# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Taylor, P.' _publ_contact_author_name 'Taylor, P.' _publ_contact_author_email p.g.taylor@open.ac.uk _publ_section_title ; Further studies of fluoride ion entrapment in octasilsesquioxane cages; X-ray crystal structure studies and factors that affect their formation ; # Attachment '- Cif Files.cif' data_compound3 #TrackingRef '- Cif Files.cif' _database_code_depnum_ccdc_archive 'CCDC 835362' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H68 Cl8 F N O12 Si8' _chemical_formula_sum 'C64 H68 Cl8 F N O12 Si8' _chemical_formula_weight 1570.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 27.2513(11) _cell_length_b 21.4772(9) _cell_length_c 12.7007(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.431(2) _cell_angle_gamma 90.00 _cell_volume 7230.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11587 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3248 _exptl_absorpt_coefficient_mu 0.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9418 _exptl_absorpt_correction_T_max 0.9800 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39431 _diffrn_reflns_av_R_equivalents 0.0938 _diffrn_reflns_av_sigmaI/netI 0.1316 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.03 _reflns_number_total 12430 _reflns_number_gt 6506 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+100.9870P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12430 _refine_ls_number_parameters 1004 _refine_ls_number_restraints 877 _refine_ls_R_factor_all 0.2399 _refine_ls_R_factor_gt 0.1427 _refine_ls_wR_factor_ref 0.2777 _refine_ls_wR_factor_gt 0.2307 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.0532(3) 0.4971(5) 0.3649(7) 0.031(2) Uani 1 1 d U . . C12 C 0.0531(4) 0.5495(5) 0.4273(8) 0.045(3) Uani 1 1 d U . . H12 H 0.0423 0.5881 0.3928 0.054 Uiso 1 1 calc R . . C13 C 0.0684(4) 0.5474(6) 0.5396(9) 0.053(3) Uani 1 1 d U . . H13 H 0.0670 0.5840 0.5808 0.063 Uiso 1 1 calc R . . C14 C 0.0851(4) 0.4935(5) 0.5905(8) 0.042(2) Uani 1 1 d U . . C15 C 0.0862(4) 0.4389(5) 0.5316(9) 0.052(3) Uani 1 1 d U . . H15 H 0.0981 0.4010 0.5670 0.062 Uiso 1 1 calc R . . C16 C 0.0694(4) 0.4415(5) 0.4198(9) 0.047(3) Uani 1 1 d U . . H16 H 0.0689 0.4042 0.3791 0.056 Uiso 1 1 calc R . . C21 C 0.1683(3) 0.5049(4) 0.0874(7) 0.034(2) Uani 1 1 d U . . C22 C 0.1957(4) 0.5593(5) 0.0968(8) 0.039(3) Uani 1 1 d U . . H22 H 0.1780 0.5969 0.0737 0.046 Uiso 1 1 calc R . . C23 C 0.2471(4) 0.5629(5) 0.1377(9) 0.047(3) Uani 1 1 d U . . H23 H 0.2643 0.6017 0.1432 0.057 Uiso 1 1 calc R . . C24 C 0.2727(4) 0.5085(5) 0.1702(9) 0.052(3) Uani 1 1 d U . . C25 C 0.2479(4) 0.4513(5) 0.1574(10) 0.052(3) Uani 1 1 d U . . H25 H 0.2659 0.4135 0.1768 0.063 Uiso 1 1 calc R . . C26 C 0.1970(4) 0.4514(5) 0.1162(9) 0.045(3) Uani 1 1 d U . . H26 H 0.1800 0.4124 0.1065 0.054 Uiso 1 1 calc R . . C31 C -0.0538(4) 0.3252(4) 0.1334(8) 0.034(2) Uani 1 1 d U . . C32 C -0.0862(5) 0.2840(5) 0.0677(9) 0.061(4) Uani 1 1 d U . . H32 H -0.0968 0.2930 -0.0074 0.073 Uiso 1 1 calc R . . C33 C -0.1040(5) 0.2294(5) 0.1073(9) 0.064(4) Uani 1 1 d U . . H33 H -0.1262 0.2020 0.0601 0.077 Uiso 1 1 calc R . . C34 C -0.0887(5) 0.2171(4) 0.2142(9) 0.048(3) Uani 1 1 d U . . C35 C -0.0569(5) 0.2557(5) 0.2837(10) 0.062(4) Uani 1 1 d U . . H35 H -0.0471 0.2465 0.3588 0.075 Uiso 1 1 calc R . . C36 C -0.0393(4) 0.3091(5) 0.2421(9) 0.047(3) Uani 1 1 d U . . H36 H -0.0164 0.3355 0.2899 0.056 Uiso 1 1 calc R . . C41 C 0.0590(3) 0.3325(4) -0.1441(7) 0.028(2) Uani 1 1 d U . . C42 C 0.0857(4) 0.2876(4) -0.0768(8) 0.031(2) Uani 1 1 d U . . H42 H 0.0917 0.2928 -0.0006 0.037 Uiso 1 1 calc R . . C43 C 0.1040(4) 0.2354(5) -0.1174(8) 0.041(3) Uani 1 1 d U . . H43 H 0.1215 0.2046 -0.0692 0.049 Uiso 1 1 calc R . . C44 C 0.0971(4) 0.2274(4) -0.2273(8) 0.038(3) Uani 1 1 d U . . C45 C 0.0713(5) 0.2706(6) -0.2955(9) 0.068(4) Uani 1 1 d U . . H45 H 0.0661 0.2655 -0.3716 0.082 Uiso 1 1 calc R . . C46 C 0.0524(4) 0.3228(5) -0.2534(9) 0.056(3) Uani 1 1 d U . . H46 H 0.0342 0.3529 -0.3021 0.067 Uiso 1 1 calc R . . O1 O 0.0825(2) 0.4997(3) 0.1651(4) 0.0288(13) Uani 1 1 d U . . O2 O 0.0840(2) 0.4400(3) -0.0216(5) 0.0336(16) Uani 1 1 d U . . O3 O 0.0820(2) 0.5663(3) -0.0162(5) 0.0317(16) Uani 1 1 d U . . O4 O 0.0023(3) 0.3739(3) -0.0033(5) 0.0327(14) Uani 1 1 d U . . O5 O 0.0010(2) 0.4344(3) 0.1826(5) 0.0324(16) Uani 1 1 d U . . O6 O -0.0006(2) 0.5604(3) 0.1867(5) 0.0317(16) Uani 1 1 d U . . F1 F 0.0000 0.5000 0.0000 0.0381(18) Uani 1 2 d S . . Si1 Si 0.03263(10) 0.49779(12) 0.21489(19) 0.0301(6) Uani 1 1 d U . . Si2 Si 0.09863(10) 0.50250(12) 0.04968(19) 0.0295(6) Uani 1 1 d U . . Si3 Si -0.03121(11) 0.39674(11) 0.0797(2) 0.0310(7) Uani 1 1 d U . . Si4 Si 0.03461(11) 0.40136(12) -0.0855(2) 0.0312(7) Uani 1 1 d U . . Cl17 Cl 0.10552(12) 0.49147(17) 0.7313(2) 0.0646(9) Uani 1 1 d . . . Cl27 Cl 0.33678(13) 0.51174(18) 0.2290(4) 0.0949(14) Uani 1 1 d . . . Cl37 Cl -0.11291(13) 0.15052(13) 0.2644(2) 0.0620(9) Uani 1 1 d . . . Cl47 Cl 0.12101(13) 0.16085(13) -0.2766(2) 0.0576(9) Uani 1 1 d . . . C51 C 0.4552(5) -0.1275(6) 0.7116(9) 0.052(3) Uani 1 1 d U . . C52 C 0.4203(5) -0.1114(6) 0.6189(11) 0.073(4) Uani 1 1 d U . . H52 H 0.4030 -0.0729 0.6159 0.087 Uiso 1 1 calc R . . C53 C 0.4099(6) -0.1506(7) 0.5297(12) 0.085(4) Uani 1 1 d U . . H53 H 0.3858 -0.1384 0.4664 0.102 Uiso 1 1 calc R . . C54 C 0.4340(6) -0.2062(6) 0.5318(12) 0.071(4) Uani 1 1 d U . . C55 C 0.4681(6) -0.2248(6) 0.6256(12) 0.075(4) Uani 1 1 d U . . H55 H 0.4849 -0.2637 0.6289 0.090 Uiso 1 1 calc R . . C56 C 0.4771(5) -0.1852(5) 0.7138(11) 0.067(4) Uani 1 1 d U . . H56 H 0.4995 -0.1986 0.7789 0.080 Uiso 1 1 calc R . . C61 C 0.6349(5) -0.1129(5) 0.9607(11) 0.056(3) Uani 1 1 d U . . C62 C 0.6332(5) -0.1500(6) 0.8706(11) 0.067(4) Uani 1 1 d U . . H62 H 0.6028 -0.1532 0.8160 0.080 Uiso 1 1 calc R . . C63 C 0.6757(6) -0.1825(8) 0.8599(14) 0.096(5) Uani 1 1 d U . . H63 H 0.6747 -0.2079 0.7982 0.115 Uiso 1 1 calc R . . C64 C 0.7187(6) -0.1776(8) 0.9381(17) 0.104(6) Uani 1 1 d U . . C65 C 0.7220(6) -0.1422(8) 1.0249(17) 0.112(6) Uani 1 1 d U . . H65 H 0.7527 -0.1396 1.0788 0.135 Uiso 1 1 calc R . . C66 C 0.6802(5) -0.1093(7) 1.0353(14) 0.082(4) Uani 1 1 d U . . H66 H 0.6827 -0.0830 1.0965 0.098 Uiso 1 1 calc R . . C71 C 0.6226(5) 0.1283(6) 0.9496(12) 0.061(3) Uani 1 1 d U . . C72 C 0.6640(5) 0.1421(6) 1.0341(14) 0.081(4) Uani 1 1 d U . . H72 H 0.6668 0.1219 1.1018 0.098 Uiso 1 1 calc R . . C73 C 0.7021(5) 0.1850(6) 1.0234(16) 0.089(5) Uani 1 1 d U . . H73 H 0.7291 0.1953 1.0828 0.107 Uiso 1 1 calc R . . C74 C 0.6980(6) 0.2108(7) 0.9229(18) 0.094(5) Uani 1 1 d U . . C75 C 0.6582(6) 0.2000(6) 0.8392(15) 0.087(5) Uani 1 1 d U . . H75 H 0.6558 0.2206 0.7720 0.105 Uiso 1 1 calc R . . C76 C 0.6209(5) 0.1587(6) 0.8523(13) 0.071(4) Uani 1 1 d U . . H76 H 0.5933 0.1510 0.7927 0.085 Uiso 1 1 calc R . . C81 C 0.4408(5) 0.1177(5) 0.7056(11) 0.059(3) Uani 1 1 d U . . C82 C 0.4702(6) 0.1371(9) 0.6445(13) 0.127(7) Uani 1 1 d U . . H82 H 0.5046 0.1249 0.6628 0.152 Uiso 1 1 calc R . . C83 C 0.4532(7) 0.1757(10) 0.5516(13) 0.128(7) Uani 1 1 d U . . H83 H 0.4760 0.1892 0.5099 0.154 Uiso 1 1 calc R . . C84 C 0.4050(7) 0.1922(7) 0.5246(12) 0.080(4) Uani 1 1 d U . . C85 C 0.3744(8) 0.1731(8) 0.5873(17) 0.130(6) Uani 1 1 d U . . H85 H 0.3399 0.1850 0.5697 0.155 Uiso 1 1 calc R . . C86 C 0.3927(7) 0.1362(8) 0.6771(16) 0.123(6) Uani 1 1 d U . . H86 H 0.3702 0.1235 0.7201 0.148 Uiso 1 1 calc R . . O7 O 0.5319(3) -0.0898(3) 0.8829(6) 0.053(2) Uani 1 1 d U . . O8 O 0.5940(2) 0.0059(3) 0.9628(6) 0.0508(19) Uani 1 1 d U . . O9 O 0.5236(3) 0.0900(3) 0.8713(6) 0.051(2) Uani 1 1 d U . . O10 O 0.4623(3) -0.0045(3) 0.7829(6) 0.0533(19) Uani 1 1 d U . . O11 O 0.5718(3) -0.0814(3) 1.0961(6) 0.049(2) Uani 1 1 d U . . O12 O 0.5635(3) 0.0915(3) 1.0886(6) 0.0464(19) Uani 1 1 d U . . F2 F 0.5000 0.0000 1.0000 0.057(2) Uani 1 2 d S . . Si5 Si 0.47239(13) -0.07448(15) 0.8302(3) 0.0522(9) Uani 1 1 d U . . Si6 Si 0.57841(12) -0.06664(15) 0.9760(3) 0.0505(9) Uani 1 1 d U . . Si7 Si 0.57219(12) 0.07530(14) 0.9702(3) 0.0498(9) Uani 1 1 d U . . Si8 Si 0.46569(13) 0.06783(15) 0.8236(3) 0.0512(9) Uani 1 1 d U . . Cl57 Cl 0.42427(18) -0.25238(18) 0.4173(3) 0.1030(15) Uani 1 1 d . . . Cl67 Cl 0.7710(2) -0.2192(4) 0.9191(7) 0.215(4) Uani 1 1 d . . . Cl77 Cl 0.74463(19) 0.2635(2) 0.9080(6) 0.165(3) Uani 1 1 d . . . Cl87 Cl 0.3843(2) 0.2412(2) 0.4123(4) 0.1264(19) Uani 1 1 d . . . C101 C 0.3299(8) 0.5334(12) 0.843(2) 0.089(8) Uani 0.472(8) 1 d PDU A 1 H10A H 0.3401 0.5749 0.8216 0.107 Uiso 0.472(8) 1 calc PR A 1 H10B H 0.3289 0.5355 0.9203 0.107 Uiso 0.472(8) 1 calc PR A 1 C102 C 0.3697(7) 0.4859(15) 0.830(2) 0.105(9) Uani 0.472(8) 1 d PDU A 1 H10C H 0.3685 0.4550 0.8873 0.126 Uiso 0.472(8) 1 calc PR A 1 H10D H 0.3539 0.4649 0.7613 0.126 Uiso 0.472(8) 1 calc PR A 1 C103 C 0.4219(8) 0.4867(17) 0.828(2) 0.107(10) Uani 0.472(8) 1 d PDU A 1 H10E H 0.4347 0.4435 0.8386 0.129 Uiso 0.472(8) 1 calc PR A 1 H10F H 0.4247 0.5003 0.7555 0.129 Uiso 0.472(8) 1 calc PR A 1 C104 C 0.4525(5) 0.5235(13) 0.903(2) 0.22(2) Uani 0.472(8) 1 d PDU A 1 H10G H 0.4612 0.5018 0.9728 0.328 Uiso 0.472(8) 1 calc PR A 1 H10H H 0.4350 0.5624 0.9111 0.328 Uiso 0.472(8) 1 calc PR A 1 H10I H 0.4834 0.5327 0.8790 0.328 Uiso 0.472(8) 1 calc PR A 1 C105 C 0.2593(12) 0.4527(11) 0.7899(19) 0.075(8) Uani 0.472(8) 1 d PDU A 1 H10J H 0.2774 0.4238 0.7512 0.090 Uiso 0.472(8) 1 calc PR A 1 H10K H 0.2228 0.4494 0.7561 0.090 Uiso 0.472(8) 1 calc PR A 1 C106 C 0.2684(10) 0.4325(12) 0.9081(18) 0.081(8) Uani 0.472(8) 1 d PDU A 1 H10L H 0.2492 0.4600 0.9466 0.097 Uiso 0.472(8) 1 calc PR A 1 H10M H 0.3047 0.4368 0.9431 0.097 Uiso 0.472(8) 1 calc PR A 1 C107 C 0.2515(11) 0.3626(14) 0.917(3) 0.094(9) Uani 0.472(8) 1 d PDU A 1 H10N H 0.2689 0.3349 0.8755 0.113 Uiso 0.472(8) 1 calc PR A 1 H10O H 0.2602 0.3490 0.9941 0.113 Uiso 0.472(8) 1 calc PR A 1 C108 C 0.1976(12) 0.3596(17) 0.875(3) 0.085(12) Uani 0.472(8) 1 d PDU A 1 H10P H 0.1811 0.3921 0.9088 0.128 Uiso 0.472(8) 1 calc PR A 1 H10Q H 0.1851 0.3187 0.8908 0.128 Uiso 0.472(8) 1 calc PR A 1 H10R H 0.1898 0.3661 0.7964 0.128 Uiso 0.472(8) 1 calc PR A 1 C109 C 0.2761(9) 0.5264(13) 0.6530(15) 0.076(7) Uani 0.472(8) 1 d PDU A 1 H10S H 0.2851 0.5700 0.6401 0.092 Uiso 0.472(8) 1 calc PR A 1 H10T H 0.3026 0.4992 0.6360 0.092 Uiso 0.472(8) 1 calc PR A 1 C110 C 0.2277(10) 0.5115(17) 0.5775(18) 0.083(8) Uani 0.472(8) 1 d PDU A 1 H11A H 0.1999 0.5359 0.5955 0.100 Uiso 0.472(8) 1 calc PR A 1 H11B H 0.2199 0.4667 0.5809 0.100 Uiso 0.472(8) 1 calc PR A 1 C111 C 0.2349(10) 0.5301(16) 0.4569(17) 0.076(8) Uani 0.472(8) 1 d PDU A 1 H11C H 0.2450 0.5744 0.4567 0.091 Uiso 0.472(8) 1 calc PR A 1 H11D H 0.2623 0.5045 0.4398 0.091 Uiso 0.472(8) 1 calc PR A 1 C112 C 0.1910(14) 0.521(2) 0.378(2) 0.106(14) Uani 0.472(8) 1 d PDU A 1 H11E H 0.1714 0.4871 0.4003 0.158 Uiso 0.472(8) 1 calc PR A 1 H11F H 0.1995 0.5097 0.3095 0.158 Uiso 0.472(8) 1 calc PR A 1 H11G H 0.1709 0.5592 0.3682 0.158 Uiso 0.472(8) 1 calc PR A 1 C113 C 0.2392(8) 0.5644(9) 0.809(2) 0.045(6) Uani 0.472(8) 1 d PDU A 1 H11H H 0.2050 0.5551 0.7644 0.054 Uiso 0.472(8) 1 calc PR A 1 H11I H 0.2388 0.5562 0.8852 0.054 Uiso 0.472(8) 1 calc PR A 1 C114 C 0.2494(8) 0.6330(11) 0.797(2) 0.074(7) Uani 0.472(8) 1 d PDU A 1 H11J H 0.2590 0.6417 0.7282 0.089 Uiso 0.472(8) 1 calc PR A 1 H11K H 0.2766 0.6479 0.8581 0.089 Uiso 0.472(8) 1 calc PR A 1 C115 C 0.1981(10) 0.6640(14) 0.800(3) 0.096(9) Uani 0.472(8) 1 d PDU A 1 H11L H 0.1814 0.6405 0.8487 0.116 Uiso 0.472(8) 1 calc PR A 1 H11M H 0.2038 0.7072 0.8271 0.116 Uiso 0.472(8) 1 calc PR A 1 C116 C 0.1662(10) 0.6643(16) 0.691(2) 0.113(13) Uani 0.472(8) 1 d PDU A 1 H11N H 0.1428 0.6290 0.6821 0.170 Uiso 0.472(8) 1 calc PR A 1 H11O H 0.1873 0.6608 0.6382 0.170 Uiso 0.472(8) 1 calc PR A 1 H11P H 0.1470 0.7033 0.6786 0.170 Uiso 0.472(8) 1 calc PR A 1 N1 N 0.2766(7) 0.5189(10) 0.7759(14) 0.072(7) Uani 0.472(8) 1 d PDU A 1 C201 C 0.3234(9) 0.4850(13) 0.7588(17) 0.092(7) Uani 0.528(8) 1 d PDU A 2 H20A H 0.3227 0.4449 0.7203 0.111 Uiso 0.528(8) 1 calc PR A 2 H20B H 0.3352 0.5171 0.7144 0.111 Uiso 0.528(8) 1 calc PR A 2 C202 C 0.3623(8) 0.4798(15) 0.865(2) 0.128(10) Uani 0.528(8) 1 d PDU A 2 H20C H 0.3463 0.5047 0.9135 0.154 Uiso 0.528(8) 1 calc PR A 2 H20D H 0.3577 0.4361 0.8852 0.154 Uiso 0.528(8) 1 calc PR A 2 C203 C 0.4142(8) 0.4890(15) 0.913(2) 0.113(9) Uani 0.528(8) 1 d PDU A 2 H20E H 0.4200 0.5342 0.9070 0.135 Uiso 0.528(8) 1 calc PR A 2 H20F H 0.4177 0.4809 0.9915 0.135 Uiso 0.528(8) 1 calc PR A 2 C204 C 0.4550(9) 0.4606(11) 0.888(2) 0.136(13) Uani 0.528(8) 1 d PDU A 2 H20G H 0.4840 0.4629 0.9499 0.205 Uiso 0.528(8) 1 calc PR A 2 H20H H 0.4632 0.4817 0.8256 0.205 Uiso 0.528(8) 1 calc PR A 2 H20I H 0.4469 0.4168 0.8696 0.205 Uiso 0.528(8) 1 calc PR A 2 C205 C 0.2450(11) 0.4565(10) 0.829(2) 0.078(8) Uani 0.528(8) 1 d PDU A 2 H20J H 0.2096 0.4696 0.8228 0.093 Uiso 0.528(8) 1 calc PR A 2 H20K H 0.2629 0.4599 0.9061 0.093 Uiso 0.528(8) 1 calc PR A 2 C206 C 0.2455(12) 0.3888(10) 0.794(2) 0.089(7) Uani 0.528(8) 1 d PDU A 2 H20L H 0.2809 0.3751 0.8019 0.107 Uiso 0.528(8) 1 calc PR A 2 H20M H 0.2280 0.3851 0.7170 0.107 Uiso 0.528(8) 1 calc PR A 2 C207 C 0.2191(17) 0.3448(14) 0.864(4) 0.095(11) Uani 0.528(8) 1 d PDU A 2 H20N H 0.2345 0.3508 0.9415 0.115 Uiso 0.528(8) 1 calc PR A 2 H20O H 0.1828 0.3555 0.8506 0.115 Uiso 0.528(8) 1 calc PR A 2 C208 C 0.2246(13) 0.2813(13) 0.834(3) 0.138(14) Uani 0.528(8) 1 d PDU A 2 H20P H 0.2049 0.2740 0.7602 0.207 Uiso 0.528(8) 1 calc PR A 2 H20Q H 0.2123 0.2538 0.8842 0.207 Uiso 0.528(8) 1 calc PR A 2 H20R H 0.2602 0.2724 0.8382 0.207 Uiso 0.528(8) 1 calc PR A 2 C209 C 0.2358(9) 0.4999(12) 0.6451(15) 0.082(7) Uani 0.528(8) 1 d PDU A 2 H20S H 0.2381 0.4578 0.6146 0.098 Uiso 0.528(8) 1 calc PR A 2 H20T H 0.2003 0.5064 0.6488 0.098 Uiso 0.528(8) 1 calc PR A 2 C210 C 0.2484(12) 0.5461(15) 0.569(2) 0.112(8) Uani 0.528(8) 1 d PDU A 2 H21A H 0.2793 0.5328 0.5473 0.134 Uiso 0.528(8) 1 calc PR A 2 H21B H 0.2552 0.5869 0.6063 0.134 Uiso 0.528(8) 1 calc PR A 2 C211 C 0.2020(13) 0.5532(14) 0.462(2) 0.109(10) Uani 0.528(8) 1 d PDU A 2 H21C H 0.1708 0.5648 0.4847 0.131 Uiso 0.528(8) 1 calc PR A 2 H21D H 0.2099 0.5869 0.4156 0.131 Uiso 0.528(8) 1 calc PR A 2 C212 C 0.1941(14) 0.4980(18) 0.404(2) 0.114(14) Uani 0.528(8) 1 d PDU A 2 H21E H 0.2184 0.4949 0.3578 0.171 Uiso 0.528(8) 1 calc PR A 2 H21F H 0.1597 0.4975 0.3580 0.171 Uiso 0.528(8) 1 calc PR A 2 H21G H 0.1985 0.4626 0.4537 0.171 Uiso 0.528(8) 1 calc PR A 2 C213 C 0.2688(8) 0.5666(9) 0.812(2) 0.073(7) Uani 0.528(8) 1 d PDU A 2 H21H H 0.2865 0.5649 0.8896 0.088 Uiso 0.528(8) 1 calc PR A 2 H21I H 0.2879 0.5952 0.7754 0.088 Uiso 0.528(8) 1 calc PR A 2 C214 C 0.2163(10) 0.5931(12) 0.803(3) 0.106(9) Uani 0.528(8) 1 d PDU A 2 H21J H 0.1965 0.5674 0.8429 0.127 Uiso 0.528(8) 1 calc PR A 2 H21K H 0.1976 0.5969 0.7265 0.127 Uiso 0.528(8) 1 calc PR A 2 C215 C 0.2287(13) 0.6580(11) 0.857(2) 0.116(10) Uani 0.528(8) 1 d PDU A 2 H21L H 0.2238 0.6568 0.9313 0.139 Uiso 0.528(8) 1 calc PR A 2 H21M H 0.2645 0.6681 0.8605 0.139 Uiso 0.528(8) 1 calc PR A 2 C216 C 0.1975(16) 0.7050(14) 0.797(3) 0.166(17) Uani 0.528(8) 1 d PDU A 2 H21N H 0.2164 0.7279 0.7526 0.250 Uiso 0.528(8) 1 calc PR A 2 H21O H 0.1868 0.7338 0.8472 0.250 Uiso 0.528(8) 1 calc PR A 2 H21P H 0.1677 0.6858 0.7500 0.250 Uiso 0.528(8) 1 calc PR A 2 N2 N 0.2694(7) 0.5011(9) 0.7631(13) 0.069(6) Uani 0.528(8) 1 d PDU A 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 C11 0.031(5) 0.036(5) 0.034(5) -0.002(5) 0.023(4) -0.001(5) C12 0.070(8) 0.039(6) 0.029(6) 0.004(5) 0.017(5) 0.010(5) C13 0.060(8) 0.058(7) 0.042(7) -0.011(6) 0.016(6) 0.014(6) C14 0.029(5) 0.058(7) 0.039(6) 0.005(6) 0.012(4) -0.001(5) C15 0.062(8) 0.049(7) 0.041(7) 0.028(6) 0.005(6) 0.008(6) C16 0.061(7) 0.039(6) 0.036(6) 0.014(5) 0.002(5) 0.009(5) C21 0.040(6) 0.027(5) 0.038(5) 0.005(5) 0.015(4) 0.006(5) C22 0.046(7) 0.037(6) 0.034(6) 0.008(5) 0.012(5) 0.010(5) C23 0.050(7) 0.037(6) 0.052(7) 0.005(5) 0.007(6) -0.004(5) C24 0.042(6) 0.058(7) 0.053(7) 0.011(6) 0.005(5) -0.003(6) C25 0.043(7) 0.036(6) 0.085(9) 0.017(6) 0.030(6) 0.013(5) C26 0.034(6) 0.040(6) 0.066(8) -0.001(5) 0.022(6) -0.009(5) C31 0.046(6) 0.028(5) 0.034(6) 0.005(4) 0.023(5) 0.016(4) C32 0.116(11) 0.036(6) 0.033(6) 0.004(5) 0.023(7) -0.013(7) C33 0.124(11) 0.039(6) 0.030(6) 0.003(5) 0.017(7) -0.029(7) C34 0.084(9) 0.022(5) 0.042(7) 0.014(5) 0.026(6) 0.002(5) C35 0.085(9) 0.054(7) 0.043(7) 0.027(6) 0.003(6) -0.022(7) C36 0.037(6) 0.053(6) 0.045(7) 0.024(6) 0.000(5) -0.007(5) C41 0.035(6) 0.023(4) 0.027(5) 0.007(4) 