# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2312 data_global # SUBMISSION DETAILS _publ_contact_author_name 'Dr P.L. Arnold' _publ_contact_author_address ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England UK ; _publ_contact_author_email Polly.Arnold@nottingham.ac.uk _publ_contact_author_fax '0115 951 3563' _publ_contact_author_phone '0115 951 3437' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' #=========================================================================== === # TITLE AND AUTHOR LIST _publ_section_title ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Arnold, Polly L.' #<--'Last name, first name' ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England UK ; 'Blake, Alexander J.' #<--'Last name, first name' ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England UK ; 'Hall, Sarah N.' #<--'Last name, first name' ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England UK ; 'Ward, Benjamin D.' #<--'Last name, first name' ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England UK ; 'Wilson, Claire' #<--'Last name, first name' ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England UK ; ## Data blocks for individual structures follow. These are to be ## separated by a line containing only the string #=== END ## The file should also be terminated by the same string. ## =========================================================== data_cysioh _exptl_special_details ; Crystals were grown at -30 deg C from a concentrated pentane solution of CYSIOH. A crystal was mounted in a film of RS3000 perfluoropolyether on a dual-stage glass fibre and transferred to the diffractometer. ; _refine_special_details ; Positional disorder of some cyclopentyl groups was identified and modelled, and the partial atoms refined as isotropic. Hydroxyl H atoms were not located and H atoms on pivot atoms for disorder components were not placed. Other H atoms were placed geometrically. Apparently isolated hydrogen atoms H70E, H70F, H70G, H70K, H70L, H70M, H70N, H70O and H70P, and H73B derive from different disorder components. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 99002 _chemical_melting_point 200-202 _chemical_formula_moiety 'C41 H80 O12 Si8' _chemical_formula_sum 'C41 H80 O12 Si8' _chemical_formula_weight 989.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 22.0658(10) _cell_length_b 17.1093(8) _cell_length_c 29.2595(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.651(2) _cell_angle_gamma 90.00 _cell_volume 10636.8(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 41673 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4272 _exptl_absorpt_coefficient_mu 0.255 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details 'SHELXTL version 5.1 (Bruker, 1997)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enraf Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius kappaCCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 39063 _diffrn_reflns_av_R_equivalents 0.1129 _diffrn_reflns_av_sigmaI/netI 0.1602 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15030 _reflns_number_gt 7633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL; PLATON (Spek, 2000)' _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^)+(0.1152P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _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 0.00(16) _refine_ls_number_reflns 15030 _refine_ls_number_parameters 1069 _refine_ls_number_restraints 831 _refine_ls_R_factor_all 0.173 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.2153 _refine_ls_wR_factor_gt 0.1690 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.179 _refine_ls_shift/su_mean 0.008 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.10128(13) 0.36808(16) 0.67943(8) 0.0457(7) Uani 1 1 d U . . Si2 Si 0.17056(15) 0.13959(16) 0.80749(9) 0.0531(8) Uani 1 1 d U B . Si3 Si 0.17431(13) 0.48479(15) 0.75843(8) 0.0439(7) Uani 1 1 d U . . Si4 Si 0.06988(14) 0.26558(16) 0.75887(9) 0.0488(7) Uani 1 1 d U . . Si5 Si 0.14331(13) 0.38533(16) 0.83567(8) 0.0465(7) Uani 1 1 d U C . Si6 Si 0.29347(12) 0.38555(16) 0.76311(8) 0.0468(7) Uani 1 1 d DU . . Si7 Si 0.26037(13) 0.28106(16) 0.84073(9) 0.0495(7) Uani 1 1 d U . . Si21 Si 0.42511(14) 0.26412(17) 0.56051(9) 0.0523(7) Uani 1 1 d U . . Si22 Si 0.37300(13) 0.20335(17) 0.64399(8) 0.0495(7) Uani 1 1 d U . . Si23 Si 0.34514(13) 0.13892(16) 0.49417(8) 0.0467(7) Uani 1 1 d U . . Si24 Si 0.23518(16) 0.26176(19) 0.46711(9) 0.0660(9) Uani 1 1 d U I . Si25 Si 0.29316(13) 0.07909(16) 0.57504(8) 0.0462(7) Uani 1 1 d U . . Si26 Si 0.33216(19) 0.39331(18) 0.50577(10) 0.0766(10) Uani 1 1 d U . . Si27 Si 0.17863(14) 0.1967(2) 0.54661(9) 0.0633(9) Uani 1 1 d U L . O1 O 0.1585(3) 0.3386(4) 0.6588(2) 0.0577(17) Uani 1 1 d U . . O2 O 0.2795(3) 0.3523(5) 0.7098(2) 0.076(2) Uani 1 1 d U D . O3 O 0.0825(3) 0.2973(3) 0.70987(18) 0.0490(16) Uani 1 1 d U . . O4 O 0.0908(3) 0.3316(3) 0.79969(19) 0.0480(15) Uani 1 1 d U . . O5 O 0.1109(3) 0.1875(4) 0.7751(2) 0.0553(17) Uani 1 1 d U . . O6 O 0.1275(3) 0.4408(3) 0.71504(18) 0.0487(15) Uani 1 1 d U . . O7 O 0.2303(3) 0.1968(4) 0.8232(2) 0.0665(18) Uani 1 1 d U B . O9 O 0.2809(4) 0.3192(4) 0.7969(2) 0.081(2) Uani 1 1 d U D . O17 O 0.2444(3) 0.4574(4) 0.7623(2) 0.0555(16) Uani 1 1 d U D . O20 O 0.1913(3) 0.2394(5) 0.5004(2) 0.083(2) Uani 1 1 d U . . O21 O 0.1957(3) 0.2573(4) 0.59173(19) 0.0612(18) Uani 1 1 d U . . O22 O 0.3171(3) 0.2641(4) 0.6487(2) 0.0657(18) Uani 1 1 d U . . O23 O 0.3385(3) 0.1241(4) 0.61954(19) 0.0562(17) Uani 1 1 d U . . O24 O 0.4119(3) 0.2424(4) 0.6099(2) 0.0618(17) Uani 1 1 d U . . O26 O 0.2253(3) 0.1225(4) 0.5607(2) 0.0595(17) Uani 1 1 d U . . O27 O 0.3167(4) 0.4651(4) 0.5349(2) 0.083(2) Uani 1 1 d U K . O28 O 0.2714(4) 0.3422(5) 0.4864(3) 0.103(3) Uani 1 1 d U I . O29 O 0.3867(3) 0.3407(4) 0.5398(2) 0.0670(18) Uani 1 1 d U K . O30 O 0.3232(3) 0.0821(3) 0.53061(19) 0.0497(15) Uani 1 1 d U . . O31 O 0.2862(3) 0.1936(4) 0.46844(19) 0.0572(17) Uani 1 1 d U . . O32 O 0.4022(3) 0.1929(4) 0.52276(19) 0.0517(16) Uani 1 1 d U . . O51 O 0.1574(3) 0.4615(3) 0.80715(19) 0.0508(16) Uani 1 1 d U . . O91 O 0.2073(3) 0.3347(4) 0.8545(2) 0.0571(17) Uani 1 1 d U C . O200 O 0.1869(3) 0.0691(3) 0.77709(19) 0.0557(17) Uani 1 1 d U . . C10 C 0.0344(5) 0.3999(4) 0.6309(2) 0.056(2) Uani 1 1 d DU A . H10A H -0.0033 0.4053 0.6434 0.067 Uiso 1 1 calc R . . C11 C 0.0458(5) 0.4783(5) 0.6090(3) 0.072(3) Uani 1 1 d DU A . H11A H 0.0253 0.5212 0.6220 0.086 Uiso 1 1 calc R . . H11B H 0.0915 0.4893 0.6165 0.086 Uiso 1 1 calc R . . C12 C 0.0183(6) 0.4730(8) 0.5557(3) 0.106(5) Uani 1 1 d DU . . C13 C -0.004(4) 0.3913(12) 0.5434(5) 0.37(7) Uiso 0.39(4) 1 d PDU A 1 H13A H 0.0145 0.3704 0.5184 0.450 Uiso 0.39(4) 1 calc PR A 1 H13B H -0.0501 0.3898 0.5315 0.450 Uiso 0.39(4) 1 calc PR A 1 C17 C 0.0352(9) 0.3846(8) 0.5474(4) 0.056(8) Uiso 0.61(4) 1 d PDU A 2 H17A H 0.0097 0.3649 0.5163 0.067 Uiso 0.61(4) 1 calc PR A 2 H17B H 0.0804 0.3785 0.5493 0.067 Uiso 0.61(4) 1 calc PR A 2 C14 C 0.0182(5) 0.3431(6) 0.5884(3) 0.084(4) Uani 1 1 d DU . . C20 C 0.1560(7) 0.1000(7) 0.8615(4) 0.089(4) Uani 1 1 d DU . . C21 C 0.144(3) 0.0185(13) 0.8746(14) 0.115(19) Uiso 0.31(2) 1 d PDU B 1 H21A H 0.1810 -0.0154 0.8753 0.138 Uiso 0.31(2) 1 calc PR B 1 H21B H 0.1066 -0.0037 0.8521 0.138 Uiso 0.31(2) 1 calc PR B 1 C22 C 0.135(2) 0.027(2) 0.9242(12) 0.106(19) Uiso 0.31(2) 1 d PDU B 1 H22A H 0.1755 0.0269 0.9487 0.127 Uiso 0.31(2) 1 calc PR B 1 H22B H 0.1086 -0.0165 0.9308 0.127 Uiso 0.31(2) 1 calc PR B 1 C25 C 0.1063(8) 0.0383(9) 0.8517(5) 0.071(6) Uiso 0.69(2) 1 d PDU B 2 H25A H 0.1247 -0.0130 0.8471 0.085 Uiso 0.69(2) 1 calc PR B 2 H25B H 0.0728 0.0512 0.8225 0.085 Uiso 0.69(2) 1 calc PR B 2 C26 C 0.0795(10) 0.0354(9) 0.8939(6) 0.101(8) Uiso 0.69(2) 1 d PDU B 2 H26A H 0.0954 -0.0113 0.9134 0.122 Uiso 0.69(2) 1 calc PR B 2 H26B H 0.0330 0.0323 0.8831 0.122 Uiso 0.69(2) 1 calc PR B 2 C23 C 0.0994(7) 0.1089(7) 0.9230(4) 0.106(5) Uani 1 1 d DU . . C24 C 0.1302(6) 0.1581(6) 0.8919(3) 0.086(4) Uani 1 1 d DU B . H24A H 0.1648 0.1901 0.9118 0.103 Uiso 1 1 calc R . . H24B H 0.0989 0.1935 0.8714 0.103 Uiso 1 1 calc R . . C30 C 0.1690(4) 0.5919(6) 0.7509(3) 0.051(2) Uani 1 1 d DU . . H30A H 0.1256 0.6085 0.7509 0.061 Uiso 1 1 calc R . . C31 C 0.1820(6) 0.6218(6) 0.7062(3) 0.077(3) Uani 1 1 d DU . . H31A H 0.2152 0.5900 0.6982 0.092 Uiso 1 1 calc R . . H31B H 0.1435 0.6187 0.6794 0.092 Uiso 1 1 calc R . . C32 C 0.2030(6) 0.7041(6) 0.7146(4) 0.083(4) Uani 1 1 d DU . . H32A H 0.1696 0.7402 0.6971 0.100 Uiso 1 1 calc R . . H32B H 0.2414 0.7132 0.7040 0.100 Uiso 1 1 calc R . . C33 C 0.2162(6) 0.7168(6) 0.7668(4) 0.088(4) Uani 1 1 d DU . . H33A H 0.2579 0.7415 0.7795 0.106 Uiso 1 1 calc R . . H33B H 0.1837 0.7509 0.7740 0.106 Uiso 1 1 calc R . . C34 C 0.2149(6) 0.6389(6) 0.7875(3) 0.073(3) Uani 1 1 d DU . . H34A H 0.2013 0.6422 0.8170 0.087 Uiso 1 1 calc R . . H34B H 0.2572 0.6147 0.7950 0.087 Uiso 1 1 calc R . . C40 C -0.0141(4) 0.2459(5) 0.7489(3) 0.051(2) Uani 1 1 d DU . . H40A H -0.0251 0.1989 0.7279 0.061 Uiso 1 1 calc R . . C41 C -0.0342(5) 0.2304(8) 0.7942(3) 0.084(4) Uani 1 1 d DU . . H41A H -0.0225 0.1769 0.8063 0.101 Uiso 1 1 calc R . . H41B H -0.0146 0.2685 0.8194 0.101 Uiso 1 1 calc R . . C42 C -0.1048(5) 0.2402(8) 0.7788(4) 0.100(4) Uani 1 1 d DU . . H42A H -0.1207 0.2552 0.8062 0.119 Uiso 1 1 calc R . . H42B H -0.1254 0.1908 0.7653 0.119 Uiso 1 1 calc R . . C43 C -0.1183(5) 0.3042(7) 0.7415(4) 0.088(4) Uani 1 1 d DU . . H43A H -0.1286 0.3540 0.7550 0.105 Uiso 1 1 calc R . . H43B H -0.1539 0.2894 0.7142 0.105 Uiso 1 1 calc R . . C44 C -0.0575(4) 0.3122(6) 0.7263(4) 0.071(3) Uani 1 1 d DU . . H44A H -0.0668 0.3093 0.6913 0.085 Uiso 1 1 calc R . . H44B H -0.0373 0.3631 0.7369 0.085 Uiso 1 1 calc R . . C50 C 0.1144(5) 0.4175(5) 0.8859(3) 0.056(3) Uani 1 1 d DU . . C51 C 0.0999(7) 0.3611(8) 0.9181(5) 0.054(4) Uiso 0.647(10) 1 d PDU C 1 H51A H 0.1388 0.3388 0.9393 0.065 Uiso 0.647(10) 1 calc PR C 1 H51B H 0.0735 0.3182 0.9006 0.065 Uiso 0.647(10) 1 calc PR C 1 C52 C 0.0625(9) 0.4117(10) 0.9471(6) 0.077(5) Uiso 0.647(10) 1 d PDU C 1 H52A H 0.0256 0.3818 0.9506 0.093 Uiso 0.647(10) 1 calc PR C 1 H52B H 0.0901 0.4226 0.9792 0.093 Uiso 0.647(10) 1 calc PR C 1 C55 C 0.1604(11) 0.4574(17) 0.9236(8) 0.066(9) Uiso 0.353(10) 1 d PDU C 2 H55C H 0.1805 0.5021 0.9119 0.079 Uiso 0.353(10) 1 calc PR C 2 H55D H 0.1930 0.4215 0.9423 0.079 Uiso 0.353(10) 1 calc PR C 2 C56 C 0.1117(13) 0.484(3) 0.9517(8) 0.117(15) Uiso 0.353(10) 1 d PDU C 2 H56C H 0.1159 0.4487 0.9791 0.140 Uiso 0.353(10) 1 calc PR C 2 H56D H 0.1234 0.5372 0.9644 0.140 Uiso 0.353(10) 1 calc PR C 2 C53 C 0.0415(7) 0.4854(8) 0.9226(5) 0.101(4) Uani 1 1 d U . . C54 C 0.0544(5) 0.4655(7) 0.8735(4) 0.080(3) Uani 1 1 d DU C . H54A H 0.0191 0.4352 0.8532 0.095 Uiso 1 1 calc R . . H54B H 0.0601 0.5140 0.8566 0.095 Uiso 1 1 calc R . . C60 C 0.3753(4) 0.4220(8) 0.7841(6) 0.112(14) Uiso 0.73(3) 1 d PDU D 1 C61 C 0.4249(6) 0.3686(7) 0.7736(5) 0.074(6) Uiso 0.73(3) 1 d PDU D 1 H61A H 0.4057 0.3348 0.7461 0.089 Uiso 0.73(3) 1 calc PR D 1 H61B H 0.4431 0.3347 0.8013 0.089 Uiso 0.73(3) 1 calc PR D 1 C62 C 0.4765(8) 0.4192(11) 0.7628(11) 0.157(11) Uiso 0.73(3) 1 d PDU D 1 H62A H 0.4811 0.4074 0.7307 0.189 Uiso 0.73(3) 1 calc PR D 1 H62B H 0.5174 0.4097 0.7864 0.189 Uiso 0.73(3) 1 calc PR D 1 C69 C 0.3754(5) 0.4224(7) 0.7836(6) 0.016(13) Uiso 0.27(3) 1 d PDU D 2 C65 C 0.4391(7) 0.391(4) 0.812(3) 0.36(9) Uiso 0.27(3) 1 d PDU D 2 H65A H 0.4439 0.3353 0.8037 0.437 Uiso 0.27(3) 1 calc PR D 2 H65B H 0.4428 0.3937 0.8466 0.437 Uiso 0.27(3) 1 calc PR D 2 C66 C 0.4897(5) 0.441(2) 0.800(2) 0.11(2) Uiso 0.27(3) 1 d PDU D 2 H66A H 0.5173 0.4653 0.8285 0.130 Uiso 0.27(3) 1 calc PR D 2 H66B H 0.5159 0.4093 0.7841 0.130 Uiso 0.27(3) 1 calc PR D 2 C63 C 0.4552(6) 0.5050(11) 0.7655(7) 0.160(8) Uani 1 1 d DU . . C64 C 0.3859(5) 0.5017(6) 0.7636(4) 0.093(4) Uani 1 1 d DU D . H64A H 0.3596 0.5069 0.7305 0.112 Uiso 1 1 calc R E 1 H64B H 0.3749 0.5445 0.7828 0.112 Uiso 1 1 calc R E 1 C70 C 0.3281(5) 0.2700(7) 0.8916(3) 0.078(3) Uani 1 1 d U D . H70A H 0.3443 0.3238 0.9014 0.094 Uiso 1 1 calc R . . C71 C 0.3194(6) 0.2296(9) 0.9358(3) 0.102(4) Uani 1 1 d U . . H71A H 0.3002 0.2657 0.9544 0.122 Uiso 1 1 calc R D . H71B H 0.2921 0.1830 0.9271 0.122 Uiso 1 1 calc R . . C72 C 0.3848(7) 0.2063(10) 0.9640(4) 0.123(5) Uani 1 1 d U D . H72A H 0.4030 0.2466 0.9881 0.147 Uiso 1 1 calc R . . H72B H 0.3837 0.1559 0.9804 0.147 Uiso 1 1 calc R . . C73 C 0.4224(7) 0.1992(11) 0.9298(5) 0.138(6) Uani 1 1 d U . . H73A H 0.4363 0.1444 0.9284 0.165 Uiso 1 1 calc R D . H73B H 0.4602 0.2328 0.9395 0.165 Uiso 1 1 calc R . . C74 C 0.3815(6) 0.2246(9) 0.8813(4) 0.105(5) Uani 1 1 d U D . H74A H 0.4058 0.2578 0.8649 0.126 Uiso 1 1 calc R . . H74B H 0.3654 0.1785 0.8612 0.126 Uiso 1 1 calc R . . C210 C 0.5102(5) 0.2803(6) 0.5691(3) 0.065(3) Uani 1 1 d DU F . H21C H 0.5219 0.3280 0.5893 0.077 Uiso 1 1 calc R . . C211 C 0.5309(5) 0.2945(8) 0.5238(4) 0.083(3) Uani 1 1 d DU . . C212 C 0.6007(6) 0.2747(14) 0.5391(7) 0.049(11) Uiso 0.48(6) 1 d PDU F 1 H21F H 0.6258 0.3220 0.5510 0.059 Uiso 0.48(6) 1 calc PR F 1 H21G H 0.6143 0.2537 0.5119 0.059 Uiso 0.48(6) 1 calc PR F 1 C216 C 0.585(2) 0.238(4) 0.5267(7) 0.182(19) Uiso 0.52(6) 1 d PDU F 2 H21H H 0.6190 0.2647 0.5159 0.218 Uiso 0.52(6) 1 calc PR F 2 H21I H 0.5707 0.1924 0.5062 0.218 Uiso 0.52(6) 1 calc PR F 2 C213 C 0.6102(6) 0.2131(9) 0.5785(4) 0.102(5) Uani 1 1 d DU . . C214 C 0.5517(5) 0.2135(8) 0.5950(4) 0.090(4) Uani 1 1 d U F . H21J H 0.5624 0.2218 0.6298 0.108 Uiso 1 1 calc R . . H21K H 0.5294 0.1630 0.5876 0.108 Uiso 1 1 calc R . . C220 C 0.4276(5) 0.1782(7) 0.7025(3) 0.063(3) Uani 1 1 d U G . H24C H 0.4500 0.2267 0.7170 0.076 Uiso 1 1 calc R . . C221 C 0.4762(5) 0.1170(8) 0.6993(3) 0.087(4) Uani 1 1 d DU . . C222 C 0.495(2) 0.089(3) 0.7509(8) 0.079(14) Uiso 0.41(7) 1 d PDU G 1 H24E H 0.4957 0.0312 0.7520 0.095 Uiso 0.41(7) 1 calc PR G 1 H24F H 0.5372 0.1087 0.7674 0.095 Uiso 0.41(7) 1 calc PR G 1 C223 C 0.4472(15) 0.119(5) 0.7756(7) 0.121(17) Uiso 0.41(7) 1 d PDU G 1 H24G H 0.4354 0.0775 0.7951 0.146 Uiso 0.41(7) 1 calc PR G 1 H24H H 0.4645 0.1641 0.7963 0.146 Uiso 0.41(7) 1 calc PR G 1 C226 C 0.4782(19) 0.058(2) 0.7393(14) 0.114(11) Uiso 0.59(7) 1 d PDU G 2 H24I H 0.4642 0.0061 0.7258 0.137 Uiso 0.59(7) 1 calc PR G 2 H24J H 0.5216 0.0536 0.7600 0.137 Uiso 0.59(7) 1 calc PR G 2 C227 C 0.4383(11) 0.086(2) 0.7651(11) 0.083(10) Uiso 0.59(7) 1 d PDU G 2 H24K H 0.4634 0.1105 0.7946 0.100 Uiso 0.59(7) 1 calc PR G 2 H24L H 0.4151 0.0410 0.7740 0.100 Uiso 0.59(7) 1 calc PR G 2 C224 C 0.3925(5) 0.1431(8) 0.7369(3) 0.084(4) Uani 1 1 d DU . . C230 C 0.3686(5) 0.0816(6) 0.4482(3) 0.056(2) Uani 1 1 d U H . H23C H 0.4080 0.0522 0.4636 0.068 Uiso 1 1 calc R . . C231 C 0.3808(6) 0.1332(6) 0.4068(3) 0.073(3) Uani 1 1 d DU . . C232 C 0.326(3) 0.117(3) 0.3634(16) 0.11(3) Uiso 0.24(4) 1 d PDU H 1 H23E H 0.2897 0.1515 0.3627 0.135 Uiso 0.24(4) 1 calc PR H 1 H23F H 0.3386 0.1239 0.3336 0.135 Uiso 0.24(4) 1 calc PR H 1 C233 C 0.311(2) 0.033(2) 0.3710(5) 0.029(12) Uiso 0.24(4) 1 d PDU H 1 H23G H 0.3413 -0.0020 0.3611 0.035 Uiso 0.24(4) 1 calc PR H 1 H23H H 0.2682 0.0199 0.3520 0.035 Uiso 0.24(4) 1 calc PR H 1 C236 C 0.3603(9) 0.0781(10) 0.3635(5) 0.084(7) Uiso 0.76(4) 1 d PDU H 2 H23I H 0.3281 0.1042 0.3378 0.100 Uiso 0.76(4) 1 calc PR H 2 H23J H 0.3970 0.0657 0.3514 0.100 Uiso 0.76(4) 1 calc PR H 2 C237 C 0.3342(14) 0.0054(14) 0.3775(7) 0.121(8) Uiso 0.76(4) 1 d PDU H 2 H23K H 0.3657 -0.0372 0.3822 0.145 Uiso 0.76(4) 1 calc PR H 2 H23L H 0.2964 -0.0109 0.3524 0.145 Uiso 0.76(4) 1 calc PR H 2 C234 C 0.3170(6) 0.0223(6) 0.4239(3) 0.072(3) Uani 1 1 d DU . . C240 C 0.1858(4) 0.2710(6) 0.4051(3) 0.072(3) Uani 1 1 d DU . . C241 C 0.1584(5) 0.1941(6) 0.3826(3) 0.086(4) Uani 1 1 d DU I . C242 C 0.0913(6) 0.2072(11) 0.3538(5) 0.103(6) Uiso 0.794(19) 1 d PDU I 1 H22C H 0.0888 0.2082 0.3195 0.123 Uiso 0.794(19) 1 calc PR I 1 H22D H 0.0639 0.1646 0.3597 0.123 Uiso 0.794(19) 1 calc PR I 1 C243 C 0.0707(6) 0.2841(11) 0.3690(9) 0.143(8) Uiso 0.794(19) 1 d PDU I 1 H22E H 0.0373 0.2761 0.3854 0.172 Uiso 0.794(19) 1 calc PR I 1 H22F H 0.0539 0.3181 0.3411 0.172 Uiso 0.794(19) 1 calc PR I 1 C244 C 0.1281(8) 0.3215(10) 0.4025(6) 0.101(6) Uiso 0.794(19) 1 d PDU I 1 H22G H 0.1214 0.3266 0.4345 0.121 Uiso 0.794(19) 1 calc PR I 1 H22H H 0.1346 0.3744 0.3910 0.121 Uiso 0.794(19) 1 calc PR I 1 C246 C 0.0855(16) 0.261(2) 0.3505(9) 0.017(11) Uiso 0.206(19) 1 d PDU I 2 H22I H 0.0936 0.2949 0.3254 0.020 Uiso 0.206(19) 1 calc PR I 2 H22J H 0.0456 0.2319 0.3388 0.020 Uiso 0.206(19) 1 calc PR I 2 C247 C 0.0912(19) 0.303(2) 0.3969(12) 0.039(14) Uiso 0.206(19) 1 d PDU I 2 H22K H 0.0975 0.2655 0.4235 0.046 Uiso 0.206(19) 1 calc PR I 2 H22L H 0.0534 0.3350 0.3955 0.046 Uiso 0.206(19) 1 calc PR I 2 C248 C 0.1495(15) 0.355(2) 0.4022(12) 0.030(12) Uiso 0.206(19) 1 d PDU I 2 H22M H 0.1614 0.3860 0.4318 0.036 Uiso 0.206(19) 1 calc PR I 2 H22N H 0.1493 0.3866 0.3739 0.036 Uiso 0.206(19) 1 calc PR I 2 C250 C 0.2850(4) -0.0217(5) 0.5914(3) 0.059(2) Uani 1 1 d DU J . H25C H 0.2662 -0.0213 0.6189 0.071 Uiso 1 1 calc R . . C251 C 0.3467(5) -0.0673(6) 0.6068(4) 0.085(4) Uani 1 1 d DU . . C252 C 0.3305(9) -0.1531(7) 0.5967(11) 0.101(11) Uiso 0.57(4) 1 d PDU J 1 H25E H 0.3612 -0.1784 0.5823 0.121 Uiso 0.57(4) 1 calc PR J 1 H25F H 0.3307 -0.1811 0.6263 0.121 Uiso 0.57(4) 1 calc PR J 1 C253 C 0.2664(10) -0.1540(9) 0.5631(11) 0.095(11) Uiso 0.57(4) 1 d PDU J 1 H25K H 0.2377 -0.1839 0.5774 0.114 Uiso 0.57(4) 1 calc PR J 1 H25L H 0.2681 -0.1811 0.5336 0.114 Uiso 0.57(4) 1 calc PR J 1 C256 C 0.3419(15) -0.136(3) 0.570(2) 0.17(2) Uiso 0.43(4) 1 d PDU J 2 H25I H 0.3746 -0.1301 0.5530 0.210 Uiso 0.43(4) 1 calc PR J 2 H25J H 0.3486 -0.1869 0.5871 0.210 Uiso 0.43(4) 1 calc PR J 2 C257 C 0.2782(12) -0.134(3) 0.5360(15) 0.149(19) Uiso 0.43(4) 1 d PDU J 2 H25G H 0.2573 -0.1856 0.5356 0.179 Uiso 0.43(4) 1 calc PR J 2 H25H H 0.2819 -0.1235 0.5036 0.179 Uiso 0.43(4) 1 calc PR J 2 C254 C 0.2401(6) -0.0716(6) 0.5508(4) 0.084(4) Uani 1 1 d DU . . C260 C 0.3871(12) 0.4402(12) 0.4653(6) 0.054(6) Uiso 0.430(7) 1 d PDU K 1 H26C H 0.4293 0.4533 0.4869 0.065 Uiso 0.430(7) 1 calc PR K 1 C261 C 0.3959(10) 0.3755(9) 0.4305(6) 0.035(5) Uiso 0.430(7) 1 d PDU K 1 H26D H 0.4365 0.3484 0.4435 0.042 Uiso 0.430(7) 1 calc PR K 1 H26E H 0.3616 0.3366 0.4259 0.042 Uiso 0.430(7) 1 calc PR K 1 C262 C 0.3949(17) 0.4111(15) 0.3871(7) 0.079(10) Uiso 0.430(7) 1 d PDU K 1 H26F H 0.3569 0.3957 0.3619 0.095 Uiso 0.430(7) 1 calc PR K 1 H26G H 0.4328 0.3974 0.3769 0.095 Uiso 0.430(7) 1 calc PR K 1 C263 C 0.394(2) 0.4913(17) 0.3976(11) 0.19(2) Uiso 0.430(7) 1 d PDU K 1 H26H H 0.3668 0.5200 0.3702 0.225 Uiso 0.430(7) 1 calc PR K 1 H26I H 0.4368 0.5133 0.4050 0.225 Uiso 0.430(7) 1 calc PR K 1 C264 C 0.3669(17) 0.4981(13) 0.4413(10) 0.108(11) Uiso 0.430(7) 1 d PDU K 1 H26J H 0.3818 0.5466 0.4593 0.129 Uiso 0.430(7) 1 calc PR K 1 H26K H 0.3203 0.4982 0.4314 0.129 Uiso 0.430(7) 1 calc PR K 1 C269 C 0.3510(13) 0.4281(12) 0.4528(6) 0.089(7) Uiso 0.570(7) 1 d PDU K 2 H26L H 0.3953 0.4468 0.4651 0.107 Uiso 0.570(7) 1 calc PR K 2 C265 C 0.3565(14) 0.3632(12) 0.4167(9) 0.118(9) Uiso 0.570(7) 1 d PDU K 2 H26S H 0.3912 0.3267 0.4311 0.142 Uiso 0.570(7) 1 calc PR K 2 H26T H 0.3168 0.3331 0.4063 0.142 Uiso 0.570(7) 1 calc PR K 2 C266 C 0.3689(17) 0.4031(15) 0.3783(9) 0.146(15) Uiso 0.570(7) 1 d PDU K 2 H26M H 0.3498 0.3759 0.3479 0.175 Uiso 0.570(7) 1 calc PR K 2 H26N H 0.4147 0.4087 0.3824 0.175 Uiso 0.570(7) 1 calc PR K 2 C267 C 0.3402(14) 0.4765(14) 0.3800(8) 0.128(10) Uiso 0.570(7) 1 d PDU K 2 H26O H 0.3011 0.4808 0.3537 0.154 Uiso 0.570(7) 1 calc PR K 2 H26P H 0.3690 0.5190 0.3765 0.154 Uiso 0.570(7) 1 calc PR K 2 C268 C 0.3247(15) 0.4835(13) 0.4283(9) 0.125(10) Uiso 0.570(7) 1 d PDU K 2 H26Q H 0.3406 0.5337 0.4438 0.150 Uiso 0.570(7) 1 calc PR K 2 H26R H 0.2787 0.4811 0.4238 0.150 Uiso 0.570(7) 1 calc PR K 2 C270 C 0.0955(5) 0.1728(6) 0.5301(3) 0.098(4) Uani 1 1 d DU . . C271 C 0.058(3) 0.138(3) 0.4823(4) 0.33(4) Uiso 0.64(3) 1 d PDU L 1 H27B H 0.0271 0.1768 0.4648 0.398 Uiso 0.64(3) 1 calc PR L 1 H27C H 0.0872 0.1251 0.4628 0.398 Uiso 0.64(3) 1 calc PR L 1 C272 C 0.0248(11) 0.0649(11) 0.4924(7) 0.095(9) Uiso 0.64(3) 1 d PDU L 1 H27D H -0.0213 0.0712 0.4802 0.114 Uiso 0.64(3) 1 calc PR L 1 H27E H 0.0377 0.0191 0.4765 0.114 Uiso 0.64(3) 1 calc PR L 1 C275 C 0.0798(10) 0.1191(9) 0.4862(4) 0.013(8) Uiso 0.36(3) 1 d PDU L 2 H27F H 0.0410 0.1375 0.4629 0.016 Uiso 0.36(3) 1 calc PR L 2 H27G H 0.1146 0.1196 0.4709 0.016 Uiso 0.36(3) 1 calc PR L 2 C276 C 0.070(2) 0.0364(9) 0.5028(9) 0.116(18) Uiso 0.36(3) 1 d PDU L 2 H27H H 0.0405 0.0062 0.4776 0.139 Uiso 0.36(3) 1 calc PR L 2 H27I H 0.1104 0.0077 0.5134 0.139 Uiso 0.36(3) 1 calc PR L 2 C273 C 0.0424(10) 0.0531(9) 0.5442(5) 0.223(12) Uani 1 1 d DU . . C274 C 0.0766(7) 0.1269(8) 0.5686(3) 0.119(5) Uani 1 1 d DU L . H27L H 0.0483 0.1584 0.5824 0.143 Uiso 1 1 calc R . . H27M H 0.1143 0.1123 0.5943 0.143 Uiso 1 1 calc R . . Si40 Si 0.19923(13) 0.04162(16) 0.72653(9) 0.0523(7) Uani 1 1 d DU . . C400 C 0.1327(4) -0.0217(5) 0.6964(3) 0.074(3) Uani 1 1 d DU . . C401 C 0.2045(5) 0.1292(5) 0.6905(3) 0.058(3) Uani 1 1 d DU . . H40B H 0.1650 0.1588 0.6843 0.087 Uiso 1 1 calc R . . H40C H 0.2118 0.1129 0.6603 0.087 Uiso 1 1 calc R . . H40D H 0.2394 0.1623 0.7078 0.087 Uiso 1 1 calc R . . C402 C 0.2735(5) -0.0174(6) 0.7398(3) 0.073(3) Uani 1 1 d DU . . H40E H 0.2691 -0.0631 0.7588 0.110 Uiso 1 1 calc R . . H40F H 0.3088 0.0148 0.7576 0.110 Uiso 1 1 calc R . . H40G H 0.2814 -0.0345 0.7100 0.110 Uiso 1 1 calc R . . C403 C 0.0703(4) 0.0256(6) 0.6837(4) 0.091(4) Uani 1 1 d DU . . H40H H 0.0354 -0.0085 0.6676 0.136 Uiso 1 1 calc R . . H40I H 0.0736 0.0692 0.6627 0.136 Uiso 1 1 calc R . . H40J H 0.0624 0.0462 0.7129 0.136 Uiso 1 1 calc R . . C404 C 0.1458(6) -0.0588(7) 0.6518(4) 0.105(4) Uani 1 1 d DU . . H40K H 0.1104 -0.0922 0.6359 0.158 Uiso 1 1 calc R . . H40L H 0.1843 -0.0902 0.6612 0.158 Uiso 1 1 calc R . . H40M H 0.1511 -0.0173 0.6301 0.158 Uiso 1 1 calc R . . C405 C 0.1253(6) -0.0878(6) 0.7303(4) 0.108(4) Uani 1 1 d DU . . H40N H 0.0863 -0.1166 0.7163 0.162 Uiso 1 1 calc R . . H40O H 0.1236 -0.0653 0.7607 0.162 Uiso 1 1 calc R . . H40P H 0.1612 -0.1235 0.7354 0.162 Uiso 1 1 calc R . . Si50 Si 0.2859(2) 0.5273(3) 0.56394(17) 0.062(2) Uiso 0.596(9) 1 d PDU K 1 C500 C 0.3517(5) 0.5788(7) 0.6054(4) 0.097(7) Uiso 0.596(9) 1 d PDU K 1 C501 C 0.2399(10) 0.5992(12) 0.5204(8) 0.154(11) Uiso 0.596(9) 1 d PDU K 1 H50A H 0.2677 0.6246 0.5038 0.231 Uiso 0.596(9) 1 calc PR K 1 H50B H 0.2220 0.6388 0.5372 0.231 Uiso 0.596(9) 1 calc PR K 1 H50C H 0.2059 0.5722 0.4973 0.231 Uiso 0.596(9) 1 calc PR K 1 C502 C 0.2373(6) 0.4759(9) 0.5978(5) 0.169(7) Uiso 0.596(9) 1 d PDU K 1 H50D H 0.2638 0.4393 0.6203 0.253 Uiso 0.596(9) 1 calc PR K 1 H50E H 0.2033 0.4472 0.5757 0.253 Uiso 0.596(9) 1 calc PR K 1 H50F H 0.2191 0.5143 0.6151 0.253 Uiso 0.596(9) 1 calc PR K 1 C503 C 0.3978(9) 0.5202(12) 0.6370(7) 0.172(13) Uiso 0.596(9) 1 d PDU K 1 H50G H 0.4323 0.5488 0.6586 0.259 Uiso 0.596(9) 1 calc PR K 1 H50H H 0.4149 0.4855 0.6169 0.259 Uiso 0.596(9) 1 calc PR K 1 H50I H 0.3755 0.4891 0.6554 0.259 Uiso 0.596(9) 1 calc PR K 1 C504 C 0.3243(6) 0.6389(7) 0.6340(4) 0.118(5) Uiso 0.596(9) 1 d PDU K 1 H50J H 0.3588 0.6666 0.6562 0.177 Uiso 0.596(9) 1 calc PR K 1 H50K H 0.2988 0.6115 0.6517 0.177 Uiso 0.596(9) 1 calc PR K 1 H50L H 0.2979 0.6765 0.6122 0.177 Uiso 0.596(9) 1 calc PR K 1 C505 C 0.3881(6) 0.6246(9) 0.5756(5) 0.159(7) Uiso 0.596(9) 1 d PDU K 1 H50M H 0.4233 0.6526 0.5969 0.238 Uiso 0.596(9) 1 calc PR K 1 H50N H 0.3597 0.6621 0.5552 0.238 Uiso 0.596(9) 1 calc PR K 1 H50O H 0.4042 0.5880 0.5560 0.238 Uiso 0.596(9) 1 calc PR K 1 Si70 Si 0.3143(3) 0.4973(4) 0.5856(2) 0.054(3) Uiso 0.404(9) 1 d PDU K 2 C700 C 0.3240(5) 0.6046(6) 0.5846(4) 0.038(6) Uiso 0.404(9) 1 d PDU K 2 C701 C 0.3825(7) 0.4544(11) 0.6309(7) 0.055(7) Uiso 0.404(9) 1 d PDU K 2 H70B H 0.4216 0.4673 0.6227 0.082 Uiso 0.404(9) 1 calc PR K 2 H70C H 0.3777 0.3975 0.6314 0.082 Uiso 0.404(9) 1 calc PR K 2 H70D H 0.3840 0.4758 0.6622 0.082 Uiso 0.404(9) 1 calc PR K 2 C702 C 0.2373(6) 0.4759(9) 0.5978(5) 0.169(7) Uiso 0.40 1 d PDU K 2 H70E H 0.2034 0.5009 0.5735 0.253 Uiso 0.404(9) 