . . . C37 C -0.1341(5) 0.1759(4) 0.6092(5) 0.0537(12) Uani 1 1 d . . . H37A H -0.2009 0.1977 0.5653 0.081 Uiso 1 1 calc R . . H37B H -0.0652 0.1937 0.5873 0.081 Uiso 1 1 calc R . . H37C H -0.0912 0.2178 0.6830 0.081 Uiso 1 1 calc R . . C38 C -0.3407(4) -0.0098(4) 0.6478(3) 0.0421(9) Uani 1 1 d . . . H38A H -0.4125 0.0077 0.6052 0.063 Uiso 1 1 calc R . . H38B H -0.2918 0.0370 0.7207 0.063 Uiso 1 1 calc R . . H38C H -0.3808 -0.0900 0.6455 0.063 Uiso 1 1 calc R . . C39 C -0.3214(4) -0.0649(5) 0.4524(3) 0.0523(11) Uani 1 1 d . . . H39A H -0.3860 -0.0393 0.4126 0.078 Uiso 1 1 calc R . . H39B H -0.3705 -0.1450 0.4475 0.078 Uiso 1 1 calc R . . H39C H -0.2605 -0.0551 0.4232 0.078 Uiso 1 1 calc R . . Si6 Si 0.21406(9) -0.08565(8) 0.66048(7) 0.0292(2) Uani 1 1 d . . . C40 C 0.3293(5) -0.1208(4) 0.7683(3) 0.0424(9) Uani 1 1 d . . . H40A H 0.3888 -0.1343 0.7472 0.064 Uiso 1 1 calc R . . H40B H 0.2753 -0.1891 0.7815 0.064 Uiso 1 1 calc R . . H40C H 0.3842 -0.0576 0.8325 0.064 Uiso 1 1 calc R . . C41 C 0.1146(5) -0.2040(4) 0.5373(3) 0.0519(11) Uani 1 1 d . . . H41A H 0.1765 -0.2201 0.5217 0.078 Uiso 1 1 calc R . . H41B H 0.0616 -0.1825 0.4790 0.078 Uiso 1 1 calc R . . H41C H 0.0535 -0.2717 0.5464 0.078 Uiso 1 1 calc R . . C42 C 0.3234(4) 0.0426(4) 0.6381(3) 0.0386(8) Uani 1 1 d . . . H42A H 0.4041 0.0390 0.6462 0.058 Uiso 1 1 calc R . . H42B H 0.3505 0.1104 0.6894 0.058 Uiso 1 1 calc R . . H42C H 0.2731 0.0462 0.5668 0.058 Uiso 1 1 calc R . . C43 C 0.0048(3) -0.0916(3) 0.2762(2) 0.0234(6) Uani 1 1 d . . . C44 C -0.0320(3) -0.1898(2) 0.2374(2) 0.0222(6) Uani 1 1 d . . . C45 C -0.0696(3) -0.3056(3) 0.1942(2) 0.0225(6) Uani 1 1 d . . . C46 C 0.0208(3) -0.3291(3) 0.1732(2) 0.0238(6) Uani 1 1 d . . . C47 C -0.0222(4) -0.4410(3) 0.1253(3) 0.0304(7) Uani 1 1 d . . . H47A H 0.0360 -0.4585 0.1093 0.036 Uiso 1 1 calc R . . C48 C -0.1482(4) -0.5267(3) 0.1007(3) 0.0366(9) Uani 1 1 d . . . H48A H -0.1770 -0.6020 0.0659 0.044 Uiso 1 1 calc R . . C49 C -0.2328(4) -0.5033(3) 0.1266(3) 0.0315(8) Uani 1 1 d . . . H49A H -0.3172 -0.5641 0.1118 0.038 Uiso 1 1 calc R . . C50 C -0.1982(3) -0.3934(3) 0.1738(3) 0.0276(7) Uani 1 1 d . . . Si7 Si 0.19733(9) -0.21608(7) 0.21122(8) 0.0281(2) Uani 1 1 d . . . C51 C 0.2935(4) -0.1305(4) 0.3516(4) 0.0488(11) Uani 1 1 d . . . H51A H 0.3839 -0.0732 0.3675 0.073 Uiso 1 1 calc R . . H51B H 0.3016 -0.1803 0.3973 0.073 Uiso 1 1 calc R . . H51C H 0.2454 -0.0931 0.3637 0.073 Uiso 1 1 calc R . . C52 C 0.1873(5) -0.1218(4) 0.1230(4) 0.0507(11) Uani 1 1 d . . . H52A H 0.2788 -0.0640 0.1419 0.076 Uiso 1 1 calc R . . H52B H 0.1367 -0.0850 0.1310 0.076 Uiso 1 1 calc R . . H52C H 0.1411 -0.1669 0.0498 0.076 Uiso 1 1 calc R . . C53 C 0.2926(4) -0.2866(3) 0.1933(4) 0.0426(9) Uani 1 1 d . . . H53A H 0.3860 -0.2294 0.2167 0.064 Uiso 1 1 calc R . . H53B H 0.2492 -0.3266 0.1188 0.064 Uiso 1 1 calc R . . H53C H 0.2925 -0.3409 0.2350 0.064 Uiso 1 1 calc R . . Si8 Si -0.31731(9) -0.36818(8) 0.20914(8) 0.0319(2) Uani 1 1 d . . . C54 C -0.2390(5) -0.3010(4) 0.3509(4) 0.0592(14) Uani 1 1 d . . . H54A H -0.3096 -0.3084 0.3685 0.089 Uiso 1 1 calc R . . H54B H -0.1759 -0.2206 0.3678 0.089 Uiso 1 1 calc R . . H54C H -0.1900 -0.3383 0.3916 0.089 Uiso 1 1 calc R . . C55 C -0.4630(4) -0.5093(4) 0.1798(4) 0.0587(13) Uani 1 1 d . . . H55A H -0.5242 -0.4985 0.2004 0.088 Uiso 1 1 calc R . . H55B H -0.4290 -0.5558 0.2194 0.088 Uiso 1 1 calc R . . H55C H -0.5120 -0.5475 0.1043 0.088 Uiso 1 1 calc R . . C56 C -0.3834(8) -0.2826(8) 0.1327(8) 0.116(4) Uani 1 1 d . . . H56A H -0.4477 -0.2745 0.1508 0.174 Uiso 1 1 calc R . . H56B H -0.4292 -0.3204 0.0574 0.174 Uiso 1 1 calc R . . H56C H -0.3083 -0.2076 0.1493 0.174 Uiso 1 1 calc R . . Li1 Li 0.1944(6) 0.1864(5) 0.5553(4) 0.0359(14) Uani 1 1 d . . . O1 O 0.2997(3) 0.2854(2) 0.6917(2) 0.0429(7) Uani 1 1 d . . . C57 C 0.4384(4) 0.3711(3) 0.7356(3) 0.0400(9) Uani 1 1 d . . . H57A H 0.4465 0.4264 0.6940 0.048 Uiso 1 1 calc R . . H57B H 0.4953 0.3366 0.7359 0.048 Uiso 1 1 calc R . . C58 C 0.4808(5) 0.4272(5) 0.8442(4) 0.075(2) Uani 1 1 d . . . H58A H 0.5710 0.4370 0.8933 0.090 Uiso 1 1 calc R . . H58B H 0.4862 0.5028 0.8486 0.090 Uiso 1 1 calc R . . C59 C 0.3813(5) 0.3563(5) 0.8718(4) 0.0595(13) Uani 1 1 d . . . H59A H 0.3618 0.4031 0.9111 0.071 Uiso 1 1 calc R . . H59B H 0.4147 0.3117 0.9162 0.071 Uiso 1 1 calc R . . C60 C 0.2587(5) 0.2805(5) 0.7716(4) 0.0633(16) Uani 1 1 d . . . H60A H 0.2197 0.2020 0.7767 0.076 Uiso 1 1 calc R . . H60B H 0.1898 0.3059 0.7542 0.076 Uiso 1 1 calc R . . Li2 Li -0.1120(7) -0.0544(5) 0.1386(4) 0.0363(13) Uani 1 1 d . . . O2 O -0.2222(3) -0.1421(2) -0.00361(18) 0.0321(5) Uani 1 1 d . . . C61 C -0.2280(4) -0.2446(3) -0.0476(3) 0.0341(8) Uani 1 1 d . . . H61A H -0.2674 -0.3062 -0.0192 0.041 Uiso 1 1 calc R . . H61B H -0.1363 -0.2316 -0.0305 0.041 Uiso 1 1 calc R . . C62 C -0.3166(4) -0.2753(3) -0.1653(3) 0.0373(9) Uani 1 1 d . . . H62A H -0.3661 -0.3583 -0.1974 0.045 Uiso 1 1 calc R . . H62B H -0.2630 -0.2382 -0.1997 0.045 Uiso 1 1 calc R . . C63 C -0.4126(4) -0.2294(3) -0.1724(3) 0.0377(8) Uani 1 1 d . . . H63A H -0.4501 -0.2131 -0.2406 0.045 Uiso 1 1 calc R . . H63B H -0.4880 -0.2836 -0.1636 0.045 Uiso 1 1 calc R . . C64 C -0.3229(4) -0.1214(3) -0.0818(3) 0.0332(8) Uani 1 1 d . . . H64A H -0.2800 -0.0560 -0.1051 0.040 Uiso 1 1 calc R . . H64B H -0.3761 -0.1056 -0.0535 0.040 Uiso 1 1 calc R . . C65 C -0.1936(7) 0.5145(8) 0.8161(7) 0.106(3) Uani 0.50 1 d PD A 1 H65A H -0.2200 0.4372 0.7819 0.158 Uiso 0.50 1 calc PR A 1 H65B H -0.2647 0.5335 0.7756 0.158 Uiso 0.50 1 calc PR A 1 H65C H -0.1809 0.5196 0.8875 0.158 Uiso 0.50 1 calc PR A 1 C65B C -0.1936(7) 0.5145(8) 0.8161(7) 0.106(3) Uani 0.50 1 d PD B 2 H65D H -0.1527 0.5723 0.8817 0.158 Uiso 0.50 1 calc PR B 2 H65E H -0.2415 0.4395 0.8232 0.158 Uiso 0.50 1 calc PR B 2 H65F H -0.2576 0.5287 0.7584 0.158 Uiso 0.50 1 calc PR B 2 C66 C -0.0629(11) 0.5964(11) 0.8209(14) 0.096(3) Uani 0.50 1 d PD A 1 H66A H -0.0269 0.6721 0.8666 0.116 Uiso 0.50 1 calc PR A 1 H66B H -0.0795 0.6032 0.7496 0.116 Uiso 0.50 1 calc PR A 1 C66B C -0.0859(12) 0.5187(14) 0.7929(13) 0.096(3) Uani 0.50 1 d PD B 2 H66C H -0.1147 0.5190 0.7186 0.116 Uiso 0.50 1 calc PR B 2 H66D H -0.0806 0.4480 0.7995 0.116 Uiso 0.50 1 calc PR B 2 C67 C 0.0391(10) 0.5535(9) 0.8645(7) 0.053(2) Uani 0.50 1 d PD A 1 H67A H 0.0996 0.5992 0.9390 0.063 Uiso 0.50 1 calc PR A 1 H67B H -0.0136 0.4758 0.8661 0.063 Uiso 0.50 1 calc PR A 1 C67B C 0.0554(12) 0.6177(15) 0.8603(18) 0.131(7) Uani 0.50 1 d PDU B 2 H67C H 0.0507 0.6881 0.8505 0.157 Uiso 0.50 1 calc PR B 2 H67D H 0.0816 0.6201 0.9348 0.157 Uiso 0.50 1 calc PR B 2 C68 C 0.1296(10) 0.5453(12) 0.8272(9) 0.096(5) Uani 0.50 1 d PD A 1 H68A H 0.1245 0.5836 0.7710 0.115 Uiso 0.50 1 calc PR A 1 H68B H 0.0955 0.4643 0.7953 0.115 Uiso 0.50 1 calc PR A 1 C68B C 0.1650(19) 0.620(3) 0.842(2) 0.205(15) Uani 0.50 1 d PDU B 2 H68C H 0.2121 0.6971 0.8369 0.246 Uiso 0.50 1 calc PR B 2 H68D H 0.1191 0.5682 0.7710 0.246 Uiso 0.50 1 calc PR B 2 C69 C 0.2739(8) 0.5945(8) 0.9084(7) 0.106(2) Uani 0.50 1 d PD A 1 H69A H 0.3113 0.6760 0.9370 0.160 Uiso 0.50 1 calc PR A 1 H69B H 0.3247 0.5819 0.8767 0.160 Uiso 0.50 1 calc PR A 1 H69C H 0.2808 0.5580 0.9652 0.160 Uiso 0.50 1 calc PR A 1 C69B C 0.2739(8) 0.5945(8) 0.9084(7) 0.106(2) Uani 0.50 1 d PDU B 2 H69D H 0.2776 0.5936 0.9768 0.160 Uiso 0.50 1 calc PR B 2 H69E H 0.3609 0.6527 0.9188 0.160 Uiso 0.50 1 calc PR B 2 H69F H 0.2550 0.5203 0.8734 0.160 Uiso 0.50 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 Fe1 0.0293(2) 0.0257(2) 0.0215(2) 0.00686(16) 0.01150(18) 0.01353(19) C1 0.0211(14) 0.0271(15) 0.0184(14) 0.0077(12) 0.0107(12) 0.0126(12) C2 0.0235(14) 0.0236(14) 0.0224(15) 0.0071(11) 0.0137(12) 0.0137(12) C3 0.0248(14) 0.0172(13) 0.0162(13) 0.0029(11) 0.0072(12) 0.0093(12) C4 0.0248(14) 0.0201(14) 0.0208(14) 0.0046(11) 0.0117(12) 0.0113(12) C5 0.0225(14) 0.0279(15) 0.0234(15) 0.0078(12) 0.0079(13) 0.0131(13) C6 0.0344(17) 0.0326(16) 0.0207(15) 0.0120(13) 0.0094(14) 0.0181(15) C7 0.0353(17) 0.0284(16) 0.0247(15) 0.0129(13) 0.0176(14) 0.0149(14) C8 0.0278(15) 0.0205(14) 0.0209(14) 0.0058(11) 0.0124(13) 0.0119(13) Si1 0.0265(4) 0.0340(5) 0.0278(4) 0.0143(4) 0.0170(4) 0.0187(4) C9 0.0280(16) 0.0406(19) 0.044(2) 0.0149(15) 0.0203(16) 0.0194(15) C10 0.051(2) 0.079(3) 0.0258(17) 0.0117(18) 0.0218(17) 0.042(2) C11 0.044(2) 0.043(2) 0.078(3) 0.038(2) 0.045(2) 0.0250(18) Si2 0.0233(4) 0.0255(4) 0.0288(4) 0.0124(3) 0.0153(4) 0.0111(3) C12 0.0284(17) 0.0259(16) 0.045(2) 0.0087(15) 0.0120(16) 0.0080(14) C13 0.0376(19) 0.058(2) 0.049(2) 0.0314(19) 0.0307(18) 0.0229(19) C14 0.0300(16) 0.0329(17) 0.0337(17) 0.0104(14) 0.0183(14) 0.0175(14) C15 0.0235(14) 0.0165(14) 