0.010(4) 0.012(4) C42 0.044(6) 0.027(5) 0.022(5) -0.003(4) 0.010(4) 0.005(4) C43 0.057(7) 0.038(6) 0.028(6) 0.006(5) 0.010(5) 0.010(5) C44 0.048(7) 0.034(5) 0.034(6) -0.012(5) 0.016(5) 0.006(5) C45 0.103(10) 0.071(8) 0.028(6) -0.004(6) 0.009(6) 0.051(7) C46 0.071(8) 0.061(7) 0.037(6) 0.004(6) 0.016(6) 0.045(6) O1 0.036(3) 0.031(3) 0.025(3) 0.001(3) 0.016(3) 0.005(3) O2 0.044(4) 0.025(3) 0.035(4) 0.005(3) 0.016(3) 0.010(3) O3 0.041(4) 0.027(3) 0.032(4) 0.000(3) 0.019(3) -0.001(3) O4 0.047(4) 0.026(3) 0.028(3) -0.002(3) 0.015(3) 0.009(3) O5 0.043(4) 0.027(3) 0.031(4) 0.005(3) 0.017(3) 0.002(3) O6 0.045(4) 0.027(3) 0.029(4) 0.009(3) 0.019(3) 0.010(3) F1 0.051(5) 0.029(4) 0.038(4) 0.001(4) 0.017(4) 0.005(4) Si1 0.0431(15) 0.0254(12) 0.0271(12) 0.0014(13) 0.0186(11) 0.0073(13) Si2 0.0366(15) 0.0264(12) 0.0289(13) 0.0050(13) 0.0144(11) 0.0065(13) Si3 0.0460(18) 0.0229(13) 0.0288(15) 0.0079(12) 0.0184(13) 0.0065(12) Si4 0.0410(17) 0.0268(13) 0.0314(16) 0.0035(12) 0.0196(13) 0.0087(12) Cl17 0.064(2) 0.101(3) 0.0298(13) 0.0061(17) 0.0133(13) 0.0052(19) Cl27 0.047(2) 0.084(3) 0.139(4) 0.030(3) -0.008(2) -0.0142(18) Cl37 0.092(2) 0.0438(16) 0.0535(19) 0.0145(14) 0.0243(17) -0.0202(16) Cl47 0.087(2) 0.0435(16) 0.0445(17) -0.0082(13) 0.0190(16) 0.0244(15) C51 0.059(8) 0.062(7) 0.044(7) -0.012(6) 0.029(6) -0.008(6) C52 0.081(10) 0.067(8) 0.076(9) -0.037(7) 0.031(8) -0.008(7) C53 0.093(11) 0.076(9) 0.090(10) -0.044(8) 0.032(9) -0.006(8) C54 0.104(11) 0.058(8) 0.071(9) -0.023(7) 0.063(8) -0.040(8) C55 0.118(11) 0.036(6) 0.089(10) -0.018(7) 0.063(9) -0.023(7) C56 0.089(10) 0.045(7) 0.072(9) -0.014(6) 0.030(7) -0.025(7) C61 0.051(7) 0.041(6) 0.088(9) -0.002(6) 0.038(7) 0.000(5) C62 0.076(9) 0.056(7) 0.073(9) -0.002(7) 0.029(7) 0.017(7) C63 0.095(12) 0.101(11) 0.092(11) -0.011(10) 0.026(10) 0.036(10) C64 0.073(11) 0.100(12) 0.150(15) -0.011(11) 0.047(11) 0.038(9) C65 0.071(11) 0.103(12) 0.161(16) -0.017(12) 0.024(11) 0.003(10) C66 0.036(8) 0.082(9) 0.130(12) -0.028(9) 0.023(8) 0.005(7) C71 0.041(7) 0.054(7) 0.096(10) -0.004(7) 0.034(7) -0.009(6) C72 0.069(9) 0.057(8) 0.132(13) -0.004(8) 0.052(9) -0.014(7) C73 0.050(8) 0.064(9) 0.163(15) -0.024(10) 0.041(9) -0.023(7) C74 0.076(10) 0.052(8) 0.168(17) 0.006(10) 0.057(11) -0.022(8) C75 0.101(12) 0.051(8) 0.131(13) 0.009(9) 0.071(10) 0.016(8) C76 0.072(9) 0.049(7) 0.109(11) -0.002(7) 0.056(8) -0.012(7) C81 0.076(9) 0.042(6) 0.075(9) 0.000(6) 0.051(7) -0.003(6) C82 0.074(11) 0.224(18) 0.070(10) 0.050(12) -0.008(9) -0.014(12) C83 0.087(12) 0.218(18) 0.074(11) 0.055(12) 0.009(10) -0.032(13) C84 0.101(12) 0.081(9) 0.065(9) -0.001(8) 0.035(9) 0.018(9) C85 0.139(15) 0.116(13) 0.148(15) 0.053(12) 0.064(13) 0.075(11) C86 0.126(14) 0.108(12) 0.155(15) 0.059(11) 0.073(12) 0.063(11) O7 0.055(5) 0.043(4) 0.067(5) -0.022(4) 0.024(4) -0.006(4) O8 0.043(4) 0.042(4) 0.078(5) -0.011(4) 0.036(4) -0.011(4) O9 0.053(5) 0.043(4) 0.063(5) -0.015(4) 0.028(4) -0.013(4) O10 0.053(5) 0.051(4) 0.061(5) -0.021(4) 0.024(4) -0.010(4) O11 0.046(5) 0.043(4) 0.067(5) -0.009(4) 0.029(4) -0.009(3) O12 0.042(4) 0.041(4) 0.061(5) -0.013(4) 0.024(4) -0.011(3) F2 0.050(5) 0.050(5) 0.077(6) -0.014(5) 0.030(5) -0.008(5) Si5 0.053(2) 0.0503(19) 0.060(2) -0.0168(17) 0.0281(18) -0.0143(16) Si6 0.046(2) 0.0451(18) 0.069(2) -0.0142(17) 0.0307(18) -0.0113(15) Si7 0.045(2) 0.0429(17) 0.070(2) -0.0145(17) 0.0288(18) -0.0141(15) Si8 0.052(2) 0.0475(19) 0.062(2) -0.0122(17) 0.0273(18) -0.0095(16) Cl57 0.165(4) 0.074(2) 0.092(3) -0.044(2) 0.075(3) -0.046(3) Cl67 0.123(5) 0.231(7) 0.298(9) -0.054(7) 0.061(5) 0.107(5) Cl77 0.111(4) 0.094(3) 0.322(8) 0.004(4) 0.113(5) -0.050(3) Cl87 0.213(6) 0.095(3) 0.073(3) 0.009(2) 0.039(3) 0.037(3) C101 0.097(17) 0.080(15) 0.096(16) -0.017(14) 0.033(14) -0.017(14) C102 0.113(17) 0.116(16) 0.086(16) -0.032(15) 0.022(14) 0.001(16) C103 0.10(2) 0.14(2) 0.082(18) -0.045(19) 0.039(17) 0.007(19) C104 0.24(4) 0.22(4) 0.21(4) -0.06(4) 0.06(3) 0.00(4) C105 0.088(15) 0.088(15) 0.054(14) -0.010(13) 0.027(13) -0.029(13) C106 0.102(18) 0.091(17) 0.050(14) -0.011(14) 0.019(14) -0.014(15) C107 0.11(2) 0.095(17) 0.073(17) -0.010(15) 0.009(16) -0.028(16) C108 0.13(3) 0.08(2) 0.050(19) 0.019(18) 0.02(2) -0.04(2) C109 0.080(15) 0.088(14) 0.064(13) -0.001(13) 0.024(13) -0.006(13) C110 0.092(16) 0.093(17) 0.068(15) -0.005(16) 0.024(15) -0.024(14) C111 0.077(17) 0.092(17) 0.055(14) -0.013(14) 0.010(14) -0.022(15) C112 0.16(3) 0.13(3) 0.036(15) 0.02(2) 0.048(19) 0.00(3) C113 0.020(12) 0.055(12) 0.062(13) -0.020(11) 0.017(11) 0.006(11) C114 0.060(14) 0.072(14) 0.083(15) -0.024(13) -0.001(13) 0.020(12) C115 0.069(16) 0.064(15) 0.118(18) -0.031(16) -0.055(15) 0.028(15) C116 0.09(2) 0.10(2) 0.16(3) -0.01(2) 0.03(2) 0.06(2) N1 0.081(12) 0.081(13) 0.056(11) -0.004(11) 0.021(10) -0.019(11) C201 0.099(15) 0.099(15) 0.078(13) -0.041(12) 0.021(12) -0.021(13) C202 0.125(18) 0.111(17) 0.132(19) -0.042(16) -0.005(16) 0.005(16) C203 0.109(18) 0.139(19) 0.088(16) -0.048(17) 0.019(15) -0.015(17) C204 0.19(3) 0.09(2) 0.13(3) -0.01(2) 0.02(3) 0.04(2) C205 0.111(17) 0.074(14) 0.045(14) 0.009(12) 0.009(13) -0.014(13) C206 0.119(17) 0.075(14) 0.078(15) 0.009(13) 0.032(13) -0.027(14) C207 0.13(2) 0.081(18) 0.087(19) -0.021(16) 0.041(18) -0.009(18) C208 0.13(3) 0.10(3) 0.20(4) -0.05(3) 0.06(3) -0.03(2) C209 0.092(15) 0.093(15) 0.063(13) -0.013(15) 0.026(13) -0.044(13) C210 0.131(17) 0.128(17) 0.071(14) -0.004(15) 0.011(14) -0.038(15) C211 0.14(2) 0.13(2) 0.062(16) -0.010(16) 0.026(17) -0.029(19) C212 0.10(2) 0.16(3) 0.11(3) -0.01(3) 0.07(2) -0.01(2) C213 0.079(15) 0.071(13) 0.067(13) -0.016(12) 0.012(13) 0.003(13) C214 0.109(17) 0.084(15) 0.101(15) -0.024(14) -0.027(15) 0.027(14) C215 0.13(2) 0.078(16) 0.108(19) -0.029(16) -0.039(17) 0.016(16) C216 0.18(3) 0.11(3) 0.16(3) -0.06(3) -0.05(3) 0.05(3) N2 0.094(12) 0.063(11) 0.050(10) -0.003(10) 0.018(9) -0.022(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C11 C12 1.378(13) . ? C11 C16 1.402(13) . ? C11 Si1 1.857(9) . ? C12 C13 1.391(14) . ? C12 H12 0.9500 . ? C13 C14 1.352(14) . ? C13 H13 0.9500 . ? C14 C15 1.395(15) . ? C14 Cl17 1.745(10) . ? C15 C16 1.387(14) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C22 1.378(13) . ? C21 C26 1.390(13) . ? C21 Si2 1.849(9) . ? C22 C23 1.378(14) . ? C22 H22 0.9500 . ? C23 C24 1.375(14) . ? C23 H23 0.9500 . ? C24 C25 1.392(15) . ? C24 Cl27 1.735(11) . ? C25 C26 1.366(14) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C32 1.383(14) . ? C31 C36 1.388(13) . ? C31 Si3 1.844(10) . ? C32 C33 1.406(14) . ? C32 H32 0.9500 . ? C33 C34 1.351(14) . ? C33 H33 0.9500 . ? C34 C35 1.366(15) . ? C34 Cl37 1.755(10) . ? C35 C36 1.395(14) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C46 1.375(13) . ? C41 C42 1.380(12) . ? C41 Si4 1.847(9) . ? C42 C43 1.374(13) . ? C42 H42 0.9500 . ? C43 C44 1.375(13) . ? C43 H43 0.9500 . ? C44 C45 1.351(14) . ? C44 Cl47 1.747(9) . ? C45 C46 1.390(14) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? O1 Si1 1.626(6) . ? O1 Si2 1.627(6) . ? O2 Si2 1.617(7) . ? O2 Si4 1.627(7) . ? O3 Si2 1.615(6) . ? O3 Si3 1.637(7) 3_565 ? O4 Si3 1.622(7) . ? O4 Si4 1.625(7) . ? O5 Si1 1.613(7) . ? O5 Si3 1.612(7) . ? O6 Si1 1.613(6) . ? O6 Si4 1.623(6) 3_565 ? Si3 O3 1.637(7) 3_565 ? Si4 O6 1.623(6) 3_565 ? C51 C52 1.374(17) . ? C51 C56 1.375(16) . ? C51 Si5 1.859(12) . ? C52 C53 1.386(17) . ? C52 H52 0.9500 . ? C53 C54 1.360(19) . ? C53 H53 0.9500 . ? C54 C55 1.388(19) . ? C54 Cl57 1.729(13) . ? C55 C56 1.382(16) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 C66 1.373(17) . ? C61 C62 1.386(17) . ? C61 Si6 1.880(12) . ? C62 C63 1.386(18) . ? C62 H62 0.9500 . ? C63 C64 1.35(2) . ? C63 H63 0.9500 . ? C64 C65 1.32(2) . ? C64 Cl67 1.745(15) . ? C65 C66 1.375(19) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C71 C76 1.389(18) . ? C71 C72 1.398(18) . ? C71 Si7 1.849(12) . ? C72 C73 1.416(17) . ? C72 H72 0.9500 . ? C73 C74 1.37(2) . ? C73 H73 0.9500 . ? C74 C75 1.35(2) . ? C74 Cl77 1.745(14) . ? C75 C76 1.387(18) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C81 C82 1.306(19) . ? C81 C86 1.336(19) . ? C81 Si8 1.839(13) . ? C82 C83 1.43(2) . ? C82 H82 0.9500 . ? C83 C84 1.33(2) . ? C83 H83 0.9500 . ? C84 C85 1.35(2) . ? C84 Cl87 1.757(15) . ? C85 C86 1.38(2) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? O7 Si6 1.599(8) . ? O7 Si5 1.637(8) . ? O8 Si7 1.616(8) . ? O8 Si6 1.632(7) . ? O9 Si8 1.626(8) . ? O9 Si7 1.629(8) . ? O10 Si5 1.617(8) . ? O10 Si8 1.634(8) . ? O11 Si6 1.609(8) . ? O11 Si8 1.628(8) 3_657 ? O12 Si7 1.614(8) . ? O12 Si5 1.619(8) 3_657 ? Si5 O12 1.619(8) 3_657 ? Si8 O11 1.628(8) 3_657 ? C101 C102 1.53(2) . ? C101 N1 1.53(2) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 C103 1.426(16) . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.36(2) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9800 . ? C104 H10H 0.9800 . ? C104 H10I 0.9800 . ? C105 N1 1.52(2) . ? C105 C106 1.53(2) . ? C105 H10J 0.9900 . ? C105 H10K 0.9900 . ? C106 C107 1.58(3) . ? C106 H10L 0.9900 . ? C106 H10M 0.9900 . ? C107 C108 1.45(4) . ? C107 H10N 0.9900 . ? C107 H10O 0.9900 . ? C108 H10P 0.9800 . ? C108 H10Q 0.9800 . ? C108 H10R 0.9800 . ? C109 C110 1.48(2) . ? C109 N1 1.57(2) . ? C109 H10S 0.9900 . ? C109 H10T 0.9900 . ? C110 C111 1.64(3) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.386(18) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? C113 C114 1.51(2) . ? C113 N1 1.54(2) . ? C113 H11H 0.9900 . ? C113 H11I 0.9900 . ? C114 C115 1.55(3) . ? C114 H11J 0.9900 . ? C114 H11K 0.9900 . ? C115 C116 1.45(2) . ? C115 H11L 0.9900 . ? C115 H11M 0.9900 . ? C116 H11N 0.9800 . ? C116 H11O 0.9800 . ? C116 H11P 0.9800 . ? C201 C202 1.51(2) . ? C201 N2 1.52(2) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 C203 1.418(16) . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.371(17) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9800 . ? C204 H20H 0.9800 . ? C204 H20I 0.9800 . ? C205 N2 1.52(2) . ? C205 C206 1.52(2) . ? C205 H20J 0.9900 . ? C205 H20K 0.9900 . ? C206 C207 1.57(3) . ? C206 H20L 0.9900 . ? C206 H20M 0.9900 . ? C207 C208 1.43(4) . ? C207 H20N 0.9900 . ? C207 H20O 0.9900 . ? C208 H20P 0.9800 . ? C208 H20Q 0.9800 . ? C208 H20R 0.9800 . ? C209 C210 1.48(2) . ? C209 N2 1.56(2) . ? C209 H20S 0.9900 . ? C209 H20T 0.9900 . ? C210 C211 1.64(3) . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.39(2) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 H21E 0.9800 . ? C212 H21F 0.9800 . ? C212 H21G 0.9800 . ? C213 C214 1.52(2) . ? C213 N2 1.54(2) . ? C213 H21H 0.9900 . ? C213 H21I 0.9900 . ? C214 C215 1.55(2) . ? C214 H21J 0.9900 . ? C214 H21K 0.9900 . ? C215 C216 1.420(18) . ? C215 H21L 0.9900 . ? C215 H21M 0.9900 . ? C216 H21N 0.9800 . ? C216 H21O 0.9800 . ? C216 H21P 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 C11 C16 116.9(8) . . ? C12 C11 Si1 122.9(8) . . ? C16 C11 Si1 120.2(7) . . ? C11 C12 C13 121.5(10) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C14 C13 C12 120.4(10) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.6(9) . . ? C13 C14 Cl17 120.2(9) . . ? C15 C14 Cl17 119.1(8) . . ? C16 C15 C14 118.2(9) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C15 C16 C11 122.2(10) . . ? C15 C16 H16 118.9 . . ? C11 C16 H16 118.9 . . ? C22 C21 C26 114.8(9) . . ? C22 C21 Si2 123.3(7) . . ? C26 C21 Si2 121.7(7) . . ? C21 C22 C23 124.3(9) . . ? C21 C22 H22 117.9 . . ? C23 C22 H22 117.9 . . ? C24 C23 C22 117.7(10) . . ? C24 C23 H23 121.1 . . ? C22 C23 H23 121.1 . . ? C23 C24 C25 121.2(10) . . ? C23 C24 Cl27 119.0(9) . . ? C25 C24 Cl27 119.9(9) . . ? C26 C25 C24 117.8(10) . . ? C26 C25 H25 121.1 . . ? C24 C25 H25 121.1 . . ? C25 C26 C21 124.1(10) . . ? C25 C26 H26 118.0 . . ? C21 C26 H26 118.0 . . ? C32 C31 C36 115.8(9) . . ? C32 C31 Si3 122.1(8) . . ? C36 C31 Si3 122.1(8) . . ? C31 C32 C33 122.9(10) . . ? C31 C32 H32 118.6 . . ? C33 C32 H32 118.6 . . ? C34 C33 C32 118.1(11) . . ? C34 C33 H33 120.9 . . ? C32 C33 H33 120.9 . . ? C33 C34 C35 122.1(10) . . ? C33 C34 Cl37 118.1(9) . . ? C35 C34 Cl37 119.7(8) . . ? C34 C35 C36 118.6(10) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C31 C36 C35 122.5(10) . . ? C31 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C46 C41 C42 116.5(8) . . ? C46 C41 Si4 123.6(7) . . ? C42 C41 Si4 119.9(7) . . ? C43 C42 C41 121.6(9) . . ? C43 C42 H42 119.2 . . ? C41 C42 H42 119.2 . . ? C42 C43 C44 120.4(9) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C45 C44 C43 119.6(9) . . ? C45 C44 Cl47 121.0(8) . . ? C43 C44 Cl47 119.5(8) . . ? C44 C45 C46 119.4(10) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C41 C46 C45 122.5(10) . . ? C41 C46 H46 118.7 . . ? C45 C46 H46 118.7 . . ? Si1 O1 Si2 140.9(4) . . ? Si2 O2 Si4 140.4(4) . . ? Si2 O3 Si3 140.4(4) . 3_565 ? Si3 O4 Si4 141.1(4) . . ? Si1 O5 Si3 141.9(4) . . ? Si1 O6 Si4 141.7(4) . 3_565 ? O5 Si1 O6 114.1(3) . . ? O5 Si1 O1 111.6(3) . . ? O6 Si1 O1 111.6(3) . . ? O5 Si1 C11 105.6(4) . . ? O6 Si1 C11 104.8(4) . . ? O1 Si1 C11 108.6(4) . . ? O3 Si2 O2 114.3(3) . . ? O3 Si2 O1 113.4(3) . . ? O2 Si2 O1 113.0(3) . . ? O3 Si2 C21 105.0(4) . . ? O2 Si2 C21 105.9(4) . . ? O1 Si2 C21 104.1(4) . . ? O5 Si3 O4 113.4(4) . . ? O5 Si3 O3 113.3(3) . 3_565 ? O4 Si3 O3 111.4(4) . 3_565 ? O5 Si3 C31 106.5(4) . . ? O4 Si3 C31 105.9(4) . . ? O3 Si3 C31 105.6(4) 3_565 . ? O6 Si4 O4 113.4(4) 3_565 . ? O6 Si4 O2 113.0(3) 3_565 . ? O4 Si4 O2 111.9(4) . . ? O6 Si4 C41 106.2(4) 3_565 . ? O4 Si4 C41 105.5(4) . . ? O2 Si4 C41 106.0(4) . . ? C52 C51 C56 117.1(12) . . ? C52 C51 Si5 122.4(10) . . ? C56 C51 Si5 120.6(10) . . ? C51 C52 C53 121.2(13) . . ? C51 C52 H52 119.4 . . ? C53 C52 H52 119.4 . . ? C54 C53 C52 120.7(15) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C53 C54 C55 119.5(13) . . ? C53 C54 Cl57 120.6(13) . . ? C55 C54 Cl57 119.8(11) . . ? C54 C55 C56 118.5(13) . . ? C54 C55 H55 120.8 . . ? C56 C55 H55 120.8 . . ? C51 C56 C55 122.9(14) . . ? C51 C56 H56 118.6 . . ? C55 C56 H56 118.6 . . ? C66 C61 C62 117.1(12) . . ? C66 C61 Si6 121.7(10) . . ? C62 C61 Si6 121.2(10) . . ? C61 C62 C63 120.1(14) . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C64 C63 C62 119.4(15) . . ? C64 C63 H63 120.3 . . ? C62 C63 H63 120.3 . . ? C65 C64 C63 122.3(16) . . ? C65 C64 Cl67 120.6(16) . . ? C63 C64 Cl67 117.0(15) . . ? C64 C65 C66 118.6(17) . . ? C64 C65 H65 120.7 . . ? C66 C65 H65 120.7 . . ? C65 C66 C61 122.5(15) . . ? C65 C66 H66 118.8 . . ? C61 C66 H66 118.8 . . ? C76 C71 C72 116.0(12) . . ? C76 C71 Si7 122.9(11) . . ? C72 C71 Si7 121.1(11) . . ? C71 C72 C73 122.8(15) . . ? C71 C72 H72 118.6 . . ? C73 C72 H72 118.6 . . ? C74 C73 C72 116.7(16) . . ? C74 C73 H73 121.7 . . ? C72 C73 H73 121.7 . . ? C75 C74 C73 122.7(15) . . ? C75 C74 Cl77 119.8(16) . . ? C73 C74 Cl77 117.3(15) . . ? C74 C75 C76 119.5(16) . . ? C74 C75 H75 120.3 . . ? C76 C75 H75 120.3 . . ? C75 C76 C71 122.2(15) . . ? C75 C76 H76 118.9 . . ? C71 C76 H76 118.9 . . ? C82 C81 C86 116.2(15) . . ? C82 C81 Si8 120.6(12) . . ? C86 C81 Si8 123.1(11) . . ? C81 C82 C83 123.4(16) . . ? C81 C82 H82 118.3 . . ? C83 C82 H82 118.3 . . ? C84 C83 C82 118.7(16) . . ? C84 C83 H83 120.7 . . ? C82 C83 H83 120.7 . . ? C83 C84 C85 118.6(16) . . ? C83 C84 Cl87 118.9(14) . . ? C85 C84 Cl87 122.5(14) . . ? C84 C85 C86 120.6(18) . . ? C84 C85 H85 119.7 . . ? C86 C85 H85 119.7 . . ? C81 C86 C85 122.5(18) . . ? C81 C86 H86 118.8 . . ? C85 C86 H86 118.8 . . ? Si6 O7 Si5 141.2(5) . . ? Si7 O8 Si6 140.1(4) . . ? Si8 O9 Si7 140.8(5) . . ? Si5 O10 Si8 140.7(5) . . ? Si6 O11 Si8 141.6(5) . 3_657 ? Si7 O12 Si5 141.8(5) . 3_657 ? O10 Si5 O12 111.7(4) . 3_657 ? O10 Si5 O7 113.9(4) . . ? O12 Si5 O7 112.5(4) 3_657 . ? O10 Si5 C51 106.1(5) . . ? O12 Si5 C51 107.6(5) 3_657 . ? O7 Si5 C51 104.3(5) . . ? O7 Si6 O11 113.3(4) . . ? O7 Si6 O8 113.6(4) . . ? O11 Si6 O8 111.9(4) . . ? O7 Si6 C61 106.7(5) . . ? O11 Si6 C61 105.6(5) . . ? O8 Si6 C61 104.8(4) . . ? O12 Si7 O8 112.8(4) . . ? O12 Si7 O9 114.1(4) . . ? O8 Si7 O9 112.2(4) . . ? O12 Si7 C71 105.9(5) . . ? O8 Si7 C71 105.4(5) . . ? O9 Si7 C71 105.6(5) . . ? O9 Si8 O11 114.2(4) . 