1 calc PR K 2 H70F H 0.2375 0.4964 0.6291 0.253 Uiso 0.404(9) 1 calc PR K 2 H70G H 0.2305 0.4193 0.5971 0.253 Uiso 0.404(9) 1 calc PR K 2 C703 C 0.2716(9) 0.6407(12) 0.5436(6) 0.080(9) Uiso 0.404(9) 1 d PDU K 2 H70H H 0.2770 0.6975 0.5434 0.120 Uiso 0.404(9) 1 calc PR K 2 H70I H 0.2303 0.6284 0.5483 0.120 Uiso 0.404(9) 1 calc PR K 2 H70J H 0.2744 0.6189 0.5133 0.120 Uiso 0.404(9) 1 calc PR K 2 C704 C 0.3243(6) 0.6389(7) 0.6340(4) 0.118(5) Uiso 0.40 1 d PDU K 2 H70K H 0.3314 0.6954 0.6341 0.177 Uiso 0.404(9) 1 calc PR K 2 H70L H 0.3580 0.6143 0.6586 0.177 Uiso 0.404(9) 1 calc PR K 2 H70M H 0.2837 0.6284 0.6404 0.177 Uiso 0.404(9) 1 calc PR K 2 C705 C 0.3881(6) 0.6246(9) 0.5756(5) 0.159(7) Uiso 0.40 1 d PDU K 2 H70N H 0.3939 0.6814 0.5767 0.238 Uiso 0.404(9) 1 calc PR K 2 H70O H 0.3889 0.6050 0.5443 0.238 Uiso 0.404(9) 1 calc PR K 2 H70P H 0.4219 0.6000 0.6001 0.238 Uiso 0.404(9) 1 calc PR K 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 Si1 0.0492(17) 0.0542(18) 0.0360(13) -0.0036(11) 0.0154(11) 0.0027(14) Si2 0.083(2) 0.0388(17) 0.0461(14) 0.0039(12) 0.0317(14) 0.0085(15) Si3 0.0500(17) 0.0424(16) 0.0422(13) -0.0008(11) 0.0175(12) 0.0001(14) Si4 0.0577(18) 0.0499(19) 0.0448(14) -0.0029(12) 0.0237(13) -0.0058(15) Si5 0.0576(18) 0.0523(18) 0.0346(13) -0.0016(11) 0.0209(12) 0.0045(14) Si6 0.0481(17) 0.0570(19) 0.0382(13) 0.0001(12) 0.0165(12) 0.0070(14) Si7 0.0588(19) 0.0483(19) 0.0441(14) 0.0061(12) 0.0183(13) 0.0108(15) Si21 0.0635(19) 0.0506(19) 0.0509(15) -0.0087(13) 0.0295(14) -0.0092(15) Si22 0.0480(17) 0.070(2) 0.0345(13) -0.0101(12) 0.0178(12) -0.0044(15) Si23 0.0600(18) 0.0498(18) 0.0339(12) -0.0035(11) 0.0187(12) 0.0034(14) Si24 0.085(2) 0.073(2) 0.0354(14) -0.0020(13) 0.0098(14) 0.0237(18) Si25 0.0535(18) 0.0503(18) 0.0393(13) -0.0045(12) 0.0203(12) -0.0065(14) Si26 0.130(3) 0.052(2) 0.0574(18) -0.0006(15) 0.0419(19) 0.020(2) Si27 0.0563(19) 0.096(3) 0.0375(14) -0.0158(14) 0.0117(13) 0.0195(17) O1 0.062(4) 0.063(5) 0.058(4) -0.003(3) 0.034(3) 0.005(4) O2 0.062(5) 0.119(6) 0.046(3) -0.019(4) 0.015(3) 0.028(4) O3 0.059(4) 0.049(4) 0.042(3) -0.001(3) 0.018(3) -0.007(3) O4 0.062(4) 0.039(4) 0.048(3) -0.004(3) 0.024(3) -0.003(3) O5 0.064(4) 0.047(4) 0.062(4) -0.001(3) 0.030(3) 0.012(3) O6 0.055(4) 0.050(4) 0.043(3) 0.002(3) 0.017(3) -0.004(3) O7 0.071(4) 0.048(4) 0.077(4) -0.007(3) 0.015(3) 0.008(3) O9 0.099(6) 0.078(5) 0.082(4) 0.033(4) 0.050(4) 0.032(4) O17 0.055(4) 0.049(4) 0.066(4) -0.001(3) 0.022(3) 0.008(3) O20 0.090(5) 0.129(6) 0.033(3) 0.008(3) 0.021(3) 0.050(4) O21 0.086(5) 0.057(4) 0.040(3) -0.004(3) 0.017(3) 0.014(4) O22 0.067(5) 0.073(5) 0.064(4) -0.014(3) 0.029(3) 0.003(4) O23 0.057(4) 0.073(4) 0.041(3) -0.014(3) 0.017(3) -0.003(3) O24 0.065(5) 0.072(5) 0.057(3) -0.017(3) 0.031(3) -0.008(4) O26 0.055(4) 0.070(4) 0.058(4) -0.020(3) 0.023(3) -0.001(3) O27 0.131(7) 0.059(5) 0.060(4) -0.013(3) 0.030(4) 0.030(4) O28 0.128(6) 0.069(5) 0.090(5) -0.024(4) -0.009(5) 0.022(4) O29 0.082(5) 0.055(4) 0.073(4) -0.008(3) 0.036(4) 0.003(4) O30 0.057(4) 0.049(4) 0.050(3) -0.008(3) 0.027(3) 0.003(3) O31 0.071(4) 0.063(4) 0.038(3) -0.003(3) 0.013(3) 0.023(3) O32 0.056(4) 0.057(4) 0.048(3) -0.009(3) 0.024(3) -0.008(3) O51 0.062(4) 0.051(4) 0.043(3) -0.002(3) 0.021(3) -0.001(3) O91 0.066(4) 0.058(4) 0.052(3) -0.003(3) 0.024(3) 0.012(3) O200 0.083(5) 0.043(4) 0.047(3) 0.006(3) 0.029(3) 0.014(3) C10 0.053(6) 0.070(7) 0.047(5) 0.004(4) 0.019(4) 0.013(5) C11 0.103(9) 0.065(6) 0.048(5) 0.003(4) 0.020(5) 0.021(6) C12 0.105(10) 0.148(11) 0.055(5) 0.045(7) 0.004(7) 0.031(10) C14 0.087(9) 0.098(7) 0.051(6) -0.009(5) -0.007(6) -0.006(7) C20 0.159(12) 0.068(8) 0.064(6) 0.003(5) 0.072(7) 0.005(7) C23 0.158(14) 0.089(10) 0.098(9) 0.014(7) 0.083(9) 0.001(9) C24 0.118(10) 0.104(9) 0.053(6) -0.001(6) 0.052(6) 0.007(8) C30 0.044(6) 0.055(5) 0.060(5) 0.005(4) 0.023(4) 0.003(4) C31 0.118(10) 0.050(6) 0.061(5) 0.012(4) 0.021(6) -0.010(7) C32 0.111(10) 0.054(7) 0.093(6) 0.001(5) 0.040(7) -0.013(7) C33 0.107(10) 0.059(7) 0.097(7) -0.014(5) 0.024(7) -0.001(7) C34 0.099(9) 0.056(6) 0.060(5) -0.020(4) 0.018(6) 0.004(6) C40 0.059(5) 0.035(6) 0.064(5) 0.012(4) 0.024(4) -0.013(4) C41 0.066(6) 0.122(11) 0.079(7) 0.024(6) 0.043(6) 0.007(7) C42 0.081(7) 0.117(12) 0.123(10) 0.029(8) 0.068(7) 0.043(8) C43 0.088(8) 0.082(9) 0.105(9) 0.004(6) 0.048(7) 0.026(7) C44 0.066(6) 0.058(7) 0.088(7) 0.009(5) 0.020(5) -0.002(5) C50 0.073(7) 0.049(7) 0.054(5) -0.016(4) 0.032(5) -0.001(5) C53 0.120(11) 0.108(11) 0.110(9) 0.003(8) 0.088(8) 0.033(9) C54 0.071(8) 0.084(9) 0.091(7) -0.028(6) 0.035(6) 0.004(6) C63 0.087(9) 0.156(17) 0.23(2) 0.032(15) 0.041(12) -0.030(12) C64 0.099(8) 0.078(9) 0.111(9) -0.010(7) 0.043(8) -0.024(7) C70 0.076(7) 0.098(9) 0.052(5) -0.014(5) 0.004(4) 0.021(6) C71 0.100(8) 0.159(13) 0.039(5) 0.002(6) 0.008(5) 0.034(9) C72 0.122(10) 0.170(15) 0.062(7) 0.024(8) -0.001(6) 0.036(11) C73 0.109(10) 0.206(18) 0.090(8) 0.066(11) 0.014(7) 0.059(11) C74 0.088(8) 0.163(13) 0.067(6) 0.030(8) 0.027(5) 0.055(8) C210 0.061(5) 0.071(8) 0.067(6) -0.019(5) 0.027(5) -0.014(5) C211 0.064(7) 0.115(10) 0.082(7) 0.012(6) 0.043(6) -0.005(7) C213 0.071(8) 0.164(14) 0.089(8) 0.032(8) 0.051(7) 0.020(8) C214 0.067(7) 0.126(11) 0.088(8) 0.021(7) 0.039(6) 0.002(7) C220 0.066(7) 0.086(8) 0.038(4) -0.013(4) 0.016(4) -0.002(5) C221 0.071(8) 0.129(11) 0.065(7) 0.017(7) 0.023(5) 0.042(7) C224 0.083(8) 0.122(11) 0.050(6) 0.025(6) 0.026(5) 0.029(7) C230 0.071(7) 0.064(7) 0.039(5) -0.008(4) 0.025(4) 0.009(5) C231 0.117(10) 0.068(8) 0.045(5) -0.018(5) 0.038(6) -0.019(7) C234 0.109(9) 0.077(8) 0.039(5) -0.020(5) 0.035(5) -0.020(6) C240 0.078(8) 0.093(8) 0.036(4) 0.004(5) -0.002(4) 0.031(6) C241 0.087(9) 0.109(9) 0.043(6) -0.008(6) -0.013(6) 0.007(7) C250 0.066(7) 0.067(5) 0.059(5) 0.003(4) 0.041(5) 0.003(5) C251 0.095(8) 0.046(7) 0.118(9) 0.008(6) 0.034(7) 0.013(6) C254 0.111(9) 0.046(7) 0.094(8) -0.011(6) 0.029(6) -0.011(6) C270 0.074(6) 0.173(12) 0.052(6) -0.047(6) 0.026(5) -0.006(6) C273 0.35(3) 0.122(15) 0.129(15) 0.004(11) -0.048(17) -0.058(15) C274 0.119(11) 0.145(14) 0.098(9) -0.013(8) 0.036(8) -0.021(9) Si40 0.0686(19) 0.0480(18) 0.0445(14) 0.0024(12) 0.0224(13) 0.0090(15) C400 0.078(6) 0.068(8) 0.092(7) -0.025(5) 0.048(6) -0.026(5) C401 0.071(7) 0.051(6) 0.053(5) 0.013(4) 0.018(5) 0.004(5) C402 0.085(7) 0.081(8) 0.060(6) 0.014(5) 0.029(5) 0.032(6) C403 0.062(6) 0.112(10) 0.101(9) -0.023(7) 0.028(6) -0.022(6) C404 0.135(11) 0.106(11) 0.089(7) -0.052(7) 0.054(8) -0.027(8) C405 0.157(13) 0.061(8) 0.138(10) -0.016(6) 0.096(10) -0.018(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O1 1.619(7) . YES Si1 O3 1.622(6) . YES Si1 O6 1.625(6) . Y Si1 C10 1.833(8) . ? Si2 O200 1.596(6) . Y Si2 O7 1.605(8) . Yes Si2 O5 1.622(7) . Yes Si2 C20 1.827(10) . ? Si3 O17 1.591(7) . Yes Si3 O6 1.593(6) . Yes Si3 O51 1.617(6) . Yes Si3 C30 1.846(10) . ? Si4 O5 1.612(7) . Yes Si4 O4 1.618(6) . Yes Si4 O3 1.626(6) . Yes Si4 C40 1.828(9) . ? Si5 O91 1.622(7) . Yes Si5 O51 1.623(6) . Yes Si5 O4 1.624(6) . Yes Si5 C50 1.837(9) . ? Si6 O9 1.578(7) . Yes Si6 O2 1.611(6) . Yes Si6 O17 1.633(7) . Yes Si6 C60 1.851(11) . ? Si6 C69 1.855(11) . ? Si7 O9 1.609(7) . Yes Si7 O7 1.612(7) . Yes Si7 O91 1.620(7) . Yes Si7 C70 1.812(10) . ? Si21 O29 1.589(7) . Yes Si21 O24 1.593(7) . Yes Si21 O32 1.631(6) . Yes Si21 C210 1.847(10) . ? Si22 O23 1.623(7) . Yes Si22 O24 1.625(7) . Yes Si22 O22 1.648(7) . Yes Si22 C220 1.859(9) . ? Si23 O32 1.603(7) . Yes Si23 O30 1.611(6) . Yes Si23 O31 1.614(7) . Yes Si23 C230 1.848(9) . ? Si24 O20 1.593(8) . Yes Si24 O31 1.614(7) . Yes Si24 O28 1.615(9) . Yes Si24 C240 1.854(8) . ? Si25 O23 1.608(6) . Yes Si25 O30 1.611(6) . Yes Si25 O26 1.623(7) . Yes Si25 C250 1.812(10) . ? Si26 O28 1.573(9) . Yes Si26 O27 1.585(7) . Yes Si26 O29 1.614(8) . Yes Si26 C269 1.810(17) . ? Si26 C260 2.07(2) . ? Si27 O26 1.616(7) . Yes Si27 O20 1.626(7) . Yes Si27 O21 1.640(6) . Yes Si27 C270 1.813(11) . ? O27 Si70 1.597(9) . Yes O27 Si50 1.620(8) . Yes O200 Si40 1.644(6) . Yes C10 C11 1.536(6) . ? C10 C14 1.543(7) . ? C11 C12 1.515(7) . ? C12 C13 1.492(16) . ? C12 C17 1.59(2) . ? C13 C14 1.518(10) . ? C17 C14 1.524(8) . ? C20 C21 1.487(15) . ? C20 C25 1.494(18) . ? C20 C24 1.541(14) . ? C21 C22 1.528(15) . ? C22 C23 1.60(4) . ? C25 C26 1.508(13) . ? C26 C23 1.515(13) . ? C23 C24 1.528(11) . ? C30 C34 1.494(11) . ? C30 C31 1.503(12) . ? C31 C32 1.482(12) . ? C32 C33 1.492(15) . ? C33 C34 1.468(12) . ? C40 C44 1.517(10) . ? C40 C41 1.532(10) . ? C41 C42 1.509(10) . ? C42 C43 1.519(11) . ? C43 C44 1.528(9) . ? C50 C51 1.444(14) . ? C50 C55 1.452(16) . ? C50 C54 1.515(14) . ? C51 C52 1.59(2) . ? C52 C53 1.463(19) . ? C55 C56 1.59(2) . ? C56 C53 1.55(3) . ? C53 C54 1.574(15) . ? C60 C61 1.520(8) . ? C60 C64 1.533(19) . ? C61 C62 1.531(10) . ? C62 C63 1.55(2) . ? C69 C64 1.519(12) . ? C69 C65 1.529(13) . ? C65 C66 1.536(10) . ? C66 C63 1.531(13) . ? C63 C64 1.517(11) . ? C70 C74 1.509(15) . ? C70 C71 1.525(16) . ? C71 C72 1.510(16) . ? C72 C73 1.468(19) . ? C73 C74 1.523(15) . ? C210 C214 1.531(15) . ? C210 C211 1.535(10) . ? C211 C216 1.521(8) . ? C211 C212 1.521(9) . ? C212 C213 1.535(12) . ? C216 C213 1.530(9) . ? C213 C214 1.495(15) . ? C220 C221 1.519(15) . ? C220 C224 1.548(15) . ? C221 C222 1.532(9) . ? C221 C226 1.534(17) . ? C222 C223 1.51(4) . ? C223 C224 1.47(2) . ? C226 C227 1.39(3) . ? C227 C224 1.491(18) . ? C230 C234 1.548(14) . ? C230 C231 1.579(14) . ? C231 C232 1.523(9) . ? C231 C236 1.546(14) . ? C232 C233 1.507(10) . ? C233 C234 1.531(9) . ? C236 C237 1.474(17) . ? C237 C234 1.535(16) . ? C240 C241 1.522(7) . ? C240 C244 1.524(12) . ? C240 C248 1.63(4) . ? C241 C242 1.510(11) . ? C241 C246 1.99(4) . ? C242 C243 1.499(14) . ? C243 C244 1.518(12) . ? C246 C247 1.510(17) . ? C247 C248 1.533(15) . ? C250 C251 1.527(10) . ? C250 C254 1.575(14) . ? C251 C252 1.521(8) . ? C251 C256 1.58(4) . ? C252 C253 1.488(14) . ? C253 C254 1.531(13) . ? C256 C257 1.489(16) . ? C257 C254 1.498(14) . ? C260 C264 1.23(2) . ? C260 C261 1.551(16) . ? C261 C262 1.404(15) . ? C262 C263 1.408(16) . ? C263 C264 1.554(17) . ? C269 C268 1.23(2) . ? C269 C265 1.560(16) . ? C265 C266 1.404(16) . ? C266 C267 1.413(16) . ? C267 C268 1.546(16) . ? C270 C274 1.523(8) . ? C270 C271 1.534(8) . ? C270 C275 1.540(9) . ? C271 C272 1.526(8) . ? C272 C273 1.47(2) . ? C275 C276 1.530(13) . ? C276 C273 1.522(9) . ? C273 C274 1.544(7) . ? Si40 C400 1.847(8) . ? Si40 C401 1.854(8) . ? Si40 C402 1.874(9) . ? C400 C405 1.542(6) . ? C400 C404 1.546(7) . ? C400 C403 1.555(7) . ? Si50 C500 1.846(10) . ? Si50 C501 1.863(11) . ? Si50 C502 1.864(11) . ? C500 C503 1.545(8) . ? C500 C505 1.547(8) . ? C500 C504 1.547(8) . ? Si70 C700 1.849(10) . ? Si70 C701 1.866(11) . ? C700 C703 1.551(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Si1 O3 108.2(4) . . ? O1 Si1 O6 107.4(3) . . ? O3 Si1 O6 108.6(3) . . ? O1 Si1 C10 110.4(4) . . ? O3 Si1 C10 112.1(4) . . ? O6 Si1 C10 110.0(3) . . ? O200 Si2 O7 109.2(4) . . ? O200 Si2 O5 109.0(3) . . ? O7 Si2 O5 109.5(4) . . ? O200 Si2 C20 108.8(4) . . ? O7 Si2 C20 107.5(5) . . ? O5 Si2 C20 112.8(5) . . ? O17 Si3 O6 109.0(4) . . ? O17 Si3 O51 108.4(3) . . ? O6 Si3 O51 109.4(3) . . ? O17 Si3 C30 109.3(4) . . ? O6 Si3 C30 111.6(4) . . ? O51 Si3 C30 109.1(4) . . ? O5 Si4 O4 109.6(3) . . ? O5 Si4 O3 108.7(4) . . ? O4 Si4 O3 109.6(3) . . ? O5 Si4 C40 111.0(4) . . ? O4 Si4 C40 108.8(4) . . ? O3 Si4 C40 109.2(3) . . ? O91 Si5 O51 109.5(4) . . ? O91 Si5 O4 108.7(3) . . ? O51 Si5 O4 108.9(3) . . ? O91 Si5 C50 110.4(4) . . ? O51 Si5 C50 109.1(4) . . ? O4 Si5 C50 110.3(4) . . ? O9 Si6 O2 109.4(4) . . ? O9 Si6 O17 108.8(4) . . ? O2 Si6 O17 107.3(3) . . ? O9 Si6 C60 110.8(6) . . ? O2 Si6 C60 110.8(5) . . ? O17 Si6 C60 109.5(5) . . ? O9 Si6 C69 111.3(6) . . ? O2 Si6 C69 110.4(6) . . ? O17 Si6 C69 109.5(5) . . ? C60 Si6 C69 0.5(9) . . ? O9 Si7 O7 106.8(4) . . ? O9 Si7 O91 110.2(4) . . ? O7 Si7 O91 108.8(4) . . ? O9 Si7 C70 110.5(5) . . ? O7 Si7 C70 110.2(5) . . ? O91 Si7 C70 110.2(4) . . ? O29 Si21 O24 109.1(4) . . ? O29 Si21 O32 108.8(4) . . ? O24 Si21 O32 110.0(4) . . ? O29 Si21 C210 110.3(5) . . ? O24 Si21 C210 109.8(4) . . ? O32 