0.0225(14) 0.0031(11) 0.0109(12) 0.0077(12) C16 0.0277(15) 0.0306(17) 0.0197(14) 0.0079(12) 0.0117(13) 0.0182(14) C17 0.0294(15) 0.0235(15) 0.0167(14) 0.0062(11) 0.0071(13) 0.0100(13) C18 0.0326(17) 0.0310(17) 0.0216(15) 0.0099(13) 0.0138(14) 0.0134(14) C19 0.0333(18) 0.0357(19) 0.0295(17) 0.0063(14) 0.0166(15) 0.0079(16) C20 0.050(2) 0.0256(17) 0.0363(19) 0.0018(14) 0.0213(18) 0.0026(16) C21 0.0415(19) 0.0220(15) 0.0308(17) 0.0023(13) 0.0166(15) 0.0096(15) C22 0.0386(17) 0.0243(15) 0.0180(14) 0.0074(12) 0.0122(13) 0.0144(14) Si3 0.0274(4) 0.0345(5) 0.0301(4) 0.0143(4) 0.0179(4) 0.0154(4) C23 0.0357(19) 0.052(2) 0.047(2) 0.0173(18) 0.0262(18) 0.0195(18) C24 0.0403(19) 0.043(2) 0.041(2) 0.0068(16) 0.0268(17) 0.0188(17) C25 0.046(2) 0.065(3) 0.065(3) 0.040(2) 0.039(2) 0.039(2) Si4 0.0335(4) 0.0231(4) 0.0189(4) 0.0045(3) 0.0085(3) 0.0162(4) C26 0.060(3) 0.041(2) 0.141(6) 0.030(3) 0.065(4) 0.031(2) C27 0.046(2) 0.074(3) 0.044(2) -0.010(2) 0.011(2) 0.032(2) C28 0.089(4) 0.134(5) 0.051(3) 0.052(3) 0.037(3) 0.084(4) C29 0.0235(14) 0.0251(14) 0.0185(14) 0.0057(11) 0.0109(12) 0.0123(12) C30 0.0200(13) 0.0238(14) 0.0212(15) 0.0057(11) 0.0084(12) 0.0095(12) C31 0.0240(14) 0.0173(13) 0.0167(13) 0.0024(11) 0.0062(12) 0.0038(12) C32 0.0271(15) 0.0309(17) 0.0205(14) 0.0087(12) 0.0124(13) 0.0088(14) C33 0.0388(18) 0.045(2) 0.0351(18) 0.0186(16) 0.0252(16) 0.0191(17) C34 0.048(2) 0.050(2) 0.0282(17) 0.0224(16) 0.0224(17) 0.0213(18) C35 0.0341(17) 0.0379(18) 0.0282(17) 0.0169(14) 0.0110(15) 0.0149(15) C36 0.0292(16) 0.0253(15) 0.0221(15) 0.0082(12) 0.0107(13) 0.0123(13) Si5 0.0263(4) 0.0394(5) 0.0335(5) 0.0178(4) 0.0181(4) 0.0170(4) C37 0.049(2) 0.051(2) 0.083(3) 0.045(2) 0.038(2) 0.033(2) C38 0.0367(19) 0.045(2) 0.048(2) 0.0133(17) 0.0269(18) 0.0157(17) C39 0.0332(19) 0.091(3) 0.033(2) 0.016(2) 0.0150(17) 0.031(2) Si6 0.0345(5) 0.0304(4) 0.0248(4) 0.0098(3) 0.0121(4) 0.0193(4) C40 0.052(2) 0.044(2) 0.038(2) 0.0154(16) 0.0166(18) 0.0332(19) C41 0.074(3) 0.045(2) 0.0299(19) 0.0029(16) 0.016(2) 0.032(2) C42 0.0337(18) 0.053(2) 0.044(2) 0.0233(17) 0.0232(17) 0.0276(17) C43 0.0265(15) 0.0228(15) 0.0210(14) 0.0081(12) 0.0123(12) 0.0110(13) C44 0.0226(14) 0.0205(15) 0.0202(14) 0.0083(11) 0.0102(12) 0.0071(12) C45 0.0282(15) 0.0239(15) 0.0134(13) 0.0092(11) 0.0078(12) 0.0125(13) C46 0.0321(16) 0.0249(15) 0.0208(14) 0.0106(12) 0.0129(13) 0.0185(13) C47 0.0381(18) 0.0298(17) 0.0275(16) 0.0102(13) 0.0140(15) 0.0217(15) C48 0.044(2) 0.0184(15) 0.0315(17) 0.0031(13) 0.0084(16) 0.0122(15) C49 0.0310(16) 0.0226(15) 0.0261(16) 0.0067(12) 0.0068(14) 0.0074(14) C50 0.0295(16) 0.0184(14) 0.0230(15) 0.0084(12) 0.0083(13) 0.0057(13) Si7 0.0271(4) 0.0250(4) 0.0391(5) 0.0130(4) 0.0186(4) 0.0153(4) C51 0.0265(17) 0.048(2) 0.054(2) -0.0025(19) 0.0113(17) 0.0135(17) C52 0.055(2) 0.050(2) 0.086(3) 0.044(2) 0.053(3) 0.037(2) C53 0.048(2) 0.044(2) 0.056(2) 0.0237(18) 0.034(2) 0.0284(19) Si8 0.0300(4) 0.0329(5) 0.0361(5) 0.0167(4) 0.0207(4) 0.0120(4) C54 0.052(2) 0.050(2) 0.058(3) -0.007(2) 0.039(2) -0.001(2) C55 0.035(2) 0.055(3) 0.058(3) -0.002(2) 0.029(2) -0.006(2) C56 0.125(6) 0.199(8) 0.198(9) 0.172(8) 0.145(7) 0.142(6) Li1 0.034(3) 0.033(3) 0.024(3) -0.001(2) 0.013(2) 0.004(3) O1 0.0343(13) 0.0491(15) 0.0223(12) -0.0091(11) 0.0133(11) 0.0034(12) C57 0.0320(18) 0.042(2) 0.0280(18) 0.0002(15) 0.0136(15) 0.0052(16) C58 0.046(2) 0.083(4) 0.032(2) -0.018(2) 0.019(2) -0.020(3) C59 0.058(3) 0.081(3) 0.032(2) 0.014(2) 0.026(2) 0.021(3) C60 0.047(2) 0.070(3) 0.039(2) -0.020(2) 0.029(2) -0.005(2) Li2 0.047(3) 0.045(3) 0.019(3) 0.007(2) 0.013(3) 0.027(3) O2 0.0345(12) 0.0279(12) 0.0201(11) 0.0023(9) 0.0068(10) 0.0103(10) C61 0.0438(19) 0.0319(17) 0.0262(17) 0.0069(13) 0.0152(15) 0.0199(16) C62 0.049(2) 0.0298(17) 0.0235(17) 0.0030(13) 0.0167(16) 0.0124(16) C63 0.0324(17) 0.0398(19) 0.0251(16) 0.0033(15) 0.0064(14) 0.0121(16) C64 0.0382(18) 0.0317(17) 0.0257(16) 0.0059(13) 0.0097(15) 0.0195(15) C65 0.096(5) 0.144(7) 0.094(5) 0.047(5) 0.048(5) 0.068(5) C65B 0.096(5) 0.144(7) 0.094(5) 0.047(5) 0.048(5) 0.068(5) C66 0.088(7) 0.100(8) 0.094(8) 0.014(7) 0.047(6) 0.039(8) C66B 0.088(7) 0.100(8) 0.094(8) 0.014(7) 0.047(6) 0.039(8) C67 0.081(7) 0.067(6) 0.052(5) 0.032(5) 0.044(5) 0.057(6) C67B 0.130(8) 0.130(8) 0.132(8) 0.039(4) 0.065(4) 0.060(4) C68 0.132(14) 0.073(8) 0.080(9) 0.027(7) 0.060(10) 0.038(9) C68B 0.204(15) 0.204(15) 0.205(15) 0.059(5) 0.098(8) 0.097(8) C69 0.108(3) 0.112(3) 0.110(3) 0.032(3) 0.060(3) 0.053(3) C69B 0.108(3) 0.112(3) 0.110(3) 0.032(3) 0.060(3) 0.053(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 Fe1 C15 2.032(3) . ? Fe1 C29 2.040(3) . ? Fe1 C43 2.049(3) . ? Fe1 C1 2.051(3) . ? Fe1 Li2 2.726(6) . ? Fe1 Li1 2.762(5) . ? C1 C2 1.212(5) . ? C1 Li2 2.186(7) . ? C2 C3 1.451(4) . ? C2 Li2 2.584(7) . ? C3 C8 1.412(5) . ? C3 C4 1.417(5) . ? C4 C5 1.401(5) . ? C4 Si1 1.894(3) . ? C5 C6 1.393(5) . ? C5 H5A 0.9500 . ? C6 C7 1.376(5) . ? C6 H6A 0.9500 . ? C7 C8 1.402(5) . ? C7 H7A 0.9500 . ? C8 Si2 1.900(3) . ? Si1 C11 1.870(4) . ? Si1 C10 1.879(4) . ? Si1 C9 1.879(4) . ? 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 . ? Si2 C13 1.862(4) . ? Si2 C12 1.875(4) . ? Si2 C14 1.882(4) . ? 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 1.224(5) . ? C15 Li1 2.193(7) . ? C16 C17 1.440(5) . ? C16 Li1 2.601(7) . ? C17 C22 1.413(5) . ? C17 C18 1.427(5) . ? C18 C19 1.379(5) . ? C18 Si3 1.906(4) . ? C19 C20 1.382(6) . ? C19 H19A 0.9500 . ? C20 C21 1.398(6) . ? C20 H20A 0.9500 . ? C21 C22 1.411(5) . ? C21 H21A 0.9500 . ? C22 Si4 1.913(4) . ? Si3 C25 1.872(4) . ? Si3 C24 1.873(4) . ? Si3 C23 1.884(4) . ? 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 . ? Si4 C28 1.847(5) . ? Si4 C26 1.864(5) . ? Si4 C27 1.874(5) . ? 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 1.224(5) . ? C29 Li1 2.176(6) . ? C30 C31 1.445(4) . ? C30 Li1 2.577(6) . ? C31 C32 1.413(5) . ? C31 C36 1.423(5) . ? C32 C33 1.402(5) . ? C32 Si5 1.895(4) . ? C33 C34 1.381(6) . ? C33 H33A 0.9500 . ? C34 C35 1.387(6) . ? C34 H34A 0.9500 . ? C35 C36 1.399(5) . ? C35 H35A 0.9500 . ? C36 Si6 1.902(4) . ? Si5 C37 1.865(4) . ? Si5 C39 1.877(4) . ? Si5 C38 1.882(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? Si6 C42 1.861(4) . ? Si6 C41 1.864(4) . ? Si6 C40 1.874(4) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.216(5) . ? C43 Li2 2.160(7) . ? C44 C45 1.445(4) . ? C44 Li2 2.647(7) . ? C45 C46 1.418(5) . ? C45 C50 1.431(5) . ? C46 C47 1.396(5) . ? C46 Si7 1.892(3) . ? C47 C48 1.383(6) . ? C47 H47A 0.9500 . ? C48 C49 1.388(6) . ? C48 H48A 0.9500 . ? C49 C50 1.400(5) . ? C49 H49A 0.9500 . ? C50 Si8 1.893(4) . ? Si7 C51 1.866(5) . ? Si7 C52 1.868(4) . ? Si7 C53 1.873(4) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? Si8 C54 1.845(5) . ? Si8 C56 1.849(11) . ? Si8 C55 1.874(4) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? Li1 O1 1.875(6) . ? O1 C57 1.438(4) . ? O1 C60 1.448(5) . ? C57 C58 1.479(6) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.448(7) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.476(6) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? Li2 O2 1.890(6) . ? O2 C64 1.440(5) . ? O2 C61 1.447(5) . ? C61 C62 1.514(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.521(6) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.520(5) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.511(9) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.519(9) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C66B C67B 1.518(10) . ? C66B H66C 0.9900 . ? C66B H66D 0.9900 . ? C67 C68 1.474(9) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C67B C68B 1.477(10) . ? C67B H67C 0.9900 . ? C67B H67D 0.9900 . ? C68 C69 1.485(9) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C68B H68C 0.9900 . ? C68B H68D 0.9900 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 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 C15 Fe1 C29 103.00(12) . . ? C15 Fe1 C43 122.14(13) . . ? C29 Fe1 C43 104.36(12) . . ? C15 Fe1 C1 102.34(12) . . ? C29 Fe1 C1 123.30(12) . . ? C43 Fe1 C1 103.40(12) . . ? C15 Fe1 Li2 123.36(17) . . ? C29 Fe1 Li2 133.62(17) . . ? C43 Fe1 Li2 51.43(17) . . ? C1 Fe1 Li2 52.17(17) . . ? C15 Fe1 Li1 51.75(15) . . ? C29 Fe1 Li1 51.26(15) . . ? C43 Fe1 Li1 129.50(17) . . ? C1 Fe1 Li1 127.10(17) . . ? Li2 Fe1 Li1 175.1(2) . . ? C2 C1 Fe1 165.7(3) . . ? C2 C1 Li2 94.6(3) . . ? Fe1 C1 Li2 80.01(19) . . ? C1 C2 C3 179.5(4) . . ? C1 C2 Li2 57.5(2) . . ? C3 C2 Li2 122.6(2) . . ? C8 C3 C4 122.3(3) . . ? C8 C3 C2 118.9(3) . . ? C4 C3 C2 118.8(3) . . ? C5 C4 C3 117.1(3) . . ? C5 C4 Si1 120.7(2) . . ? C3 C4 Si1 122.2(2) . . ? C6 C5 C4 121.4(3) . . ? C6 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? C7 C6 C5 120.0(3) . