# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H78 Bi2 N4 O4 Si4' _chemical_formula_weight 1209.38 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.819(2) _cell_length_b 11.045(3) _cell_length_c 13.189(3) _cell_angle_alpha 111.32(2) _cell_angle_beta 97.198(19) _cell_angle_gamma 101.63(2) _cell_volume 1273.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1754 _cell_measurement_theta_min 2.8651 _cell_measurement_theta_max 29.0122 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 7.030 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3337 _exptl_absorpt_correction_T_max 0.7201 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.1903 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8581 _diffrn_reflns_av_R_equivalents 0.1256 _diffrn_reflns_av_unetI/netI 0.2156 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4957 _reflns_number_gt 3407 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrysAlisPro _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 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. Both the two ethyl groups of the NEt2 are disordered, treated in a splitting mode, and refined in PARTs. The constraints by SIMU combined with DELU are applied for the C1, C2, C3, C4, C12, C18, C1A, C2A, C3A, and C4A atoms. The restraint by DIFX is used for the bonds among the disordered NEt2 group. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] 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 'refined in a riding mode to the carrier atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4957 _refine_ls_number_parameters 284 _refine_ls_number_restraints 187 _refine_ls_R_factor_all 0.1278 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1335 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi -0.42211(6) 0.24544(5) -0.45425(5) 0.02457(18) Uani 1 1 d . . . Si1 Si -0.2897(4) 0.0182(4) -0.3805(3) 0.0218(9) Uani 1 1 d . . . Si2 Si -0.1796(5) 0.0663(4) -0.1357(3) 0.0300(10) Uani 1 1 d . . . O1 O -0.4344(10) -0.0995(9) -0.4042(8) 0.035(3) Uani 1 1 d . . . O2 O -0.3077(9) 0.1093(8) -0.4541(7) 0.027(2) Uiso 1 1 d . . . N1 N -0.3009(14) 0.3216(10) -0.5478(9) 0.036(3) Uani 1 1 d D . . N2 N -0.2484(11) 0.1196(10) -0.2380(8) 0.020(2) Uiso 1 1 d . . . C1 C -0.268(6) 0.459(2) -0.537(4) 0.049(4) Uani 0.41(4) 1 d PDU A 2 H1B H -0.1665 0.4881 -0.5386 0.059 Uiso 0.41(4) 1 calc PR A 2 H1C H -0.2808 0.5168 -0.4628 0.059 Uiso 0.41(4) 1 calc PR A 2 C2 C -0.360(4) 0.484(5) -0.628(4) 0.050(4) Uani 0.41(4) 1 d PDU A 2 H2A H -0.3464 0.5814 -0.6057 0.075 Uiso 0.41(4) 1 calc PR A 2 H2B H -0.4606 0.4406 -0.6366 0.075 Uiso 0.41(4) 1 calc PR A 2 H2C H -0.3309 0.4462 -0.6986 0.075 Uiso 0.41(4) 1 calc PR A 2 C1A C -0.252(4) 0.4685(18) -0.501(3) 0.047(4) Uani 0.59(4) 1 d PDU A 1 H1AA H -0.1515 0.4956 -0.5065 0.057 Uiso 0.59(4) 1 calc PR A 1 H1AB H -0.2556 0.5040 -0.4216 0.057 Uiso 0.59(4) 1 calc PR A 1 C2A C -0.341(3) 0.533(3) -0.561(3) 0.049(4) Uani 0.59(4) 1 d PDU A 1 H2AA H -0.3315 0.6264 -0.5107 0.074 Uiso 0.59(4) 1 calc PR A 1 H2AB H -0.4414 0.4818 -0.5825 0.074 Uiso 0.59(4) 1 calc PR A 1 H2AC H -0.3067 0.5322 -0.6279 0.074 Uiso 0.59(4) 1 calc PR A 1 C10 C -0.1423(15) -0.0605(14) -0.4177(10) 0.032(4) Uani 1 1 d . . . H10A H -0.1672 -0.1201 -0.4971 0.049 Uiso 1 1 calc R . . H10B H -0.1274 -0.1130 -0.3733 0.049 Uiso 1 1 calc R . . H10C H -0.0547 0.0102 -0.4022 0.049 Uiso 1 1 calc R . . C3 C -0.304(4) 0.242(5) -0.6633(19) 0.049(4) Uani 0.53(7) 1 d PDU A 2 H3A H -0.3241 0.2902 -0.7111 0.059 Uiso 0.53(7) 1 calc PR A 2 H3B H -0.3764 0.1539 -0.6915 0.059 Uiso 0.53(7) 1 calc PR A 2 C4 C -0.152(4) 0.223(4) -0.659(3) 0.049(4) Uani 0.53(7) 1 d PDU A 2 H4A H -0.1347 0.1915 -0.7348 0.074 Uiso 0.53(7) 1 calc PR A 2 H4B H -0.1432 0.1560 -0.6281 0.074 Uiso 0.53(7) 1 calc PR A 2 H4C H -0.0826 0.3090 -0.6122 0.074 Uiso 0.53(7) 1 calc PR A 2 C3A C -0.269(6) 0.232(5) -0.649(3) 0.049(4) Uani 0.47(7) 1 d PDU A 1 H3AA H -0.3339 0.2322 -0.7132 0.059 Uiso 0.47(7) 1 calc PR A 1 H3AB H -0.2952 0.1399 -0.6515 0.059 Uiso 0.47(7) 1 calc PR A 1 C4A C -0.117(5) 0.258(5) -0.671(4) 0.050(4) Uani 0.47(7) 1 d PDU A 1 H4AA H -0.1129 0.1853 -0.7396 0.075 Uiso 0.47(7) 1 calc PR A 1 H4AB H -0.0489 0.2616 -0.6082 0.075 Uiso 0.47(7) 1 calc PR A 1 H4AC H -0.0917 0.3444 -0.6789 0.075 Uiso 0.47(7) 1 calc PR A 1 C11 C -0.2625(14) 0.2562(13) -0.2056(11) 0.026(3) Uani 1 1 d . . . C12 C -0.1512(15) 0.3582(12) -0.2101(11) 0.026(3) Uani 1 1 d U . . C13 C -0.1730(16) 0.4841(13) -0.1896(12) 0.033(3) Uani 1 1 d U . . H13A H -0.1013 0.5521 -0.1950 0.040 Uiso 1 1 calc R . . C14 C -0.2963(16) 0.5126(14) -0.1616(11) 0.034(3) Uani 1 1 d U . . H14A H -0.3101 0.5993 -0.1486 0.041 Uiso 1 1 calc R . . C15 C -0.3999(16) 0.4154(14) -0.1524(12) 0.035(4) Uani 1 1 d U . . H15A H -0.4815 0.4389 -0.1279 0.042 Uiso 1 1 calc R . . C16 C -0.3907(15) 0.2864(14) -0.1769(11) 0.028(3) Uani 1 1 d U . . C17 C -0.215(2) 0.1628(17) 0.0024(12) 0.060(6) Uani 1 1 d . . . H17A H -0.2362 0.2461 0.0029 0.090 Uiso 1 1 calc R . . H17B H -0.1315 0.1852 0.0612 0.090 Uiso 1 1 calc R . . H17C H -0.2973 0.1079 0.0157 0.090 Uiso 1 1 calc R . . C18 C 0.0131(19) 0.0874(19) -0.1144(16) 0.069(6) Uani 1 1 d . . . H18A H 0.0402 0.0594 -0.1869 0.104 Uiso 1 1 calc R . . H18B H 0.0394 0.0318 -0.0759 0.104 Uiso 1 1 calc R . . H18C H 0.0630 0.1824 -0.0692 0.104 Uiso 1 1 calc R . . C19 C -0.2685(18) -0.1171(15) -0.1779(13) 0.054(5) Uani 1 1 d . . . H19A H -0.2529 -0.1694 -0.2513 0.081 Uiso 1 1 calc R . . H19B H -0.3710 -0.1297 -0.1816 0.081 Uiso 1 1 calc R . . H19C H -0.2282 -0.1479 -0.1229 0.081 Uiso 1 1 calc R . . C121 C -0.0083(15) 0.3326(15) -0.2325(12) 0.035(4) Uani 1 1 d . . . H12A H -0.0111 0.2375 -0.2438 0.042 Uiso 1 1 calc R . . C122 C 0.021(2) 0.3533(18) -0.3380(15) 0.065(6) Uani 1 1 d . . . H12B H 0.1063 0.3245 -0.3566 0.098 Uiso 1 1 calc R . . H12C H 0.0369 0.4490 -0.3242 0.098 Uiso 1 1 calc R . . H12D H -0.0606 0.2997 -0.4002 0.098 Uiso 1 1 calc R . . C123 C 0.1159(17) 0.4279(16) -0.1357(13) 0.051(5) Uani 1 1 d . . . H12E H 0.1025 0.4140 -0.0679 0.077 Uiso 1 1 calc R . . H12F H 0.1192 0.5215 -0.1236 0.077 Uiso 1 1 calc R . . H12G H 0.2054 0.4092 -0.1535 0.077 Uiso 1 1 calc R . . C261 C -0.5142(16) 0.1793(14) -0.1716(12) 0.037(4) Uani 1 1 d . . . H26A H -0.4803 0.0977 -0.1784 0.044 Uiso 1 1 calc R . . C262 C -0.5615(18) 0.2294(16) -0.0614(12) 0.050(5) Uani 1 1 d . . . H26B H -0.6411 0.1596 -0.0616 0.075 Uiso 1 1 calc R . . H26C H -0.5922 0.3113 -0.0521 0.075 Uiso 1 1 calc R . . H26D H -0.4819 0.2497 0.0002 0.075 Uiso 1 1 calc R . . C263 C -0.6391(15) 0.1388(15) -0.2696(12) 0.037(4) Uani 1 1 d . . . H26E H -0.7134 0.0641 -0.2706 0.055 Uiso 1 1 calc R . . H26F H -0.6060 0.1104 -0.3396 0.055 Uiso 1 1 calc R . . H26G H -0.6780 0.2160 -0.2616 0.055 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 Bi1 0.0275(3) 0.0202(3) 0.0233(3) 0.0076(2) 0.0068(2) 0.0020(2) Si1 0.023(2) 0.021(2) 0.016(2) 0.0021(16) 0.0047(17) 0.0035(16) Si2 0.034(2) 0.032(2) 0.027(2) 0.017(2) 0.0035(19) 0.0060(19) O1 0.027(6) 0.036(6) 0.031(6) 0.006(5) 0.013(5) -0.002(5) N1 0.059(9) 0.017(6) 0.038(8) 0.016(6) 0.013(7) 0.011(6) C1 0.046(9) 0.060(8) 0.045(9) 0.027(7) 0.022(8) 0.004(7) C2 0.047(9) 0.061(8) 0.045(9) 0.026(7) 0.021(8) 0.003(7) C1A 0.044(9) 0.060(8) 0.044(9) 0.029(7) 0.023(8) 0.002(6) C2A 0.046(9) 0.061(8) 0.045(9) 0.027(7) 0.021(8) 0.004(7) C10 0.031(8) 0.052(10) 0.016(8) 0.010(7) 0.003(6) 0.025(8) C3 0.046(9) 0.061(8) 0.043(8) 0.026(7) 0.022(8) 0.003(7) C4 0.047(9) 0.060(8) 0.044(8) 0.027(7) 0.022(8) 0.003(7) C3A 0.046(9) 0.060(8) 0.044(8) 0.027(7) 0.022(8) 0.003(7) C4A 0.046(9) 0.061(8) 0.045(9) 0.026(7) 0.021(8) 0.003(7) C11 0.028(8) 0.032(8) 0.017(7) 0.006(7) 0.005(6) 0.016(7) C12 0.036(8) 0.012(6) 0.016(7) -0.006(6) 0.007(7) -0.003(5) C13 0.046(8) 0.023(6) 0.041(9) 0.024(7) 0.016(8) 0.004(6) C14 0.042(8) 0.024(6) 0.028(8) 0.005(7) -0.001(7) 0.007(5) C15 0.040(8) 0.038(7) 0.032(9) 0.012(7) 0.017(8) 0.018(6) C16 0.034(8) 0.037(6) 0.024(8) 0.022(7) 0.013(7) 0.008(6) C17 0.106(17) 0.053(11) 0.033(10) 0.024(9) 0.000(10) 0.039(11) C18 0.059(13) 0.104(15) 0.083(14) 0.081(13) 0.016(11) 0.019(12) C19 0.053(12) 0.055(11) 0.052(11) 0.032(10) -0.008(9) 0.003(9) C121 0.033(9) 0.037(9) 0.036(9) 0.018(8) 0.008(7) 0.003(7) C122 0.060(13) 0.083(14) 0.063(13) 0.039(11) 0.027(11) 0.016(11) C123 0.035(10) 0.061(12) 0.056(12) 0.020(10) 0.001(9) 0.023(9) C261 0.044(10) 0.033(9) 0.041(10) 0.016(8) 0.029(9) 0.012(8) C262 0.046(11) 0.061(12) 0.039(10) 0.014(9) 0.019(9) 0.012(9) C263 0.025(8) 0.043(9) 0.034(9) 0.008(8) 0.005(7) 0.004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi1 O2 2.051(9) . ? Bi1 O1 2.075(9) 2_454 ? Bi1 N1 2.089(11) . ? Si1 O1 1.629(9) . ? Si1 O2 1.650(10) . ? Si1 N2 1.745(10) . ? Si1 C10 1.862(13) . ? Si2 N2 1.771(12) . ? Si2 C18 1.832(18) . ? Si2 C17 1.864(15) . ? Si2 C19 1.875(15) . ? O1 Bi1 2.075(9) 2_454 ? N1 C1 1.438(19) . ? N1 C3 1.449(18) . ? N1 C1A 1.459(17) . ? N1 C3A 1.461(18) . ? N2 C11 1.451(16) . ? C1 C2 1.549(19) . ? C1 H1B 0.9900 . ? C1 H1C 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C1A C2A 1.542(18) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? C2A H2AA 0.9800 . ? C2A H2AB 0.9800 . ? C2A H2AC 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C3 C4 1.541(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C3A C4A 1.548(19) . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C4A H4AA 0.9800 . ? C4A H4AB 0.9800 . ? C4A H4AC 0.9800 . ? C11 C12 1.427(18) . ? C11 C16 1.427(18) . ? C12 C13 1.384(18) . ? C12 C121 1.530(19) . ? C13 C14 1.372(19) . ? C13 H13A 0.9500 . ? C14 C15 1.373(19) . ? C14 H14A 0.9500 . ? C15 C16 1.366(18) . ? C15 H15A 0.9500 . ? C16 C261 1.542(18) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C121 C123 1.53(2) . ? C121 C122 1.54(2) . ? C121 H12A 1.0000 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C122 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C123 H12G 0.9800 . ? C261 C262 1.523(17) . ? C261 C263 1.53(2) . ? C261 H26A 1.0000 . ? C262 H26B 0.9800 . ? C262 H26C 0.9800 . ? C262 H26D 0.9800 . ? C263 H26E 0.9800 . ? C263 H26F 0.9800 . ? C263 H26G 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 O2 Bi1 O1 89.7(4) . 2_454 ? O2 Bi1 N1 93.5(4) . . ? O1 Bi1 N1 92.6(4) 2_454 . ? O1 Si1 O2 112.6(6) . . ? O1 Si1 N2 106.9(5) . . ? O2 Si1 N2 110.6(5) . . ? O1 Si1 C10 109.3(6) . . ? O2 Si1 C10 107.8(6) . . ? N2 Si1 C10 109.5(6) . . ? N2 Si2 C18 113.9(7) . . ? N2 Si2 C17 110.9(6) . . ? C18 Si2 C17 106.7(9) . . ? N2 Si2 C19 109.2(7) . . ? C18 Si2 C19 107.8(9) . . ? C17 Si2 C19 108.2(8) . . ? Si1 O1 Bi1 135.2(5) . 2_454 ? Si1 O2 Bi1 134.9(5) . . ? C1 N1 C3 105(3) . . ? C1 N1 C1A 17(2) . . ? C3 N1 C1A 121(3) . . ? C1 N1 C3A 112(3) . . ? C3 N1 C3A 16(3) . . ? C1A N1 C3A 125(3) . . ? C1 N1 Bi1 125(2) . . ? C3 N1 Bi1 122(2) . . ? C1A N1 Bi1 113.9(15) . . ? C3A N1 Bi1 122(2) . . ? C11 N2 Si1 117.0(9) . . ? C11 N2 Si2 120.1(8) . . ? Si1 N2 Si2 122.7(6) . . ? N1 C1 C2 114(3) . . ? N1 C1 H1B 108.6 . . ? C2 C1 H1B 108.6 . . ? N1 C1 H1C 108.6 . . ? C2 C1 H1C 108.6 . . ? H1B C1 H1C 107.6 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C1A C2A 113(2) . . ? N1 C1A H1AA 108.9 . . ? C2A C1A H1AA 108.9 . . ? N1 C1A H1AB 108.9 . . ? C2A C1A H1AB 108.9 . . ? H1AA C1A H1AB 107.7 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C3 C4 103(3) . . ? N1 C3 H3A 111.1 . . ? C4 C3 H3A 111.1 . . ? N1 C3 H3B 111.1 . . ? C4 C3 H3B 111.2 . . ? H3A C3 H3B 109.1 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C3A C4A 120(3) . . ? N1 C3A H3AA 107.2 . . ? C4A C3A H3AA 107.2 . . ? N1 C3A H3AB 107.2 . . ? C4A C3A H3AB 107.2 . . ? H3AA C3A H3AB 106.8 . . ? C12 C11 C16 120.0(13) . . ? C12 C11 N2 119.5(11) . . ? C16 C11 N2 120.4(12) . . ? C13 C12 C11 118.4(12) . . ? C13 C12 C121 120.0(12) . . ? C11 C12 C121 121.6(12) . . ? C14 C13 C12 121.2(13) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C13 C14 C15 119.8(14) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C16 C15 C14 122.9(13) . . ? C16 C15 H15A 118.5 . . ? C14 C15 H15A 118.5 . . ? C15 C16 C11 117.5(13) . . ? C15 C16 C261 120.7(12) . . ? C11 C16 C261 121.8(13) . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C123 C121 C12 111.9(12) . . ? C123 C121 C122 107.5(13) . . ? C12 C121 C122 110.9(14) . . ? C123 C121 H12A 108.8 . . ? C12 C121 H12A 108.8 . . ? C122 C121 H12A 108.8 . . ? C121 C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C122 H12D 109.5 . . ? H12B C122 H12D 109.5 . . ? H12C C122 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C121 C123 H12G 109.5 . . ? H12E C123 H12G 109.5 . . ? H12F C123 H12G 109.5 . . ? C262 C261 C263 110.5(12) . . ? C262 C261 C16 111.8(12) . . ? C263 C261 C16 109.6(13) . . ? C262 C261 H26A 108.3 . . ? C263 C261 H26A 108.3 . . ? C16 C261 H26A 108.3 . . ? C261 C262 H26B 109.5 . . ? C261 C262 H26C 109.5 . . ? H26B C262 H26C 109.5 . . ? C261 C262 H26D 109.5 . . ? H26B C262 H26D 109.5 . . ? H26C C262 H26D 109.5 . . ? C261 C263 H26E 109.5 . . ? C261 C263 H26F 109.5 . . ? H26E C263 H26F 109.5 . . ? C261 C263 H26G 109.5 . . ? H26E C263 H26G 109.5 . . ? H26F C263 H26G 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.393 _refine_diff_density_min -1.479 _refine_diff_density_rms 0.257 _database_code_depnum_ccdc_archive 'CCDC 941559' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H118 N4 O8 Sb2 Si8' _chemical_formula_weight 1539.84 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7585(7) _cell_length_b 14.3218(9) _cell_length_c 14.4294(9) _cell_angle_alpha 82.922(5) _cell_angle_beta 86.529(5) _cell_angle_gamma 86.857(5) _cell_volume 1995.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5757 _cell_measurement_theta_min 2.7087 _cell_measurement_theta_max 29.1162 _exptl_crystal_description prism _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7856 _exptl_absorpt_correction_T_max 0.9054 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.1903 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14836 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_unetI/netI 0.0828 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7821 _reflns_number_gt 6474 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrysAlisPro _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 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^)+(0.0166P)^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 'refined in a riding mode to the carrier atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7821 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0696 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Sb1 Sb 0.49922(2) 0.149723(15) 0.423856(16) 0.02408(7) Uani 1 1 d . . . Si1 Si 0.79203(10) 0.19448(6) 0.29462(7) 0.0264(2) Uani 1 1 d . . . Si2 Si 0.57053(9) 0.05187(6) 0.63827(6) 0.0208(2) Uani 1 1 d . . . Si3 Si 0.64948(10) 0.33626(7) 0.15510(8) 0.0360(3) Uani 1 1 d . . . Si4 Si 0.48220(10) 0.14182(7) 0.81823(7) 0.0284(2) Uani 1 1 d . . . O1 O 0.5278(2) 0.03842(14) 0.35560(15) 0.0253(5) Uani 1 1 d . . . O2 O 0.6005(2) 0.09054(14) 0.52862(15) 0.0252(5) Uani 1 1 d . . . O3 O 0.6533(2) 0.21254(15) 0.36077(15) 0.0302(6) Uani 1 1 d . . . O4 O 0.7772(2) 0.09502(15) 0.25253(17) 0.0370(6) Uani 1 1 d . . . H4A H 0.7064 0.0692 0.2770 0.055 Uiso 1 1 calc R . . N1 N 0.7983(2) 0.28822(17) 0.20801(18) 0.0224(6) Uani 1 1 d . . . N2 N 0.4911(2) 0.14002(17) 0.69633(17) 0.0196(6) Uani 1 1 d . . . C10 C 0.9472(3) 0.1859(2) 0.3619(3) 0.0374(9) Uani 1 1 d . . . H10A H 0.9357 0.1388 0.4168 0.056 Uiso 1 1 calc R . . H10B H 0.9619 0.2472 0.3822 0.056 Uiso 1 1 calc R . . H10C H 1.0268 0.1670 0.3225 0.056 Uiso 1 1 calc R . . C11 C 0.9319(3) 0.3215(2) 0.1749(2) 0.0285(8) Uani 1 1 d . . . C12 C 0.9826(4) 0.3986(3) 0.2110(3) 0.0372(9) Uani 1 1 d . . . C13 C 1.1130(4) 0.4291(3) 0.1778(3) 0.0532(12) Uani 1 1 d . . . H13A H 1.1484 0.4815 0.2013 0.064 Uiso 1 1 calc R . . C14 C 1.1899(4) 0.3846(3) 0.1123(3) 0.0591(13) Uani 1 1 d . . . H14A H 1.2776 0.4063 0.0903 0.071 Uiso 1 1 calc R . . C15 C 1.1396(4) 0.3081(3) 0.0784(3) 0.0566(12) Uani 1 1 d . . . H15A H 1.1945 0.2767 0.0340 0.068 Uiso 1 1 calc R . . C16 C 1.0098(4) 0.2757(3) 0.1076(3) 0.0378(9) Uani 1 1 d . . . C17 C 0.6978(5) 0.4039(3) 0.0408(3) 0.0742(16) Uani 1 1 d . . . H17A H 0.7442 0.3613 -0.0006 0.111 Uiso 1 1 calc R . . H17B H 0.7599 0.4530 0.0504 0.111 Uiso 1 1 calc R . . H17C H 0.6149 0.4332 0.0123 0.111 Uiso 1 1 calc R . . C18 C 0.5453(4) 0.4135(3) 0.2306(3) 0.0600(13) Uani 1 1 d . . . H18A H 0.5984 0.4674 0.2398 0.090 Uiso 1 1 calc R . . H18B H 0.5225 0.3776 0.2913 0.090 Uiso 1 1 calc R . . H18C H 0.4605 0.4360 0.2003 0.090 Uiso 1 1 calc R . . C19 C 0.5409(4) 0.2402(3) 0.1325(3) 0.0466(11) Uani 1 1 d . . . H19A H 0.5968 0.1942 0.0998 0.070 Uiso 1 1 calc R . . H19B H 0.4658 0.2664 0.0937 0.070 Uiso 1 1 calc R . . H19C H 0.5028 0.2091 0.1921 0.070 Uiso 1 1 calc R . . C20 C 0.7367(3) 0.0080(2) 0.6862(3) 0.0382(9) Uani 1 1 d . . . H20A H 0.7806 -0.0383 0.6478 0.057 Uiso 1 1 calc R . . H20B H 0.7209 -0.0217 0.7506 0.057 Uiso 1 1 calc R . . H20C H 0.7967 0.0608 0.6856 0.057 Uiso 1 1 calc R . . C21 C 0.4296(3) 0.2185(2) 0.6371(2) 0.0221(7) Uani 1 1 d . . . C22 C 0.5132(3) 0.2937(2) 0.5989(2) 0.0283(8) Uani 1 1 d . . . C23 C 0.4543(4) 0.3643(2) 0.5367(3) 0.0409(10) Uani 1 1 d . . . H23A H 0.5089 0.4144 0.5093 0.049 Uiso 1 1 calc R . . C24 C 0.3198(4) 0.3638(2) 0.5138(3) 0.0425(10) Uani 1 1 d . . . H24A H 0.2828 0.4125 0.4703 0.051 Uiso 1 1 calc R . . C25 C 0.2392(4) 0.2928(2) 0.5539(2) 0.0332(9) Uani 1 1 d . . . H25A H 0.1456 0.2937 0.5389 0.040 Uiso 1 1 calc R . . C26 C 0.2913(3) 0.2195(2) 0.6158(2) 0.0238(7) Uani 1 1 d . . . C27 C 0.3753(4) 0.2465(3) 0.8475(3) 0.0477(11) Uani 1 1 d . . . H27A H 0.2797 0.2392 0.8335 0.072 Uiso 1 1 calc R . . H27B H 0.4097 0.3032 0.8102 0.072 Uiso 1 1 calc R . . H27C H 0.3801 0.2524 0.9141 0.072 Uiso 1 1 calc R . . C28 C 0.4048(5) 0.0347(3) 0.8784(3) 0.0576(12) Uani 1 1 d . . . H28A H 0.4608 -0.0209 0.8634 0.086 Uiso 1 1 calc R . . H28B H 0.3116 0.0311 0.8577 0.086 Uiso 1 1 calc R . . H28C H 0.4009 0.0370 0.9461 0.086 Uiso 1 1 calc R . . C29 C 0.6557(4) 0.1475(3) 0.8642(3) 0.0526(12) Uani 1 1 d . . . H29A H 0.7067 0.0869 0.8611 0.079 Uiso 1 1 calc R . . H29B H 0.6458 0.1610 0.9293 0.079 Uiso 1 1 calc R . . H29C H 0.7058 0.1975 0.8263 0.079 Uiso 1 1 calc R . . C121 C 0.9038(4) 0.4510(2) 0.2832(3) 0.0419(10) Uani 1 1 d . . . H12A H 0.8204 0.4154 0.3055 0.050 Uiso 1 1 calc R . . C122 C 0.8556(5) 0.5499(3) 0.2390(4) 0.0734(15) Uani 1 1 d . . . H12B H 0.7963 0.5806 0.2846 0.110 Uiso 1 1 calc R . . H12C H 0.8042 0.5443 0.1838 0.110 Uiso 1 1 calc R . . H12D H 0.9357 0.5876 0.2204 0.110 Uiso 1 1 calc R . . C123 C 0.9858(4) 0.4601(3) 0.3674(3) 0.0542(12) Uani 1 1 d . . . H12E H 1.0235 0.3979 0.3924 0.081 Uiso 1 1 calc R . . H12F H 0.9257 0.4863 0.4156 0.081 Uiso 1 1 calc R . . H12G H 1.0613 0.5020 0.3486 0.081 Uiso 1 1 calc R . . C161 C 0.9628(4) 0.1913(3) 0.0662(3) 0.0479(11) Uani 1 1 d . . . H16A H 0.8640 0.1834 0.0868 0.057 Uiso 1 1 calc R . . C162 C 1.0434(4) 0.1000(3) 0.1014(3) 0.0686(14) Uani 1 1 d . . . H16B H 1.0268 0.0864 0.1693 0.103 Uiso 1 1 calc R . . H16C H 1.1418 0.1076 0.0866 0.103 Uiso 1 1 calc R . . H16D H 1.0130 0.0479 0.0709 0.103 Uiso 1 1 calc R . . C163 C 0.9722(4) 0.2059(4) -0.0409(3) 0.0804(17) Uani 1 1 d . . . H16E H 0.9270 0.2666 -0.0631 0.121 Uiso 1 1 calc R . . H16F H 0.9266 0.1551 -0.0647 0.121 Uiso 1 1 calc R . . H16G H 1.0690 0.2051 -0.0634 0.121 Uiso 1 1 calc R . . C221 C 0.6596(3) 0.3002(2) 0.6253(3) 0.0344(9) Uani 1 1 d . . . H22A H 0.6901 0.2379 0.6588 0.041 Uiso 1 1 calc R . . C222 C 0.7590(4) 0.3233(3) 0.5416(3) 0.0547(12) Uani 1 1 d . . . H22B H 0.7581 0.2744 0.4998 0.082 Uiso 1 1 calc R . . H22C H 0.8519 0.3261 0.5630 0.082 Uiso 1 1 calc R . . H22D H 0.7311 0.3844 0.5079 0.082 Uiso 1 1 calc R . . C223 C 0.6684(4) 0.3750(3) 0.6916(3) 0.0564(12) Uani 1 1 d . . . H22E H 0.6109 0.3582 0.7487 0.085 Uiso 1 1 calc R . . H22F H 0.6358 0.4364 0.6609 0.085 Uiso 1 1 calc R . . H22G H 0.7640 0.3783 0.7077 0.085 Uiso 1 1 calc R . . C261 C 0.1964(3) 0.1414(2) 0.6558(2) 0.0265(8) Uani 1 1 d . . . H26A H 0.2485 0.0976 0.7021 0.032 Uiso 1 1 calc R . . C262 C 0.0691(3) 0.1793(3) 0.7072(3) 0.0442(10) Uani 1 1 d . . . H26B H 0.0959 0.2223 0.7499 0.066 Uiso 1 1 calc R . . H26C H 0.0215 0.1268 0.7430 0.066 Uiso 1 1 calc R . . H26D H 0.0076 0.2131 0.6619 0.066 Uiso 1 1 calc R . . C263 C 0.1560(4) 0.0847(2) 0.5803(3) 