3_657 ? O9 Si8 O10 112.0(4) . . ? O11 Si8 O10 111.7(4) 3_657 . ? O9 Si8 C81 106.0(5) . . ? O11 Si8 C81 103.9(5) 3_657 . ? O10 Si8 C81 108.2(5) . . ? C102 C101 N1 114.2(18) . . ? C102 C101 H10A 108.7 . . ? N1 C101 H10A 108.7 . . ? C102 C101 H10B 108.7 . . ? N1 C101 H10B 108.7 . . ? H10A C101 H10B 107.6 . . ? C103 C102 C101 137(2) . . ? C103 C102 H10C 102.9 . . ? C101 C102 H10C 102.9 . . ? C103 C102 H10D 102.9 . . ? C101 C102 H10D 102.9 . . ? H10C C102 H10D 105.1 . . ? C104 C103 C102 117(2) . . ? C104 C103 H10E 108.1 . . ? C102 C103 H10E 108.1 . . ? C104 C103 H10F 108.1 . . ? C102 C103 H10F 108.1 . . ? H10E C103 H10F 107.3 . . ? C103 C104 H10G 109.5 . . ? C103 C104 H10H 109.5 . . ? H10G C104 H10H 109.5 . . ? C103 C104 H10I 109.5 . . ? H10G C104 H10I 109.5 . . ? H10H C104 H10I 109.5 . . ? N1 C105 C106 113.4(18) . . ? N1 C105 H10J 108.9 . . ? C106 C105 H10J 108.9 . . ? N1 C105 H10K 108.9 . . ? C106 C105 H10K 108.9 . . ? H10J C105 H10K 107.7 . . ? C105 C106 C107 111(2) . . ? C105 C106 H10L 109.4 . . ? C107 C106 H10L 109.4 . . ? C105 C106 H10M 109.4 . . ? C107 C106 H10M 109.4 . . ? H10L C106 H10M 108.0 . . ? C108 C107 C106 108(2) . . ? C108 C107 H10N 110.2 . . ? C106 C107 H10N 110.2 . . ? C108 C107 H10O 110.2 . . ? C106 C107 H10O 110.2 . . ? H10N C107 H10O 108.5 . . ? C107 C108 H10P 109.5 . . ? C107 C108 H10Q 109.5 . . ? H10P C108 H10Q 109.5 . . ? C107 C108 H10R 109.5 . . ? H10P C108 H10R 109.5 . . ? H10Q C108 H10R 109.5 . . ? C110 C109 N1 115.1(17) . . ? C110 C109 H10S 108.5 . . ? N1 C109 H10S 108.5 . . ? C110 C109 H10T 108.5 . . ? N1 C109 H10T 108.5 . . ? H10S C109 H10T 107.5 . . ? C109 C110 C111 105.7(17) . . ? C109 C110 H11A 110.6 . . ? C111 C110 H11A 110.6 . . ? C109 C110 H11B 110.6 . . ? C111 C110 H11B 110.6 . . ? H11A C110 H11B 108.7 . . ? C112 C111 C110 112(2) . . ? C112 C111 H11C 109.3 . . ? C110 C111 H11C 109.3 . . ? C112 C111 H11D 109.3 . . ? C110 C111 H11D 109.3 . . ? H11C C111 H11D 107.9 . . ? C111 C112 H11E 109.5 . . ? C111 C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C111 C112 H11G 109.5 . . ? H11E C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? C114 C113 N1 116.5(16) . . ? C114 C113 H11H 108.2 . . ? N1 C113 H11H 108.2 . . ? C114 C113 H11I 108.2 . . ? N1 C113 H11I 108.2 . . ? H11H C113 H11I 107.3 . . ? C113 C114 C115 103.2(19) . . ? C113 C114 H11J 111.1 . . ? C115 C114 H11J 111.1 . . ? C113 C114 H11K 111.1 . . ? C115 C114 H11K 111.1 . . ? H11J C114 H11K 109.1 . . ? C116 C115 C114 109(2) . . ? C116 C115 H11L 109.9 . . ? C114 C115 H11L 109.9 . . ? C116 C115 H11M 109.9 . . ? C114 C115 H11M 109.9 . . ? H11L C115 H11M 108.3 . . ? C115 C116 H11N 109.5 . . ? C115 C116 H11O 109.5 . . ? H11N C116 H11O 109.5 . . ? C115 C116 H11P 109.5 . . ? H11N C116 H11P 109.5 . . ? H11O C116 H11P 109.5 . . ? C105 N1 C113 108.6(17) . . ? C105 N1 C101 113.8(18) . . ? C113 N1 C101 108.7(16) . . ? C105 N1 C109 106.4(16) . . ? C113 N1 C109 110.6(17) . . ? C101 N1 C109 108.7(16) . . ? C202 C201 N2 117.9(17) . . ? C202 C201 H20A 107.8 . . ? N2 C201 H20A 107.8 . . ? C202 C201 H20B 107.8 . . ? N2 C201 H20B 107.8 . . ? H20A C201 H20B 107.2 . . ? C203 C202 C201 143(3) . . ? C203 C202 H20C 101.2 . . ? C201 C202 H20C 101.2 . . ? C203 C202 H20D 101.2 . . ? C201 C202 H20D 101.2 . . ? H20C C202 H20D 104.5 . . ? C204 C203 C202 128(2) . . ? C204 C203 H20E 105.3 . . ? C202 C203 H20E 105.3 . . ? C204 C203 H20F 105.3 . . ? C202 C203 H20F 105.3 . . ? H20E C203 H20F 106.0 . . ? C203 C204 H20G 109.5 . . ? C203 C204 H20H 109.5 . . ? H20G C204 H20H 109.5 . . ? C203 C204 H20I 109.5 . . ? H20G C204 H20I 109.5 . . ? H20H C204 H20I 109.5 . . ? N2 C205 C206 114.1(19) . . ? N2 C205 H20J 108.7 . . ? C206 C205 H20J 108.7 . . ? N2 C205 H20K 108.7 . . ? C206 C205 H20K 108.7 . . ? H20J C205 H20K 107.6 . . ? C205 C206 C207 112(2) . . ? C205 C206 H20L 109.2 . . ? C207 C206 H20L 109.2 . . ? C205 C206 H20M 109.2 . . ? C207 C206 H20M 109.2 . . ? H20L C206 H20M 107.9 . . ? C208 C207 C206 110(3) . . ? C208 C207 H20N 109.7 . . ? C206 C207 H20N 109.7 . . ? C208 C207 H20O 109.7 . . ? C206 C207 H20O 109.7 . . ? H20N C207 H20O 108.2 . . ? C207 C208 H20P 109.5 . . ? C207 C208 H20Q 109.5 . . ? H20P C208 H20Q 109.5 . . ? C207 C208 H20R 109.5 . . ? H20P C208 H20R 109.5 . . ? H20Q C208 H20R 109.5 . . ? C210 C209 N2 116.0(16) . . ? C210 C209 H20S 108.3 . . ? N2 C209 H20S 108.3 . . ? C210 C209 H20T 108.3 . . ? N2 C209 H20T 108.3 . . ? H20S C209 H20T 107.4 . . ? C209 C210 C211 110.6(19) . . ? C209 C210 H21A 109.5 . . ? C211 C210 H21A 109.5 . . ? C209 C210 H21B 109.5 . . ? C211 C210 H21B 109.5 . . ? H21A C210 H21B 108.1 . . ? C212 C211 C210 111(2) . . ? C212 C211 H21C 109.4 . . ? C210 C211 H21C 109.4 . . ? C212 C211 H21D 109.4 . . ? C210 C211 H21D 109.4 . . ? H21C C211 H21D 108.0 . . ? C211 C212 H21E 109.5 . . ? C211 C212 H21F 109.5 . . ? H21E C212 H21F 109.5 . . ? C211 C212 H21G 109.5 . . ? H21E C212 H21G 109.5 . . ? H21F C212 H21G 109.5 . . ? C214 C213 N2 114.2(16) . . ? C214 C213 H21H 108.7 . . ? N2 C213 H21H 108.7 . . ? C214 C213 H21I 108.7 . . ? N2 C213 H21I 108.7 . . ? H21H C213 H21I 107.6 . . ? C213 C214 C215 101.4(18) . . ? C213 C214 H21J 111.5 . . ? C215 C214 H21J 111.5 . . ? C213 C214 H21K 111.5 . . ? C215 C214 H21K 111.5 . . ? H21J C214 H21K 109.3 . . ? C216 C215 C214 111(2) . . ? C216 C215 H21L 109.4 . . ? C214 C215 H21L 109.4 . . ? C216 C215 H21M 109.4 . . ? C214 C215 H21M 109.4 . . ? H21L C215 H21M 108.0 . . ? C215 C216 H21N 109.5 . . ? C215 C216 H21O 109.5 . . ? H21N C216 H21O 109.5 . . ? C215 C216 H21P 109.5 . . ? H21N C216 H21P 109.5 . . ? H21O C216 H21P 109.5 . . ? C201 N2 C205 115.2(17) . . ? C201 N2 C213 108.8(16) . . ? C205 N2 C213 107.7(16) . . ? C201 N2 C209 108.5(15) . . ? C205 N2 C209 106.4(16) . . ? C213 N2 C209 110.1(16) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.879 _refine_diff_density_min -0.805 _refine_diff_density_rms 0.103 #===END data_compound9 #TrackingRef '- Cif Files.cif' _database_code_depnum_ccdc_archive 'CCDC 835363' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H92 F N O20 Si8' _chemical_formula_sum 'C72 H92 F N O20 Si8' _chemical_formula_weight 1535.19 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6188(5) _cell_length_b 12.8071(5) _cell_length_c 46.5571(19) _cell_angle_alpha 90.00 _cell_angle_beta 92.2580(10) _cell_angle_gamma 90.00 _cell_volume 7518.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10626 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description shard _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3248 _exptl_absorpt_coefficient_mu 0.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9578 _exptl_absorpt_correction_T_max 0.9914 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 50830 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0787 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16108 _reflns_number_gt 10226 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1689P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16108 _refine_ls_number_parameters 931 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1206 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.2543 _refine_ls_wR_factor_gt 0.2001 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9089(3) -0.2054(3) 0.06428(8) 0.0216(8) Uani 1 1 d . . . C2 C 0.9112(3) -0.3105(3) 0.07332(8) 0.0263(9) Uani 1 1 d . . . H2 H 0.8750 -0.3298 0.0900 0.032 Uiso 1 1 calc R . . C3 C 0.9648(3) -0.3861(3) 0.05851(9) 0.0306(10) Uani 1 1 d . . . H3 H 0.9649 -0.4564 0.0651 0.037 Uiso 1 1 calc R . . C4 C 1.0189(3) -0.3597(3) 0.03398(8) 0.0251(8) Uani 1 1 d . . . C5 C 1.0151(3) -0.2579(3) 0.02379(9) 0.0260(9) Uani 1 1 d . . . H5 H 1.0489 -0.2398 0.0066 0.031 Uiso 1 1 calc R . . C6 C 0.9609(3) -0.1824(3) 0.03916(8) 0.0250(9) Uani 1 1 d . . . H6 H 0.9595 -0.1126 0.0322 0.030 Uiso 1 1 calc R . . C7 C 1.1294(3) -0.4177(3) -0.00389(9) 0.0325(10) Uani 1 1 d . . . H7A H 1.0784 -0.3956 -0.0191 0.049 Uiso 1 1 calc R . . H7B H 1.1660 -0.4809 -0.0100 0.049 Uiso 1 1 calc R . . H7C H 1.1813 -0.3620 -0.0001 0.049 Uiso 1 1 calc R . . C8 C 0.5108(3) -0.0674(3) 0.06763(8) 0.0220(8) Uani 1 1 d . . . C9 C 0.4812(3) -0.0129(3) 0.04258(9) 0.0341(10) Uani 1 1 d . . . H9 H 0.5171 0.0502 0.0384 0.041 Uiso 1 1 calc R . . C10 C 0.4001(4) -0.0478(3) 0.02333(9) 0.0364(10) Uani 1 1 d . . . H10 H 0.3843 -0.0104 0.0061 0.044 Uiso 1 1 calc R . . C11 C 0.3448(3) -0.1347(3) 0.02940(9) 0.0310(10) Uani 1 1 d . . . C12 C 0.3685(4) -0.1894(4) 0.05473(11) 0.0507(14) Uani 1 1 d . . . H12 H 0.3290 -0.2499 0.0593 0.061 Uiso 1 1 calc R . . C13 C 0.4506(4) -0.1548(4) 0.07350(10) 0.0462(12) Uani 1 1 d . . . H13 H 0.4655 -0.1924 0.0908 0.055 Uiso 1 1 calc R . . C14 C 0.2399(4) -0.1267(4) -0.01442(10) 0.0470(13) Uani 1 1 d . . . H14A H 0.2136 -0.0562 -0.0107 0.070 Uiso 1 1 calc R . . H14B H 0.1852 -0.1666 -0.0252 0.070 Uiso 1 1 calc R . . H14C H 0.3037 -0.1223 -0.0257 0.070 Uiso 1 1 calc R . . C15 C 0.5472(3) -0.1142(3) 0.17834(7) 0.0190(8) Uani 1 1 d . . . C16 C 0.4362(3) -0.1050(3) 0.17411(8) 0.0244(8) Uani 1 1 d . . . H16 H 0.4083 -0.0524 0.1616 0.029 Uiso 1 1 calc R . . C17 C 0.3673(3) -0.1700(3) 0.18760(9) 0.0283(9) Uani 1 1 d . . . H17 H 0.2930 -0.1614 0.1843 0.034 Uiso 1 1 calc R . . C18 C 0.4051(3) -0.2483(3) 0.20600(9) 0.0264(9) Uani 1 1 d . . . C19 C 0.5145(3) -0.2592(3) 0.21156(8) 0.0245(8) Uani 1 1 d . . . H19 H 0.5416 -0.3112 0.2244 0.029 Uiso 1 1 calc R . . C20 C 0.5825(3) -0.1911(3) 0.19762(8) 0.0221(8) Uani 1 1 d . . . H20 H 0.6567 -0.1977 0.2015 0.027 Uiso 1 1 calc R . . C21 C 0.3670(4) -0.4007(3) 0.23420(11) 0.0403(12) Uani 1 1 d . . . H21A H 0.4163 -0.4430 0.2233 0.061 Uiso 1 1 calc R . . H21B H 0.3064 -0.4437 0.2393 0.061 Uiso 1 1 calc R . . H21C H 0.4034 -0.3746 0.2517 0.061 Uiso 1 1 calc R . . C22 C 0.9288(3) -0.2215(3) 0.17646(8) 0.0221(8) Uani 1 1 d . . . C23 C 0.8657(3) -0.3035(3) 0.18536(9) 0.0264(9) Uani 1 1 d . . . H23 H 0.7955 -0.3092 0.1773 0.032 Uiso 1 1 calc R . . C24 C 0.9004(3) -0.3777(3) 0.20554(8) 0.0266(9) Uani 1 1 d . . . H24 H 0.8542 -0.4319 0.2112 0.032 Uiso 1 1 calc R . . C25 C 1.0023(3) -0.3717(3) 0.21716(8) 0.0275(9) Uani 1 1 d . . . C26 C 1.0700(3) -0.2919(3) 0.20863(9) 0.0303(9) Uani 1 1 d . . . H26 H 1.1410 -0.2883 0.2162 0.036 Uiso 1 1 calc R . . C27 C 1.0323(3) -0.2185(3) 0.18904(9) 0.0257(9) Uani 1 1 d . . . H27 H 1.0782 -0.1634 0.1838 0.031 Uiso 1 1 calc R . . C28 C 0.9730(4) -0.5091(4) 0.25071(10) 0.0410(12) Uani 1 1 d . . . H28A H 0.9167 -0.4680 0.2592 0.061 Uiso 1 1 calc R . . H28B H 1.0114 -0.5487 0.2658 0.061 Uiso 1 1 calc R . . H28C H 0.9417 -0.5576 0.2365 0.061 Uiso 1 1 calc R . . C30 C 1.1034(3) 0.1117(3) 0.05060(8) 0.0258(9) Uani 1 1 d . . . H30 H 1.0966 0.0382 0.0525 0.031 Uiso 1 1 calc R . . C31 C 1.1806(3) 0.1502(3) 0.03306(9) 0.0309(10) Uani 1 1 d . . . H31 H 1.2260 0.1037 0.0235 0.037 Uiso 1 1 calc R . . C32 C 1.1911(3) 0.2572(3) 0.02964(8) 0.0264(9) Uani 1 1 d . . . C33 C 1.1267(3) 0.3243(3) 0.04448(9) 0.0293(9) Uani 1 1 d . . . H33 H 1.1351 0.3977 0.0427 0.035 Uiso 1 1 calc R . . C34 C 1.0506(3) 0.2848(3) 0.06186(9) 0.0261(9) Uani 1 1 d . . . H34 H 1.0069 0.3321 0.0717 0.031 Uiso 1 1 calc R . . C35 C 1.3283(3) 0.2387(4) -0.00437(10) 0.0393(11) Uani 1 1 d . . . H35A H 1.3704 0.1923 0.0083 0.059 Uiso 1 1 calc R . . H35B H 1.3759 0.2817 -0.0156 0.059 Uiso 1 1 calc R . . H35C H 1.2829 0.1968 -0.0175 0.059 Uiso 1 1 calc R . . C36 C 0.6436(3) 0.3115(3) 0.07324(8) 0.0215(8) Uani 1 1 d . . . C37 C 0.6983(3) 0.4045(3) 0.06736(9) 0.0286(9) Uani 1 1 d . . . H37 H 0.7711 0.4101 0.0731 0.034 Uiso 1 1 calc R . . C38 C 0.6491(3) 0.4879(3) 0.05346(9) 0.0286(9) Uani 1 1 d . . . H38 H 0.6882 0.5493 0.0495 0.034 Uiso 1 1 calc R . . C39 C 0.5419(3) 0.4813(3) 0.04529(8) 0.0272(9) Uani 1 1 d . . . C40 C 0.4856(3) 0.3909(3) 0.05021(8) 0.0265(9) Uani 1 1 d . . . H40 H 0.4129 0.3856 0.0443 0.032 Uiso 1 1 calc R . . C41 C 0.5378(3) 0.3071(3) 0.06402(9) 0.0269(9) Uani 1 1 d . . . H41 H 0.4992 0.2448 0.0672 0.032 Uiso 1 1 calc R . . C42 C 0.3900(3) 0.5635(4) 0.02311(10) 0.0412(12) Uani 1 1 d . . . H42A H 0.3788 0.5041 0.0101 0.062 Uiso 1 1 calc R . . H42B H 0.3695 0.6282 0.0131 0.062 Uiso 1 1 calc R . . H42C H 0.3467 0.5545 0.0400 0.062 Uiso 1 1 calc R . . C43 C 0.6851(3) 0.2878(3) 0.18567(8) 0.0184(8) Uani 1 1 d . . . C44 C 0.6618(3) 0.3904(3) 0.17715(8) 0.0240(8) Uani 1 1 d . . . H44 H 0.6547 0.4065 0.1572 0.029 Uiso 1 1 calc R . . C45 C 0.6490(3) 0.4683(3) 0.19703(8) 0.0281(9) Uani 1 1 d . . . H45 H 0.6334 0.5373 0.1906 0.034 Uiso 1 1 calc R . . C46 C 0.6584(3) 0.4480(3) 0.22644(8) 0.0234(8) Uani 1 1 d . . . C47 C 0.6805(3) 0.3476(3) 0.23531(8) 0.0275(9) Uani 1 1 d . . . H47 H 0.6865 0.3319 0.2553 0.033 Uiso 1 1 calc R . . C48 C 0.6939(3) 0.2690(3) 0.21517(9) 0.0269(9) Uani 1 1 d . . . H48 H 0.7097 0.2003 0.2217 0.032 Uiso 1 1 calc R . . C49 C 0.6384(4) 0.5111(4) 0.27401(8) 0.0372(11) Uani 1 1 d . . . H49A H 0.5873 0.4549 0.2770 0.056 Uiso 1 1 calc R . . H49B H 0.6155 0.5744 0.2839 0.056 Uiso 1 1 calc R . . H49C H 0.7085 0.4900 0.2818 0.056 Uiso 1 1 calc R . . C50 C 1.0632(3) 0.1673(3) 0.17849(8) 0.0206(8) Uani 1 1 d . . . C51 C 1.1666(3) 0.1282(3) 0.17803(9) 0.0302(9) Uani 1 1 d . . . H51 H 1.1794 0.0670 0.1672 0.036 Uiso 1 1 calc R . . C52 C 1.2517(3) 0.1759(3) 0.19297(9) 0.0329(10) Uani 1 1 d . . . H52 H 1.3208 0.1467 0.1925 0.039 Uiso 1 1 calc R . . C53 C 1.2343(3) 0.2659(3) 0.20844(9) 0.0321(10) Uani 1 1 d . . . C54 C 1.1320(4) 0.3056(4) 0.21005(11) 0.0403(11) Uani 1 1 d . . . H54 H 1.1194 0.3661 0.2212 0.048 Uiso 1 1 calc R . . C55 C 1.0492(3) 0.2563(3) 0.19534(9) 0.0308(9) Uani 1 1 d . . . H55 H 0.9797 0.2840 0.1967 0.037 Uiso 1 1 calc R . . C56 C 1.4191(4) 0.2884(4) 0.21994(13) 0.0563(15) Uani 1 1 d . . . H56A H 1.4273 0.2166 0.2270 0.085 Uiso 1 1 calc R . . H56B H 1.4668 0.3346 0.2312 0.085 Uiso 1 1 calc R . . H56C H 1.4366 0.2914 0.1996 0.085 Uiso 1 1 calc R . . C57 C 0.3855(3) -0.4437(3) 0.14161(9) 0.0284(9) Uani 1 1 d . . . H57A H 0.3780 -0.3787 0.1529 0.034 Uiso 1 1 calc R . . H57B H 0.4123 -0.4985 0.1550 0.034 Uiso 1 1 calc R . . C58 C 0.4684(3) -0.4253(3) 0.11937(9) 0.0323(10) Uani 1 1 d . . . H58A H 0.4980 -0.4930 0.1132 0.039 Uiso 1 1 calc R . . H58B H 0.4353 -0.3906 0.1023 0.039 Uiso 1 1 calc R . . C59 C 0.5565(3) -0.3571(4) 0.13225(9) 0.0339(10) Uani 1 1 d . . . H59A H 0.5811 -0.3876 0.1509 0.041 Uiso 1 1 calc R . . H59B H 0.5269 -0.2872 0.1362 0.041 Uiso 1 1 calc R . . C60 C 0.6521(4) -0.3437(4) 0.11352(11) 0.0448(12) Uani 1 1 d . . . H60A H 0.6850 -0.4119 0.1104 0.067 Uiso 1 1 calc R . . H60B H 0.7037 -0.2970 0.1231 0.067 Uiso 1 1 calc R . . H60C H 0.6289 -0.3136 0.0950 0.067 Uiso 1 1 calc R . . C61 C 0.2280(4) -0.3911(3) 0.11069(10) 0.0361(10) Uani 1 1 d . . . H61A H 0.2667 -0.3904 0.0926 0.043 Uiso 1 1 calc R . . H61B H 0.1534 -0.4098 0.1057 0.043 Uiso 1 1 calc R . . C62 C 0.2299(3) -0.2822(3) 0.12307(10) 0.0360(10) Uani 1 1 d . . . H62A H 0.2099 -0.2853 0.1434 0.043 Uiso 1 1 calc R . . H62B H 0.3031 -0.2544 0.1227 0.043 Uiso 1 1 calc R . . C63 C 0.1563(4) -0.2092(3) 0.10702(12) 0.0457(12) Uani 1 1 d . . . H63A H 0.0823 -0.2301 0.1104 0.055 Uiso 1 1 calc R . . H63B H 0.1675 -0.2164 0.0862 0.055 Uiso 1 1 calc R . . C64 C 0.1706(4) -0.0960(4) 0.11539(12) 0.0497(13) Uani 1 1 d . . . H64A H 0.1583 -0.0877 0.1359 0.075 Uiso 1 1 calc R . . H64B H 0.1199 -0.0530 0.1042 0.075 Uiso 1 1 calc R . . H64C H 0.2430 -0.0738 0.1115 0.075 Uiso 1 1 calc R . . C65 C 0.2819(3) -0.5756(3) 0.11220(9) 0.0321(10) Uani 1 1 d . . . H65A H 0.2088 -0.5969 0.1064 0.038 Uiso 1 1 calc R . . H65B H 0.3189 -0.5587 0.0944 0.038 Uiso 1 1 calc R . . C66 C 0.3372(4) -0.6684(3) 0.12638(9) 0.0339(10) Uani 1 1 d . . . H66A H 0.3127 -0.6772 0.1462 0.041 Uiso 1 1 calc R . . H66B H 0.4148 -0.6564 0.1275 0.041 Uiso 1 1 calc R . . C67 C 0.3124(3) -0.7673(3) 0.10881(10) 0.0364(11) Uani 1 1 d . . . H67A H 0.2368 -0.7856 0.1107 0.044 Uiso 1 1 calc R . . H67B H 0.3239 -0.7530 0.0883 0.044 Uiso 1 1 calc R . . C68 C 0.3810(4) -0.8599(4) 0.11855(11) 0.0451(12) Uani 1 1 d . . . H68A H 0.4560 -0.8418 0.1171 0.068 Uiso 1 1 calc R . . H68B H 0.3641 -0.9204 0.1063 0.068 Uiso 1 1 calc R . . H68C H 0.3668 -0.8770 0.1386 0.068 Uiso 1 1 calc R . . C69 C 0.2071(3) -0.4927(4) 0.15639(10) 0.0376(11) Uani 1 1 d . . . H69A H 0.2265 -0.5611 0.1650 0.045 Uiso 1 1 calc R . . H69B H 0.2274 -0.4386 0.1708 0.045 Uiso 1 1 calc R . . C70 C 0.0869(4) -0.4900(4) 0.15205(11) 0.0506(13) Uani 1 1 d . . . H70A H 0.0569 -0.4962 0.1713 0.061 Uiso 1 1 calc R . . H70B H 0.0680 -0.4196 0.1447 0.061 Uiso 1 1 calc R . . C71 C 0.0305(4) -0.5659(4) 0.13325(11) 0.0519(14) Uani 1 1 d . . . H71A H 0.0576 -0.6368 0.1377 0.062 Uiso 1 1 calc R . . H71B H 0.0460 -0.5504 0.1130 0.062 Uiso 1 1 calc R . . C72 C -0.0899(4) -0.5646(4) 0.13650(12) 0.0488(13) Uani 1 1 d . . . H72A H -0.1056 -0.5720 0.1568 0.073 Uiso 1 1 calc R . . H72B H -0.1222 -0.6226 0.1256 0.073 Uiso 1 1 calc R . . H72C H -0.1189 -0.4983 0.1292 0.073 Uiso 1 1 calc R . . C229 C 1.0349(3) 0.1763(3) 0.06562(8) 0.0211(8) Uani 1 1 d . . . N1 N 0.2754(3) -0.4763(3) 0.13005(7) 0.0282(8) Uani 1 1 d . . . O1 O 0.72683(19) -0.09197(19) 0.08066(5) 0.0209(6) Uani 1 1 d . . . O2 O 0.59550(19) -0.0502(2) 