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C6 C7 C8 121.8(3) . . ? C6 C7 H7A 119.1 . . ? C8 C7 H7A 119.1 . . ? C7 C8 C3 117.2(3) . . ? C7 C8 Si2 120.0(2) . . ? C3 C8 Si2 122.6(2) . . ? C11 Si1 C10 110.8(2) . . ? C11 Si1 C9 109.26(18) . . ? C10 Si1 C9 107.45(19) . . ? C11 Si1 C4 110.81(17) . . ? C10 Si1 C4 109.86(17) . . ? C9 Si1 C4 108.59(16) . . ? 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 . . ? C13 Si2 C12 110.17(19) . . ? C13 Si2 C14 106.48(19) . . ? C12 Si2 C14 109.74(16) . . ? C13 Si2 C8 108.67(17) . . ? C12 Si2 C8 108.59(16) . . ? C14 Si2 C8 113.17(14) . . ? 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 . . ? C16 C15 Fe1 162.1(3) . . ? C16 C15 Li1 94.9(3) . . ? Fe1 C15 Li1 81.54(18) . . ? C15 C16 C17 174.4(3) . . ? C15 C16 Li1 57.1(2) . . ? C17 C16 Li1 128.5(2) . . ? C22 C17 C18 121.7(3) . . ? C22 C17 C16 119.8(3) . . ? C18 C17 C16 118.6(3) . . ? C19 C18 C17 117.8(3) . . ? C19 C18 Si3 120.3(3) . . ? C17 C18 Si3 121.9(2) . . ? C18 C19 C20 122.1(4) . . ? C18 C19 H19A 118.9 . . ? C20 C19 H19A 118.9 . . ? C19 C20 C21 120.1(3) . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C20 C21 C22 120.7(4) . . ? C20 C21 H21A 119.6 . . ? C22 C21 H21A 119.6 . . ? C21 C22 C17 117.6(3) . . ? C21 C22 Si4 114.2(3) . . ? C17 C22 Si4 128.0(2) . . ? C25 Si3 C24 109.3(2) . . ? C25 Si3 C23 108.88(19) . . ? C24 Si3 C23 108.37(19) . . ? C25 Si3 C18 110.27(18) . . ? C24 Si3 C18 111.61(17) . . ? C23 Si3 C18 108.35(19) . . ? 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 . . ? C28 Si4 C26 108.4(3) . . ? C28 Si4 C27 109.2(3) . . ? C26 Si4 C27 103.7(3) . . ? C28 Si4 C22 109.0(2) . . ? C26 Si4 C22 118.02(18) . . ? C27 Si4 C22 108.19(18) . . ? 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 . . ? C30 C29 Fe1 165.8(3) . . ? C30 C29 Li1 94.4(3) . . ? Fe1 C29 Li1 81.76(19) . . ? C29 C30 C31 176.8(3) . . ? C29 C30 Li1 57.4(2) . . ? C31 C30 Li1 125.8(2) . . ? C32 C31 C36 122.2(3) . . ? C32 C31 C30 119.5(3) . . ? C36 C31 C30 118.2(3) . . ? C33 C32 C31 117.3(3) . . ? C33 C32 Si5 119.7(3) . . ? C31 C32 Si5 123.0(2) . . ? C34 C33 C32 121.5(4) . . ? C34 C33 H33A 119.3 . . ? C32 C33 H33A 119.3 . . ? C33 C34 C35 120.3(3) . . ? C33 C34 H34A 119.8 . . ? C35 C34 H34A 119.8 . . ? C34 C35 C36 121.6(3) . . ? C34 C35 H35A 119.2 . . ? C36 C35 H35A 119.2 . . ? C35 C36 C31 117.0(3) . . ? C35 C36 Si6 119.4(3) . . ? C31 C36 Si6 123.5(2) . . ? C37 Si5 C39 112.1(2) . . ? C37 Si5 C38 108.9(2) . . ? C39 Si5 C38 107.35(19) . . ? C37 Si5 C32 108.72(18) . . ? C39 Si5 C32 111.7(2) . . ? C38 Si5 C32 107.98(18) . . ? Si5 C37 H37A 109.5 . . ? Si5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si5 C38 H38A 109.5 . . ? Si5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si5 C39 H39A 109.5 . . ? Si5 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si5 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 Si6 C41 108.1(2) . . ? C42 Si6 C40 107.01(19) . . ? C41 Si6 C40 109.2(2) . . ? C42 Si6 C36 113.53(17) . . ? C41 Si6 C36 110.9(2) . . ? C40 Si6 C36 107.89(18) . . ? Si6 C40 H40A 109.5 . . ? Si6 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si6 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si6 C41 H41A 109.5 . . ? Si6 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si6 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si6 C42 H42A 109.5 . . ? Si6 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si6 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 Fe1 167.5(3) . . ? C44 C43 Li2 99.5(3) . . ? Fe1 C43 Li2 80.7(2) . . ? C43 C44 C45 177.4(3) . . ? C43 C44 Li2 53.6(2) . . ? C45 C44 Li2 128.4(2) . . ? C46 C45 C50 122.1(3) . . ? C46 C45 C44 119.5(3) . . ? C50 C45 C44 118.4(3) . . ? C47 C46 C45 118.0(3) . . ? C47 C46 Si7 119.3(3) . . ? C45 C46 Si7 122.7(2) . . ? C48 C47 C46 121.0(4) . . ? C48 C47 H47A 119.5 . . ? C46 C47 H47A 119.5 . . ? C47 C48 C49 120.3(3) . . ? C47 C48 H48A 119.9 . . ? C49 C48 H48A 119.9 . . ? C48 C49 C50 122.4(3) . . ? C48 C49 H49A 118.8 . . ? C50 C49 H49A 118.8 . . ? C49 C50 C45 116.1(3) . . ? C49 C50 Si8 120.0(3) . . ? C45 C50 Si8 123.9(3) . . ? C51 Si7 C52 110.1(2) . . ? C51 Si7 C53 107.5(2) . . ? C52 Si7 C53 108.6(2) . . ? C51 Si7 C46 112.41(18) . . ? C52 Si7 C46 109.46(18) . . ? C53 Si7 C46 108.59(17) . . ? Si7 C51 H51A 109.5 . . ? Si7 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si7 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si7 C52 H52A 109.5 . . ? Si7 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si7 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Si7 C53 H53A 109.5 . . ? Si7 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si7 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C54 Si8 C56 109.5(4) . . ? C54 Si8 C55 105.7(2) . . ? C56 Si8 C55 108.8(3) . . ? C54 Si8 C50 112.6(2) . . ? C56 Si8 C50 112.0(2) . . ? C55 Si8 C50 108.0(2) . . ? Si8 C54 H54A 109.5 . . ? Si8 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? Si8 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Si8 C55 H55A 109.5 . . ? Si8 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? Si8 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? Si8 C56 H56A 109.5 . . ? Si8 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? Si8 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O1 Li1 C29 135.1(3) . . ? O1 Li1 C15 130.8(3) . . ? C29 Li1 C15 93.7(2) . . ? O1 Li1 C30 108.3(3) . . ? C29 Li1 C30 28.27(13) . . ? C15 Li1 C30 120.9(2) . . ? O1 Li1 C16 103.1(3) . . ? C29 Li1 C16 120.3(3) . . ? C15 Li1 C16 27.97(13) . . ? C30 Li1 C16 148.4(2) . . ? O1 Li1 Fe1 173.6(4) . . ? C29 Li1 Fe1 46.98(13) . . ? C15 Li1 Fe1 46.71(13) . . ? C30 Li1 Fe1 74.66(16) . . ? C16 Li1 Fe1 73.73(17) . . ? C57 O1 C60 109.7(3) . . ? C57 O1 Li1 124.6(3) . . ? C60 O1 Li1 125.4(3) . . ? O1 C57 C58 106.1(3) . . ? O1 C57 H57A 110.5 . . ? C58 C57 H57A 110.5 . . ? O1 C57 H57B 110.5 . . ? C58 C57 H57B 110.5 . . ? H57A C57 H57B 108.7 . . ? C59 C58 C57 107.8(4) . . ? C59 C58 H58A 110.1 . . ? C57 C58 H58A 110.1 . . ? C59 C58 H58B 110.1 . . ? C57 C58 H58B 110.1 . . ? H58A C58 H58B 108.5 . . ? C58 C59 C60 106.2(4) . . ? C58 C59 H59A 110.5 . . ? C60 C59 H59A 110.5 . . ? C58 C59 H59B 110.5 . . ? C60 C59 H59B 110.5 . . ? H59A C59 H59B 108.7 . . ? O1 C60 C59 106.8(3) . . ? O1 C60 H60A 110.4 . . ? C59 C60 H60A 110.4 . . ? O1 C60 H60B 110.4 . . ? C59 C60 H60B 110.4 . . ? H60A C60 H60B 108.6 . . ? O2 Li2 C43 130.4(4) . . ? O2 Li2 C1 133.1(4) . . ? C43 Li2 C1 95.5(2) . . ? O2 Li2 C2 106.4(3) . . ? C43 Li2 C2 123.0(3) . . ? C1 Li2 C2 27.88(14) . . ? O2 Li2 C44 103.6(3) . . ? C43 Li2 C44 26.94(13) . . ? C1 Li2 C44 121.1(3) . . ? C2 Li2 C44 149.0(3) . . ? O2 Li2 Fe1 175.3(4) . . ? C43 Li2 Fe1 47.89(14) . . ? C1 Li2 Fe1 47.82(13) . . ? C2 Li2 Fe1 75.15(17) . . ? C44 Li2 Fe1 74.35(16) . . ? C64 O2 C61 110.1(3) . . ? C64 O2 Li2 123.8(3) . . ? C61 O2 Li2 125.8(3) . . ? O2 C61 C62 106.1(3) . . ? O2 C61 H61A 110.5 . . ? C62 C61 H61A 110.5 . . ? O2 C61 H61B 110.5 . . ? C62 C61 H61B 110.5 . . ? H61A C61 H61B 108.7 . . ? C61 C62 C63 101.8(3) . . ? C61 C62 H62A 111.4 . . ? C63 C62 H62A 111.4 . . ? C61 C62 H62B 111.4 . . ? C63 C62 H62B 111.4 . . ? H62A C62 H62B 109.3 . . ? C64 C63 C62 103.2(3) . . ? C64 C63 H63A 111.1 . . ? C62 C63 H63A 111.1 . . ? C64 C63 H63B 111.1 . . ? C62 C63 H63B 111.1 . . ? H63A C63 H63B 109.1 . . ? O2 C64 C63 105.2(3) . . ? O2 C64 H64A 110.7 . . ? C63 C64 H64A 110.7 . . ? O2 C64 H64B 110.7 . . ? C63 C64 H64B 110.7 . . ? H64A C64 H64B 108.8 . . ? C66 C65 H65A 109.5 . . ? C66 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C66 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C65 C66 C67 109.3(9) . . ? C65 C66 H66A 109.8 . . ? C67 C66 H66A 109.8 . . ? C65 C66 H66B 109.8 . . ? C67 C66 H66B 109.8 . . ? H66A C66 H66B 108.3 . . ? C67B C66B H66C 107.9 . . ? C67B C66B H66D 107.9 . . ? H66C C66B H66D 107.2 . . ? C68 C67 C66 129.7(9) . . ? C68 C67 H67A 104.8 . . ? C66 C67 H67A 104.8 . . ? C68 C67 H67B 104.8 . . ? C66 C67 H67B 104.8 . . ? H67A C67 H67B 105.8 . . ? C68B C67B C66B 118.1(14) . . ? C68B C67B H67C 107.8 . . ? C66B C67B H67C 107.8 . . ? C68B C67B H67D 107.8 . . ? C66B C67B H67D 107.8 . . ? H67C C67B H67D 107.1 . . ? C67 C68 C69 115.7(9) . . ? C67 C68 H68A 108.4 . . ? C69 C68 H68A 108.4 . . ? C67 C68 H68B 108.4 . . ? C69 C68 H68B 108.4 . . ? H68A C68 H68B 107.4 . . ? C67B C68B H68C 105.4 . . ? C67B C68B H68D 105.4 . . ? H68C C68B H68D 106.0 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.32 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.598 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.068 # Attachment 'GMY8FMI.cif' data_gmy8fmi _database_code_depnum_ccdc_archive 'CCDC 830018' #TrackingRef 'GMY8FMI.