0.0375(9) Uani 1 1 d . . . H26E H 0.2378 0.0515 0.5552 0.056 Uiso 1 1 calc R . . H26F H 0.1148 0.1271 0.5299 0.056 Uiso 1 1 calc R . . H26G H 0.0892 0.0387 0.6071 0.056 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 Sb1 0.03074(14) 0.02039(13) 0.02067(12) -0.00209(9) 0.00451(9) -0.00466(9) Si1 0.0341(6) 0.0227(5) 0.0216(5) 0.0005(4) 0.0002(4) -0.0025(4) Si2 0.0213(5) 0.0218(5) 0.0196(5) -0.0035(4) -0.0009(4) -0.0022(4) Si3 0.0337(6) 0.0333(6) 0.0398(6) 0.0017(5) -0.0080(5) 0.0025(5) Si4 0.0332(6) 0.0334(6) 0.0198(5) -0.0074(4) -0.0018(4) -0.0041(5) O1 0.0304(13) 0.0236(12) 0.0228(12) -0.0054(10) 0.0040(10) -0.0090(10) O2 0.0296(13) 0.0228(12) 0.0224(12) -0.0012(10) 0.0060(10) -0.0039(10) O3 0.0402(14) 0.0253(13) 0.0248(13) -0.0039(11) 0.0105(11) -0.0107(11) O4 0.0447(15) 0.0282(13) 0.0379(15) -0.0048(12) 0.0069(12) -0.0091(12) N1 0.0210(14) 0.0205(14) 0.0239(15) 0.0037(12) 0.0036(12) -0.0029(12) N2 0.0189(14) 0.0203(14) 0.0196(14) -0.0026(12) -0.0003(11) -0.0001(11) C10 0.044(2) 0.032(2) 0.036(2) 0.0018(18) -0.0107(18) -0.0007(18) C11 0.0217(18) 0.032(2) 0.030(2) 0.0062(17) -0.0012(15) -0.0076(15) C12 0.032(2) 0.034(2) 0.044(2) 0.0051(19) -0.0013(18) -0.0115(17) C13 0.047(3) 0.053(3) 0.060(3) 0.001(2) -0.001(2) -0.020(2) C14 0.033(2) 0.082(4) 0.060(3) 0.001(3) 0.007(2) -0.023(2) C15 0.032(2) 0.090(4) 0.049(3) -0.013(3) 0.010(2) -0.011(2) C16 0.030(2) 0.054(3) 0.030(2) -0.007(2) 0.0018(17) -0.0061(19) C17 0.076(3) 0.072(3) 0.066(3) 0.036(3) -0.022(3) -0.002(3) C18 0.044(3) 0.048(3) 0.091(4) -0.023(3) -0.013(2) 0.016(2) C19 0.040(2) 0.050(3) 0.052(3) -0.009(2) -0.012(2) 0.000(2) C20 0.033(2) 0.040(2) 0.043(2) -0.012(2) -0.0092(18) 0.0064(17) C21 0.0275(18) 0.0219(18) 0.0168(17) -0.0057(14) 0.0028(14) 0.0023(14) C22 0.035(2) 0.0206(18) 0.030(2) -0.0073(16) 0.0066(16) -0.0048(16) C23 0.049(3) 0.021(2) 0.050(3) 0.0018(19) 0.010(2) -0.0034(18) C24 0.047(3) 0.029(2) 0.047(3) 0.0090(19) -0.003(2) 0.0101(19) C25 0.031(2) 0.033(2) 0.034(2) -0.0011(18) -0.0006(17) 0.0064(17) C26 0.0244(18) 0.0247(18) 0.0222(18) -0.0050(15) 0.0030(14) -0.0006(15) C27 0.054(3) 0.058(3) 0.033(2) -0.017(2) 0.0030(19) 0.004(2) C28 0.095(4) 0.057(3) 0.022(2) 0.002(2) -0.008(2) -0.025(3) C29 0.050(3) 0.079(3) 0.034(2) -0.022(2) -0.0133(19) -0.001(2) C121 0.043(2) 0.028(2) 0.055(3) -0.006(2) -0.001(2) -0.0062(18) C122 0.102(4) 0.036(3) 0.085(4) -0.009(3) -0.028(3) 0.002(3) C123 0.058(3) 0.052(3) 0.056(3) -0.011(2) -0.005(2) -0.023(2) C161 0.033(2) 0.075(3) 0.039(2) -0.024(2) 0.0062(18) -0.003(2) C162 0.060(3) 0.072(3) 0.079(4) -0.037(3) -0.004(3) 0.013(3) C163 0.057(3) 0.152(5) 0.040(3) -0.039(3) 0.013(2) -0.032(3) C221 0.034(2) 0.027(2) 0.044(2) -0.0099(18) 0.0036(17) -0.0108(16) C222 0.039(2) 0.079(3) 0.051(3) -0.027(3) 0.012(2) -0.018(2) C223 0.054(3) 0.061(3) 0.060(3) -0.028(3) 0.009(2) -0.025(2) C261 0.0203(18) 0.0297(19) 0.0291(19) -0.0013(16) -0.0034(15) -0.0013(15) C262 0.036(2) 0.052(3) 0.046(3) -0.008(2) 0.0083(19) -0.0094(19) C263 0.042(2) 0.035(2) 0.036(2) -0.0005(19) -0.0058(18) -0.0082(18) _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 Sb1 O3 1.918(2) . ? Sb1 O2 1.937(2) . ? Sb1 O1 1.973(2) . ? Si1 O4 1.632(2) . ? Si1 O3 1.636(2) . ? Si1 N1 1.719(3) . ? Si1 C10 1.838(3) . ? Si2 O2 1.625(2) . ? Si2 O1 1.643(2) 2_656 ? Si2 N2 1.724(3) . ? Si2 C20 1.849(3) . ? Si3 N1 1.749(3) . ? Si3 C17 1.856(4) . ? Si3 C19 1.853(4) . ? Si3 C18 1.866(4) . ? Si4 N2 1.759(3) . ? Si4 C28 1.843(4) . ? Si4 C27 1.856(4) . ? Si4 C29 1.865(4) . ? O1 Si2 1.643(2) 2_656 ? O4 H4A 0.8400 . ? N1 C11 1.446(4) . ? N2 C21 1.451(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.400(5) . ? C11 C12 1.404(5) . ? C12 C13 1.405(5) . ? C12 C121 1.506(5) . ? C13 C14 1.368(6) . ? C13 H13A 0.9500 . ? C14 C15 1.379(6) . ? C14 H14A 0.9500 . ? C15 C16 1.396(5) . ? C15 H15A 0.9500 . ? C16 C161 1.517(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.401(4) . ? C21 C22 1.423(4) . ? C22 C23 1.389(5) . ? C22 C221 1.511(5) . ? C23 C24 1.375(5) . ? C23 H23A 0.9500 . ? C24 C25 1.369(5) . ? C24 H24A 0.9500 . ? C25 C26 1.387(4) . ? C25 H25A 0.9500 . ? C26 C261 1.528(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C121 C123 1.518(5) . ? C121 C122 1.541(5) . ? C121 H12A 1.0000 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C122 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C123 H12G 0.9800 . ? C161 C163 1.531(5) . ? C161 C162 1.535(5) . ? C161 H16A 1.0000 . ? C162 H16B 0.9800 . ? C162 H16C 0.9800 . ? C162 H16D 0.9800 . ? C163 H16E 0.9800 . ? C163 H16F 0.9800 . ? C163 H16G 0.9800 . ? C221 C222 1.518(5) . ? C221 C223 1.531(5) . ? C221 H22A 1.0000 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C222 H22D 0.9800 . ? C223 H22E 0.9800 . ? C223 H22F 0.9800 . ? C223 H22G 0.9800 . ? C261 C263 1.519(4) . ? C261 C262 1.517(4) . ? C261 H26A 1.0000 . ? C262 H26B 0.9800 . ? C262 H26C 0.9800 . ? C262 H26D 0.9800 . ? C263 H26E 0.9800 . ? C263 H26F 0.9800 . ? C263 H26G 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 O3 Sb1 O2 95.07(9) . . ? O3 Sb1 O1 94.11(9) . . ? O2 Sb1 O1 92.83(9) . . ? O4 Si1 O3 107.31(12) . . ? O4 Si1 N1 111.97(13) . . ? O3 Si1 N1 106.58(12) . . ? O4 Si1 C10 108.95(15) . . ? O3 Si1 C10 111.47(15) . . ? N1 Si1 C10 110.51(15) . . ? O2 Si2 O1 108.22(12) . 2_656 ? O2 Si2 N2 109.95(12) . . ? O1 Si2 N2 110.64(12) 2_656 . ? O2 Si2 C20 107.48(14) . . ? O1 Si2 C20 107.50(14) 2_656 . ? N2 Si2 C20 112.88(15) . . ? N1 Si3 C17 109.32(16) . . ? N1 Si3 C19 109.63(15) . . ? C17 Si3 C19 107.8(2) . . ? N1 Si3 C18 111.91(17) . . ? C17 Si3 C18 110.1(2) . . ? C19 Si3 C18 107.98(18) . . ? N2 Si4 C28 110.68(15) . . ? N2 Si4 C27 109.24(15) . . ? C28 Si4 C27 109.00(18) . . ? N2 Si4 C29 111.84(15) . . ? C28 Si4 C29 107.4(2) . . ? C27 Si4 C29 108.57(18) . . ? Si2 O1 Sb1 127.40(12) 2_656 . ? Si2 O2 Sb1 138.44(13) . . ? Si1 O3 Sb1 142.17(13) . . ? Si1 O4 H4A 109.5 . . ? C11 N1 Si1 117.8(2) . . ? C11 N1 Si3 120.7(2) . . ? Si1 N1 Si3 121.25(15) . . ? C21 N2 Si2 115.4(2) . . ? C21 N2 Si4 119.25(19) . . ? Si2 N2 Si4 125.37(14) . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 120.7(3) . . ? C16 C11 N1 119.6(3) . . ? C12 C11 N1 119.7(3) . . ? C11 C12 C13 118.4(4) . . ? C11 C12 C121 123.3(3) . . ? C13 C12 C121 118.3(4) . . ? C14 C13 C12 121.2(4) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C13 C14 C15 119.8(4) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C14 C15 C16 121.5(4) . . ? C14 C15 H15A 119.2 . . ? C16 C15 H15A 119.2 . . ? C15 C16 C11 118.4(4) . . ? C15 C16 C161 117.8(4) . . ? C11 C16 C161 123.8(3) . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si3 C19 H19A 109.5 . . ? Si3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 120.3(3) . . ? C26 C21 N2 120.8(3) . . ? C22 C21 N2 118.8(3) . . ? C23 C22 C21 117.5(3) . . ? C23 C22 C221 119.8(3) . . ? C21 C22 C221 122.6(3) . . ? C24 C23 C22 122.1(3) . . ? C24 C23 H23A 119.0 . . ? C22 C23 H23A 119.0 . . ? C25 C24 C23 119.7(3) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C24 C25 C26 121.4(3) . . ? C24 C25 H25A 119.3 . . ? C26 C25 H25A 119.3 . . ? C25 C26 C21 118.9(3) . . ? C25 C26 C261 118.5(3) . . ? C21 C26 C261 122.6(3) . . ? Si4 C27 H27A 109.5 . . ? Si4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si4 C29 H29A 109.5 . . ? Si4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C12 C121 C123 113.2(3) . . ? C12 C121 C122 110.3(4) . . ? C123 C121 C122 109.2(3) . . ? C12 C121 H12A 108.0 . . ? C123 C121 H12A 108.0 . . ? C122 C121 H12A 108.0 . . ? C121 C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C122 H12D 109.5 . . ? H12B C122 H12D 109.5 . . ? H12C C122 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C121 C123 H12G 109.5 . . ? H12E C123 H12G 109.5 . . ? H12F C123 H12G 109.5 . . ? C16 C161 C163 112.1(4) . . ? C16 C161 C162 112.0(3) . . ? C163 C161 C162 109.7(4) . . ? C16 C161 H16A 107.6 . . ? C163 C161 H16A 107.6 . . ? C162 C161 H16A 107.6 . . ? C161 C162 H16B 109.5 . . ? C161 C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C161 C162 H16D 109.5 . . ? H16B C162 H16D 109.5 . . ? H16C C162 H16D 109.5 . . ? C161 C163 H16E 109.5 . . ? C161 C163 H16F 109.5 . . ? H16E C163 H16F 109.5 . . ? C161 C163 H16G 109.5 . . ? H16E C163 H16G 109.5 . . ? H16F C163 H16G 109.5 . . ? C22 C221 C222 113.3(3) . . ? C22 C221 C223 110.7(3) . . ? C222 C221 C223 108.3(3) . . ? C22 C221 H22A 108.1 . . ? C222 C221 H22A 108.1 . . ? C223 C221 H22A 108.1 . . ? C221 C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C221 C222 H22D 109.5 . . ? H22B C222 H22D 109.5 . . ? H22C C222 H22D 109.5 . . ? C221 C223 H22E 109.5 . . ? C221 C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C221 C223 H22G 109.5 . . ? H22E C223 H22G 109.5 . . ? H22F C223 H22G 109.5 . . ? C263 C261 C262 110.2(3) . . ? C263 C261 C26 111.5(3) . . ? C262 C261 C26 112.1(3) . . ? C263 C261 H26A 107.6 . . ? C262 C261 H26A 107.6 . . ? C26 C261 H26A 107.6 . . ? C261 C262 H26B 109.5 . . ? C261 C262 H26C 109.5 . . ? H26B C262 H26C 109.5 . . ? C261 C262 H26D 109.5 . . ? H26B C262 H26D 109.5 . . ? H26C C262 H26D 109.5 . . ? C261 C263 H26E 109.5 . . ? C261 C263 H26F 109.5 . . ? H26E C263 H26F 109.5 . . ? C261 C263 H26G 109.5 . . ? H26E C263 H26G 109.5 . . ? H26F C263 H26G 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.531 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 941560' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H89 Ge2 N3 O6 Si6' _chemical_formula_weight 1117.94 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 24.8315(3) _cell_length_b 24.8315(3) _cell_length_c 16.6832(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8908.7(2) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20344 _cell_measurement_theta_min 2.7820 _cell_measurement_theta_max 29.1544 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3564 _exptl_absorpt_coefficient_mu 1.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6632 _exptl_absorpt_correction_T_max 0.7573 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhanced (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.1903 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61089 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_unetI/netI 0.0328 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10449 _reflns_number_gt 8113 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrysAlisPro _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 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. One SiMe3 group and one 2,6-iPr2C6H3 group are disordered, treated in a splitting mode, and refined in PARTs. The constraints by SIMU combined with DELU are applied for the atoms of Si2, C17, C18, C19, Si2A, C18A, and C19A. The restraint by DFIX is used for the bonds of C121-C122, C121-C123, C22D-C22F, C22E-C22F, C22-C221, C26-C261, C22A-C22F, C26a-C26D and the bonds within the SiMe3 groups of Si2C17C18C19 and Si2AC17AC18AC19A. ; _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^)+(0.0542P)^2^+30.1078P] 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 'refined in a riding mode to the carrier atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 10449 _refine_ls_number_parameters 547 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.1816 _refine_ls_wR_factor_gt 0.1702 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.208 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.3333 -0.3333 1.00069(15) 0.0495(5) Uani 1 3 d S . . Ge2 Ge 0.3333 -0.3333 0.77447(15) 0.0581(6) Uani 1 3 d S . . Ge3 Ge 0.3333 -0.3333 1.50424(15) 0.0503(5) Uani 1 3 d S . . Ge4 Ge 0.3333 -0.3333 1.27864(14) 0.0522(6) Uani 1 3 d S . . Ge5 Ge 0.0000 0.0000 0.56950(8) 0.0111(4) Uiso 1 3 d S . . Ge6 Ge 0.0000 0.0000 0.34587(7) 0.0089(3) Uiso 1 3 d S . . Si1 Si 0.22399(10) -0.35173(10) 0.8863(3) 0.0547(8) Uani 1 1 d . B . Si3 Si 0.31455(10) -0.24246(11) 1.3938(3) 0.0522(8) Uani 1 1 d . A . Si4 Si 0.26746(11) -0.14862(10) 1.3845(3) 0.0490(7) Uani 1 1 d . A . Si5 Si -0.09177(8) -0.10991(8) 0.4579(2) 0.0175(3) Uani 1 1 d . . . Si6 Si -0.18546(8) -0.25095(8) 0.4587(2) 0.0216(4) Uani 1 1 d . . . N1 N 0.1473(3) -0.4094(3) 0.8880(8) 0.052(2) Uani 1 1 d . . . N2 N 0.2564(3) -0.2239(3) 1.3918(7) 0.048(2) Uani 1 1 d . . . N3 N -0.1101(2) -0.1863(2) 0.4586(6) 0.0173(11) Uani 1 1 d . . . O1 O 0.2589(3) -0.3561(4) 0.9671(7) 0.062(2) Uani 1 1 d . . . O2 O 0.2577(3) -0.3639(3) 0.8111(6) 0.061(2) Uani 1 1 d . . . O3 O 0.3021(3) -0.2894(3) 1.4684(6) 0.054(2) Uani 1 1 d . . . O4 O 0.3116(3) -0.2812(3) 1.3135(6) 0.061(2) Uani 1 1 d . . . O5 O -0.0495(4) -0.0744(3) 0.5362(4) 0.0291(16) Uani 1 1 d . . . O6 O -0.0494(3) -0.0747(3) 0.3782(5) 0.0305(17) Uani 1 1 d . . . C10 C 0.2322(4) -0.2739(4) 0.8783(10) 0.068(4) Uani 1 1 d . . . H10A H 0.2765 -0.2423 0.8776 0.102 Uiso 1 1 calc R B . H10B H 0.2121 -0.2668 0.9244 0.102 Uiso 1 1 calc R . . H10C H 0.2125 -0.2713 0.8287 0.102 Uiso 1 1 calc R . . C11 C 0.1325(2) -0.47410(17) 0.8804(5) 0.052(3) Uani 1 1 d G B . C12 C 0.1248(3) -0.5072(3) 0.9507(4) 0.056(3) Uani 1 1 d G . . C13 C 0.1068(3) -0.5699(3) 0.9472(4) 0.047(3) Uani 1 1 d G B . H13A H 0.1016 -0.5926 0.9952 0.056 Uiso 1 1 calc R . . C14 C 0.0966(2) -0.59949(17) 0.8734(5) 0.050(3) Uani 1 1 d G . . H14A H 0.0843 -0.6423 0.8710 0.060 Uiso 1 1 calc R B . C15 C 0.1043(3) -0.5663(3) 0.8031(4) 0.051(3) Uani 1 1 d G B . H15A H 0.0973 -0.5865 0.7526 0.061 Uiso 1 1 calc R . . C16 C 0.1222(3) -0.5036(3) 0.8066(4) 0.041(2) Uiso 1 1 d G . . C121 C 0.1361(5) -0.4780(5) 1.0334(9) 0.065(4) Uani 1 1 d D B . H12A H 0.1503 -0.4328 1.0263 0.078 Uiso 1 1 calc R . . C122 C 0.1868(5) -0.4831(5) 1.0839(8) 0.067(4) Uani 1 1 d D . . H12B H 0.2256 -0.4654 1.0532 0.101 Uiso 1 1 calc R B . H12C H 0.1723 -0.5269 1.0956 0.101 Uiso 1 1 calc R . . H12D H 0.1940 -0.4601 1.1342 0.101 Uiso 1 1 calc R . . C123 C 0.0751(5) -0.5076(6) 1.0891(10) 0.077(4) Uani 1 1 d D . . H12E H 0.0417 -0.5047 1.0616 0.115 Uiso 1 1 calc R B . H12F H 0.0847 -0.4848 1.1399 0.115 Uiso 1 1 calc R . . H12G H 0.0615 -0.5514 1.0997 0.115 Uiso 1 1 calc R . . C161 C 0.1306(5) -0.4700(5) 0.7289(8) 0.060(3) Uani 1 1 d . B . H16A H 0.1458 -0.4253 0.7414 0.072 Uiso 1 1 calc R . . C162 C 0.0700(6) -0.4952(6) 0.6804(10) 0.081(4) Uani 1 1 d . . . H16B H 0.0383 -0.4931 0.7131 0.122 Uiso 1 1 calc R B . H16C H 0.0553 -0.5385 0.6653 0.122 Uiso 1 1 calc R . . H16D H 0.0778 -0.4701 0.6319 0.122 Uiso 1 1 calc R . . C163 C 0.1780(6) -0.4732(6) 0.6753(9) 0.073(4) Uani 1 1 d . . . H16E H 0.2177 -0.4562 0.7037 0.110 Uiso 1 1 calc R B . H16F H 0.1837 -0.4488 0.6266 0.110 Uiso 1 1 calc R . . H16G H 0.1634 -0.5165 0.6607 0.110 Uiso 1 1 calc R . . C20 C 0.3917(5) -0.1722(5) 1.4046(10) 0.075(4) Uani 1 1 d . . . H20A H 0.4238 -0.1840 1.4053 0.113 Uiso 1 1 calc R A . H20B H 0.3931 -0.1511 1.4549 0.113 Uiso 1 1 calc R . . H20C H 0.3990 -0.1441 1.3595 0.113 Uiso 1 1 calc R . . C21 C 0.1917(3) -0.2760(4) 1.3798(7) 0.026(4) Uiso 0.508(17) 1 d PG A 2 C22 C 0.1606(4) -0.3000(4) 1.3078(6) 0.013(3) Uiso 0.508(17) 1 d PGD A 2 C23 C 0.0978(4) -0.3444(5) 1.3080(6) 0.024(4) Uiso 0.508(17) 1 d PG A 2 H23A H 0.0766 -0.3607 1.2587 0.029 Uiso 0.508(17) 1 calc PR A 2 C24 C 0.0659(3) -0.3648(4) 1.3801(7) 0.019(3) Uiso 0.508(17) 1 d PG A 2 H24A H 0.0229 -0.3951 1.3803 0.023 Uiso 0.508(17) 1 calc PR A 2 C25 C 0.0969(4) -0.3409(4) 1.4521(6) 0.013(3) Uiso 0.508(17) 1 d PG A 2 H25A H 0.0752 -0.3548 1.5015 0.015 Uiso 0.508(17) 1 calc PR A 2 C26 C 0.1598(4) -0.2965(5) 1.4520(6) 0.036(4) Uiso 0.508(17) 1 d PGD A 2 C221 C 0.1919(7) -0.2808(7) 1.2289(9) 0.017(4) Uiso 0.508(17) 1 d PD A 2 H22A H 0.2367 -0.2493 1.2381 0.020 Uiso 0.508(17) 1 calc PR A 2 C222 C 0.1888(11) -0.3364(10) 1.1799(15) 0.045(5) Uiso 0.508(17) 1 d P A 2 H22B H 0.2070 -0.3565 1.2117 0.068 Uiso 0.508(17) 1 calc PR A 2 H22C H 0.2122 -0.3207 1.1298 0.068 Uiso 0.508(17) 1 calc PR A 2 H22D H 0.1453 -0.3667 1.1677 0.068 Uiso 0.508(17) 1 calc PR A 2 C223 C 0.1640(10) -0.2520(10) 1.1736(14) 0.044(5) Uiso 0.508(17) 1 d P A 2 H22E H 0.1642 -0.2170 1.2009 0.066 Uiso 0.508(17) 1 calc PR A 2 H22F H 0.1212 -0.2834 1.1600 0.066 Uiso 0.508(17) 1 calc PR A 2 H22G H 0.1888 -0.2372 1.1244 0.066 Uiso 0.508(17) 1 calc PR A 2 C261 C 0.1903(8) -0.2733(7) 1.5337(12) 0.020(4) Uiso 0.508(17) 1 d PD A 2 H26A H 0.2353 -0.2437 1.5224 0.024 Uiso 0.508(17) 1 calc PR A 2 C262 C 0.1892(9) -0.3235(9) 1.5870(13) 0.036(5) Uiso 0.508(17) 1 d P A 2 H26B H 0.2042 -0.3472 1.5566 0.054 Uiso 0.508(17) 1 calc PR A 2 H26C H 0.1465 -0.3516 1.6051 0.054 Uiso 0.508(17) 1 calc PR A 2 H26D H 0.2161 -0.3042 1.6336 0.054 Uiso 0.508(17) 1 calc PR A 2 C263 C 0.1660(11) -0.2342(11) 1.5808(15) 0.046(6) Uiso 0.508(17) 1 d P A 2 H26E H 0.1672 -0.2021 1.5454 0.069 Uiso 0.508(17) 1 calc PR A 2 H26F H 0.1925 -0.2144 1.6276 0.069 Uiso 0.508(17) 1 calc PR A 2 H26G H 0.1231 -0.2618 1.5985 0.069 Uiso 0.508(17) 1 calc PR A 2 C21A C 0.1912(4) -0.2744(5) 1.4082(8) 0.021(4) Uiso 0.492(17) 1 d PG A 1 C22A C 0.1556(5) -0.3025(6) 1.3404(7) 0.039(5) Uiso 0.492(17) 1 d PGD A 1 C23A C 0.0932(5) -0.3474(5) 1.3482(7) 0.034(4) Uiso 0.492(17) 1 d PG A 1 H23B H 0.0689 -0.3666 1.3018 0.040 Uiso 0.492(17) 1 calc PR A 1 C24A C 0.0664(4) -0.3642(5) 1.4238(8) 0.024(4) Uiso 0.492(17) 1 d PG A 1 H24B H 0.0238 -0.3949 1.4291 0.029 Uiso 0.492(17) 1 calc PR A 1 C25A C 0.1020(4) -0.3361(5) 1.4916(7) 0.034(4) Uiso 0.492(17) 1 d PG A 1 H25B H 0.0837 -0.3476 1.5433 0.040 Uiso 0.492(17) 1 calc PR A 1 C26A C 0.1643(4) -0.2912(5) 1.4839(7) 0.012(3) Uiso 0.492(17) 1 d PGD A 1 C22D C 0.1557(12) -0.2567(12) 1.2077(17) 0.060(7) Uiso 0.492(17) 1 d PD A 1 H22H H 0.1540 -0.2229 1.2359 0.091 Uiso 0.492(17) 1 calc PR A 1 H22I H 0.1137 -0.2880 1.1908 0.091 Uiso 0.492(17) 1 calc PR A 1 H22J H 0.1826 -0.2399 1.1606 0.091 Uiso 0.492(17) 1 calc PR A 1 C22E C 0.1814(11) -0.3422(10) 1.2149(14) 0.047(6) Uiso 0.492(17) 1 d PD A 1 H22K H 0.1974 -0.3639 1.2475 0.071 Uiso 0.492(17) 1 calc PR A 1 H22L H 0.2073 -0.3249 1.1670 0.071 Uiso 0.492(17) 1 calc PR A 1 H22M H 0.1385 -0.3715 1.1988 0.071 Uiso 0.492(17) 1 calc PR A 1 C22F C 0.1827(10) -0.2876(9) 1.2657(13) 0.041(5) Uiso 0.492(17) 1 d PD A 1 H22N H 0.2275 -0.2562 1.2743 0.049 Uiso 0.492(17) 1 calc PR A 1 C26D C 0.1984(8) -0.2647(8) 1.5645(12) 0.024(4) Uiso 0.492(17) 1 d PD A 1 H26H H 0.2433 -0.2347 1.5532 0.028 Uiso 0.492(17) 1 calc PR A 1 C26E C 0.1940(10) -0.3176(10) 1.6238(15) 0.044(5) Uiso 0.492(17) 1 d P A 1 H26I H 0.2166 -0.2983 1.6735 0.066 Uiso 0.492(17) 1 calc PR A 1 H26J H 0.2125 -0.3399 1.5980 0.066 Uiso 0.492(17) 1 calc PR A 1 H26K H 0.1503 -0.3468 1.6363 0.066 Uiso 0.492(17) 1 calc PR A 1 C26F C 0.1712(10) -0.2309(10) 1.6116(14) 0.038(5) Uiso 0.492(17) 1 d P A 1 H26L H 0.1691 -0.2002 1.5769 0.057 Uiso 0.492(17) 1 calc PR A 1 H26M H 0.1978 -0.2098 1.6579 0.057 Uiso 0.492(17) 1 calc PR A 1 H26N H 0.1294 -0.2611 1.6303 0.057 Uiso 0.492(17) 1 calc PR A 1 C27 C 0.1902(4) -0.1531(4) 1.3822(10) 0.061(3) Uani 1 1 d . . . H27A H 0.1658 -0.1789 1.3369 0.091 Uiso 1 1 calc R A . H27B H 0.1962 -0.1111 1.3762 0.091 Uiso 1 1 calc R . . H27C H 0.1679 -0.1714 1.4323 0.091 Uiso 1 1 calc R . . C28 C 0.3100(6) -0.1101(5) 1.2912(8) 0.060(3) Uani 1 1 d . . . H28A H 0.2881 -0.1365 1.2450 0.090 Uiso 1 1 calc R A . H28B H 0.3522 -0.1037 1.2938 0.090 Uiso 1 1 calc R . . H28C H 0.3120 -0.0699 1.2855 0.090 Uiso 1 1 calc R . . C29 C 0.3096(5) -0.0995(5) 1.4727(5) 0.040(2) Uani 1 1 d . . . H29A H 0.3509 -0.0955 1.4764 0.060 Uiso 1 1 calc R A . H29B H 0.2860 -0.1190 1.5216 0.060 Uiso 1 1 calc R . . H29C H 0.3141 -0.0582 1.4664 0.060 Uiso 1 1 calc R . . C30 C -0.1611(3) -0.1016(4) 0.4572(9) 0.0346(18) Uani 1 1 d . . . H30A H -0.1484 -0.0573 0.4568 0.052 Uiso 1 1 calc R . . H30B H -0.1860 -0.1212 0.5053 0.052 Uiso 1 1 calc R . . H30C H -0.1859 -0.1217 0.4093 0.052 Uiso 1 1 calc R . . C31 C -0.05987(18) -0.2005(2) 0.4554(4) 0.0175(14) Uani 1 1 d G . . C32 C -0.0377(3) -0.2093(3) 0.3829(3) 0.0213(19) Uani 1 1 d G . . C33 C 0.0071(3) -0.2273(3) 0.3824(4) 0.038(2) Uani 1 1 d G . . H33A H 0.0222 -0.2333 0.3329 0.045 Uiso 1 1 calc R . . C34 C 0.0296(2) -0.2365(2) 0.4543(5) 0.0343(18) Uiso 1 1 d G . . H34A H 0.0602 -0.2489 0.4539 0.041 Uiso 1 1 calc R . . C35 C 0.0074(3) -0.2277(3) 0.5267(4) 0.032(2) Uani 1 1 d G . . H35A H 0.0228 -0.2341 0.5758 0.039 Uiso 1 1 calc R . . C36 C -0.0373(3) -0.2097(3) 0.5273(3) 0.027(2) Uani 1 1 d G . . C37 C -0.2309(5) -0.2515(5) 0.5477(8) 0.047(3) Uani 1 1 d . . . H37A H -0.2089 -0.2510 0.5967 0.071 Uiso 1 1 calc R . . H37B H -0.2720 -0.2891 