Si21 C210 108.8(4) . . ? O23 Si22 O24 109.6(3) . . ? O23 Si22 O22 106.9(4) . . ? O24 Si22 O22 108.8(4) . . ? O23 Si22 C220 108.8(4) . . ? O24 Si22 C220 110.0(4) . . ? O22 Si22 C220 112.6(4) . . ? O32 Si23 O30 109.7(3) . . ? O32 Si23 O31 109.3(4) . . ? O30 Si23 O31 108.0(4) . . ? O32 Si23 C230 110.5(4) . . ? O30 Si23 C230 110.8(4) . . ? O31 Si23 C230 108.5(4) . . ? O20 Si24 O31 110.3(4) . . ? O20 Si24 O28 108.4(5) . . ? O31 Si24 O28 109.4(5) . . ? O20 Si24 C240 109.0(4) . . ? O31 Si24 C240 107.9(4) . . ? O28 Si24 C240 111.9(4) . . ? O23 Si25 O30 109.7(3) . . ? O23 Si25 O26 108.6(3) . . ? O30 Si25 O26 109.2(3) . . ? O23 Si25 C250 109.1(4) . . ? O30 Si25 C250 109.6(4) . . ? O26 Si25 C250 110.7(4) . . ? O28 Si26 O27 109.8(5) . . ? O28 Si26 O29 109.5(4) . . ? O27 Si26 O29 109.4(4) . . ? O28 Si26 C269 104.1(9) . . ? O27 Si26 C269 109.8(7) . . ? O29 Si26 C269 114.0(8) . . ? O28 Si26 C260 125.7(7) . . ? O27 Si26 C260 104.6(6) . . ? O29 Si26 C260 96.6(7) . . ? C269 Si26 C260 22.8(8) . . ? O26 Si27 O20 108.9(4) . . ? O26 Si27 O21 107.4(3) . . ? O20 Si27 O21 109.4(4) . . ? O26 Si27 C270 114.8(5) . . ? O20 Si27 C270 105.6(4) . . ? O21 Si27 C270 110.7(4) . . ? Si1 O3 Si4 149.7(4) . . ? Si4 O4 Si5 152.3(4) . . ? Si4 O5 Si2 153.4(4) . . ? Si3 O6 Si1 156.2(4) . . ? Si2 O7 Si7 150.7(5) . . ? Si6 O9 Si7 157.8(5) . . ? Si3 O17 Si6 148.3(4) . . ? Si24 O20 Si27 152.3(5) . . ? Si25 O23 Si22 150.7(4) . . ? Si21 O24 Si22 155.4(5) . . ? Si27 O26 Si25 154.9(5) . . ? Si26 O27 Si70 146.5(5) . . ? Si26 O27 Si50 166.6(7) . . ? Si70 O27 Si50 33.2(3) . . ? Si26 O28 Si24 153.2(6) . . ? Si21 O29 Si26 158.0(5) . . ? Si25 O30 Si23 144.7(4) . . ? Si23 O31 Si24 154.0(4) . . ? Si23 O32 Si21 147.1(4) . . ? Si3 O51 Si5 140.6(4) . . ? Si7 O91 Si5 147.1(4) . . ? Si2 O200 Si40 146.6(4) . . ? C11 C10 C14 104.0(5) . . ? C11 C10 Si1 113.3(6) . . ? C14 C10 Si1 113.7(6) . . ? C12 C11 C10 108.2(6) . . ? C13 C12 C11 108.6(6) . . ? C13 C12 C17 31(4) . . ? C11 C12 C17 99.7(7) . . ? C12 C13 C14 107.0(12) . . ? C14 C17 C12 101.9(8) . . ? C13 C14 C17 32(4) . . ? C13 C14 C10 107.9(8) . . ? C17 C14 C10 106.7(7) . . ? C21 C20 C25 39(2) . . ? C21 C20 C24 109.9(16) . . ? C25 C20 C24 101.6(10) . . ? C21 C20 Si2 130.8(14) . . ? C25 C20 Si2 112.7(9) . . ? C24 C20 Si2 116.0(8) . . ? C20 C21 C22 103.6(18) . . ? C21 C22 C23 105(2) . . ? C20 C25 C26 107.1(10) . . ? C25 C26 C23 108.4(10) . . ? C26 C23 C24 103.4(8) . . ? C26 C23 C22 49.5(16) . . ? C24 C23 C22 101.8(14) . . ? C23 C24 C20 106.3(9) . . ? C34 C30 C31 100.9(9) . . ? C34 C30 Si3 116.1(6) . . ? C31 C30 Si3 114.9(7) . . ? C32 C31 C30 107.6(8) . . ? C31 C32 C33 106.0(8) . . ? C34 C33 C32 105.6(8) . . ? C33 C34 C30 106.2(8) . . ? C44 C40 C41 102.2(7) . . ? C44 C40 Si4 115.2(6) . . ? C41 C40 Si4 114.3(6) . . ? C42 C41 C40 103.8(7) . . ? C41 C42 C43 106.3(8) . . ? C42 C43 C44 104.9(7) . . ? C40 C44 C43 107.9(7) . . ? C51 C50 C55 92.9(14) . . ? C51 C50 C54 100.7(10) . . ? C55 C50 C54 108.3(14) . . ? C51 C50 Si5 120.5(8) . . ? C55 C50 Si5 115.2(13) . . ? C54 C50 Si5 116.1(7) . . ? C50 C51 C52 102.9(11) . . ? C53 C52 C51 110.3(12) . . ? C50 C55 C56 95.5(16) . . ? C53 C56 C55 115.8(16) . . ? C52 C53 C56 65.3(19) . . ? C52 C53 C54 98.7(11) . . ? C56 C53 C54 95.6(12) . . ? C50 C54 C53 105.1(9) . . ? C61 C60 C64 105.2(8) . . ? C61 C60 Si6 114.9(9) . . ? C64 C60 Si6 114.1(9) . . ? C60 C61 C62 108.6(8) . . ? C61 C62 C63 105.8(8) . . ? C64 C69 C65 108.4(9) . . ? C64 C69 Si6 114.5(8) . . ? C65 C69 Si6 136.7(16) . . ? C69 C65 C66 106.7(8) . . ? C63 C66 C65 107.0(6) . . ? C64 C63 C66 108.5(7) . . ? C64 C63 C62 106.3(10) . . ? C66 C63 C62 42(2) . . ? C63 C64 C69 106.0(7) . . ? C63 C64 C60 106.1(7) . . ? C69 C64 C60 0.4(7) . . ? C74 C70 C71 102.7(9) . . ? C74 C70 Si7 114.0(7) . . ? C71 C70 Si7 118.6(9) . . ? C72 C71 C70 105.2(11) . . ? C73 C72 C71 106.4(10) . . ? C72 C73 C74 108.0(11) . . ? C70 C74 C73 105.1(10) . . ? C214 C210 C211 105.6(9) . . ? C214 C210 Si21 114.0(8) . . ? C211 C210 Si21 115.7(7) . . ? C216 C211 C212 29(3) . . ? C216 C211 C210 105.4(14) . . ? C212 C211 C210 103.0(9) . . ? C211 C212 C213 107.2(10) . . ? C211 C216 C213 107.5(11) . . ? C214 C213 C216 102.0(19) . . ? C214 C213 C212 106.6(10) . . ? C216 C213 C212 28(2) . . ? C213 C214 C210 107.3(9) . . ? C221 C220 C224 105.0(9) . . ? C221 C220 Si22 113.3(6) . . ? C224 C220 Si22 112.0(7) . . ? C220 C221 C222 99.1(15) . . ? C220 C221 C226 106.3(14) . . ? C222 C221 C226 25.5(17) . . ? C223 C222 C221 109(2) . . ? C224 C223 C222 105.0(12) . . ? C227 C226 C221 108(2) . . ? C226 C227 C224 110.9(18) . . ? C223 C224 C227 26(2) . . ? C223 C224 C220 99.0(18) . . ? C227 C224 C220 103.4(13) . . ? C234 C230 C231 105.7(7) . . ? C234 C230 Si23 111.4(7) . . ? C231 C230 Si23 113.6(7) . . ? C232 C231 C236 38(3) . . ? C232 C231 C230 106(2) . . ? C236 C231 C230 102.4(9) . . ? C233 C232 C231 102(2) . . ? C232 C233 C234 107(3) . . ? C237 C236 C231 109.7(13) . . ? C236 C237 C234 107.1(14) . . ? C233 C234 C237 25.6(16) . . ? C233 C234 C230 103.6(14) . . ? C237 C234 C230 101.7(11) . . ? C241 C240 C244 103.8(8) . . ? C241 C240 C248 127.2(11) . . ? C244 C240 C248 26.9(11) . . ? C241 C240 Si24 114.2(6) . . ? C244 C240 Si24 111.1(8) . . ? C248 C240 Si24 106.0(12) . . ? C242 C241 C240 109.2(7) . . ? C242 C241 C246 26.6(9) . . ? C240 C241 C246 83.2(9) . . ? C243 C242 C241 107.2(7) . . ? C242 C243 C244 107.1(8) . . ? C243 C244 C240 109.5(9) . . ? C247 C246 C241 89(2) . . ? C246 C247 C248 103.3(17) . . ? C247 C248 C240 83(2) . . ? C251 C250 C254 106.0(8) . . ? C251 C250 Si25 114.8(7) . . ? C254 C250 Si25 113.9(7) . . ? C252 C251 C250 106.9(10) . . ? C252 C251 C256 35(2) . . ? C250 C251 C256 106.9(9) . . ? C253 C252 C251 105.7(11) . . ? C252 C253 C254 112.2(11) . . ? C257 C256 C251 108.6(19) . . ? C256 C257 C254 108.8(16) . . ? C257 C254 C253 37(2) . . ? C257 C254 C250 108.5(10) . . ? C253 C254 C250 101.6(10) . . ? C264 C260 C261 107.0(10) . . ? C264 C260 Si26 118(2) . . ? C261 C260 Si26 107.1(14) . . ? C262 C261 C260 108.1(12) . . ? C261 C262 C263 102.8(16) . . ? C262 C263 C264 106.7(15) . . ? C260 C264 C263 104.5(12) . . ? C268 C269 C265 105.3(11) . . ? C268 C269 Si26 124.8(18) . . ? C265 C269 Si26 115.0(15) . . ? C266 C265 C269 105.3(14) . . ? C265 C266 C267 102.6(17) . . ? C266 C267 C268 108.2(13) . . ? C269 C268 C267 106.7(11) . . ? C274 C270 C271 106.8(6) . . ? C274 C270 C275 105.3(6) . . ? C271 C270 C275 21(3) . . ? C274 C270 Si27 112.2(8) . . ? C271 C270 Si27 126(2) . . ? C275 C270 Si27 110.0(10) . . ? C272 C271 C270 108.0(7) . . ? C273 C272 C271 107.7(8) . . ? C276 C275 C270 107.8(8) . . ? C273 C276 C275 101.5(10) . . ? C272 C273 C276 42.2(16) . . ? C272 C273 C274 109.0(8) . . ? C276 C273 C274 105.8(7) . . ? C270 C274 C273 106.0(6) . . ? O200 Si40 C400 107.1(4) . . ? O200 Si40 C401 109.4(4) . . ? C400 Si40 C401 111.5(4) . . ? O200 Si40 C402 108.4(4) . . ? C400 Si40 C402 108.7(4) . . ? C401 Si40 C402 111.6(5) . . ? C405 C400 C404 108.6(8) . . ? C405 C400 C403 107.1(6) . . ? C404 C400 C403 111.7(8) . . ? C405 C400 Si40 109.3(6) . . ? C404 C400 Si40 109.7(6) . . ? C403 C400 Si40 110.3(6) . . ? O27 Si50 C500 106.9(5) . . ? O27 Si50 C501 107.7(9) . . ? C500 Si50 C501 108.7(8) . . ? O27 Si50 C502 110.6(6) . . ? C500 Si50 C502 109.9(6) . . ? C501 Si50 C502 112.9(8) . . ? C503 C500 C505 107.9(10) . . ? C503 C500 C504 113.5(10) . . ? C505 C500 C504 107.9(9) . . ? C503 C500 Si50 110.9(10) . . ? C505 C500 Si50 107.9(8) . . ? C504 C500 Si50 108.6(7) . . ? O27 Si70 C700 107.2(5) . . ? O27 Si70 C701 107.5(8) . . ? C700 Si70 C701 109.2(7) . . ? C703 C700 Si70 110.0(9) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.639 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.071 #=== END data_SMSICY _exptl_special_details ; Crystals were grown at -30 deg C from a concentrated pentane solution. A crystal was mounted in a film of RS3000 perfluoropolyether on a dual-stage glass fibre and transferred to the diffractometer. ; _refine_special_details ; Positional disorder in some cyclopentyl groups, and the aryloxide group was identified and modelled, with the partial atoms refined as isotropic. H atoms on pivot atoms for disorder components were not placed. Other H atoms were placed geometrically. The crystal is twinned and the Flack parameter refines to 0.489(13). Apparently close contacts between H(60A) and H(73B), and between H(24C) and H(27F) derive from different disorder components. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 00001 _chemical_melting_point ? _chemical_formula_moiety 'C96 H177 Li2 O25 Si16 Sm' _chemical_formula_sum 'C96 H177 Li2 O25 Si16 Sm' _chemical_formula_weight 2345.04 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' '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' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 17.540(2) _cell_length_b 31.945(3) _cell_length_c 21.300(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11935(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6141 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.28 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4980 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_process_details 'SHELXTL version 5.1 (Bruker, 1997)' _diffrn_ambient_temperature 150(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 SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 75523 _diffrn_reflns_av_R_equivalents 0.113 _diffrn_reflns_av_sigmaI/netI 0.067 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.00 _reflns_number_total 28966 _reflns_number_gt 17406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL; PLATON (Spek, 2000)' _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^)+(0.0724P)^2^+66.2040P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _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 0.489(13) _refine_ls_number_reflns 23196 _refine_ls_number_parameters 1240 _refine_ls_number_restraints 887 _refine_ls_R_factor_all 0.112 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.199 _refine_ls_wR_factor_gt 0.175 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.08 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.002 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm Sm 0.41586(2) 0.245638(13) 0.13889(5) 0.03140(11) Uani 1 1 d U . . Li1 Li 0.5272(8) 0.3092(4) 0.0897(7) 0.0263(18) Uani 1 1 d U . . Li2 Li 0.5133(10) 0.1800(5) 0.2100(9) 0.041(3) Uani 1 1 d U G . Si1 Si 0.55949(15) 0.27621(7) 0.24277(13) 0.0253(5) Uani 1 1 d U . . Si2 Si 0.40044(15) 0.36030(7) 0.15884(13) 0.0288(6) Uani 1 1 d U . . Si3 Si 0.47282(15) 0.35483(7) 0.29193(13) 0.0276(5) Uani 1 1 d U B . Si4 Si 0.59935(14) 0.41315(7) 0.24340(13) 0.0270(5) Uani 1 1 d U . . Si5 Si 0.65282(14) 0.33857(7) 0.15847(12) 0.0247(5) Uani 1 1 d U . . Si6 Si 0.50680(15) 0.43792(7) 0.12797(14) 0.0304(6) Uani 1 1 d U . . Si7 Si 0.62128(16) 0.39236(7) 0.04297(13) 0.0314(6) Uani 1 1 d U . . Si21 Si 0.39195(17) 0.13345(8) 0.12104(14) 0.0385(7) Uani 1 1 d U C . Si22 Si 0.56257(16) 0.21669(7) 0.03436(14) 0.0302(6) Uani 1 1 d U . . Si23 Si 0.46704(19) 0.13948(8) -0.01139(15) 0.0413(7) Uani 1 1 d U D . Si24 Si 0.5865(2) 0.07756(9) 0.03661(16) 0.0453(7) Uani 1 1 d DU E . Si25 Si 0.49199(19) 0.05390(8) 0.15124(16) 0.0441(8) Uani 1 1 d U G . Si26 Si 0.64962(17) 0.15104(7) 0.12031(14) 0.0352(7) Uani 1 1 d U G . Si27 Si 0.59273(18) 0.10463(8) 0.24033(15) 0.0398(7) Uani 1 1 d U G . O1 O 0.5067(4) 0.23972(19) 0.2166(3) 0.0275(13) Uani 1 1 d U . . O2 O 0.4318(3) 0.31735(17) 0.1312(4) 0.0323(13) Uani 1 1 d U . . O3 O 0.5847(4) 0.3789(2) -0.0227(3) 0.0394(14) Uani 1 1 d U . . O4 O 0.5097(4) 0.30852(17) 0.2853(3) 0.0310(14) Uani 1 1 d U . . O5 O 0.4162(4) 0.36335(19) 0.2338(3) 0.0366(14) Uani 1 1 d U . . O6 O 0.5953(3) 0.30305(18) 0.1826(3) 0.0293(13) Uani 1 1 d U . . O7 O 0.5406(4) 0.38853(19) 0.2903(3) 0.0352(14) Uani 1 1 d U . . O8 O 0.4480(4) 0.39932(18) 0.1275(3) 0.0355(15) Uani 1 1 d U . . O9 O 0.6476(4) 0.37942(17) 0.2025(3) 0.0322(14) Uani 1 1 d U . . O10 O 0.5505(4) 0.44152(19) 0.1956(3) 0.0364(15) Uani 1 1 d U . . O11 O 0.5703(4) 0.42902(19) 0.0735(3) 0.0377(16) Uani 1 1 d U . . O12 O 0.6176(4) 0.35014(17) 0.0880(3) 0.0272(12) Uani 1 1 d U . . O21 O 