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C64 H102 Li2 Mn O2 Si8), 2(C5 H12)' _chemical_formula_sum 'C69 H114 Li2 Mn O2 Si8' _chemical_formula_weight 1269.14 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'I 2' _symmetry_space_group_name_Hall 'I 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 15.2016(8) _cell_length_b 12.4057(6) _cell_length_c 20.7660(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.6680(10) _cell_angle_gamma 90.00 _cell_volume 3903.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9922 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 30.50 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1374 _exptl_absorpt_coefficient_mu 0.330 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9334 _exptl_absorpt_correction_T_max 0.9572 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21551 _diffrn_reflns_av_R_equivalents 0.0110 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 30.50 _reflns_number_total 11838 _reflns_number_gt 11460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2010-11.3) (Bruker, 2010)' _computing_cell_refinement 'SAINT (7.68A) (Bruker, 2009)' _computing_data_reduction 'SAINT (7.68A) (Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0613P)^2^+0.8503P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.404(8) _refine_ls_number_reflns 11838 _refine_ls_number_parameters 410 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.057 _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 Mn1 Mn 0.5000 0.662550(19) 1.0000 0.02082(5) Uani 1 2 d S . . Si1 Si 0.56779(3) 0.56581(3) 0.769281(18) 0.02901(8) Uani 1 1 d . . . Si2 Si 0.61035(2) 1.01047(3) 0.852174(17) 0.02628(7) Uani 1 1 d . . . Si3 Si 0.20501(3) 0.73789(4) 0.85452(2) 0.03538(9) Uani 1 1 d . . . Si4 Si 0.30732(3) 0.29700(3) 0.926936(18) 0.02945(8) Uani 1 1 d . . . Li1 Li 0.66663(15) 0.6469(2) 0.94869(13) 0.0352(5) Uani 1 1 d . . . C1 C 0.54875(8) 0.73879(10) 0.91896(6) 0.0249(2) Uani 1 1 d . . . C2 C 0.57519(7) 0.76164(9) 0.86648(6) 0.02152(19) Uani 1 1 d . . . C3 C 0.60309(7) 0.79014(10) 0.80402(5) 0.02054(18) Uani 1 1 d . . . C4 C 0.60823(8) 0.70805(10) 0.75677(6) 0.0239(2) Uani 1 1 d . . . C5 C 0.64031(9) 0.73708(12) 0.69803(6) 0.0306(2) Uani 1 1 d . . . H5 H 0.6444 0.6838 0.6655 0.037 Uiso 1 1 calc R . . C6 C 0.66642(11) 0.84221(13) 0.68598(6) 0.0345(3) Uani 1 1 d . . . H6 H 0.6898 0.8596 0.6462 0.041 Uiso 1 1 calc R . . C7 C 0.65825(9) 0.92156(11) 0.73229(6) 0.0302(2) Uani 1 1 d . . . H7 H 0.6753 0.9933 0.7233 0.036 Uiso 1 1 calc R . . C8 C 0.62550(8) 0.89869(9) 0.79209(6) 0.0223(2) Uani 1 1 d . . . C9 C 0.44606(11) 0.56821(15) 0.77606(9) 0.0438(4) Uani 1 1 d . . . H9A H 0.4164 0.5982 0.7364 0.066 Uiso 1 1 calc R . . H9B H 0.4330 0.6131 0.8129 0.066 Uiso 1 1 calc R . . H9C H 0.4249 0.4947 0.7824 0.066 Uiso 1 1 calc R . . C10 C 0.62207(11) 0.49846(11) 0.84265(7) 0.0352(3) Uani 1 1 d . . . H10A H 0.6212 0.4202 0.8363 0.053 Uiso 1 1 calc R . . H10B H 0.5902 0.5167 0.8803 0.053 Uiso 1 1 calc R . . H10C H 0.6833 0.5232 0.8497 0.053 Uiso 1 1 calc R . . C11 C 0.59513(14) 0.48317(14) 0.69821(8) 0.0458(4) Uani 1 1 d . . . H11A H 0.5729 0.4096 0.7028 0.069 Uiso 1 1 calc R . . H11B H 0.6593 0.4812 0.6962 0.069 Uiso 1 1 calc R . . H11C H 0.5675 0.5154 0.6585 0.069 Uiso 1 1 calc R . . C12 C 0.69352(12) 0.99708(13) 0.92320(7) 0.0391(3) Uani 1 1 d . . . H12A H 0.6859 1.0561 0.9536 0.059 Uiso 1 1 calc R . . H12B H 0.7531 1.0001 0.9085 0.059 Uiso 1 1 calc R . . H12C H 0.6852 0.9280 0.9447 0.059 Uiso 1 1 calc R . . C13 C 0.62725(12) 1.14225(11) 0.81061(8) 0.0383(3) Uani 1 1 d . . . H13A H 0.5827 1.1504 0.7741 0.058 Uiso 1 1 calc R . . H13B H 0.6863 1.1437 0.7948 0.058 Uiso 1 1 calc R . . H13C H 0.6217 1.2015 0.8412 0.058 Uiso 1 1 calc R . . C14 C 0.49570(11) 1.01190(13) 0.87840(9) 0.0406(3) Uani 1 1 d . . . H14A H 0.4852 0.9456 0.9022 0.061 Uiso 1 1 calc R . . H14B H 0.4533 1.0165 0.8403 0.061 Uiso 1 1 calc R . . H14C H 0.4884 1.0743 0.9064 0.061 Uiso 1 1 calc R . . C15 C 0.38204(8) 0.58102(10) 0.96446(6) 0.0248(2) Uani 1 1 d . . . H15 H 0.3987 0.5087 0.9829 0.030 Uiso 1 1 calc R . . C16 C 0.31702(8) 0.55098(10) 0.93055(5) 0.0228(2) Uani 1 1 d . . . C17 C 0.24451(8) 0.51152(11) 0.88810(6) 0.0246(2) Uani 1 1 d . . . C18 C 0.18942(9) 0.58641(13) 0.85233(6) 0.0309(3) Uani 1 1 d . . . C19 C 0.11862(11) 0.54344(17) 0.81241(8) 0.0450(4) Uani 1 1 d . . . H19 H 0.0803 0.5913 0.7879 0.054 Uiso 1 1 calc R . . C20 C 0.10323(12) 0.43384(18) 0.80786(9) 0.0496(4) Uani 1 1 d . . . H20 H 0.0541 0.4074 0.7814 0.059 Uiso 1 1 calc R . . C21 C 0.15975(11) 0.36240(15) 0.84208(8) 0.0424(4) Uani 1 1 d . . . H21 H 0.1494 0.2871 0.8377 0.051 Uiso 1 1 calc R . . C22 C 0.23150(9) 0.39845(12) 0.88286(6) 0.0294(2) Uani 1 1 d . . . C23 C 0.31696(12) 0.78510(17) 0.84016(12) 0.0541(5) Uani 1 1 d . . . H23A H 0.3183 0.8641 0.8409 0.081 Uiso 1 1 calc R . . H23B H 0.3325 0.7593 0.7979 0.081 Uiso 1 1 calc R . . H23C H 0.3595 0.7570 0.8740 0.081 Uiso 1 1 calc R . . C24 C 0.12875(15) 0.7965(2) 0.78803(11) 0.0629(6) Uani 1 1 d . . . H24A H 0.1318 0.8753 0.7899 0.094 Uiso 1 1 calc R . . H24B H 0.0682 0.7730 0.7933 0.094 Uiso 1 1 calc R . . H24C H 0.1464 0.7716 0.7462 0.094 Uiso 1 1 calc R . . C25 C 0.17178(14) 0.79292(15) 0.93240(10) 0.0485(4) Uani 1 1 d . . . H25A H 0.2114 0.7649 0.9681 0.073 Uiso 1 1 calc R . . H25B H 0.1110 0.7710 0.9384 0.073 Uiso 1 1 calc R . . H25C H 0.1754 0.8718 0.9317 0.073 Uiso 1 1 calc R . . C26 C 0.29908(14) 0.30825(13) 1.01615(7) 0.0436(4) Uani 1 1 d . . . H26A H 0.2400 0.2861 1.0265 0.065 Uiso 1 1 calc R . . H26B H 0.3096 0.3831 1.0298 0.065 Uiso 1 1 calc R . . H26C H 0.3433 0.2614 1.0389 0.065 Uiso 1 1 calc R . . C27 C 0.27038(12) 0.15852(14) 0.90045(8) 0.0428(3) Uani 1 1 d . . . H27A H 0.2744 0.1512 0.8538 0.064 Uiso 1 1 calc R . . H27B H 0.2091 0.1474 0.9105 0.064 Uiso 1 1 calc R . . H27C H 0.3083 0.1046 0.9233 0.064 Uiso 1 1 calc R . . C28 C 0.42494(10) 0.31533(13) 0.90829(9) 0.0377(3) Uani 1 1 d . . . H28A H 0.4624 0.2639 0.9336 0.057 Uiso 1 1 calc R . . H28B H 0.4440 0.3890 0.9194 0.057 Uiso 1 1 calc R . . H28C H 0.4299 0.3028 0.8621 0.057 Uiso 1 1 calc R . . O31 O 0.78344(6) 0.64883(9) 0.92450(5) 0.0329(2) Uani 1 1 d . . . C31 C 0.85196(9) 0.57555(13) 0.95028(8) 0.0351(3) Uani 0.67 1 d P A 1 H31A H 0.8313 0.5000 0.9466 0.042 Uiso 0.67 1 calc PR A 1 H31B H 0.8687 0.5916 0.9964 0.042 Uiso 0.67 1 calc PR A 1 C32 C 0.92949(15) 0.5930(3) 0.91044(14) 0.0377(5) Uani 0.67 1 d P A 1 H32A H 0.9861 0.5857 0.9372 0.045 Uiso 0.67 1 calc PR A 1 H32B H 0.9285 0.5412 0.8741 0.045 Uiso 0.67 1 calc PR A 1 C33 C 0.91599(11) 0.70693(18) 0.88626(12) 0.0535(5) Uani 0.67 1 d P A 1 H33A H 0.9454 0.7589 0.9172 0.064 Uiso 0.67 1 calc PR A 1 H33B H 0.9404 0.7160 0.8438 0.064 Uiso 0.67 1 calc PR A 1 C31B C 0.85196(9) 0.57555(13) 0.95028(8) 0.0351(3) Uani 0.33 1 d P A 2 H31C H 0.8469 0.5048 0.9282 0.042 Uiso 0.33 1 calc PR A 2 H31D H 0.8487 0.5645 0.9972 0.042 Uiso 0.33 1 calc PR A 2 C32B C 0.9410(3) 0.6344(4) 0.9362(3) 0.0320(8) Uani 0.33 1 d P A 2 H32C H 0.9665 0.6730 0.9751 0.038 Uiso 0.33 1 calc PR A 2 H32D H 0.9849 0.5820 0.9225 0.038 Uiso 0.33 1 calc PR A 2 C33B C 0.91599(11) 0.70693(18) 0.88626(12) 0.0535(5) Uani 0.33 1 d P A 2 H33C H 0.9346 0.6784 0.8450 0.064 Uiso 0.33 1 calc PR A 2 H33D H 0.9462 0.7767 0.8950 0.064 Uiso 0.33 1 calc PR A 2 C34 C 0.81916(10) 0.72412(16) 0.88045(9) 0.0428(4) Uani 1 1 d . A . H34A H 0.8049 0.7991 0.8922 0.051 Uiso 1 1 calc R B 1 H34B H 0.7944 0.7104 0.8356 0.051 Uiso 1 1 calc R B 1 C41 C 0.0219(5) -0.0159(6) 1.0029(5) 0.071(2) Uiso 0.35 1 d PDU C -1 H41A H 0.0460 -0.0133 1.0481 0.107 Uiso 0.35 1 calc PR C -1 H41B H 0.0345 -0.0864 0.9844 0.107 Uiso 0.35 1 calc PR C -1 H41C H -0.0421 -0.0048 1.0006 0.107 Uiso 0.35 1 calc PR C -1 C42 C 0.0613(12) 0.0663(10) 0.9673(10) 0.179(8) Uiso 0.35 1 d PDU C -1 H42A H 0.0674 0.0393 0.9230 0.214 Uiso 0.35 1 calc PR C -1 H42B H 0.1215 0.0799 0.9876 0.214 Uiso 0.35 1 calc PR C -1 C43 C 0.0134(7) 0.1696(8) 0.9625(5) 0.093(3) Uiso 0.35 1 d PD C -1 H43A H 0.0343 0.2105 0.9258 0.112 Uiso 0.35 1 calc PR C -1 H43B H -0.0499 0.1539 0.9520 0.112 Uiso 0.35 1 calc PR C -1 C44 C 0.0214(12) 0.2397(9) 1.0198(6) 0.130(5) Uiso 0.35 1 d PDU C -1 H44A H 0.0787 0.2321 1.0456 0.156 Uiso 0.35 1 calc PR C -1 H44B H -0.0280 0.2309 1.0477 0.156 Uiso 0.35 1 calc PR C -1 C45 C 0.0145(9) 0.3459(7) 0.9786(5) 0.079(2) Uiso 0.35 1 d PDU C -1 H45A H 0.0199 0.3284 0.9331 0.118 Uiso 0.35 1 calc PR C -1 H45B H 0.0620 0.3952 0.9939 0.118 Uiso 0.35 1 calc PR C -1 H45C H -0.0427 0.3803 0.9831 0.118 Uiso 0.35 1 calc PR C -1 C46 C -0.0196(11) 0.3502(11) 0.9918(10) 0.054(4) Uiso 0.15 1 d PDU D -2 H46A H -0.0646 0.3852 0.9625 0.081 Uiso 0.15 1 calc