0.5468 0.071 Uiso 1 1 calc R . . H37C H -0.2358 -0.2147 0.5465 0.071 Uiso 1 1 calc R . . C38 C -0.2272(5) -0.2530(5) 0.3625(6) 0.039(3) Uani 1 1 d . . . H38A H -0.2024 -0.2523 0.3164 0.059 Uiso 1 1 calc R . . H38B H -0.2329 -0.2168 0.3604 0.059 Uiso 1 1 calc R . . H38C H -0.2679 -0.2911 0.3610 0.059 Uiso 1 1 calc R . . C39 C -0.1807(4) -0.3233(4) 0.4641(8) 0.038(2) Uani 1 1 d . . . H39A H -0.1571 -0.3251 0.4181 0.058 Uiso 1 1 calc R . . H39B H -0.2227 -0.3596 0.4633 0.058 Uiso 1 1 calc R . . H39C H -0.1597 -0.3234 0.5138 0.058 Uiso 1 1 calc R . . C321 C -0.0589(5) -0.1998(5) 0.3013(7) 0.037(3) Uani 1 1 d . . . H32A H -0.0900 -0.1861 0.3102 0.044 Uiso 1 1 calc R . . C322 C -0.0904(6) -0.2597(5) 0.2551(7) 0.046(3) Uani 1 1 d . . . H32B H -0.1038 -0.2525 0.2028 0.068 Uiso 1 1 calc R . . H32C H -0.1267 -0.2906 0.2850 0.068 Uiso 1 1 calc R . . H32D H -0.0612 -0.2750 0.2471 0.068 Uiso 1 1 calc R . . C323 C -0.0048(6) -0.1490(6) 0.2559(7) 0.049(3) Uani 1 1 d . . . H32E H -0.0191 -0.1435 0.2034 0.073 Uiso 1 1 calc R . . H32F H 0.0274 -0.1605 0.2486 0.073 Uiso 1 1 calc R . . H32G H 0.0124 -0.1101 0.2862 0.073 Uiso 1 1 calc R . . C361 C -0.0573(5) -0.1983(5) 0.6117(6) 0.030(2) Uani 1 1 d . . . H36A H -0.0876 -0.1835 0.6031 0.036 Uiso 1 1 calc R . . C362 C -0.0905(7) -0.2589(6) 0.6622(8) 0.060(4) Uani 1 1 d . . . H36B H -0.1026 -0.2499 0.7141 0.090 Uiso 1 1 calc R . . H36C H -0.0621 -0.2751 0.6706 0.090 Uiso 1 1 calc R . . H36D H -0.1276 -0.2899 0.6336 0.090 Uiso 1 1 calc R . . C363 C -0.0027(5) -0.1482(5) 0.6602(7) 0.043(3) Uani 1 1 d . . . H36E H 0.0193 -0.1102 0.6282 0.065 Uiso 1 1 calc R . . H36F H 0.0260 -0.1632 0.6741 0.065 Uiso 1 1 calc R . . H36G H -0.0184 -0.1394 0.7094 0.065 Uiso 1 1 calc R . . Si2 Si 0.0844(6) -0.3954(6) 0.8823(12) 0.041(3) Uani 0.59(4) 1 d PDU B 2 C17 C 0.0101(7) -0.4701(7) 0.877(2) 0.042(4) Uani 0.59(4) 1 d PDU B 2 H17A H 0.0074 -0.4967 0.9217 0.063 Uiso 0.59(4) 1 calc PR B 2 H17B H 0.0084 -0.4911 0.8261 0.063 Uiso 0.59(4) 1 calc PR B 2 H17C H -0.0247 -0.4621 0.8791 0.063 Uiso 0.59(4) 1 calc PR B 2 C18 C 0.0885(12) -0.3431(11) 0.7995(19) 0.053(5) Uani 0.59(4) 1 d PDU B 2 H18A H 0.1279 -0.3038 0.8027 0.080 Uiso 0.59(4) 1 calc PR B 2 H18B H 0.0538 -0.3350 0.8045 0.080 Uiso 0.59(4) 1 calc PR B 2 H18C H 0.0858 -0.3631 0.7478 0.080 Uiso 0.59(4) 1 calc PR B 2 C19 C 0.0824(12) -0.3590(10) 0.9728(19) 0.053(5) Uani 0.59(4) 1 d PDU B 2 H19A H 0.0790 -0.3855 1.0184 0.079 Uiso 0.59(4) 1 calc PR B 2 H19B H 0.0464 -0.3529 0.9723 0.079 Uiso 0.59(4) 1 calc PR B 2 H19C H 0.1206 -0.3187 0.9778 0.079 Uiso 0.59(4) 1 calc PR B 2 Si2A Si 0.0825(10) -0.3980(10) 0.9126(16) 0.048(4) Uani 0.41(4) 1 d PDU B 1 C17A C 0.0088(16) -0.4760(15) 0.912(2) 0.055(9) Uiso 0.41(4) 1 d PDU B 1 H17D H 0.0093 -0.5011 0.9569 0.083 Uiso 0.41(4) 1 calc PR B 1 H17E H 0.0059 -0.4975 0.8614 0.083 Uiso 0.41(4) 1 calc PR B 1 H17F H -0.0272 -0.4701 0.9170 0.083 Uiso 0.41(4) 1 calc PR B 1 C18A C 0.0749(15) -0.3559(16) 0.824(2) 0.048(5) Uani 0.41(4) 1 d PDU B 1 H18D H 0.1119 -0.3145 0.8204 0.071 Uiso 0.41(4) 1 calc PR B 1 H18E H 0.0379 -0.3517 0.8308 0.071 Uiso 0.41(4) 1 calc PR B 1 H18F H 0.0708 -0.3794 0.7752 0.071 Uiso 0.41(4) 1 calc PR B 1 C19A C 0.0872(16) -0.3598(15) 1.009(2) 0.045(5) Uani 0.41(4) 1 d PDU B 1 H19D H 0.1251 -0.3190 1.0103 0.067 Uiso 0.41(4) 1 calc PR B 1 H19E H 0.0883 -0.3855 1.0529 0.067 Uiso 0.41(4) 1 calc PR B 1 H19F H 0.0508 -0.3547 1.0152 0.067 Uiso 0.41(4) 1 calc PR B 1 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 Ge1 0.0230(5) 0.0230(5) 0.1024(15) 0.000 0.000 0.0115(3) Ge2 0.0366(7) 0.0366(7) 0.1010(17) 0.000 0.000 0.0183(3) Ge3 0.0267(6) 0.0267(6) 0.0977(15) 0.000 0.000 0.0133(3) Ge4 0.0288(6) 0.0288(6) 0.0990(17) 0.000 0.000 0.0144(3) Si1 0.0170(11) 0.0166(11) 0.130(3) -0.0076(17) -0.0055(17) 0.0080(9) Si3 0.0157(11) 0.0183(11) 0.122(3) -0.0067(17) -0.0032(17) 0.0081(9) Si4 0.0218(12) 0.0154(11) 0.111(2) 0.0031(16) 0.0116(16) 0.0100(10) Si5 0.0101(8) 0.0105(8) 0.0320(9) 0.0015(14) 0.0045(14) 0.0053(7) Si6 0.0113(9) 0.0140(9) 0.0361(9) -0.0009(14) 0.0031(14) 0.0037(7) N1 0.015(3) 0.015(3) 0.128(7) -0.015(5) -0.010(5) 0.008(3) N2 0.018(3) 0.015(3) 0.112(7) -0.003(5) 0.000(5) 0.008(3) N3 0.010(3) 0.011(3) 0.032(3) -0.005(4) 0.004(4) 0.006(2) O1 0.019(3) 0.040(4) 0.123(7) 0.022(5) -0.007(4) 0.014(3) O2 0.019(3) 0.029(4) 0.134(7) -0.020(4) -0.004(4) 0.010(3) O3 0.028(3) 0.028(4) 0.109(7) 0.002(4) -0.001(4) 0.017(3) O4 0.036(4) 0.028(4) 0.125(7) -0.020(4) -0.013(4) 0.020(3) O5 0.038(4) 0.021(3) 0.026(4) -0.003(3) 0.001(3) 0.013(3) O6 0.027(4) 0.008(3) 0.047(5) -0.003(3) -0.002(3) 0.002(3) C10 0.022(4) 0.022(4) 0.153(12) -0.002(7) -0.001(7) 0.007(4) C11 0.013(4) 0.014(4) 0.131(11) 0.009(6) 0.007(6) 0.008(3) C12 0.010(4) 0.013(4) 0.144(10) -0.017(6) -0.001(5) 0.005(3) C13 0.016(4) 0.025(5) 0.099(8) -0.001(5) 0.002(5) 0.010(4) C14 0.018(4) 0.010(3) 0.118(9) -0.006(5) 0.000(5) 0.005(3) C15 0.024(5) 0.027(5) 0.104(9) -0.008(5) -0.009(5) 0.014(4) C121 0.026(5) 0.018(5) 0.151(13) 0.026(6) 0.015(6) 0.011(4) C122 0.045(6) 0.039(6) 0.114(11) -0.005(6) -0.002(6) 0.018(5) C123 0.041(6) 0.054(7) 0.125(12) 0.002(8) 0.014(7) 0.016(5) C161 0.037(6) 0.030(5) 0.114(11) -0.001(5) -0.007(6) 0.016(4) C162 0.054(7) 0.062(8) 0.123(12) 0.002(7) -0.026(8) 0.024(6) C163 0.065(8) 0.046(6) 0.108(10) -0.013(6) -0.024(7) 0.027(6) C20 0.024(5) 0.024(5) 0.179(14) -0.013(7) 0.003(8) 0.013(4) C27 0.030(5) 0.023(4) 0.139(10) 0.013(6) 0.006(7) 0.020(4) C28 0.051(7) 0.028(5) 0.104(10) 0.002(5) -0.002(6) 0.021(5) C29 0.045(5) 0.033(5) 0.042(7) 0.002(4) 0.013(4) 0.019(4) C30 0.017(3) 0.021(4) 0.073(5) 0.009(6) 0.007(6) 0.015(3) C31 0.011(3) 0.009(3) 0.034(3) 0.010(4) -0.001(4) 0.006(2) C32 0.021(4) 0.016(4) 0.022(4) 0.008(3) 0.013(3) 0.006(3) C33 0.028(5) 0.023(5) 0.067(7) 0.007(5) 0.004(5) 0.016(4) C35 0.020(4) 0.023(4) 0.057(6) 0.009(4) -0.011(4) 0.012(3) C36 0.013(3) 0.008(3) 0.056(6) 0.006(4) 0.014(4) 0.002(3) C37 0.022(5) 0.029(5) 0.087(9) -0.009(6) 0.017(5) 0.010(4) C38 0.033(5) 0.034(5) 0.043(6) -0.011(5) -0.007(4) 0.012(4) C39 0.033(4) 0.021(4) 0.055(6) -0.011(5) 0.007(6) 0.010(3) C321 0.043(6) 0.035(5) 0.038(6) 0.004(5) -0.004(5) 0.024(4) C322 0.070(7) 0.045(6) 0.031(6) -0.007(5) -0.006(5) 0.035(6) C323 0.056(7) 0.045(6) 0.054(8) 0.018(6) 0.035(6) 0.031(5) C361 0.038(5) 0.035(5) 0.022(5) 0.009(4) -0.005(4) 0.022(4) C362 0.072(8) 0.056(7) 0.057(9) 0.026(6) 0.010(6) 0.036(6) C363 0.050(6) 0.044(6) 0.043(7) -0.011(5) -0.016(5) 0.029(5) Si2 0.013(2) 0.018(2) 0.091(8) -0.002(4) 0.004(4) 0.0081(18) C17 0.011(5) 0.023(5) 0.094(12) -0.011(6) -0.004(7) 0.010(3) C18 0.028(8) 0.027(7) 0.105(11) -0.001(6) -0.012(8) 0.014(6) C19 0.032(7) 0.020(6) 0.103(10) -0.013(7) 0.002(9) 0.012(5) Si2A 0.027(5) 0.030(5) 0.089(10) -0.020(7) -0.010(7) 0.016(4) C18A 0.020(9) 0.028(9) 0.095(11) -0.015(8) -0.009(9) 0.012(8) C19A 0.029(8) 0.025(8) 0.093(10) -0.018(9) -0.007(10) 0.022(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O1 1.733(7) . ? Ge1 O1 1.733(8) 3_655 ? Ge1 O1 1.733(7) 2_545 ? Ge2 O2 1.747(8) . ? Ge2 O2 1.747(8) 3_655 ? Ge2 O2 1.747(8) 2_545 ? Ge3 O3 1.731(7) . ? Ge3 O3 1.731(7) 2_545 ? Ge3 O3 1.731(7) 3_655 ? Ge4 O4 1.733(8) . ? Ge4 O4 1.733(8) 2_545 ? Ge4 O4 1.733(8) 3_655 ? Ge5 O5 1.722(7) 2 ? Ge5 O5 1.722(7) . ? Ge5 O5 1.722(7) 3 ? Ge6 O6 1.720(7) 2 ? Ge6 O6 1.720(7) . ? Ge6 O6 1.720(7) 3 ? Si1 O2 1.619(9) . ? Si1 O1 1.635(10) . ? Si1 N1 1.718(7) . ? Si1 C10 1.844(10) . ? Si3 O3 1.626(10) . ? Si3 O4 1.629(9) . ? Si3 N2 1.722(7) . ? Si3 C20 1.845(10) . ? Si4 N2 1.753(7) . ? Si4 C28 1.855(13) . ? Si4 C29 1.862(10) . ? Si4 C27 1.867(8) . ? Si5 O5 1.631(7) . ? Si5 O6 1.648(8) . ? Si5 N3 1.714(5) . ? Si5 C30 1.834(7) . ? Si6 N3 1.754(5) . ? Si6 C39 1.861(8) . ? Si6 C37 1.862(12) . ? Si6 C38 1.897(11) . ? N1 C11 1.464(7) . ? N1 Si2 1.763(15) . ? N1 Si2A 1.82(2) . ? N2 C21 1.488(9) . ? N2 C21A 1.496(10) . ? N3 C31 1.457(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 C121 1.520(16) . ? C13 C14 1.3900 . ? C13 H13A 0.9500 . ? C14 C15 1.3900 . ? C14 H14A 0.9500 . ? C15 C16 1.3900 . ? C15 H15A 0.9500 . ? C16 C161 1.499(13) . ? C121 C122 1.571(16) . ? C121 C123 1.608(15) . ? C121 H12A 1.0000 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C122 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C123 H12G 0.9800 . ? C161 C163 1.512(18) . ? C161 C162 1.539(16) . ? C161 H16A 1.0000 . ? C162 H16B 0.9800 . ? C162 H16C 0.9800 . ? C162 H16D 0.9800 . ? C163 H16E 0.9800 . ? C163 H16F 0.9800 . ? C163 H16G 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 C221 1.481(16) . ? C23 C24 1.3900 . ? C23 H23A 0.9500 . ? C24 C25 1.3900 . ? C24 H24A 0.9500 . ? C25 C26 1.3900 . ? C25 H25A 0.9500 . ? C26 C261 1.526(19) . ? C221 C223 1.53(3) . ? C221 C222 1.57(3) . ? C221 H22A 1.0000 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C222 H22D 0.9800 . ? C223 H22E 0.9800 . ? C223 H22F 0.9800 . ? C223 H22G 0.9800 . ? C261 C262 1.52(3) . ? C261 C263 1.59(3) . ? C261 H26A 1.0000 . ? C262 H26B 0.9800 . ? C262 H26C 0.9800 . ? C262 H26D 0.9800 . ? C263 H26E 0.9800 . ? C263 H26F 0.9800 . ? C263 H26G 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C22F 1.38(2) . ? C22A C23A 1.3900 . ? C23A C24A 1.3900 . ? C23A H23B 0.9500 . ? C24A C25A 1.3900 . ? C24A H24B 0.9500 . ? C25A C26A 1.3900 . ? C25A H25B 0.9500 . ? C26A C26D 1.551(18) . ? C22D C22F 1.58(3) . ? C22D H22H 0.9800 . ? C22D H22I 0.9800 . ? C22D H22J 0.9800 . ? C22E C22F 1.58(3) . ? C22E H22K 0.9800 . ? C22E H22L 0.9800 . ? C22E H22M 0.9800 . ? C22F H22N 1.0000 . ? C26D C26F 1.53(3) . ? C26D C26E 1.60(3) . ? C26D H26H 1.0000 . ? C26E H26I 0.9800 . ? C26E H26J 0.9800 . ? C26E H26K 0.9800 . ? C26F H26L 0.9800 . ? C26F H26M 0.9800 . ? C26F H26N 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C32 C321 1.520(11) . ? C33 C34 1.3900 . ? C33 H33A 0.9500 . ? C34 C35 1.3900 . ? C34 H34A 0.9500 . ? C35 C36 1.3900 . ? C35 H35A 0.9500 . ? C36 C361 1.567(11) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C321 C323 1.508(15) . ? C321 C322 1.500(14) . ? C321 H32A 1.0000 . ? C322 H32B 0.9800 . ? C322 H32C 0.9800 . ? C322 H32D 0.9800 . ? C323 H32E 0.9800 . ? C323 H32F 0.9800 . ? C323 H32G 0.9800 . ? C361 C363 1.533(14) . ? C361 C362 1.553(14) . ? C361 H36A 1.0000 . ? C362 H36B 0.9800 . ? C362 H36C 0.9800 . ? C362 H36D 0.9800 . ? C363 H36E 0.9800 . ? C363 H36F 0.9800 . ? C363 H36G 0.9800 . ? Si2 C19 1.77(2) . ? Si2 C17 1.852(17) . ? Si2 C18 1.86(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? Si2A C19A 1.84(3) . ? Si2A C18A 1.87(3) . ? Si2A C17A 1.89(3) . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ge1 O1 110.0(4) . 3_655 ? O1 Ge1 O1 110.0(4) . 2_545 ? O1 Ge1 O1 110.0(4) 3_655 2_545 ? O2 Ge2 O2 108.5(4) . 3_655 ? O2 Ge2 O2 108.5(4) . 2_545 ? O2 Ge2 O2 108.5(4) 3_655 2_545 ? O3 Ge3 O3 108.7(4) . 2_545 ? O3 Ge3 O3 108.7(4) . 3_655 ? O3 Ge3 O3 108.7(4) 2_545 3_655 ? O4 Ge4 O4 109.3(3) . 2_545 ? O4 Ge4 O4 109.3(3) . 3_655 ? O4 Ge4 O4 109.3(3) 2_545 3_655 ? O5 Ge5 O5 110.1(2) 2 . ? O5 Ge5 O5 110.1(2) 2 3 ? O5 Ge5 O5 110.1(2) . 3 ? O6 Ge6 O6 110.6(3) 2 . ? O6 Ge6 O6 110.6(3) 2 3 ? O6 Ge6 O6 110.6(3) . 3 ? O2 Si1 O1 106.6(4) . . ? O2 Si1 N1 108.6(5) . . ? O1 Si1 N1 109.6(5) . . ? O2 Si1 C10 110.0(6) . . ? O1 Si1 C10 110.2(6) . . ? N1 Si1 C10 111.8(4) . . ? O3 Si3 O4 105.6(4) . . ? O3 Si3 N2 108.8(5) . . ? O4 Si3 N2 110.2(5) . . ? O3 Si3 C20 109.8(6) . . ? O4 Si3 C20 111.0(6) . . ? N2 Si3 C20 111.2(4) . . ? N2 Si4 C28 110.7(5) . . ? N2 Si4 C29 112.4(5) . . ? C28 Si4 C29 109.7(4) . . ? N2 Si4 C27 109.3(3) . . ? C28 Si4 C27 108.4(6) . . ? C29 Si4 C27 106.2(6) . . ? O5 Si5 O6 107.0(2) . . ? O5 Si5 N3 109.6(4) . . ? O6 Si5 N3 109.8(4) . . ? O5 Si5 C30 109.2(5) . . ? O6 Si5 C30 108.7(5) . . ? N3 Si5 C30 112.4(3) . . ? N3 Si6 C39 109.3(3) . . ? N3 Si6 C37 111.9(5) . . ? C39 Si6 C37 106.6(5) . . ? N3 Si6 C38 110.0(5) . . ? C39 Si6 C38 108.2(5) . . ? C37 Si6 C38 110.7(4) . . ? C11 N1 Si1 118.6(4) . . ? C11 N1 Si2 116.8(6) . . ? Si1 N1 Si2 123.8(5) . . ? C11 N1 Si2A 115.8(8) . . ? Si1 N1 Si2A 125.0(7) . . ? Si2 N1 Si2A 16.2(7) . . ? C21 N2 C21A 18.4(5) . . ? C21 N2 Si3 117.1(6) . . ? C21A N2 Si3 118.3(6) . . ? C21 N2 Si4 116.3(6) . . ? C21A N2 Si4 115.7(6) . . ? Si3 N2 Si4 125.5(4) . . ? C31 N3 Si5 118.8(4) . . ? C31 N3 Si6 115.4(3) . . ? Si5 N3 Si6 125.7(3) . . ? Si1 O1 Ge1 139.4(6) . . ? Si1 O2 Ge2 137.2(5) . . ? Si3 O3 Ge3 137.0(5) . . ? Si3 O4 Ge4 141.1(6) . . ? Si5 O5 Ge5 139.4(5) . . ? Si5 O6 Ge6 138.4(5) . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 120.0 . . ? C12 C11 N1 117.5(7) . . ? C16 C11 N1 122.4(7) . . ? C11 C12 C13 120.0 . . ? C11 C12 C121 123.1(6) . . ? C13 C12 C121 116.9(6) . . ? C12 C13 C14 120.0 . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 C161 117.8(6) . . ? C11 C16 C161 122.2(6) . . ? C12 C121 C122 114.3(9) . . ? C12 C121 C123 113.5(9) . . ? C122 C121 C123 105.3(11) . . ? C12 C121 H12A 107.8 . . ? C122 C121 H12A 107.8 . . ? C123 C121 H12A 107.8 . . ? C121 C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C122 H12D 109.5 . . ? H12B C122 H12D 109.5 . . ? H12C C122 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C121 C123 H12G 109.5 . . ? H12E C123 H12G 109.5 . . ? H12F C123 H12G 109.5 . . ? C16 C161 C163 112.2(9) . . ? C16 C161 C162 113.1(10) . . ? C163 C161 C162 107.2(11) . . ? C16 C161 H16A 108.1 . . ? C163 C161 H16A 108.1 . . ? C162 C161 H16A 108.1 . . ? C161 C162 H16B 109.5 . . ? C161 C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C161 C162 H16D 109.5 . . ? H16B C162 H16D 109.5 . . ? H16C C162 H16D 109.5 . . ? C161 C163 H16E 109.5 . . ? C161 C163 H16F 109.5 . . ? H16E C163 H16F 109.5 . . ? C161 C163 H16G 109.5 . . ? H16E C163 H16G 109.5 . . ? H16F C163 H16G 109.5 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 120.0 . . ? C22 C21 N2 127.9(8) . . ? C26 C21 N2 111.8(8) . . ? C21 C22 C23 120.0 . . ? C21 C22 C221 122.8(8) . . ? C23 C22 C221 117.2(8) . . ? C24 C23 C22 120.0 . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 C261 116.5(9) . . ? C21 C26 C261 123.5(9) . . ? C22 C221 C223 113.5(14) . . ? C22 C221 C222 113.1(14) . . ? C223 C221 C222 105.2(15) . . ? C22 C221 H22A 108.3 . . ? C223 C221 H22A 108.3 . . ? C222 C221 H22A 108.3 . . ? C221 C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C221 C222 H22D 109.5 . . ? H22B C222 H22D 109.5 . . ? H22C C222 H22D 109.5 . . ? C221 C223 H22E 109.5 . . ? C221 C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C221 C223 H22G 109.5 . . ? H22E C223 H22G 109.5 . . ? H22F C223 H22G 109.5 . . ? C26 C261 C262 114.3(14) . . ? C26 C261 C263 113.8(14) . . ? C262 C261 C263 110.9(16) . . ? C26 C261 H26A 105.7 . . ? C262 C261 H26A 105.7 . . ? C263 C261 H26A 105.7 . . ? C261 C262 H26B 109.5 . . ? C261 C262 H26C 109.5 . . ? H26B C262 H26C 109.5 . . ? C261 C262 H26D 109.5 . . ? H26B C262 H26D 109.5 . . ? H26C C262 H26D 109.5 . . ? C261 C263 H26E 109.5 . . ? C261 C263 H26F 109.5 . . ? H26E C263 H26F 109.5 . . ? C261 C263 H26G 109.5 . . ? H26E C263 H26G 109.5 . . ? H26F C263 H26G 109.5 . . ? C22A C21A C26A 120.0 . . ? C22A C21A N2 114.9(9) . . ? C26A C21A N2 125.0(9) . . ? C22F C22A C21A 119.9(11) . . ? C22F C22A C23A 120.0(11) . . ? C21A C22A C23A 120.0 . . ? C22A C23A C24A 120.0 . . ? C22A C23A H23B 120.0 . . ? C24A C23A H23B 120.0 . . ? C25A C24A C23A 120.0 . . ? C25A C24A H24B 120.0 . . ? C23A C24A H24B 120.0 . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25B 120.0 . . ? C26A C25A H25B 120.0 . . ? C25A C26A C21A 120.0 . . ? C25A C26A C26D 114.4(9) . . ? C21A C26A C26D 125.6(9) . . ? C22F C22D H22H 109.5 . . ? C22F C22D H22I 109.5 . . ? H22H C22D H22I 109.5 . . ? C22F C22D H22J 109.5 . . ? H22H C22D H22J 109.5 . . ? H22I C22D H22J 109.5 . . ? C22F C22E H22K 109.5 . . ? C22F C22E H22L 109.5 . . ? H22K C22E H22L 109.5 . . ? C22F C22E H22M 109.5 . . ? H22K C22E H22M 109.5 . . ? H22L C22E H22M 109.5 . . ? C22A C22F C22E 117.2(17) . . ? C22A C22F C22D 114.5(17) . . ? C22E C22F C22D 104.8(18) . . ? C22A C22F H22N 106.5 . . ? C22E C22F H22N 106.5 . . ? C22D C22F H22N 106.5 . . ? C26F C26D C26A 112.5(15) . . ? C26F C26D C26E 105.3(16) . . ? C26A C26D C26E 112.8(14) . . ? C26F C26D H26H 108.7 . . ? C26A C26D H26H 108.7 . . ? C26E C26D H26H 108.7 . . ? C26D C26E H26I 109.5 . . ? C26D C26E H26J 109.5 . . ? H26I C26E H26J 109.5 . . ? C26D C26E H26K 109.5 . . ? H26I C26E H26K 109.5 . . ? H26J C26E H26K 109.5 . . ? C26D C26F H26L 109.5 . . ? C26D C26F H26M 109.5 . . ? H26L C26F H26M 109.5 . . ? C26D C26F H26N 109.5 . . ? H26L C26F H26N 109.5 . . ? H26M C26F H26N 109.5 . . ? Si4 C27 H27A 109.5 . . ? Si4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si4 C29 H29A 109.5 . . ? Si4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si5 C30 H30A 109.5 . . ? Si5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 120.0 . . ? C32 C31 N3 121.7(6) . . ? C36 C31 N3 118.2(6) . . ? C31 C32 C33 120.0 . . ? C31 C32 C321 124.0(6) . . ? C33 C32 C321 116.0(6) . . ? C34 C33 C32 120.0 . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C33 C34 C35 120.0 . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 C361 116.2(5) . . ? C31 C36 C361 123.8(5) . . ? Si6 C37 H37A 109.5 . . ? Si6 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si6 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si6 C38 H38A 109.5 . . ? Si6 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si6 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si6 C39 H39A 109.5 . . ? Si6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C323 C321 C322 112.1(10) . . ? C323 C321 C32 110.3(9) . . ? C322 C321 C32 110.9(8) . . ? C323 C321 H32A 107.8 . . ? C322 C321 H32A 107.8 . . ? C32 C321 H32A 107.8 . . ? C321 C322 H32B 109.5 . . ? C321 C322 H32C 109.5 . . ? H32B C322 H32C 109.5 . . ? C321 C322 H32D 109.5 . . ? H32B C322 H32D 109.5 . . ? H32C C322 H32D 109.5 . . ? C321 C323 H32E 109.5 . . ? C321 C323 H32F 109.5 . . ? H32E C323 H32F 109.5 . . ? C321 C323 H32G 109.5 . . ? H32E C323 H32G 109.5 . . ? H32F C323 H32G 109.5 . . ? C363 C361 C362 109.0(9) . . ? C363 C361 C36 113.0(9) . . ? C362 C361 C36 111.9(9) . . ? C363 C361 H36A 107.6 . . ? C362 C361 H36A 107.6 . . ? C36 C361 H36A 107.6 . . ? C361 C362 H36B 109.5 . . ? C361 C362 H36C 109.5 . . ? H36B C362 H36C 109.5 . . ? C361 C362 H36D 109.5 . . ? H36B C362 H36D 109.5 . . ? H36C C362 H36D 109.5 . . ? C361 C363 H36E 109.5 . . ? C361 C363 H36F 109.5 . . ? H36E C363 H36F 109.5 . . ? C361 C363 H36G 109.5 . . ? H36E C363 H36G 109.5 . . ? H36F C363 H36G 109.5 . . ? N1 Si2 C19 108.0(11) . . ? N1 Si2 C17 110.0(8) . . ? C19 Si2 C17 106.6(11) . . ? N1 Si2 C18 115.6(10) . . ? C19 Si2 C18 106.3(11) . . ? C17 Si2 C18 109.8(11) . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 Si2A C19A 116.4(14) . . ? N1 Si2A C18A 104.7(16) . . ? C19A Si2A C18A 113.5(16) . . ? N1 Si2A C17A 108.6(16) . . ? C19A Si2A C17A 108.3(16) . . ? C18A Si2A C17A 104.6(15) . . ? Si2A C17A H17D 109.5 . . ? Si2A C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? Si2A C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? Si2A C18A H18D 109.5 . . ? Si2A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? Si2A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? Si2A C19A H19D 109.5 . . ? Si2A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? Si2A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.742 _refine_diff_density_min -4.661 _refine_diff_density_rms 0.118 _database_code_depnum_ccdc_archive 'CCDC 941561' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H80 Al2 N2 O6 Si4' _chemical_formula_weight 875.40 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.273(2) _cell_length_b 11.090(2) _cell_length_c 12.605(3) _cell_angle_alpha 97.36(3) _cell_angle_beta 97.64(3) _cell_angle_gamma 114.32(3) _cell_volume 1270.