0.12366(5) 0.0209(6) Uani 1 1 d . . . O3 O 0.75337(19) -0.10292(19) 0.16277(5) 0.0205(6) Uani 1 1 d . . . O4 O 0.88145(19) -0.14681(19) 0.11980(5) 0.0194(5) Uani 1 1 d . . . O5 O 0.82913(19) 0.19735(19) 0.08499(5) 0.0199(6) Uani 1 1 d . . . O6 O 0.69198(19) 0.23146(19) 0.12766(5) 0.0202(6) Uani 1 1 d . . . O7 O 0.94965(19) -0.01405(19) 0.16136(5) 0.0205(6) Uani 1 1 d . . . O8 O 0.98279(19) 0.1364(2) 0.12256(5) 0.0207(6) Uani 1 1 d . . . O9 O 0.84786(19) 0.17012(19) 0.16593(5) 0.0202(5) Uani 1 1 d . . . O10 O 0.65258(19) 0.08026(19) 0.16700(5) 0.0201(6) Uani 1 1 d . . . O11 O 0.63752(19) 0.09941(19) 0.08394(5) 0.0215(6) Uani 1 1 d . . . O12 O 0.91655(19) 0.00361(19) 0.07984(5) 0.0216(6) Uani 1 1 d . . . O13 O 1.0742(2) -0.4392(2) 0.02185(6) 0.0339(7) Uani 1 1 d . . . O14 O 0.2648(2) -0.1772(3) 0.01199(7) 0.0471(9) Uani 1 1 d . . . O15 O 0.3303(2) -0.3140(2) 0.21687(7) 0.0362(7) Uani 1 1 d . . . O16 O 1.0449(2) -0.4406(2) 0.23703(6) 0.0350(7) Uani 1 1 d . . . O17 O 1.2641(2) 0.3044(2) 0.01243(6) 0.0339(7) Uani 1 1 d . . . O18 O 0.4997(2) 0.5688(2) 0.03214(7) 0.0381(8) Uani 1 1 d . . . O19 O 0.6440(2) 0.5315(2) 0.24404(6) 0.0313(7) Uani 1 1 d . . . O20 O 1.3118(2) 0.3214(3) 0.22295(8) 0.0479(9) Uani 1 1 d . . . Si1 Si 0.85385(8) -0.10315(8) 0.08754(2) 0.0183(2) Uani 1 1 d . . . Si2 Si 0.62530(8) -0.02450(8) 0.09073(2) 0.0189(2) Uani 1 1 d . . . Si3 Si 0.64289(8) -0.04096(8) 0.15655(2) 0.0181(2) Uani 1 1 d . . . Si4 Si 0.87552(8) -0.11468(8) 0.15338(2) 0.0184(2) Uani 1 1 d . . . Si5 Si 0.93439(8) 0.12457(8) 0.08973(2) 0.0186(2) Uani 1 1 d . . . Si6 Si 0.70564(8) 0.20211(8) 0.09387(2) 0.0188(2) Uani 1 1 d . . . Si7 Si 0.72073(8) 0.18460(8) 0.15951(2) 0.0182(2) Uani 1 1 d . . . Si8 Si 0.95350(8) 0.11115(8) 0.15550(2) 0.0186(2) Uani 1 1 d . . . F1 F 0.78715(16) 0.04412(16) 0.12309(4) 0.0257(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0215(19) 0.023(2) 0.0200(18) 0.0008(15) -0.0009(15) 0.0037(15) C2 0.038(2) 0.019(2) 0.023(2) -0.0016(16) 0.0075(17) -0.0017(17) C3 0.045(3) 0.019(2) 0.028(2) 0.0038(17) 0.0036(19) 0.0019(18) C4 0.028(2) 0.020(2) 0.027(2) -0.0054(17) 0.0008(16) 0.0041(16) C5 0.023(2) 0.027(2) 0.029(2) 0.0001(17) 0.0093(16) 0.0025(16) C6 0.034(2) 0.018(2) 0.0231(19) -0.0008(16) 0.0045(17) 0.0028(16) C7 0.030(2) 0.035(2) 0.034(2) -0.0079(19) 0.0117(18) 0.0035(19) C8 0.023(2) 0.022(2) 0.0204(18) 0.0020(16) 0.0005(15) -0.0009(16) C9 0.037(2) 0.033(2) 0.032(2) 0.0003(19) -0.0042(19) -0.008(2) C10 0.044(3) 0.039(3) 0.026(2) 0.0059(19) -0.0095(19) -0.002(2) C11 0.029(2) 0.036(2) 0.027(2) -0.0034(18) -0.0071(17) -0.0095(19) C12 0.056(3) 0.055(3) 0.040(3) 0.008(2) -0.012(2) -0.030(3) C13 0.056(3) 0.047(3) 0.035(3) 0.011(2) -0.011(2) -0.018(2) C14 0.045(3) 0.060(3) 0.035(3) 0.003(2) -0.018(2) -0.017(2) C15 0.023(2) 0.0167(19) 0.0170(17) -0.0020(14) 0.0009(15) -0.0011(15) C16 0.024(2) 0.026(2) 0.0238(19) 0.0019(16) -0.0011(16) 0.0006(16) C17 0.017(2) 0.031(2) 0.037(2) 0.0010(19) -0.0030(17) 0.0001(16) C18 0.025(2) 0.026(2) 0.028(2) 0.0002(17) 0.0048(17) -0.0022(17) C19 0.027(2) 0.023(2) 0.024(2) 0.0029(16) 0.0033(16) -0.0004(16) C20 0.0205(19) 0.026(2) 0.0201(18) -0.0050(16) 0.0016(15) -0.0017(15) C21 0.039(3) 0.031(3) 0.052(3) 0.011(2) 0.012(2) -0.007(2) C22 0.023(2) 0.024(2) 0.0198(18) -0.0006(16) 0.0004(15) 0.0002(16) C23 0.024(2) 0.022(2) 0.033(2) 0.0014(17) -0.0005(17) -0.0012(16) C24 0.034(2) 0.019(2) 0.027(2) 0.0028(17) 0.0070(17) -0.0022(17) C25 0.032(2) 0.024(2) 0.026(2) 0.0048(17) 0.0026(17) 0.0055(17) C26 0.022(2) 0.032(2) 0.036(2) 0.0120(19) -0.0067(17) -0.0004(17) C27 0.022(2) 0.024(2) 0.032(2) 0.0069(17) 0.0010(17) -0.0002(16) C28 0.051(3) 0.035(3) 0.038(3) 0.024(2) 0.012(2) 0.011(2) C30 0.029(2) 0.020(2) 0.029(2) -0.0019(17) 0.0036(17) -0.0004(16) C31 0.031(2) 0.027(2) 0.035(2) -0.0014(19) 0.0127(18) -0.0002(18) C32 0.025(2) 0.029(2) 0.025(2) 0.0078(17) -0.0004(16) -0.0026(17) C33 0.036(2) 0.021(2) 0.032(2) 0.0073(17) 0.0026(18) 0.0012(17) C34 0.029(2) 0.020(2) 0.028(2) 0.0011(17) 0.0003(17) 0.0030(16) C35 0.034(3) 0.047(3) 0.037(3) 0.002(2) 0.014(2) -0.009(2) C36 0.022(2) 0.024(2) 0.0185(18) 0.0003(15) 0.0009(15) 0.0017(15) C37 0.027(2) 0.027(2) 0.031(2) 0.0018(18) -0.0041(17) -0.0002(17) C38 0.032(2) 0.021(2) 0.032(2) 0.0055(17) -0.0018(18) -0.0010(17) C39 0.031(2) 0.025(2) 0.026(2) 0.0060(17) 0.0032(17) 0.0101(17) C40 0.019(2) 0.034(2) 0.026(2) 0.0066(17) 0.0000(16) 0.0050(17) C41 0.026(2) 0.026(2) 0.029(2) 0.0030(17) 0.0004(17) 0.0010(17) C42 0.036(3) 0.046(3) 0.041(3) 0.017(2) 0.000(2) 0.017(2) C43 0.0175(18) 0.0159(19) 0.0218(18) 0.0001(15) 0.0006(15) -0.0028(14) C44 0.033(2) 0.023(2) 0.0163(17) -0.0026(15) 0.0004(16) -0.0009(16) C45 0.044(3) 0.0138(19) 0.026(2) 0.0006(16) 0.0038(18) 0.0013(17) C46 0.029(2) 0.020(2) 0.0213(19) -0.0073(16) 0.0006(16) -0.0030(16) C47 0.032(2) 0.029(2) 0.0208(19) 0.0019(17) 0.0008(17) 0.0042(18) C48 0.033(2) 0.0149(19) 0.033(2) 0.0043(17) 0.0023(18) 0.0041(16) C49 0.056(3) 0.037(3) 0.019(2) -0.0095(19) 0.0056(19) -0.003(2) C50 0.0193(19) 0.025(2) 0.0173(17) 0.0029(15) 0.0002(14) -0.0032(15) C51 0.027(2) 0.033(2) 0.030(2) -0.0078(18) -0.0028(17) 0.0024(18) C52 0.022(2) 0.041(3) 0.035(2) -0.006(2) -0.0029(18) -0.0001(18) C53 0.028(2) 0.034(2) 0.033(2) 0.0031(19) -0.0072(18) -0.0087(19) C54 0.037(3) 0.032(3) 0.051(3) -0.021(2) -0.008(2) -0.001(2) C55 0.024(2) 0.031(2) 0.037(2) -0.0070(19) -0.0031(18) -0.0016(18) C56 0.029(3) 0.066(4) 0.072(4) 0.010(3) -0.017(3) -0.016(2) C57 0.030(2) 0.030(2) 0.025(2) 0.0003(17) -0.0032(17) 0.0033(17) C58 0.036(2) 0.032(2) 0.029(2) -0.0010(19) -0.0001(18) -0.0002(19) C59 0.034(2) 0.035(3) 0.032(2) 0.0002(19) -0.0048(19) -0.0014(19) C60 0.041(3) 0.040(3) 0.053(3) 0.001(2) -0.001(2) -0.009(2) C61 0.036(3) 0.036(3) 0.036(2) -0.002(2) -0.006(2) 0.003(2) C62 0.038(3) 0.029(2) 0.041(3) -0.002(2) 0.000(2) 0.0019(19) C63 0.049(3) 0.032(3) 0.056(3) 0.001(2) -0.007(2) 0.008(2) C64 0.044(3) 0.034(3) 0.071(4) -0.006(3) -0.006(3) 0.005(2) C65 0.038(3) 0.026(2) 0.032(2) -0.0043(18) 0.0017(19) 0.0008(18) C66 0.039(3) 0.027(2) 0.035(2) -0.0024(19) 0.005(2) -0.0003(19) C67 0.033(2) 0.028(2) 0.049(3) -0.001(2) 0.008(2) -0.0031(19) C68 0.051(3) 0.029(3) 0.056(3) 0.003(2) 0.016(2) 0.005(2) C69 0.037(3) 0.032(2) 0.045(3) -0.001(2) 0.014(2) -0.001(2) C70 0.051(3) 0.050(3) 0.052(3) -0.006(3) 0.017(2) -0.006(3) C71 0.065(4) 0.048(3) 0.044(3) 0.000(2) 0.015(3) -0.006(3) C72 0.041(3) 0.048(3) 0.057(3) -0.003(3) 0.001(2) -0.006(2) C229 0.025(2) 0.0196(19) 0.0184(18) 0.0034(15) 0.0012(15) -0.0008(15) N1 0.0325(19) 0.0215(18) 0.0305(18) -0.0011(15) -0.0015(15) 0.0000(14) O1 0.0212(13) 0.0197(14) 0.0215(13) -0.0013(11) -0.0010(10) 0.0007(11) O2 0.0191(13) 0.0261(15) 0.0170(12) -0.0026(11) -0.0033(10) -0.0025(11) O3 0.0203(13) 0.0202(14) 0.0211(13) 0.0028(11) 0.0014(10) 0.0019(10) O4 0.0247(14) 0.0157(13) 0.0178(13) -0.0010(10) -0.0007(10) 0.0025(10) O5 0.0216(13) 0.0179(13) 0.0202(13) 0.0018(10) 0.0011(10) 0.0020(10) O6 0.0272(14) 0.0150(13) 0.0180(13) -0.0019(10) -0.0017(11) 0.0013(11) O7 0.0222(13) 0.0161(13) 0.0230(13) 0.0016(11) -0.0016(10) -0.0019(10) O8 0.0192(13) 0.0245(14) 0.0184(13) 0.0014(11) 0.0009(10) -0.0031(11) O9 0.0179(13) 0.0202(13) 0.0225(13) -0.0004(11) 0.0008(10) -0.0002(10) O10 0.0215(13) 0.0177(13) 0.0213(13) -0.0003(10) 0.0021(10) -0.0009(10) O11 0.0250(14) 0.0193(14) 0.0200(13) 0.0005(11) -0.0042(11) 0.0001(11) O12 0.0264(14) 0.0152(13) 0.0236(13) 0.0018(11) 0.0054(11) 0.0001(11) O13 0.0426(18) 0.0251(16) 0.0346(17) -0.0035(13) 0.0074(14) 0.0098(13) O14 0.0426(19) 0.061(2) 0.0363(18) 0.0015(16) -0.0149(15) -0.0219(16) O15 0.0279(16) 0.0339(17) 0.0471(19) 0.0121(14) 0.0066(14) -0.0070(13) O16 0.0396(18) 0.0305(17) 0.0348(17) 0.0167(13) 0.0011(13) 0.0050(13) O17 0.0316(16) 0.0299(16) 0.0412(18) 0.0084(14) 0.0121(13) -0.0035(13) O18 0.0379(18) 0.0304(17) 0.0454(19) 0.0157(14) -0.0056(14) 0.0091(14) O19 0.0528(19) 0.0216(15) 0.0195(14) -0.0054(12) 0.0025(13) 0.0038(13) O20 0.0299(18) 0.050(2) 0.062(2) -0.0157(18) -0.0159(16) -0.0133(15) Si1 0.0209(5) 0.0170(5) 0.0170(5) 0.0000(4) 0.0007(4) -0.0003(4) Si2 0.0205(5) 0.0190(5) 0.0170(5) -0.0007(4) -0.0018(4) 0.0003(4) Si3 0.0196(5) 0.0177(5) 0.0170(5) -0.0009(4) 0.0009(4) -0.0008(4) Si4 0.0198(5) 0.0174(5) 0.0178(5) 0.0002(4) -0.0002(4) -0.0002(4) Si5 0.0211(5) 0.0170(5) 0.0176(5) 0.0007(4) 0.0009(4) 0.0000(4) Si6 0.0212(5) 0.0176(5) 0.0175(5) 0.0000(4) -0.0012(4) 0.0014(4) Si7 0.0203(5) 0.0177(5) 0.0166(5) -0.0004(4) -0.0004(4) 0.0005(4) Si8 0.0203(5) 0.0179(5) 0.0176(5) 0.0012(4) -0.0003(4) -0.0011(4) F1 0.0286(12) 0.0257(12) 0.0229(11) 0.0006(9) 0.0004(9) 0.0008(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.395(5) . ? C1 C2 1.410(5) . ? C1 Si1 1.852(4) . ? C2 C3 1.381(5) . ? C3 C4 1.395(5) . ? C4 O13 1.368(4) . ? C4 C5 1.388(5) . ? C5 C6 1.398(5) . ? C7 O13 1.436(5) . ? C8 C13 1.387(6) . ? C8 C9 1.398(5) . ? C8 Si2 1.850(4) . ? C9 C10 1.407(6) . ? C10 C11 1.349(6) . ? C11 O14 1.381(5) . ? C11 C12 1.394(6) . ? C12 C13 1.400(6) . ? C14 O14 1.414(5) . ? C15 C20 1.393(5) . ? C15 C16 1.412(5) . ? C15 Si3 1.861(4) . ? C16 C17 1.374(5) . ? C17 C18 1.391(6) . ? C18 O15 1.376(4) . ? C18 C19 1.400(5) . ? C19 C20 1.401(5) . ? C21 O15 1.439(5) . ? C22 C23 1.391(5) . ? C22 C27 1.411(5) . ? C22 Si4 1.849(4) . ? C23 C24 1.395(5) . ? C24 C25 1.377(6) . ? C25 O16 1.373(5) . ? C25 C26 1.400(5) . ? C26 C27 1.382(5) . ? C28 O16 1.430(5) . ? C30 C31 1.387(5) . ? C30 C229 1.403(5) . ? C31 C32 1.387(6) . ? C32 O17 1.384(4) . ? C32 C33 1.385(6) . ? C33 C34 1.377(5) . ? C34 C229 1.415(5) . ? C35 O17 1.424(5) . ? C36 C41 1.386(5) . ? C36 C37 1.409(5) . ? C36 Si6 1.855(4) . ? C37 C38 1.383(5) . ? C38 C39 1.394(6) . ? C39 O18 1.374(5) . ? C39 C40 1.382(5) . ? C40 C41 1.402(5) . ? C42 O18 1.433(5) . ? C43 C48 1.394(5) . ? C43 C44 1.401(5) . ? C43 Si7 1.864(4) . ? C44 C45 1.375(5) . ? C45 C46 1.394(5) . ? C46 O19 1.364(4) . ? C46 C47 1.376(5) . ? C47 C48 1.391(6) . ? C49 O19 1.424(4) . ? C50 C51 1.398(5) . ? C50 C55 1.399(5) . ? C50 Si8 1.861(4) . ? C51 C52 1.396(6) . ? C52 C53 1.382(6) . ? C53 O20 1.366(5) . ? C53 C54 1.391(6) . ? C54 C55 1.380(6) . ? C56 O20 1.430(6) . ? C57 C58 1.520(5) . ? C57 N1 1.527(5) . ? C58 C59 1.519(6) . ? C59 C60 1.526(6) . ? C61 C62 1.509(6) . ? C61 N1 1.522(5) . ? C62 C63 1.496(6) . ? C63 C64 1.511(6) . ? C65 C66 1.517(6) . ? C65 N1 1.523(5) . ? C66 C67 1.533(6) . ? C67 C68 1.527(6) . ? C69 C70 1.522(6) . ? C69 N1 1.541(5) . ? C70 C71 1.473(7) . ? C71 C72 1.534(7) . ? C229 Si5 1.849(4) . ? O1 Si1 1.628(3) . ? O1 Si2 1.630(3) . ? O2 Si3 1.626(3) . ? O2 Si2 1.627(3) . ? O3 Si3 1.620(3) . ? O3 Si4 1.626(3) . ? O4 Si4 1.621(3) . ? O4 Si1 1.627(3) . ? O5 Si6 1.629(3) . ? O5 Si5 1.630(3) . ? O6 Si7 1.627(3) . ? O6 Si6 1.633(3) . ? O7 Si4 1.627(3) . ? O7 Si8 1.627(3) . ? O8 Si8 1.624(3) . ? O8 Si5 1.631(3) . ? O9 Si8 1.623(3) . ? O9 Si7 1.631(3) . ? O10 Si3 1.630(3) . ? O10 Si7 1.634(3) . ? O11 Si2 1.627(3) . ? O11 Si6 1.628(3) . ? O12 Si1 1.627(3) . ? O12 Si5 1.629(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 116.6(3) . . ? C6 C1 Si1 122.7(3) . . ? C2 C1 Si1 120.3(3) . . ? C3 C2 C1 121.7(4) . . ? C2 C3 C4 120.3(4) . . ? O13 C4 C5 124.7(3) . . ? O13 C4 C3 115.6(3) . . ? C5 C4 C3 119.8(3) . . ? C4 C5 C6 119.1(4) . . ? C1 C6 C5 122.6(4) . . ? C13 C8 C9 115.9(4) . . ? C13 C8 Si2 123.2(3) . . ? C9 C8 Si2 120.9(3) . . ? C8 C9 C10 122.5(4) . . ? C11 C10 C9 119.9(4) . . ? C10 C11 O14 125.0(4) . . ? C10 C11 C12 119.7(4) . . ? O14 C11 C12 115.2(4) . . ? C11 C12 C13 119.9(4) . . ? C8 C13 C12 122.0(4) . . ? C20 C15 C16 116.1(3) . . ? C20 C15 Si3 120.6(3) . . ? C16 C15 Si3 122.9(3) . . ? C17 C16 C15 121.9(4) . . ? C16 C17 C18 120.7(4) . . ? O15 C18 C17 116.3(3) . . ? O15 C18 C19 123.8(4) . . ? C17 C18 C19 119.9(4) . . ? C18 C19 C20 118.0(4) . . ? C15 C20 C19 123.5(4) . . ? C23 C22 C27 115.4(4) . . ? C23 C22 Si4 122.1(3) . . ? C27 C22 Si4 122.0(3) . . ? C22 C23 C24 123.1(4) . . ? C25 C24 C23 119.3(4) . . ? O16 C25 C24 124.3(4) . . ? O16 C25 C26 115.7(4) . . ? C24 C25 C26 120.0(4) . . ? C27 C26 C25 119.1(4) . . ? C26 C27 C22 123.0(4) . . ? C31 C30 C229 123.0(4) . . ? C32 C31 C30 119.5(4) . . ? O17 C32 C33 115.8(3) . . ? O17 C32 C31 124.6(4) . . ? C33 C32 C31 119.7(4) . . ? C34 C33 C32 120.1(4) . . ? C33 C34 C229 122.5(4) . . ? C41 C36 C37 116.6(4) . . ? C41 C36 Si6 120.7(3) . . ? C37 C36 Si6 122.6(3) . . ? C38 C37 C36 122.0(4) . . ? C37 C38 C39 119.6(4) . . ? O18 C39 C40 124.4(4) . . ? O18 C39 C38 115.2(4) . . ? C40 C39 C38 120.3(4) . . ? C39 C40 C41 118.8(4) . . ? C36 C41 C40 122.7(4) . . ? C48 C43 C44 116.7(3) . . ? C48 C43 Si7 120.6(3) . . ? C44 C43 Si7 122.2(3) . . ? C45 C44 C43 121.3(4) . . ? C44 C45 C46 121.2(4) . . ? O19 C46 C47 125.6(4) . . ? O19 C46 C45 115.8(3) . . ? C47 C46 C45 118.5(3) . . ? C46 C47 C48 120.2(4) . . ? C47 C48 C43 122.1(4) . . ? C51 C50 C55 116.1(4) . . ? C51 C50 Si8 121.8(3) . . ? C55 C50 Si8 122.0(3) . . ? C52 C51 C50 122.3(4) . . ? C53 C52 C51 119.3(4) . . ? O20 C53 C52 124.5(4) . . ? O20 C53 C54 115.5(4) . . ? C52 C53 C54 120.0(4) . . ? C55 C54 C53 119.5(4) . . ? C54 C55 C50 122.7(4) . . ? C58 C57 N1 116.3(3) . . ? C59 C58 C57 109.5(3) . . ? C58 C59 C60 114.9(4) . . ? C62 C61 N1 115.8(4) . . ? C63 C62 C61 112.7(4) . . ? C62 C63 C64 113.9(4) . . ? C66 C65 N1 116.8(3) . . ? C65 C66 C67 109.5(4) . . ? C68 C67 C66 112.4(4) . . ? C70 C69 N1 118.5(4) . . ? C71 C70 C69 121.3(4) . . ? C70 C71 C72 113.1(4) . . ? C30 C229 C34 115.2(3) . . ? C30 C229 Si5 122.8(3) . . ? C34 C229 Si5 121.9(3) . . ? C61 N1 C65 107.7(3) . . ? C61 N1 C57 110.2(3) . . ? C65 N1 C57 110.6(3) . . ? C61 N1 C69 110.4(3) . . ? C65 N1 C69 111.3(3) . . ? C57 N1 C69 106.7(3) . . ? Si1 O1 Si2 140.26(17) . . ? Si3 O2 Si2 141.50(17) . . ? Si3 O3 Si4 144.64(17) . . ? Si4 O4 Si1 141.85(17) . . ? Si6 O5 Si5 140.31(17) . . ? Si7 O6 Si6 139.88(16) . . ? Si4 O7 Si8 139.72(17) . . ? Si8 O8 Si5 140.88(16) . . ? Si8 O9 Si7 144.25(17) . . ? Si3 O10 Si7 138.50(16) . . ? Si2 O11 Si6 141.79(17) . . ? Si1 O12 Si5 143.11(16) . . ? C4 O13 C7 118.3(3) . . ? C11 O14 C14 117.5(3) . . ? C18 O15 C21 117.9(3) . . ? C25 O16 C28 117.1(3) . . ? C32 O17 C35 117.8(3) . . ? C39 O18 C42 116.4(3) . . ? C46 O19 C49 117.2(3) . . ? C53 O20 C56 117.4(4) . . ? O12 Si1 O4 113.83(14) . . ? O12 Si1 O1 111.48(14) . . ? O4 Si1 O1 112.65(13) . . ? O12 Si1 C1 105.57(15) . . ? O4 Si1 C1 103.01(15) . . ? O1 Si1 C1 109.64(15) . . ? O2 Si2 O11 114.10(14) . . ? O2 Si2 O1 112.17(14) . . ? O11 Si2 O1 112.31(14) . . ? O2 Si2 C8 106.48(15) . . ? O11 Si2 C8 104.73(15) . . ? O1 Si2 C8 106.26(15) . . ? O3 Si3 O2 114.48(13) . . ? O3 Si3 O10 111.06(14) . . ? O2 Si3 O10 111.79(14) . . ? O3 Si3 C15 103.17(15) . . ? O2 Si3 C15 104.71(15) . . ? O10 Si3 C15 111.12(14) . . ? O4 Si4 O3 111.30(14) . . ? O4 Si4 O7 111.92(13) . . ? O3 Si4 O7 114.08(14) . . ? O4 Si4 C22 110.07(15) . . ? O3 Si4 C22 103.82(15) . . ? O7 Si4 C22 105.11(15) . . ? O12 Si5 O5 113.74(14) . . ? O12 Si5 O8 113.32(14) . . ? O5 Si5 O8 110.28(13) . . ? O12 Si5 C229 105.04(15) . . ? O5 Si5 C229 106.73(15) . . ? O8 Si5 C229 107.16(15) . . ? O11 Si6 O5 113.41(13) . . ? O11 Si6 O6 112.64(13) . . ? O5 Si6 O6 113.03(14) . . ? O11 Si6 C36 104.81(15) . . ? O5 Si6 C36 106.59(15) . . ? O6 Si6 C36 105.46(15) . . ? O6 Si7 O9 113.05(13) . . ? O6 Si7 O10 113.32(14) . . ? O9 Si7 O10 112.95(13) . . ? O6 Si7 C43 106.45(15) . . ? O9 Si7 C43 102.78(15) . . ? O10 Si7 C43 107.33(14) . . ? O9 Si8 O8 114.21(14) . . ? O9 Si8 O7 112.21(13) . . ? O8 Si8 O7 111.35(14) . . ? O9 Si8 C50 104.44(15) . . ? O8 Si8 C50 105.91(14) . . ? O7 Si8 C50 108.11(15) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.773 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.157 #===END data_compound11 #TrackingRef '- Cif Files.cif' _database_code_depnum_ccdc_archive 'CCDC 835364' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H108 F N O12 Si8' _chemical_formula_sum 'C94 H108 F N O12 Si8' _chemical_formula_weight 1687.53 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5940(3) _cell_length_b 15.2028(3) _cell_length_c 22.2570(4) _cell_angle_alpha 86.9340(10) _cell_angle_beta 85.9290(10) _cell_angle_gamma 75.9750(10) _cell_volume 4448.28(15) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 19292 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.184 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9334 _exptl_absorpt_correction_T_max 0.9818 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66463 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.64 _reflns_number_total 20347 _reflns_number_gt 