PR D -2 H46B H 0.0320 0.3976 0.9985 0.081 Uiso 0.15 1 calc PR D -2 H46C H -0.0437 0.3363 1.0334 0.081 Uiso 0.15 1 calc PR D -2 C47 C 0.007(2) 0.2456(13) 0.9629(16) 0.125(6) Uiso 0.15 1 d PDU D -2 H47A H 0.0713 0.2334 0.9735 0.150 Uiso 0.15 1 calc PR D -2 H47B H -0.0038 0.2484 0.9153 0.150 Uiso 0.15 1 calc PR D -2 C48 C -0.0444(9) 0.1547(11) 0.9893(8) 0.058(3) Uiso 0.15 1 d PD D -2 H48A H -0.0925 0.1308 0.9575 0.069 Uiso 0.15 1 calc PR D -2 H48B H -0.0700 0.1762 1.0298 0.069 Uiso 0.15 1 calc PR D -2 C49 C 0.0249(19) 0.067(3) 1.002(3) 0.162(11) Uiso 0.15 1 d PDU D -2 H49A H 0.0434 0.0379 0.9606 0.194 Uiso 0.15 1 calc PR D -2 H49B H 0.0776 0.0955 1.0274 0.194 Uiso 0.15 1 calc PR D -2 C50 C -0.019(3) -0.019(2) 1.0387(19) 0.142(11) Uiso 0.15 1 d PDU D -2 H50A H -0.0486 0.0147 1.0739 0.213 Uiso 0.15 1 calc PR D -2 H50B H 0.0252 -0.0701 1.0566 0.213 Uiso 0.15 1 calc PR D -2 H50C H -0.0629 -0.0564 1.0096 0.213 Uiso 0.15 1 calc PR D -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 Mn1 0.02043(10) 0.02270(11) 0.02007(10) 0.000 0.00618(7) 0.000 Si1 0.03323(18) 0.02391(15) 0.03037(17) -0.00674(13) 0.00546(13) -0.00444(13) Si2 0.03210(16) 0.01964(14) 0.02739(15) -0.00034(12) 0.00419(12) 0.00052(12) Si3 0.03535(18) 0.0392(2) 0.03247(18) 0.01379(16) 0.00784(14) 0.01498(16) Si4 0.03599(18) 0.02469(16) 0.02741(16) -0.00275(13) 0.00095(13) 0.00036(13) Li1 0.0242(10) 0.0399(13) 0.0431(12) 0.0056(11) 0.0119(9) 0.0037(9) C1 0.0260(5) 0.0228(5) 0.0269(5) -0.0014(4) 0.0074(4) 0.0007(4) C2 0.0215(4) 0.0194(4) 0.0241(5) -0.0007(4) 0.0048(4) 0.0006(4) C3 0.0194(4) 0.0229(5) 0.0195(4) -0.0004(4) 0.0026(3) -0.0005(4) C4 0.0246(5) 0.0260(5) 0.0214(5) -0.0032(4) 0.0035(4) -0.0004(4) C5 0.0383(6) 0.0337(6) 0.0205(5) -0.0034(5) 0.0060(4) -0.0008(5) C6 0.0440(8) 0.0383(7) 0.0224(5) 0.0037(5) 0.0100(5) -0.0033(6) C7 0.0357(6) 0.0297(6) 0.0256(5) 0.0048(5) 0.0059(5) -0.0040(5) C8 0.0230(5) 0.0224(5) 0.0218(5) 0.0013(4) 0.0025(4) -0.0009(4) C9 0.0366(7) 0.0434(8) 0.0515(9) -0.0118(7) 0.0039(6) -0.0114(6) C10 0.0463(8) 0.0215(5) 0.0385(7) -0.0006(5) 0.0084(6) 0.0024(5) C11 0.0602(10) 0.0373(8) 0.0412(8) -0.0176(6) 0.0122(7) -0.0093(7) C12 0.0525(9) 0.0323(7) 0.0313(6) -0.0069(5) -0.0049(6) 0.0020(6) C13 0.0483(8) 0.0235(6) 0.0431(7) 0.0037(5) 0.0027(6) -0.0049(5) C14 0.0423(7) 0.0265(6) 0.0557(9) 0.0006(6) 0.0207(7) 0.0073(6) C15 0.0263(5) 0.0232(5) 0.0251(5) 0.0022(4) 0.0029(4) 0.0001(4) C16 0.0240(5) 0.0236(5) 0.0213(5) 0.0023(4) 0.0041(4) 0.0045(4) C17 0.0221(5) 0.0318(6) 0.0200(4) -0.0005(4) 0.0022(4) 0.0055(4) C18 0.0260(5) 0.0411(7) 0.0254(5) 0.0028(5) 0.0013(4) 0.0105(5) C19 0.0332(7) 0.0640(11) 0.0359(7) -0.0024(7) -0.0096(6) 0.0164(7) C20 0.0362(8) 0.0616(11) 0.0475(9) -0.0153(8) -0.0170(7) 0.0052(7) C21 0.0358(7) 0.0474(8) 0.0420(8) -0.0133(7) -0.0084(6) -0.0021(6) C22 0.0272(5) 0.0346(6) 0.0259(5) -0.0056(5) -0.0009(4) 0.0004(5) C23 0.0415(8) 0.0479(9) 0.0741(13) 0.0275(9) 0.0118(8) 0.0094(7) C24 0.0519(10) 0.0729(14) 0.0636(12) 0.0343(11) 0.0032(9) 0.0258(10) C25 0.0599(10) 0.0369(8) 0.0505(9) 0.0018(7) 0.0153(8) 0.0057(8) C26 0.0706(11) 0.0314(7) 0.0287(6) 0.0021(5) 0.0033(7) -0.0026(7) C27 0.0543(9) 0.0280(6) 0.0463(8) -0.0078(6) 0.0056(7) -0.0047(7) C28 0.0325(6) 0.0316(6) 0.0488(8) -0.0010(6) 0.0017(6) 0.0067(5) O31 0.0234(4) 0.0388(5) 0.0377(5) 0.0068(4) 0.0097(3) 0.0025(4) C31 0.0279(6) 0.0383(7) 0.0401(7) 0.0054(6) 0.0080(5) 0.0047(5) C32 0.0252(9) 0.0501(14) 0.0381(12) -0.0062(11) 0.0051(8) 0.0057(9) C33 0.0260(6) 0.0597(11) 0.0760(13) 0.0262(10) 0.0119(7) -0.0007(7) C31B 0.0279(6) 0.0383(7) 0.0401(7) 0.0054(6) 0.0080(5) 0.0047(5) C32B 0.0168(15) 0.042(2) 0.038(2) 0.013(2) 0.0059(15) 0.0015(15) C33B 0.0260(6) 0.0597(11) 0.0760(13) 0.0262(10) 0.0119(7) -0.0007(7) C34 0.0294(6) 0.0530(9) 0.0474(8) 0.0203(7) 0.0122(6) 0.0074(6) _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 Mn1 C1 2.1163(12) 2_657 ? Mn1 C1 2.1163(12) . ? Mn1 C15 2.1372(13) . ? Mn1 C15 2.1372(13) 2_657 ? Mn1 Li1 2.833(2) 2_657 ? Mn1 Li1 2.833(2) . ? Si1 C9 1.8674(17) . ? Si1 C10 1.8696(16) . ? Si1 C11 1.8713(16) . ? Si1 C4 1.8934(13) . ? Si2 C14 1.8679(16) . ? Si2 C12 1.8703(16) . ? Si2 C13 1.8761(15) . ? Si2 C8 1.8919(12) . ? Si3 C23 1.847(2) . ? Si3 C25 1.8627(19) . ? Si3 C24 1.8755(19) . ? Si3 C18 1.8942(17) . ? Si4 C26 1.8722(16) . ? Si4 C28 1.8738(16) . ? Si4 C27 1.8758(17) . ? Si4 C22 1.8917(15) . ? Li1 O31 1.884(2) . ? Li1 C15 2.165(3) 2_657 ? Li1 C1 2.170(3) . ? Li1 C2 2.546(3) . ? Li1 C16 2.769(3) 2_657 ? C1 C2 1.2251(17) . ? C2 C3 1.4411(16) . ? C3 C8 1.4158(16) . ? C3 C4 1.4207(16) . ? C4 C5 1.3973(17) . ? C5 C6 1.392(2) . ? C5 H5 0.9500 . ? C6 C7 1.389(2) . ? C6 H6 0.9500 . ? C7 C8 1.4038(16) . ? C7 H7 0.9500 . ? 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 1.2242(17) . ? C15 Li1 2.165(3) 2_657 ? C15 H15 1.0000 . ? C16 C17 1.4400(17) . ? C16 Li1 2.769(3) 2_657 ? C17 C18 1.4195(18) . ? C17 C22 1.420(2) . ? C18 C19 1.409(2) . ? C19 C20 1.382(3) . ? C19 H19 0.9500 . ? C20 C21 1.389(3) . ? C20 H20 0.9500 . ? C21 C22 1.3988(19) . ? C21 H21 0.9500 . ? 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 . ? O31 C34 1.4438(18) . ? O31 C31 1.4517(17) . ? C31 C32 1.510(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.508(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.483(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C32B H32C 0.9900 . ? C32B H32D 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C41 C42 1.421(9) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.473(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.470(9) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.569(9) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.502(10) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.503(10) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.524(10) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.499(10) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 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 C1 Mn1 C1 126.91(7) 2_657 . ? C1 Mn1 C15 98.50(5) 2_657 . ? C1 Mn1 C15 105.97(5) . . ? C1 Mn1 C15 105.97(5) 2_657 2_657 ? C1 Mn1 C15 98.50(5) . 2_657 ? C15 Mn1 C15 123.51(7) . 2_657 ? C1 Mn1 Li1 49.45(6) 2_657 2_657 ? C1 Mn1 Li1 135.33(7) . 2_657 ? C15 Mn1 Li1 49.22(6) . 2_657 ? C15 Mn1 Li1 126.05(7) 2_657 2_657 ? C1 Mn1 Li1 135.33(7) 2_657 . ? C1 Mn1 Li1 49.45(6) . . ? C15 Mn1 Li1 126.05(7) . . ? C15 Mn1 Li1 49.22(6) 2_657 . ? Li1 Mn1 Li1 172.16(11) 2_657 . ? C9 Si1 C10 108.67(8) . . ? C9 Si1 C11 110.69(8) . . ? C10 Si1 C11 106.63(8) . . ? C9 Si1 C4 109.29(7) . . ? C10 Si1 C4 113.68(6) . . ? C11 Si1 C4 107.87(7) . . ? C14 Si2 C12 110.96(9) . . ? C14 Si2 C13 106.97(8) . . ? C12 Si2 C13 109.33(8) . . ? C14 Si2 C8 111.46(7) . . ? C12 Si2 C8 110.14(6) . . ? C13 Si2 C8 107.86(7) . . ? C23 Si3 C25 110.03(11) . . ? C23 Si3 C24 106.30(10) . . ? C25 Si3 C24 107.59(11) . . ? C23 Si3 C18 115.21(8) . . ? C25 Si3 C18 110.01(8) . . ? C24 Si3 C18 107.34(10) . . ? C26 Si4 C28 109.71(9) . . ? C26 Si4 C27 108.42(8) . . ? C28 Si4 C27 108.57(8) . . ? C26 Si4 C22 110.00(7) . . ? C28 Si4 C22 111.92(7) . . ? C27 Si4 C22 108.14(7) . . ? O31 Li1 C15 128.32(14) . 2_657 ? O31 Li1 C1 133.77(14) . . ? C15 Li1 C1 96.03(10) 2_657 . ? O31 Li1 C2 106.81(12) . . ? C15 Li1 C2 124.38(11) 2_657 . ? C1 Li1 C2 28.72(5) . . ? O31 Li1 C16 103.28(11) . 2_657 ? C15 Li1 C16 25.12(5) 2_657 2_657 ? C1 Li1 C16 119.64(10) . 2_657 ? C2 Li1 C16 148.35(10) . 2_657 ? O31 Li1 Mn1 171.89(15) . . ? C15 Li1 Mn1 48.38(6) 2_657 . ? C1 Li1 Mn1 47.81(6) . . ? C2 Li1 Mn1 76.00(7) . . ? C16 Li1 Mn1 72.89(6) 2_657 . ? C2 C1 Mn1 166.47(10) . . ? C2 C1 Li1 92.95(11) . . ? Mn1 C1 Li1 82.74(8) . . ? C1 C2 C3 177.86(12) . . ? C1 C2 Li1 58.33(9) . . ? C3 C2 Li1 123.78(9) . . ? C8 C3 C4 122.24(10) . . ? C8 C3 C2 118.91(10) . . ? C4 C3 C2 118.84(11) . . ? C5 C4 C3 117.44(12) . . ? C5 C4 Si1 120.02(10) . . ? C3 C4 Si1 122.45(9) . . ? C6 C5 C4 121.55(12) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C7 C6 C5 119.79(12) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 121.83(12) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.1 . . ? C7 C8 C3 117.04(11) . . ? C7 C8 Si2 120.41(9) . . ? C3 C8 Si2 122.54(8) . . ? 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 . . ? C16 C15 Mn1 163.38(10) . . ? C16 C15 Li1 106.24(11) . 2_657 ? Mn1 C15 Li1 82.39(8) . 2_657 ? C16 C15 H15 96.5 . . ? Mn1 C15 H15 96.5 . . ? Li1 C15 H15 96.5 2_657 . ? C15 C16 C17 176.10(13) . . ? C15 C16 Li1 48.64(9) . 2_657 ? C17 C16 Li1 135.11(9) . 