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3916 _cell_measurement_theta_min 6.08 _cell_measurement_theta_max 54.75 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 0.194 _exptl_absorpt_correction_type 'empirical absorption correction' _exptl_absorpt_correction_T_min 0.9441 _exptl_absorpt_correction_T_max 0.9641 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'rigaku raxis rapid IP area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10419 _diffrn_reflns_av_R_equivalents 0.1024 _diffrn_reflns_av_unetI/netI 0.1285 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4893 _reflns_number_gt 2818 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'rapid auto (rigaku 2004)' _computing_cell_refinement 'rapid auto (rigaku 2004)' _computing_data_reduction 'rapid auto (rigaku 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 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^)+(0.0638P)^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 'refined in a riding mode to the carrier atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4893 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1312 _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.1565 _refine_ls_wR_factor_gt 0.1384 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.33542(10) 0.77403(10) 0.42551(7) 0.0318(3) Uani 1 1 d . . . Si2 Si 0.03886(10) 0.61267(11) 0.26554(8) 0.0370(3) Uani 1 1 d . . . Al1 Al 0.67993(11) 0.94733(11) 0.47456(8) 0.0321(3) Uani 1 1 d . . . O1 O 0.5043(2) 0.8300(2) 0.41643(17) 0.0353(6) Uani 1 1 d . . . O2 O 0.2970(2) 0.8923(2) 0.47718(17) 0.0360(6) Uani 1 1 d . . . O3 O 0.7585(2) 0.9735(2) 0.34795(17) 0.0373(6) Uani 1 1 d . . . N1 N 0.2297(3) 0.6977(3) 0.2936(2) 0.0290(7) Uani 1 1 d . . . C1 C 0.7981(4) 0.8811(4) 0.5610(3) 0.0488(11) Uani 1 1 d . . . H1A H 0.7590 0.8585 0.6264 0.073 Uiso 1 1 calc R . . H1B H 0.8990 0.9513 0.5829 0.073 Uiso 1 1 calc R . . H1C H 0.7958 0.8003 0.5173 0.073 Uiso 1 1 calc R . . C2 C 0.2912(4) 0.6447(4) 0.5130(3) 0.0437(10) Uani 1 1 d . . . H2B H 0.3450 0.6878 0.5883 0.066 Uiso 1 1 calc R . . H2C H 0.3194 0.5743 0.4852 0.066 Uiso 1 1 calc R . . H2D H 0.1862 0.6042 0.5116 0.066 Uiso 1 1 calc R . . C3 C -0.0392(4) 0.6312(5) 0.1295(3) 0.0589(13) Uani 1 1 d . . . H3A H -0.0206 0.7257 0.1322 0.088 Uiso 1 1 calc R . . H3B H -0.1446 0.5737 0.1111 0.088 Uiso 1 1 calc R . . H3C H 0.0068 0.6039 0.0737 0.088 Uiso 1 1 calc R . . C4 C -0.0344(4) 0.6811(4) 0.3725(3) 0.0495(11) Uani 1 1 d . . . H4A H 0.0034 0.6686 0.4437 0.074 Uiso 1 1 calc R . . H4B H -0.1412 0.6333 0.3557 0.074 Uiso 1 1 calc R . . H4C H -0.0040 0.7777 0.3744 0.074 Uiso 1 1 calc R . . C5 C -0.0309(4) 0.4277(4) 0.2606(4) 0.0596(12) Uani 1 1 d . . . H5A H 0.0139 0.4125 0.3281 0.089 Uiso 1 1 calc R . . H5B H -0.0061 0.3860 0.1979 0.089 Uiso 1 1 calc R . . H5C H -0.1371 0.3872 0.2532 0.089 Uiso 1 1 calc R . . C6 C 0.7289(4) 0.8609(4) 0.2592(3) 0.0439(10) Uani 1 1 d . . . H6A H 0.6256 0.8196 0.2204 0.053 Uiso 1 1 calc R . . H6B H 0.7509 0.7907 0.2875 0.053 Uiso 1 1 calc R . . C7 C 0.8296(4) 0.9248(4) 0.1848(3) 0.0545(11) Uani 1 1 d . . . H7A H 0.7889 0.8746 0.1082 0.065 Uiso 1 1 calc R . . H7B H 0.9273 0.9285 0.2084 0.065 Uiso 1 1 calc R . . C8 C 0.8371(5) 1.0649(4) 0.1972(3) 0.0614(13) Uani 1 1 d . . . H8A H 0.9273 1.1285 0.1780 0.074 Uiso 1 1 calc R . . H8B H 0.7517 1.0641 0.1497 0.074 Uiso 1 1 calc R . . C9 C 0.8366(4) 1.1040(4) 0.3154(3) 0.0403(9) Uani 1 1 d . . . H9A H 0.9374 1.1534 0.3592 0.048 Uiso 1 1 calc R . . H9B H 0.7849 1.1615 0.3249 0.048 Uiso 1 1 calc R . . C11 C 0.2995(3) 0.7030(4) 0.2007(3) 0.0320(8) Uani 1 1 d . . . C12 C 0.3397(4) 0.6004(4) 0.1644(3) 0.0380(9) Uani 1 1 d . . . C13 C 0.4005(4) 0.6056(4) 0.0710(3) 0.0460(10) Uani 1 1 d . . . H13A H 0.4274 0.5364 0.0458 0.055 Uiso 1 1 calc R . . C14 C 0.4223(4) 0.7086(4) 0.0150(3) 0.0464(10) Uani 1 1 d . . . H14A H 0.4613 0.7093 -0.0493 0.056 Uiso 1 1 calc R . . C15 C 0.3866(4) 0.8113(4) 0.0533(3) 0.0434(10) Uani 1 1 d . . . H15A H 0.4037 0.8835 0.0156 0.052 Uiso 1 1 calc R . . C16 C 0.3265(3) 0.8114(3) 0.1456(3) 0.0327(9) Uani 1 1 d . . . C121 C 0.3250(4) 0.4871(4) 0.2252(3) 0.0413(9) Uani 1 1 d . . . H12A H 0.2631 0.4890 0.2797 0.050 Uiso 1 1 calc R . . C122 C 0.4730(4) 0.5080(4) 0.2884(3) 0.0594(12) Uani 1 1 d . . . H12B H 0.5154 0.5924 0.3432 0.089 Uiso 1 1 calc R . . H12C H 0.5386 0.5129 0.2376 0.089 Uiso 1 1 calc R . . H12D H 0.4599 0.4322 0.3250 0.089 Uiso 1 1 calc R . . C123 C 0.2489(5) 0.3466(4) 0.1495(3) 0.0604(12) Uani 1 1 d . . . H12E H 0.1554 0.3346 0.1077 0.091 Uiso 1 1 calc R . . H12F H 0.2318 0.2769 0.1935 0.091 Uiso 1 1 calc R . . H12G H 0.3112 0.3388 0.0990 0.091 Uiso 1 1 calc R . . C161 C 0.2950(4) 0.9294(3) 0.1862(3) 0.0349(9) Uani 1 1 d . . . H16A H 0.2301 0.9022 0.2399 0.042 Uiso 1 1 calc R . . C162 C 0.4385(4) 1.0532(4) 0.2466(3) 0.0476(10) Uani 1 1 d . . . H16B H 0.4852 1.0288 0.3078 0.071 Uiso 1 1 calc R . . H16C H 0.4165 1.1278 0.2744 0.071 Uiso 1 1 calc R . . H16D H 0.5046 1.0812 0.1958 0.071 Uiso 1 1 calc R . . C163 C 0.2181(4) 0.9719(4) 0.0959(3) 0.0505(11) Uani 1 1 d . . . H16E H 0.1316 0.8926 0.0532 0.076 Uiso 1 1 calc R . . H16F H 0.2850 1.0110 0.0478 0.076 Uiso 1 1 calc R . . H16G H 0.1886 1.0391 0.1288 0.076 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 0.0359(5) 0.0295(6) 0.0287(5) 0.0063(4) 0.0086(4) 0.0123(5) Si2 0.0342(5) 0.0322(6) 0.0383(6) 0.0053(5) 0.0077(4) 0.0089(5) Al1 0.0339(5) 0.0342(7) 0.0292(6) 0.0059(5) 0.0073(4) 0.0156(5) O1 0.0309(12) 0.0342(15) 0.0348(13) 0.0015(11) 0.0064(10) 0.0102(11) O2 0.0437(14) 0.0305(15) 0.0320(13) 0.0000(11) 0.0113(11) 0.0150(12) O3 0.0446(13) 0.0303(15) 0.0315(13) 0.0024(11) 0.0152(11) 0.0100(12) N1 0.0312(14) 0.0250(17) 0.0277(15) 0.0054(12) 0.0072(12) 0.0090(13) C1 0.054(2) 0.062(3) 0.041(2) 0.010(2) 0.0049(19) 0.037(2) C2 0.056(2) 0.038(2) 0.035(2) 0.0146(17) 0.0098(18) 0.017(2) C3 0.045(2) 0.067(3) 0.048(2) 0.013(2) -0.0038(19) 0.012(2) C4 0.037(2) 0.050(3) 0.056(2) 0.004(2) 0.0167(18) 0.015(2) C5 0.044(2) 0.031(3) 0.091(3) 0.007(2) 0.017(2) 0.005(2) C6 0.055(2) 0.034(2) 0.040(2) 0.0002(17) 0.0115(19) 0.019(2) C7 0.059(2) 0.057(3) 0.050(2) 0.008(2) 0.025(2) 0.024(2) C8 0.089(3) 0.047(3) 0.044(2) 0.009(2) 0.027(2) 0.022(3) C9 0.044(2) 0.035(2) 0.043(2) 0.0126(18) 0.0156(18) 0.0142(19) C11 0.0328(18) 0.029(2) 0.0282(18) 0.0002(16) 0.0015(15) 0.0110(17) C12 0.039(2) 0.036(2) 0.035(2) 0.0011(17) 0.0067(17) 0.0141(18) C13 0.049(2) 0.044(3) 0.047(2) -0.005(2) 0.0103(19) 0.025(2) C14 0.049(2) 0.053(3) 0.033(2) 0.002(2) 0.0153(18) 0.018(2) C15 0.050(2) 0.045(3) 0.036(2) 0.0107(18) 0.0122(18) 0.019(2) C16 0.0329(18) 0.028(2) 0.0286(18) 0.0010(16) 0.0036(15) 0.0075(17) C121 0.047(2) 0.032(2) 0.047(2) 0.0049(18) 0.0084(18) 0.0197(19) C122 0.064(3) 0.054(3) 0.072(3) 0.020(2) 0.008(2) 0.036(2) C123 0.068(3) 0.038(3) 0.069(3) 0.002(2) 0.014(2) 0.020(2) C161 0.044(2) 0.029(2) 0.0323(19) 0.0115(16) 0.0108(16) 0.0141(18) C162 0.056(2) 0.036(2) 0.048(2) 0.0093(19) 0.0113(19) 0.017(2) C163 0.057(2) 0.047(3) 0.048(2) 0.016(2) 0.008(2) 0.023(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 O2 1.605(2) . ? Si1 O1 1.611(2) . ? Si1 N1 1.750(3) . ? Si1 C2 1.866(4) . ? Si2 N1 1.751(3) . ? Si2 C4 1.854(4) . ? Si2 C5 1.863(4) . ? Si2 C3 1.867(4) . ? Al1 O2 1.711(3) 2_676 ? Al1 O1 1.719(2) . ? Al1 O3 1.884(2) . ? Al1 C1 1.947(4) . ? O2 Al1 1.711(3) 2_676 ? O3 C6 1.464(4) . ? O3 C9 1.479(4) . ? N1 C11 1.448(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.509(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.511(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.500(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.406(5) . ? C11 C16 1.412(5) . ? C12 C13 1.400(5) . ? C12 C121 1.519(5) . ? C13 C14 1.375(5) . ? C13 H13A 0.9500 . ? C14 C15 1.383(5) . ? C14 H14A 0.9500 . ? C15 C16 1.388(5) . ? C15 H15A 0.9500 . ? C16 C161 1.518(5) . ? C121 C122 1.531(5) . ? C121 C123 1.539(5) . ? C121 H12A 1.0000 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C122 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C123 H12G 0.9800 . ? C161 C163 1.532(5) . ? C161 C162 1.551(4) . ? C161 H16A 1.0000 . ? C162 H16B 0.9800 . ? C162 H16C 0.9800 . ? C162 H16D 0.9800 . ? C163 H16E 0.9800 . ? C163 H16F 0.9800 . ? C163 H16G 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 O2 Si1 O1 112.08(13) . . ? O2 Si1 N1 109.95(13) . . ? O1 Si1 N1 107.57(13) . . ? O2 Si1 C2 108.28(16) . . ? O1 Si1 C2 110.09(16) . . ? N1 Si1 C2 108.83(15) . . ? N1 Si2 C4 110.11(15) . . ? N1 Si2 C5 113.03(16) . . ? C4 Si2 C5 107.4(2) . . ? N1 Si2 C3 110.72(16) . . ? C4 Si2 C3 109.1(2) . . ? C5 Si2 C3 106.3(2) . . ? O2 Al1 O1 116.31(13) 2_676 . ? O2 Al1 O3 99.94(12) 2_676 . ? O1 Al1 O3 99.94(11) . . ? O2 Al1 C1 116.69(15) 2_676 . ? O1 Al1 C1 115.40(16) . . ? O3 Al1 C1 104.59(15) . . ? Si1 O1 Al1 145.51(15) . . ? Si1 O2 Al1 158.62(16) . 2_676 ? C6 O3 C9 110.4(3) . . ? C6 O3 Al1 122.2(2) . . ? C9 O3 Al1 126.8(2) . . ? C11 N1 Si1 120.09(19) . . ? C11 N1 Si2 116.50(19) . . ? Si1 N1 Si2 123.41(16) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C2 H2D 109.5 . . ? H2B C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? Si2 C3 H3A 109.5 . . ? Si2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 C7 104.1(3) . . ? O3 C6 H6A 110.9 . . ? C7 C6 H6A 110.9 . . ? O3 C6 H6B 110.9 . . ? C7 C6 H6B 110.9 . . ? H6A C6 H6B 108.9 . . ? C6 C7 C8 102.9(3) . . ? C6 C7 H7A 111.2 . . ? C8 C7 H7A 111.2 . . ? C6 C7 H7B 111.2 . . ? C8 C7 H7B 111.2 . . ? H7A C7 H7B 109.1 . . ? C9 C8 C7 104.7(3) . . ? C9 C8 H8A 110.8 . . ? C7 C8 H8A 110.8 . . ? C9 C8 H8B 110.8 . . ? C7 C8 H8B 110.8 . . ? H8A C8 H8B 108.9 . . ? O3 C9 C8 104.1(3) . . ? O3 C9 H9A 110.9 . . ? C8 C9 H9A 110.9 . . ? O3 C9 H9B 110.9 . . ? C8 C9 H9B 110.9 . . ? H9A C9 H9B 109.0 . . ? C12 C11 C16 119.8(3) . . ? C12 C11 N1 120.5(3) . . ? C16 C11 N1 119.8(3) . . ? C13 C12 C11 118.8(4) . . ? C13 C12 C121 118.8(3) . . ? C11 C12 C121 122.4(3) . . ? C14 C13 C12 121.6(4) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C13 C14 C15 119.2(4) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? C14 C15 C16 121.6(4) . . ? C14 C15 H15A 119.2 . . ? C16 C15 H15A 119.2 . . ? C15 C16 C11 119.0(3) . . ? C15 C16 C161 119.2(3) . . ? C11 C16 C161 121.8(3) . . ? C12 C121 C122 111.6(3) . . ? C12 C121 C123 112.7(3) . . ? C122 C121 C123 109.7(3) . . ? C12 C121 H12A 107.5 . . ? C122 C121 H12A 107.5 . . ? C123 C121 H12A 107.5 . . ? C121 C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C122 H12D 109.5 . . ? H12B C122 H12D 109.5 . . ? H12C C122 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C121 C123 H12G 109.5 . . ? H12E C123 H12G 109.5 . . ? H12F C123 H12G 109.5 . . ? C16 C161 C163 113.9(3) . . ? C16 C161 C162 110.2(3) . . ? C163 C161 C162 108.8(3) . . ? C16 C161 H16A 107.9 . . ? C163 C161 H16A 107.9 . . ? C162 C161 H16A 107.9 . . ? C161 C162 H16B 109.5 . . ? C161 C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C161 C162 H16D 109.5 . . ? H16B C162 H16D 109.5 . . ? H16C C162 H16D 109.5 . . ? C161 C163 H16E 109.5 . . ? C161 C163 H16F 109.5 . . ? H16E C163 H16F 109.5 . . ? C161 C163 H16G 109.5 . . ? H16E C163 H16G 109.5 . . ? H16F C163 H16G 109.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.347 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.065 _database_code_depnum_ccdc_archive 'CCDC 941562' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H119 Bi4 N4 O12 Si8' _chemical_formula_weight 2269.33 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 '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)/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 15.5155(5) _cell_length_b 21.6905(6) _cell_length_c 27.1120(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.249(3) _cell_angle_gamma 90.00 _cell_volume 9117.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7225 _cell_measurement_theta_min 2.6991 _cell_measurement_theta_max 29.0251 _exptl_crystal_description stick _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4428 _exptl_absorpt_coefficient_mu 7.854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3026 _exptl_absorpt_correction_T_max 0.6948 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhanced (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.1903 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65416 _diffrn_reflns_av_R_equivalents 0.1286 _diffrn_reflns_av_unetI/netI 0.1347 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 26.00 _reflns_number_total 17902 _reflns_number_gt 11664 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrysAlisPro _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 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. One toluene molecule is disordered, treated in a splittling mode, and refined in PARTs. The constraints by SIMU combined with DELU are applied for the atoms of C11, C12, C13, C14, C15, C16, C1, C2, C3, C4, C5, C6, C7, C1A, C2A, C3A, C4A, C5A, C6A, and C7A. The restraint by DFIX is used for the bonds of C1-C7 and C1A-C7A and the bonds within the hexane molecule of C51C52C53C54C55C56. ; _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^)+(0.0205P)^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 'refined in a riding mode to the carrier atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17902 _refine_ls_number_parameters 900 _refine_ls_number_restraints 391 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.012 _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 Bi1 Bi 0.44347(3) 0.677454(19) 0.841527(16) 0.02199(11) Uani 1 1 d . . . Bi2 Bi 0.13176(3) 0.70001(2) 0.792243(15) 0.02130(11) Uani 1 1 d . . . Bi3 Bi 0.23655(3) 0.771145(19) 0.959058(15) 0.02038(11) Uani 1 1 d . . . Bi4 Bi 0.32392(3) 0.896601(19) 0.804806(16) 0.02372(11) Uani 1 1 d . . . Si1 Si 0.2484(2) 0.63756(14) 0.89075(11) 0.0209(7) Uani 1 1 d . . . Si2 Si 0.1426(2) 0.83276(14) 0.85084(11) 0.0207(7) Uani 1 1 d . . . Si3 Si 0.4107(2) 0.81581(14) 0.90349(11) 0.0212(7) Uani 1 1 d . . . Si4 Si 0.3328(2) 0.75153(14) 0.75451(11) 0.0196(7) Uani 1 1 d . . . Si11 Si 0.2073(2) 0.55045(16) 0.97675(12) 0.0337(9) Uani 1 1 d . . . Si21 Si -0.0034(2) 0.92822(17) 0.85361(13) 0.0341(9) Uani 1 1 d . . . Si31 Si 0.5593(2) 0.88194(16) 0.95979(14) 0.0347(9) Uani 1 1 d . . . Si41 Si 0.3797(2) 0.75444(16) 0.64562(12) 0.0323(9) Uani 1 1 d . . . O11 O 0.1648(4) 0.6584(3) 0.8580(3) 0.0279(19) Uani 1 1 d . . . O12 O 0.2652(4) 0.6829(3) 0.9385(2) 0.0218(18) Uani 1 1 d . . . O13 O 0.3308(5) 0.6325(3) 0.8566(2) 0.0254(19) Uani 1 1 d . . . O21 O 0.1969(5) 0.8759(3) 0.8139(2) 0.0228(18) Uani 1 1 d . . . O22 O 0.0860(4) 0.7809(3) 0.8202(3) 0.0236(18) Uani 1 1 d . . . O23 O 0.2075(4) 0.7988(3) 0.8892(2) 0.0210(17) Uani 1 1 d . . . O31 O 0.3767(5) 0.8766(3) 0.8741(3) 0.0283(19) Uani 1 1 d . . . O32 O 0.3584(4) 0.8061(3) 0.9538(2) 0.0202(17) Uani 1 1 d . . . O33 O 0.3980(4) 0.7576(3) 0.8672(2) 0.0219(18) Uani 1 1 d . . . O41 O 0.4091(4) 0.7040(3) 0.7710(2) 0.0264(19) Uani 1 1 d . . . O42 O 0.2489(5) 0.7384(3) 0.7853(2) 0.0247(18) Uani 1 1 d . . . O43 O 0.3620(5) 0.8223(3) 0.7629(2) 0.0247(18) Uani 1 1 d . . . N1 N 0.2305(6) 0.5645(4) 0.9154(3) 0.025(2) Uani 1 1 d . . . N2 N 0.0711(6) 0.8795(4) 0.8823(3) 0.025(2) Uani 1 1 d . . . N3 N 0.5206(6) 0.8241(4) 0.9199(3) 0.027(2) Uani 1 1 d . . . N4 N 0.3075(6) 0.7390(4) 0.6913(3) 0.019(2) Uani 1 1 d . . . C11 C 0.2328(7) 0.5145(3) 0.8819(3) 0.053(2) Uani 1 1 d GU . . C12 C 0.3103(6) 0.4844(4) 0.8746(3) 0.058(2) Uani 1 1 d GU . . C13 C 0.3128(6) 0.4344(4) 0.8426(3) 0.062(3) Uani 1 1 d GU . . H13A H 0.3658 0.4138 0.8377 0.074 Uiso 1 1 calc R . . C14 C 0.2377(7) 0.4146(3) 0.8178(3) 0.065(3) Uani 1 1 d GU . . H14A H 0.2394 0.3804 0.7960 0.078 Uiso 1 1 calc R . . C15 C 0.1602(6) 0.4447(4) 0.8251(3) 0.062(3) Uani 1 1 d GU . . H15A H 0.1088 0.4312 0.8081 0.074 Uiso 1 1 calc R . . C16 C 0.1577(6) 0.4947(4) 0.8571(3) 0.055(2) Uani 1 1 d GU . . C17 C 0.1899(9) 0.4669(5) 0.9866(4) 0.049(4) Uani 1 1 d . . . H17A H 0.1308 0.4560 0.9759 0.074 Uiso 1 1 calc R . . H17B H 0.1989 0.4572 1.0218 0.074 Uiso 1 1 calc R . . H17C H 0.2307 0.4432 0.9675 0.074 Uiso 1 1 calc R . . C18 C 0.1076(8) 0.5914(6) 0.9933(4) 0.046(4) Uani 1 1 d . . . H18A H 0.1162 0.6360 0.9903 0.068 Uiso 1 1 calc R . . H18B H 0.0941 0.5814 1.0274 0.068 Uiso 1 1 calc R . . H18C H 0.0597 0.5785 0.9711 0.068 Uiso 1 1 calc R . . C19 C 0.2970(8) 0.5743(6) 1.0208(4) 0.045(4) Uani 1 1 d . . . H19A H 0.3123 0.6174 1.0145 0.068 Uiso 1 1 calc R . . H19B H 0.3473 0.5480 1.0161 0.068 Uiso 1 1 calc R . . H19C H 0.2783 0.5701 1.0547 0.068 Uiso 1 1 calc R . . C21 C 0.0738(5) 0.8713(4) 0.9357(2) 0.031(3) Uani 1 1 d G . . C22 C 0.0263(5) 0.8243(4) 0.9565(3) 0.039(3) Uani 1 1 d G . . C23 C 0.0325(6) 0.8142(4) 1.0072(3) 0.052(4) Uani 1 1 d G . . H23A H 0.0001 0.7821 1.0214 0.062 Uiso 1 1 calc R . . C24 C 0.0862(6) 0.8510(5) 1.0370(2) 0.066(5) Uani 1 1 d G . . H24A H 0.0904 0.8441 1.0716 0.079 Uiso 1 1 calc R . . C25 C 0.1336(5) 0.8980(4) 1.0162(3) 0.048(4) Uani 1 1 d G . . H25A H 0.1703 0.9232 1.0366 0.057 Uiso 1 1 calc R . . C26 C 0.1274(5) 0.9082(3) 0.9656(3) 0.035(3) Uani 1 1 d G . . C27 C -0.0786(8) 0.9596(6) 0.8991(5) 0.051(4) Uani 1 1 d . . . H27A H -0.0455 0.9748 0.9281 0.076 Uiso 1 1 calc R . . H27B H -0.1180 0.9270 0.9091 0.076 Uiso 1 1 calc R . . H27C H -0.1119 0.9936 0.8840 0.076 Uiso 1 1 calc R . . C28 C -0.0649(8) 0.8873(7) 0.8053(5) 0.059(5) Uani 1 1 d . . . H28A H -0.0252 0.8692 0.7820 0.088 Uiso 1 1 calc R . . H28B H -0.1037 0.9162 0.7877 0.088 Uiso 1 1 calc R . . H28C H -0.0988 0.8545 0.8201 0.088 Uiso 1 1 calc R . . C29 C 0.0528(8) 0.9925(6) 0.8233(5) 0.055(4) Uani 1 1 d . . . H29A H 0.1031 0.9764 0.8067 0.082 Uiso 1 1 calc R . . H29B H 0.0718 1.0228 0.8483 0.082 Uiso 1 1 calc R . . H29C H 0.0134 1.0122 0.7990 0.082 Uiso 1 1 calc R . . C31 C 0.5754(4) 0.7764(3) 0.9037(3) 0.028(3) Uani 1 1 d G . . C32 C 0.5907(5) 0.7242(4) 0.9324(2) 0.033(3) Uani 1 1 d G . . C33 C 0.6433(5) 0.6774(3) 0.9155(3) 0.042(4) Uani 1 1 d G . . H33A H 0.6538 0.6417 0.9351 0.051 Uiso 1 1 calc R . . C34 C 0.6807(5) 0.6830(3) 0.8699(3) 0.059(5) Uani 1 1 d G . . H34A H 0.7166 0.6510 0.8584 0.070 Uiso 1 1 calc R . . C35 C 0.6653(5) 0.7352(4) 0.8412(3) 0.041(3) Uani 1 1 d G . . H35A H 0.6908 0.7390 0.8101 0.049 Uiso 1 1 calc R . . C36 C 0.6127(5) 0.7819(3) 0.8581(3) 0.034(3) Uani 1 1 d G . . C37 C 0.6750(8) 0.8715(6) 0.9700(5) 0.064(5) Uani 1 1 d . . . H37A H 0.7046 0.8830 0.9401 0.097 Uiso 1 1 calc R . . H37B H 0.6872 0.8282 0.9780 0.097 Uiso 1 1 calc R . . H37C H 0.6956 0.8977 0.9975 0.097 Uiso 1 1 calc R . . C38 C 0.5083(9) 0.8801(7) 1.0203(5) 0.064(5) Uani 1 1 d . . . H38A H 0.4454 0.8819 1.0153 0.097 Uiso 1 1 calc R . . H38B H 0.5280 0.9156 1.0401 0.097 Uiso 1 1 calc R . . H38C H 0.5244 0.8419 1.0377 0.097 Uiso 1 1 calc R . . C39 C 0.5345(9) 0.9572(6) 0.9326(5) 0.063(5) Uani 1 1 d . . . H39A H 0.5638 0.9614 0.9014 0.095 Uiso 1 1 calc R . . H39B H 0.5543 0.9898 0.9554 0.095 Uiso 1 1 calc R . . H39C H 0.4720 0.9609 0.9264 0.095 Uiso 1 1 calc R . . C41 C 0.2259(4) 0.7088(3) 0.6811(2) 0.020(3) Uani 1 1 d G . . C42 C 0.1529(5) 0.7446(2) 0.6713(3) 0.024(3) Uani 1 1 d G . . C43 C 0.0726(4) 0.7167(3) 0.6650(2) 0.031(3) Uani 1 1 d G . . H43A H 0.0227 0.7411 0.6582 0.037 Uiso 1 1 calc R . . C44 C 0.0652(4) 0.6530(3) 0.6685(3) 0.033(3) Uani 1 1 d G . . H44A H 0.0103 0.6339 0.6642 0.040 Uiso 1 1 calc R . . C45 C 0.1382(5) 0.6172(2) 0.6783(3) 0.038(3) Uani 1 1 d G . . H45A H 0.1332 0.5736 0.6807 0.045 Uiso 1 1 calc R . . C46 C 0.2185(4) 0.6451(3) 0.6846(2) 0.024(3) Uani 1 1 d G . . C47 C 0.4075(9) 0.8379(6) 0.6450(5) 0.062(5) Uani 1 1 d . . . H47A H 0.3559 0.8620 0.6357 0.094 Uiso 1 1 calc R . . H47B H 0.4520 0.8452 0.6209 0.094 Uiso 1 1 calc R . . H47C H 0.4293 0.8505 0.6779 0.094 Uiso 1 1 calc R . . C48 C 0.4834(8) 0.7110(7) 0.6561(5) 0.063(5) Uani 1 1 d . . . H48A H 0.4724 0.6667 0.6527 0.095 Uiso 1 1 calc R . . H48B H 0.5073 0.7198 0.6893 0.095 Uiso 1 1 calc R . . H48C H 0.5247 0.7239 0.6316 0.095 Uiso 1 1 calc R . . C49 C 0.3307(8) 0.7341(6) 0.5847(4) 0.041(3) Uani 1 1 d . . . H49A H 0.2731 0.7525 0.5811 0.061 Uiso 1 1 calc R . . H49B H 0.3260 0.6891 0.5820 0.061 Uiso 1 1 calc R . . H49C H 0.3669 0.7498 0.5587 0.061 Uiso 1 1 calc R . . C121 C 0.3947(10) 0.5005(6) 0.8993(6) 0.058(4) Uani 1 1 d . . . H12A H 0.3857 0.5412 0.9157 0.070 Uiso 1 1 calc R . . C122 C 0.4263(10) 0.4568(6) 0.9402(6) 0.076(5) Uani 1 1 d . . . H12B H 0.4781 0.4740 0.9569 0.114 Uiso 1 1 calc R . . H12C H 0.4401 0.4167 0.9259 0.114 Uiso 1 1 calc R . . H12D H 0.3811 0.4516 0.9641 0.114 Uiso 1 1 calc R . . C123 C 0.4675(10) 0.5103(7) 0.8645(6) 0.075(5) Uani 1 1 d . . . H12E H 0.4519 0.5434 0.8412 0.112 Uiso 1 1 calc R . . H12F H 0.4776 0.4722 0.8463 0.112 Uiso 1 1 calc R . . H12G H 0.5201 0.5218 0.8836 0.112 Uiso 1 1 calc R . . C161 C 0.0709(9) 0.5250(7) 0.8620(5) 0.056(4) Uani 1 1 d . . . H16A H 0.0803 0.5639 0.8813 0.068 Uiso 1 1 calc R . . C162 C 0.0068(9) 0.4856(7) 0.8892(5) 0.076(6) Uani 1 1 d . . . H16B H 0.0351 0.4686 0.9192 0.114 Uiso 1 1 calc R . . H16C H -0.0137 0.4519 0.8678 0.114 Uiso 1 1 calc R . . H16D H -0.0423 