14182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+13.4266P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20347 _refine_ls_number_parameters 1054 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1162 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.1782 _refine_ls_wR_factor_gt 0.1559 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.09227(7) 0.56095(6) 0.08469(4) 0.01761(18) Uani 1 1 d . . . O1 O 0.03710(17) 0.65013(14) 0.04516(9) 0.0201(5) Uani 1 1 d . . . Si2 Si -0.03424(7) 0.67916(5) -0.01145(4) 0.01770(18) Uani 1 1 d . . . O4 O -0.14505(16) 0.65850(14) 0.00317(10) 0.0207(5) Uani 1 1 d . . . Si3 Si 0.19703(7) 0.42713(6) -0.01258(4) 0.01791(18) Uani 1 1 d . . . O5 O 0.17846(16) 0.49065(14) 0.04541(9) 0.0201(5) Uani 1 1 d . . . O6 O 0.16804(16) 0.48226(14) -0.07594(9) 0.0203(5) Uani 1 1 d . . . Si4 Si -0.07091(7) 0.45503(6) 0.10864(4) 0.01782(18) Uani 1 1 d . . . O3 O 0.02049(17) 0.63776(14) -0.07419(10) 0.0210(5) Uani 1 1 d . . . O2 O 0.01176(16) 0.51199(14) 0.12206(9) 0.0202(5) Uani 1 1 d . . . C41 C -0.1202(2) 0.4132(2) 0.18147(14) 0.0228(7) Uani 1 1 d . . . H41 H -0.1430 0.4533 0.2136 0.027 Uiso 1 1 calc R . . C42 C -0.1234(3) 0.3260(2) 0.18846(15) 0.0264(7) Uani 1 1 d . . . H42 H -0.1003 0.2911 0.1538 0.032 Uiso 1 1 calc R . . C43 C -0.1569(3) 0.2752(2) 0.24099(16) 0.0288(8) Uani 1 1 d . . . C44 C -0.1514(3) 0.1833(3) 0.23515(19) 0.0375(9) Uani 1 1 d . . . H44 H -0.1285 0.1563 0.1976 0.045 Uiso 1 1 calc R . . C45 C -0.1789(3) 0.1302(3) 0.2834(2) 0.0489(11) Uani 1 1 d . . . H45 H -0.1752 0.0677 0.2788 0.059 Uiso 1 1 calc R . . C46 C -0.2114(3) 0.1692(3) 0.33781(19) 0.0469(11) Uani 1 1 d . . . H46 H -0.2298 0.1333 0.3710 0.056 Uiso 1 1 calc R . . C47 C -0.2177(3) 0.2596(3) 0.34470(18) 0.0449(11) Uani 1 1 d . . . H47 H -0.2401 0.2859 0.3826 0.054 Uiso 1 1 calc R . . C48 C -0.1911(3) 0.3131(3) 0.29629(16) 0.0356(9) Uani 1 1 d . . . H48 H -0.1965 0.3758 0.3012 0.043 Uiso 1 1 calc R . . C31 C 0.3354(2) 0.3792(2) -0.01943(14) 0.0228(7) Uani 1 1 d . . . H31 H 0.3623 0.3354 -0.0489 0.027 Uiso 1 1 calc R . . C32 C 0.3989(3) 0.4038(2) 0.01543(15) 0.0241(7) Uani 1 1 d . . . H32 H 0.3687 0.4466 0.0450 0.029 Uiso 1 1 calc R . . C33 C 0.5103(3) 0.3727(2) 0.01356(16) 0.0266(7) Uani 1 1 d . . . C38 C 0.5664(3) 0.3156(2) -0.02957(17) 0.0319(8) Uani 1 1 d . . . H38 H 0.5326 0.2951 -0.0600 0.038 Uiso 1 1 calc R . . C37 C 0.6717(3) 0.2880(3) -0.02894(19) 0.0409(10) Uani 1 1 d . . . H37 H 0.7092 0.2490 -0.0588 0.049 Uiso 1 1 calc R . . C36 C 0.7217(3) 0.3172(3) 0.0149(2) 0.0408(10) Uani 1 1 d . . . H36 H 0.7934 0.2973 0.0156 0.049 Uiso 1 1 calc R . . C35 C 0.6681(3) 0.3751(3) 0.0577(2) 0.0414(10) Uani 1 1 d . . . H35 H 0.7026 0.3961 0.0875 0.050 Uiso 1 1 calc R . . C34 C 0.5627(3) 0.4026(2) 0.05697(18) 0.0321(8) Uani 1 1 d . . . H34 H 0.5258 0.4425 0.0866 0.038 Uiso 1 1 calc R . . C21 C -0.0554(2) 0.8036(2) -0.02199(14) 0.0201(6) Uani 1 1 d . . . H21 H -0.0648 0.8388 0.0129 0.024 Uiso 1 1 calc R . . C22 C -0.0584(2) 0.8469(2) -0.07608(15) 0.0228(7) Uani 1 1 d . . . H22 H -0.0473 0.8097 -0.1101 0.027 Uiso 1 1 calc R . . C23 C -0.0767(2) 0.9453(2) -0.08910(15) 0.0218(7) Uani 1 1 d . . . C24 C -0.0977(3) 1.0084(2) -0.04375(16) 0.0252(7) Uani 1 1 d . . . H24 H -0.1021 0.9879 -0.0028 0.030 Uiso 1 1 calc R . . C25 C -0.1120(3) 1.1004(2) -0.05753(17) 0.0282(7) Uani 1 1 d . . . H25 H -0.1249 1.1423 -0.0260 0.034 Uiso 1 1 calc R . . C26 C -0.1077(3) 1.1317(2) -0.11709(18) 0.0325(8) Uani 1 1 d . . . H26 H -0.1173 1.1948 -0.1265 0.039 Uiso 1 1 calc R . . C27 C -0.0893(3) 1.0706(2) -0.16278(17) 0.0315(8) Uani 1 1 d . . . H27 H -0.0879 1.0917 -0.2037 0.038 Uiso 1 1 calc R . . C28 C -0.0728(3) 0.9781(2) -0.14876(16) 0.0263(7) Uani 1 1 d . . . H28 H -0.0587 0.9365 -0.1804 0.032 Uiso 1 1 calc R . . C11 C 0.1619(3) 0.6063(2) 0.13938(14) 0.0226(7) Uani 1 1 d . . . H11 H 0.2261 0.6162 0.1253 0.027 Uiso 1 1 calc R . . C12 C 0.1319(3) 0.6264(2) 0.19612(16) 0.0288(8) Uani 1 1 d . . . H12 H 0.0742 0.6064 0.2125 0.035 Uiso 1 1 calc R . . C13 C 0.1786(3) 0.6769(2) 0.23680(16) 0.0297(8) Uani 1 1 d . . . C18 C 0.2702(3) 0.7005(3) 0.22179(18) 0.0370(9) Uani 1 1 d . . . H18 H 0.3078 0.6804 0.1854 0.044 Uiso 1 1 calc R . . C17 C 0.3070(4) 0.7533(3) 0.2598(2) 0.0475(11) Uani 1 1 d . . . H17 H 0.3697 0.7689 0.2492 0.057 Uiso 1 1 calc R . . C16 C 0.2531(4) 0.7833(3) 0.3127(2) 0.0511(12) Uani 1 1 d . . . H16 H 0.2783 0.8197 0.3383 0.061 Uiso 1 1 calc R . . C15 C 0.1635(4) 0.7603(4) 0.3278(2) 0.0610(14) Uani 1 1 d . . . H15 H 0.1261 0.7808 0.3641 0.073 Uiso 1 1 calc R . . C14 C 0.1263(4) 0.7072(3) 0.29057(18) 0.0487(11) Uani 1 1 d . . . H14 H 0.0640 0.6912 0.3020 0.058 Uiso 1 1 calc R . . Si5 Si -0.19616(7) 0.07836(6) 0.51092(4) 0.01840(18) Uani 1 1 d . . . O8 O -0.13961(17) 0.15998(14) 0.49632(10) 0.0215(5) Uani 1 1 d . . . Si6 Si -0.02715(7) 0.17702(6) 0.48077(4) 0.01858(18) Uani 1 1 d . . . O10 O 0.04390(17) 0.15101(14) 0.53768(10) 0.0224(5) Uani 1 1 d . . . Si7 Si -0.09539(7) -0.06490(6) 0.41937(4) 0.01845(18) Uani 1 1 d . . . O11 O -0.18156(16) 0.00904(14) 0.45622(9) 0.0204(5) Uani 1 1 d . . . O12 O -0.01192(17) -0.02154(14) 0.38036(9) 0.0200(5) Uani 1 1 d . . . Si8 Si -0.07386(7) -0.03426(6) 0.61086(4) 0.01863(18) Uani 1 1 d . . . O9 O 0.02732(17) 0.13160(14) 0.41902(9) 0.0219(5) Uani 1 1 d . . . O7 O -0.16887(17) 0.02753(14) 0.57568(9) 0.0204(5) Uani 1 1 d . . . C81 C -0.1297(3) -0.0608(2) 0.68571(14) 0.0226(7) Uani 1 1 d . . . H81 H -0.1633 -0.0119 0.7102 0.027 Uiso 1 1 calc R . . C82 C -0.1250(3) -0.1448(2) 0.70699(15) 0.0257(7) Uani 1 1 d . . . H82 H -0.0860 -0.1915 0.6824 0.031 Uiso 1 1 calc R . . C83 C -0.1718(3) -0.1763(2) 0.76347(15) 0.0259(7) Uani 1 1 d . . . C84 C -0.1425(3) -0.2667(2) 0.78245(16) 0.0285(7) Uani 1 1 d . . . H84 H -0.0925 -0.3075 0.7588 0.034 Uiso 1 1 calc R . . C85 C -0.1847(3) -0.2989(3) 0.83510(17) 0.0335(8) Uani 1 1 d . . . H85 H -0.1639 -0.3612 0.8471 0.040 Uiso 1 1 calc R . . C86 C -0.2567(3) -0.2403(3) 0.86997(16) 0.0344(9) Uani 1 1 d . . . H86 H -0.2852 -0.2620 0.9063 0.041 Uiso 1 1 calc R . . C87 C -0.2876(3) -0.1497(3) 0.85190(16) 0.0330(8) Uani 1 1 d . . . H87 H -0.3377 -0.1092 0.8757 0.040 Uiso 1 1 calc R . . C88 C -0.2453(3) -0.1180(2) 0.79897(16) 0.0290(7) Uani 1 1 d . . . H88 H -0.2667 -0.0558 0.7868 0.035 Uiso 1 1 calc R . . C71 C -0.1615(3) -0.1136(2) 0.36481(14) 0.0219(7) Uani 1 1 d . . . H71 H -0.2231 -0.1291 0.3788 0.026 Uiso 1 1 calc R . . C72 C -0.1301(3) -0.1288(2) 0.30724(14) 0.0235(7) Uani 1 1 d . . . H72 H -0.0762 -0.1027 0.2919 0.028 Uiso 1 1 calc R . . C73 C -0.1690(3) -0.1812(2) 0.26480(15) 0.0264(7) Uani 1 1 d . . . C78 C -0.2533(3) -0.2164(3) 0.27860(17) 0.0342(8) Uani 1 1 d . . . H78 H -0.2921 -0.2020 0.3155 0.041 Uiso 1 1 calc R . . C77 C -0.2822(4) -0.2724(3) 0.23936(19) 0.0483(11) Uani 1 1 d . . . H77 H -0.3400 -0.2961 0.2496 0.058 Uiso 1 1 calc R . . C76 C -0.2264(4) -0.2934(3) 0.1853(2) 0.0496(12) Uani 1 1 d . . . H76 H -0.2457 -0.3320 0.1585 0.059 Uiso 1 1 calc R . . C75 C -0.1441(3) -0.2589(3) 0.17039(18) 0.0446(11) Uani 1 1 d . . . H75 H -0.1058 -0.2734 0.1333 0.054 Uiso 1 1 calc R . . C74 C -0.1162(3) -0.2024(3) 0.20979(17) 0.0376(9) Uani 1 1 d . . . H74 H -0.0594 -0.1776 0.1987 0.045 Uiso 1 1 calc R . . C61 C -0.0476(2) 0.3006(2) 0.46771(14) 0.0220(7) Uani 1 1 d . . . H61 H -0.0673 0.3376 0.5017 0.026 Uiso 1 1 calc R . . C62 C -0.0370(3) 0.3418(2) 0.41449(14) 0.0230(7) Uani 1 1 d . . . H62 H -0.0133 0.3035 0.3815 0.028 Uiso 1 1 calc R . . C63 C -0.0577(2) 0.4404(2) 0.40056(15) 0.0235(7) Uani 1 1 d . . . C64 C -0.0810(3) 0.5039(2) 0.44570(17) 0.0289(8) Uani 1 1 d . . . H64 H -0.0859 0.4838 0.4867 0.035 Uiso 1 1 calc R . . C65 C -0.0971(3) 0.5957(2) 0.43141(19) 0.0358(9) Uani 1 1 d . . . H65 H -0.1105 0.6378 0.4627 0.043 Uiso 1 1 calc R . . C66 C -0.0938(3) 0.6265(3) 0.3724(2) 0.0425(10) Uani 1 1 d . . . H66 H -0.1053 0.6897 0.3630 0.051 Uiso 1 1 calc R . . C67 C -0.0738(3) 0.5651(3) 0.32645(19) 0.0399(9) Uani 1 1 d . . . H67 H -0.0735 0.5860 0.2855 0.048 Uiso 1 1 calc R . . C68 C -0.0541(3) 0.4728(2) 0.34110(16) 0.0280(7) Uani 1 1 d . . . H68 H -0.0377 0.4308 0.3097 0.034 Uiso 1 1 calc R . . C51 C -0.3333(3) 0.1337(2) 0.51699(14) 0.0228(7) Uani 1 1 d . . . H51 H -0.3558 0.1825 0.5435 0.027 Uiso 1 1 calc R . . C52 C -0.4026(3) 0.1090(2) 0.48627(15) 0.0252(7) Uani 1 1 d . . . H52 H -0.3774 0.0604 0.4599 0.030 Uiso 1 1 calc R . . C53 C -0.5132(3) 0.1478(2) 0.48812(15) 0.0267(7) Uani 1 1 d . . . C58 C -0.5745(3) 0.1021(2) 0.46153(16) 0.0290(8) Uani 1 1 d . . . H58 H -0.5438 0.0469 0.4424 0.035 Uiso 1 1 calc R . . C57 C -0.6791(3) 0.1344(2) 0.46200(17) 0.0316(8) Uani 1 1 d . . . H57 H -0.7193 0.1013 0.4438 0.038 Uiso 1 1 calc R . . C56 C -0.7243(3) 0.2151(3) 0.48916(19) 0.0387(9) Uani 1 1 d . . . H56 H -0.7958 0.2384 0.4894 0.046 Uiso 1 1 calc R . . C55 C -0.6643(3) 0.2613(3) 0.5160(2) 0.0470(11) Uani 1 1 d . . . H55 H -0.6953 0.3166 0.5349 0.056 Uiso 1 1 calc R . . C54 C -0.5606(3) 0.2288(3) 0.51579(19) 0.0417(10) Uani 1 1 d . . . H54 H -0.5210 0.2616 0.5347 0.050 Uiso 1 1 calc R . . F2 F 0.0000 0.0000 0.5000 0.0237(6) Uani 1 2 d S . . F1 F 0.0000 0.5000 0.0000 0.0229(6) Uani 1 2 d S . . N1 N 0.4890(2) 0.2515(3) 0.25789(14) 0.0424(9) Uani 1 1 d . . . C101 C 0.3763(3) 0.2921(4) 0.27142(19) 0.0470(11) Uani 1 1 d . . . H10A H 0.3524 0.3404 0.2405 0.056 Uiso 1 1 calc R . . H10B H 0.3391 0.2444 0.2677 0.056 Uiso 1 1 calc R . . C102 C 0.3490(4) 0.3320(4) 0.3332(2) 0.0635(15) Uani 1 1 d . . . H10C H 0.3961 0.3698 0.3414 0.076 Uiso 1 1 calc R . . H10D H 0.3552 0.2826 0.3646 0.076 Uiso 1 1 calc R . . C103 C 0.2348(4) 0.3926(6) 0.3349(3) 0.138(4) Uani 1 1 d . . . H10E H 0.2263 0.4342 0.2989 0.165 Uiso 1 1 calc R . . H10F H 0.1876 0.3525 0.3332 0.165 Uiso 1 1 calc R . . C109 C 0.5020(3) 0.2213(3) 0.19294(17) 0.0411(10) Uani 1 1 d . . . H10G H 0.4559 0.1810 0.1882 0.049 Uiso 1 1 calc R . . H10H H 0.4803 0.2755 0.1660 0.049 Uiso 1 1 calc R . . C110 C 0.6088(3) 0.1721(4) 0.17245(19) 0.0518(12) Uani 1 1 d . . . H11A H 0.6326 0.1190 0.2000 0.062 Uiso 1 1 calc R . . H11B H 0.6550 0.2131 0.1742 0.062 Uiso 1 1 calc R . . C111 C 0.6122(4) 0.1405(3) 0.10841(18) 0.0462(10) Uani 1 1 d . . . H11C H 0.5662 0.0994 0.1067 0.055 Uiso 1 1 calc R . . H11D H 0.5883 0.1936 0.0809 0.055 Uiso 1 1 calc R . . C112 C 0.7196(4) 0.0913(4) 0.0879(2) 0.0653(15) Uani 1 1 d . . . H11E H 0.7657 0.1311 0.0913 0.098 Uiso 1 1 calc R . . H11F H 0.7210 0.0748 0.0458 0.098 Uiso 1 1 calc R . . H11G H 0.7414 0.0363 0.1133 0.098 Uiso 1 1 calc R . . C113 C 0.5508(3) 0.3201(3) 0.26523(19) 0.0446(11) Uani 1 1 d . . . H11H H 0.6221 0.2935 0.2513 0.053 Uiso 1 1 calc R . . H11I H 0.5501 0.3315 0.3087 0.053 Uiso 1 1 calc R . . C114 C 0.5147(4) 0.4103(4) 0.2316(2) 0.0543(12) Uani 1 1 d . . . H11J H 0.4993 0.3993 0.1902 0.065 Uiso 1 1 calc R . . H11K H 0.4512 0.4449 0.2522 0.065 Uiso 1 1 calc R . . C115 C 0.5932(4) 0.4656(3) 0.2284(2) 0.0585(13) Uani 1 1 d . . . H11L H 0.6560 0.4312 0.2070 0.070 Uiso 1 1 calc R . . H11M H 0.6099 0.4746 0.2699 0.070 Uiso 1 1 calc R . . C116 C 0.5584(5) 0.5576(4) 0.1965(3) 0.0747(17) Uani 1 1 d . . . H11N H 0.5376 0.5494 0.1563 0.112 Uiso 1 1 calc R . . H11O H 0.6144 0.5882 0.1926 0.112 Uiso 1 1 calc R . . H11P H 0.5008 0.5945 0.2198 0.112 Uiso 1 1 calc R . . C106 C 0.4732(4) 0.0938(4) 0.2998(2) 0.0537(12) Uani 1 1 d . . . H10I H 0.4575 0.0865 0.2578 0.064 Uiso 1 1 calc R . . H10J H 0.4082 0.1094 0.3243 0.064 Uiso 1 1 calc R . . C107 C 0.5386(4) 0.0037(4) 0.3242(2) 0.0663(15) Uani 1 1 d . . . H10K H 0.5961 -0.0186 0.2947 0.080 Uiso 1 1 calc R . . H10L H 0.5672 0.0146 0.3621 0.080 Uiso 1 1 calc R . . C108 C 0.4791(5) -0.0687(4) 0.3364(3) 0.0792(18) Uani 1 1 d . . . H10M H 0.4236 -0.0480 0.3668 0.119 Uiso 1 1 calc R . . H10N H 0.5243 -0.1249 0.3513 0.119 Uiso 1 1 calc R . . H10O H 0.4509 -0.0801 0.2991 0.119 Uiso 1 1 calc R . . C121 C 0.5801(5) 0.4557(5) 0.4247(2) 0.0731(17) Uani 1 1 d . . . C126 C 0.6505(5) 0.5032(5) 0.4044(2) 0.0724(17) Uani 1 1 d . . . H126 H 0.7197 0.4800 0.4131 0.087 Uiso 1 1 calc R . . C125 C 0.6231(7) 0.5831(5) 0.3721(3) 0.089(2) Uani 1 1 d . . . H125 H 0.6729 0.6151 0.3585 0.107 Uiso 1 1 calc R . . C124 C 0.5265(8) 0.6164(6) 0.3596(4) 0.123(4) Uani 1 1 d . . . H124 H 0.5080 0.6711 0.3360 0.147 Uiso 1 1 calc R . . C122 C 0.4805(5) 0.4890(7) 0.4131(4) 0.111(3) Uani 1 1 d . . . H122 H 0.4312 0.4564 0.4267 0.134 Uiso 1 1 calc R . . C104 C 0.2070(6) 0.4479(6) 0.3910(4) 0.122(3) Uani 1 1 d . . . H10P H 0.2173 0.4072 0.4269 0.183 Uiso 1 1 calc R . . H10Q H 0.1356 0.4812 0.3910 0.183 Uiso 1 1 calc R . . H10R H 0.2501 0.4909 0.3915 0.183 Uiso 1 1 calc R . . C123 C 0.4524(7) 0.5715(8) 0.3810(5) 0.148(5) Uani 1 1 d . . . H123 H 0.3830 0.5969 0.3738 0.177 Uiso 1 1 calc R . . C131 C 0.5778(4) 0.8874(3) 0.0668(2) 0.0557(13) Uani 1 1 d . . . C134 C 0.4019(7) 0.9038(5) 0.1386(6) 0.121(4) Uani 1 1 d . . . H134 H 0.3418 0.9073 0.1638 0.145 Uiso 1 1 calc R . . C135 C 0.3984(7) 0.9098(5) 0.0819(7) 0.136(5) Uani 1 1 d . . . H135 H 0.3345 0.9204 0.0646 0.163 Uiso 1 1 calc R . . C132 C 0.5797(5) 0.8842(5) 0.1270(3) 0.088(2) Uani 1 1 d . . . H132 H 0.6427 0.8763 0.1450 0.105 Uiso 1 1 calc R . . C136 C 0.4851(8) 0.9014(5) 0.0446(3) 0.106(3) Uani 1 1 d . . . H136 H 0.4797 0.9056 0.0022 0.128 Uiso 1 1 calc R . . C137 C 0.6744(7) 0.8758(4) 0.0270(4) 0.136(4) Uani 1 1 d . . . H13A H 0.7322 0.8432 0.0498 0.204 Uiso 1 1 calc R . . H13B H 0.6845 0.9356 0.0134 0.204 Uiso 1 1 calc R . . H13C H 0.6693 0.8412 -0.0081 0.204 Uiso 1 1 calc R . . C127 C 0.6043(9) 0.3756(6) 0.4615(4) 0.162(5) Uani 1 1 d . . . H12A H 0.6731 0.3671 0.4751 0.243 Uiso 1 1 calc R . . H12B H 0.6010 0.3235 0.4383 0.243 Uiso 1 1 calc R . . H12C H 0.5557 0.3806 0.4966 0.243 Uiso 1 1 calc R . . C133 C 0.4932(8) 0.8922(7) 0.1627(3) 0.127(3) Uani 1 1 d . . . H133 H 0.4965 0.8895 0.2053 0.152 Uiso 1 1 calc R . . C105 C 0.5261(3) 0.1705(4) 0.30089(18) 0.0494(12) Uani 1 1 d . . . H10S H 0.5996 0.1458 0.2914 0.059 Uiso 1 1 calc R . . H10T H 0.5182 0.1925 0.3424 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0177(4) 0.0165(4) 0.0191(4) -0.0020(3) -0.0022(3) -0.0043(3) O1 0.0217(12) 0.0176(10) 0.0220(11) -0.0023(8) -0.0032(9) -0.0055(9) Si2 0.0182(4) 0.0151(4) 0.0198(4) -0.0007(3) -0.0018(3) -0.0038(3) O4 0.0198(12) 0.0163(10) 0.0255(11) -0.0018(8) -0.0003(9) -0.0036(9) Si3 0.0165(4) 0.0174(4) 0.0197(4) -0.0010(3) -0.0021(3) -0.0035(3) O5 0.0189(12) 0.0207(11) 0.0207(11) -0.0024(8) -0.0033(9) -0.0037(9) O6 0.0182(11) 0.0212(11) 0.0207(11) 0.0000(8) -0.0005(9) -0.0035(9) Si4 0.0166(4) 0.0183(4) 0.0187(4) 0.0001(3) -0.0015(3) -0.0044(3) O3 0.0242(12) 0.0163(10) 0.0220(11) 0.0018(8) -0.0013(9) -0.0047(9) O2 0.0200(12) 0.0219(11) 0.0196(11) -0.0007(8) -0.0020(9) -0.0065(9) C41 0.0178(16) 0.0288(17) 0.0214(16) -0.0011(13) -0.0022(12) -0.0047(13) C42 0.0232(18) 0.0307(18) 0.0245(17) 0.0009(13) 0.0015(13) -0.0062(14) C43 0.0192(17) 0.0369(19) 0.0295(18) 0.0089(15) -0.0033(14) -0.0066(14) C44 0.028(2) 0.033(2) 0.047(2) 0.0090(17) 0.0046(17) -0.0045(16) C45 0.037(2) 0.044(2) 0.063(3) 0.026(2) -0.007(2) -0.0093(19) C46 0.033(2) 0.070(3) 0.038(2) 0.029(2) -0.0084(18) -0.019(2) C47 0.035(2) 0.077(3) 0.029(2) 0.009(2) -0.0084(17) -0.026(2) C48 0.030(2) 0.052(2) 0.0291(19) 0.0032(17) -0.0039(15) -0.0189(18) C31 0.0224(17) 0.0213(15) 0.0232(16) -0.0018(12) 0.0012(13) -0.0028(13) C32 0.0214(17) 0.0229(16) 0.0266(17) -0.0001(13) 0.0002(13) -0.0033(13) C33 0.0205(17) 0.0213(16) 0.0382(19) 0.0069(14) -0.0058(14) -0.0057(13) C38 0.0217(18) 0.0350(19) 0.038(2) 0.0040(16) -0.0020(15) -0.0054(15) C37 0.024(2) 0.044(2) 0.048(2) 0.0076(18) 0.0068(17) 0.0004(17) C36 0.0184(19) 0.033(2) 0.069(3) 0.0126(19) -0.0053(18) -0.0048(15) C35 0.029(2) 0.033(2) 0.067(3) 0.0069(19) -0.022(2) -0.0121(16) C34 0.0224(19) 0.0267(18) 0.048(2) -0.0004(16) -0.0084(16) -0.0068(14) C21 0.0194(16) 0.0156(14) 0.0258(16) -0.0024(12) -0.0026(12) -0.0041(12) C22 0.0219(17) 0.0188(15) 0.0286(17) -0.0039(12) -0.0025(13) -0.0057(12) C23 0.0202(17) 0.0194(15) 0.0263(16) 0.0003(12) -0.0028(13) -0.0052(12) C24 0.0211(17) 0.0236(16) 0.0310(18) 0.0000(13) -0.0048(14) -0.0049(13) C25 0.0266(19) 0.0199(16) 0.038(2) -0.0039(14) -0.0029(15) -0.0043(13) C26 0.031(2) 0.0190(16) 0.046(2) 0.0040(15) -0.0026(16) -0.0047(14) C27 0.031(2) 0.0318(19) 0.0319(19) 0.0088(15) -0.0063(15) -0.0082(15) C28 0.0243(18) 0.0265(17) 0.0295(18) -0.0015(14) -0.0038(14) -0.0083(14) C11 0.0217(17) 0.0223(16) 0.0244(16) -0.0029(12) -0.0036(13) -0.0058(13) C12 0.0261(19) 0.0346(19) 0.0297(18) -0.0052(15) -0.0026(14) -0.0139(15) C13 0.034(2) 0.0301(18) 0.0271(18) -0.0072(14) -0.0097(15) -0.0083(15) C18 0.036(2) 0.047(2) 