2_657 ? C18 C17 C22 122.28(12) . . ? C18 C17 C16 119.18(12) . . ? C22 C17 C16 118.54(11) . . ? C19 C18 C17 116.76(15) . . ? C19 C18 Si3 118.53(11) . . ? C17 C18 Si3 124.71(11) . . ? C20 C19 C18 121.98(15) . . ? C20 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? C19 C20 C21 119.91(15) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 121.68(17) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C21 C22 C17 117.34(14) . . ? C21 C22 Si4 119.64(12) . . ? C17 C22 Si4 123.01(10) . . ? 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 . . ? C34 O31 C31 110.07(10) . . ? C34 O31 Li1 126.01(12) . . ? C31 O31 Li1 123.87(12) . . ? O31 C31 C32 106.07(14) . . ? O31 C31 H31A 110.5 . . ? C32 C31 H31A 110.5 . . ? O31 C31 H31B 110.5 . . ? C32 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? C33 C32 C31 103.04(17) . . ? C33 C32 H32A 111.2 . . ? C31 C32 H32A 111.2 . . ? C33 C32 H32B 111.2 . . ? C31 C32 H32B 111.2 . . ? H32A C32 H32B 109.1 . . ? C34 C33 C32 105.62(16) . . ? C34 C33 H33A 110.6 . . ? C32 C33 H33A 110.6 . . ? C34 C33 H33B 110.6 . . ? C32 C33 H33B 110.6 . . ? H33A C33 H33B 108.7 . . ? H32C C32B H32D 108.9 . . ? O31 C34 C33 106.11(13) . . ? O31 C34 H34A 110.5 . . ? C33 C34 H34A 110.5 . . ? O31 C34 H34B 110.5 . . ? C33 C34 H34B 110.5 . . ? H34A C34 H34B 108.7 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C41 C42 C43 115.6(10) . . ? C41 C42 H42A 108.4 . . ? C43 C42 H42A 108.4 . . ? C41 C42 H42B 108.4 . . ? C43 C42 H42B 108.4 . . ? H42A C42 H42B 107.4 . . ? C44 C43 C42 116.9(11) . . ? C44 C43 H43A 108.1 . . ? C42 C43 H43A 108.1 . . ? C44 C43 H43B 108.1 . . ? C42 C43 H43B 108.1 . . ? H43A C43 H43B 107.3 . . ? C43 C44 C45 93.3(8) . . ? C43 C44 H44A 113.0 . . ? C45 C44 H44A 113.0 . . ? C43 C44 H44B 113.0 . . ? C45 C44 H44B 113.0 . . ? H44A C44 H44B 110.4 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C46 C47 C48 109.5(12) . . ? C46 C47 H47A 109.8 . . ? C48 C47 H47A 109.8 . . ? C46 C47 H47B 109.8 . . ? C48 C47 H47B 109.8 . . ? H47A C47 H47B 108.2 . . ? C47 C48 C49 102.8(12) . . ? C47 C48 H48A 111.2 . . ? C49 C48 H48A 111.2 . . ? C47 C48 H48B 111.2 . . ? C49 C48 H48B 111.2 . . ? H48A C48 H48B 109.1 . . ? C50 C49 C48 105.1(13) . . ? C50 C49 H49A 110.7 . . ? C48 C49 H49A 110.7 . . ? C50 C49 H49B 110.7 . . ? C48 C49 H49B 110.7 . . ? H49A C49 H49B 108.8 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 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 C1 Mn1 Li1 C15 69.17(11) 2_657 . . 2_657 ? C1 Mn1 Li1 C15 174.16(12) . . . 2_657 ? C15 Mn1 Li1 C15 -105.90(10) . . . 2_657 ? C1 Mn1 Li1 C1 -104.99(11) 2_657 . . . ? C15 Mn1 Li1 C1 79.93(9) . . . . ? C15 Mn1 Li1 C1 -174.16(12) 2_657 . . . ? C1 Mn1 Li1 C2 -111.33(8) 2_657 . . . ? C1 Mn1 Li1 C2 -6.34(5) . . . . ? C15 Mn1 Li1 C2 73.60(9) . . . . ? C15 Mn1 Li1 C2 179.50(11) 2_657 . . . ? C1 Mn1 Li1 C16 62.77(10) 2_657 . . 2_657 ? C1 Mn1 Li1 C16 167.76(11) . . . 2_657 ? C15 Mn1 Li1 C16 -112.31(7) . . . 2_657 ? C15 Mn1 Li1 C16 -6.40(5) 2_657 . . 2_657 ? C1 Mn1 C1 C2 -166.0(5) 2_657 . . . ? C15 Mn1 C1 C2 -52.0(5) . . . . ? C15 Mn1 C1 C2 76.6(5) 2_657 . . . ? Li1 Mn1 C1 C2 -99.4(5) 2_657 . . . ? Li1 Mn1 C1 C2 72.1(4) . . . . ? C1 Mn1 C1 Li1 121.87(9) 2_657 . . . ? C15 Mn1 C1 Li1 -124.10(9) . . . . ? C15 Mn1 C1 Li1 4.47(9) 2_657 . . . ? Li1 Mn1 C1 Li1 -171.51(12) 2_657 . . . ? O31 Li1 C1 C2 23.8(2) . . . . ? C15 Li1 C1 C2 -171.51(12) 2_657 . . . ? C16 Li1 C1 C2 179.40(13) 2_657 . . . ? Mn1 Li1 C1 C2 -167.12(10) . . . . ? O31 Li1 C1 Mn1 -169.1(2) . . . . ? C15 Li1 C1 Mn1 -4.38(9) 2_657 . . . ? C2 Li1 C1 Mn1 167.12(10) . . . . ? C16 Li1 C1 Mn1 -13.48(11) 2_657 . . . ? Mn1 C1 C2 Li1 -70.9(4) . . . . ? O31 Li1 C2 C1 -162.31(17) . . . . ? C15 Li1 C2 C1 10.25(14) 2_657 . . . ? C16 Li1 C2 C1 -1.0(2) 2_657 . . . ? Mn1 Li1 C2 C1 9.80(8) . . . . ? O31 Li1 C2 C3 18.09(18) . . . . ? C15 Li1 C2 C3 -169.35(13) 2_657 . . . ? C1 Li1 C2 C3 -179.60(15) . . . . ? C16 Li1 C2 C3 179.40(19) 2_657 . . . ? Mn1 Li1 C2 C3 -169.80(10) . . . . ? Li1 C2 C3 C8 -110.43(13) . . . . ? Li1 C2 C3 C4 68.79(15) . . . . ? C8 C3 C4 C5 2.77(17) . . . . ? C2 C3 C4 C5 -176.42(11) . . . . ? C8 C3 C4 Si1 -173.80(9) . . . . ? C2 C3 C4 Si1 7.01(15) . . . . ? C9 Si1 C4 C5 -112.65(12) . . . . ? C10 Si1 C4 C5 125.77(11) . . . . ? C11 Si1 C4 C5 7.75(13) . . . . ? C9 Si1 C4 C3 63.83(12) . . . . ? C10 Si1 C4 C3 -57.75(12) . . . . ? C11 Si1 C4 C3 -175.76(11) . . . . ? C3 C4 C5 C6 0.1(2) . . . . ? Si1 C4 C5 C6 176.73(11) . . . . ? C4 C5 C6 C7 -2.0(2) . . . . ? C5 C6 C7 C8 1.1(2) . . . . ? C6 C7 C8 C3 1.58(19) . . . . ? C6 C7 C8 Si2 -177.06(11) . . . . ? C4 C3 C8 C7 -3.56(17) . . . . ? C2 C3 C8 C7 175.63(11) . . . . ? C4 C3 C8 Si2 175.05(9) . . . . ? C2 C3 C8 Si2 -5.76(15) . . . . ? C14 Si2 C8 C7 126.48(11) . . . . ? C12 Si2 C8 C7 -109.90(11) . . . . ? C13 Si2 C8 C7 9.35(12) . . . . ? C14 Si2 C8 C3 -52.08(12) . . . . ? C12 Si2 C8 C3 71.53(12) . . . . ? C13 Si2 C8 C3 -169.22(10) . . . . ? C1 Mn1 C15 C16 118.1(4) 2_657 . . . ? C1 Mn1 C15 C16 -14.3(4) . . . . ? C15 Mn1 C15 C16 -126.2(4) 2_657 . . . ? Li1 Mn1 C15 C16 122.6(4) 2_657 . . . ? Li1 Mn1 C15 C16 -65.4(4) . . . . ? C1 Mn1 C15 Li1 -4.48(9) 2_657 . . 2_657 ? C1 Mn1 C15 Li1 -136.89(9) . . . 2_657 ? C15 Mn1 C15 Li1 111.15(9) 2_657 . . 2_657 ? Li1 Mn1 C15 Li1 172.02(12) . . . 2_657 ? Mn1 C15 C16 Li1 -119.6(4) . . . 2_657 ? Li1 C16 C17 C18 76.18(17) 2_657 . . . ? Li1 C16 C17 C22 -104.72(16) 2_657 . . . ? C22 C17 C18 C19 2.0(2) . . . . ? C16 C17 C18 C19 -178.95(13) . . . . ? C22 C17 C18 Si3 -177.75(10) . . . . ? C16 C17 C18 Si3 1.31(17) . . . . ? C23 Si3 C18 C19 -128.20(14) . . . . ? C25 Si3 C18 C19 106.75(14) . . . . ? C24 Si3 C18 C19 -10.03(15) . . . . ? C23 Si3 C18 C17 51.54(15) . . . . ? C25 Si3 C18 C17 -73.51(14) . . . . ? C24 Si3 C18 C17 169.70(13) . . . . ? C17 C18 C19 C20 -0.2(3) . . . . ? Si3 C18 C19 C20 179.56(16) . . . . ? C18 C19 C20 C21 -1.6(3) . . . . ? C19 C20 C21 C22 1.6(3) . . . . ? C20 C21 C22 C17 0.1(3) . . . . ? C20 C21 C22 Si4 -178.85(15) . . . . ? C18 C17 C22 C21 -1.9(2) . . . . ? C16 C17 C22 C21 179.00(13) . . . . ? C18 C17 C22 Si4 176.95(10) . . . . ? C16 C17 C22 Si4 -2.12(17) . . . . ? C26 Si4 C22 C21 -114.76(14) . . . . ? C28 Si4 C22 C21 123.02(14) . . . . ? C27 Si4 C22 C21 3.47(15) . . . . ? C26 Si4 C22 C17 66.38(13) . . . . ? C28 Si4 C22 C17 -55.84(13) . . . . ? C27 Si4 C22 C17 -175.39(12) . . . . ? C15 Li1 O31 C34 -155.89(17) 2_657 . . . ? C1 Li1 O31 C34 4.6(3) . . . . ? C2 Li1 O31 C34 16.3(2) . . . . ? C16 Li1 O31 C34 -153.76(14) 2_657 . . . ? C15 Li1 O31 C31 21.5(3) 2_657 . . . ? C1 Li1 O31 C31 -177.95(17) . . . . ? C2 Li1 O31 C31 -166.28(12) . . . . ? C16 Li1 O31 C31 23.66(18) 2_657 . . . ? C34 O31 C31 C32 -11.1(2) . . . . ? Li1 O31 C31 C32 171.07(18) . . . . ? O31 C31 C32 C33 25.3(2) . . . . ? C31 C32 C33 C34 -30.3(2) . . . . ? C31 O31 C34 C33 -8.2(2) . . . . ? Li1 O31 C34 C33 169.57(17) . . . . ? C32 C33 C34 O31 24.2(2) . . . . ? C41 C42 C43 C44 77(2) . . . . ? C42 C43 C44 C45 147.5(12) . . . . ? C46 C47 C48 C49 -138(3) . . . . ? C47 C48 C49 C50 171(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.504 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.049 # Attachment 'gmy10fmi.cif' data_gmy10fmi _database_code_depnum_ccdc_archive 'CCDC 830019' #TrackingRef 'gmy10fmi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H84 Si8 V, C16 H32 Li O4' _chemical_formula_sum 'C72 H116 Li O4 Si8 V' _chemical_formula_weight 1328.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' _symmetry_space_group_name_Hall 'P 4abw 2nw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 14.7882(3) _cell_length_b 14.7882(3) _cell_length_c 38.0825(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8328.30(13) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9857 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 67.79 _exptl_crystal_description Needle _exptl_crystal_colour Blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2872 _exptl_absorpt_coefficient_mu 2.403 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7115 _exptl_absorpt_correction_T_max 0.8673 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII DUO CCD' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45018 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 68.57 _reflns_number_total 7380 _reflns_number_gt 6824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2010-7) (Bruker, 2010)' _computing_cell_refinement 'SAINT (7.68A) (Bruker, 2009)' _computing_data_reduction 'SAINT (7.68A) (Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0643P)^2^+1.2522P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(5) _refine_ls_number_reflns 7380 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 V1 V 0.97806(2) -0.02194(2) 0.0000 0.03153(12) Uani 1 2 d S . . C1 C 0.93491(15) -0.09592(15) 0.04128(6) 0.0400(5) Uani 1 1 d . . . C2 C 0.89510(15) -0.13431(14) 0.06509(6) 0.0390(5) Uani 1 1 d . . . C3 C 