0.4291(4) 0.17442(19) 0.1520(4) 0.0397(16) Uani 1 1 d U . . O22 O 0.5128(4) 0.25200(18) 0.0664(3) 0.0309(14) Uani 1 1 d U . . O23 O 0.5319(4) 0.12741(19) 0.2871(3) 0.0426(15) Uani 1 1 d U . . O24 O 0.4078(5) 0.1328(2) 0.0453(4) 0.0478(17) Uani 1 1 d U . . O25 O 0.5077(4) 0.18480(19) -0.0045(3) 0.0397(16) Uani 1 1 d U . . O26 O 0.4300(4) 0.09170(19) 0.1494(4) 0.0498(19) Uani 1 1 d U . . O27 O 0.5335(5) 0.1033(2) -0.0085(4) 0.054(2) Uani 1 1 d U . . O28 O 0.6071(4) 0.1903(2) 0.0898(3) 0.0381(15) Uani 1 1 d U . . O29 O 0.5360(5) 0.0508(2) 0.0859(4) 0.0505(18) Uani 1 1 d U . . O30 O 0.6390(4) 0.1094(2) 0.0776(4) 0.0449(17) Uani 1 1 d U . . O31 O 0.6080(4) 0.14232(19) 0.1890(3) 0.0339(14) Uani 1 1 d U . . O32 O 0.5528(5) 0.0648(2) 0.2057(4) 0.0451(18) Uani 1 1 d U . . O800 O 0.2914(3) 0.2461(2) 0.1379(7) 0.0529(15) Uani 1 1 d U H . C10 C 0.6424(6) 0.2584(3) 0.2913(5) 0.0341(19) Uani 1 1 d DU . . H10A H 0.6801 0.2442 0.2633 0.041 Uiso 1 1 calc R . . C11 C 0.6833(7) 0.2951(3) 0.3264(6) 0.055(3) Uani 1 1 d DU . . H11A H 0.7393 0.2929 0.3212 0.066 Uiso 1 1 calc R . . H11B H 0.6665 0.3224 0.3092 0.066 Uiso 1 1 calc R . . C12 C 0.6624(9) 0.2917(4) 0.3933(6) 0.076(4) Uani 1 1 d DU . . H12A H 0.6364 0.3175 0.4074 0.092 Uiso 1 1 calc R . . H12B H 0.7086 0.2876 0.4193 0.092 Uiso 1 1 calc R . . C13 C 0.6097(11) 0.2545(4) 0.3998(6) 0.074(4) Uani 1 1 d DU . . H13A H 0.6218 0.2387 0.4386 0.089 Uiso 1 1 calc R . . H13B H 0.5560 0.2640 0.4022 0.089 Uiso 1 1 calc R . . C14 C 0.6207(9) 0.2281(3) 0.3450(5) 0.064(4) Uani 1 1 d DU . . H14A H 0.5733 0.2127 0.3348 0.076 Uiso 1 1 calc R . . H14B H 0.6620 0.2076 0.3525 0.076 Uiso 1 1 calc R . . C20 C 0.2966(5) 0.3697(3) 0.1457(6) 0.043(2) Uani 1 1 d U A . H20A H 0.2700 0.3422 0.1501 0.052 Uiso 1 1 calc R . . C21 C 0.2639(7) 0.3995(4) 0.1966(7) 0.063(4) Uani 1 1 d DU . . C22 C 0.1915(9) 0.4184(7) 0.1686(8) 0.057(6) Uiso 0.67(4) 1 d PDU A 1 H22A H 0.1486 0.3982 0.1671 0.068 Uiso 0.67(4) 1 calc PR A 1 H22B H 0.1755 0.4444 0.1900 0.068 Uiso 0.67(4) 1 calc PR A 1 C23 C 0.226(2) 0.4263(8) 0.1051(11) 0.116(11) Uiso 0.67(4) 1 d PDU A 1 H23A H 0.2599 0.4511 0.1073 0.139 Uiso 0.67(4) 1 calc PR A 1 H23B H 0.1852 0.4323 0.0744 0.139 Uiso 0.67(4) 1 calc PR A 1 C26 C 0.1841(19) 0.395(4) 0.1692(18) 0.21(5) Uiso 0.33(4) 1 d PDU A 2 H26A H 0.1658 0.3655 0.1738 0.257 Uiso 0.33(4) 1 calc PR A 2 H26B H 0.1477 0.4137 0.1904 0.257 Uiso 0.33(4) 1 calc PR A 2 C27 C 0.1927(10) 0.4062(9) 0.1003(11) 0.024(8) Uiso 0.33(4) 1 d PDU A 2 H27A H 0.1908 0.4370 0.0944 0.029 Uiso 0.33(4) 1 calc PR A 2 H27B H 0.1523 0.3931 0.0746 0.029 Uiso 0.33(4) 1 calc PR A 2 C24 C 0.2717(7) 0.3888(5) 0.0832(7) 0.079(4) Uani 1 1 d DU . . C30 C 0.4193(6) 0.3609(3) 0.3679(4) 0.037(2) Uani 1 1 d DU . . C31 C 0.4727(7) 0.3605(4) 0.4253(4) 0.052(3) Uani 1 1 d DU B . C32 C 0.4324(15) 0.3851(8) 0.4764(8) 0.049(8) Uiso 0.45(3) 1 d PDU B 1 H32A H 0.4682 0.3938 0.5100 0.059 Uiso 0.45(3) 1 calc PR B 1 H32B H 0.3899 0.3690 0.4951 0.059 Uiso 0.45(3) 1 calc PR B 1 C33 C 0.403(3) 0.4227(7) 0.4391(11) 0.076(11) Uiso 0.45(3) 1 d PDU B 1 H33A H 0.3553 0.4335 0.4570 0.091 Uiso 0.45(3) 1 calc PR B 1 H33B H 0.4417 0.4455 0.4387 0.091 Uiso 0.45(3) 1 calc PR B 1 C34 C 0.3909(18) 0.4057(5) 0.3738(10) 0.041(7) Uiso 0.45(3) 1 d PDU B 1 H34A H 0.4179 0.4236 0.3431 0.049 Uiso 0.45(3) 1 calc PR B 1 H34B H 0.3358 0.4066 0.3638 0.049 Uiso 0.45(3) 1 calc PR B 1 C36 C 0.4464(12) 0.4038(9) 0.4596(12) 0.059(7) Uiso 0.55(3) 1 d PDU B 2 H36A H 0.4474 0.4007 0.5058 0.071 Uiso 0.55(3) 1 calc PR B 2 H36B H 0.4801 0.4273 0.4474 0.071 Uiso 0.55(3) 1 calc PR B 2 C37 C 0.3637(12) 0.4111(7) 0.4358(8) 0.046(6) Uiso 0.55(3) 1 d PDU B 2 H37A H 0.3274 0.3926 0.4579 0.055 Uiso 0.55(3) 1 calc PR B 2 H37B H 0.3481 0.4406 0.4425 0.055 Uiso 0.55(3) 1 calc PR B 2 C38 C 0.3663(17) 0.4010(7) 0.3672(9) 0.049(6) Uiso 0.55(3) 1 d PDU B 2 H38A H 0.3892 0.4241 0.3426 0.059 Uiso 0.55(3) 1 calc PR B 2 H38B H 0.3150 0.3945 0.3505 0.059 Uiso 0.55(3) 1 calc PR B 2 C40 C 0.6659(5) 0.4459(2) 0.2891(4) 0.0329(19) Uani 1 1 d DU . . H40A H 0.6855 0.4285 0.3247 0.040 Uiso 1 1 calc R . . C41 C 0.7353(5) 0.4610(3) 0.2508(4) 0.041(2) Uani 1 1 d DU . . H41A H 0.7722 0.4380 0.2441 0.049 Uiso 1 1 calc R . . H41B H 0.7193 0.4723 0.2095 0.049 Uiso 1 1 calc R . . C42 C 0.7694(5) 0.4954(3) 0.2920(5) 0.051(3) Uani 1 1 d DU . . H42A H 0.8056 0.4834 0.3228 0.061 Uiso 1 1 calc R . . H42B H 0.7968 0.5163 0.2660 0.061 Uiso 1 1 calc R . . C43 C 0.7018(5) 0.5155(3) 0.3253(7) 0.068(4) Uani 1 1 d DU . . H43A H 0.6907 0.5433 0.3069 0.082 Uiso 1 1 calc R . . H43B H 0.7132 0.5193 0.3705 0.082 Uiso 1 1 calc R . . C44 C 0.6333(4) 0.4864(3) 0.3170(5) 0.042(2) Uani 1 1 d DU . . H44A H 0.5953 0.4989 0.2882 0.051 Uiso 1 1 calc R . . H44B H 0.6084 0.4808 0.3579 0.051 Uiso 1 1 calc R . . C50 C 0.7538(5) 0.3191(3) 0.1558(4) 0.037(2) Uani 1 1 d DU . . H50A H 0.7548 0.2937 0.1831 0.044 Uiso 1 1 calc R . . C51 C 0.8127(5) 0.3488(3) 0.1835(5) 0.047(3) Uani 1 1 d DU . . H51A H 0.8108 0.3486 0.2300 0.056 Uiso 1 1 calc R . . H51B H 0.8050 0.3778 0.1683 0.056 Uiso 1 1 calc R . . C52 C 0.8882(5) 0.3307(4) 0.1594(6) 0.058(3) Uani 1 1 d DU . . H52A H 0.9290 0.3521 0.1600 0.070 Uiso 1 1 calc R . . H52B H 0.9045 0.3065 0.1852 0.070 Uiso 1 1 calc R . . C53 C 0.8703(6) 0.3172(4) 0.0929(6) 0.061(3) Uani 1 1 d DU . . H53A H 0.9024 0.2931 0.0806 0.073 Uiso 1 1 calc R . . H53B H 0.8798 0.3405 0.0632 0.073 Uiso 1 1 calc R . . C54 C 0.7848(5) 0.3049(3) 0.0922(5) 0.040(2) Uani 1 1 d DU . . H54A H 0.7577 0.3191 0.0574 0.048 Uiso 1 1 calc R . . H54B H 0.7789 0.2742 0.0871 0.048 Uiso 1 1 calc R . . C60 C 0.4616(5) 0.4888(3) 0.1125(5) 0.038(2) Uani 1 1 d DU . . H60A H 0.4282 0.4858 0.0747 0.045 Uiso 1 1 calc R . . C61 C 0.4118(6) 0.5048(3) 0.1676(5) 0.047(3) Uani 1 1 d DU . . H61A H 0.3585 0.5089 0.1538 0.056 Uiso 1 1 calc R . . H61B H 0.4125 0.4845 0.2028 0.056 Uiso 1 1 calc R . . C62 C 0.4461(8) 0.5449(4) 0.1868(6) 0.071(4) Uani 1 1 d DU . . H62A H 0.4837 0.5405 0.2209 0.085 Uiso 1 1 calc R . . H62B H 0.4063 0.5644 0.2019 0.085 Uiso 1 1 calc R . . C63 C 0.4840(7) 0.5618(3) 0.1298(8) 0.066(3) Uani 1 1 d DU . . H63A H 0.4465 0.5752 0.1015 0.080 Uiso 1 1 calc R . . H63B H 0.5237 0.5825 0.1411 0.080 Uiso 1 1 calc R . . C64 C 0.5177(7) 0.5250(3) 0.1004(7) 0.062(4) Uani 1 1 d DU . . H64A H 0.5680 0.5187 0.1192 0.074 Uiso 1 1 calc R . . H64B H 0.5244 0.5296 0.0548 0.074 Uiso 1 1 calc R . . C70 C 0.7215(5) 0.4110(3) 0.0353(4) 0.044(2) Uani 1 1 d DU . . H70A H 0.7505 0.4008 0.0727 0.053 Uiso 1 1 calc R . . C71 C 0.7656(6) 0.3980(4) -0.0234(5) 0.065(3) Uani 1 1 d DU . . H71A H 0.7833 0.3686 -0.0200 0.078 Uiso 1 1 calc R . . H71B H 0.7336 0.4008 -0.0615 0.078 Uiso 1 1 calc R . . C72 C 0.8326(7) 0.4280(4) -0.0254(7) 0.092(4) Uani 1 1 d DU . . H72A H 0.8524 0.4307 -0.0688 0.111 Uiso 1 1 calc R . . H72B H 0.8743 0.4181 0.0022 0.111 Uiso 1 1 calc R . . C73 C 0.8010(8) 0.4696(4) -0.0022(9) 0.118(6) Uani 1 1 d DU . . H73A H 0.7897 0.4884 -0.0379 0.141 Uiso 1 1 calc R . . H73B H 0.8380 0.4836 0.0259 0.141 Uiso 1 1 calc R . . C74 C 0.7281(7) 0.4588(3) 0.0334(7) 0.078(4) Uani 1 1 d DU . . H74A H 0.6833 0.4710 0.0118 0.094 Uiso 1 1 calc R . . H74B H 0.7303 0.4702 0.0766 0.094 Uiso 1 1 calc R . . C210 C 0.2861(6) 0.1293(3) 0.1299(6) 0.058(3) Uani 1 1 d DU . . C211 C 0.2484(7) 0.1028(5) 0.0775(6) 0.081(5) Uani 1 1 d DU C . C212 C 0.191(3) 0.0723(16) 0.1053(11) 0.23(3) Uiso 0.55(3) 1 d PDU C 1 H21C H 0.2083 0.0431 0.0982 0.279 Uiso 0.55(3) 1 calc PR C 1 H21D H 0.1407 0.0761 0.0858 0.279 Uiso 0.55(3) 1 calc PR C 1 C213 C 0.1881(13) 0.0819(10) 0.1751(11) 0.087(10) Uiso 0.55(3) 1 d PDU C 1 H21E H 0.1829 0.0559 0.1999 0.105 Uiso 0.55(3) 1 calc PR C 1 H21F H 0.1445 0.1006 0.1848 0.105 Uiso 0.55(3) 1 calc PR C 1 C214 C 0.2636(12) 0.1036(7) 0.1893(7) 0.044(6) Uiso 0.55(3) 1 d PDU C 1 H21G H 0.3034 0.0825 0.1989 0.053 Uiso 0.55(3) 1 calc PR C 1 H21H H 0.2581 0.1223 0.2260 0.053 Uiso 0.55(3) 1 calc PR C 1 C216 C 0.1673(9) 0.1002(8) 0.1045(9) 0.039(7) Uiso 0.45(3) 1 d PDU C 2 H21I H 0.1478 0.0713 0.0994 0.047 Uiso 0.45(3) 1 calc PR C 2 H21J H 0.1335 0.1192 0.0806 0.047 Uiso 0.45(3) 1 calc PR C 2 C217 C 0.1645(15) 0.1122(13) 0.1745(11) 0.081(11) Uiso 0.45(3) 1 d PDU C 2 H21K H 0.1422 0.0893 0.1998 0.097 Uiso 0.45(3) 1 calc PR C 2 H21L H 0.1340 0.1379 0.1809 0.097 Uiso 0.45(3) 1 calc PR C 2 C218 C 0.2488(16) 0.1195(15) 0.1922(8) 0.092(14) Uiso 0.45(3) 1 d PDU C 2 H21M H 0.2539 0.1433 0.2217 0.110 Uiso 0.45(3) 1 calc PR C 2 H21N H 0.2713 0.0942 0.2115 0.110 Uiso 0.45(3) 1 calc PR C 2 C220 C 0.6371(6) 0.2359(3) -0.0212(4) 0.051(3) Uani 1 1 d DU . . C221 C 0.6046(9) 0.2682(3) -0.0669(5) 0.078(5) Uani 1 1 d DU . . H22C H 0.5580 0.2810 -0.0490 0.094 Uiso 1 1 calc R . . H22D H 0.6424 0.2907 -0.0744 0.094 Uiso 1 1 calc R . . C222 C 0.5857(11) 0.2465(4) -0.1281(6) 0.111(7) Uani 1 1 d DU . . H22E H 0.5905 0.2660 -0.1641 0.134 Uiso 1 1 calc R . . H22F H 0.5332 0.2350 -0.1273 0.134 Uiso 1 1 calc R . . C223 C 0.6448(8) 0.2114(4) -0.1321(5) 0.072(4) Uani 1 1 d DU . . H22G H 0.6895 0.2206 -0.1569 0.087 Uiso 1 1 calc R . . H22H H 0.6225 0.1864 -0.1526 0.087 Uiso 1 1 calc R . . C224 C 0.6688(6) 0.2010(3) -0.0641(5) 0.053(3) Uani 1 1 d DU . . H22L H 0.7250 0.1998 -0.0609 0.063 Uiso 1 1 calc R . . H22M H 0.6478 0.1735 -0.0514 0.063 Uiso 1 1 calc R . . C230 C 0.4137(7) 0.1361(3) -0.0856(5) 0.053(3) Uani 1 1 d DU . . C231 C 0.3491(12) 0.1045(8) -0.0913(12) 0.072(9) Uiso 0.52(3) 1 d PDU D 1 H23C H 0.3051 0.1166 -0.1139 0.086 Uiso 0.52(3) 1 calc PR D 1 H23D H 0.3321 0.0948 -0.0494 0.086 Uiso 0.52(3) 1 calc PR D 1 C232 C 0.385(2) 0.0688(7) -0.129(3) 0.17(2) Uiso 0.52(3) 1 d PDU D 1 H23E H 0.3996 0.0456 -0.1003 0.209 Uiso 0.52(3) 1 calc PR D 1 H23F H 0.3485 0.0580 -0.1601 0.209 Uiso 0.52(3) 1 calc PR D 1 C233 C 0.4557(14) 0.0861(7) -0.1616(15) 0.081(10) Uiso 0.52(3) 1 d PDU D 1 H23G H 0.4506 0.0831 -0.2076 0.097 Uiso 0.52(3) 1 calc PR D 1 H23H H 0.5017 0.0706 -0.1479 0.097 Uiso 0.52(3) 1 calc PR D 1 C234 C 0.4630(14) 0.1323(7) -0.1440(10) 0.047(9) Uiso 0.52(3) 1 d PDU D 1 H23I H 0.5166 0.1398 -0.1348 0.057 Uiso 0.52(3) 1 calc PR D 1 H23J H 0.4437 0.1506 -0.1781 0.057 Uiso 0.52(3) 1 calc PR D 1 C235 C 0.374(2) 0.0934(7) -0.0875(8) 0.064(9) Uiso 0.48(3) 1 d PDU D 2 H23K H 0.4047 0.0719 -0.0657 0.077 Uiso 0.48(3) 1 calc PR D 2 H23L H 0.3230 0.0950 -0.0673 0.077 Uiso 0.48(3) 1 calc PR D 2 C236 C 0.3663(13) 0.0832(7) -0.1570(9) 0.049(7) Uiso 0.48(3) 1 d PDU D 2 H23M H 0.3155 0.0919 -0.1726 0.059 Uiso 0.48(3) 1 calc PR D 2 H23N H 0.3719 0.0527 -0.1637 0.059 Uiso 0.48(3) 1 calc PR D 2 C237 C 0.429(2) 0.1070(11) -0.1922(9) 0.097(14) Uiso 0.48(3) 1 d PDU D 2 H23O H 0.4076 0.1226 -0.2282 0.117 Uiso 0.48(3) 1 calc PR D 2 H23P H 0.4683 0.0873 -0.2081 0.117 Uiso 0.48(3) 1 calc PR D 2 C238 C 0.465(2) 0.1377(15) -0.1435(14) 0.11(2) Uiso 0.48(3) 1 d PDU D 2 H23Q H 0.5172 0.1289 -0.1327 0.135 Uiso 0.48(3) 1 calc PR D 2 H23R H 0.4663 0.1664 -0.1608 0.135 Uiso 0.48(3) 1 calc PR D 2 C240 C 0.6484(6) 0.0441(4) -0.0082(6) 0.076(4) Uani 1 1 d DU . . C241 C 0.7011(12) 0.0647(6) -0.0551(10) 0.098(9) Uiso 0.622(16) 1 d PDU E 1 H24B H 0.7202 0.0917 -0.0388 0.117 Uiso 0.622(16) 1 calc PR E 1 H24C H 0.6743 0.0697 -0.0954 0.117 Uiso 0.622(16) 1 calc PR E 1 C242 C 0.7668(13) 0.0336(7) -0.0641(11) 0.112(11) Uiso 0.622(16) 1 d PDU E 1 H24D H 0.7654 0.0217 -0.1069 0.134 Uiso 0.622(16) 1 calc PR E 1 H24E H 0.8163 0.0479 -0.0581 0.134 Uiso 0.622(16) 1 calc PR E 1 C243 C 0.7566(11) -0.0009(5) -0.0151(9) 0.063(6) Uiso 0.622(16) 1 d PDU E 1 H24F H 0.8053 -0.0061 0.0070 0.075 Uiso 0.622(16) 1 calc PR E 1 H24G H 0.7401 -0.0272 -0.0356 0.075 Uiso 0.622(16) 1 calc PR E 1 C244 C 0.6958(10) 0.0142(6) 0.0311(7) 0.069(6) Uiso 0.622(16) 1 d PDU E 1 H24H H 0.6646 -0.0095 0.0467 0.083 Uiso 0.622(16) 1 calc PR E 1 H24I H 0.7192 0.0288 0.0674 0.083 Uiso 0.622(16) 1 calc PR E 1 C245 C 0.7339(8) 0.0517(10) -0.003(2) 0.106(17) Uiso 0.378(16) 1 d PDU E 2 H24J H 0.7500 0.0498 0.0417 0.127 Uiso 0.378(16) 1 calc PR E 2 H24K H 0.7467 0.0800 -0.0186 0.127 Uiso 0.378(16) 1 calc PR E 2 C246 C 0.7753(8) 0.0183(9) -0.0417(16) 0.057(9) Uiso 0.378(16) 1 d PDU E 2 H24L H 0.7982 0.0311 -0.0796 0.068 Uiso 0.378(16) 1 calc