0.033(2) -0.0078(17) -0.0074(16) -0.0172(18) C17 0.048(3) 0.055(3) 0.048(3) -0.007(2) -0.012(2) -0.024(2) C16 0.060(3) 0.051(3) 0.048(3) -0.023(2) -0.021(2) -0.015(2) C15 0.062(3) 0.086(4) 0.040(3) -0.030(2) -0.002(2) -0.022(3) C14 0.046(3) 0.075(3) 0.031(2) -0.020(2) -0.0006(18) -0.020(2) Si5 0.0204(5) 0.0195(4) 0.0166(4) -0.0006(3) -0.0017(3) -0.0071(3) O8 0.0206(12) 0.0198(11) 0.0243(11) 0.0001(9) -0.0014(9) -0.0058(9) Si6 0.0223(5) 0.0169(4) 0.0180(4) 0.0003(3) -0.0024(3) -0.0074(3) O10 0.0276(13) 0.0207(11) 0.0206(11) 0.0001(9) -0.0044(9) -0.0087(9) Si7 0.0218(5) 0.0195(4) 0.0156(4) -0.0011(3) -0.0019(3) -0.0077(3) O11 0.0204(12) 0.0235(11) 0.0187(11) -0.0020(9) -0.0027(9) -0.0072(9) O12 0.0245(12) 0.0220(11) 0.0160(10) -0.0005(8) -0.0012(9) -0.0102(9) Si8 0.0227(5) 0.0201(4) 0.0145(4) 0.0008(3) -0.0014(3) -0.0081(3) O9 0.0273(13) 0.0212(11) 0.0187(11) 0.0012(8) -0.0010(9) -0.0092(9) O7 0.0203(12) 0.0243(11) 0.0176(11) 0.0005(8) -0.0002(9) -0.0077(9) C81 0.0275(18) 0.0257(16) 0.0155(15) -0.0021(12) 0.0000(12) -0.0082(13) C82 0.0293(19) 0.0261(17) 0.0222(16) 0.0006(13) 0.0014(13) -0.0088(14) C83 0.0275(18) 0.0317(18) 0.0223(16) 0.0041(13) -0.0036(13) -0.0153(14) C84 0.0258(19) 0.0309(18) 0.0311(18) 0.0022(14) -0.0060(14) -0.0105(14) C85 0.034(2) 0.036(2) 0.034(2) 0.0139(16) -0.0133(16) -0.0146(16) C86 0.033(2) 0.052(2) 0.0244(18) 0.0123(16) -0.0071(15) -0.0234(18) C87 0.036(2) 0.044(2) 0.0230(17) -0.0013(15) -0.0006(15) -0.0165(17) C88 0.031(2) 0.0304(18) 0.0280(18) -0.0012(14) 0.0013(14) -0.0121(15) C71 0.0234(17) 0.0221(15) 0.0218(16) -0.0001(12) -0.0044(13) -0.0076(13) C72 0.0262(18) 0.0232(16) 0.0217(16) -0.0027(12) -0.0041(13) -0.0060(13) C73 0.0295(19) 0.0273(17) 0.0219(16) -0.0052(13) -0.0048(14) -0.0039(14) C78 0.039(2) 0.042(2) 0.0273(18) -0.0101(16) -0.0018(16) -0.0193(17) C77 0.062(3) 0.055(3) 0.041(2) -0.009(2) -0.011(2) -0.036(2) C76 0.062(3) 0.050(3) 0.041(2) -0.021(2) -0.016(2) -0.012(2) C75 0.041(2) 0.060(3) 0.031(2) -0.0246(19) -0.0031(17) -0.003(2) C74 0.032(2) 0.054(2) 0.0291(19) -0.0144(17) -0.0011(16) -0.0126(18) C61 0.0241(17) 0.0195(15) 0.0240(16) -0.0024(12) -0.0033(13) -0.0074(13) C62 0.0273(18) 0.0198(15) 0.0222(16) -0.0021(12) -0.0040(13) -0.0051(13) C63 0.0205(17) 0.0194(15) 0.0301(17) 0.0008(13) -0.0051(13) -0.0032(12) C64 0.0260(19) 0.0241(17) 0.036(2) -0.0038(14) -0.0062(15) -0.0040(14) C65 0.029(2) 0.0233(18) 0.054(2) -0.0066(16) -0.0081(17) -0.0010(15) C66 0.045(3) 0.0194(18) 0.063(3) 0.0078(17) -0.013(2) -0.0070(16) C67 0.044(2) 0.033(2) 0.044(2) 0.0158(17) -0.0077(18) -0.0120(18) C68 0.0274(19) 0.0242(17) 0.0325(19) 0.0046(14) -0.0035(15) -0.0069(14) C51 0.0260(18) 0.0226(16) 0.0206(16) -0.0017(12) -0.0008(13) -0.0072(13) C52 0.0246(18) 0.0243(16) 0.0267(17) -0.0040(13) -0.0003(13) -0.0054(13) C53 0.0243(18) 0.0308(18) 0.0238(17) 0.0003(13) -0.0018(13) -0.0046(14) C58 0.0292(19) 0.0268(17) 0.0312(18) -0.0046(14) -0.0016(15) -0.0067(14) C57 0.0263(19) 0.0353(19) 0.037(2) -0.0016(15) -0.0025(15) -0.0147(15) C56 0.0217(19) 0.045(2) 0.049(2) -0.0104(18) -0.0005(17) -0.0053(16) C55 0.029(2) 0.050(3) 0.061(3) -0.026(2) -0.0015(19) -0.0016(18) C54 0.030(2) 0.043(2) 0.052(3) -0.0205(19) -0.0077(18) -0.0040(17) F2 0.0282(15) 0.0239(13) 0.0207(13) 0.0019(10) -0.0014(11) -0.0099(11) F1 0.0219(14) 0.0214(13) 0.0254(14) -0.0002(10) -0.0024(11) -0.0052(10) N1 0.0261(18) 0.076(3) 0.0299(17) -0.0127(16) 0.0010(13) -0.0190(17) C101 0.024(2) 0.084(3) 0.040(2) -0.021(2) 0.0002(17) -0.022(2) C102 0.040(3) 0.115(5) 0.043(3) -0.033(3) 0.011(2) -0.030(3) C103 0.029(3) 0.284(10) 0.124(6) -0.168(7) 0.044(3) -0.063(4) C109 0.037(2) 0.063(3) 0.0261(19) -0.0091(18) -0.0031(16) -0.016(2) C110 0.040(3) 0.079(3) 0.034(2) -0.010(2) 0.0010(19) -0.009(2) C111 0.053(3) 0.051(3) 0.034(2) -0.0026(18) 0.0026(19) -0.012(2) C112 0.072(4) 0.066(3) 0.047(3) -0.009(2) 0.011(3) 0.001(3) C113 0.025(2) 0.078(3) 0.036(2) -0.017(2) 0.0000(17) -0.020(2) C114 0.041(3) 0.080(4) 0.051(3) -0.018(2) -0.003(2) -0.028(2) C115 0.045(3) 0.060(3) 0.076(3) -0.031(3) 0.001(2) -0.019(2) C116 0.072(4) 0.069(4) 0.094(4) -0.036(3) -0.004(3) -0.031(3) C106 0.054(3) 0.078(3) 0.035(2) -0.004(2) -0.007(2) -0.025(3) C107 0.068(4) 0.088(4) 0.038(3) -0.009(3) 0.013(2) -0.013(3) C108 0.109(5) 0.076(4) 0.053(3) -0.011(3) 0.017(3) -0.027(4) C121 0.090(5) 0.082(4) 0.045(3) -0.018(3) 0.002(3) -0.014(4) C126 0.060(4) 0.108(5) 0.050(3) -0.019(3) 0.000(3) -0.021(3) C125 0.130(7) 0.085(5) 0.066(4) -0.023(4) -0.016(4) -0.043(5) C124 0.134(8) 0.093(6) 0.139(8) -0.051(5) -0.070(7) 0.006(6) C122 0.056(4) 0.152(8) 0.133(7) -0.095(6) -0.014(4) -0.016(5) C104 0.073(5) 0.189(9) 0.112(6) -0.039(6) 0.009(4) -0.044(5) C123 0.077(6) 0.139(9) 0.219(12) -0.087(8) -0.071(7) 0.024(6) C131 0.083(4) 0.025(2) 0.051(3) -0.0017(19) 0.015(3) -0.001(2) C134 0.086(6) 0.052(4) 0.201(11) -0.011(5) 0.073(7) 0.010(4) C135 0.086(6) 0.071(5) 0.268(14) 0.072(7) -0.077(8) -0.052(5) C132 0.068(4) 0.129(6) 0.061(4) 0.033(4) -0.018(3) -0.016(4) C136 0.190(9) 0.080(5) 0.082(5) 0.020(4) -0.066(6) -0.084(6) C137 0.170(8) 0.051(4) 0.157(7) -0.005(4) 0.113(7) -0.005(4) C127 0.223(12) 0.102(7) 0.142(9) -0.028(6) 0.077(8) -0.022(7) C133 0.141(8) 0.186(10) 0.051(4) -0.010(5) 0.035(5) -0.045(7) C105 0.039(2) 0.090(4) 0.024(2) -0.005(2) -0.0042(17) -0.022(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O5 1.621(2) . ? Si1 O2 1.626(2) . ? Si1 O1 1.627(2) . ? Si1 C11 1.850(3) . ? O1 Si2 1.622(2) . ? Si2 O3 1.618(2) . ? Si2 O4 1.619(2) . ? Si2 C21 1.848(3) . ? O4 Si3 1.623(2) 2_565 ? Si3 O5 1.622(2) . ? Si3 O4 1.623(2) 2_565 ? Si3 O6 1.625(2) . ? Si3 C31 1.843(3) . ? O6 Si4 1.623(2) 2_565 ? Si4 O3 1.619(2) 2_565 ? Si4 O6 1.623(2) 2_565 ? Si4 O2 1.628(2) . ? Si4 C41 1.850(3) . ? O3 Si4 1.619(2) 2_565 ? C41 C42 1.337(5) . ? C41 H41 0.9500 . ? C42 C43 1.473(5) . ? C42 H42 0.9500 . ? C43 C48 1.388(5) . ? C43 C44 1.395(5) . ? C44 C45 1.393(5) . ? C44 H44 0.9500 . ? C45 C46 1.373(7) . ? C45 H45 0.9500 . ? C46 C47 1.373(7) . ? C46 H46 0.9500 . ? C47 C48 1.395(5) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C31 C32 1.330(5) . ? C31 H31 0.9500 . ? C32 C33 1.472(5) . ? C32 H32 0.9500 . ? C33 C38 1.386(5) . ? C33 C34 1.397(5) . ? C38 C37 1.391(5) . ? C38 H38 0.9500 . ? C37 C36 1.377(6) . ? C37 H37 0.9500 . ? C36 C35 1.376(6) . ? C36 H36 0.9500 . ? C35 C34 1.392(5) . ? C35 H35 0.9500 . ? C34 H34 0.9500 . ? C21 C22 1.339(4) . ? C21 H21 0.9500 . ? C22 C23 1.471(4) . ? C22 H22 0.9500 . ? C23 C28 1.395(5) . ? C23 C24 1.397(4) . ? C24 C25 1.385(5) . ? C24 H24 0.9500 . ? C25 C26 1.386(5) . ? C25 H25 0.9500 . ? C26 C27 1.383(5) . ? C26 H26 0.9500 . ? C27 C28 1.391(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C11 C12 1.328(5) . ? C11 H11 0.9500 . ? C12 C13 1.485(5) . ? C12 H12 0.9500 . ? C13 C14 1.389(5) . ? C13 C18 1.390(5) . ? C18 C17 1.393(5) . ? C18 H18 0.9500 . ? C17 C16 1.379(6) . ? C17 H17 0.9500 . ? C16 C15 1.363(7) . ? C16 H16 0.9500 . ? C15 C14 1.386(6) . ? C15 H15 0.9500 . ? C14 H14 0.9500 . ? Si5 O8 1.619(2) . ? Si5 O7 1.622(2) . ? Si5 O11 1.623(2) . ? Si5 C51 1.848(3) . ? O8 Si6 1.622(2) . ? Si6 O9 1.620(2) . ? Si6 O10 1.621(2) . ? Si6 C61 1.842(3) . ? O10 Si7 1.623(2) 2_556 ? Si7 O11 1.623(2) . ? Si7 O10 1.623(2) 2_556 ? Si7 O12 1.624(2) . ? Si7 C71 1.845(3) . ? O12 Si8 1.627(2) 2_556 ? Si8 O9 1.620(2) 2_556 ? Si8 O7 1.625(2) . ? Si8 O12 1.627(2) 2_556 ? Si8 C81 1.847(3) . ? O9 Si8 1.620(2) 2_556 ? C81 C82 1.327(4) . ? C81 H81 0.9500 . ? C82 C83 1.478(4) . ? C82 H82 0.9500 . ? C83 C84 1.387(5) . ? C83 C88 1.393(5) . ? C84 C85 1.385(5) . ? C84 H84 0.9500 . ? C85 C86 1.378(6) . ? C85 H85 0.9500 . ? C86 C87 1.386(5) . ? C86 H86 0.9500 . ? C87 C88 1.389(5) . ? C87 H87 0.9500 . ? C88 H88 0.9500 . ? C71 C72 1.336(4) . ? C71 H71 0.9500 . ? C72 C73 1.471(4) . ? C72 H72 0.9500 . ? C73 C74 1.387(5) . ? C73 C78 1.388(5) . ? C78 C77 1.389(5) . ? C78 H78 0.9500 . ? C77 C76 1.386(6) . ? C77 H77 0.9500 . ? C76 C75 1.360(6) . ? C76 H76 0.9500 . ? C75 C74 1.392(5) . ? C75 H75 0.9500 . ? C74 H74 0.9500 . ? C61 C62 1.325(4) . ? C61 H61 0.9500 . ? C62 C63 1.477(4) . ? C62 H62 0.9500 . ? C63 C68 1.389(5) . ? C63 C64 1.397(5) . ? C64 C65 1.382(5) . ? C64 H64 0.9500 . ? C65 C66 1.372(6) . ? C65 H65 0.9500 . ? C66 C67 1.389(6) . ? C66 H66 0.9500 . ? C67 C68 1.388(5) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C51 C52 1.337(5) . ? C51 H51 0.9500 . ? C52 C53 1.475(5) . ? C52 H52 0.9500 . ? C53 C58 1.386(5) . ? C53 C54 1.396(5) . ? C58 C57 1.387(5) . ? C58 H58 0.9500 . ? C57 C56 1.382(5) . ? C57 H57 0.9500 . ? C56 C55 1.380(6) . ? C56 H56 0.9500 . ? C55 C54 1.376(6) . ? C55 H55 0.9500 . ? C54 H54 0.9500 . ? N1 C113 1.512(5) . ? N1 C101 1.522(5) . ? N1 C109 1.525(5) . ? N1 C105 1.525(6) . ? C101 C102 1.517(6) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 C103 1.600(8) . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.517(8) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C109 C110 1.515(6) . ? C109 H10G 0.9900 . ? C109 H10H 0.9900 . ? C110 C111 1.522(6) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.521(6) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? C113 C114 1.516(7) . ? C113 H11H 0.9900 . ? C113 H11I 0.9900 . ? C114 C115 1.506(6) . ? C114 H11J 0.9900 . ? C114 H11K 0.9900 . ? C115 C116 1.519(8) . ? C115 H11L 0.9900 . ? C115 H11M 0.9900 . ? C116 H11N 0.9800 . ? C116 H11O 0.9800 . ? C116 H11P 0.9800 . ? C106 C105 1.513(6) . ? C106 C107 1.537(7) . ? C106 H10I 0.9900 . ? C106 H10J 0.9900 . ? C107 C108 1.520(8) . ? C107 H10K 0.9900 . ? C107 H10L 0.9900 . ? C108 H10M 0.9800 . ? C108 H10N 0.9800 . ? C108 H10O 0.9800 . ? C121 C122 1.363(9) . ? C121 C126 1.371(9) . ? C121 C127 1.415(10) . ? C126 C125 1.363(9) . ? C126 H126 0.9500 . ? C125 C124 1.331(11) . ? C125 H125 0.9500 . ? C124 C123 1.393(14) . ? C124 H124 0.9500 . ? C122 C123 1.393(14) . ? C122 H122 0.9500 . ? C104 H10P 0.9800 . ? C104 H10Q 0.9800 . ? C104 H10R 0.9800 . ? C123 H123 0.9500 . ? C131 C132 1.340(7) . ? C131 C136 1.350(10) . ? C131 C137 1.511(8) . ? C134 C135 1.263(13) . ? C134 C133 1.355(13) . ? C134 H134 0.9500 . ? C135 C136 1.377(13) . ? C135 H135 0.9500 . ? C132 C133 1.356(10) . ? C132 H132 0.9500 . ? C136 H136 0.9500 . ? C137 H13A 0.9800 . ? C137 H13B 0.9800 . ? C137 H13C 0.9800 . ? C127 H12A 0.9800 . ? C127 H12B 0.9800 . ? C127 H12C 0.9800 . ? C133 H133 0.9500 . ? C105 H10S 0.9900 . ? C105 H10T 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Si1 O2 112.72(12) . . ? O5 Si1 O1 112.73(12) . . ? O2 Si1 O1 112.80(12) . . ? O5 Si1 C11 105.47(13) . . ? O2 Si1 C11 108.34(13) . . ? O1 Si1 C11 104.01(13) . . ? Si2 O1 Si1 141.01(14) . . ? O3 Si2 O4 113.03(12) . . ? O3 Si2 O1 113.03(12) . . ? O4 Si2 O1 111.58(12) . . ? O3 Si2 C21 105.71(13) . . ? O4 Si2 C21 106.50(13) . . ? O1 Si2 C21 106.35(13) . . ? Si2 O4 Si3 139.75(14) . 2_565 ? O5 Si3 O4 113.32(12) . 2_565 ? O5 Si3 O6 114.21(12) . . ? O4 Si3 O6 111.23(12) 2_565 . ? O5 Si3 C31 105.00(13) . . ? O4 Si3 C31 106.36(13) 2_565 . ? O6 Si3 C31 105.91(13) . . ? Si1 O5 Si3 143.47(15) . . ? Si4 O6 Si3 140.50(15) 2_565 . ? O3 Si4 O6 113.08(12) 2_565 2_565 ? O3 Si4 O2 112.91(12) 2_565 . ? O6 Si4 O2 112.19(12) 2_565 . ? O3 Si4 C41 102.77(13) 2_565 . ? O6 Si4 C41 106.70(13) 2_565 . ? O2 Si4 C41 108.44(13) . . ? Si2 O3 Si4 144.48(14) . 2_565 ? Si1 O2 Si4 138.72(14) . . ? C42 C41 Si4 119.4(3) . . ? C42 C41 H41 120.3 . . ? Si4 C41 H41 120.3 . . ? C41 C42 C43 130.6(3) . . ? C41 C42 H42 114.7 . . ? C43 C42 H42 114.7 . . ? C48 C43 C44 118.3(3) . . ? C48 C43 C42 123.8(3) . . ? C44 C43 C42 117.9(3) . . ? C45 C44 C43 121.2(4) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C46 C45 C44 119.3(4) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C47 C46 C45 120.6(4) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C46 C47 C48 120.2(4) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C43 C48 C47 120.4(4) . . ? C43 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C32 C31 Si3 122.3(3) . . ? C32 C31 H31 118.8 . . ? Si3 C31 H31 118.8 . . ? C31 C32 C33 127.7(3) . . ? C31 C32 H32 116.2 . . ? C33 C32 H32 116.2 . . ? C38 C33 C34 118.0(3) . . ? C38 C33 C32 123.4(3) . . ? C34 C33 C32 118.7(3) . . ? C33 C38 C37 120.9(4) . . ? C33 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C36 C37 C38 120.2(4) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C35 C36 C37 120.3(4) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C35 C34 119.4(4) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C34 C33 121.3(4) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C22 C21 Si2 123.6(2) . . ? C22 C21 H21 118.2 . . ? Si2 C21 H21 118.2 . . ? C21 C22 C23 127.7(3) . . ? C21 C22 H22 116.2 . . ? C23 C22 H22 116.2 . . ? C28 C23 C24 117.8(3) . . ? C28 C23 C22 119.7(3) . . ? C24 C23 C22 122.6(3) . . ? C25 C24 C23 121.1(3) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 120.3(3) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 119.7(3) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 119.9(3) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C23 121.3(3) . . ? C27 C28 H28 119.4 . . ? C23 C28 H28 119.4 . . ? C12 C11 Si1 127.0(3) . . ? C12 C11 H11 116.5 . . ? Si1 C11 H11 116.5 . . ? C11 C12 C13 127.0(3) . . ? C11 C12 H12 116.5 . . ? C13 C12 H12 116.5 . . ? C14 C13 C18 118.0(3) . . ? C14 C13 C12 119.1(4) . . ? C18 C13 C12 122.8(3) . . ? C13 C18 C17 120.3(4) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C16 C17 C18 120.6(4) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C15 C16 C17 119.4(4) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C15 C14 120.6(4) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C14 C13 121.0(4) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? O8 Si5 O7 112.28(12) . . ? O8 Si5 O11 113.08(12) . . ? O7 Si5 O11 113.31(12) . . ? O8 Si5 C51 105.34(13) . . ? O7 Si5 C51 106.48(13) . . ? O11 Si5 C51 105.56(13) . . ? Si5 O8 Si6 140.82(15) . . ? O9 Si6 O10 113.11(12) . . ? O9 Si6 O8 113.46(12) . . ? O10 Si6 O8 112.08(12) . . ? O9 Si6 C61 106.27(13) . . ? O10 Si6 C61 106.03(13) . . ? O8 Si6 C61 105.08(13) . . ? Si6 O10 Si7 141.19(15) . 2_556 ? O11 Si7 O10 111.93(12) . 2_556 ? O11 Si7 O12 113.81(12) . . ? O10 Si7 O12 112.73(12) 2_556 . ? O11 Si7 C71 106.81(14) . . ? O10 Si7 C71 104.23(13) 2_556 . ? O12 Si7 C71 106.52(13) . . ? Si7 O11 Si5 141.80(15) . . ? Si7 O12 Si8 140.66(14) . 2_556 ? O9 Si8 O7 112.92(12) 2_556 . ? O9 Si8 O12 112.95(12) 2_556 2_556 ? O7 Si8 O12 111.54(12) . 2_556 ? O9 Si8 C81 105.26(13) 2_556 . ? O7 Si8 C81 104.68(14) . . ? O12 Si8 C81 108.88(13) 2_556 . ? Si6 O9 Si8 142.08(15) . 