0.84564(16) -0.17589(14) 0.09316(6) 0.0390(5) Uani 1 1 d . . . C4 C 0.75215(16) -0.15863(14) 0.09615(6) 0.0390(5) Uani 1 1 d . . . C5 C 0.70673(17) -0.19693(15) 0.12485(6) 0.0424(5) Uani 1 1 d . . . H5A H 0.6438 -0.1862 0.1276 0.051 Uiso 1 1 calc R . . C6 C 0.75129(17) -0.24989(16) 0.14927(6) 0.0457(5) Uani 1 1 d . . . H6A H 0.7193 -0.2745 0.1687 0.055 Uiso 1 1 calc R . . C7 C 0.84226(18) -0.26686(16) 0.14533(7) 0.0473(6) Uani 1 1 d . . . H7A H 0.8718 -0.3043 0.1620 0.057 Uiso 1 1 calc R . . C8 C 0.89242(16) -0.23091(15) 0.11767(6) 0.0428(5) Uani 1 1 d . . . Si1 Si 0.68900(4) -0.08615(4) 0.063517(17) 0.04119(15) Uani 1 1 d . . . C9 C 0.73537(18) 0.03097(17) 0.06221(7) 0.0520(6) Uani 1 1 d . . . H9A H 0.7014 0.0669 0.0451 0.078 Uiso 1 1 calc R . . H9B H 0.7992 0.0289 0.0554 0.078 Uiso 1 1 calc R . . H9C H 0.7299 0.0586 0.0855 0.078 Uiso 1 1 calc R . . C10 C 0.69036(18) -0.13772(19) 0.01872(7) 0.0519(6) Uani 1 1 d . . . H10A H 0.6572 -0.0987 0.0024 0.078 Uiso 1 1 calc R . . H10B H 0.6616 -0.1974 0.0195 0.078 Uiso 1 1 calc R . . H10C H 0.7530 -0.1442 0.0107 0.078 Uiso 1 1 calc R . . C11 C 0.56900(17) -0.0773(2) 0.07918(7) 0.0538(6) Uani 1 1 d . . . H11A H 0.5342 -0.0399 0.0628 0.081 Uiso 1 1 calc R . . H11B H 0.5679 -0.0494 0.1025 0.081 Uiso 1 1 calc R . . H11C H 0.5422 -0.1378 0.0804 0.081 Uiso 1 1 calc R . . Si2 Si 1.01733(5) -0.25521(5) 0.11324(2) 0.05003(17) Uani 1 1 d . . . C12 C 1.0454(2) -0.30213(19) 0.06939(8) 0.0687(9) Uani 1 1 d . . . H12A H 1.1105 -0.3139 0.0680 0.103 Uiso 1 1 calc R . . H12B H 1.0283 -0.2586 0.0512 0.103 Uiso 1 1 calc R . . H12C H 1.0122 -0.3587 0.0658 0.103 Uiso 1 1 calc R . . C13 C 1.0509(2) -0.3409(2) 0.14711(9) 0.0664(8) Uani 1 1 d . . . H13A H 1.1157 -0.3538 0.1450 0.100 Uiso 1 1 calc R . . H13B H 1.0164 -0.3967 0.1435 0.100 Uiso 1 1 calc R . . H13C H 1.0382 -0.3170 0.1706 0.100 Uiso 1 1 calc R . . C14 C 1.08302(19) -0.1494(2) 0.12105(10) 0.0676(8) Uani 1 1 d . . . H14A H 1.1478 -0.1621 0.1187 0.101 Uiso 1 1 calc R . . H14B H 1.0705 -0.1268 0.1448 0.101 Uiso 1 1 calc R . . H14C H 1.0653 -0.1036 0.1038 0.101 Uiso 1 1 calc R . . C15 C 0.96346(14) 0.10971(14) 0.01357(6) 0.0351(4) Uani 1 1 d . . . C16 C 0.96427(14) 0.18596(14) 0.02545(6) 0.0359(4) Uani 1 1 d . . . C17 C 0.96813(15) 0.27478(14) 0.04086(6) 0.0382(5) Uani 1 1 d . . . C18 C 1.02753(17) 0.28920(15) 0.06930(6) 0.0432(5) Uani 1 1 d . . . C19 C 1.0302(2) 0.37610(17) 0.08406(7) 0.0538(7) Uani 1 1 d . . . H19A H 1.0693 0.3877 0.1033 0.065 Uiso 1 1 calc R . . C20 C 0.9772(2) 0.44482(17) 0.07105(7) 0.0600(7) Uani 1 1 d . . . H20A H 0.9798 0.5031 0.0815 0.072 Uiso 1 1 calc R . . C21 C 0.9207(2) 0.42991(16) 0.04308(7) 0.0550(7) Uani 1 1 d . . . H21A H 0.8851 0.4785 0.0344 0.066 Uiso 1 1 calc R . . C22 C 0.91391(17) 0.34463(15) 0.02700(6) 0.0441(5) Uani 1 1 d . . . Si3 Si 1.09840(6) 0.19567(5) 0.08787(2) 0.05609(19) Uani 1 1 d . . . C23 C 1.1616(3) 0.2428(3) 0.12647(8) 0.0797(10) Uani 1 1 d . . . H23A H 1.1994 0.1954 0.1368 0.120 Uiso 1 1 calc R . . H23B H 1.1184 0.2647 0.1441 0.120 Uiso 1 1 calc R . . H23C H 1.1999 0.2931 0.1187 0.120 Uiso 1 1 calc R . . C24 C 1.1836(2) 0.1561(3) 0.05508(9) 0.0835(11) Uani 1 1 d . . . H24A H 1.1524 0.1311 0.0346 0.125 Uiso 1 1 calc R . . H24B H 1.2217 0.1093 0.0657 0.125 Uiso 1 1 calc R . . H24C H 1.2215 0.2072 0.0478 0.125 Uiso 1 1 calc R . . C25 C 1.0236(3) 0.1037(2) 0.10484(8) 0.0789(10) Uani 1 1 d . . . H25A H 0.9894 0.0773 0.0853 0.118 Uiso 1 1 calc R . . H25B H 0.9816 0.1288 0.1222 0.118 Uiso 1 1 calc R . . H25C H 1.0607 0.0568 0.1159 0.118 Uiso 1 1 calc R . . Si4 Si 0.83790(5) 0.32579(4) -0.011908(19) 0.05020(18) Uani 1 1 d . . . C26 C 0.7735(2) 0.43233(18) -0.02065(8) 0.0614(7) Uani 1 1 d . . . H26A H 0.7336 0.4234 -0.0409 0.092 Uiso 1 1 calc R . . H26B H 0.8160 0.4815 -0.0256 0.092 Uiso 1 1 calc R . . H26C H 0.7372 0.4479 0.0000 0.092 Uiso 1 1 calc R . . C27 C 0.7522(2) 0.23619(17) -0.00264(8) 0.0626(7) Uani 1 1 d . . . H27A H 0.7136 0.2278 -0.0233 0.094 Uiso 1 1 calc R . . H27B H 0.7150 0.2544 0.0174 0.094 Uiso 1 1 calc R . . H27C H 0.7831 0.1793 0.0028 0.094 Uiso 1 1 calc R . . C28 C 0.9091(2) 0.2961(2) -0.05069(7) 0.0688(9) Uani 1 1 d . . . H28A H 0.8702 0.2862 -0.0712 0.103 Uiso 1 1 calc R . . H28B H 0.9433 0.2409 -0.0457 0.103 Uiso 1 1 calc R . . H28C H 0.9512 0.3457 -0.0556 0.103 Uiso 1 1 calc R . . Li1 Li 0.4930(3) 0.4930(3) 0.0000 0.0605(16) Uani 1 2 d S . . O1 O 0.57187(12) 0.51946(12) 0.03942(5) 0.0554(4) Uani 1 1 d . . . C29 C 0.60314(19) 0.60787(18) 0.04958(7) 0.0545(6) Uani 1 1 d . . . H29A H 0.5628 0.6345 0.0676 0.065 Uiso 1 1 calc R . . H29B H 0.6052 0.6489 0.0290 0.065 Uiso 1 1 calc R . . C30 C 0.6962(2) 0.59305(18) 0.06420(8) 0.0569(7) Uani 1 1 d . . . H30A H 0.7143 0.6429 0.0801 0.068 Uiso 1 1 calc R . . H30B H 0.7416 0.5867 0.0453 0.068 Uiso 1 1 calc R . . C31 C 0.6837(2) 0.5052(2) 0.08411(8) 0.0657(8) Uani 1 1 d . . . H31A H 0.6624 0.5168 0.1083 0.079 Uiso 1 1 calc R . . H31B H 0.7411 0.4708 0.0852 0.079 Uiso 1 1 calc R . . C32 C 0.61256(19) 0.45405(19) 0.06300(8) 0.0595(7) Uani 1 1 d . . . H32A H 0.6409 0.4044 0.0495 0.071 Uiso 1 1 calc R . . H32B H 0.5663 0.4280 0.0788 0.071 Uiso 1 1 calc R . . O2 O 0.36727(13) 0.50396(16) 0.01438(6) 0.0738(6) Uani 1 1 d . . . C33 C 0.3364(2) 0.5247(3) 0.04898(10) 0.0739(9) Uani 1 1 d . . . H33A H 0.3260 0.5906 0.0515 0.089 Uiso 1 1 calc R . . H33B H 0.3815 0.5056 0.0667 0.089 Uiso 1 1 calc R . . C34 C 0.2501(3) 0.4739(3) 0.05371(13) 0.1035(14) Uani 1 1 d . . . H34A H 0.2618 0.4122 0.0627 0.124 Uiso 1 1 calc R . . H34B H 0.2095 0.5057 0.0703 0.124 Uiso 1 1 calc R . . C35 C 0.2101(3) 0.4707(4) 0.01813(14) 0.1214(18) Uani 1 1 d . . . H35A H 0.1694 0.5228 0.0142 0.146 Uiso 1 1 calc R . . H35B H 0.1756 0.4140 0.0146 0.146 Uiso 1 1 calc R . . C36 C 0.2900(2) 0.4746(3) -0.00610(12) 0.0974(13) Uani 1 1 d . . . H36A H 0.3016 0.4142 -0.0164 0.117 Uiso 1 1 calc R . . H36B H 0.2783 0.5177 -0.0255 0.117 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 V1 0.03041(16) 0.03041(16) 0.0338(3) -0.00153(13) 0.00153(13) -0.00096(19) C1 0.0425(12) 0.0347(11) 0.0428(13) -0.0023(9) 0.0031(9) -0.0043(9) C2 0.0425(12) 0.0330(11) 0.0414(13) -0.0049(9) 0.0021(9) -0.0029(9) C3 0.0471(12) 0.0301(10) 0.0397(13) -0.0062(8) 0.0069(9) -0.0075(9) C4 0.0488(13) 0.0309(11) 0.0372(12) -0.0062(8) 0.0081(9) -0.0059(9) C5 0.0472(13) 0.0339(11) 0.0461(14) -0.0044(9) 0.0116(10) -0.0053(9) C6 0.0562(14) 0.0377(12) 0.0431(13) 0.0024(9) 0.0128(10) -0.0075(10) C7 0.0550(15) 0.0391(12) 0.0478(15) 0.0039(10) 0.0056(10) -0.0036(10) C8 0.0495(13) 0.0347(11) 0.0441(13) -0.0016(9) 0.0043(10) -0.0065(9) Si1 0.0447(3) 0.0400(3) 0.0388(3) -0.0048(2) 0.0053(2) -0.0038(3) C9 0.0563(15) 0.0411(13) 0.0588(16) -0.0001(11) 0.0008(12) -0.0002(11) C10 0.0500(14) 0.0621(16) 0.0437(15) -0.0076(11) 0.0072(11) -0.0088(12) C11 0.0495(14) 0.0627(16) 0.0492(16) -0.0007(12) 0.0077(11) 0.0038(12) Si2 0.0492(4) 0.0396(3) 0.0613(4) 0.0042(3) 0.0085(3) -0.0002(3) C12 0.091(2) 0.0442(15) 0.071(2) 0.0081(13) 0.0300(16) 0.0148(14) C13 0.0601(17) 0.0680(19) 0.071(2) 0.0158(15) 0.0025(13) 0.0077(14) C14 0.0431(15) 0.0527(16) 0.107(3) -0.0036(15) 0.0014(14) -0.0045(12) C15 0.0324(11) 0.0369(11) 0.0360(12) 0.0003(8) 0.0004(8) 0.0010(8) C16 0.0380(11) 0.0375(12) 0.0323(12) 0.0012(8) 0.0008(8) -0.0010(8) C17 0.0436(12) 0.0329(11) 0.0380(13) -0.0006(8) 0.0104(9) -0.0053(9) C18 0.0477(13) 0.0422(12) 0.0396(13) -0.0060(9) 0.0105(10) -0.0109(10) C19 0.0653(17) 0.0496(14) 0.0466(15) -0.0117(11) 0.0111(12) -0.0221(12) C20 0.087(2) 0.0365(13) 0.0562(17) -0.0104(11) 0.0172(15) -0.0165(13) C21 0.0796(19) 0.0317(12) 0.0539(17) -0.0006(10) 0.0171(13) -0.0010(12) C22 0.0549(14) 0.0329(11) 0.0446(14) 0.0013(9) 0.0112(10) 0.0005(10) Si3 0.0628(4) 0.0583(4) 0.0472(4) -0.0127(3) -0.0154(3) -0.0003(3) C23 0.091(2) 0.087(2) 0.061(2) -0.0214(16) -0.0273(16) -0.0088(19) C24 0.0563(18) 0.105(3) 0.089(3) -0.046(2) -0.0218(16) 0.0165(18) C25 0.134(3) 0.0518(16) 0.0507(18) 0.0073(12) -0.0284(18) -0.0193(18) Si4 0.0650(4) 0.0366(3) 0.0491(4) 0.0034(3) -0.0013(3) 0.0144(3) C26 0.0706(18) 0.0440(14) 0.0694(19) 0.0095(12) 0.0084(14) 0.0194(13) C27 0.0652(17) 0.0430(14) 0.079(2) 0.0049(13) -0.0239(15) 0.0069(12) C28 0.094(2) 0.0667(19) 0.0459(17) 0.0009(13) -0.0036(14) 0.0366(17) Li1 0.055(2) 0.055(2) 0.072(5) 0.004(2) -0.004(2) -0.008(3) O1 0.0533(10) 0.0520(10) 0.0610(12) 0.0127(8) -0.0055(8) 0.0022(8) C29 0.0681(17) 0.0478(14) 0.0475(15) 0.0029(11) -0.0026(12) 0.0166(12) C30 0.0686(18) 0.0454(14) 0.0568(17) -0.0099(12) -0.0117(13) 0.0123(12) C31 0.0760(19) 0.0659(18) 0.0552(18) 0.0068(13) -0.0064(14) 0.0254(15) C32 0.0624(17) 0.0518(15) 0.0643(18) 0.0219(13) 0.0037(13) 0.0078(12) O2 0.0506(11) 0.0883(16) 0.0824(16) -0.0009(11) -0.0016(10) -0.0077(10) C33 0.0672(19) 0.073(2) 0.082(2) 0.0090(17) 0.0066(16) 0.0036(16) C34 0.061(2) 0.127(4) 0.122(4) 0.025(3) 0.012(2) -0.010(2) C35 0.063(2) 0.155(5) 0.147(4) 0.020(4) -0.009(3) -0.031(3) C36 0.061(2) 0.117(3) 0.114(3) -0.007(3) -0.019(2) -0.022(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 V1 C1 2.019(2) 7_645 ? V1 C1 2.019(2) . ? V1 C15 2.026(2) . ? V1 C15 2.026(2) 7_645 ? C1 C2 1.221(3) . ? C2 C3 1.434(3) . ? C3 C4 1.411(3) . ? C3 C8 1.418(3) . ? C4 C5 1.402(3) . ? C4 Si1 1.888(2) . ? C5 C6 1.383(4) . ? C5 H5A 0.9500 . ? C6 C7 1.377(4) . ? C6 H6A 0.9500 . ? C7 C8 1.394(3) . ? C7 H7A 0.9500 . ? C8 Si2 1.889(3) . ? Si1 C9 1.863(3) . ? Si1 C10 1.869(3) . ? Si1 C11 1.877(3) . ? 