PR E 2 H24M H 0.8163 0.0052 -0.0167 0.068 Uiso 0.378(16) 1 calc PR E 2 C247 C 0.7156(12) -0.0144(6) -0.0603(14) 0.051(8) Uiso 0.378(16) 1 d PDU E 2 H24N H 0.7238 -0.0407 -0.0367 0.061 Uiso 0.378(16) 1 calc PR E 2 H24O H 0.7190 -0.0206 -0.1058 0.061 Uiso 0.378(16) 1 calc PR E 2 C248 C 0.6373(9) 0.0041(8) -0.0445(17) 0.072(11) Uiso 0.378(16) 1 d PDU E 2 H24P H 0.6087 0.0099 -0.0836 0.086 Uiso 0.378(16) 1 calc PR E 2 H24Q H 0.6075 -0.0161 -0.0192 0.086 Uiso 0.378(16) 1 calc PR E 2 C250 C 0.4484(7) 0.0029(3) 0.1680(6) 0.053(3) Uani 1 1 d U . . H25A H 0.4198 0.0049 0.2085 0.064 Uiso 1 1 calc R G . C251 C 0.3922(9) -0.0122(4) 0.1156(7) 0.074(4) Uani 1 1 d U F . H25B H 0.3389 -0.0069 0.1287 0.089 Uiso 1 1 calc R . . H25C H 0.4019 0.0034 0.0762 0.089 Uiso 1 1 calc R . . C252 C 0.4039(12) -0.0570(5) 0.1055(10) 0.132(9) Uani 1 1 d DU . . C253 C 0.4647(10) -0.0714(4) 0.1510(9) 0.063(6) Uiso 0.84(5) 1 d PDU F 1 H25E H 0.5004 -0.0909 0.1300 0.076 Uiso 0.84(5) 1 calc PR F 1 H25F H 0.4412 -0.0860 0.1871 0.076 Uiso 0.84(5) 1 calc PR F 1 C257 C 0.4888(18) -0.061(3) 0.118(4) 0.08(4) Uiso 0.16(5) 1 d PDU F 2 H25G H 0.5181 -0.0519 0.0804 0.100 Uiso 0.16(5) 1 calc PR F 2 H25H H 0.5023 -0.0902 0.1277 0.100 Uiso 0.16(5) 1 calc PR F 2 C254 C 0.5071(9) -0.0325(3) 0.1734(9) 0.091(5) Uani 1 1 d DU F . C260 C 0.7534(5) 0.1597(3) 0.1310(4) 0.042(2) Uani 1 1 d DU . . H26C H 0.7747 0.1339 0.1511 0.050 Uiso 1 1 calc R G . C261 C 0.7761(6) 0.1965(3) 0.1715(5) 0.049(3) Uani 1 1 d DU G . H26D H 0.7661 0.1909 0.2165 0.059 Uiso 1 1 calc R . . H26E H 0.7485 0.2222 0.1589 0.059 Uiso 1 1 calc R . . C262 C 0.8629(7) 0.2005(4) 0.1584(7) 0.065(3) Uani 1 1 d U . . H26F H 0.8795 0.2300 0.1625 0.078 Uiso 1 1 calc R G . H26G H 0.8924 0.1833 0.1885 0.078 Uiso 1 1 calc R . . C263 C 0.8753(7) 0.1853(4) 0.0928(7) 0.062(3) Uani 1 1 d U G . H26H H 0.9152 0.1635 0.0919 0.075 Uiso 1 1 calc R . . H26I H 0.8912 0.2087 0.0653 0.075 Uiso 1 1 calc R . . C264 C 0.7983(6) 0.1673(4) 0.0708(5) 0.055(3) Uani 1 1 d DU G . H26J H 0.7713 0.1874 0.0433 0.067 Uiso 1 1 calc R . . H26K H 0.8058 0.1408 0.0475 0.067 Uiso 1 1 calc R . . C270 C 0.6783(7) 0.0861(3) 0.2807(5) 0.048(2) Uani 1 1 d U . . H27C H 0.6602 0.0692 0.3174 0.058 Uiso 1 1 calc R G . C271 C 0.7331(6) 0.1191(4) 0.3074(7) 0.060(3) Uani 1 1 d U G . H27D H 0.7239 0.1465 0.2873 0.071 Uiso 1 1 calc R . . H27E H 0.7252 0.1221 0.3532 0.071 Uiso 1 1 calc R . . C272 C 0.8143(7) 0.1042(4) 0.2940(7) 0.067(3) Uani 1 1 d U . . H27F H 0.8469 0.1071 0.3316 0.081 Uiso 1 1 calc R G . H27G H 0.8372 0.1203 0.2590 0.081 Uiso 1 1 calc R . . C273 C 0.8046(8) 0.0581(4) 0.2760(7) 0.069(3) Uani 1 1 d U G . H27H H 0.8028 0.0402 0.3139 0.083 Uiso 1 1 calc R . . H27I H 0.8472 0.0487 0.2490 0.083 Uiso 1 1 calc R . . C274 C 0.7288(7) 0.0561(4) 0.2402(6) 0.060(3) Uani 1 1 d U G . H27J H 0.7079 0.0273 0.2396 0.072 Uiso 1 1 calc R . . H27K H 0.7342 0.0664 0.1966 0.072 Uiso 1 1 calc R . . Si40 Si 0.55053(17) 0.39784(8) -0.08931(13) 0.0394(6) Uani 1 1 d DU . . C400 C 0.5653(8) 0.4562(3) -0.0897(6) 0.063(3) Uani 1 1 d DU . . H40B H 0.6199 0.4624 -0.0867 0.095 Uiso 1 1 calc R . . H40C H 0.5386 0.4687 -0.0539 0.095 Uiso 1 1 calc R . . H40D H 0.5450 0.4680 -0.1289 0.095 Uiso 1 1 calc R . . C401 C 0.6033(7) 0.3733(4) -0.1547(5) 0.062(3) Uani 1 1 d DU . . H40E H 0.5950 0.3430 -0.1540 0.093 Uiso 1 1 calc R . . H40F H 0.6579 0.3792 -0.1501 0.093 Uiso 1 1 calc R . . H40G H 0.5851 0.3848 -0.1947 0.093 Uiso 1 1 calc R . . C402 C 0.4456(5) 0.3865(3) -0.0951(5) 0.048(2) Uani 1 1 d DU . . C403 C 0.4199(7) 0.3910(4) -0.1632(5) 0.062(3) Uani 1 1 d DU . . H40H H 0.3652 0.3851 -0.1662 0.092 Uiso 1 1 calc R . . H40I H 0.4481 0.3711 -0.1894 0.092 Uiso 1 1 calc R . . H40J H 0.4300 0.4195 -0.1777 0.092 Uiso 1 1 calc R . . C404 C 0.4286(8) 0.3421(4) -0.0726(8) 0.083(5) Uani 1 1 d DU . . H40K H 0.3737 0.3366 -0.0760 0.124 Uiso 1 1 calc R . . H40L H 0.4446 0.3390 -0.0288 0.124 Uiso 1 1 calc R . . H40M H 0.4564 0.3220 -0.0987 0.124 Uiso 1 1 calc R . . C405 C 0.4009(7) 0.4169(4) -0.0534(6) 0.066(3) Uani 1 1 d DU . . H40N H 0.3463 0.4109 -0.0567 0.099 Uiso 1 1 calc R . . H40O H 0.4106 0.4457 -0.0671 0.099 Uiso 1 1 calc R . . H40P H 0.4172 0.4137 -0.0097 0.099 Uiso 1 1 calc R . . Si50 Si 0.4919(3) 0.12787(16) 0.3593(3) 0.0410(18) Uiso 0.531(11) 1 d PDU G 1 C500 C 0.5686(12) 0.1303(8) 0.4214(12) 0.052(7) Uiso 0.531(11) 1 d PDU G 1 H50B H 0.5978 0.1562 0.4166 0.078 Uiso 0.531(11) 1 calc PR G 1 H50C H 0.6027 0.1062 0.4169 0.078 Uiso 0.531(11) 1 calc PR G 1 H50D H 0.5450 0.1297 0.4631 0.078 Uiso 0.531(11) 1 calc PR G 1 C501 C 0.4281(11) 0.1741(5) 0.3614(11) 0.050(5) Uiso 0.531(11) 1 d PDU G 1 H50E H 0.3890 0.1714 0.3288 0.074 Uiso 0.531(11) 1 calc PR G 1 H50F H 0.4580 0.1996 0.3540 0.074 Uiso 0.531(11) 1 calc PR G 1 H50G H 0.4035 0.1759 0.4027 0.074 Uiso 0.531(11) 1 calc PR G 1 C502 C 0.4382(9) 0.0776(4) 0.3709(7) 0.053(6) Uiso 0.531(11) 1 d PDU G 1 C503 C 0.3733(13) 0.0764(8) 0.3236(11) 0.075(8) Uiso 0.531(11) 1 d PDU G 1 H50H H 0.3443 0.0504 0.3289 0.113 Uiso 0.531(11) 1 calc PR G 1 H50I H 0.3942 0.0776 0.2810 0.113 Uiso 0.531(11) 1 calc PR G 1 H50J H 0.3395 0.1004 0.3304 0.113 Uiso 0.531(11) 1 calc PR G 1 C504 C 0.4902(13) 0.0397(6) 0.3663(11) 0.074(7) Uiso 0.531(11) 1 d PDU G 1 H50K H 0.4603 0.0141 0.3730 0.111 Uiso 0.531(11) 1 calc PR G 1 H50L H 0.5301 0.0416 0.3983 0.111 Uiso 0.531(11) 1 calc PR G 1 H50M H 0.5136 0.0388 0.3245 0.111 Uiso 0.531(11) 1 calc PR G 1 C505 C 0.4058(14) 0.0789(7) 0.4379(8) 0.071(7) Uiso 0.531(11) 1 d PDU G 1 H50N H 0.3774 0.0531 0.4463 0.107 Uiso 0.531(11) 1 calc PR G 1 H50O H 0.3715 0.1030 0.4422 0.107 Uiso 0.531(11) 1 calc PR G 1 H50P H 0.4477 0.0815 0.4681 0.107 Uiso 0.531(11) 1 calc PR G 1 Si70 Si 0.4581(5) 0.1171(3) 0.3363(4) 0.062(3) Uiso 0.469(11) 1 d PDU G 2 C700 C 0.405(2) 0.0698(8) 0.3091(16) 0.093(12) Uiso 0.469(11) 1 d PDU G 2 H70B H 0.3831 0.0751 0.2674 0.139 Uiso 0.469(11) 1 calc PR G 2 H70C H 0.3632 0.0637 0.3387 0.139 Uiso 0.469(11) 1 calc PR G 2 H70D H 0.4393 0.0458 0.3071 0.139 Uiso 0.469(11) 1 calc PR G 2 C701 C 0.4013(15) 0.1657(6) 0.3330(14) 0.068(8) Uiso 0.469(11) 1 d PDU G 2 H70E H 0.4322 0.1892 0.3482 0.102 Uiso 0.469(11) 1 calc PR G 2 H70F H 0.3560 0.1627 0.3596 0.102 Uiso 0.469(11) 1 calc PR G 2 H70G H 0.3856 0.1710 0.2896 0.102 Uiso 0.469(11) 1 calc PR G 2 C702 C 0.4991(11) 0.1065(6) 0.4158(8) 0.066(8) Uiso 0.469(11) 1 d PDU G 2 C703 C 0.5295(19) 0.0616(7) 0.4182(16) 0.114(14) Uiso 0.469(11) 1 d PDU G 2 H70H H 0.5513 0.0561 0.4597 0.172 Uiso 0.469(11) 1 calc PR G 2 H70I H 0.5690 0.0580 0.3861 0.172 Uiso 0.469(11) 1 calc PR G 2 H70J H 0.4877 0.0420 0.4102 0.172 Uiso 0.469(11) 1 calc PR G 2 C704 C 0.5587(16) 0.1381(10) 0.4350(16) 0.087(15) Uiso 0.469(11) 1 d PDU G 2 H70K H 0.5779 0.1312 0.4770 0.131 Uiso 0.469(11) 1 calc PR G 2 H70L H 0.5359 0.1661 0.4357 0.131 Uiso 0.469(11) 1 calc PR G 2 H70M H 0.6009 0.1376 0.4049 0.131 Uiso 0.469(11) 1 calc PR G 2 C705 C 0.4337(14) 0.1089(9) 0.4635(11) 0.076(10) Uiso 0.469(11) 1 d PDU G 2 H70N H 0.4537 0.1038 0.5058 0.114 Uiso 0.469(11) 1 calc PR G 2 H70O H 0.3954 0.0876 0.4534 0.114 Uiso 0.469(11) 1 calc PR G 2 H70P H 0.4104 0.1367 0.4618 0.114 Uiso 0.469(11) 1 calc PR G 2 C800 C 0.2202(4) 0.25283(18) 0.1359(5) 0.052(2) Uani 1 1 d DU . . C801 C 0.1807(6) 0.2650(3) 0.1923(4) 0.037(5) Uiso 0.532(15) 1 d PDU H 1 C802 C 0.1126(10) 0.2885(5) 0.1856(11) 0.075(8) Uiso 0.532(15) 1 d PDU H 1 H80A H 0.0848 0.2972 0.2216 0.090 Uiso 0.532(15) 1 calc PR H 1 C803 C 0.0872(14) 0.2987(6) 0.1263(8) 0.079(8) Uiso 0.532(15) 1 d PDU H 1 H80B H 0.0414 0.3144 0.1228 0.095 Uiso 0.532(15) 1 calc PR H 1 C804 C 0.1247(10) 0.2872(5) 0.0713(10) 0.065(7) Uiso 0.532(15) 1 d PDU H 1 H80C H 0.1043 0.2951 0.0317 0.078 Uiso 0.532(15) 1 calc PR H 1 C805 C 0.1936(6) 0.2637(3) 0.0742(5) 0.052(6) Uiso 0.532(15) 1 d PDU H 1 C851 C 0.1751(14) 0.2485(4) 0.1922(9) 0.064(8) Uiso 0.468(15) 1 d PDU H 2 C852 C 0.0964(17) 0.2392(9) 0.186(2) 0.18(3) Uiso 0.468(15) 1 d PDU H 2 H85A H 0.0653 0.2361 0.2227 0.215 Uiso 0.468(15) 1 calc PR H 2 C853 C 0.0657(18) 0.2347(11) 0.127(2) 0.26(4) Uiso 0.468(15) 1 d PDU H 2 H85B H 0.0129 0.2285 0.1238 0.318 Uiso 0.468(15) 1 calc PR H 2 C854 C 0.1080(19) 0.2387(9) 0.072(2) 0.16(2) Uiso 0.468(15) 1 d PDU H 2 H85C H 0.0835 0.2353 0.0327 0.194 Uiso 0.468(15) 1 calc PR H 2 C855 C 0.1869(17) 0.2479(4) 0.0743(11) 0.123(19) Uiso 0.468(15) 1 d PDU H 2 C810 C 0.2087(6) 0.2536(3) 0.2571(4) 0.058(3) Uani 1 1 d DU . . C811 C 0.256(3) 0.2141(13) 0.2555(11) 0.14(2) Uiso 0.45(6) 1 d PDU H 1 H81A H 0.2234 0.1900 0.2473 0.213 Uiso 0.45(6) 1 calc PR H 1 H81B H 0.2819 0.2105 0.2961 0.213 Uiso 0.45(6) 1 calc PR H 1 H81C H 0.2947 0.2164 0.2222 0.213 Uiso 0.45(6) 1 calc PR H 1 C812 C 0.1408(11) 0.247(2) 0.3008(11) 0.120(18) Uiso 0.45(6) 1 d PDU H 1 H81D H 0.1019 0.2303 0.2794 0.179 Uiso 0.45(6) 1 calc PR H 1 H81E H 0.1192 0.2742 0.3125 0.179 Uiso 0.45(6) 1 calc PR H 1 H81F H 0.1577 0.2322 0.3387 0.179 Uiso 0.45(6) 1 calc PR H 1 C813 C 0.256(4) 0.2898(11) 0.2825(16) 0.23(4) Uiso 0.45(6) 1 d PDU H 1 H81G H 0.2229 0.3105 0.3021 0.348 Uiso 0.45(6) 1 calc PR H 1 H81H H 0.2847 0.3028 0.2480 0.348 Uiso 0.45(6) 1 calc PR H 1 H81I H 0.2925 0.2791 0.3139 0.348 Uiso 0.45(6) 1 calc PR H 1 C831 C 0.2231(18) 0.2071(4) 0.2621(9) 0.060(9) Uiso 0.55(6) 1 d PDU H 2 H83A H 0.1756 0.1919 0.2540 0.091 Uiso 0.55(6) 1 calc PR H 2 H83B H 0.2414 0.2004 0.3044 0.091 Uiso 0.55(6) 1 calc PR H 2 H83C H 0.2616 0.1988 0.2312 0.091 Uiso 0.55(6) 1 calc PR H 2 C832 C 0.1494(12) 0.2651(10) 0.3064(6) 0.075(9) Uiso 0.55(6) 1 d PDU H 2 H83D H 0.1021 0.2498 0.2981 0.113 Uiso 0.55(6) 1 calc PR H 2 H83E H 0.1395 0.2952 0.3048 0.113 Uiso 0.55(6) 1 calc PR H 2 H83F H 0.1686 0.2576 0.3481 0.113 Uiso 0.55(6) 1 calc PR H 2 C833 C 0.2819(11) 0.2776(7) 0.2717(9) 0.063(10) Uiso 0.55(6) 1 d PDU H 2 H83G H 0.3161 0.2764 0.2354 0.095 Uiso 0.55(6) 1 calc PR H 2 H83H H 0.3070 0.2650 0.3082 0.095 Uiso 0.55(6) 1 calc PR H 2 H83I H 0.2694 0.3069 0.2809 0.095 Uiso 0.55(6) 1 calc PR H 2 C820 C 0.2302(5) 0.2521(3) 0.0126(4) 0.051(3) Uani 1 1 d DU . . C821 C 0.1907(15) 0.2738(10) -0.0415(7) 0.111(17) Uiso 0.40(5) 1 d PDU H 1 H82A H 0.2254 0.2755 -0.0774 0.166 Uiso 0.40(5) 1 calc PR H 1 H82B H 0.1758 0.3022 -0.0287 0.166 Uiso 0.40(5) 1 calc PR H 1 H82C H 0.1451 0.2580 -0.0534 0.166 Uiso 0.40(5) 1 calc PR H 1 C822 C 0.3147(7) 0.2634(9) 0.0127(9) 0.040(8) Uiso 0.40(5) 1 d PDU H 1 H82D H 0.3324 0.2668 -0.0307 0.060 Uiso 0.40(5) 1 calc PR H 1 H82E H 0.3437 0.2410 0.0330 0.060 Uiso 0.40(5) 1 calc PR H 1 H82F H 0.3222 0.2896 0.0357 0.060 Uiso 0.40(5) 1 calc PR H 1 C823 C 0.2234(17) 0.2047(4) 0.0039(11) 0.052(10) Uiso 0.40(5) 1 d PDU H 1 H82G H 0.2486 0.1965 -0.0353 0.078 Uiso 0.40(5) 1 calc PR H 1 H82H H 0.1695 0.1968 0.0021 0.078 Uiso 0.40(5) 1 calc PR H 1 H82I H 0.2479 0.1904 0.0392 0.078 Uiso 0.40(5) 1 calc PR H 1 C841 C 0.2186(19) 0.2897(7) -0.0318(9) 0.110(12) Uiso 0.60(5) 1 d PDU H 2 H84A H 0.2519 0.2866 -0.0685 0.165 Uiso 0.60(5) 1 calc PR H 2 H84B H 0.2313 0.3156 -0.0097 0.165 Uiso 0.60(5) 1 calc PR H 2 H84C H 0.1653 0.2906 -0.0455 0.165 Uiso 0.60(5) 1 calc PR H 2 C842 C 0.3159(6) 0.2453(10) 0.0199(8) 0.071(7) Uiso 0.60(5) 1 d PDU H 2 H84D H 0.3412 0.2499 -0.0205 0.107 Uiso 0.60(5) 1 calc PR H 2 H84E H 0.3255 0.2166 0.0341 0.107 Uiso 0.60(5) 1 calc PR H 2 H84F H 0.3362 0.2650 0.0510 0.107 Uiso 0.60(5) 1 calc PR H 2 C843 C 0.1947(16) 0.2139(8) -0.0160(12) 0.151(16) Uiso 0.60(5) 1 d PDU H 2 H84G H 0.2132 0.2104 -0.0591 0.226 Uiso 0.60(5) 1 calc PR H 2 H84H H 0.1391 0.2170 -0.0164 0.226 Uiso 0.60(5) 1 calc PR H 2 H84I H 0.2085 0.1892 0.0088 0.226 Uiso 0.60(5) 1 calc PR H 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 Sm 0.02737(18) 0.0350(2) 0.03187(19) -0.0026(3) 0.0016(3) -0.0028(2) Li1 0.022(4) 0.024(4) 0.033(6) 0.004(4) -0.002(3) 0.002(3) Li2 0.045(7) 0.025(4) 0.053(8) -0.005(4) -0.007(5) 0.000(4) Si1 0.0277(13) 0.0190(11) 0.0292(14) -0.0016(9) 0.0001(11) 0.0001(9) Si2 0.0265(13) 0.0279(11) 0.0321(15) -0.0054(9) 0.0009(10) 0.0037(9) Si3 0.0329(14) 0.0231(11) 0.0266(14) -0.0045(9) 0.0080(11) -0.0012(10) Si4 0.0250(13) 0.0216(11) 0.0345(15) -0.0032(10) 0.0003(10) -0.0001(9) Si5 0.0228(12) 0.0219(11) 