2_556 ? Si5 O7 Si8 141.26(15) . . ? C82 C81 Si8 123.2(3) . . ? C82 C81 H81 118.4 . . ? Si8 C81 H81 118.4 . . ? C81 C82 C83 129.3(3) . . ? C81 C82 H82 115.3 . . ? C83 C82 H82 115.3 . . ? C84 C83 C88 118.1(3) . . ? C84 C83 C82 119.7(3) . . ? C88 C83 C82 122.2(3) . . ? C85 C84 C83 121.4(3) . . ? C85 C84 H84 119.3 . . ? C83 C84 H84 119.3 . . ? C86 C85 C84 119.8(3) . . ? C86 C85 H85 120.1 . . ? C84 C85 H85 120.1 . . ? C85 C86 C87 119.9(3) . . ? C85 C86 H86 120.1 . . ? C87 C86 H86 120.1 . . ? C86 C87 C88 119.9(4) . . ? C86 C87 H87 120.0 . . ? C88 C87 H87 120.0 . . ? C87 C88 C83 120.8(3) . . ? C87 C88 H88 119.6 . . ? C83 C88 H88 119.6 . . ? C72 C71 Si7 125.4(3) . . ? C72 C71 H71 117.3 . . ? Si7 C71 H71 117.3 . . ? C71 C72 C73 127.7(3) . . ? C71 C72 H72 116.2 . . ? C73 C72 H72 116.2 . . ? C74 C73 C78 117.4(3) . . ? C74 C73 C72 119.4(3) . . ? C78 C73 C72 123.0(3) . . ? C73 C78 C77 121.1(4) . . ? C73 C78 H78 119.4 . . ? C77 C78 H78 119.4 . . ? C76 C77 C78 119.8(4) . . ? C76 C77 H77 120.1 . . ? C78 C77 H77 120.1 . . ? C75 C76 C77 120.2(4) . . ? C75 C76 H76 119.9 . . ? C77 C76 H76 119.9 . . ? C76 C75 C74 119.6(4) . . ? C76 C75 H75 120.2 . . ? C74 C75 H75 120.2 . . ? C73 C74 C75 121.8(4) . . ? C73 C74 H74 119.1 . . ? C75 C74 H74 119.1 . . ? C62 C61 Si6 124.9(3) . . ? C62 C61 H61 117.5 . . ? Si6 C61 H61 117.5 . . ? C61 C62 C63 127.5(3) . . ? C61 C62 H62 116.3 . . ? C63 C62 H62 116.3 . . ? C68 C63 C64 117.8(3) . . ? C68 C63 C62 120.2(3) . . ? C64 C63 C62 122.1(3) . . ? C65 C64 C63 120.8(4) . . ? C65 C64 H64 119.6 . . ? C63 C64 H64 119.6 . . ? C66 C65 C64 120.6(4) . . ? C66 C65 H65 119.7 . . ? C64 C65 H65 119.7 . . ? C65 C66 C67 119.9(3) . . ? C65 C66 H66 120.0 . . ? C67 C66 H66 120.0 . . ? C68 C67 C66 119.2(4) . . ? C68 C67 H67 120.4 . . ? C66 C67 H67 120.4 . . ? C67 C68 C63 121.6(3) . . ? C67 C68 H68 119.2 . . ? C63 C68 H68 119.2 . . ? C52 C51 Si5 123.8(3) . . ? C52 C51 H51 118.1 . . ? Si5 C51 H51 118.1 . . ? C51 C52 C53 128.1(3) . . ? C51 C52 H52 115.9 . . ? C53 C52 H52 115.9 . . ? C58 C53 C54 117.5(3) . . ? C58 C53 C52 119.0(3) . . ? C54 C53 C52 123.5(3) . . ? C53 C58 C57 122.1(3) . . ? C53 C58 H58 119.0 . . ? C57 C58 H58 119.0 . . ? C56 C57 C58 119.4(3) . . ? C56 C57 H57 120.3 . . ? C58 C57 H57 120.3 . . ? C55 C56 C57 119.2(4) . . ? C55 C56 H56 120.4 . . ? C57 C56 H56 120.4 . . ? C54 C55 C56 121.2(4) . . ? C54 C55 H55 119.4 . . ? C56 C55 H55 119.4 . . ? C55 C54 C53 120.6(4) . . ? C55 C54 H54 119.7 . . ? C53 C54 H54 119.7 . . ? C113 N1 C101 111.2(3) . . ? C113 N1 C109 109.9(3) . . ? C101 N1 C109 107.2(3) . . ? C113 N1 C105 108.3(3) . . ? C101 N1 C105 110.0(3) . . ? C109 N1 C105 110.3(3) . . ? C102 C101 N1 114.9(3) . . ? C102 C101 H10A 108.5 . . ? N1 C101 H10A 108.5 . . ? C102 C101 H10B 108.5 . . ? N1 C101 H10B 108.5 . . ? H10A C101 H10B 107.5 . . ? C101 C102 C103 109.0(4) . . ? C101 C102 H10C 109.9 . . ? C103 C102 H10C 109.9 . . ? C101 C102 H10D 109.9 . . ? C103 C102 H10D 109.9 . . ? H10C C102 H10D 108.3 . . ? C104 C103 C102 112.6(5) . . ? C104 C103 H10E 109.1 . . ? C102 C103 H10E 109.1 . . ? C104 C103 H10F 109.1 . . ? C102 C103 H10F 109.1 . . ? H10E C103 H10F 107.8 . . ? C110 C109 N1 115.1(3) . . ? C110 C109 H10G 108.5 . . ? N1 C109 H10G 108.5 . . ? C110 C109 H10H 108.5 . . ? N1 C109 H10H 108.5 . . ? H10G C109 H10H 107.5 . . ? C109 C110 C111 110.8(4) . . ? C109 C110 H11A 109.5 . . ? C111 C110 H11A 109.5 . . ? C109 C110 H11B 109.5 . . ? C111 C110 H11B 109.5 . . ? H11A C110 H11B 108.1 . . ? C112 C111 C110 110.7(4) . . ? C112 C111 H11C 109.5 . . ? C110 C111 H11C 109.5 . . ? C112 C111 H11D 109.5 . . ? C110 C111 H11D 109.5 . . ? H11C C111 H11D 108.1 . . ? C111 C112 H11E 109.5 . . ? C111 C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C111 C112 H11G 109.5 . . ? H11E C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? N1 C113 C114 115.1(3) . . ? N1 C113 H11H 108.5 . . ? C114 C113 H11H 108.5 . . ? N1 C113 H11I 108.5 . . ? C114 C113 H11I 108.5 . . ? H11H C113 H11I 107.5 . . ? C115 C114 C113 111.6(4) . . ? C115 C114 H11J 109.3 . . ? C113 C114 H11J 109.3 . . ? C115 C114 H11K 109.3 . . ? C113 C114 H11K 109.3 . . ? H11J C114 H11K 108.0 . . ? C114 C115 C116 113.1(4) . . ? C114 C115 H11L 109.0 . . ? C116 C115 H11L 109.0 . . ? C114 C115 H11M 109.0 . . ? C116 C115 H11M 109.0 . . ? H11L C115 H11M 107.8 . . ? C115 C116 H11N 109.5 . . ? C115 C116 H11O 109.5 . . ? H11N C116 H11O 109.5 . . ? C115 C116 H11P 109.5 . . ? H11N C116 H11P 109.5 . . ? H11O C116 H11P 109.5 . . ? C105 C106 C107 112.0(4) . . ? C105 C106 H10I 109.2 . . ? C107 C106 H10I 109.2 . . ? C105 C106 H10J 109.2 . . ? C107 C106 H10J 109.2 . . ? H10I C106 H10J 107.9 . . ? C108 C107 C106 112.7(5) . . ? C108 C107 H10K 109.0 . . ? C106 C107 H10K 109.0 . . ? C108 C107 H10L 109.0 . . ? C106 C107 H10L 109.0 . . ? H10K C107 H10L 107.8 . . ? C107 C108 H10M 109.5 . . ? C107 C108 H10N 109.5 . . ? H10M C108 H10N 109.5 . . ? C107 C108 H10O 109.5 . . ? H10M C108 H10O 109.5 . . ? H10N C108 H10O 109.5 . . ? C122 C121 C126 119.9(7) . . ? C122 C121 C127 117.1(9) . . ? C126 C121 C127 122.9(8) . . ? C125 C126 C121 121.1(7) . . ? C125 C126 H126 119.4 . . ? C121 C126 H126 119.4 . . ? C124 C125 C126 120.1(8) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C125 C124 C123 120.3(9) . . ? C125 C124 H124 119.8 . . ? C123 C124 H124 119.8 . . ? C121 C122 C123 118.8(9) . . ? C121 C122 H122 120.6 . . ? C123 C122 H122 120.6 . . ? C103 C104 H10P 109.5 . . ? C103 C104 H10Q 109.5 . . ? H10P C104 H10Q 109.5 . . ? C103 C104 H10R 109.5 . . ? H10P C104 H10R 109.5 . . ? H10Q C104 H10R 109.5 . . ? C124 C123 C122 119.6(8) . . ? C124 C123 H123 120.2 . . ? C122 C123 H123 120.2 . . ? C132 C131 C136 116.0(6) . . ? C132 C131 C137 121.2(7) . . ? C136 C131 C137 122.7(7) . . ? C135 C134 C133 118.7(8) . . ? C135 C134 H134 120.7 . . ? C133 C134 H134 120.7 . . ? C134 C135 C136 121.5(9) . . ? C134 C135 H135 119.3 . . ? C136 C135 H135 119.3 . . ? C131 C132 C133 121.1(7) . . ? C131 C132 H132 119.5 . . ? C133 C132 H132 119.5 . . ? C131 C136 C135 121.6(7) . . ? C131 C136 H136 119.2 . . ? C135 C136 H136 119.2 . . ? C131 C137 H13A 109.5 . . ? C131 C137 H13B 109.5 . . ? H13A C137 H13B 109.5 . . ? C131 C137 H13C 109.5 . . ? H13A C137 H13C 109.5 . . ? H13B C137 H13C 109.5 . . ? C121 C127 H12A 109.5 . . ? C121 C127 H12B 109.5 . . ? H12A C127 H12B 109.5 . . ? C121 C127 H12C 109.5 . . ? H12A C127 H12C 109.5 . . ? H12B C127 H12C 109.5 . . ? C134 C133 C132 121.0(8) . . ? C134 C133 H133 119.5 . . ? C132 C133 H133 119.5 . . ? C106 C105 N1 116.0(3) . . ? C106 C105 H10S 108.3 . . ? N1 C105 H10S 108.3 . . ? C106 C105 H10T 108.3 . . ? N1 C105 H10T 108.3 . . ? H10S C105 H10T 107.4 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.64 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.125 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.079 #===END data_compound17 #TrackingRef '- Cif Files.cif' _database_code_depnum_ccdc_archive 'CCDC 835365' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H68 F25 N O12 Si8' _chemical_formula_sum 'C40 H68 F25 N O12 Si8' _chemical_formula_weight 1454.67 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.5495(4) _cell_length_b 15.8583(4) _cell_length_c 16.7260(4) _cell_angle_alpha 93.1750(10) _cell_angle_beta 108.8610(10) _cell_angle_gamma 114.5910(10) _cell_volume 3238.86(14) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 14446 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9607 _exptl_absorpt_correction_T_max 0.9885 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64160 _diffrn_reflns_av_R_equivalents 0.0889 _diffrn_reflns_av_sigmaI/netI 0.0969 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14825 _reflns_number_gt 9607 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+5.9859P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14825 _refine_ls_number_parameters 782 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1203 _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.1942 _refine_ls_wR_factor_gt 0.1681 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.70171(9) 0.57695(7) 0.12075(7) 0.0191(2) Uani 1 1 d . . . Si2 Si 0.49986(9) 0.41912(7) 0.13434(7) 0.0190(2) Uani 1 1 d . . . Si3 Si 0.42916(9) 0.31473(7) -0.05109(7) 0.0188(2) Uani 1 1 d . . . Si4 Si 0.63051(9) 0.47260(8) -0.06529(7) 0.0196(2) Uani 1 1 d . . . F1 F 0.5000 0.5000 0.0000 0.0236(7) Uani 1 2 d S . . O1 O 0.6255(2) 0.49740(19) 0.16035(17) 0.0217(6) Uani 1 1 d . . . N1 N 0.0047(3) 0.2774(2) 0.2554(2) 0.0253(8) Uani 1 1 d . . . O2 O 0.4574(2) 0.33394(18) 0.05234(17) 0.0215(6) Uani 1 1 d . . . F2 F 0.5000 0.0000 -0.5000 0.0245(7) Uani 1 2 d S . . O3 O 0.5371(2) 0.36627(18) -0.07432(17) 0.0204(6) Uani 1 1 d . . . O4 O 0.7074(2) 0.52832(18) 0.03492(17) 0.0200(6) Uani 1 1 d . . . Si5 Si 0.28860(9) -0.05027(8) -0.57322(7) 0.0198(2) Uani 1 1 d . . . Si6 Si 0.46686(9) 0.14760(8) -0.46574(7) 0.0197(2) Uani 1 1 d . . . Si7 Si 0.56733(9) 0.05681(8) -0.32951(7) 0.0197(2) Uani 1 1 d . . . Si8 Si 0.38960(9) -0.14071(7) -0.43702(7) 0.0189(2) Uani 1 1 d . . . O5 O 0.6697(2) 0.66306(18) 0.10557(17) 0.0202(6) Uani 1 1 d . . . O6 O 0.4163(2) 0.46456(19) 0.12301(17) 0.0222(6) Uani 1 1 d . . . O7 O 0.3469(2) 0.06141(19) -0.52566(18) 0.0225(6) Uani 1 1 d . . . O8 O 0.5188(2) 0.12628(19) -0.37211(17) 0.0229(6) Uani 1 1 d . . . O9 O 0.4740(2) -0.05327(19) -0.35384(17) 0.0208(6) Uani 1 1 d . . . O10 O 0.2979(2) -0.11905(19) -0.50542(17) 0.0213(6) Uani 1 1 d . . . O11 O 0.5500(2) 0.18064(19) -0.51602(18) 0.0218(6) Uani 1 1 d . . . C11 C 0.8422(3) 0.6322(3) 0.2048(3) 0.0228(8) Uani 1 1 d . . . H11A H 0.8905 0.6845 0.1854 0.027 Uiso 1 1 calc R . . H11B H 0.8414 0.6604 0.2588 0.027 Uiso 1 1 calc R . . O12 O 0.6738(2) 0.06733(19) -0.34821(17) 0.0211(6) Uani 1 1 d . . . C12 C 0.8902(3) 0.5628(3) 0.2249(3) 0.0243(9) Uani 1 1 d . . . H12A H 0.8382 0.5071 0.2384 0.029 Uiso 1 1 calc R . . H12B H 0.8985 0.5398 0.1727 0.029 Uiso 1 1 calc R . . C13 C 0.9974(4) 0.6051(3) 0.2982(3) 0.0299(10) Uani 1 1 d . . . F14 F 0.9916(2) 0.6324(2) 0.37362(17) 0.0426(7) Uani 1 1 d . . . F15 F 1.0412(2) 0.54432(19) 0.31346(19) 0.0421(7) Uani 1 1 d . . . F16 F 1.0732(2) 0.68258(19) 0.2870(2) 0.0415(7) Uani 1 1 d . . . C21 C 0.4912(3) 0.3579(3) 0.2249(3) 0.0224(8) Uani 1 1 d . . . H21A H 0.5377 0.3254 0.2340 0.027 Uiso 1 1 calc R . . H21B H 0.5183 0.4051 0.2788 0.027 Uiso 1 1 calc R . . C22 C 0.3722(3) 0.2851(3) 0.2038(3) 0.0276(9) Uani 1 1 d . . . H22A H 0.3281 0.3194 0.1996 0.033 Uiso 1 1 calc R . . H22B H 0.3438 0.2432 0.1463 0.033 Uiso 1 1 calc R . . C23 C 0.3560(4) 0.2245(3) 0.2681(3) 0.0327(10) Uani 1 1 d . . . F24 F 0.2497(2) 0.1673(2) 0.2500(2) 0.0580(9) Uani 1 1 d . . . F25 F 0.3961(3) 0.2754(2) 0.34887(19) 0.0531(8) Uani 1 1 d . . . F26 F 0.4041(2) 0.16811(19) 0.2728(2) 0.0442(7) Uani 1 1 d . . . C31 C 0.3779(3) 0.1848(3) -0.0847(3) 0.0236(9) Uani 1 1 d . . . H31A H 0.4345 0.1677 -0.0501 0.028 Uiso 1 1 calc R . . H31B H 0.3123 0.1512 -0.0710 0.028 Uiso 1 1 calc R . . C32 C 0.3487(4) 0.1494(3) -0.1805(3) 0.0284(9) Uani 1 1 d . . . H32A H 0.2934 0.1676 -0.2154 0.034 Uiso 1 1 calc R . . H32B H 0.4148 0.1813 -0.1940 0.034 Uiso 1 1 calc R . . C33 C 0.3054(4) 0.0451(3) -0.2057(3) 0.0337(10) Uani 1 1 d . . . F34 F 0.2789(3) 0.0145(2) -0.2903(2) 0.0682(10) Uani 1 1 d . . . F35 F 0.3758(2) 0.01419(19) -0.1629(2) 0.0479(8) Uani 1 1 d . . . F36 F 0.2140(2) -0.00367(18) -0.1904(2) 0.0442(7) Uani 1 1 d . . . C41 C 0.7218(3) 0.4576(3) -0.1146(3) 0.0251(9) Uani 1 1 d . . . H41A H 0.6762 0.4176 -0.1738 0.030 Uiso 1 1 calc R . . H41B H 0.7709 0.5208 -0.1200 0.030 Uiso 1 1 calc R . . C42 C 0.7924(4) 0.4131(4) -0.0657(3) 0.0366(11) Uani 1 1 d . . . H42A H 0.8396 0.4530 -0.0065 0.044 Uiso 1 1 calc R . . H42B H 0.7444 0.3495 -0.0602 0.044 Uiso 1 1 calc R . . C43 C 0.8627(5) 0.4036(4) -0.1103(4) 0.0499(14) Uani 1 1 d . . . F44 F 0.9261(4) 0.3659(3) -0.0661(3) 0.0942(15) Uani 1 1 d . . . F45 F 0.8052(3) 0.3492(3) -0.1899(3) 0.0771(12) Uani 1 1 d . . . F46 F 0.9323(3) 0.4877(2) -0.1185(3) 0.0607(9) Uani 1 1 d . . . C51 C 0.1413(3) -0.0814(3) -0.6254(3) 0.0238(8) Uani 1 1 d . . . H51A H 0.0974 -0.1514 -0.6436 0.029 Uiso 1 1 calc R . . H51B H 0.1184 -0.0584 -0.5828 0.029 Uiso 1 1 calc R . . C52 C 0.1188(4) -0.0380(4) -0.7038(4) 0.0488(15) Uani 1 1 d . . . H52A H 0.1744 0.0295 -0.6880 0.059 Uiso 1 1 calc R . . H52B H 0.1280 -0.0709 -0.7505 0.059 Uiso 1 1 calc R . . C53 C 0.0085(4) -0.0429(4) -0.7383(4) 0.0406(12) Uani 1 1 d . . . F54 F -0.0080(4) 0.0039(3) -0.6801(3) 0.0969(16) Uani 1 1 d . . . F55 F -0.0089(3) -0.0049(3) -0.8077(3) 0.0876(14) Uani 1 1 d . . . F56 F -0.0725(2) -0.1295(2) -0.7620(2) 0.0574(9) Uani 1 1 d . . . C61 C 0.4457(3) 0.2521(3) -0.4397(3) 0.0235(8) Uani 1 1 d . . . H61A H 0.5177 0.3074 -0.4065 0.028 Uiso 1 1 calc R . . H61B H 0.4118 0.2680 -0.4944 0.028 Uiso 1 1 calc R . . C62 C 0.3731(4) 0.2350(3) -0.3871(3) 0.0295(10) Uani 1 1 d . . . H62A H 0.2982 0.1856 -0.4235 0.035 Uiso 1 1 calc R . . H62B H 0.4015 0.2105 -0.3366 0.035 Uiso 1 1 calc R . . C63 C 0.3678(4) 0.3220(3) -0.3557(3) 0.0355(11) Uani 1 1 d . . . F64 F 0.4660(3) 0.3923(2) -0.3041(2) 0.0672(10) Uani 1 1 d . . . F65 F 0.3034(3) 0.3044(2) -0.3101(2) 0.0541(9) Uani 1 1 d . . . F66 F 0.3276(3) 0.3582(2) -0.4198(2) 0.0494(8) Uani 1 1 d . . . C71 C 0.6154(4) 0.0994(3) -0.2110(3) 0.0258(9) Uani 1 1 d . . . H71A H 0.6715 0.1668 -0.1946 0.031 Uiso 1 1 calc R . . H71B H 0.5531 0.0968 -0.1973 0.031 Uiso 1 1 calc R . . C72 C 0.6638(4) 0.0433(3) -0.1560(3) 0.0338(10) Uani 1 1 d . . . H72A H 0.6084 -0.0244 -0.1728 0.041 Uiso 1 1 calc R . . H72B H 0.7273 0.0471 -0.1684 0.041 Uiso 1 1 calc R . . C73 C 0.6997(4) 0.0782(4) -0.0608(3) 0.0431(12) Uani 1 1 d . . . F74 F 0.7446(3) 0.0293(3) -0.0131(2) 0.0755(11) Uani 1 1 d . . . F75 F 0.7755(3) 0.1693(3) -0.0316(2) 0.0654(10) Uani 1 1 d . . . F76 F 0.6175(3) 0.0708(3) -0.0382(2) 0.0700(11) Uani 1 1 d . . . C81 C 0.3146(3) -0.2415(3) -0.3940(3) 0.0234(8) Uani 1 1 d . . . H81A H 0.3680 -0.2544 -0.3492 0.028 Uiso 1 1 calc R . . H81B H 0.2730 -0.2234 -0.3661 0.028 Uiso 1 1 calc R . . C82 C 0.2359(4) -0.3318(3) -0.4642(3) 0.0325(10) Uani 1 1 d . . . H82A H 0.1747 -0.3223 -0.5026 0.039 Uiso 1 1 calc R . . H82B H 0.2746 -0.3422 -0.4997 0.039 Uiso 1 1 calc R . . C83 C 0.1898(4) -0.4191(3) -0.4308(3) 0.0296(10) Uani 1 1 d . . . F84 F 0.1339(2) -0.4116(2) -0.3821(2) 0.0508(8) Uani 1 1 d . . . F85 F 0.1193(3) -0.49726(19) -0.49411(19) 0.0495(8) Uani 1 1 d . . . F86 F 0.2651(2) -0.44024(19) -0.3799(2) 0.0500(8) Uani 1 1 d . . . C101 C -0.0107(4) 0.2172(3) 0.3228(3) 0.0289(7) Uani 1 1 d U . . H10A H -0.0774 0.1559 0.2937 0.035 Uiso 1 1 calc R . . H10B H 0.0520 0.2030 0.3438 0.035 Uiso 1 1 calc R . . C102 C -0.0207(4) 0.2605(3) 0.4006(3) 0.0310(7) Uani 1 1 d U . . H10C H -0.0811 0.2778 0.3811 0.037 Uiso 1 1 calc R . . H10D H 0.0479 0.3191 0.4338 0.037 Uiso 1 1 calc R . . C103 C -0.0430(4) 0.1893(3) 0.4584(3) 0.0321(7) Uani 1 1 d U . . H10E H -0.0631 0.2134 0.5027 0.039 Uiso 1 1 calc R . . H10F H -0.1063 0.1283 0.4227 0.039 Uiso 1 1 calc R . . C105 C 0.1076(4) 0.3714(4) 0.2962(4) 0.0472(10) Uani 1 1 d U . . H10G H 0.0992 0.4065 0.3420 0.057 Uiso 1 1 calc R . . H10H H 0.1137 0.4093 0.2514 0.057 Uiso 1 1 calc R . . C106 C 0.2137(4) 0.3649(4) 0.3358(4) 0.0529(9) Uani 1 1 d U . . H10I H 0.2254 0.3323 0.2906 0.063 Uiso 1 1 calc R . . H10J H 0.2097 0.3276 0.3812 0.063 Uiso 1 1 calc R . . C107 C 0.3108(4) 0.4677(4) 0.3760(5) 0.0621(10) Uani 1 1 d U . . H10K H 0.3207 0.4990 0.3277 0.075 Uiso 1 1 calc R . . H10L H 0.2883 0.5034 0.4095 0.075 Uiso 1 1 calc R . . C108 C 0.4162(5) 0.4785(5) 0.4318(5) 0.0816(15) Uani 1 1 d U . . H10M H 0.4072 0.4411 0.4760 0.122 Uiso 1 1 calc R . . H10N H 0.4649 0.5457 0.4600 0.122 Uiso 1 1 calc R . . H10O H 0.4478 0.4560 0.3972 0.122 Uiso 1 1 calc R . . C109 C 0.0096(4) 0.2175(3) 0.1841(3) 0.0338(8) Uani 1 1 d U . . H10P H -0.0630 0.1615 0.1555 0.041 Uiso 1 1 calc R . . H10Q H 0.0625 0.1936 0.2117 0.041 Uiso 1 1 calc R . . C110 C 0.0415(4) 0.2659(3) 0.1143(3) 0.0366(7) Uani 1 1 d U . . H11C H -0.0136 0.2858 0.0823 0.044 Uiso 1 1 calc R . . H11D H 0.1131 0.3234 0.1414 0.044 Uiso 1 1 calc R . . C111 C 0.0484(4) 0.1973(4) 0.0523(3) 0.0385(8) Uani 1 1 d U . . H11E H -0.0243 0.1412 0.0243 0.046 Uiso 1 1 calc R . . H11F H 0.1005 0.1751 0.0856 0.046 Uiso 1 1 calc R . . C112 C 0.0850(5) 0.2416(4) -0.0174(3) 0.0477(10) Uani 1 1 d U . . H11G H 0.0343 0.2646 -0.0502 0.071 Uiso 1 1 calc R . . H11H H 0.0855 0.1938 -0.0568 0.071 Uiso 1 1 calc R . . H11I H 0.1587 0.2950 0.0098 0.071 Uiso 1 1 calc R . . C113 C -0.0894(3) 0.3028(3) 0.2199(3) 0.0281(7) Uani 1 1 d U . . H11J H -0.0811 0.3509 0.2656 0.034 Uiso 1 1 calc R . . H11K H -0.0816 0.3330 0.1707 0.034 Uiso 1 1 calc R . . C114 C -0.2049(3) 0.2214(3) 0.1895(3) 0.0284(6) Uani 1 1 d U . . H11L H -0.2152 0.1904 0.2379 0.034 Uiso 1 1 calc R . . H11M H -0.2164 0.1733 0.1421 0.034 Uiso 1 1 calc R . . C115 C -0.2880(3) 0.2592(3) 0.1575(3) 0.0301(7) Uani 1 1 d U . . H11N H -0.2705 0.3125 0.2029 0.036 Uiso 1 1 calc R . . H11O H -0.2822 0.2842 0.1055 0.036 Uiso 1 1 calc R . . C116 C -0.4044(4) 0.1834(3) 0.1354(3) 0.0329(9) Uani 1 1 d U . . H11P H -0.4226 0.1309 0.0897 0.049 Uiso 1 1 calc R . . H11Q H -0.4547 0.2107 0.1151 0.049 Uiso 1 1 calc R . . H11R H -0.4110 0.1594 0.1871 0.049 Uiso 1 1 calc R . . C104 C 0.0536(5) 0.1713(6) 0.5039(4) 0.0662(19) Uani 1 1 d . . . H10R H 0.0728 0.1457 0.4605 0.099 Uiso 1 1 calc R . . H10S H 0.0341 0.1254 0.5399 0.099 Uiso 1 1 calc R . . H10T H 0.1162 0.2311 0.5405 0.099 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0194(5) 0.0181(5) 0.0184(5) 0.0049(4) 0.0064(5) 0.0078(4) Si2 0.0203(5) 0.0187(5) 0.0178(5) 0.0054(4) 0.0075(5) 0.0085(5) Si3 0.0213(6) 0.0161(5) 0.0179(5) 0.0036(4) 0.0067(5) 0.0083(4) Si4 0.0207(5) 0.0196(5) 0.0199(6) 0.0046(4) 0.0084(5) 0.0101(5) F1 0.0247(17) 0.0222(17) 0.0215(17) 0.0042(13) 0.0071(14) 0.0100(14) O1 0.0203(14) 0.0198(14) 0.0216(14) 0.0061(11) 0.0067(12) 0.0069(12) N1 0.0260(19) 0.0184(17) 0.031(2) 0.0045(15) 0.0123(16) 0.0085(15) O2 0.0264(15) 0.0182(14) 0.0199(14) 0.0052(11) 0.0090(12) 0.0100(12) F2 0.0255(17) 0.0276(18) 0.0228(17) 0.0066(14) 0.0105(15) 0.0134(15) O3 0.0220(14) 0.0180(14) 0.0205(14) 0.0028(11) 0.0087(12) 0.0084(12) O4 0.0184(14) 0.0209(14) 0.0199(14) 0.0027(11) 0.0078(12) 0.0081(12) Si5 0.0194(5) 0.0201(6) 0.0207(6) 0.0061(4) 0.0080(5) 0.0093(5) Si6 0.0227(6) 0.0192(5) 0.0206(6) 0.0053(4) 0.0098(5) 0.0113(5) Si7 0.0216(6) 0.0199(5) 0.0176(5) 0.0034(4) 0.0075(5) 0.0095(5) Si8 0.0196(5) 0.0194(5) 0.0196(5) 0.0058(4) 0.0086(5) 0.0095(5) O5 0.0199(14) 0.0191(14) 0.0204(14) 0.0046(11) 0.0051(12) 0.0098(12) O6 0.0254(15) 0.0233(15) 0.0215(15) 0.0082(12) 0.0099(12) 0.0133(13) O7 0.0199(14) 