0.5111 0.8983 0.114 Uiso 1 1 calc R . . C163 C 0.0325(10) 0.5433(7) 0.8105(5) 0.069(5) Uani 1 1 d . . . H16E H -0.0191 0.5686 0.8144 0.104 Uiso 1 1 calc R . . H16F H 0.0170 0.5059 0.7918 0.104 Uiso 1 1 calc R . . H16G H 0.0753 0.5668 0.7927 0.104 Uiso 1 1 calc R . . C221 C -0.0359(7) 0.7831(6) 0.9268(5) 0.043(4) Uani 1 1 d . . . H22A H -0.0327 0.7964 0.8915 0.052 Uiso 1 1 calc R . . C222 C -0.1287(9) 0.7907(8) 0.9403(6) 0.087(6) Uani 1 1 d . . . H22B H -0.1397 0.8340 0.9482 0.130 Uiso 1 1 calc R . . H22C H -0.1400 0.7649 0.9691 0.130 Uiso 1 1 calc R . . H22D H -0.1668 0.7780 0.9124 0.130 Uiso 1 1 calc R . . C223 C -0.0123(8) 0.7151(6) 0.9282(5) 0.054(4) Uani 1 1 d . . . H22E H -0.0510 0.6923 0.9054 0.081 Uiso 1 1 calc R . . H22F H -0.0182 0.6993 0.9618 0.081 Uiso 1 1 calc R . . H22G H 0.0474 0.7099 0.9185 0.081 Uiso 1 1 calc R . . C261 C 0.1787(9) 0.9599(6) 0.9442(5) 0.052(4) Uani 1 1 d . . . H26A H 0.1782 0.9549 0.9076 0.063 Uiso 1 1 calc R . . C262 C 0.1374(9) 1.0230(6) 0.9561(6) 0.066(5) Uani 1 1 d . . . H26B H 0.0786 1.0246 0.9415 0.098 Uiso 1 1 calc R . . H26C H 0.1718 1.0562 0.9422 0.098 Uiso 1 1 calc R . . H26D H 0.1357 1.0281 0.9919 0.098 Uiso 1 1 calc R . . C263 C 0.2726(8) 0.9622(6) 0.9636(5) 0.056(4) Uani 1 1 d . . . H26E H 0.3017 0.9238 0.9550 0.085 Uiso 1 1 calc R . . H26F H 0.2743 0.9671 0.9995 0.085 Uiso 1 1 calc R . . H26G H 0.3018 0.9971 0.9486 0.085 Uiso 1 1 calc R . . C321 C 0.5511(8) 0.7151(6) 0.9812(5) 0.043(4) Uani 1 1 d . . . H32A H 0.5182 0.7537 0.9880 0.051 Uiso 1 1 calc R . . C322 C 0.6186(9) 0.7084(6) 1.0234(5) 0.064(5) Uani 1 1 d . . . H32B H 0.6584 0.7435 1.0231 0.097 Uiso 1 1 calc R . . H32C H 0.6508 0.6700 1.0193 0.097 Uiso 1 1 calc R . . H32D H 0.5898 0.7075 1.0550 0.097 Uiso 1 1 calc R . . C323 C 0.4858(8) 0.6620(5) 0.9821(5) 0.045(4) Uani 1 1 d . . . H32E H 0.4400 0.6690 0.9568 0.067 Uiso 1 1 calc R . . H32F H 0.4606 0.6600 1.0147 0.067 Uiso 1 1 calc R . . H32G H 0.5151 0.6230 0.9755 0.067 Uiso 1 1 calc R . . C361 C 0.6031(8) 0.8368(6) 0.8258(5) 0.043(4) Uani 1 1 d . . . H36A H 0.5552 0.8619 0.8391 0.052 Uiso 1 1 calc R . . C362 C 0.6821(10) 0.8773(7) 0.8277(5) 0.072(5) Uani 1 1 d . . . H36B H 0.6943 0.8907 0.8618 0.108 Uiso 1 1 calc R . . H36C H 0.6718 0.9134 0.8066 0.108 Uiso 1 1 calc R . . H36D H 0.7314 0.8540 0.8160 0.108 Uiso 1 1 calc R . . C363 C 0.5784(8) 0.8238(7) 0.7716(5) 0.057(4) Uani 1 1 d . . . H36E H 0.5255 0.7991 0.7695 0.086 Uiso 1 1 calc R . . H36F H 0.6251 0.8012 0.7564 0.086 Uiso 1 1 calc R . . H36G H 0.5687 0.8629 0.7541 0.086 Uiso 1 1 calc R . . C421 C 0.1563(8) 0.8142(6) 0.6661(5) 0.041(4) Uani 1 1 d . . . H42A H 0.2169 0.8276 0.6744 0.050 Uiso 1 1 calc R . . C422 C 0.1339(10) 0.8342(7) 0.6129(5) 0.074(6) Uani 1 1 d . . . H42B H 0.1361 0.8792 0.6107 0.111 Uiso 1 1 calc R . . H42C H 0.0758 0.8198 0.6033 0.111 Uiso 1 1 calc R . . H42D H 0.1756 0.8162 0.5908 0.111 Uiso 1 1 calc R . . C423 C 0.0977(9) 0.8478(6) 0.7002(4) 0.048(4) Uani 1 1 d . . . H42E H 0.1121 0.8360 0.7344 0.072 Uiso 1 1 calc R . . H42F H 0.0376 0.8369 0.6919 0.072 Uiso 1 1 calc R . . H42G H 0.1054 0.8924 0.6964 0.072 Uiso 1 1 calc R . . C461 C 0.2970(8) 0.6031(5) 0.6942(4) 0.037(3) Uani 1 1 d . . . H46A H 0.3483 0.6299 0.7016 0.045 Uiso 1 1 calc R . . C462 C 0.3145(9) 0.5654(6) 0.6476(5) 0.054(4) Uani 1 1 d . . . H46B H 0.3148 0.5930 0.6189 0.081 Uiso 1 1 calc R . . H46C H 0.2691 0.5344 0.6424 0.081 Uiso 1 1 calc R . . H46D H 0.3706 0.5450 0.6516 0.081 Uiso 1 1 calc R . . C463 C 0.2841(9) 0.5621(5) 0.7386(4) 0.046(4) Uani 1 1 d . . . H46E H 0.2761 0.5877 0.7678 0.069 Uiso 1 1 calc R . . H46F H 0.3348 0.5357 0.7441 0.069 Uiso 1 1 calc R . . H46G H 0.2329 0.5362 0.7325 0.069 Uiso 1 1 calc R . . C51 C -0.1197(14) 0.7028(10) 0.7721(8) 0.030(6) Uiso 0.50 1 d PD . . H51A H -0.1098 0.7346 0.7973 0.045 Uiso 0.50 1 calc PR . . H51B H -0.0642 0.6858 0.7626 0.045 Uiso 0.50 1 calc PR . . H51C H -0.1553 0.6699 0.7853 0.045 Uiso 0.50 1 calc PR . . C52 C -0.161(2) 0.7281(15) 0.7319(11) 0.085(11) Uiso 0.50 1 d PD . . H52A H -0.2139 0.7436 0.7468 0.102 Uiso 0.50 1 calc PR . . H52B H -0.1254 0.7654 0.7274 0.102 Uiso 0.50 1 calc PR . . C53 C -0.189(2) 0.7190(14) 0.6873(11) 0.076(10) Uiso 0.50 1 d PD . . H53A H -0.2265 0.6829 0.6927 0.091 Uiso 0.50 1 calc PR . . H53B H -0.1364 0.7011 0.6735 0.091 Uiso 0.50 1 calc PR . . C54 C -0.228(2) 0.7415(14) 0.6450(11) 0.070(10) Uiso 0.50 1 d PD . . H54A H -0.2785 0.7153 0.6370 0.084 Uiso 0.50 1 calc PR . . H54B H -0.2495 0.7832 0.6524 0.084 Uiso 0.50 1 calc PR . . C55 C -0.181(2) 0.7457(16) 0.6034(13) 0.106(14) Uiso 0.50 1 d PD . . H55A H -0.2168 0.7259 0.5768 0.127 Uiso 0.50 1 calc PR . . H55B H -0.1303 0.7186 0.6092 0.127 Uiso 0.50 1 calc PR . . C56 C -0.150(2) 0.7989(15) 0.5833(13) 0.097(12) Uiso 0.50 1 d PD . . H56A H -0.1075 0.7885 0.5588 0.145 Uiso 0.50 1 calc PR . . H56B H -0.1224 0.8242 0.6094 0.145 Uiso 0.50 1 calc PR . . H56C H -0.1976 0.8220 0.5673 0.145 Uiso 0.50 1 calc PR . . C1 C 0.2971(15) 1.0297(13) 0.7348(11) 0.114(9) Uani 0.55(3) 1 d PGDU A 2 C2 C 0.3820(18) 1.0146(12) 0.7255(9) 0.114(9) Uani 0.55(3) 1 d PGU A 2 H2A H 0.3960 0.9985 0.6942 0.137 Uiso 0.55(3) 1 calc PR A 2 C3 C 0.4464(12) 1.0229(11) 0.7620(12) 0.113(9) Uani 0.55(3) 1 d PGU A 2 H3A H 0.5044 1.0126 0.7556 0.136 Uiso 0.55(3) 1 calc PR A 2 C4 C 0.4258(16) 1.0464(12) 0.8078(10) 0.113(9) Uani 0.55(3) 1 d PGU A 2 H4A H 0.4698 1.0521 0.8327 0.136 Uiso 0.55(3) 1 calc PR A 2 C5 C 0.3409(19) 1.0615(13) 0.8170(9) 0.114(9) Uani 0.55(3) 1 d PGU A 2 H5A H 0.3269 1.0775 0.8483 0.137 Uiso 0.55(3) 1 calc PR A 2 C6 C 0.2765(12) 1.0531(13) 0.7805(12) 0.113(9) Uani 0.55(3) 1 d PGU A 2 H6A H 0.2185 1.0635 0.7869 0.136 Uiso 0.55(3) 1 calc PR A 2 C7 C 0.221(2) 1.0200(15) 0.7003(16) 0.115(9) Uani 0.55(3) 1 d PDU A 2 H7AA H 0.2401 1.0157 0.6665 0.173 Uiso 0.55(3) 1 calc PR A 2 H7AB H 0.1818 1.0554 0.7021 0.173 Uiso 0.55(3) 1 calc PR A 2 H7AC H 0.1902 0.9825 0.7097 0.173 Uiso 0.55(3) 1 calc PR A 2 C1A C 0.304(2) 1.0320(16) 0.7273(10) 0.101(9) Uani 0.45(3) 1 d PGDU A 1 C2A C 0.392(2) 1.0389(15) 0.7379(11) 0.101(9) Uani 0.45(3) 1 d PGU A 1 H2AA H 0.4318 1.0348 0.7123 0.121 Uiso 0.45(3) 1 calc PR A 1 C3A C 0.4216(16) 1.0518(16) 0.7858(13) 0.101(9) Uani 0.45(3) 1 d PGU A 1 H3AA H 0.4817 1.0566 0.7930 0.121 Uiso 0.45(3) 1 calc PR A 1 C4A C 0.363(2) 1.0578(16) 0.8232(9) 0.101(9) Uani 0.45(3) 1 d PGU A 1 H4AA H 0.3837 1.0666 0.8559 0.121 Uiso 0.45(3) 1 calc PR A 1 C5A C 0.276(2) 1.0509(16) 0.8126(11) 0.101(9) Uani 0.45(3) 1 d PGU A 1 H5AA H 0.2358 1.0549 0.8382 0.121 Uiso 0.45(3) 1 calc PR A 1 C6A C 0.2459(16) 1.0380(16) 0.7647(13) 0.101(9) Uani 0.45(3) 1 d PGU A 1 H6AA H 0.1859 1.0332 0.7575 0.121 Uiso 0.45(3) 1 calc PR A 1 C7A C 0.276(3) 1.0034(19) 0.6750(13) 0.102(9) Uani 0.45(3) 1 d PDU A 1 H7A H 0.3275 0.9866 0.6595 0.152 Uiso 0.45(3) 1 calc PR A 1 H7B H 0.2505 1.0356 0.6539 0.152 Uiso 0.45(3) 1 calc PR A 1 H7C H 0.2345 0.9703 0.6795 0.152 Uiso 0.45(3) 1 calc PR A 1 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 Bi1 0.0215(2) 0.0217(2) 0.0227(2) -0.0004(2) 0.00045(19) 0.00394(19) Bi2 0.0231(2) 0.0243(2) 0.0163(2) -0.00066(19) -0.00182(19) -0.00200(19) Bi3 0.0218(2) 0.0242(2) 0.0151(2) -0.00120(19) 0.00025(18) 0.00139(19) Bi4 0.0296(3) 0.0182(2) 0.0235(2) 0.0012(2) 0.0028(2) 0.0005(2) Si1 0.0257(19) 0.0186(18) 0.0186(17) 0.0012(14) 0.0019(15) -0.0013(14) Si2 0.0211(18) 0.0253(18) 0.0156(17) 0.0005(14) -0.0007(14) 0.0031(14) Si3 0.0194(18) 0.0196(18) 0.0244(18) -0.0021(14) -0.0021(14) -0.0001(13) Si4 0.0212(18) 0.0188(17) 0.0188(17) -0.0021(14) 0.0019(14) 0.0015(13) Si11 0.049(2) 0.032(2) 0.0199(19) 0.0064(16) 0.0021(17) -0.0059(17) Si21 0.033(2) 0.042(2) 0.028(2) 0.0021(17) -0.0001(17) 0.0219(17) Si31 0.028(2) 0.026(2) 0.049(2) -0.0150(18) -0.0041(18) -0.0013(15) Si41 0.033(2) 0.044(2) 0.0203(18) 0.0027(17) 0.0054(16) -0.0037(17) O11 0.023(5) 0.030(5) 0.031(5) -0.001(4) -0.005(4) -0.006(3) O12 0.024(4) 0.031(5) 0.010(4) 0.003(3) 0.003(3) 0.001(3) O13 0.037(5) 0.021(4) 0.018(4) -0.004(3) 0.000(4) 0.002(4) O21 0.031(5) 0.023(4) 0.014(4) 0.004(3) 0.005(4) 0.014(3) O22 0.016(4) 0.027(5) 0.029(4) 0.004(4) 0.006(4) 0.005(3) O23 0.028(4) 0.020(4) 0.015(4) -0.001(3) -0.001(3) 0.012(3) O31 0.034(5) 0.019(4) 0.031(5) -0.009(4) -0.001(4) 0.000(4) O32 0.025(4) 0.022(4) 0.013(4) -0.007(3) -0.002(3) 0.000(3) O33 0.021(4) 0.021(4) 0.024(4) -0.004(3) 0.004(4) 0.006(3) O41 0.026(5) 0.034(5) 0.019(4) -0.004(4) 0.002(4) 0.009(4) O42 0.034(5) 0.028(5) 0.011(4) -0.001(3) 0.000(4) -0.002(4) O43 0.030(5) 0.024(4) 0.021(4) 0.006(4) 0.003(4) -0.007(4) N1 0.035(6) 0.022(5) 0.018(5) -0.006(4) 0.001(5) 0.008(4) N2 0.032(6) 0.030(6) 0.013(5) 0.014(4) 0.003(4) 0.000(4) N3 0.025(6) 0.016(5) 0.040(6) -0.004(5) -0.009(5) 0.003(4) N4 0.032(6) 0.009(5) 0.018(5) 0.006(4) 0.006(4) 0.000(4) C11 0.102(7) 0.024(5) 0.034(5) -0.004(4) 0.019(5) -0.010(4) C12 0.106(7) 0.031(5) 0.040(5) -0.006(4) 0.019(5) -0.007(5) C13 0.110(7) 0.034(5) 0.042(5) -0.007(4) 0.022(5) -0.004(5) C14 0.117(7) 0.035(5) 0.043(5) -0.013(4) 0.019(5) -0.009(4) C15 0.110(7) 0.036(5) 0.041(5) -0.010(4) 0.018(5) -0.015(5) C16 0.105(7) 0.029(5) 0.033(5) -0.004(4) 0.017(5) -0.012(5) C17 0.079(11) 0.031(8) 0.037(8) -0.002(7) -0.002(8) -0.021(7) C18 0.057(10) 0.054(10) 0.026(7) -0.006(7) 0.011(7) 0.004(7) C19 0.052(9) 0.053(9) 0.029(7) 0.024(7) -0.018(7) -0.006(7) C21 0.041(8) 0.037(8) 0.016(6) 0.003(6) 0.001(6) 0.026(6) C22 0.026(8) 0.054(9) 0.037(8) 0.012(7) 0.023(6) 0.015(7) C23 0.061(10) 0.068(11) 0.027(8) 0.021(8) 0.029(7) 0.014(8) C24 0.064(12) 0.105(15) 0.029(9) -0.006(9) 0.012(9) 0.034(10) C25 0.050(10) 0.065(11) 0.027(8) -0.012(7) -0.005(7) 0.020(8) C26 0.040(8) 0.033(8) 0.032(8) -0.009(6) -0.002(7) 0.012(6) C27 0.039(9) 0.064(10) 0.049(9) 0.004(8) 0.001(7) 0.023(7) C28 0.041(9) 0.088(12) 0.046(9) -0.006(8) -0.025(7) 0.035(8) C29 0.050(10) 0.054(10) 0.061(10) 0.016(8) 0.010(8) 0.023(8) C31 0.022(7) 0.026(7) 0.038(8) -0.004(6) 0.004(6) -0.005(5) C32 0.020(7) 0.032(8) 0.046(8) -0.004(7) -0.010(6) -0.001(6) C33 0.027(8) 0.035(8) 0.063(10) -0.005(7) -0.016(7) 0.003(6) C34 0.027(8) 0.045(10) 0.103(14) -0.022(10) -0.001(9) 0.007(7) C35 0.025(8) 0.060(10) 0.038(8) 0.014(7) 0.010(6) 0.007(7) C36 0.018(7) 0.037(8) 0.047(8) -0.012(7) 0.009(6) 0.003(6) C37 0.050(10) 0.061(11) 0.081(12) -0.020(9) -0.020(9) -0.018(8) C38 0.062(11) 0.071(11) 0.060(10) -0.030(9) -0.008(9) -0.016(9) C39 0.064(11) 0.054(10) 0.071(11) -0.016(9) 0.002(9) -0.017(8) C41 0.018(6) 0.033(7) 0.010(6) -0.001(5) 0.002(5) -0.008(5) C42 0.022(7) 0.031(7) 0.018(6) -0.007(5) 0.001(5) 0.000(5) C43 0.041(8) 0.036(8) 0.014(6) 0.007(6) -0.006(6) -0.012(6) C44 0.028(8) 0.054(9) 0.019(7) 0.003(6) 0.005(6) -0.010(6) C45 0.059(10) 0.029(8) 0.026(7) -0.019(6) 0.004(7) -0.010(7) C46 0.043(8) 0.020(7) 0.010(6) -0.005(5) 0.002(5) 0.002(6) C47 0.074(11) 0.068(11) 0.046(9) 0.006(8) 0.009(9) -0.032(9) C48 0.047(10) 0.104(13) 0.040(9) 0.018(9) 0.020(8) 0.025(9) C49 0.047(9) 0.043(9) 0.033(8) 0.009(7) 0.009(7) -0.010(7) C121 0.077(12) 0.023(8) 0.076(12) 0.008(8) 0.024(10) 0.031(8) C122 0.073(12) 0.052(11) 0.105(14) 0.029(10) 0.019(11) 0.029(9) C123 0.080(13) 0.055(11) 0.092(13) 0.023(9) 0.044(11) 0.035(9) C161 0.075(12) 0.055(10) 0.037(9) 0.006(8) -0.020(8) -0.024(8) C162 0.071(12) 0.091(13) 0.065(11) 0.022(10) -0.014(10) -0.054(10) C163 0.090(13) 0.068(11) 0.046(9) 0.009(8) -0.024(9) -0.045(9) C221 0.015(7) 0.055(10) 0.060(10) 0.018(8) 0.013(7) 0.011(6) C222 0.049(11) 0.098(15) 0.115(16) 0.006(12) 0.033(11) -0.001(10) C223 0.024(8) 0.067(11) 0.071(11) 0.016(9) 0.002(7) 0.012(7) C261 0.067(11) 0.051(10) 0.038(9) -0.024(7) -0.004(8) 0.008(8) C262 0.061(11) 0.045(10) 0.088(13) -0.011(9) -0.017(10) 0.010(8) C263 0.049(10) 0.039(9) 0.081(11) -0.033(8) -0.009(9) 0.012(7) C321 0.049(9) 0.042(9) 0.037(8) 0.000(7) -0.012(7) 0.000(7) C322 0.079(12) 0.048(10) 0.064(11) 0.002(8) -0.020(9) -0.020(8) C323 0.051(9) 0.041(9) 0.041(8) 0.019(7) -0.007(7) -0.003(7) C361 0.037(9) 0.044(9) 0.050(9) 0.007(7) 0.014(7) 0.009(7) C362 0.083(13) 0.070(12) 0.064(11) 0.010(9) 0.005(10) -0.034(10) C363 0.038(9) 0.082(12) 0.051(10) 0.031(9) 0.005(8) -0.019(8) C421 0.036(8) 0.039(9) 0.050(9) 0.015(7) 0.007(7) 0.020(6) C422 0.119(15) 0.069(11) 0.039(9) 0.033(8) 0.053(10) 0.052(10) C423 0.076(11) 0.035(8) 0.031(8) 0.018(7) -0.020(8) -0.011(7) C461 0.056(9) 0.018(7) 0.037(8) -0.001(6) -0.006(7) 0.001(6) C462 0.065(10) 0.037(9) 0.060(10) -0.022(8) -0.010(8) 0.020(7) C463 0.072(11) 0.019(7) 0.044(8) 0.006(6) -0.016(8) 0.015(7) C1 0.080(13) 0.060(11) 0.20(2) 0.039(12) -0.011(12) 0.001(9) C2 0.080(13) 0.060(11) 0.20(2) 0.038(12) -0.010(12) 0.000(9) C3 0.079(13) 0.059(11) 0.20(2) 0.040(12) -0.010(12) 0.000(9) C4 0.079(13) 0.059(11) 0.20(2) 0.036(12) -0.011(12) -0.001(9) C5 0.080(13) 0.060(11) 0.20(2) 0.036(12) -0.011(12) 0.000(9) C6 0.079(13) 0.058(11) 0.20(2) 0.038(12) -0.011(12) 0.002(9) C7 0.080(13) 0.062(11) 0.20(2) 0.037(12) -0.011(12) 0.001(9) C1A 0.104(17) 0.072(14) 0.130(17) 0.011(13) 0.041(14) 0.003(12) C2A 0.104(17) 0.072(14) 0.129(17) 0.011(13) 0.043(14) 0.001(12) C3A 0.104(17) 0.071(14) 0.131(17) 0.010(13) 0.041(14) 0.001(12) C4A 0.105(17) 0.071(14) 0.131(17) 0.008(13) 0.041(14) 0.003(12) C5A 0.104(17) 0.071(14) 0.130(17) 0.010(13) 0.042(14) 0.003(12) C6A 0.104(17) 0.071(14) 0.131(17) 0.010(13) 0.041(14) 0.004(12) C7A 0.104(17) 0.072(14) 0.131(17) 0.009(13) 0.042(14) 0.003(12) _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 Bi1 O33 2.011(7) . ? Bi1 O41 2.047(7) . ? Bi1 O13 2.057(7) . ? Bi2 O42 2.014(7) . ? Bi2 O11 2.046(7) . ? Bi2 O22 2.049(7) . ? Bi3 O23 2.020(6) . ? Bi3 O12 2.047(7) . ? Bi3 O32 2.047(7) . ? Bi4 O21 2.045(7) . ? Bi4 O31 2.067(7) . ? Bi4 O43 2.071(7) . ? Si1 O11 1.609(7) . ? Si1 O13 1.611(8) . ? Si1 O12 1.639(7) . ? Si1 N1 1.747(9) . ? Si2 O23 1.600(7) . ? Si2 O21 1.629(8) . ? Si2 O22 1.634(7) . ? Si2 N2 1.750(9) . ? Si3 O33 1.607(7) . ? Si3 O31 1.617(8) . ? Si3 O32 1.627(7) . ? Si3 N3 1.755(9) . ? Si4 O42 1.600(8) . ? Si4 O43 1.615(7) . ? Si4 O41 1.620(7) . ? Si4 N4 1.763(9) . ? Si11 N1 1.742(9) . ? Si11 C17 1.854(11) . ? Si11 C18 1.855(12) . ? Si11 C19 1.870(11) . ? Si21 N2 1.728(9) . ? Si21 C28 1.821(12) . ? Si21 C29 1.853(13) . ? Si21 C27 1.859(12) . ? Si31 N3 1.747(9) . ? Si31 C37 1.820(13) . ? Si31 C39 1.827(14) . ? Si31 C38 1.851(14) . ? Si41 N4 1.736(9) . ? Si41 C49 1.845(11) . ? Si41 C47 1.861(13) . ? Si41 C48 1.876(13) . ? N1 C11 1.417(10) . ? N2 C21 1.457(9) . ? N3 C31 1.420(10) . ? N4 C41 1.443(10) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 C121 1.488(16) . ? C13 C14 1.3900 . ? C13 H13A 0.9500 . ? C14 C15 1.3900 . ? C14 H14A 0.9500 . ? C15 C16 1.3900 . ? C15 H15A 0.9500 . ? C16 C161 1.510(16) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 C221 1.524(14) . ? C23 C24 1.3900 . ? C23 H23A 0.9500 . ? C24 C25 1.3900 . ? C24 H24A 0.9500 . ? C25 C26 1.3900 . ? C25 H25A 0.9500 . ? C26 C261 1.505(15) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C32 C321 1.495(14) . ? C33 C34 1.3900 . ? C33 H33A 0.9500 . ? C34 C35 1.3900 . ? C34 H34A 0.9500 . ? C35 C36 1.3900 . ? C35 H35A 0.9500 . ? C36 C361 1.481(13) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C42 C421 1.517(13) . ? C43 C44 1.3900 . ? C43 H43A 0.9500 . ? C44 C45 1.3900 . ? C44 H44A 0.9500 . ? C45 C46 1.3900 . ? C45 H45A 0.9500 . ? C46 C461 1.533(13) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C121 C123 1.516(18) . ? C121 C122 1.525(17) . ? C121 H12A 1.0000 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C122 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C123 H12G 0.9800 . ? C161 C162 1.525(17) . ? C161 C163 1.546(16) . ? C161 H16A 1.0000 . ? C162 H16B 0.9800 . ? C162 H16C 0.9800 . ? C162 H16D 0.9800 . ? C163 H16E 0.9800 . ? C163 H16F 0.9800 . ? C163 H16G 0.9800 . ? C221 C222 1.510(17) . ? C221 C223 1.520(16) . ? C221 H22A 1.0000 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C222 H22D 0.9800 . ? C223 H22E 0.9800 . ? C223 H22F 0.9800 . ? C223 H22G 0.9800 . ? C261 C263 1.528(17) . ? C261 C262 1.549(17) . ? C261 H26A 1.0000 . ? C262 H26B 0.9800 . ? C262 H26C 0.9800 . ? C262 H26D 0.9800 . ? C263 H26E 0.9800 . ? C263 H26F 0.9800 . ? C263 H26G 0.9800 . ? C321 C322 1.527(15) . ? C321 C323 1.535(16) . ? C321 H32A 1.0000 . ? C322 H32B 0.9800 . ? C322 H32C 0.9800 . ? C322 H32D 0.9800 . ? C323 H32E 0.9800 . ? C323 H32F 0.9800 . ? C323 H32G 0.9800 . ? C361 C362 1.507(17) . ? C361 C363 1.530(16) . ? C361 H36A 1.0000 . ? C362 H36B 0.9800 . ? C362 H36C 0.9800 . ? C362 H36D 0.9800 . ? C363 H36E 0.9800 . ? C363 H36F 0.9800 . ? C363 H36G 0.9800 . ? C421 C423 1.510(16) . ? C421 C422 1.533(16) . ? C421 H42A 1.0000 . ? C422 H42B 0.9800 . ? C422 H42C 0.9800 . ? C422 H42D 0.9800 . ? C423 H42E 0.9800 . ? C423 H42F 0.9800 . ? C423 H42G 0.9800 . ? C461 C463 1.517(15) . ? C461 C462 1.539(15) . ? C461 H46A 1.0000 . ? C462 H46B 0.9800 . ? C462 H46C 0.9800 . ? C462 H46D 0.9800 . ? C463 H46E 0.9800 . ? C463 H46F 0.9800 . ? C463 H46G 0.9800 . ? C51 C52 1.36(3) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.28(3) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.36(3) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.37(3) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.37(3) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 C7 1.49(3) . ? C2 C3 1.3900 . ? C2 H2A 0.9500 . ? C3 C4 1.3900 . ? C3 H3A 0.9500 . ? C4 C5 1.3900 . ? C4 H4A 0.9500 . ? C5 C6 1.3900 . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 H7AA 0.9800 . ? C7 H7AB 0.9800 . ? C7 H7AC 0.9800 . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C1A C7A 1.59(3) . ? C2A C3A 1.3900 . ? C2A H2AA 0.9500 . ? C3A C4A 1.3900 . ? C3A H3AA 0.9500 . ? C4A C5A 1.3900 . ? C4A H4AA 0.9500 . ? C5A C6A 1.3900 . ? C5A H5AA 0.9500 . ? C6A H6AA 0.9500 . ? C7A H7A 0.9800 . ? C7A H7B 0.9800 . ? C7A H7C 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 O33 Bi1 O41 89.9(3) . . ? O33 Bi1 O13 91.6(3) . . ? O41 Bi1 O13 97.2(3) . . ? O42 Bi2 O11 93.9(3) . . ? O42 Bi2 O22 90.4(3) . . ? O11 Bi2 O22 97.7(3) . . ? O23 Bi3 O12 93.7(3) . . ? O23 Bi3 O32 89.8(3) . . ? O12 Bi3 O32 96.6(3) . . ? O21 Bi4 O31 101.2(3) . . ? O21 Bi4 O43 101.1(3) . . ? O31 Bi4 O43 103.0(3) . . ? O11 Si1 O13 110.1(4) . . ? O11 Si1 O12 111.5(4) . . ? O13 Si1 O12 113.0(4) . . ? O11 Si1 N1 109.2(4) . . ? O13 Si1 N1 107.5(4) . . ? O12 Si1 N1 105.3(4) . . ? O23 Si2 O21 109.6(4) . . ? O23 Si2 O22 109.0(4) . . ? O21 Si2 O22 111.3(4) . . ? O23 Si2 N2 110.2(4) . . ? O21 Si2 N2 108.7(4) . . ? O22 Si2 N2 108.0(4) . . ? O33 Si3 O31 108.1(4) . . ? O33 Si3 O32 110.9(4) . . ? O31 Si3 O32 110.8(4) . . ? O33 Si3 N3 109.3(4) . . ? O31 Si3 N3 109.6(4) . . ? O32 Si3 N3 108.1(4) . . ? O42 Si4 O43 109.0(4) . . ? O42 Si4 O41 110.0(4) . . ? O43 Si4 O41 111.6(4) . . ? O42 Si4 N4 109.0(4) . . ? O43 Si4 N4 109.5(4) . . ? O41 Si4 N4 107.6(4) . . ? N1 Si11 C17 110.2(5) . . ? N1 Si11 C18 110.7(5) . . ? C17 Si11 C18 107.8(6) . . ? N1 Si11 C19 112.6(5) . . ? C17 Si11 C19 106.7(6) . . ? C18 Si11 C19 108.6(6) . . ? N2 Si21 C28 110.4(5) . . ? N2 Si21 C29 109.9(5) . . ? C28 Si21 C29 106.9(7) . . ? N2 Si21 C27 110.5(5) . . ? C28 Si21 C27 109.3(6) . . ? C29 Si21 C27 109.7(6) . . ? N3 Si31 C37 108.6(6) . . ? N3 Si31 C39 109.3(5) . . ? C37 Si31 C39 111.3(7) . . ? N3 Si31 C38 112.6(6) . . ? C37 Si31 C38 108.4(7) . . ? C39 Si31 C38 106.6(7) . . ? N4 Si41 C49 109.7(5) . . ? N4 Si41 C47 110.5(5) . . ? C49 Si41 C47 108.2(6) . . ? N4 Si41 C48 111.7(5) . . ? C49 Si41 C48 109.7(6) . . ? C47 Si41 C48 107.0(7) . . ? Si1 O11 Bi2 140.7(4) . . ? Si1 O12 Bi3 138.3(4) . . ? Si1 O13 Bi1 141.3(4) . . ? Si2 O21 Bi4 136.4(4) . . ? Si2 O22 Bi2 126.2(4) . . ? Si2 O23 Bi3 149.1(4) . . ? Si3 O31 Bi4 136.7(4) . . ? Si3 O32 Bi3 126.8(4) . . ? Si3 O33 Bi1 148.7(4) . . ? Si4 O41 Bi1 126.7(4) . . ? Si4 O42 Bi2 151.4(4) . . ? Si4 O43 Bi4 137.1(4) . . ? C11 N1 Si11 119.4(7) . . ? C11 N1 Si1 116.1(6) . . ? Si11 N1 Si1 124.5(5) . . ? C21 N2 Si21 121.0(7) . . ? C21 N2 Si2 114.8(6) . . ? Si21 N2 Si2 124.0(5) . . ? C31 N3 Si31 121.3(6) . . ? C31 N3 Si3 115.7(6) . . ? Si31 N3 Si3 122.5(5) . . ? C41 N4 Si41 122.4(6) . . ? C41 N4 Si4 114.7(6) . . ? Si41 N4 Si4 122.6(5) . . ? C12 C11 C16 120.0 . . ? C12 C11 N1 119.6(8) . . ? C16 C11 N1 120.3(8) . . ? C11 C12 C13 120.0 . . ? C11 C12 C121 125.2(8) . . ? C13 C12 C121 114.8(8) . . ? C14 C13 C12 120.0 . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 C161 116.2(8) . . ? C11 C16 C161 123.8(8) . . ? Si11 C17 H17A 109.5 . . ? Si11 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si11 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si11 C18 H18A 109.5 . . ? Si11 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si11 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si11 C19 H19A 109.5 . . ? Si11 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si11 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C21 C26 120.0 . . ? C22 C21 N2 119.8(7) . . ? C26 C21 N2 120.1(7) . . ? C23 C22 C21 120.0 . . ? C23 C22 C221 116.6(8) . . ? C21 C22 C221 123.4(8) . . ? C22 C23 C24 120.0 . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 C261 118.7(8) . . ? C21 C26 C261 121.3(8) . . ? Si21 C27 H27A 109.5 . . ? Si21 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si21 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si21 C28 H28A 109.5 . . ? Si21 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si21 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si21 C29 H29A 109.5 . . ? Si21 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si21 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C31 C36 120.0 . . ? C32 C31 N3 120.7(7) . . ? C36 C31 N3 119.3(7) . . ? C33 C32 C31 120.0 . . ? C33 C32 C321 117.6(8) . . ? C31 C32 C321 122.4(8) . . ? C32 C33 C34 120.0 . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 C361 116.0(8) . . ? C31 C36 C361 124.0(8) . . ? Si31 C37 H37A 109.5 . . ? Si31 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si31 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si31 C38 H38A 109.5 . . ? Si31 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si31 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si31 C39 H39A 109.5 . . ? Si31 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si31 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C41 C46 120.0 . . ? C42 C41 N4 119.0(6) . . ? C46 C41 N4 120.8(6) . . ? C41 C42 C43 120.0 . . ? C41 C42 C421 122.8(7) . . ? C43 C42 C421 117.2(7) . . ? C42 C43 C44 120.0 . . ? C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 H45A 120.0 . . ? C44 C45 H45A 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 C461 117.6(7) . . ? C41 C46 C461 122.3(7) . . ? Si41 C47 H47A 109.5 . . ? Si41 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si41 C48 H48A 109.5 . . ? Si41 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si41 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Si41 C49 H49A 109.5 . . ? Si41 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? Si41 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C12 C121 C123 114.6(12) . . ? C12 C121 C122 115.7(12) . . ? C123 C121 C122 108.2(12) . . ? C12 C121 H12A 105.8 . . ? C123 C121 H12A 105.8 . . ? C122 C121 H12A 105.8 . . ? C121 C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C122 H12D 109.5 . . ? H12B C122 H12D 109.5 . . ? H12C C122 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C121 C123 H12G 109.5 . . ? H12E C123 H12G 109.5 . . ? H12F C123 H12G 109.5 . . ? C16 C161 C162 113.5(12) . . ? C16 C161 C163 110.2(12) . . ? C162 C161 C163 110.2(11) . . ? C16 C161 H16A 107.5 . . ? C162 C161 H16A 107.5 . . ? C163 C161 H16A 107.5 . . ? C161 C162 H16B 109.5 . . ? C161 C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C161 C162 H16D 109.5 . . ? H16B C162 H16D 109.5 . . ? H16C C162 H16D 109.5 . . ? C161 C163 H16E 109.5 . . ? C161 C163 H16F 109.5 . . ? H16E C163 H16F 109.5 . . ? C161 C163 H16G 109.5 . . ? H16E C163 H16G 109.5 . . ? H16F C163 H16G 109.5 . . ? C222 C221 C223 109.2(11) . . ? C222 C221 C22 113.4(11) . . ? C223 C221 C22 114.2(10) . . ? C222 C221 H22A 106.5 . . ? C223 C221 H22A 106.5 . . ? C22 C221 H22A 106.5 . . ? C221 C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C221 C222 H22D 109.5 . . ? H22B C222 H22D 109.5 . . ? H22C C222 H22D 109.5 . . ? C221 C223 H22E 109.5 . . ? C221 C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C221 C223 H22G 109.5 . . ? H22E C223 H22G 109.5 . . ? H22F C223 H22G 109.5 . . ? C26 C261 C263 113.8(11) . . ? C26 C261 C262 110.5(11) . . ? C263 C261 C262 107.3(11) . . ? C26 C261 H26A 108.4 . . ? C263 C261 H26A 108.4 . . ? C262 C261 H26A 108.4 . . ? C261 C262 H26B 109.5 . . ? C261 C262 H26C 109.5 . . ? H26B C262 H26C 109.5 . . ? C261 C262 H26D 109.5 . . ? H26B C262 H26D 109.5 . . ? H26C C262 H26D 109.5 . . ? C261 C263 H26E 109.5 . . ? C261 C263 H26F 109.5 . . ? H26E C263 H26F 109.5 . . ? C261 C263 H26G 109.5 . . ? H26E C263 H26G 109.5 . . ? H26F C263 H26G 109.5 . . ? C32 C321 C322 112.5(11) . . ? C32 C321 C323 114.0(10) . . ? C322 C321 C323 110.5(10) . . ? C32 C321 H32A 106.4 . . ? C322 C321 H32A 106.4 . . ? C323 C321 H32A 106.4 . . ? C321 C322 H32B 109.5 . . ? C321 C322 H32C 109.5 . . ? H32B C322 H32C 109.5 . . ? C321 C322 H32D 109.5 . . ? H32B C322 H32D 109.5 . . ? H32C C322 H32D 109.5 . . ? C321 C323 H32E 109.5 . . ? C321 C323 H32F 109.5 . . ? H32E C323 H32F 109.5 . . ? C321 C323 H32G 109.5 . . ? H32E C323 H32G 109.5 . . ? H32F C323 H32G 109.5 . . ? C36 C361 C362 112.6(11) . . ? C36 C361 C363 115.8(11) . . ? C362 C361 C363 108.2(11) . . ? C36 C361 H36A 106.5 . . ? C362 C361 H36A 106.5 . . ? C363 C361 H36A 106.5 . . ? C361 C362 H36B 109.5 . . ? C361 C362 H36C 109.5 . . ? H36B C362 H36C 109.5 . . ? C361 C362 H36D 109.5 . . ? H36B C362 H36D 109.5 . . ? H36C C362 H36D 109.5 . . ? C361 C363 H36E 109.5 . . ? C361 C363 H36F 109.5 . . ? H36E C363 H36F 109.5 . . ? C361 C363 H36G 109.5 . . ? H36E C363 H36G 109.5 . . ? H36F C363 H36G 109.5 . . ? C423 C421 C42 113.6(10) . . ? C423 C421 C422 108.6(10) . . ? C42 C421 C422 111.1(11) . . ? C423 C421 H42A 107.8 . . ? C42 C421 H42A 107.8 . . ? C422 C421 H42A 107.8 . . ? C421 C422 H42B 109.5 . . ? C421 C422 H42C 109.5 . . ? H42B C422 H42C 109.5 . . ? C421 C422 H42D 109.5 . . ? H42B C422 H42D 109.5 . . ? H42C C422 H42D 109.5 . . ? C421 C423 H42E 109.5 . . ? C421 C423 H42F 109.5 . . ? H42E C423 H42F 109.5 . . ? C421 C423 H42G 109.5 . . ? H42E C423 H42G 109.5 . . ? H42F C423 H42G 109.5 . . ? C463 C461 C46 110.8(10) . . ? C463 C461 C462 111.9(10) . . ? C46 C461 C462 109.9(9) . . ? C463 C461 H46A 108.0 . . ? C46 C461 H46A 108.0 . . ? C462 C461 H46A 108.0 . . ? C461 C462 H46B 109.5 . . ? C461 C462 H46C 109.5 . . ? H46B C462 H46C 109.5 . . ? C461 C462 H46D 109.5 . . ? H46B C462 H46D 109.5 . . ? H46C C462 H46D 109.5 . . ? C461 C463 H46E 109.5 . . ? C461 C463 H46F 109.5 . . ? H46E C463 H46F 109.5 . . ? C461 C463 H46G 109.5 . . ? H46E C463 H46G 109.5 . . ? H46F C463 H46G 109.5 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C51 146(3) . . ? C53 C52 H52A 100.4 . . ? C51 C52 H52A 100.4 . . ? C53 C52 H52B 100.4 . . ? C51 C52 H52B 100.4 . . ? H52A C52 H52B 104.3 . . ? C52 C53 C54 149(3) . . ? C52 C53 H53A 99.4 . . ? C54 C53 H53A 99.4 . . ? C52 C53 H53B 99.4 . . ? C54 C53 H53B 99.4 . . ? H53A C53 H53B 104.0 . . ? C55 C54 C53 119(3) . . ? C55 C54 H54A 107.5 . . ? C53 C54 H54A 107.5 . . ? C55 C54 H54B 107.5 . . ? C53 C54 H54B 107.5 . . ? H54A C54 H54B 107.0 . . ? C54 C55 C56 126(4) . . ? C54 C55 H55A 105.8 . . ? C56 C55 H55A 105.8 . . ? C54 C55 H55B 105.8 . . ? C56 C55 H55B 105.8 . . ? H55A C55 H55B 106.2 . . ? C55 C56 H56A 109.4 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C2 C1 C6 120.0 . . ? C2 C1 C7 126(3) . . ? C6 C1 C7 114(3) . . ? C3 C2 C1 120.0 . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? C1 C7 H7AA 109.5 . . ? C1 C7 H7AB 109.5 . . ? H7AA C7 H7AB 109.5 . . ? C1 C7 H7AC 109.5 . . ? H7AA C7 H7AC 109.5 . . ? H7AB C7 H7AC 109.5 . . ? C2A C1A C6A 120.0 . . ? C2A C1A C7A 117(3) . . ? C6A C1A C7A 122(3) . . ? C1A C2A C3A 120.0 . . ? C1A C2A H2AA 120.0 . . ? C3A C2A H2AA 120.0 . . ? C4A C3A C2A 120.0 . . ? C4A C3A H3AA 120.0 . . ? C2A C3A H3AA 120.0 . . ? C5A C4A C3A 120.0 . . ? C5A C4A H4AA 120.0 . . ? C3A C4A H4AA 120.0 . . ? C4A C5A C6A 120.0 . . ? C4A C5A H5AA 120.0 . . ? C6A C5A H5AA 120.0 . . ? C5A C6A C1A 120.0 . . ? C5A C6A H6AA 120.0 . . ? C1A C6A H6AA 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.499 _refine_diff_density_min -1.129 _refine_diff_density_rms 0.231 _database_code_depnum_ccdc_archive 'CCDC 941563' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93 H176 Al6 N4 O18.75 Si8' _chemical_formula_weight 2036.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 18.6059(5) _cell_length_b 18.7005(5) _cell_length_c 35.0951(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12211.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15781 _cell_measurement_theta_min 2.6948 _cell_measurement_theta_max 28.9642 _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4408 _exptl_absorpt_coefficient_mu 0.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9288 _exptl_absorpt_correction_T_max 0.9635 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhanced (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.1903 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90833 _diffrn_reflns_av_R_equivalents 0.0915 _diffrn_reflns_av_unetI/netI 0.0946 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 26.00 _reflns_number_total 23933 _reflns_number_gt 17220 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrysAlisPro _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 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. One THF molecule is disordered, treated in splitting mode, and refined in PARTs. The constraints by SIMU combined with DELU are applied for the atoms of O7, C01, C02, C03, C04, O8, C05, C06, C07, C08, O9, C4, C5, C6, C7, O17, C54, C55, C56, C57, O18, C58, C59, C60, C61, O19, C61, C62, C63, and C64. The restraint by DFIX is used for the bonds within the THF molecules of O21C71C72C73C74, O21AC71AC72AC73AC74A, and O22C75C76C77C78. ; _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^)+(0.1012P)^2^+5.0249P] 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 'refined in riding mode to the acrrier atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 23933 _refine_ls_number_parameters 1229 _refine_ls_number_restraints 1246 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.2045 _refine_ls_wR_factor_gt 0.1860 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.044 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al -0.02201(9) 0.16867(9) 0.93190(5) 0.0341(4) Uani 1 1 d . . . Al2 Al -0.08179(11) 0.22011(10) 0.82278(5) 0.0411(5) Uani 1 1 d . . . Al3 Al -0.20969(8) 0.29430(9) 0.91498(5) 0.0309(4) Uani 1 1 d . . . Si1 Si -0.16326(8) 0.14078(7) 0.88764(4) 0.0244(3) Uani 1 1 d . . . Si2 Si -0.05023(7) 0.31707(8) 0.89138(4) 0.0255(3) Uani 1 1 d . . . Si3 Si -0.17999(9) -0.01829(8) 0.90401(5) 0.0331(4) Uani 1 1 d . . . Si4 Si -0.02255(8) 0.46607(8) 0.92359(5) 0.0334(4) Uani 1 1 d . . . N1 N -0.2128(2) 0.0626(2) 0.88624(12) 0.0278(10) Uani 1 1 d . . . N2 N -0.0006(2) 0.3959(2) 0.89326(12) 0.0264(10) Uani 1 1 d . . . O1 O -0.09328(19) 0.12295(19) 0.91247(11) 0.0331(9) Uani 1 1 d . . . O2 O -0.1414(2) 0.16396(19) 0.84503(10) 0.0341(9) Uani 1 1 d . . . O3 O -0.2095(2) 0.20312(18) 0.90748(10) 0.0331(9) Uani 1 1 d . . . O4 O -0.00920(19) 0.25214(19) 0.91274(11) 0.0346(9) Uani 1 1 d . . . O5 O -0.0626(2) 0.29647(19) 0.84732(10) 0.0349(9) Uani 1 1 d . . . O6 O -0.12562(18) 0.33348(19) 0.91207(10) 0.0305(8) Uani 1 1 d . . . C1 C 0.0620(4) 0.1110(4) 0.9412(3) 0.065(2) Uani 1 1 d . . . H1A H 0.0794 0.0911 0.9171 0.097 Uiso 1 1 calc R . . H1B H 0.0497 0.0719 0.9587 0.097 Uiso 1 1 calc R . . H1C H 0.0997 0.1406 0.9527 0.097 Uiso 1 1 calc R . . C2 C -0.0961(5) 0.2310(4) 0.76782(17) 0.068(2) Uani 1 1 d . . . H2A H -0.1427 0.2539 0.7631 0.102 Uiso 1 1 calc R . . H2B H -0.0952 0.1839 0.7556 0.102 Uiso 1 1 calc R . . H2C H -0.0577 0.2608 0.7572 0.102 Uiso 1 1 calc R . . C3 C -0.2682(3) 0.3292(3) 0.95637(19) 0.0476(16) Uani 1 1 d . . . H3A H -0.2619 0.2982 0.9786 0.071 Uiso 1 1 calc R . . H3B H -0.3188 0.3291 0.9487 0.071 Uiso 1 1 calc R . . H3C H -0.2535 0.3780 0.9629 0.071 Uiso 1 1 calc R . . O7 O -0.0551(2) 0.1882(3) 0.98218(13) 0.0565(10) Uani 1 1 d U . . C01 C -0.0116(4) 0.2308(5) 1.0077(2) 0.0693(13) Uani 1 1 d U . . H01A H 0.0093 0.2722 0.9941 0.083 Uiso 1 1 calc R . . H01B H 0.0280 0.2018 1.0185 0.083 Uiso 1 1 calc R . . C02 C -0.0612(4) 0.2552(5) 1.0384(2) 0.0754(14) Uani 1 1 d U . . H02A H -0.0505 0.2299 1.0625 0.090 Uiso 1 1 calc R . . H02B H -0.0556 0.3072 1.0427 0.090 Uiso 1 1 calc R . . C03 C -0.1330(5) 0.2396(5) 1.0262(3) 0.0808(14) Uani 1 1 d U . . H03A H -0.1561 0.2834 1.0162 0.097 Uiso 1 1 calc R . . H03B H -0.1618 0.2218 1.0480 0.097 Uiso 1 1 calc R . . C04 C -0.1293(4) 0.1848(4) 0.9962(2) 0.0637(13) Uani 1 1 d U . . H04A H -0.1402 0.1368 1.0067 0.076 Uiso 1 1 calc R . . H04B H -0.1638 0.1955 0.9755 0.076 Uiso 1 1 calc R . . O8 O 0.0074(3) 0.1711(3) 0.82661(15) 0.0649(11) Uani 1 1 d U . . C05 C 0.0183(5) 0.0963(5) 0.8194(3) 0.0777(14) Uani 1 1 d U . . H05A H -0.0188 0.0771 0.8020 0.093 Uiso 1 1 calc R . . H05B H 0.0177 0.0684 0.8434 0.093 Uiso 1 1 calc R . . C06 C 0.0898(5) 0.0952(5) 0.8017(3) 0.0849(14) Uani 1 1 d U . . H06A H 0.1134 0.0484 0.8058 0.102 Uiso 1 1 calc R . . H06B H 0.0862 0.1041 0.7739 0.102 Uiso 1 1 calc R . . C07 C 0.1301(5) 0.1523(5) 0.8203(3) 0.0804(14) Uani 1 1 d U . . H07A H 0.1704 0.1688 0.8040 0.096 Uiso 1 1 calc R . . H07B H 0.1494 0.1363 0.8451 0.096 Uiso 1 1 calc R . . C08 C 0.0762(4) 0.2092(4) 0.8253(3) 0.0698(13) Uani 1 1 d U . . H08A H 0.0847 0.2358 0.8493 0.084 Uiso 1 1 calc R . . H08B H 0.0775 0.2433 0.8037 0.084 Uiso 1 1 calc R . . O9 O -0.2546(2) 0.3250(3) 0.86985(13) 0.0571(10) Uani 1 1 d U . . C4 C -0.3094(4) 0.2834(5) 0.8501(2) 0.0722(13) Uani 1 1 d U . . H4A H -0.3513 0.2745 0.8669 0.087 Uiso 1 1 calc R . . H4B H -0.2899 0.2371 0.8413 0.087 Uiso 1 1 calc R . . C5 C -0.3295(5) 0.3294(5) 0.8175(2) 0.0779(14) Uani 1 1 d U . . H5A H -0.3447 0.3000 0.7955 0.093 Uiso 1 1 calc R . . H5B H -0.3692 0.3621 0.8245 0.093 Uiso 1 1 calc R . . C6 C -0.2646(5) 0.3695(5) 0.8086(3) 0.0816(14) Uani 1 1 d U . . H6A H -0.2764 0.4146 0.7952 0.098 Uiso 1 1 calc R . . H6B H -0.2319 0.3409 0.7923 0.098 Uiso 1 1 calc R . . C7 C -0.2320(5) 0.3840(5) 0.8455(2) 0.0742(14) Uani 1 1 d U . . H7A H -0.1789 0.3855 0.8434 0.089 Uiso 1 1 calc R . . H7B H -0.2491 0.4302 0.8558 0.089 Uiso 1 1 calc R . . C11 C -0.2832(3) 0.0655(3) 0.87006(16) 0.0276(12) Uani 1 1 d . . . C12 C -0.2941(3) 0.0535(3) 0.83048(17) 0.0383(14) Uani 1 1 d . . . C13 C -0.3629(4) 0.0570(4) 0.8158(2) 0.061(2) Uani 1 1 d . . . H13A H -0.3698 0.0493 0.7893 0.073 Uiso 1 1 calc R . . C14 C -0.4201(4) 0.0708(4) 0.8378(3) 0.066(2) Uani 1 1 d . . . H14A H -0.4667 0.0723 0.8267 0.079 Uiso 1 1 calc R . . C15 C -0.4117(4) 0.0829(4) 0.8762(2) 0.0542(18) Uani 1 1 d . . . H15A H -0.4524 0.0933 0.8915 0.065 Uiso 1 1 calc R . . C16 C -0.3436(3) 0.0798(3) 0.89271(18) 0.0354(13) Uani 1 1 d . . . C17 C -0.0935(4) -0.0434(4) 0.8808(2) 0.060(2) Uani 1 1 d . . . H17A H -0.1002 -0.0453 0.8531 0.090 Uiso 1 1 calc R . . H17B H -0.0781 -0.0904 0.8901 0.090 Uiso 1 1 calc R . . H17C H -0.0568 -0.0077 0.8870 0.090 Uiso 1 1 calc R . . C18 C -0.2466(3) -0.0898(3) 0.89400(19) 0.0429(15) Uani 1 1 d . . . H18A H -0.2920 -0.0785 0.9068 0.064 Uiso 1 1 calc R . . H18B H -0.2282 -0.1356 0.9035 0.064 Uiso 1 1 calc R . . H18C H -0.2546 -0.0931 0.8665 0.064 Uiso 1 1 calc R . . C19 C -0.1651(4) -0.0139(4) 0.9566(2) 0.061(2) Uani 1 1 d . . . H19A H -0.2095 0.0013 0.9692 0.091 Uiso 1 1 calc R . . H19B H -0.1268 0.0205 0.9622 0.091 Uiso 1 1 calc R . . H19C H -0.1512 -0.0613 0.9661 0.091 Uiso 1 1 calc R . . C21 C 0.0610(3) 0.3994(3) 0.86797(16) 0.0320(13) Uani 1 1 d . . . C22 C 0.0509(4) 0.4239(3) 0.83032(17) 0.0419(15) Uani 1 1 d . . . C23 C 0.1097(4) 0.4225(4) 0.8056(2) 0.059(2) Uani 1 1 d . . . H23A H 0.1039 0.4393 0.7802 0.071 Uiso 1 1 calc R . . C24 C 0.1755(4) 0.3975(4) 0.8169(2) 0.060(2) Uani 1 1 d . . . H24A H 0.2141 0.3949 0.7992 0.073 Uiso 1 1 calc R . . C25 C 0.1850(4) 0.3765(4) 0.8535(2) 0.0590(19) Uani 1 1 d . . . H25A H 0.2315 0.3617 0.8615 0.071 Uiso 1 1 calc R . . C26 C 0.1292(3) 0.3759(3) 0.87997(17) 0.0378(14) Uani 1 1 d . . . C27 C 0.0484(4) 0.5356(4) 0.9224(2) 0.0569(19) Uani 1 1 d . . . H27A H 0.0950 0.5139 0.9285 0.085 Uiso 1 1 calc R . . H27B H 0.0374 0.5729 0.9412 0.085 Uiso 1 1 calc R . . H27C H 0.0505 0.5569 0.8969 0.085 Uiso 1 1 calc R . . C28 C -0.1097(3) 0.5103(3) 0.91048(19) 0.0425(15) Uani 1 1 d . . . H28A H -0.1057 0.5313 0.8850 0.064 Uiso 1 1 calc R . . H28B H -0.1207 0.5480 0.9290 0.064 Uiso 1 1 calc R . . H28C H -0.1484 0.4746 0.9106 0.064 Uiso 1 1 calc R . . C29 C -0.0302(4) 0.4334(4) 0.97330(17) 0.0478(16) Uani 1 1 d . . . H29A H 0.0143 0.4088 0.9805 0.072 Uiso 1 1 calc R . . H29B H -0.0707 0.4002 0.9752 0.072 Uiso 1 1 calc R . . H29C H -0.0381 0.4741 0.9904 0.072 Uiso 1 1 calc R . . C121 C -0.2308(4) 0.0367(4) 0.80381(17) 0.056(2) Uani 1 1 d . . . H12A H -0.1854 0.0404 0.8189 0.067 Uiso 1 1 calc R . . C122 C -0.2275(5) 0.0918(6) 0.7714(2) 0.100(4) Uani 1 1 d . . . H12B H -0.2185 0.1394 0.7821 0.149 Uiso 1 1 calc R . . H12C H -0.2733 0.0920 0.7577 0.149 Uiso 1 1 calc R . . H12D H -0.1886 0.0792 0.7539 0.149 Uiso 1 1 calc R . . C123 C -0.2364(5) -0.0394(5) 0.7882(3) 0.090(3) Uani 1 1 d . . . H12E H -0.2499 -0.0721 0.8088 0.135 Uiso 1 1 calc R . . H12F H -0.1898 -0.0539 0.7777 0.135 Uiso 1 1 calc R . . H12G H -0.2729 -0.0410 0.7681 0.135 Uiso 1 1 calc R . . C161 C -0.3372(3) 0.0922(3) 0.93559(18) 0.0409(15) Uani 1 1 d . . . H16A H -0.2851 0.0972 0.9421 0.049 Uiso 1 1 calc R . . C162 C -0.3755(4) 0.1592(4) 0.9481(2) 0.067(2) Uani 1 1 d . . . H16B H -0.3607 0.1993 0.9319 0.101 Uiso 1 1 calc R . . H16C H -0.3633 0.1697 0.9747 0.101 Uiso 1 1 calc R . . H16D H -0.4276 0.1522 0.9458 0.101 Uiso 1 1 calc R . . C163 C -0.3673(4) 0.0267(4) 0.9573(2) 0.061(2) Uani 1 1 d . . . H16E H -0.3570 0.0317 0.9846 0.091 Uiso 1 1 calc R . . H16F H -0.3447 -0.0170 0.9477 0.091 Uiso 1 1 calc R . . H16G H -0.4194 0.0239 0.9535 0.091 Uiso 1 1 calc R . . C221 C -0.0203(4) 0.4563(3) 0.81667(18) 0.0487(17) Uani 1 1 d . . . H22A H -0.0576 0.4453 0.8363 0.058 Uiso 1 1 calc R . . C222 C -0.0465(5) 0.4253(4) 0.7786(2) 0.074(2) Uani 1 1 d . . . H22B H -0.0429 0.3731 0.7792 0.111 Uiso 1 1 calc R . . H22C H -0.0166 0.4439 0.7578 0.111 Uiso 1 1 calc R . . H22D H -0.0966 0.4392 0.7743 0.111 Uiso 1 1 calc R . . C223 C -0.0155(5) 0.5376(4) 0.8131(2) 0.071(2) Uani 1 1 d . . . H22E H 0.0016 0.5580 0.8372 0.106 Uiso 1 1 calc R . . H22F H -0.0631 0.5570 0.8071 0.106 Uiso 1 1 calc R . . H22G H 0.0181 0.5501 0.7926 0.106 Uiso 1 1 calc R . . C261 C 0.1444(3) 0.3512(3) 0.91979(19) 0.0421(15) Uani 1 1 d . . . H26A H 0.0986 0.3543 0.9346 0.051 Uiso 1 1 calc R . . C262 C 0.1999(4) 0.3992(4) 0.9395(2) 0.062(2) Uani 1 1 d . . . H26B H 0.1818 0.4484 0.9405 0.093 Uiso 1 1 calc R . . H26C H 0.2451 0.3981 0.9252 0.093 Uiso 1 1 calc R . . H26D H 0.2082 0.3820 0.9655 0.093 Uiso 1 1 calc R . . C263 C 0.1701(4) 0.2740(4) 0.9213(2) 0.059(2) Uani 1 1 d . . . H26E H 0.1326 0.2425 0.9113 0.089 Uiso 1 1 calc R . . H26F H 0.1807 0.2610 0.9478 0.089 Uiso 1 1 calc R . . H26G H 0.2137 0.2689 0.9059 0.089 Uiso 1 1 calc R . . Al4 Al 0.37077(9) 0.71819(9) 0.82987(4) 0.0287(4) Uani 1 1 d . . . Al5 Al 0.51104(8) 0.79343(8) 0.91594(4) 0.0259(3) Uani 1 1 d . . . Al6 Al 0.32410(8) 0.66931(8) 0.94178(4) 0.0228(3) Uani 1 1 d . . . Si5 Si 0.34935(7) 0.81683(7) 0.89933(4) 0.0223(3) Uani 1 1 d . . . Si6 Si 0.45951(7) 0.63955(7) 0.89280(4) 0.0224(3) Uani 1 1 d . . . Si7 Si 0.32403(8) 0.96571(8) 0.93266(4) 0.0303(3) Uani 1 1 d . . . Si8 Si 0.48077(8) 0.48220(8) 0.91178(4) 0.0316(4) Uani 1 1 d . . . N3 N 0.3001(2) 0.8957(2) 0.90255(12) 0.0268(10) Uani 1 1 d . . . N4 N 0.5085(2) 0.5601(2) 0.88975(11) 0.0203(9) Uani 1 1 d . . . O11 O 0.35496(19) 0.79519(18) 0.85499(10) 0.0292(8) Uani 1 1 d . . . O12 O 0.42803(18) 0.83367(19) 0.91680(10) 0.0289(8) Uani 1 1 d . . . O13 O 0.31097(19) 0.75316(18) 0.92309(10) 0.0301(8) Uani 1 1 d . . . O14 O 0.43063(19) 0.66173(19) 0.85129(10) 0.0314(9) Uani 1 1 d . . . O15 O 0.50934(18) 0.70248(18) 0.90958(10) 0.0294(8) Uani 1 1 d . . . O16 O 0.39418(18) 0.62271(18) 0.92129(11) 0.0298(8) Uani 1 1 d . . . C31 C 0.2393(3) 0.9007(3) 0.87732(16) 0.0299(12) Uani 1 1 d . . . C32 C 0.2479(3) 0.9263(3) 0.84016(16) 0.0363(14) Uani 1 1 d . . . C33 C 0.1893(4) 0.9238(4) 0.8149(2) 0.0585(19) Uani 1 1 d . . . H33A H 0.1953 0.9399 0.7894 0.070 Uiso 1 1 calc R . . C34 C 0.1238(4) 0.8983(4) 0.8265(2) 0.066(2) Uani 1 1 d . . . H34A H 0.0849 0.8957 0.8090 0.079 Uiso 