0.0295(14) -0.0044(9) 0.0014(9) 0.0008(9) Si6 0.0331(13) 0.0234(10) 0.0346(16) 0.0007(10) 0.0000(11) 0.0026(9) Si7 0.0412(15) 0.0217(11) 0.0313(14) 0.0015(10) 0.0084(12) 0.0024(11) Si21 0.0431(16) 0.0311(13) 0.0412(19) -0.0040(11) 0.0001(12) -0.0075(11) Si22 0.0349(15) 0.0235(12) 0.0323(15) -0.0026(10) 0.0072(12) 0.0019(10) Si23 0.057(2) 0.0303(13) 0.0365(17) -0.0085(11) -0.0020(14) -0.0073(13) Si24 0.061(2) 0.0323(14) 0.0427(18) -0.0097(12) 0.0036(15) 0.0043(14) Si25 0.0588(18) 0.0256(12) 0.048(2) -0.0003(11) -0.0032(14) -0.0060(11) Si26 0.0409(16) 0.0241(12) 0.0407(18) -0.0001(10) 0.0066(12) 0.0035(11) Si27 0.0510(18) 0.0287(13) 0.0396(16) 0.0018(11) -0.0009(14) -0.0044(12) O1 0.026(3) 0.028(3) 0.029(3) -0.002(2) 0.004(2) 0.000(2) O2 0.026(3) 0.033(2) 0.038(4) -0.009(3) 0.002(3) 0.004(2) O3 0.044(4) 0.036(3) 0.038(3) 0.002(3) 0.001(3) 0.002(3) O4 0.035(4) 0.023(3) 0.036(4) -0.003(2) 0.004(3) -0.001(2) O5 0.037(4) 0.035(3) 0.038(3) -0.005(3) 0.003(3) 0.003(3) O6 0.025(3) 0.029(3) 0.034(3) 0.000(2) -0.006(2) -0.001(2) O7 0.039(4) 0.032(3) 0.035(4) 0.000(3) 0.003(3) -0.003(3) O8 0.041(3) 0.028(3) 0.038(4) -0.004(3) 0.003(3) -0.001(2) O9 0.033(4) 0.022(3) 0.041(4) -0.007(2) 0.003(3) 0.000(2) O10 0.039(4) 0.026(3) 0.045(4) -0.003(3) -0.008(3) 0.005(3) O11 0.044(4) 0.024(3) 0.044(4) 0.004(3) 0.013(3) 0.004(3) O12 0.025(3) 0.021(3) 0.035(3) -0.002(2) 0.006(3) 0.002(2) O21 0.038(4) 0.034(3) 0.048(5) -0.003(3) -0.004(3) -0.005(2) O22 0.029(4) 0.029(3) 0.034(3) -0.006(2) 0.003(3) -0.003(2) O23 0.054(4) 0.032(3) 0.042(4) 0.001(3) 0.011(3) -0.008(3) O24 0.056(5) 0.048(4) 0.040(4) -0.005(3) -0.002(3) -0.008(3) O25 0.055(5) 0.027(3) 0.037(4) -0.008(3) 0.004(3) -0.002(3) O26 0.061(4) 0.029(3) 0.059(5) 0.005(3) -0.003(4) -0.001(3) O27 0.085(6) 0.026(3) 0.051(5) -0.008(3) -0.006(4) 0.003(3) O28 0.035(4) 0.041(3) 0.039(4) -0.002(3) 0.001(3) 0.002(3) O29 0.064(5) 0.036(4) 0.052(4) -0.003(3) -0.001(4) -0.010(3) O30 0.041(4) 0.043(4) 0.050(4) -0.014(3) 0.015(3) 0.001(3) O31 0.037(3) 0.029(3) 0.036(3) -0.003(2) 0.002(3) -0.001(2) O32 0.057(5) 0.025(3) 0.054(4) 0.000(3) -0.012(3) -0.005(3) O800 0.028(2) 0.063(4) 0.068(4) -0.008(4) 0.006(5) -0.003(3) C10 0.039(5) 0.020(4) 0.043(5) 0.000(3) -0.007(4) 0.003(4) C11 0.054(7) 0.042(5) 0.068(7) 0.005(5) -0.032(5) -0.004(5) C12 0.088(10) 0.077(8) 0.064(7) -0.035(7) -0.036(7) 0.009(7) C13 0.106(12) 0.074(9) 0.041(6) 0.001(5) 0.012(7) 0.010(7) C14 0.104(11) 0.039(6) 0.047(7) 0.010(4) -0.025(7) -0.002(6) C20 0.027(4) 0.046(5) 0.057(7) -0.008(5) -0.004(5) 0.006(3) C21 0.048(7) 0.072(8) 0.070(7) -0.023(7) 0.000(6) 0.028(6) C24 0.042(7) 0.131(14) 0.064(7) 0.018(8) -0.009(6) 0.006(8) C30 0.038(6) 0.045(5) 0.029(4) -0.008(4) 0.007(4) 0.001(5) C31 0.070(8) 0.063(7) 0.025(5) -0.011(5) 0.002(5) 0.006(6) C40 0.032(5) 0.026(4) 0.040(5) -0.005(3) 0.002(4) 0.002(3) C41 0.036(5) 0.041(5) 0.045(6) -0.016(4) 0.010(4) -0.014(4) C42 0.041(5) 0.041(6) 0.070(8) -0.017(5) -0.002(5) -0.010(4) C43 0.067(8) 0.060(7) 0.078(9) -0.034(6) 0.021(7) -0.017(6) C44 0.045(5) 0.038(5) 0.043(6) -0.016(4) 0.002(4) 0.002(4) C50 0.024(3) 0.042(5) 0.045(6) -0.002(4) 0.004(3) 0.003(3) C51 0.029(5) 0.042(6) 0.069(7) -0.006(5) -0.008(5) 0.014(4) C52 0.020(4) 0.048(6) 0.106(9) -0.014(6) 0.002(5) -0.003(4) C53 0.022(5) 0.080(8) 0.081(8) 0.002(6) 0.018(5) -0.002(5) C54 0.022(4) 0.028(5) 0.070(7) -0.009(4) 0.012(4) 0.007(4) C60 0.039(6) 0.029(4) 0.045(6) 0.009(4) 0.004(4) 0.009(4) C61 0.050(6) 0.031(4) 0.060(7) 0.000(4) 0.012(5) 0.020(4) C62 0.081(10) 0.058(7) 0.073(8) -0.021(6) 0.011(7) 0.002(6) C63 0.051(7) 0.040(5) 0.108(11) -0.003(6) 0.008(7) -0.010(5) C64 0.063(8) 0.031(5) 0.091(10) 0.012(5) 0.030(7) -0.001(5) C70 0.043(5) 0.052(5) 0.038(5) 0.002(4) 0.002(4) -0.011(4) C71 0.039(6) 0.085(7) 0.069(8) 0.014(6) 0.019(6) 0.000(6) C72 0.064(9) 0.153(12) 0.060(9) 0.041(9) 0.008(6) -0.047(8) C73 0.096(13) 0.115(9) 0.143(17) 0.040(11) -0.010(10) -0.069(10) C74 0.083(10) 0.057(6) 0.094(11) 0.013(7) -0.012(8) -0.027(6) C210 0.044(5) 0.070(7) 0.059(8) -0.017(6) 0.003(5) -0.020(5) C211 0.055(8) 0.115(12) 0.073(10) -0.022(8) -0.010(7) -0.039(9) C220 0.059(7) 0.022(5) 0.071(6) 0.005(4) 0.039(5) 0.009(4) C221 0.123(13) 0.049(7) 0.063(8) 0.018(5) 0.054(8) 0.036(7) C222 0.119(16) 0.073(11) 0.142(14) -0.008(9) -0.063(13) 0.033(9) C223 0.094(11) 0.060(8) 0.063(7) -0.007(6) 0.019(7) 0.012(7) C224 0.046(7) 0.042(5) 0.070(7) 0.002(5) 0.030(5) 0.014(5) C230 0.066(8) 0.055(6) 0.038(5) -0.001(5) 0.001(5) -0.031(6) C240 0.066(9) 0.081(9) 0.081(10) -0.042(7) 0.000(6) 0.015(7) C250 0.063(7) 0.033(4) 0.064(7) 0.007(5) 0.004(5) -0.010(4) C251 0.079(9) 0.051(6) 0.092(11) -0.004(6) -0.012(7) -0.018(6) C252 0.171(19) 0.073(9) 0.153(19) -0.065(11) -0.050(15) 0.030(12) C254 0.090(10) 0.032(5) 0.151(16) 0.018(7) -0.016(9) 0.001(6) C260 0.043(4) 0.034(4) 0.049(6) 0.001(4) 0.000(4) 0.007(3) C261 0.048(5) 0.033(5) 0.066(7) 0.001(4) 0.006(5) 0.011(4) C262 0.051(6) 0.060(7) 0.084(9) -0.009(6) -0.007(6) -0.005(6) C263 0.034(6) 0.062(7) 0.091(9) -0.014(7) 0.012(6) 0.001(5) C264 0.042(6) 0.063(7) 0.061(6) 0.001(5) 0.007(5) -0.002(5) C270 0.062(5) 0.029(5) 0.054(6) 0.001(4) -0.001(5) 0.008(4) C271 0.046(6) 0.056(6) 0.077(9) -0.007(5) -0.014(6) 0.009(5) C272 0.053(6) 0.052(6) 0.096(10) 0.005(6) 0.008(7) 0.013(5) C273 0.065(7) 0.055(6) 0.088(11) 0.010(6) 0.002(7) 0.013(6) C274 0.068(7) 0.052(6) 0.061(8) -0.004(5) 0.013(6) 0.010(5) Si40 0.0461(16) 0.0366(14) 0.0354(14) 0.0042(11) 0.0001(12) 0.0028(12) C400 0.082(9) 0.039(5) 0.069(8) 0.014(5) -0.011(7) -0.015(5) C401 0.070(8) 0.078(8) 0.038(5) 0.001(5) 0.004(5) 0.017(7) C402 0.039(5) 0.046(5) 0.057(6) -0.002(5) -0.008(4) 0.000(4) C403 0.058(7) 0.065(7) 0.062(6) -0.011(5) -0.016(6) 0.022(7) C404 0.069(9) 0.070(7) 0.110(12) 0.027(7) -0.026(9) -0.020(7) C405 0.043(6) 0.100(9) 0.055(7) -0.009(6) -0.004(5) 0.010(6) C800 0.033(4) 0.077(6) 0.046(4) 0.001(6) 0.013(8) 0.020(5) C810 0.063(8) 0.070(8) 0.040(5) -0.013(5) -0.004(6) -0.006(6) C820 0.054(7) 0.060(7) 0.040(5) -0.009(5) -0.022(5) -0.001(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 Sm O800 2.183(5) . ? Sm O21 2.304(6) . ? Sm O22 2.306(7) . ? Sm O1 2.306(7) . ? Sm O2 2.314(6) . ? Sm Li1 3.006(14) . ? Sm Li2 3.101(17) . ? Li1 O2 1.910(16) . ? Li1 O22 1.911(15) . ? Li1 O12 2.056(15) . ? Li1 O6 2.320(16) . ? Li1 Si5 2.807(14) . ? Li1 Si2 3.127(15) . ? Li2 O1 1.917(16) . ? Li2 O21 1.935(19) . ? Li2 O31 2.098(18) . ? Li2 O23 2.370(18) . ? Li2 Si27 2.855(16) . ? Si1 O1 1.589(7) . ? Si1 O4 1.627(6) . ? Si1 O6 1.665(7) . ? Si1 C10 1.873(10) . ? Si2 O2 1.592(6) . ? Si2 O5 1.622(8) . ? Si2 O8 1.642(7) . ? Si2 C20 1.867(9) . ? Si3 O7 1.604(7) . ? Si3 O5 1.612(8) . ? Si3 O4 1.621(6) . ? Si3 C30 1.881(10) . ? Si4 O10 1.611(7) . ? Si4 O9 1.623(6) . ? Si4 O7 1.637(7) . ? Si4 C40 1.845(9) . ? Si5 O6 1.604(6) . ? Si5 O9 1.609(6) . ? Si5 O12 1.665(7) . ? Si5 C50 1.877(9) . ? Si6 O8 1.608(6) . ? Si6 O11 1.633(7) . ? Si6 O10 1.635(7) . ? Si6 C60 1.838(9) . ? Si7 O3 1.597(7) . ? Si7 O11 1.611(7) . ? Si7 O12 1.656(6) . ? Si7 C70 1.864(9) . ? Si21 O21 1.603(7) . ? Si21 O26 1.609(7) . ? Si21 O24 1.637(8) . ? Si21 C210 1.870(11) . ? Si22 O22 1.581(7) . ? Si22 O25 1.627(7) . ? Si22 O28 1.648(8) . ? Si22 C220 1.867(10) . ? Si23 O24 1.607(9) . ? Si23 O25 1.621(7) . ? Si23 O27 1.644(9) . ? Si23 C230 1.840(12) . ? Si24 O27 1.569(9) . ? Si24 O29 1.618(8) . ? Si24 O30 1.626(8) . ? Si24 C240 1.798(11) . ? Si25 O29 1.595(9) . ? Si25 O32 1.613(8) . ? Si25 O26 1.626(7) . ? Si25 C250 1.834(11) . ? Si26 O28 1.597(7) . ? Si26 O30 1.622(7) . ? Si26 O31 1.660(7) . ? Si26 C260 1.854(10) . ? Si27 O32 1.628(7) . ? Si27 O23 1.631(7) . ? Si27 O31 1.648(7) . ? Si27 C270 1.829(11) . ? O3 Si40 1.655(7) . ? O23 Si50 1.691(9) . ? O23 Si70 1.697(11) . ? O800 C800 1.268(8) . ? C10 C14 1.546(12) . ? C10 C11 1.565(12) . ? C11 C12 1.477(15) . ? C12 C13 1.51(2) . ? C13 C14 1.453(14) . ? C20 C24 1.527(18) . ? C20 C21 1.553(15) . ? C21 C26 1.523(10) . ? C21 C22 1.526(9) . ? C22 C23 1.504(10) . ? C23 C24 1.514(10) . ? C26 C27 1.521(10) . ? C27 C24 1.537(10) . ? C30 C34 1.520(7) . ? C30 C31 1.540(8) . ? C30 C38 1.58(2) . ? C31 C32 1.518(10) . ? C31 C36 1.63(3) . ? C32 C33 1.527(9) . ? C33 C34 1.509(9) . ? C36 C37 1.554(18) . ? C37 C38 1.497(18) . ? C40 C44 1.534(8) . ? C40 C41 1.544(8) . ? C41 C42 1.529(6) . ? C42 C43 1.525(7) . ? C43 C44 1.530(7) . ? C50 C51 1.522(12) . ? C50 C54 1.529(11) . ? C51 C52 1.534(12) . ? C52 C53 1.515(18) . ? C53 C54 1.551(12) . ? C60 C64 1.540(12) . ? C60 C61 1.548(12) . ? C61 C62 1.474(14) . ? C62 C63 1.49(2) . ? C63 C64 1.455(13) . ? C70 C71 1.528(8) . ? C70 C74 1.532(8) . ? C71 C72 1.517(8) . ? C72 C73 1.523(8) . ? C73 C74 1.526(8) . ? C210 C218 1.513(10) . ? C210 C211 1.550(12) . ? C210 C214 1.560(14) . ? C211 C212 1.516(8) . ? C211 C216 1.536(9) . ? C212 C213 1.520(9) . ? C213 C214 1.525(8) . ? C216 C217 1.538(15) . ? C217 C218 1.544(16) . ? C220 C221 1.530(7) . ? C220 C224 1.545(11) . ? C221 C222 1.513(8) . ? C222 C223 1.530(8) . ? C223 C224 1.543(11) . ? C230 C234 1.519(7) . ? C230 C231 1.522(9) . ? C230 C238 1.524(10) . ? C230 C235 1.532(10) . ? C231 C232 1.529(6) . ? C232 C233 1.526(7) . ? C233 C234 1.528(6) . ? C235 C236 1.521(8) . ? C236 C237 1.536(13) . ? C237 C238 1.556(14) . ? C240 C248 1.505(9) . ? C240 C241 1.512(9) . ? C240 C244 1.517(9) . ? C240 C245 1.524(9) . ? C241 C242 1.532(6) . ? C242 C243 1.528(7) . ? C243 C244 1.531(6) . ? C245 C246 1.532(6) . ? C246 C247 1.532(7) . ? C247 C248 1.533(6) . ? C250 C254 1.535(18) . ? C250 C251 1.564(18) . ? C251 C252 1.464(19) . ? C252 C253 1.513(9) . ? C252 C257 1.517(10) . ? C253 C254 1.522(9) . ? C257 C254 1.522(10) . ? C260 C261 1.513(8) . ? C260 C264 1.524(9) . ? C261 C262 1.555(16) . ? C262 C263 1.494(18) . ? C263 C264 1.542(16) . ? C270 C271 1.534(15) . ? C270 C274 1.564(15) . ? C271 C272 1.529(16) . ? C272 C273 1.530(17) . ? C273 C274 1.534(18) . ? Si40 C401 1.847(10) . ? Si40 C402 1.880(10) . ? Si40 C400 1.883(10) . ? C402 C403 1.524(11) . ? C402 C404 1.529(11) . ? C402 C405 1.532(11) . ? Si50 C501 1.854(14) . ? Si50 C502 1.878(14) . ? Si50 C500 1.889(16) . ? C502 C504 1.521(13) . ? C502 C503 1.521(13) . ? C502 C505 1.536(13) . ? Si70 C701 1.846(15) . ? Si70 C700 1.871(17) . ? Si70 C702 1.872(15) . ? C702 C704 1.509(13) . ? C702 C703 1.530(13) . ? C702 C705 1.534(14) . ? C800 C805 1.437(9) . ? C800 C801 1.440(9) . ? C800 C851 1.443(11) . ? C800 C855 1.44(2) . ? C801 C802 1.417(19) . ? C801 C810 1.509(8) . ? C802 C803 1.38(2) . ? C803 C804 1.39(2) . ? C804 C805 1.423(19) . ? C805 C820 1.508(8) . ? C851 C852 1.42(2) . ? C851 C810 1.51(3) . ? C852 C853 1.38(2) . ? C853 C854 1.39(2) . ? C854 C855 1.42(2) . ? C855 C820 1.52(3) . ? C810 C831 1.511(8) . ? C810 C811 1.513(7) . ? C810 C832 1.522(9) . ? C810 C813 1.527(7) . ? C810 C812 1.527(7) . ? C810 C833 1.528(9) . ? C820 C843 1.502(8) . ? C820 C821 1.513(7) . ? C820 C822 1.524(7) . ? C820 C842 1.527(8) . ? C820 C823 1.532(8) . ? C820 C841 1.540(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O800 Sm O21 96.2(3) . . ? O800 Sm O22 136.9(4) . . ? O21 Sm O22 95.4(2) . . ? O800 Sm O1 134.3(4) . . ? O21 Sm O1 76.3(2) . . ? O22 Sm O1 88.78(19) . . ? O800 Sm O2 96.5(2) . . ? O21 Sm O2 166.96(19) . . ? O22 Sm O2 77.1(2) . . ? O1 Sm O2 92.8(2) . . ? O800 Sm Li1 129.9(4) . . ? O21 Sm Li1 130.1(3) . . ? O22 Sm Li1 39.5(3) . . ? O1 Sm Li1 81.8(3) . . ? O2 Sm Li1 39.4(3) . . ? O800 Sm Li2 124.1(4) . . ? O21 Sm Li2 38.5(3) . . ? O22 Sm Li2 88.9(4) . . ? O1 Sm Li2 38.1(3) . . ? O2 Sm Li2 129.6(3) . . ? Li1 Sm Li2 105.6(4) . . ? O2 Li1 O22 97.7(7) . . ? O2 Li1 O12 126.7(8) . . ? O22 Li1 O12 134.9(8) . . ? O2 Li1 O6 93.9(7) . . ? O22 Li1 O6 102.0(6) . . ? O12 Li1 O6 70.9(5) . . ? O2 Li1 Si5 113.6(7) . . ? O22 Li1 Si5 124.0(7) . . ? O12 Li1 Si5 36.0(3) . . ? O6 Li1 Si5 34.8(3) . . ? O2 Li1 Sm 50.3(4) . . ? O22 Li1 Sm 50.1(4) . . ? O12 Li1 Sm 159.6(7) . . ? O6 Li1 Sm 88.8(5) . . ? Si5 Li1 Sm 123.6(5) . . ? O2 Li1 Si2 24.2(3) . . ? O22 Li1 Si2 121.8(6) . . ? O12 Li1 Si2 103.0(5) . . ? O6 Li1 Si2 90.5(5) . . ? Si5 Li1 Si2 97.9(4) . . ? Sm Li1 Si2 74.1(3) . . ? O1 Li2 O21 95.3(8) . . ? O1 Li2 O31 129.4(9) . . ? O21 Li2 O31 114.6(8) . . ? O1 