0.0198(14) 0.0268(15) 0.0031(12) 0.0081(12) 0.0092(12) O8 0.0278(15) 0.0223(15) 0.0219(15) 0.0055(12) 0.0099(13) 0.0141(13) O9 0.0222(14) 0.0216(14) 0.0164(14) 0.0047(11) 0.0066(12) 0.0085(12) O10 0.0193(14) 0.0213(14) 0.0236(15) 0.0077(11) 0.0075(12) 0.0098(12) O11 0.0258(15) 0.0209(14) 0.0247(15) 0.0078(12) 0.0141(13) 0.0124(12) C11 0.021(2) 0.024(2) 0.023(2) 0.0051(17) 0.0060(17) 0.0112(17) O12 0.0209(14) 0.0239(14) 0.0190(14) 0.0046(11) 0.0077(12) 0.0107(12) C12 0.025(2) 0.019(2) 0.023(2) 0.0010(16) 0.0026(18) 0.0094(18) C13 0.027(2) 0.029(2) 0.032(2) 0.0040(19) 0.008(2) 0.014(2) F14 0.0409(16) 0.0561(18) 0.0243(14) -0.0012(13) -0.0002(12) 0.0273(15) F15 0.0364(15) 0.0383(16) 0.0465(17) 0.0051(13) -0.0004(13) 0.0253(13) F16 0.0223(13) 0.0320(15) 0.0606(19) 0.0055(13) 0.0110(13) 0.0081(12) C21 0.022(2) 0.023(2) 0.023(2) 0.0076(17) 0.0101(18) 0.0102(17) C22 0.022(2) 0.031(2) 0.031(2) 0.0162(19) 0.0127(19) 0.0100(19) C23 0.034(2) 0.029(2) 0.041(3) 0.019(2) 0.017(2) 0.016(2) F24 0.0379(17) 0.061(2) 0.082(2) 0.0515(19) 0.0328(17) 0.0172(16) F25 0.083(2) 0.058(2) 0.0357(17) 0.0238(15) 0.0375(17) 0.0346(18) F26 0.0503(18) 0.0320(15) 0.063(2) 0.0228(14) 0.0265(16) 0.0248(14) C31 0.025(2) 0.021(2) 0.026(2) 0.0076(17) 0.0106(18) 0.0102(18) C32 0.033(2) 0.020(2) 0.027(2) 0.0003(17) 0.007(2) 0.0110(19) C33 0.034(3) 0.025(2) 0.035(3) -0.0030(19) 0.010(2) 0.011(2) F34 0.102(3) 0.0406(18) 0.0391(18) -0.0147(14) 0.0216(19) 0.0195(19) F35 0.0389(16) 0.0271(15) 0.077(2) 0.0015(14) 0.0179(16) 0.0190(13) F36 0.0282(14) 0.0224(14) 0.065(2) -0.0026(13) 0.0119(14) 0.0027(12) C41 0.027(2) 0.029(2) 0.026(2) 0.0083(18) 0.0148(19) 0.0156(19) C42 0.036(3) 0.044(3) 0.046(3) 0.019(2) 0.022(2) 0.026(2) C43 0.053(3) 0.050(3) 0.077(4) 0.027(3) 0.041(3) 0.038(3) F44 0.098(3) 0.126(4) 0.151(4) 0.085(3) 0.086(3) 0.100(3) F45 0.085(3) 0.066(2) 0.101(3) -0.003(2) 0.066(3) 0.034(2) F46 0.0483(19) 0.060(2) 0.100(3) 0.034(2) 0.052(2) 0.0286(17) C51 0.022(2) 0.022(2) 0.027(2) 0.0073(17) 0.0079(18) 0.0097(17) C52 0.021(2) 0.063(4) 0.059(4) 0.042(3) 0.009(2) 0.017(2) C53 0.026(2) 0.036(3) 0.051(3) 0.017(2) 0.004(2) 0.014(2) F54 0.099(3) 0.107(3) 0.084(3) -0.021(2) -0.016(2) 0.090(3) F55 0.048(2) 0.107(3) 0.102(3) 0.078(3) 0.010(2) 0.036(2) F56 0.0312(16) 0.0398(18) 0.075(2) 0.0104(16) -0.0038(16) 0.0115(14) C61 0.028(2) 0.022(2) 0.023(2) 0.0052(16) 0.0106(18) 0.0133(18) C62 0.041(3) 0.031(2) 0.030(2) 0.0117(19) 0.021(2) 0.022(2) C63 0.044(3) 0.039(3) 0.034(3) 0.008(2) 0.021(2) 0.025(2) F64 0.057(2) 0.060(2) 0.066(2) -0.0316(18) 0.0154(18) 0.0218(18) F65 0.081(2) 0.067(2) 0.057(2) 0.0235(16) 0.0504(19) 0.0529(19) F66 0.072(2) 0.0500(18) 0.065(2) 0.0304(16) 0.0432(18) 0.0479(18) C71 0.029(2) 0.028(2) 0.019(2) 0.0004(17) 0.0076(18) 0.0128(19) C72 0.038(3) 0.043(3) 0.021(2) 0.010(2) 0.007(2) 0.022(2) C73 0.039(3) 0.054(3) 0.027(3) 0.010(2) 0.009(2) 0.016(3) F74 0.089(3) 0.096(3) 0.0357(19) 0.0314(19) 0.0069(19) 0.049(2) F75 0.062(2) 0.063(2) 0.0321(17) 0.0005(16) 0.0005(16) 0.0072(18) F76 0.054(2) 0.121(3) 0.0292(17) 0.0106(18) 0.0233(16) 0.030(2) C81 0.021(2) 0.025(2) 0.022(2) 0.0063(17) 0.0072(17) 0.0099(18) C82 0.034(2) 0.027(2) 0.024(2) 0.0059(18) 0.007(2) 0.006(2) C83 0.026(2) 0.024(2) 0.031(2) 0.0015(18) 0.006(2) 0.0091(19) F84 0.0519(18) 0.0330(16) 0.078(2) 0.0173(15) 0.0452(18) 0.0126(14) F85 0.0524(18) 0.0255(15) 0.0421(17) 0.0003(13) 0.0096(15) -0.0004(13) F86 0.0379(16) 0.0304(15) 0.067(2) 0.0178(14) 0.0017(15) 0.0151(13) C101 0.0304(16) 0.0296(15) 0.0309(16) 0.0074(13) 0.0136(13) 0.0158(13) C102 0.0318(15) 0.0310(15) 0.0319(15) 0.0059(12) 0.0137(13) 0.0149(13) C103 0.0321(16) 0.0325(16) 0.0317(16) 0.0057(13) 0.0138(14) 0.0138(14) C105 0.0248(16) 0.0454(19) 0.072(2) 0.0289(18) 0.0199(17) 0.0142(15) C106 0.0272(15) 0.0495(19) 0.076(2) 0.0297(17) 0.0173(16) 0.0121(14) C107 0.0324(16) 0.0546(19) 0.080(2) 0.0319(18) 0.0127(17) 0.0076(15) C108 0.048(2) 0.067(2) 0.091(3) 0.025(2) 0.009(2) 0.004(2) C109 0.0419(17) 0.0368(16) 0.0368(16) 0.0149(13) 0.0237(14) 0.0234(14) C110 0.0442(16) 0.0390(15) 0.0375(15) 0.0148(13) 0.0231(14) 0.0224(13) C111 0.0460(17) 0.0414(16) 0.0378(16) 0.0142(13) 0.0239(14) 0.0222(14) C112 0.055(2) 0.048(2) 0.042(2) 0.0136(17) 0.0246(18) 0.0213(18) C113 0.0256(14) 0.0254(14) 0.0326(15) 0.0060(12) 0.0088(13) 0.0128(12) C114 0.0256(13) 0.0258(13) 0.0322(14) 0.0055(11) 0.0085(12) 0.0124(11) C115 0.0268(13) 0.0271(14) 0.0331(14) 0.0050(12) 0.0076(12) 0.0125(12) C116 0.0267(17) 0.0301(17) 0.0352(18) 0.0017(15) 0.0050(15) 0.0128(14) C104 0.058(4) 0.115(6) 0.055(4) 0.050(4) 0.032(3) 0.055(4) _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 O5 1.624(3) . ? Si1 O1 1.632(3) . ? Si1 O4 1.634(3) . ? Si1 C11 1.854(4) . ? Si2 O1 1.616(3) . ? Si2 O6 1.621(3) . ? Si2 O2 1.625(3) . ? Si2 C21 1.853(4) . ? Si3 O2 1.622(3) . ? Si3 O5 1.622(3) 2_665 ? Si3 O3 1.626(3) . ? Si3 C31 1.855(4) . ? Si4 O6 1.624(3) 2_665 ? Si4 O4 1.625(3) . ? Si4 O3 1.627(3) . ? Si4 C41 1.858(4) . ? N1 C105 1.515(6) . ? N1 C109 1.522(5) . ? N1 C101 1.529(5) . ? N1 C113 1.533(5) . ? Si5 O7 1.627(3) . ? Si5 O12 1.627(3) 2_654 ? Si5 O10 1.629(3) . ? Si5 C51 1.860(4) . ? Si6 O11 1.619(3) . ? Si6 O8 1.626(3) . ? Si6 O7 1.628(3) . ? Si6 C61 1.861(4) . ? Si7 O8 1.621(3) . ? Si7 O12 1.621(3) . ? Si7 O9 1.628(3) . ? Si7 C71 1.854(4) . ? Si8 O9 1.622(3) . ? Si8 O10 1.627(3) . ? Si8 O11 1.627(3) 2_654 ? Si8 C81 1.857(4) . ? O5 Si3 1.622(3) 2_665 ? O6 Si4 1.624(3) 2_665 ? O11 Si8 1.627(3) 2_654 ? C11 C12 1.530(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? O12 Si5 1.627(3) 2_654 ? C12 C13 1.479(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 F16 1.339(5) . ? C13 F14 1.351(5) . ? C13 F15 1.354(5) . ? C21 C22 1.534(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.492(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 F26 1.337(5) . ? C23 F25 1.339(6) . ? C23 F24 1.344(5) . ? C31 C32 1.524(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.481(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 F35 1.337(5) . ? C33 F34 1.343(5) . ? C33 F36 1.348(5) . ? C41 C42 1.532(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.494(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 F45 1.329(7) . ? C43 F46 1.345(6) . ? C43 F44 1.349(6) . ? C51 C52 1.520(6) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.486(6) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 F56 1.313(6) . ? C53 F54 1.333(6) . ? C53 F55 1.337(6) . ? C61 C62 1.535(6) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.489(6) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 F66 1.328(5) . ? C63 F64 1.341(6) . ? C63 F65 1.344(5) . ? C71 C72 1.527(6) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.495(6) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 F76 1.331(6) . ? C73 F75 1.338(6) . ? C73 F74 1.348(6) . ? C81 C82 1.523(6) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.495(6) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 F86 1.331(5) . ? C83 F85 1.343(5) . ? C83 F84 1.356(5) . ? C101 C102 1.513(6) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 C103 1.528(6) . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.518(7) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C105 C106 1.520(7) . ? C105 H10G 0.9900 . ? C105 H10H 0.9900 . ? C106 C107 1.567(8) . ? C106 H10I 0.9900 . ? C106 H10J 0.9900 . ? C107 C108 1.446(8) . ? C107 H10K 0.9900 . ? C107 H10L 0.9900 . ? C108 H10M 0.9800 . ? C108 H10N 0.9800 . ? C108 H10O 0.9800 . ? C109 C110 1.524(6) . ? C109 H10P 0.9900 . ? C109 H10Q 0.9900 . ? C110 C111 1.517(6) . ? C110 H11C 0.9900 . ? C110 H11D 0.9900 . ? C111 C112 1.523(7) . ? C111 H11E 0.9900 . ? C111 H11F 0.9900 . ? C112 H11G 0.9800 . ? C112 H11H 0.9800 . ? C112 H11I 0.9800 . ? C113 C114 1.522(6) . ? C113 H11J 0.9900 . ? C113 H11K 0.9900 . ? C114 C115 1.526(6) . ? C114 H11L 0.9900 . ? C114 H11M 0.9900 . ? C115 C116 1.517(6) . ? C115 H11N 0.9900 . ? C115 H11O 0.9900 . ? C116 H11P 0.9800 . ? C116 H11Q 0.9800 . ? C116 H11R 0.9800 . ? C104 H10R 0.9800 . ? C104 H10S 0.9800 . ? C104 H10T 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Si1 O1 113.30(14) . . ? O5 Si1 O4 112.97(14) . . ? O1 Si1 O4 111.71(14) . . ? O5 Si1 C11 105.79(16) . . ? O1 Si1 C11 105.92(17) . . ? O4 Si1 C11 106.46(16) . . ? O1 Si2 O6 113.68(15) . . ? O1 Si2 O2 113.13(15) . . ? O6 Si2 O2 112.25(15) . . ? O1 Si2 C21 108.10(17) . . ? O6 Si2 C21 104.85(16) . . ? O2 Si2 C21 103.88(17) . . ? O2 Si3 O5 113.07(14) . 2_665 ? O2 Si3 O3 112.61(15) . . ? O5 Si3 O3 112.88(14) 2_665 . ? O2 Si3 C31 104.66(16) . . ? O5 Si3 C31 106.20(17) 2_665 . ? O3 Si3 C31 106.62(16) . . ? O6 Si4 O4 113.21(14) 2_665 . ? O6 Si4 O3 113.70(15) 2_665 . ? O4 Si4 O3 112.79(14) . . ? O6 Si4 C41 103.42(17) 2_665 . ? O4 Si4 C41 106.19(17) . . ? O3 Si4 C41 106.52(17) . . ? Si2 O1 Si1 140.11(18) . . ? C105 N1 C109 112.4(4) . . ? C105 N1 C101 110.4(4) . . ? C109 N1 C101 105.7(3) . . ? C105 N1 C113 105.8(3) . . ? C109 N1 C113 111.2(3) . . ? C101 N1 C113 111.3(3) . . ? Si3 O2 Si2 140.99(18) . . ? Si3 O3 Si4 139.57(17) . . ? Si4 O4 Si1 140.52(17) . . ? O7 Si5 O12 112.36(15) . 2_654 ? O7 Si5 O10 113.07(15) . . ? O12 Si5 O10 113.66(14) 2_654 . ? O7 Si5 C51 104.06(16) . . ? O12 Si5 C51 105.82(17) 2_654 . ? O10 Si5 C51 106.96(16) . . ? O11 Si6 O8 113.32(15) . . ? O11 Si6 O7 113.04(15) . . ? O8 Si6 O7 112.52(15) . . ? O11 Si6 C61 105.89(16) . . ? O8 Si6 C61 104.59(16) . . ? O7 Si6 C61 106.62(17) . . ? O8 Si7 O12 113.23(15) . . ? O8 Si7 O9 112.60(15) . . ? O12 Si7 O9 112.47(14) . . ? O8 Si7 C71 104.73(17) . . ? O12 Si7 C71 106.15(17) . . ? O9 Si7 C71 106.91(17) . . ? O9 Si8 O10 113.29(14) . . ? O9 Si8 O11 113.46(15) . 2_654 ? O10 Si8 O11 112.42(15) . 2_654 ? O9 Si8 C81 106.11(16) . . ? O10 Si8 C81 106.45(17) . . ? O11 Si8 C81 104.21(16) 2_654 . ? Si3 O5 Si1 142.36(18) 2_665 . ? Si2 O6 Si4 141.71(18) . 2_665 ? Si5 O7 Si6 140.66(18) . . ? Si7 O8 Si6 140.88(18) . . ? Si8 O9 Si7 140.62(18) . . ? Si8 O10 Si5 139.95(18) . . ? Si6 O11 Si8 141.38(18) . 2_654 ? C12 C11 Si1 113.8(3) . . ? C12 C11 H11A 108.8 . . ? Si1 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? Si1 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? Si7 O12 Si5 141.70(18) . 2_654 ? C13 C12 C11 113.4(3) . . ? C13 C12 H12A 108.9 . . ? C11 C12 H12A 108.9 . . ? C13 C12 H12B 108.9 . . ? C11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? F16 C13 F14 105.7(4) . . ? F16 C13 F15 105.8(3) . . ? F14 C13 F15 105.5(3) . . ? F16 C13 C12 113.6(4) . . ? F14 C13 C12 112.6(4) . . ? F15 C13 C12 113.0(4) . . ? C22 C21 Si2 109.7(3) . . ? C22 C21 H21A 109.7 . . ? Si2 C21 H21A 109.7 . . ? C22 C21 H21B 109.7 . . ? Si2 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? C23 C22 C21 114.8(4) . . ? C23 C22 H22A 108.6 . . ? C21 C22 H22A 108.6 . . ? C23 C22 H22B 108.6 . . ? C21 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? F26 C23 F25 105.7(4) . . ? F26 C23 F24 106.5(4) . . ? F25 C23 F24 105.8(4) . . ? F26 C23 C22 113.3(4) . . ? F25 C23 C22 112.8(4) . . ? F24 C23 C22 112.1(4) . . ? C32 C31 Si3 114.5(3) . . ? C32 C31 H31A 108.6 . . ? Si3 C31 H31A 108.6 . . ? C32 C31 H31B 108.6 . . ? Si3 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? C33 C32 C31 113.2(4) . . ? C33 C32 H32A 108.9 . . ? C31 C32 H32A 108.9 . . ? C33 C32 H32B 108.9 . . ? C31 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? F35 C33 F34 106.3(4) . . ? F35 C33 F36 105.4(4) . . ? F34 C33 F36 106.0(4) . . ? F35 C33 C32 113.1(4) . . ? F34 C33 C32 112.8(4) . . ? F36 C33 C32 112.6(4) . . ? C42 C41 Si4 116.1(3) . . ? C42 C41 H41A 108.3 . . ? Si4 C41 H41A 108.3 . . ? C42 C41 H41B 108.3 . . ? Si4 C41 H41B 108.3 . . ? H41A C41 H41B 107.4 . . ? C43 C42 C41 112.2(4) . . ? C43 C42 H42A 109.2 . . ? C41 C42 H42A 109.2 . . ? C43 C42 H42B 109.2 . . ? C41 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? F45 C43 F46 106.1(5) . . ? F45 C43 F44 107.2(5) . . ? F46 C43 F44 105.5(5) . . ? F45 C43 C42 112.9(5) . . ? F46 C43 C42 112.7(4) . . ? F44 C43 C42 111.9(5) . . ? C52 C51 Si5 111.8(3) . . ? C52 C51 H51A 109.3 . . ? Si5 C51 H51A 109.3 . . ? C52 C51 H51B 109.3 . . ? Si5 C51 H51B 109.3 . . ? H51A C51 H51B 107.9 . . ? C53 C52 C51 114.9(4) . . ? C53 C52 H52A 108.5 . . ? C51 C52 H52A 108.5 . . ? C53 C52 H52B 108.5 . . ? C51 C52 H52B 108.5 . . ? H52A C52 H52B 107.5 . . ? F56 C53 F54 105.3(5) . . ? F56 C53 F55 105.5(4) . . ? F54 C53 F55 105.5(4) . . ? F56 C53 C52 114.3(4) . . ? F54 C53 C52 112.0(5) . . ? F55 C53 C52 113.4(4) . . ? C62 C61 Si6 113.0(3) . . ? C62 C61 H61A 109.0 . . ? Si6 C61 H61A 109.0 . . ? C62 C61 H61B 109.0 . . ? Si6 C61 H61B 109.0 . . ? H61A C61 H61B 107.8 . . ? C63 C62 C61 113.4(4) . . ? C63 C62 H62A 108.9 . . ? C61 C62 H62A 108.9 . . ? C63 C62 H62B 108.9 . . ? C61 C62 H62B 108.9 . . ? H62A C62 H62B 107.7 . . ? F66 C63 F64 106.1(4) . . ? F66 C63 F65 106.0(4) . . ? F64 C63 F65 106.6(4) . . ? F66 C63 C62 112.9(4) . . ? F64 C63 C62 112.9(4) . . ? F65 C63 C62 111.8(4) . . ? C72 C71 Si7 114.7(3) . . ? C72 C71 H71A 108.6 . . ? Si7 C71 H71A 108.6 . . ? C72 C71 H71B 108.6 . . ? Si7 C71 H71B 108.6 . . ? H71A C71 H71B 107.6 . . ? C73 C72 C71 113.4(4) . . ? C73 C72 H72A 108.9 . . ? C71 C72 H72A 108.9 . . ? C73 C72 H72B 108.9 . . ? C71 C72 H72B 108.9 . . ? H72A C72 H72B 107.7 . . ? F76 C73 F75 106.4(4) . . ? F76 C73 F74 106.0(4) . . ? F75 C73 F74 105.3(4) . . ? F76 C73 C72 112.6(4) . . ? F75 C73 C72 113.4(4) . . ? F74 C73 C72 112.6(4) . . ? C82 C81 Si8 112.6(3) . . ? C82 C81 H81A 109.1 . . ? Si8 C81 H81A 109.1 . . ? C82 C81 H81B 109.1 . . ? Si8 C81 H81B 109.1 . . ? H81A C81 H81B 107.8 . . ? C83 C82 C81 114.4(4) . . ? C83 C82 H82A 108.7 . . ? C81 C82 H82A 108.7 . . ? C83 C82 H82B 108.7 . . ? C81 C82 H82B 108.7 . . ? H82A C82 H82B 107.6 . . ? F86 C83 F85 106.0(3) . . ? F86 C83 F84 104.8(4) . . ? F85 C83 F84 105.6(4) . . ? F86 C83 C82 113.9(4) . . ? F85 C83 C82 113.1(4) . . ? F84 C83 C82 112.7(4) . . ? C102 C101 N1 116.3(3) . . ? C102 C101 H10A 108.2 . . ? N1 C101 H10A 108.2 . . ? C102 C101 H10B 108.2 . . ? N1 C101 H10B 108.2 . . ? H10A C101 H10B 107.4 . . ? C101 C102 C103 109.8(4) . . ? C101 C102 H10C 109.7 . . ? C103 C102 H10C 109.7 . . ? C101 C102 H10D 109.7 . . ? C103 C102 H10D 109.7 . . ? H10C C102 H10D 108.2 . . ? C104 C103 C102 113.5(4) . . ? C104 C103 H10E 108.9 . . ? C102 C103 H10E 108.9 . . ? C104 C103 H10F 108.9 . . ? C102 C103 H10F 108.9 . . ? H10E C103 H10F 107.7 . . ? N1 C105 C106 115.8(4) . . ? N1 C105 H10G 108.3 . . ? C106 C105 H10G 108.3 . . ? N1 C105 H10H 108.3 . . ? C106 C105 H10H 108.3 . . ? H10G C105 H10H 107.4 . . ? C105 C106 C107 109.0(5) . . ? C105 C106 H10I 109.9 . . ? C107 C106 H10I 109.9 . . ? C105 C106 H10J 109.9 . . ? C107 C106 H10J 109.9 . . ? H10I C106 H10J 108.3 . . ? C108 C107 C106 118.5(5) . . ? C108 C107 H10K 107.7 . . ? C106 C107 H10K 107.7 . . ? C108 C107 H10L 107.7 . . ? C106 C107 H10L 107.7 . . ? H10K C107 H10L 107.1 . . ? C107 C108 H10M 109.5 . . ? C107 C108 H10N 109.5 . . ? H10M C108 H10N 109.5 . . ? C107 C108 H10O 109.5 . . ? H10M C108 H10O 109.5 . . ? H10N C108 H10O 109.5 . . ? N1 C109 C110 117.0(4) . . ? N1 C109 H10P 108.1 . . ? C110 C109 H10P 108.1 . . ? N1 C109 H10Q 108.1 . . ? C110 C109 H10Q 108.1 . . ? H10P C109 H10Q 107.3 . . ? C111 C110 C109 109.4(4) . . ? C111 C110 H11C 109.8 . . ? C109 C110 H11C 109.8 . . ? C111 C110 H11D 109.8 . . ? C109 C110 H11D 109.8 . . ? H11C C110 H11D 108.3 . . ? C110 C111 C112 112.8(4) . . ? C110 C111 H11E 109.0 . . ? C112 C111 H11E 109.0 . . ? C110 C111 H11F 109.0 . . ? C112 C111 H11F 109.0 . . ? H11E C111 H11F 107.8 . . ? C111 C112 H11G 109.5 . . ? C111 C112 H11H 109.5 . . ? H11G C112 H11H 109.5 . . ? C111 C112 H11I 109.5 . . ? H11G C112 H11I 109.5 . . ? H11H C112 H11I 109.5 . . ? C114 C113 N1 116.8(3) . . ? C114 C113 H11J 108.1 . . ? N1 C113 H11J 108.1 . . ? C114 C113 H11K 108.1 . . ? N1 C113 H11K 108.1 . . ? H11J C113 H11K 107.3 . . ? C113 C114 C115 109.9(3) . . ? C113 C114 H11L 109.7 . . ? C115 C114 H11L 109.7 . . ? C113 C114 H11M 109.7 . . ? C115 C114 H11M 109.7 . . ? H11L C114 H11M 108.2 . . ? C116 C115 C114 112.3(4) . . ? C116 C115 H11N 109.1 . . ? C114 C115 H11N 109.1 . . ? C116 C115 H11O 109.1 . . ? C114 C115 H11O 109.1 . . ? H11N C115 H11O 107.9 . . ? C115 C116 H11P 109.5 . . ? C115 C116 H11Q 109.5 . . ? H11P C116 H11Q 109.5 . . ? C115 C116 H11R 109.5 . . ? H11P C116 H11R 109.5 . . ? H11Q C116 H11R 109.5 . . ? C103 C104 H10R 109.5 . . ? C103 C104 H10S 109.5 . . ? H10R C104 H10S 109.5 . . ? C103 C104 H10T 109.5 . . ? H10R C104 H10T 109.5 . . ? H10S C104 H10T 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.096 _refine_diff_density_min -1.322 _refine_diff_density_rms 0.109 #===END