1 1 calc R . . C35 C 0.1149(3) 0.8770(4) 0.8631(2) 0.060(2) Uani 1 1 d . . . H35A H 0.0687 0.8610 0.8709 0.072 Uiso 1 1 calc R . . C36 C 0.1708(3) 0.8776(3) 0.89000(17) 0.0338(13) Uani 1 1 d . . . C37 C 0.2518(3) 1.0344(3) 0.9321(2) 0.0530(18) Uani 1 1 d . . . H37A H 0.2103 1.0169 0.9466 0.080 Uiso 1 1 calc R . . H37B H 0.2372 1.0437 0.9057 0.080 Uiso 1 1 calc R . . H37C H 0.2696 1.0786 0.9436 0.080 Uiso 1 1 calc R . . C38 C 0.4097(3) 1.0108(3) 0.91841(18) 0.0425(15) Uani 1 1 d . . . H38A H 0.4033 1.0341 0.8936 0.064 Uiso 1 1 calc R . . H38B H 0.4482 0.9752 0.9166 0.064 Uiso 1 1 calc R . . H38C H 0.4225 1.0468 0.9375 0.064 Uiso 1 1 calc R . . C39 C 0.3366(3) 0.9315(3) 0.98189(16) 0.0424(15) Uani 1 1 d . . . H39A H 0.2928 0.9069 0.9902 0.064 Uiso 1 1 calc R . . H39B H 0.3466 0.9715 0.9991 0.064 Uiso 1 1 calc R . . H39C H 0.3771 0.8980 0.9824 0.064 Uiso 1 1 calc R . . C41 C 0.5755(3) 0.5622(3) 0.86895(15) 0.0281(12) Uani 1 1 d . . . C42 C 0.6400(3) 0.5777(3) 0.88783(17) 0.0340(13) Uani 1 1 d . . . C43 C 0.7038(3) 0.5793(4) 0.8670(2) 0.0536(18) Uani 1 1 d . . . H43A H 0.7477 0.5898 0.8796 0.064 Uiso 1 1 calc R . . C44 C 0.7040(4) 0.5662(4) 0.8292(2) 0.062(2) Uani 1 1 d . . . H44A H 0.7482 0.5669 0.8155 0.074 Uiso 1 1 calc R . . C45 C 0.6416(4) 0.5520(4) 0.81033(19) 0.0512(18) Uani 1 1 d . . . H45A H 0.6430 0.5438 0.7836 0.061 Uiso 1 1 calc R . . C46 C 0.5751(3) 0.5492(3) 0.82932(15) 0.0345(13) Uani 1 1 d . . . C47 C 0.4764(4) 0.4911(3) 0.96439(17) 0.0528(18) Uani 1 1 d . . . H47A H 0.4338 0.5190 0.9714 0.079 Uiso 1 1 calc R . . H47B H 0.5196 0.5155 0.9736 0.079 Uiso 1 1 calc R . . H47C H 0.4733 0.4435 0.9760 0.079 Uiso 1 1 calc R . . C48 C 0.3906(3) 0.4536(3) 0.8947(2) 0.0541(19) Uani 1 1 d . . . H48A H 0.3539 0.4859 0.9050 0.081 Uiso 1 1 calc R . . H48B H 0.3810 0.4047 0.9034 0.081 Uiso 1 1 calc R . . H48C H 0.3895 0.4551 0.8668 0.081 Uiso 1 1 calc R . . C49 C 0.5452(3) 0.4092(3) 0.89968(18) 0.0402(14) Uani 1 1 d . . . H49A H 0.5945 0.4266 0.9028 0.060 Uiso 1 1 calc R . . H49B H 0.5377 0.3943 0.8732 0.060 Uiso 1 1 calc R . . H49C H 0.5372 0.3684 0.9167 0.060 Uiso 1 1 calc R . . C51 C 0.3794(5) 0.7312(4) 0.77555(17) 0.062(2) Uani 1 1 d . . . H51A H 0.4231 0.7586 0.7699 0.093 Uiso 1 1 calc R . . H51B H 0.3374 0.7573 0.7660 0.093 Uiso 1 1 calc R . . H51C H 0.3822 0.6844 0.7631 0.093 Uiso 1 1 calc R . . C52 C 0.5757(3) 0.8294(3) 0.95561(19) 0.0456(16) Uani 1 1 d . . . H52A H 0.5763 0.7959 0.9771 0.068 Uiso 1 1 calc R . . H52B H 0.5589 0.8762 0.9644 0.068 Uiso 1 1 calc R . . H52C H 0.6244 0.8340 0.9452 0.068 Uiso 1 1 calc R . . C53 C 0.2397(3) 0.6116(3) 0.95303(18) 0.0406(15) Uani 1 1 d . . . H53A H 0.2102 0.6069 0.9300 0.061 Uiso 1 1 calc R . . H53B H 0.2115 0.6347 0.9731 0.061 Uiso 1 1 calc R . . H53C H 0.2548 0.5641 0.9616 0.061 Uiso 1 1 calc R . . O17 O 0.2821(2) 0.6697(2) 0.83488(13) 0.0511(9) Uani 1 1 d U . . C54 C 0.2702(4) 0.5950(4) 0.8405(2) 0.0555(12) Uani 1 1 d U . . H54A H 0.2898 0.5796 0.8654 0.067 Uiso 1 1 calc R . . H54B H 0.2938 0.5669 0.8202 0.067 Uiso 1 1 calc R . . C55 C 0.1918(4) 0.5845(4) 0.8395(2) 0.0674(13) Uani 1 1 d U . . H55A H 0.1777 0.5593 0.8158 0.081 Uiso 1 1 calc R . . H55B H 0.1760 0.5555 0.8615 0.081 Uiso 1 1 calc R . . C56 C 0.1588(4) 0.6551(4) 0.8408(2) 0.0658(13) Uani 1 1 d U . . H56A H 0.1432 0.6665 0.8671 0.079 Uiso 1 1 calc R . . H56B H 0.1162 0.6569 0.8239 0.079 Uiso 1 1 calc R . . C57 C 0.2134(4) 0.7062(4) 0.8280(2) 0.0583(13) Uani 1 1 d U . . H57A H 0.2105 0.7512 0.8428 0.070 Uiso 1 1 calc R . . H57B H 0.2073 0.7174 0.8006 0.070 Uiso 1 1 calc R . . O18 O 0.5490(2) 0.8208(2) 0.86825(12) 0.0482(9) Uani 1 1 d U . . C58 C 0.5917(4) 0.7752(4) 0.8434(2) 0.0663(13) Uani 1 1 d U . . H58A H 0.6386 0.7648 0.8555 0.080 Uiso 1 1 calc R . . H58B H 0.5664 0.7294 0.8391 0.080 Uiso 1 1 calc R . . C59 C 0.6018(5) 0.8101(5) 0.8094(2) 0.0736(14) Uani 1 1 d U . . H59A H 0.5923 0.7772 0.7879 0.088 Uiso 1 1 calc R . . H59B H 0.6521 0.8270 0.8074 0.088 Uiso 1 1 calc R . . C60 C 0.5546(4) 0.8686(5) 0.8078(2) 0.0689(13) Uani 1 1 d U . . H60A H 0.5121 0.8566 0.7921 0.083 Uiso 1 1 calc R . . H60B H 0.5789 0.9106 0.7965 0.083 Uiso 1 1 calc R . . C61 C 0.5320(4) 0.8847(4) 0.8481(2) 0.0627(13) Uani 1 1 d U . . H61A H 0.5591 0.9259 0.8585 0.075 Uiso 1 1 calc R . . H61B H 0.4799 0.8952 0.8495 0.075 Uiso 1 1 calc R . . O19 O 0.3606(2) 0.6898(2) 0.99093(10) 0.0368(8) Uani 1 1 d U . . C62 C 0.3166(4) 0.7324(4) 1.01707(19) 0.0524(12) Uani 1 1 d U . . H62A H 0.2784 0.7026 1.0286 0.063 Uiso 1 1 calc R . . H62B H 0.2940 0.7730 1.0035 0.063 Uiso 1 1 calc R . . C63 C 0.3672(4) 0.7583(4) 1.0466(2) 0.0621(13) Uani 1 1 d U . . H63A H 0.3564 0.8084 1.0536 0.074 Uiso 1 1 calc R . . H63B H 0.3643 0.7282 1.0698 0.074 Uiso 1 1 calc R . . C64 C 0.4383(4) 0.7529(5) 1.0292(2) 0.0697(14) Uani 1 1 d U . . H64A H 0.4753 0.7443 1.0490 0.084 Uiso 1 1 calc R . . H64B H 0.4503 0.7977 1.0156 0.084 Uiso 1 1 calc R . . C65 C 0.4355(3) 0.6928(4) 1.00250(17) 0.0477(17) Uani 1 1 d . . . H65A H 0.4672 0.7013 0.9803 0.057 Uiso 1 1 calc R . . H65B H 0.4501 0.6477 1.0151 0.057 Uiso 1 1 calc R . . C321 C 0.3182(4) 0.9579(3) 0.82692(17) 0.0454(16) Uani 1 1 d . . . H32A H 0.3555 0.9474 0.8467 0.055 Uiso 1 1 calc R . . C322 C 0.3436(4) 0.9268(4) 0.7893(2) 0.065(2) Uani 1 1 d . . . H32B H 0.3595 0.8774 0.7932 0.097 Uiso 1 1 calc R . . H32C H 0.3837 0.9554 0.7795 0.097 Uiso 1 1 calc R . . H32D H 0.3040 0.9276 0.7709 0.097 Uiso 1 1 calc R . . C323 C 0.3115(4) 1.0400(4) 0.8230(2) 0.063(2) Uani 1 1 d . . . H32E H 0.2924 1.0600 0.8467 0.095 Uiso 1 1 calc R . . H32F H 0.2790 1.0514 0.8019 0.095 Uiso 1 1 calc R . . H32G H 0.3590 1.0605 0.8179 0.095 Uiso 1 1 calc R . . C361 C 0.1562(3) 0.8533(3) 0.92994(17) 0.0372(14) Uani 1 1 d . . . H36A H 0.2013 0.8601 0.9450 0.045 Uiso 1 1 calc R . . C362 C 0.0964(4) 0.8973(4) 0.9494(2) 0.059(2) Uani 1 1 d . . . H36B H 0.1100 0.9479 0.9497 0.089 Uiso 1 1 calc R . . H36C H 0.0897 0.8803 0.9756 0.089 Uiso 1 1 calc R . . H36D H 0.0513 0.8915 0.9352 0.089 Uiso 1 1 calc R . . C363 C 0.1357(3) 0.7742(3) 0.9323(2) 0.0495(17) Uani 1 1 d . . . H36E H 0.1727 0.7454 0.9196 0.074 Uiso 1 1 calc R . . H36F H 0.0894 0.7667 0.9197 0.074 Uiso 1 1 calc R . . H36G H 0.1321 0.7599 0.9591 0.074 Uiso 1 1 calc R . . C421 C 0.6427(3) 0.5925(3) 0.93063(18) 0.0382(14) Uani 1 1 d . . . H42A H 0.5921 0.5975 0.9398 0.046 Uiso 1 1 calc R . . C422 C 0.6766(4) 0.5288(4) 0.9518(2) 0.063(2) Uani 1 1 d . . . H42B H 0.6817 0.5405 0.9788 0.094 Uiso 1 1 calc R . . H42C H 0.7240 0.5185 0.9409 0.094 Uiso 1 1 calc R . . H42D H 0.6456 0.4867 0.9490 0.094 Uiso 1 1 calc R . . C423 C 0.6825(4) 0.6603(4) 0.9413(2) 0.062(2) Uani 1 1 d . . . H42E H 0.6670 0.6995 0.9247 0.094 Uiso 1 1 calc R . . H42F H 0.7344 0.6528 0.9383 0.094 Uiso 1 1 calc R . . H42G H 0.6720 0.6726 0.9679 0.094 Uiso 1 1 calc R . . C461 C 0.5084(4) 0.5340(4) 0.80679(16) 0.0477(17) Uani 1 1 d . . . H46A H 0.4664 0.5451 0.8236 0.057 Uiso 1 1 calc R . . C462 C 0.5037(4) 0.4532(4) 0.7963(2) 0.063(2) Uani 1 1 d . . . H46B H 0.5101 0.4243 0.8194 0.094 Uiso 1 1 calc R . . H46C H 0.5416 0.4414 0.7779 0.094 Uiso 1 1 calc R . . H46D H 0.4566 0.4430 0.7851 0.094 Uiso 1 1 calc R . . C463 C 0.5023(5) 0.5817(5) 0.7717(2) 0.080(3) Uani 1 1 d . . . H46E H 0.5027 0.6320 0.7795 0.119 Uiso 1 1 calc R . . H46F H 0.4573 0.5712 0.7583 0.119 Uiso 1 1 calc R . . H46G H 0.5430 0.5725 0.7546 0.119 Uiso 1 1 calc R . . O21 O -0.5704(15) 0.2082(16) 0.8521(8) 0.096(10) Uiso 0.25 1 d PD A 2 C71 C -0.5209(17) 0.239(2) 0.8256(11) 0.081(11) Uiso 0.25 1 d PD A 2 H71A H -0.4861 0.2035 0.8160 0.097 Uiso 0.25 1 calc PR A 2 H71B H -0.4944 0.2798 0.8371 0.097 Uiso 0.25 1 calc PR A 2 C72 C -0.5694(16) 0.2631(17) 0.7958(8) 0.059(8) Uiso 0.25 1 d PD A 2 H72A H -0.5788 0.2233 0.7779 0.071 Uiso 0.25 1 calc PR A 2 H72B H -0.5469 0.3027 0.7813 0.071 Uiso 0.25 1 calc PR A 2 C73 C -0.6382(19) 0.288(2) 0.8129(9) 0.091(12) Uiso 0.25 1 d PD A 2 H73A H -0.6796 0.2766 0.7962 0.110 Uiso 0.25 1 calc PR A 2 H73B H -0.6373 0.3397 0.8183 0.110 Uiso 0.25 1 calc PR A 2 C74 C -0.6400(17) 0.2447(19) 0.8489(10) 0.055(8) Uiso 0.25 1 d PD A 2 H74A H -0.6479 0.2763 0.8711 0.066 Uiso 0.25 1 calc PR A 2 H74B H -0.6795 0.2093 0.8479 0.066 Uiso 0.25 1 calc PR A 2 O21A O -0.5471(18) 0.2351(18) 0.8491(8) 0.098(10) Uiso 0.25 1 d PD B 1 C71A C -0.5422(13) 0.2267(14) 0.8080(7) 0.041(6) Uiso 0.25 1 d PD B 1 H71C H -0.5038 0.2583 0.7981 0.049 Uiso 0.25 1 calc PR B 1 H71D H -0.5289 0.1767 0.8020 0.049 Uiso 0.25 1 calc PR B 1 C72A C -0.6069(17) 0.243(2) 0.7900(9) 0.085(11) Uiso 0.25 1 d PD B 1 H72C H -0.6210 0.2052 0.7719 0.102 Uiso 0.25 1 calc PR B 1 H72D H -0.6033 0.2893 0.7761 0.102 Uiso 0.25 1 calc PR B 1 C73A C -0.660(2) 0.249(2) 0.8225(10) 0.088(11) Uiso 0.25 1 d PD B 1 H73C H -0.6873 0.2940 0.8206 0.105 Uiso 0.25 1 calc PR B 1 H73D H -0.6944 0.2085 0.8213 0.105 Uiso 0.25 1 calc PR B 1 C74A C -0.621(2) 0.247(3) 0.8584(11) 0.105(19) Uiso 0.25 1 d PD B 1 H74C H -0.6269 0.2923 0.8723 0.127 Uiso 0.25 1 calc PR B 1 H74D H -0.6393 0.2073 0.8746 0.127 Uiso 0.25 1 calc PR B 1 O22 O 0.1482(13) 0.2270(15) 0.6622(7) 0.107(9) Uiso 0.25 1 d PD . . C75 C 0.0705(13) 0.2337(15) 0.6478(7) 0.053(7) Uiso 0.25 1 d PD . . H75A H 0.0639 0.2715 0.6284 0.063 Uiso 0.25 1 calc PR . . H75B H 0.0496 0.1879 0.6391 0.063 Uiso 0.25 1 calc PR . . C76 C 0.0484(14) 0.2535(15) 0.6836(6) 0.048(6) Uiso 0.25 1 d PD . . H76A H 0.0125 0.2922 0.6808 0.058 Uiso 0.25 1 calc PR . . H76B H 0.0234 0.2122 0.6953 0.058 Uiso 0.25 1 calc PR . . C77 C 0.1001(15) 0.2763(17) 0.7085(9) 0.075(9) Uiso 0.25 1 d PD . . H77A H 0.0820 0.2731 0.7350 0.090 Uiso 0.25 1 calc PR . . H77B H 0.1127 0.3267 0.7032 0.090 Uiso 0.25 1 calc PR . . C78 C 0.1643(17) 0.2299(18) 0.7038(8) 0.078(10) Uiso 0.25 1 d PD . . H78A H 0.1604 0.1831 0.7168 0.094 Uiso 0.25 1 calc PR . . H78B H 0.2103 0.2538 0.7100 0.094 Uiso 0.25 1 calc PR . . 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 Al1 0.0239(8) 0.0330(9) 0.0455(10) 0.0076(8) -0.0068(7) 0.0011(7) Al2 0.0513(11) 0.0415(11) 0.0303(9) -0.0022(8) 0.0088(8) -0.0149(9) Al3 0.0239(8) 0.0292(9) 0.0396(9) -0.0013(7) 0.0013(7) 0.0022(7) Si1 0.0233(7) 0.0234(7) 0.0266(7) 0.0003(6) 0.0000(6) -0.0007(6) Si2 0.0220(7) 0.0258(7) 0.0286(7) 0.0028(6) -0.0010(6) -0.0024(6) Si3 0.0302(8) 0.0243(8) 0.0450(9) 0.0030(7) -0.0050(7) 0.0006(7) Si4 0.0254(8) 0.0306(8) 0.0441(9) -0.0053(7) -0.0027(7) -0.0011(7) N1 0.024(2) 0.028(2) 0.031(2) 0.0030(19) 0.0022(19) -0.0014(19) N2 0.025(2) 0.027(2) 0.027(2) -0.0013(18) 0.0009(19) -0.0026(18) O1 0.0268(19) 0.027(2) 0.045(2) 0.0011(17) -0.0053(18) 0.0003(16) O2 0.040(2) 0.033(2) 0.029(2) 0.0029(16) 0.0048(17) -0.0094(18) O3 0.033(2) 0.028(2) 0.038(2) -0.0025(16) 0.0066(17) -0.0019(17) O4 0.0262(19) 0.027(2) 0.051(2) 0.0042(18) -0.0070(18) -0.0001(16) O5 0.041(2) 0.033(2) 0.030(2) 0.0019(16) 0.0019(17) -0.0104(18) O6 0.0270(19) 0.033(2) 0.031(2) -0.0005(16) 0.0015(16) -0.0014(16) C1 0.032(4) 0.052(4) 0.111(7) 0.031(4) -0.007(4) 0.002(3) C2 0.114(7) 0.065(5) 0.025(3) -0.001(3) 0.001(4) -0.045(5) C3 0.041(4) 0.032(3) 0.070(5) -0.007(3) 0.012(3) 0.008(3) O7 0.045(2) 0.066(2) 0.058(2) -0.0003(19) -0.0077(18) -0.0123(19) C01 0.062(3) 0.076(3) 0.070(3) -0.009(2) -0.012(2) -0.010(2) C02 0.068(3) 0.081(3) 0.077(3) -0.011(2) -0.004(2) -0.009(3) C03 0.067(3) 0.088(3) 0.087(3) -0.016(3) -0.001(3) -0.002(3) C04 0.051(2) 0.071(3) 0.069(3) -0.004(2) -0.001(2) -0.001(2) O8 0.054(2) 0.059(2) 0.081(2) -0.009(2) 0.009(2) -0.001(2) C05 0.070(3) 0.076(3) 0.088(3) -0.007(3) 0.003(3) -0.001(3) C06 0.076(3) 0.085(3) 0.093(3) -0.009(3) 0.001(3) 0.004(3) C07 0.067(3) 0.086(3) 0.089(3) -0.008(3) 0.000(3) 0.003(3) C08 0.055(2) 0.074(3) 0.080(3) -0.009(2) 0.002(2) -0.001(2) O9 0.051(2) 0.059(2) 0.062(2) 0.0047(19) -0.0157(18) -0.0048(19) C4 0.061(3) 0.077(3) 0.078(3) -0.007(2) -0.015(2) -0.004(2) C5 0.068(3) 0.089(3) 0.076(3) -0.009(3) -0.011(2) 0.008(3) C6 0.078(3) 0.088(3) 0.078(3) 0.001(3) -0.006(3) 0.006(3) C7 0.070(3) 0.074(3) 0.079(3) 0.010(2) -0.012(2) -0.002(3) C11 0.026(3) 0.018(3) 0.039(3) 0.002(2) -0.005(2) -0.001(2) C12 0.035(3) 0.045(4) 0.035(3) 0.016(3) -0.003(3) -0.010(3) C13 0.061(5) 0.067(5) 0.054(4) 0.021(4) -0.031(4) -0.018(4) C14 0.038(4) 0.062(5) 0.098(7) 0.017(5) -0.026(4) -0.003(4) C15 0.031(4) 0.046(4) 0.085(6) 0.000(4) -0.005(4) 0.002(3) C16 0.026(3) 0.029(3) 0.052(4) 0.005(3) 0.003(3) -0.005(2) C17 0.042(4) 0.033(4) 0.106(6) -0.007(4) 0.002(4) 0.015(3) C18 0.039(3) 0.035(3) 0.056(4) 0.002(3) -0.005(3) -0.005(3) C19 0.077(5) 0.046(4) 0.060(4) 0.018(3) -0.031(4) -0.010(4) C21 0.034(3) 0.028(3) 0.034(3) -0.005(2) 0.005(2) -0.009(2) C22 0.053(4) 0.038(3) 0.035(3) 0.001(3) 0.000(3) -0.013(3) C23 0.067(5) 0.072(5) 0.040(4) 0.011(4) 0.013(4) -0.001(4) C24 0.056(5) 0.073(5) 0.052(4) 0.007(4) 0.028(4) -0.003(4) C25 0.043(4) 0.070(5) 0.064(5) 0.008(4) 0.015(4) 0.002(4) C26 0.030(3) 0.041(3) 0.043(3) -0.005(3) 0.011(3) -0.006(3) C27 0.044(4) 0.050(4) 0.077(5) -0.016(4) 0.008(4) -0.004(3) C28 0.039(3) 0.032(3) 0.057(4) -0.003(3) 0.002(3) 0.006(3) C29 0.048(4) 0.057(4) 0.038(3) -0.013(3) -0.009(3) 0.010(3) C121 0.058(4) 0.084(5) 0.026(3) -0.011(3) 0.003(3) -0.035(4) C122 0.108(7) 0.154(9) 0.037(4) 0.031(5) -0.014(4) -0.080(7) C123 0.096(7) 0.101(7) 0.072(6) -0.035(5) 0.030(5) -0.031(6) C161 0.029(3) 0.039(3) 0.055(4) -0.012(3) 0.012(3) -0.006(3) C162 0.052(4) 0.059(5) 0.090(6) -0.027(4) 0.023(4) 0.007(4) C163 0.074(5) 0.050(4) 0.059(4) 0.001(3) 0.027(4) -0.020(4) C221 0.061(4) 0.048(4) 0.038(3) 0.008(3) -0.005(3) -0.015(3) C222 0.104(7) 0.065(5) 0.053(5) 0.011(4) -0.026(5) -0.018(5) C223 0.086(6) 0.058(5) 0.068(5) 0.014(4) -0.019(5) -0.010(5) C261 0.018(3) 0.048(4) 0.060(4) -0.006(3) 0.005(3) 0.005(3) C262 0.061(5) 0.062(5) 0.063(5) -0.003(4) -0.014(4) -0.006(4) C263 0.043(4) 0.052(4) 0.083(5) 0.014(4) -0.013(4) 0.002(3) Al4 0.0306(8) 0.0298(9) 0.0258(8) 0.0006(7) -0.0055(7) 0.0033(7) Al5 0.0189(7) 0.0270(8) 0.0317(8) 0.0016(7) 0.0014(7) -0.0015(7) Al6 0.0170(7) 0.0256(8) 0.0258(8) 0.0029(6) 0.0023(6) -0.0013(6) Si5 0.0179(6) 0.0248(7) 0.0240(7) 0.0034(6) 0.0003(5) -0.0006(6) Si6 0.0205(7) 0.0254(7) 0.0215(7) -0.0005(6) -0.0002(6) 0.0017(6) Si7 0.0241(7) 0.0266(8) 0.0402(9) -0.0025(6) 0.0032(7) 0.0001(6) Si8 0.0311(8) 0.0264(8) 0.0374(9) 0.0009(7) 0.0079(7) 0.0016(7) N3 0.018(2) 0.027(2) 0.036(2) 0.0031(19) 0.0007(18) 0.0009(18) N4 0.019(2) 0.021(2) 0.021(2) -0.0026(16) 0.0020(17) -0.0009(17) O11 0.031(2) 0.031(2) 0.0256(19) 0.0082(15) 0.0014(16) -0.0010(17) O12 0.0198(17) 0.031(2) 0.036(2) -0.0025(16) 0.0009(15) -0.0011(15) O13 0.0250(19) 0.0271(19) 0.038(2) 0.0088(16) 0.0025(16) 0.0034(16) O14 0.033(2) 0.038(2) 0.0224(18) -0.0025(16) -0.0008(15) 0.0085(17) O15 0.0229(18) 0.0252(19) 0.040(2) -0.0037(16) -0.0035(16) -0.0012(15) O16 0.0230(18) 0.0261(19) 0.040(2) -0.0016(16) 0.0050(16) 0.0022(16) C31 0.021(3) 0.026(3) 0.042(3) 0.006(2) -0.005(2) 0.005(2) C32 0.040(3) 0.031(3) 0.038(3) 0.009(3) -0.004(3) 0.008(3) C33 0.059(5) 0.067(5) 0.049(4) 0.015(4) -0.016(4) -0.002(4) C34 0.047(4) 0.088(6) 0.061(5) 0.019(4) -0.031(4) 0.000(4) C35 0.022(3) 0.078(5) 0.081(6) 0.017(4) -0.011(3) -0.002(3) C36 0.025(3) 0.030(3) 0.046(3) 0.001(3) -0.007(3) -0.001(2) C37 0.038(4) 0.041(4) 0.079(5) -0.008(3) 0.009(3) 0.012(3) C38 0.038(3) 0.040(3) 0.050(4) -0.004(3) 0.007(3) -0.008(3) C39 0.039(4) 0.052(4) 0.036(3) -0.009(3) 0.006(3) -0.006(3) C41 0.027(3) 0.027(3) 0.030(3) -0.002(2) 0.003(2) 0.004(2) C42 0.022(3) 0.031(3) 0.049(4) -0.002(3) 0.000(3) 0.005(2) C43 0.029(3) 0.054(4) 0.078(5) 0.000(4) 0.007(3) -0.002(3) C44 0.035(4) 0.073(5) 0.078(6) -0.001(4) 0.027(4) 0.010(4) C45 0.056(4) 0.054(4) 0.043(4) 0.003(3) 0.026(3) 0.018(4) C46 0.038(3) 0.038(3) 0.028(3) 0.004(2) 0.011(2) 0.011(3) C47 0.072(5) 0.045(4) 0.041(4) 0.012(3) 0.019(3) 0.007(4) C48 0.028(3) 0.038(4) 0.096(6) 0.000(4) 0.004(4) -0.005(3) C49 0.047(4) 0.022(3) 0.051(4) 0.001(3) 0.003(3) 0.005(3) C51 0.110(7) 0.053(4) 0.022(3) -0.001(3) -0.015(4) 0.023(4) C52 0.034(3) 0.036(3) 0.067(4) -0.007(3) -0.010(3) -0.006(3) C53 0.027(3) 0.044(4) 0.052(4) 0.010(3) 0.004(3) -0.013(3) O17 0.0390(18) 0.047(2) 0.067(2) 0.0007(18) -0.0098(18) -0.0032(17) C54 0.056(2) 0.053(2) 0.057(2) 0.002(2) -0.004(2) -0.003(2) C55 0.059(3) 0.071(3) 0.073(3) 0.005(2) 0.000(2) -0.008(2) C56 0.052(2) 0.071(3) 0.074(3) 0.000(2) 0.000(2) -0.006(2) C57 0.046(2) 0.063(3) 0.066(3) 0.003(2) -0.008(2) 0.001(2) O18 0.0437(19) 0.052(2) 0.0488(19) 0.0098(17) 0.0142(17) 0.0010(18) C58 0.061(3) 0.069(3) 0.068(3) 0.008(2) 0.016(2) 0.004(2) C59 0.073(3) 0.083(3) 0.065(3) 0.000(3) 0.010(2) 0.001(3) C60 0.067(3) 0.077(3) 0.062(3) 0.010(2) 0.001(2) -0.005(3) C61 0.061(3) 0.065(3) 0.061(3) 0.017(2) 0.009(2) 0.002(2) O19 0.0298(17) 0.0466(19) 0.0341(17) -0.0017(16) 0.0012(15) 0.0031(16) C62 0.046(2) 0.061(3) 0.051(2) -0.008(2) 0.003(2) 0.007(2) C63 0.059(3) 0.071(3) 0.057(3) -0.003(2) -0.004(2) 0.002(2) C64 0.059(3) 0.078(3) 0.072(3) -0.009(2) -0.004(2) 0.000(2) C65 0.027(3) 0.083(5) 0.033(3) -0.013(3) -0.005(2) 0.000(3) C321 0.050(4) 0.049(4) 0.037(3) 0.014(3) 0.010(3) 0.004(3) C322 0.084(6) 0.061(5) 0.049(4) 0.023(4) 0.021(4) 0.017(4) C323 0.065(5) 0.040(4) 0.085(6) 0.022(4) 0.008(4) -0.005(4) C361 0.015(3) 0.046(4) 0.051(4) 0.009(3) 0.002(2) 0.000(2) C362 0.035(4) 0.058(5) 0.085(6) 0.004(4) 0.016(4) -0.003(3) C363 0.026(3) 0.049(4) 0.074(5) 0.015(3) 0.010(3) 0.005(3) C421 0.025(3) 0.039(3) 0.050(4) -0.010(3) -0.010(3) 0.002(3) C422 0.050(4) 0.063(5) 0.076(5) -0.001(4) -0.022(4) 0.017(4) C423 0.039(4) 0.055(5) 0.093(6) -0.017(4) -0.021(4) -0.002(3) C461 0.052(4) 0.068(4) 0.023(3) -0.013(3) -0.001(3) 0.019(4) C462 0.059(5) 0.079(5) 0.050(4) -0.029(4) -0.006(4) 0.006(4) C463 0.095(7) 0.102(7) 0.042(4) -0.007(4) -0.012(4) 0.035(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O4 1.716(4) . ? Al1 O1 1.719(4) . ? Al1 O7 1.904(5) . ? Al1 C1 1.928(7) . ? Al2 O5 1.706(4) . ? Al2 O2 1.716(4) . ? Al2 O8 1.900(5) . ? Al2 C2 1.958(6) . ? Al3 O3 1.725(4) . ? Al3 O6 1.730(4) . ? Al3 O9 1.881(5) . ? Al3 C3 1.929(6) . ? Si1 O1 1.602(4) . ? Si1 O3 1.608(4) . ? Si1 O2 1.609(4) . ? Si1 N1 1.729(4) . ? Si2 O6 1.609(4) . ? Si2 O5 1.610(4) . ? Si2 O4 1.618(4) . ? Si2 N2 1.741(4) . ? Si3 N1 1.747(4) . ? Si3 C18 1.856(6) . ? Si3 C17 1.864(7) . ? Si3 C19 1.869(7) . ? Si4 N2 1.738(4) . ? Si4 C29 1.854(6) . ? Si4 C27 1.854(7) . ? Si4 C28 1.878(6) . ? N1 C11 1.428(7) . ? N2 C21 1.451(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O7 C01 1.446(8) . ? O7 C04 1.467(8) . ? C01 C02 1.492(11) . ? C01 H01A 0.9900 . ? C01 H01B 0.9900 . ? C02 C03 1.432(11) . ? C02 H02A 0.9900 . ? C02 H02B 0.9900 . ? C03 C04 1.471(11) . ? C03 H03A 0.9900 . ? C03 H03B 0.9900 . ? C04 H04A 0.9900 . ? C04 H04B 0.9900 . ? O8 C05 1.436(9) . ? O8 C08 1.466(9) . ? C05 C06 1.470(12) . ? C05 H05A 0.9900 . ? C05 H05B 0.9900 . ? C06 C07 1.459(12) . ? C06 H06A 0.9900 . ? C06 H06B 0.9900 . ? C07 C08 1.473(11) . ? C07 H07A 0.9900 . ? C07 H07B 0.9900 . ? C08 H08A 0.9900 . ? C08 H08B 0.9900 . ? O9 C7 1.457(9) . ? O9 C4 1.457(9) . ? C4 C5 1.480(11) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.456(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.456(11) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C11 C16 1.402(8) . ? C11 C12 1.422(8) . ? C12 C13 1.380(9) . ? C12 C121 1.537(9) . ? C13 C14 1.338(11) . ? C13 H13A 0.9500 . ? C14 C15 1.377(11) . ? C14 H14A 0.9500 . ? C15 C16 1.394(9) . ? C15 H15A 0.9500 . ? C16 C161 1.527(9) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C26 1.407(8) . ? C21 C22 1.411(8) . ? C22 C23 1.397(9) . ? C22 C221 1.533(9) . ? C23 C24 1.369(10) . ? C23 H23A 0.9500 . ? C24 C25 1.357(10) . ? C24 H24A 0.9500 . ? C25 C26 1.392(9) . ? C25 H25A 0.9500 . ? C26 C261 1.499(9) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C121 C123 1.529(10) . ? C121 C122 1.535(10) . ? C121 H12A 1.0000 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C122 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C123 H12G 0.9800 . ? C161 C162 1.508(8) . ? C161 C163 1.548(9) . ? C161 H16A 1.0000 . ? C162 H16B 0.9800 . ? C162 H16C 0.9800 . ? C162 H16D 0.9800 . ? C163 H16E 0.9800 . ? C163 H16F 0.9800 . ? C163 H16G 0.9800 . ? C221 C223 1.529(10) . ? C221 C222 1.537(9) . ? C221 H22A 1.0000 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C222 H22D 0.9800 . ? C223 H22E 0.9800 . ? C223 H22F 0.9800 . ? C223 H22G 0.9800 . ? C261 C263 1.521(9) . ? C261 C262 1.535(9) . ? C261 