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 . ? Si2 C12 1.855(3) . ? Si2 C14 1.866(3) . ? Si2 C13 1.875(3) . ? 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 1.215(3) . ? C16 C17 1.440(3) . ? C17 C22 1.410(3) . ? C17 C18 1.411(3) . ? C18 C19 1.403(3) . ? C18 Si3 1.874(3) . ? C19 C20 1.376(4) . ? C19 H19A 0.9500 . ? C20 C21 1.372(4) . ? C20 H20A 0.9500 . ? C21 C22 1.406(3) . ? C21 H21A 0.9500 . ? C22 Si4 1.881(3) . ? Si3 C25 1.868(3) . ? Si3 C24 1.868(3) . ? Si3 C23 1.876(3) . ? 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 . ? Si4 C28 1.866(3) . ? Si4 C27 1.867(3) . ? Si4 C26 1.871(3) . ? 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 . ? Li1 O1 1.940(4) . ? Li1 O1 1.940(4) 7 ? Li1 O2 1.946(4) 7 ? Li1 O2 1.946(4) . ? O1 C29 1.440(3) . ? O1 C32 1.451(3) . ? C29 C30 1.500(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.515(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.525(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? O2 C33 1.428(4) . ? O2 C36 1.450(4) . ? C33 C34 1.492(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.479(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.499(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 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 C1 V1 C1 105.29(13) 7_645 . ? C1 V1 C15 116.41(9) 7_645 . ? C1 V1 C15 106.76(9) . . ? C1 V1 C15 106.77(9) 7_645 7_645 ? C1 V1 C15 116.41(9) . 7_645 ? C15 V1 C15 105.66(12) . 7_645 ? C2 C1 V1 169.3(2) . . ? C1 C2 C3 177.4(2) . . ? C4 C3 C8 121.9(2) . . ? C4 C3 C2 118.9(2) . . ? C8 C3 C2 119.2(2) . . ? C5 C4 C3 117.3(2) . . ? C5 C4 Si1 120.35(18) . . ? C3 C4 Si1 122.30(16) . . ? C6 C5 C4 121.6(2) . . ? C6 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? C7 C6 C5 119.7(2) . . ? C7 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C6 C7 C8 122.2(2) . . ? C6 C7 H7A 118.9 . . ? C8 C7 H7A 118.9 . . ? C7 C8 C3 117.2(2) . . ? C7 C8 Si2 121.01(19) . . ? C3 C8 Si2 121.82(17) . . ? C9 Si1 C10 110.55(12) . . ? C9 Si1 C11 106.94(13) . . ? C10 Si1 C11 109.20(12) . . ? C9 Si1 C4 111.30(11) . . ? C10 Si1 C4 111.34(11) . . ? C11 Si1 C4 107.35(11) . . ? 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 . . ? C12 Si2 C14 109.92(15) . . ? C12 Si2 C13 107.88(14) . . ? C14 Si2 C13 108.63(16) . . ? C12 Si2 C8 111.73(14) . . ? C14 Si2 C8 109.58(12) . . ? C13 Si2 C8 109.02(13) . . ? 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 . . ? C16 C15 V1 170.33(19) . . ? C15 C16 C17 177.2(2) . . ? C22 C17 C18 122.1(2) . . ? C22 C17 C16 119.6(2) . . ? C18 C17 C16 118.4(2) . . ? C19 C18 C17 117.6(2) . . ? C19 C18 Si3 120.6(2) . . ? C17 C18 Si3 121.77(17) . . ? C20 C19 C18 121.1(3) . . ? C20 C19 H19A 119.5 . . ? C18 C19 H19A 119.5 . . ? C21 C20 C19 120.5(2) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C22 121.7(3) . . ? C20 C21 H21A 119.1 . . ? C22 C21 H21A 119.1 . . ? C21 C22 C17 117.0(2) . . ? C21 C22 Si4 121.3(2) . . ? C17 C22 Si4 121.75(17) . . ? C25 Si3 C24 113.75(18) . . ? C25 Si3 C18 109.69(14) . . ? C24 Si3 C18 110.86(15) . . ? C25 Si3 C23 107.12(16) . . ? C24 Si3 C23 107.72(16) . . ? C18 Si3 C23 107.44(14) . . ? 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 . . ? C28 Si4 C27 111.44(16) . . ? C28 Si4 C26 110.14(13) . . ? C27 Si4 C26 106.62(13) . . ? C28 Si4 C22 108.73(13) . . ? C27 Si4 C22 111.21(12) . . ? C26 Si4 C22 108.64(13) . . ? 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 . . ? O1 Li1 O1 110.9(3) . 7 ? O1 Li1 O2 111.12(9) . 7 ? O1 Li1 O2 109.87(9) 7 7 ? O1 Li1 O2 109.87(9) . . ? O1 Li1 O2 111.12(9) 7 . ? O2 Li1 O2 103.8(3) 7 . ? C29 O1 C32 107.8(2) . . ? C29 O1 Li1 125.71(19) . . ? C32 O1 Li1 126.4(2) . . ? O1 C29 C30 105.2(2) . . ? O1 C29 H29A 110.7 . . ? C30 C29 H29A 110.7 . . ? O1 C29 H29B 110.7 . . ? C30 C29 H29B 110.7 . . ? H29A C29 H29B 108.8 . . ? C29 C30 C31 101.5(2) . . ? C29 C30 H30A 111.5 . . ? C31 C30 H30A 111.5 . . ? C29 C30 H30B 111.5 . . ? C31 C30 H30B 111.5 . . ? H30A C30 H30B 109.3 . . ? C30 C31 C32 104.2(2) . . ? C30 C31 H31A 110.9 . . ? C32 C31 H31A 110.9 . . ? C30 C31 H31B 110.9 . . ? C32 C31 H31B 110.9 . . ? H31A C31 H31B 108.9 . . ? O1 C32 C31 106.4(2) . . ? O1 C32 H32A 110.5 . . ? C31 C32 H32A 110.5 . . ? O1 C32 H32B 110.5 . . ? C31 C32 H32B 110.5 . . ? H32A C32 H32B 108.6 . . ? C33 O2 C36 108.0(3) . . ? C33 O2 Li1 125.7(2) . . ? C36 O2 Li1 125.3(3) . . ? O2 C33 C34 106.1(3) . . ? O2 C33 H33A 110.5 . . ? C34 C33 H33A 110.5 . . ? O2 C33 H33B 110.5 . . ? C34 C33 H33B 110.5 . . ? H33A C33 H33B 108.7 . . ? C35 C34 C33 104.3(3) . . ? C35 C34 H34A 110.9 . . ? C33 C34 H34A 110.9 . . ? C35 C34 H34B 110.9 . . ? C33 C34 H34B 110.9 . . ? H34A C34 H34B 108.9 . . ? C34 C35 C36 104.3(3) . . ? C34 C35 H35A 110.9 . . ? C36 C35 H35A 110.9 . . ? C34 C35 H35B 110.9 . . ? C36 C35 H35B 110.9 . . ? H35A C35 H35B 108.9 . . ? O2 C36 C35 107.5(4) . . ? O2 C36 H36A 110.2 . . ? C35 C36 H36A 110.2 . . ? O2 C36 H36B 110.2 . . ? C35 C36 H36B 110.2 . . ? H36A C36 H36B 108.5 . . ? 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 C1 V1 C1 C2 -60.2(10) 7_645 . . . ? C15 V1 C1 C2 64.2(10) . . . . ? C15 V1 C1 C2 -178.2(10) 7_645 . . . ? C8 C3 C4 C5 1.0(3) . . . . ? C2 C3 C4 C5 -177.06(19) . . . . ? C8 C3 C4 Si1 -179.58(17) . . . . ? C2 C3 C4 Si1 2.3(3) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? Si1 C4 C5 C6 -179.65(17) . . . . ? C4 C5 C6 C7 -0.8(3) . . . . ? C5 C6 C7 C8 1.2(4) . . . . ? C6 C7 C8 C3 -0.5(4) . . . . ? C6 C7 C8 Si2 179.69(19) . . . . ? C4 C3 C8 C7 -0.7(3) . . . . ? C2 C3 C8 C7 177.4(2) . . . . ? C4 C3 C8 Si2 179.15(16) . . . . ? C2 C3 C8 Si2 -2.8(3) . . . . ? C5 C4 Si1 C9 118.93(19) . . . . ? C3 C4 Si1 C9 -60.4(2) . . . . ? C5 C4 Si1 C10 -117.24(18) . . . . ? C3 C4 Si1 C10 63.4(2) . . . . ? C5 C4 Si1 C11 2.2(2) . . . . ? C3 C4 Si1 C11 -177.13(18) . . . . ? C7 C8 Si2 C12 125.8(2) . . . . ? C3 C8 Si2 C12 -54.0(2) . . . . ? C7 C8 Si2 C14 -112.1(2) . . . . ? C3 C8 Si2 C14 68.1(2) . . . . ? C7 C8 Si2 C13 6.7(2) . . . . ? C3 C8 Si2 C13 -173.2(2) . . . . ? C22 C17 C18 C19 1.0(3) . . . . ? C16 C17 C18 C19 -179.8(2) . . . . ? C22 C17 C18 Si3 179.30(18) . . . . ? C16 C17 C18 Si3 -1.5(3) . . . . ? C17 C18 C19 C20 -0.4(4) . . . . ? Si3 C18 C19 C20 -178.8(2) . . . . ? C18 C19 C20 C21 -0.4(4) . . . . ? C19 C20 C21 C22 0.7(4) . . . . ? C20 C21 C22 C17 -0.1(4) . . . . ? C20 C21 C22 Si4 -178.7(2) . . . . ? C18 C17 C22 C21 -0.7(3) . . . . ? C16 C17 C22 C21 -179.9(2) . . . . ? C18 C17 C22 Si4 177.86(17) . . . . ? C16 C17 C22 Si4 -1.3(3) . . . . ? C19 C18 Si3 C25 117.4(2) . . . . ? C17 C18 Si3 C25 -60.8(2) . . . . ? C19 C18 Si3 C24 -116.1(2) . . . . ? C17 C18 Si3 C24 65.6(2) . . . . ? C19 C18 Si3 C23 1.3(3) . . . . ? C17 C18 Si3 C23 -176.9(2) . . . . ? C21 C22 Si4 C28 115.5(2) . . . . ? C17 C22 Si4 C28 -63.0(2) . . . . ? C21 C22 Si4 C27 -121.4(2) . . . . ? C17 C22 Si4 C27 60.1(2) . . . . ? C21 C22 Si4 C26 -4.3(2) . . . . ? C17 C22 Si4 C26 177.15(19) . . . . ? O1 Li1 O1 C29 36.42(18) 7 . . . ? O2 Li1 O1 C29 158.9(2) 7 . . . ? O2 Li1 O1 C29 -86.8(3) . . . . ? O1 Li1 O1 C32 -141.0(2) 7 . . . ? O2 Li1 O1 C32 -18.5(3) 7 . . . ? O2 Li1 O1 C32 95.7(2) . . . . ? C32 O1 C29 C30 31.0(3) . . . . ? Li1 O1 C29 C30 -146.8(2) . . . . ? O1 C29 C30 C31 -39.0(3) . . . . ? C29 C30 C31 C32 32.1(3) . . . . ? C29 O1 C32 C31 -9.9(3) . . . . ? Li1 O1 C32 C31 167.9(2) . . . . ? C30 C31 C32 O1 -14.6(3) . . . . ? O1 Li1 O2 C33 -2.3(4) . . . . ? O1 Li1 O2 C33 -125.4(3) 7 . . . ? O2 Li1 O2 C33 116.6(3) 7 . . . ? O1 Li1 O2 C36 -168.9(3) . . . . ? O1 Li1 O2 C36 68.0(4) 7 . . . ? O2 Li1 O2 C36 -50.0(3) 7 . . . ? C36 O2 C33 C34 22.4(4) . . . . ? Li1 O2 C33 C34 -146.2(3) . . . . ? O2 C33 C34 C35 -31.6(5) . . . . ? C33 C34 C35 C36 28.0(5) . . . . ? C33 O2 C36 C35 -4.5(5) . . . . ? Li1 O2 C36 C35 164.1(3) . . . . ? C34 C35 C36 O2 -15.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 68.57 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.431 _refine_diff_density_min -0.176 _refine_diff_density_rms 0.042