Li2 O23 131.5(9) . . ? O21 Li2 O23 118.8(8) . . ? O31 Li2 O23 68.5(5) . . ? O1 Li2 Si27 148.4(9) . . ? O21 Li2 Si27 116.1(7) . . ? O31 Li2 Si27 34.8(3) . . ? O23 Li2 Si27 34.8(3) . . ? O1 Li2 Sm 47.9(4) . . ? O21 Li2 Sm 47.8(4) . . ? O31 Li2 Sm 136.1(8) . . ? O23 Li2 Sm 153.2(8) . . ? Si27 Li2 Sm 161.8(6) . . ? O1 Si1 O4 110.3(4) . . ? O1 Si1 O6 109.1(3) . . ? O4 Si1 O6 107.7(3) . . ? O1 Si1 C10 115.0(4) . . ? O4 Si1 C10 107.6(4) . . ? O6 Si1 C10 106.8(4) . . ? O2 Si2 O5 110.9(4) . . ? O2 Si2 O8 109.2(4) . . ? O5 Si2 O8 105.6(4) . . ? O2 Si2 C20 114.8(4) . . ? O5 Si2 C20 107.7(5) . . ? O8 Si2 C20 108.2(4) . . ? O2 Si2 Li1 29.5(3) . . ? O5 Si2 Li1 112.0(4) . . ? O8 Si2 Li1 81.0(3) . . ? C20 Si2 Li1 135.0(5) . . ? O7 Si3 O5 109.1(4) . . ? O7 Si3 O4 108.4(4) . . ? O5 Si3 O4 109.5(4) . . ? O7 Si3 C30 108.6(4) . . ? O5 Si3 C30 109.7(4) . . ? O4 Si3 C30 111.6(4) . . ? O10 Si4 O9 108.1(4) . . ? O10 Si4 O7 108.8(4) . . ? O9 Si4 O7 109.7(3) . . ? O10 Si4 C40 110.6(4) . . ? O9 Si4 C40 109.3(3) . . ? O7 Si4 C40 110.4(4) . . ? O6 Si5 O9 110.5(4) . . ? O6 Si5 O12 102.3(3) . . ? O9 Si5 O12 108.9(3) . . ? O6 Si5 C50 111.7(4) . . ? O9 Si5 C50 109.9(4) . . ? O12 Si5 C50 113.3(4) . . ? O6 Si5 Li1 55.7(4) . . ? O9 Si5 Li1 122.0(4) . . ? O12 Si5 Li1 46.6(4) . . ? C50 Si5 Li1 127.9(4) . . ? O8 Si6 O11 107.4(4) . . ? O8 Si6 O10 111.1(4) . . ? O11 Si6 O10 108.5(4) . . ? O8 Si6 C60 113.6(4) . . ? O11 Si6 C60 108.7(4) . . ? O10 Si6 C60 107.3(4) . . ? O3 Si7 O11 109.0(4) . . ? O3 Si7 O12 105.8(3) . . ? O11 Si7 O12 109.7(3) . . ? O3 Si7 C70 112.8(4) . . ? O11 Si7 C70 109.1(4) . . ? O12 Si7 C70 110.3(4) . . ? O21 Si21 O26 110.7(4) . . ? O21 Si21 O24 110.2(4) . . ? O26 Si21 O24 106.8(4) . . ? O21 Si21 C210 114.8(4) . . ? O26 Si21 C210 108.3(5) . . ? O24 Si21 C210 105.5(5) . . ? O22 Si22 O25 109.8(4) . . ? O22 Si22 O28 108.5(4) . . ? O25 Si22 O28 108.9(4) . . ? O22 Si22 C220 115.2(4) . . ? O25 Si22 C220 107.3(4) . . ? O28 Si22 C220 106.9(4) . . ? O24 Si23 O25 109.6(4) . . ? O24 Si23 O27 109.7(4) . . ? O25 Si23 O27 108.2(4) . . ? O24 Si23 C230 108.0(5) . . ? O25 Si23 C230 110.8(4) . . ? O27 Si23 C230 110.6(5) . . ? O27 Si24 O29 110.5(5) . . ? O27 Si24 O30 109.6(4) . . ? O29 Si24 O30 107.0(4) . . ? O27 Si24 C240 110.2(5) . . ? O29 Si24 C240 111.1(6) . . ? O30 Si24 C240 108.4(5) . . ? O29 Si25 O32 108.7(4) . . ? O29 Si25 O26 110.5(4) . . ? O32 Si25 O26 107.4(4) . . ? O29 Si25 C250 108.4(5) . . ? O32 Si25 C250 109.2(5) . . ? O26 Si25 C250 112.7(5) . . ? O28 Si26 O30 111.2(4) . . ? O28 Si26 O31 106.6(4) . . ? O30 Si26 O31 107.9(4) . . ? O28 Si26 C260 113.0(4) . . ? O30 Si26 C260 107.7(4) . . ? O31 Si26 C260 110.4(4) . . ? O32 Si27 O23 110.1(4) . . ? O32 Si27 O31 109.8(4) . . ? O23 Si27 O31 100.6(4) . . ? O32 Si27 C270 108.3(4) . . ? O23 Si27 C270 113.2(5) . . ? O31 Si27 C270 114.6(5) . . ? O32 Si27 Li2 110.2(4) . . ? O23 Si27 Li2 56.1(4) . . ? O31 Si27 Li2 46.6(4) . . ? C270 Si27 Li2 141.2(5) . . ? Si1 O1 Li2 136.1(7) . . ? Si1 O1 Sm 126.5(4) . . ? Li2 O1 Sm 94.0(6) . . ? Si2 O2 Li1 126.3(5) . . ? Si2 O2 Sm 141.8(4) . . ? Li1 O2 Sm 90.2(5) . . ? Si7 O3 Si40 143.0(4) . . ? Si3 O4 Si1 147.3(4) . . ? Si3 O5 Si2 148.3(5) . . ? Si5 O6 Si1 148.1(4) . . ? Si5 O6 Li1 89.4(5) . . ? Si1 O6 Li1 120.4(5) . . ? Si3 O7 Si4 143.3(5) . . ? Si6 O8 Si2 154.9(5) . . ? Si5 O9 Si4 151.7(5) . . ? Si4 O10 Si6 140.1(4) . . ? Si7 O11 Si6 142.4(4) . . ? Si7 O12 Si5 133.5(4) . . ? Si7 O12 Li1 123.9(5) . . ? Si5 O12 Li1 97.4(5) . . ? Si21 O21 Li2 130.3(6) . . ? Si21 O21 Sm 135.7(4) . . ? Li2 O21 Sm 93.6(5) . . ? Si22 O22 Li1 136.1(6) . . ? Si22 O22 Sm 129.3(4) . . ? Li1 O22 Sm 90.5(5) . . ? Si27 O23 Si50 146.1(5) . . ? Si27 O23 Si70 142.1(5) . . ? Si50 O23 Si70 28.8(3) . . ? Si27 O23 Li2 89.0(5) . . ? Si50 O23 Li2 124.5(6) . . ? Si70 O23 Li2 117.4(6) . . ? Si23 O24 Si21 148.1(6) . . ? Si23 O25 Si22 150.0(5) . . ? Si21 O26 Si25 154.4(6) . . ? Si24 O27 Si23 144.3(6) . . ? Si26 O28 Si22 156.1(5) . . ? Si25 O29 Si24 142.9(5) . . ? Si26 O30 Si24 151.6(5) . . ? Si27 O31 Si26 141.2(4) . . ? Si27 O31 Li2 98.6(6) . . ? Si26 O31 Li2 116.1(6) . . ? Si25 O32 Si27 141.2(5) . . ? C800 O800 Sm 170.5(6) . . ? C14 C10 C11 103.3(9) . . ? C14 C10 Si1 114.1(8) . . ? C11 C10 Si1 113.0(6) . . ? C12 C11 C10 106.9(9) . . ? C11 C12 C13 107.4(8) . . ? C14 C13 C12 107.5(10) . . ? C13 C14 C10 105.3(8) . . ? C24 C20 C21 104.9(9) . . ? C24 C20 Si2 118.3(9) . . ? C21 C20 Si2 110.7(8) . . ? C26 C21 C22 29(5) . . ? C26 C21 C20 91(4) . . ? C22 C21 C20 106.1(12) . . ? C23 C22 C21 94.7(16) . . ? C22 C23 C24 110.8(16) . . ? C27 C26 C21 104.7(19) . . ? C26 C27 C24 103(3) . . ? C23 C24 C20 101.5(14) . . ? C23 C24 C27 33.3(15) . . ? C20 C24 C27 101.3(13) . . ? C34 C30 C31 98.2(12) . . ? C34 C30 C38 17.5(13) . . ? C31 C30 C38 111.9(11) . . ? C34 C30 Si3 109.4(11) . . ? C31 C30 Si3 112.3(7) . . ? C38 C30 Si3 111.6(9) . . ? C32 C31 C30 106.4(12) . . ? C32 C31 C36 26.7(11) . . ? C30 C31 C36 100.1(10) . . ? C31 C32 C33 100.9(17) . . ? C34 C33 C32 104.2(16) . . ? C33 C34 C30 111.5(15) . . ? C37 C36 C31 104.3(15) . . ? C38 C37 C36 104.9(16) . . ? C37 C38 C30 100.6(14) . . ? C44 C40 C41 103.6(6) . . ? C44 C40 Si4 116.5(6) . . ? C41 C40 Si4 113.4(6) . . ? C42 C41 C40 103.3(6) . . ? C43 C42 C41 105.4(5) . . ? C42 C43 C44 107.5(5) . . ? C43 C44 C40 105.4(6) . . ? C51 C50 C54 106.8(8) . . ? C51 C50 Si5 115.0(6) . . ? C54 C50 Si5 117.5(6) . . ? C50 C51 C52 102.8(7) . . ? C53 C52 C51 103.9(8) . . ? C52 C53 C54 106.4(8) . . ? C50 C54 C53 105.0(8) . . ? C64 C60 C61 103.9(8) . . ? C64 C60 Si6 114.7(7) . . ? C61 C60 Si6 113.5(6) . . ? C62 C61 C60 105.5(8) . . ? C61 C62 C63 105.7(9) . . ? C64 C63 C62 103.9(9) . . ? C63 C64 C60 106.0(8) . . ? C71 C70 C74 102.3(7) . . ? C71 C70 Si7 117.5(7) . . ? C74 C70 Si7 113.0(7) . . ? C72 C71 C70 104.0(8) . . ? C71 C72 C73 105.1(9) . . ? C72 C73 C74 105.7(7) . . ? C73 C74 C70 107.4(7) . . ? C218 C210 C211 109.5(14) . . ? C218 C210 C214 21.6(19) . . ? C211 C210 C214 100.8(9) . . ? C218 C210 Si21 122.2(13) . . ? C211 C210 Si21 113.0(8) . . ? C214 C210 Si21 111.7(11) . . ? C212 C211 C216 38(3) . . ? C212 C211 C210 110.6(11) . . ? C216 C211 C210 98.9(11) . . ? C211 C212 C213 106.1(13) . . ? C212 C213 C214 104.6(14) . . ? C213 C214 C210 107.4(12) . . ? C211 C216 C217 112.3(15) . . ? C216 C217 C218 104.1(16) . . ? C210 C218 C217 103.4(16) . . ? C221 C220 C224 104.1(6) . . ? C221 C220 Si22 111.4(8) . . ? C224 C220 Si22 112.9(7) . . ? C222 C221 C220 108.7(6) . . ? C221 C222 C223 103.6(7) . . ? C222 C223 C224 106.8(7) . . ? C223 C224 C220 107.7(6) . . ? C234 C230 C231 107.8(9) . . ? C234 C230 C238 6(2) . . ? C231 C230 C238 113.2(11) . . ? C234 C230 C235 99.6(11) . . ? C231 C230 C235 21.3(16) . . ? C238 C230 C235 106.0(12) . . ? C234 C230 Si23 114.8(14) . . ? C231 C230 Si23 119.1(13) . . ? C238 C230 Si23 113.3(19) . . ? C235 C230 Si23 107.9(11) . . ? C230 C231 C232 103.2(14) . . ? C233 C232 C231 107.7(5) . . ? C232 C233 C234 107.8(5) . . ? C230 C234 C233 103.3(11) . . ? C236 C235 C230 104.9(10) . . ? C235 C236 C237 107.8(8) . . ? C236 C237 C238 105.8(7) . . ? C230 C238 C237 106.6(8) . . ? C248 C240 C241 96.2(17) . . ? C248 C240 C244 79.7(16) . . ? C241 C240 C244 107.7(9) . . ? C248 C240 C245 107.6(5) . . ? C241 C240 C245 51.7(19) . . ? C244 C240 C245 61.3(18) . . ? C248 C240 Si24 134.3(10) . . ? C241 C240 Si24 117.4(10) . . ? C244 C240 Si24 114.3(10) . . ? C245 C240 Si24 117.3(9) . . ? C240 C241 C242 105.0(8) . . ? C243 C242 C241 107.2(5) . . ? C242 C243 C244 107.0(5) . . ? C240 C244 C243 102.9(8) . . ? C240 C245 C246 108.3(6) . . ? C247 C246 C245 106.9(5) . . ? C246 C247 C248 107.0(5) . . ? C240 C248 C247 108.9(6) . . ? C254 C250 C251 104.4(10) . . ? C254 C250 Si25 112.9(9) . . ? C251 C250 Si25 113.4(8) . . ? C252 C251 C250 108.6(11) . . ? C251 C252 C253 107.4(12) . . ? C251 C252 C257 101(4) . . ? C253 C252 C257 34(4) . . ? C252 C253 C254 107.4(12) . . ? C252 C257 C254 107.1(15) . . ? C253 C254 C257 34(4) . . ? C253 C254 C250 104.5(11) . . ? C257 C254 C250 104(3) . . ? C261 C260 C264 102.7(8) . . ? C261 C260 Si26 116.4(7) . . ? C264 C260 Si26 115.3(7) . . ? C260 C261 C262 102.6(8) . . ? C263 C262 C261 106.5(10) . . ? C262 C263 C264 106.2(10) . . ? C260 C264 C263 104.8(9) . . ? C271 C270 C274 105.8(10) . . ? C271 C270 Si27 117.8(7) . . ? C274 C270 Si27 113.8(8) . . ? C272 C271 C270 107.4(10) . . ? C271 C272 C273 104.1(11) . . ? C272 C273 C274 105.1(10) . . ? C273 C274 C270 101.0(10) . . ? O3 Si40 C401 108.1(5) . . ? O3 Si40 C402 109.9(4) . . ? C401 Si40 C402 111.1(5) . . ? O3 Si40 C400 108.4(5) . . ? C401 Si40 C400 110.3(6) . . ? C402 Si40 C400 108.9(5) . . ? C403 C402 C404 109.0(9) . . ? C403 C402 C405 110.0(9) . . ? C404 C402 C405 107.9(10) . . ? C403 C402 Si40 109.5(7) . . ? C404 C402 Si40 110.5(8) . . ? C405 C402 Si40 109.9(7) . . ? O23 Si50 C501 106.2(8) . . ? O23 Si50 C502 108.7(6) . . ? C501 Si50 C502 112.0(8) . . ? O23 Si50 C500 110.1(9) . . ? C501 Si50 C500 112.3(11) . . ? C502 Si50 C500 107.5(8) . . ? C504 C502 C503 112.6(14) . . ? C504 C502 C505 107.7(14) . . ? C503 C502 C505 109.8(15) . . ? C504 C502 Si50 111.8(12) . . ? C503 C502 Si50 108.1(13) . . ? C505 C502 Si50 106.6(12) . . ? O23 Si70 C701 103.0(11) . . ? O23 Si70 C700 110.4(13) . . ? C701 Si70 C700 113.4(13) . . ? O23 Si70 C702 107.6(8) . . ? C701 Si70 C702 113.2(11) . . ? C700 Si70 C702 109.1(11) . . ? C704 C702 C703 112.2(17) . . ? C704 C702 C705 107.7(16) . . ? C703 C702 C705 106.6(16) . . ? C704 C702 Si70 112.9(16) . . ? C703 C702 Si70 109.5(15) . . ? C705 C702 Si70 107.6(14) . . ? O800 C800 C805 113.0(10) . . ? O800 C800 C801 119.6(10) . . ? C805 C800 C801 122.8(7) . . ? O800 C800 C851 119.7(14) . . ? C805 C800 C851 127.3(12) . . ? C801 C800 C851 21.5(6) . . ? O800 C800 C855 114.1(15) . . ? C805 C800 C855 20.7(7) . . ? C801 C800 C855 126.3(13) . . ? C851 C800 C855 121.5(12) . . ? C802 C801 C800 117.6(11) . . ? C802 C801 C810 119.7(12) . . ? C800 C801 C810 122.7(9) . . ? C803 C802 C801 119(2) . . ? C802 C803 C804 124(2) . . ? C803 C804 C805 120.1(18) . . ? C804 C805 C800 116.3(10) . . ? C804 C805 C820 116.8(12) . . ? C800 C805 C820 126.8(9) . . ? C852 C851 C800 118.8(15) . . ? C852 C851 C810 119(2) . . ? C800 C851 C810 122.4(19) . . ? C853 C852 C851 119(2) . . ? C852 C853 C854 124(3) . . ? C853 C854 C855 121(2) . . ? C854 C855 C800 116.6(14) . . ? C854 C855 C820 119(2) . . ? C800 C855 C820 125(2) . . ? C801 C810 C851 20.5(5) . . ? C801 C810 C831 110.9(7) . . ? C851 C810 C831 91.3(8) . . ? C801 C810 C811 111.2(7) . . ? C851 C810 C811 96.0(11) . . ? C831 C810 C811 24(2) . . ? C801 C810 C832 110.5(8) . . ? C851 C810 C832 113.0(11) . . ? C831 C810 C832 107.5(12) . . ? C811 C810 C832 126.3(17) . . ? C801 C810 C813 108.7(7) . . ? C851 C810 C813 128.4(10) . . ? C831 C810 C813 128.8(18) . . ? C811 C810 C813 109.5(7) . . ? C832 C810 C813 87(2) . . ? C801 C810 C812 109.7(7) . . ? C851 C810 C812 103.8(14) . . ? C831 C810 C812 87(2) . . ? C811 C810 C812 109.2(7) . . ? C832 C810 C812 23(2) . . ? C813 C810 C812 108.4(7) . . ? C801 C810 C833 109.8(7) . . ? C851 C810 C833 124.6(10) . . ? C831 C810 C833 109.8(12) . . ? C811 C810 C833 88(2) . . ? C832 C810 C833 108.2(13) . . ? C813 C810 C833 24(3) . . ? C812 C810 C833 126.9(19) . . ? C843 C820 C805 112.1(7) . . ? C843 C820 C821 82.8(13) . . ? C805 C820 C821 110.8(7) . . ? C843 C820 C822 126.6(11) . . ? C805 C820 C822 110.8(7) . . ? C821 C820 C822 109.8(7) . . ? C843 C820 C855 94.0(11) . . ? C805 C820 C855 19.7(6) . . ? C821 C820 C855 118.0(11) . . ? C822 C820 C855 120.3(12) . . ? C843 C820 C842 109.5(7) . . ? C805 C820 C842 111.4(7) . . ? C821 C820 C842 126.5(11) . . ? C822 C820 C842 22.7(11) . . ? C855 C820 C842 112.9(12) . . ? C843 C820 C823 27.5(13) . . ? C805 C820 C823 108.3(7) . . ? C821 C820 C823 109.0(7) . . ? C822 C820 C823 108.0(7) . . ? C855 C820 C823 88.7(8) . . ? C842 C820 C823 87.0(11) . . ? C843 C820 C841 109.2(7) . . ? C805 C820 C841 106.7(7) . . ? C821 C820 C841 27.8(13) . . ? C822 C820 C841 86.9(11) . . ? C855 C820 C841 122.2(8) . . ? C842 C820 C841 107.7(7) . . ? C823 C820 C841 133.3(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.92 _refine_diff_density_min -2.07 _refine_diff_density_rms 0.12 #=== END