H26A 1.0000 . ? C262 H26B 0.9800 . ? C262 H26C 0.9800 . ? C262 H26D 0.9800 . ? C263 H26E 0.9800 . ? C263 H26F 0.9800 . ? C263 H26G 0.9800 . ? Al4 O14 1.709(4) . ? Al4 O11 1.714(4) . ? Al4 O17 1.890(5) . ? Al4 C51 1.929(6) . ? Al5 O15 1.716(4) . ? Al5 O12 1.718(4) . ? Al5 O18 1.888(4) . ? Al5 C52 1.959(6) . ? Al6 O13 1.717(4) . ? Al6 O16 1.725(4) . ? Al6 O19 1.893(4) . ? Al6 C53 1.946(5) . ? Si5 O11 1.611(4) . ? Si5 O12 1.618(4) . ? Si5 O13 1.620(4) . ? Si5 N3 1.740(4) . ? Si6 O16 1.605(4) . ? Si6 O14 1.607(4) . ? Si6 O15 1.610(4) . ? Si6 N4 1.746(4) . ? Si7 N3 1.740(5) . ? Si7 C39 1.857(6) . ? Si7 C37 1.859(6) . ? Si7 C38 1.872(6) . ? Si8 N4 1.728(4) . ? Si8 C47 1.856(6) . ? Si8 C48 1.859(6) . ? Si8 C49 1.865(6) . ? N3 C31 1.440(7) . ? N4 C41 1.446(6) . ? C31 C32 1.398(8) . ? C31 C36 1.418(8) . ? C32 C33 1.406(9) . ? C32 C321 1.508(9) . ? C33 C34 1.371(10) . ? C33 H33A 0.9500 . ? C34 C35 1.356(10) . ? C34 H34A 0.9500 . ? C35 C36 1.405(8) . ? C35 H35A 0.9500 . ? C36 C361 1.499(8) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C41 C42 1.400(8) . ? C41 C46 1.412(7) . ? C42 C43 1.395(8) . ? C42 C421 1.528(8) . ? C43 C44 1.350(10) . ? C43 H43A 0.9500 . ? C44 C45 1.363(10) . ? C44 H44A 0.9500 . ? C45 C46 1.407(8) . ? C45 H45A 0.9500 . ? C46 C461 1.498(9) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? O17 C54 1.429(8) . ? O17 C57 1.470(8) . ? C54 C55 1.472(10) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.458(10) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.465(10) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? O18 C61 1.423(8) . ? O18 C58 1.454(8) . ? C58 C59 1.375(10) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.404(11) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.506(10) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? O19 C65 1.452(7) . ? O19 C62 1.464(7) . ? C62 C63 1.482(9) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.460(10) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.465(10) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C321 C322 1.517(9) . ? C321 C323 1.546(9) . ? C321 H32A 1.0000 . ? C322 H32B 0.9800 . ? C322 H32C 0.9800 . ? C322 H32D 0.9800 . ? C323 H32E 0.9800 . ? C323 H32F 0.9800 . ? C323 H32G 0.9800 . ? C361 C363 1.529(8) . ? C361 C362 1.543(8) . ? C361 H36A 1.0000 . ? C362 H36B 0.9800 . ? C362 H36C 0.9800 . ? C362 H36D 0.9800 . ? C363 H36E 0.9800 . ? C363 H36F 0.9800 . ? C363 H36G 0.9800 . ? C421 C423 1.516(8) . ? C421 C422 1.539(9) . ? C421 H42A 1.0000 . ? C422 H42B 0.9800 . ? C422 H42C 0.9800 . ? C422 H42D 0.9800 . ? C423 H42E 0.9800 . ? C423 H42F 0.9800 . ? C423 H42G 0.9800 . ? C461 C463 1.526(10) . ? C461 C462 1.557(10) . ? C461 H46A 1.0000 . ? C462 H46B 0.9800 . ? C462 H46C 0.9800 . ? C462 H46D 0.9800 . ? C463 H46E 0.9800 . ? C463 H46F 0.9800 . ? C463 H46G 0.9800 . ? O21 C71 1.43(3) . ? O21 C74 1.47(3) . ? C71 C72 1.45(3) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.49(3) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.50(3) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? O21A C74A 1.43(3) . ? O21A C71A 1.45(2) . ? C71A C72A 1.40(3) . ? C71A H71C 0.9900 . ? C71A H71D 0.9900 . ? C72A C73A 1.51(3) . ? C72A H72C 0.9900 . ? C72A H72D 0.9900 . ? C73A C74A 1.45(3) . ? C73A H73C 0.9900 . ? C73A H73D 0.9900 . ? C74A H74C 0.9900 . ? C74A H74D 0.9900 . ? O22 C78 1.49(2) . ? O22 C75 1.54(2) . ? C75 C76 1.37(2) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 C77 1.37(2) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C78 1.49(3) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 H78A 0.9900 . ? C78 H78B 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 O4 Al1 O1 113.8(2) . . ? O4 Al1 O7 103.5(2) . . ? O1 Al1 O7 102.3(2) . . ? O4 Al1 C1 117.6(3) . . ? O1 Al1 C1 114.5(3) . . ? O7 Al1 C1 102.2(3) . . ? O5 Al2 O2 114.7(2) . . ? O5 Al2 O8 100.7(2) . . ? O2 Al2 O8 103.7(2) . . ? O5 Al2 C2 116.0(3) . . ? O2 Al2 C2 115.1(3) . . ? O8 Al2 C2 103.8(3) . . ? O3 Al3 O6 114.07(19) . . ? O3 Al3 O9 100.0(2) . . ? O6 Al3 O9 102.9(2) . . ? O3 Al3 C3 116.8(2) . . ? O6 Al3 C3 114.3(2) . . ? O9 Al3 C3 106.3(3) . . ? O1 Si1 O3 110.5(2) . . ? O1 Si1 O2 110.9(2) . . ? O3 Si1 O2 110.0(2) . . ? O1 Si1 N1 105.9(2) . . ? O3 Si1 N1 109.9(2) . . ? O2 Si1 N1 109.6(2) . . ? O6 Si2 O5 110.8(2) . . ? O6 Si2 O4 110.2(2) . . ? O5 Si2 O4 109.4(2) . . ? O6 Si2 N2 106.5(2) . . ? O5 Si2 N2 108.3(2) . . ? O4 Si2 N2 111.6(2) . . ? N1 Si3 C18 108.8(3) . . ? N1 Si3 C17 111.4(3) . . ? C18 Si3 C17 108.2(3) . . ? N1 Si3 C19 111.5(3) . . ? C18 Si3 C19 108.5(3) . . ? C17 Si3 C19 108.4(4) . . ? N2 Si4 C29 110.2(3) . . ? N2 Si4 C27 110.4(3) . . ? C29 Si4 C27 107.9(3) . . ? N2 Si4 C28 112.7(3) . . ? C29 Si4 C28 108.0(3) . . ? C27 Si4 C28 107.5(3) . . ? C11 N1 Si1 117.9(3) . . ? C11 N1 Si3 119.7(3) . . ? Si1 N1 Si3 122.4(3) . . ? C21 N2 Si4 121.8(3) . . ? C21 N2 Si2 115.7(3) . . ? Si4 N2 Si2 122.5(2) . . ? Si1 O1 Al1 137.7(2) . . ? Si1 O2 Al2 138.7(2) . . ? Si1 O3 Al3 141.6(2) . . ? Si2 O4 Al1 143.0(2) . . ? Si2 O5 Al2 135.7(2) . . ? Si2 O6 Al3 137.2(2) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Al2 C2 H2A 109.5 . . ? Al2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Al2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Al3 C3 H3A 109.5 . . ? Al3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Al3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C01 O7 C04 110.1(6) . . ? C01 O7 Al1 119.9(4) . . ? C04 O7 Al1 127.3(4) . . ? O7 C01 C02 105.6(6) . . ? O7 C01 H01A 110.6 . . ? C02 C01 H01A 110.6 . . ? O7 C01 H01B 110.6 . . ? C02 C01 H01B 110.6 . . ? H01A C01 H01B 108.7 . . ? C03 C02 C01 107.4(7) . . ? C03 C02 H02A 110.2 . . ? C01 C02 H02A 110.2 . . ? C03 C02 H02B 110.2 . . ? C01 C02 H02B 110.2 . . ? H02A C02 H02B 108.5 . . ? C02 C03 C04 108.3(7) . . ? C02 C03 H03A 110.0 . . ? C04 C03 H03A 110.0 . . ? C02 C03 H03B 110.0 . . ? C04 C03 H03B 110.0 . . ? H03A C03 H03B 108.4 . . ? O7 C04 C03 104.7(6) . . ? O7 C04 H04A 110.8 . . ? C03 C04 H04A 110.8 . . ? O7 C04 H04B 110.8 . . ? C03 C04 H04B 110.8 . . ? H04A C04 H04B 108.9 . . ? C05 O8 C08 110.1(6) . . ? C05 O8 Al2 125.5(5) . . ? C08 O8 Al2 121.8(4) . . ? O8 C05 C06 102.4(7) . . ? O8 C05 H05A 111.3 . . ? C06 C05 H05A 111.3 . . ? O8 C05 H05B 111.3 . . ? C06 C05 H05B 111.3 . . ? H05A C05 H05B 109.2 . . ? C07 C06 C05 105.4(8) . . ? C07 C06 H06A 110.7 . . ? C05 C06 H06A 110.7 . . ? C07 C06 H06B 110.7 . . ? C05 C06 H06B 110.7 . . ? H06A C06 H06B 108.8 . . ? C06 C07 C08 103.4(7) . . ? C06 C07 H07A 111.1 . . ? C08 C07 H07A 111.1 . . ? C06 C07 H07B 111.1 . . ? C08 C07 H07B 111.1 . . ? H07A C07 H07B 109.0 . . ? O8 C08 C07 104.3(6) . . ? O8 C08 H08A 110.9 . . ? C07 C08 H08A 110.9 . . ? O8 C08 H08B 110.9 . . ? C07 C08 H08B 110.9 . . ? H08A C08 H08B 108.9 . . ? C7 O9 C4 109.1(6) . . ? C7 O9 Al3 126.7(4) . . ? C4 O9 Al3 123.2(5) . . ? O9 C4 C5 103.5(7) . . ? O9 C4 H4A 111.1 . . ? C5 C4 H4A 111.1 . . ? O9 C4 H4B 111.1 . . ? C5 C4 H4B 111.1 . . ? H4A C4 H4B 109.0 . . ? C6 C5 C4 104.8(7) . . ? C6 C5 H5A 110.8 . . ? C4 C5 H5A 110.8 . . ? C6 C5 H5B 110.8 . . ? C4 C5 H5B 110.8 . . ? H5A C5 H5B 108.9 . . ? C5 C6 C7 104.5(8) . . ? C5 C6 H6A 110.9 . . ? C7 C6 H6A 110.9 . . ? C5 C6 H6B 110.9 . . ? C7 C6 H6B 110.9 . . ? H6A C6 H6B 108.9 . . ? O9 C7 C6 105.1(7) . . ? O9 C7 H7A 110.7 . . ? C6 C7 H7A 110.7 . . ? O9 C7 H7B 110.7 . . ? C6 C7 H7B 110.7 . . ? H7A C7 H7B 108.8 . . ? C16 C11 C12 118.0(5) . . ? C16 C11 N1 121.1(5) . . ? C12 C11 N1 120.9(5) . . ? C13 C12 C11 119.2(6) . . ? C13 C12 C121 119.6(6) . . ? C11 C12 C121 121.2(5) . . ? C14 C13 C12 122.2(7) . . ? C14 C13 H13A 118.9 . . ? C12 C13 H13A 118.9 . . ? C13 C14 C15 120.3(7) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C14 C15 C16 120.2(7) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C15 C16 C11 120.0(6) . . ? C15 C16 C161 118.3(6) . . ? C11 C16 C161 121.7(5) . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si3 C19 H19A 109.5 . . ? Si3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C26 C21 C22 120.2(5) . . ? C26 C21 N2 121.0(5) . . ? C22 C21 N2 118.8(5) . . ? C23 C22 C21 118.0(6) . . ? C23 C22 C221 119.3(6) . . ? C21 C22 C221 122.5(6) . . ? C24 C23 C22 121.9(6) . . ? C24 C23 H23A 119.1 . . ? C22 C23 H23A 119.1 . . ? C25 C24 C23 119.3(7) . . ? C25 C24 H24A 120.3 . . ? C23 C24 H24A 120.3 . . ? C24 C25 C26 122.5(7) . . ? C24 C25 H25A 118.8 . . ? C26 C25 H25A 118.8 . . ? C25 C26 C21 118.1(6) . . ? C25 C26 C261 118.9(6) . . ? C21 C26 C261 123.0(5) . . ? Si4 C27 H27A 109.5 . . ? Si4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si4 C29 H29A 109.5 . . ? Si4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C123 C121 C122 111.3(6) . . ? C123 C121 C12 110.9(6) . . ? C122 C121 C12 110.2(7) . . ? C123 C121 H12A 108.1 . . ? C122 C121 H12A 108.1 . . ? C12 C121 H12A 108.1 . . ? C121 C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C122 H12D 109.5 . . ? H12B C122 H12D 109.5 . . ? H12C C122 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C121 C123 H12G 109.5 . . ? H12E C123 H12G 109.5 . . ? H12F C123 H12G 109.5 . . ? C162 C161 C16 112.0(6) . . ? C162 C161 C163 110.0(5) . . ? C16 C161 C163 109.7(5) . . ? C162 C161 H16A 108.3 . . ? C16 C161 H16A 108.3 . . ? C163 C161 H16A 108.3 . . ? C161 C162 H16B 109.5 . . ? C161 C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C161 C162 H16D 109.5 . . ? H16B C162 H16D 109.5 . . ? H16C C162 H16D 109.5 . . ? C161 C163 H16E 109.5 . . ? C161 C163 H16F 109.5 . . ? H16E C163 H16F 109.5 . . ? C161 C163 H16G 109.5 . . ? H16E C163 H16G 109.5 . . ? H16F C163 H16G 109.5 . . ? C223 C221 C22 111.7(6) . . ? C223 C221 C222 108.8(6) . . ? C22 C221 C222 113.4(6) . . ? C223 C221 H22A 107.6 . . ? C22 C221 H22A 107.6 . . ? C222 C221 H22A 107.6 . . ? C221 C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C221 C222 H22D 109.5 . . ? H22B C222 H22D 109.5 . . ? H22C C222 H22D 109.5 . . ? C221 C223 H22E 109.5 . . ? C221 C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C221 C223 H22G 109.5 . . ? H22E C223 H22G 109.5 . . ? H22F C223 H22G 109.5 . . ? C26 C261 C263 112.6(5) . . ? C26 C261 C262 111.5(6) . . ? C263 C261 C262 109.1(5) . . ? C26 C261 H26A 107.8 . . ? C263 C261 H26A 107.8 . . ? C262 C261 H26A 107.8 . . ? C261 C262 H26B 109.5 . . ? C261 C262 H26C 109.5 . . ? H26B C262 H26C 109.5 . . ? C261 C262 H26D 109.5 . . ? H26B C262 H26D 109.5 . . ? H26C C262 H26D 109.5 . . ? C261 C263 H26E 109.5 . . ? C261 C263 H26F 109.5 . . ? H26E C263 H26F 109.5 . . ? C261 C263 H26G 109.5 . . ? H26E C263 H26G 109.5 . . ? H26F C263 H26G 109.5 . . ? O14 Al4 O11 113.88(19) . . ? O14 Al4 O17 103.4(2) . . ? O11 Al4 O17 101.9(2) . . ? O14 Al4 C51 117.3(3) . . ? O11 Al4 C51 114.6(2) . . ? O17 Al4 C51 103.0(3) . . ? O15 Al5 O12 114.83(19) . . ? O15 Al5 O18 99.2(2) . . ? O12 Al5 O18 103.47(19) . . ? O15 Al5 C52 116.3(2) . . ? O12 Al5 C52 112.9(2) . . ? O18 Al5 C52 107.9(3) . . ? O13 Al6 O16 114.17(19) . . ? O13 Al6 O19 102.36(19) . . ? O16 Al6 O19 102.19(18) . . ? O13 Al6 C53 118.0(2) . . ? O16 Al6 C53 114.5(2) . . ? O19 Al6 C53 102.6(2) . . ? O11 Si5 O12 110.87(19) . . ? O11 Si5 O13 109.9(2) . . ? O12 Si5 O13 110.3(2) . . ? O11 Si5 N3 108.0(2) . . ? O12 Si5 N3 106.6(2) . . ? O13 Si5 N3 110.97(19) . . ? O16 Si6 O14 111.2(2) . . ? O16 Si6 O15 110.6(2) . . ? O14 Si6 O15 109.6(2) . . ? O16 Si6 N4 105.47(19) . . ? O14 Si6 N4 109.79(19) . . ? O15 Si6 N4 110.09(19) . . ? N3 Si7 C39 109.8(2) . . ? N3 Si7 C37 109.1(3) . . ? C39 Si7 C37 109.9(3) . . ? N3 Si7 C38 113.2(2) . . ? C39 Si7 C38 107.2(3) . . ? C37 Si7 C38 107.6(3) . . ? N4 Si8 C47 112.5(3) . . ? N4 Si8 C48 111.6(3) . . ? C47 Si8 C48 107.8(3) . . ? N4 Si8 C49 108.8(2) . . ? C47 Si8 C49 108.7(3) . . ? C48 Si8 C49 107.2(3) . . ? C31 N3 Si7 121.7(3) . . ? C31 N3 Si5 115.4(3) . . ? Si7 N3 Si5 122.9(2) . . ? C41 N4 Si8 120.5(3) . . ? C41 N4 Si6 117.3(3) . . ? Si8 N4 Si6 122.3(2) . . ? Si5 O11 Al4 136.0(2) . . ? Si5 O12 Al5 136.2(2) . . ? Si5 O13 Al6 143.6(2) . . ? Si6 O14 Al4 140.9(2) . . ? Si6 O15 Al5 141.5(2) . . ? Si6 O16 Al6 137.1(2) . . ? C32 C31 C36 120.0(5) . . ? C32 C31 N3 120.4(5) . . ? C36 C31 N3 119.6(5) . . ? C31 C32 C33 119.2(6) . . ? C31 C32 C321 121.4(5) . . ? C33 C32 C321 119.4(5) . . ? C34 C33 C32 121.0(6) . . ? C34 C33 H33A 119.5 . . ? C32 C33 H33A 119.5 . . ? C35 C34 C33 119.5(6) . . ? C35 C34 H34A 120.3 . . ? C33 C34 H34A 120.3 . . ? C34 C35 C36 123.0(6) . . ? C34 C35 H35A 118.5 . . ? C36 C35 H35A 118.5 . . ? C35 C36 C31 117.2(6) . . ? C35 C36 C361 119.4(5) . . ? C31 C36 C361 123.3(5) . . ? Si7 C37 H37A 109.5 . . ? Si7 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si7 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si7 C38 H38A 109.5 . . ? Si7 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si7 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si7 C39 H39A 109.5 . . ? Si7 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si7 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C41 C46 120.5(5) . . ? C42 C41 N4 120.4(5) . . ? C46 C41 N4 119.1(5) . . ? C43 C42 C41 119.0(6) . . ? C43 C42 C421 118.9(5) . . ? C41 C42 C421 122.1(5) . . ? C44 C43 C42 121.0(7) . . ? C44 C43 H43A 119.5 . . ? C42 C43 H43A 119.5 . . ? C43 C44 C45 120.6(6) . . ? C43 C44 H44A 119.7 . . ? C45 C44 H44A 119.7 . . ? C44 C45 C46 121.9(6) . . ? C44 C45 H45A 119.1 . . ? C46 C45 H45A 119.1 . . ? C45 C46 C41 117.0(6) . . ? C45 C46 C461 119.0(5) . . ? C41 C46 C461 123.9(5) . . ? Si8 C47 H47A 109.5 . . ? Si8 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si8 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si8 C48 H48A 109.5 . . ? Si8 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si8 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Si8 C49 H49A 109.5 . . ? Si8 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? Si8 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? Al4 C51 H51A 109.5 . . ? Al4 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Al4 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Al5 C52 H52A 109.5 . . ? Al5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Al5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Al6 C53 H53A 109.5 . . ? Al6 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Al6 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C54 O17 C57 110.0(5) . . ? C54 O17 Al4 128.1(4) . . ? C57 O17 Al4 121.4(4) . . ? O17 C54 C55 106.3(6) . . ? O17 C54 H54A 110.5 . . ? C55 C54 H54A 110.5 . . ? O17 C54 H54B 110.5 . . ? C55 C54 H54B 110.5 . . ? H54A C54 H54B 108.7 . . ? C56 C55 C54 107.2(7) . . ? C56 C55 H55A 110.3 . . ? C54 C55 H55A 110.3 . . ? C56 C55 H55B 110.3 . . ? C54 C55 H55B 110.3 . . ? H55A C55 H55B 108.5 . . ? C55 C56 C57 106.8(6) . . ? C55 C56 H56A 110.4 . . ? C57 C56 H56A 110.4 . . ? C55 C56 H56B 110.4 . . ? C57 C56 H56B 110.4 . . ? H56A C56 H56B 108.6 . . ? C56 C57 O17 104.5(6) . . ? C56 C57 H57A 110.9 . . ? O17 C57 H57A 110.9 . . ? C56 C57 H57B 110.9 . . ? O17 C57 H57B 110.9 . . ? H57A C57 H57B 108.9 . . ? C61 O18 C58 108.4(5) . . ? C61 O18 Al5 125.8(4) . . ? C58 O18 Al5 125.2(4) . . ? C59 C58 O18 108.5(7) . . ? C59 C58 H58A 110.0 . . ? O18 C58 H58A 110.0 . . ? C59 C58 H58B 110.0 . . ? O18 C58 H58B 110.0 . . ? H58A C58 H58B 108.4 . . ? C58 C59 C60 108.5(7) . . ? C58 C59 H59A 110.0 . . ? C60 C59 H59A 110.0 . . ? C58 C59 H59B 110.0 . . ? C60 C59 H59B 110.0 . . ? H59A C59 H59B 108.4 . . ? C59 C60 C61 107.1(7) . . ? C59 C60 H60A 110.3 . . ? C61 C60 H60A 110.3 . . ? C59 C60 H60B 110.3 . . ? C61 C60 H60B 110.3 . . ? H60A C60 H60B 108.5 . . ? O18 C61 C60 103.6(6) . . ? O18 C61 H61A 111.0 . . ? C60 C61 H61A 111.0 . . ? O18 C61 H61B 111.0 . . ? C60 C61 H61B 111.0 . . ? H61A C61 H61B 109.0 . . ? C65 O19 C62 109.9(4) . . ? C65 O19 Al6 127.4(3) . . ? C62 O19 Al6 118.7(4) . . ? O19 C62 C63 105.1(5) . . ? O19 C62 H62A 110.7 . . ? C63 C62 H62A 110.7 . . ? O19 C62 H62B 110.7 . . ? C63 C62 H62B 110.7 . . ? H62A C62 H62B 108.8 . . ? C64 C63 C62 105.2(6) . . ? C64 C63 H63A 110.7 . . ? C62 C63 H63A 110.7 . . ? C64 C63 H63B 110.7 . . ? C62 C63 H63B 110.7 . . ? H63A C63 H63B 108.8 . . ? C63 C64 C65 106.7(6) . . ? C63 C64 H64A 110.4 . . ? C65 C64 H64A 110.4 . . ? C63 C64 H64B 110.4 . . ? C65 C64 H64B 110.4 . . ? H64A C64 H64B 108.6 . . ? O19 C65 C64 104.1(5) . . ? O19 C65 H65A 110.9 . . ? C64 C65 H65A 110.9 . . ? O19 C65 H65B 110.9 . . ? C64 C65 H65B 110.9 . . ? H65A C65 H65B 109.0 . . ? C32 C321 C322 112.9(6) . . ? C32 C321 C323 110.3(6) . . ? C322 C321 C323 109.1(5) . . ? C32 C321 H32A 108.1 . . ? C322 C321 H32A 108.1 . . ? C323 C321 H32A 108.1 . . ? C321 C322 H32B 109.5 . . ? C321 C322 H32C 109.5 . . ? H32B C322 H32C 109.5 . . ? C321 C322 H32D 109.5 . . ? H32B C322 H32D 109.5 . . ? H32C C322 H32D 109.5 . . ? C321 C323 H32E 109.5 . . ? C321 C323 H32F 109.5 . . ? H32E C323 H32F 109.5 . . ? C321 C323 H32G 109.5 . . ? H32E C323 H32G 109.5 . . ? H32F C323 H32G 109.5 . . ? C36 C361 C363 112.9(5) . . ? C36 C361 C362 112.5(5) . . ? C363 C361 C362 108.2(5) . . ? C36 C361 H36A 107.7 . . ? C363 C361 H36A 107.7 . . ? C362 C361 H36A 107.7 . . ? C361 C362 H36B 109.5 . . ? C361 C362 H36C 109.5 . . ? H36B C362 H36C 109.5 . . ? C361 C362 H36D 109.5 . . ? H36B C362 H36D 109.5 . . ? H36C C362 H36D 109.5 . . ? C361 C363 H36E 109.5 . . ? C361 C363 H36F 109.5 . . ? H36E C363 H36F 109.5 . . ? C361 C363 H36G 109.5 . . ? H36E C363 H36G 109.5 . . ? H36F C363 H36G 109.5 . . ? C423 C421 C42 114.4(6) . . ? C423 C421 C422 109.2(5) . . ? C42 C421 C422 110.3(5) . . ? C423 C421 H42A 107.6 . . ? C42 C421 H42A 107.6 . . ? C422 C421 H42A 107.6 . . ? C421 C422 H42B 109.5 . . ? C421 C422 H42C 109.5 . . ? H42B C422 H42C 109.5 . . ? C421 C422 H42D 109.5 . . ? H42B C422 H42D 109.5 . . ? H42C C422 H42D 109.5 . . ? C421 C423 H42E 109.5 . . ? C421 C423 H42F 109.5 . . ? H42E C423 H42F 109.5 . . ? C421 C423 H42G 109.5 . . ? H42E C423 H42G 109.5 . . ? H42F C423 H42G 109.5 . . ? C46 C461 C463 112.1(6) . . ? C46 C461 C462 110.8(5) . . ? C463 C461 C462 111.9(6) . . ? C46 C461 H46A 107.3 . . ? C463 C461 H46A 107.3 . . ? C462 C461 H46A 107.3 . . ? C461 C462 H46B 109.5 . . ? C461 C462 H46C 109.5 . . ? H46B C462 H46C 109.5 . . ? C461 C462 H46D 109.5 . . ? H46B C462 H46D 109.5 . . ? H46C C462 H46D 109.5 . . ? C461 C463 H46E 109.5 . . ? C461 C463 H46F 109.5 . . ? H46E C463 H46F 109.5 . . ? C461 C463 H46G 109.5 . . ? H46E C463 H46G 109.5 . . ? H46F C463 H46G 109.5 . . ? C71 O21 C74 109(3) . . ? O21 C71 C72 101(3) . . ? O21 C71 H71A 111.5 . . ? C72 C71 H71A 111.5 . . ? O21 C71 H71B 111.6 . . ? C72 C71 H71B 111.6 . . ? H71A C71 H71B 109.4 . . ? C71 C72 C73 110(3) . . ? C71 C72 H72A 109.7 . . ? C73 C72 H72A 109.7 . . ? C71 C72 H72B 109.7 . . ? C73 C72 H72B 109.7 . . ? H72A C72 H72B 108.2 . . ? C72 C73 C74 101(3) . . ? C72 C73 H73A 111.6 . . ? C74 C73 H73A 111.6 . . ? C72 C73 H73B 111.6 . . ? C74 C73 H73B 111.5 . . ? H73A C73 H73B 109.4 . . ? O21 C74 C73 107(2) . . ? O21 C74 H74A 110.3 . . ? C73 C74 H74A 110.3 . . ? O21 C74 H74B 110.3 . . ? C73 C74 H74B 110.3 . . ? H74A C74 H74B 108.6 . . ? C74A O21A C71A 108(3) . . ? C72A C71A O21A 112(2) . . ? C72A C71A H71C 109.2 . . ? O21A C71A H71C 109.3 . . ? C72A C71A H71D 109.2 . . ? O21A C71A H71D 109.3 . . ? H71C C71A H71D 107.9 . . ? C71A C72A C73A 104(3) . . ? C71A C72A H72C 111.0 . . ? C73A C72A H72C 111.0 . . ? C71A C72A H72D 111.0 . . ? C73A C72A H72D 111.0 . . ? H72C C72A H72D 109.0 . . ? C74A C73A C72A 109(3) . . ? C74A C73A H73C 109.9 . . ? C72A C73A H73C 109.9 . . ? C74A C73A H73D 109.7 . . ? C72A C73A H73D 109.9 . . ? H73C C73A H73D 108.3 . . ? O21A C74A C73A 107(3) . . ? O21A C74A H74C 110.3 . . ? C73A C74A H74C 110.3 . . ? O21A C74A H74D 110.5 . . ? C73A C74A H74D 110.5 . . ? H74C C74A H74D 108.6 . . ? C78 O22 C75 120(2) . . ? C76 C75 O22 90(2) . . ? C76 C75 H75A 113.6 . . ? O22 C75 H75A 113.6 . . ? C76 C75 H75B 113.6 . . ? O22 C75 H75B 113.6 . . ? H75A C75 H75B 110.9 . . ? C77 C76 C75 117(3) . . ? C77 C76 H76A 108.0 . . ? C75 C76 H76A 108.0 . . ? C77 C76 H76B 108.0 . . ? C75 C76 H76B 108.0 . . ? H76A C76 H76B 107.2 . . ? C76 C77 C78 108(3) . . ? C76 C77 H77A 110.1 . . ? C78 C77 H77A 110.1 . . ? C76 C77 H77B 110.1 . . ? C78 C77 H77B 110.1 . . ? H77A C77 H77B 108.4 . . ? C77 C78 O22 88(2) . . ? C77 C78 H78A 113.9 . . ? O22 C78 H78A 113.9 . . ? C77 C78 H78B 113.9 . . ? O22 C78 H78B 113.9 . . ? H78A C78 H78B 111.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.838 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.083 _database_code_depnum_ccdc_archive 'CCDC 941564'