# 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_shelxl _database_code_depnum_ccdc_archive 'CCDC 894305' #TrackingRef 'CCDC.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H59 N4 O Si4 Y' _chemical_formula_sum 'C35 H59 N4 O Si4 Y' _chemical_formula_weight 753.13 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.031(3) _cell_length_b 24.184(5) _cell_length_c 14.840(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.234(5) _cell_angle_gamma 90.00 _cell_volume 4283.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 18166 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 1.503 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.300 _exptl_absorpt_correction_T_max 0.591 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21654 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.1092 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7950 _reflns_number_gt 5493 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7950 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.2024 _refine_ls_wR_factor_gt 0.1828 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.003 _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 Y1 Y 0.12178(4) 0.349688(17) 0.26795(3) 0.04525(18) Uani 1 1 d . . . Si1 Si 0.28856(18) 0.22840(7) 0.34271(15) 0.0819(6) Uani 1 1 d . . . H1 H 0.330(6) 0.265(3) 0.416(5) 0.11(2) Uiso 1 1 d . . . Si2 Si 0.11847(18) 0.23687(7) 0.17347(13) 0.0782(5) Uani 1 1 d . . . H2 H 0.058(4) 0.282(2) 0.148(3) 0.055(13) Uiso 1 1 d . . . Si3 Si -0.14562(15) 0.32339(8) 0.26112(12) 0.0728(5) Uani 1 1 d . . . H3 H -0.078(4) 0.2756(18) 0.310(3) 0.048(12) Uiso 1 1 d . . . Si4 Si -0.09635(15) 0.44122(8) 0.20718(12) 0.0715(5) Uani 1 1 d . . . H4 H -0.001(5) 0.462(3) 0.170(4) 0.091(19) Uiso 1 1 d . . . O1 O 0.1089(3) 0.35068(13) 0.4255(2) 0.0570(9) Uani 1 1 d . . . N1 N 0.2476(3) 0.42416(15) 0.2975(2) 0.0472(9) Uani 1 1 d . . . N2 N 0.2212(3) 0.39019(15) 0.1565(2) 0.0461(9) Uani 1 1 d . . . N3 N 0.1912(4) 0.26258(16) 0.2702(3) 0.0646(12) Uani 1 1 d . . . N4 N -0.0590(4) 0.37613(19) 0.2413(3) 0.0608(11) Uani 1 1 d . . . C1 C 0.2771(4) 0.42601(18) 0.2137(3) 0.0442(10) Uani 1 1 d . . . C2 C 0.3632(4) 0.46492(18) 0.1880(3) 0.0505(11) Uani 1 1 d . . . C3 C 0.4623(4) 0.4742(2) 0.2444(4) 0.0571(12) Uani 1 1 d . . . H3A H 0.4754 0.4556 0.3003 0.068 Uiso 1 1 calc R . . C4 C 0.5418(5) 0.5103(2) 0.2199(4) 0.0660(14) Uani 1 1 d . . . H4A H 0.6091 0.5154 0.2586 0.079 Uiso 1 1 calc R . . C5 C 0.5233(5) 0.5389(2) 0.1391(4) 0.0652(14) Uani 1 1 d . . . H5 H 0.5775 0.5636 0.1227 0.078 Uiso 1 1 calc R . . C6 C 0.4249(5) 0.5309(2) 0.0826(4) 0.0638(14) Uani 1 1 d . . . H6 H 0.4115 0.5506 0.0277 0.077 Uiso 1 1 calc R . . C7 C 0.3454(4) 0.49386(19) 0.1062(3) 0.0498(11) Uani 1 1 d . . . H7 H 0.2789 0.4882 0.0668 0.060 Uiso 1 1 calc R . . C8 C 0.2834(4) 0.46332(19) 0.3671(3) 0.0525(12) Uani 1 1 d . . . C9 C 0.3503(5) 0.4436(3) 0.4459(3) 0.0683(15) Uani 1 1 d . . . C10 C 0.3780(6) 0.4760(4) 0.5204(5) 0.091(2) Uani 1 1 d . . . H10 H 0.4228 0.4619 0.5717 0.109 Uiso 1 1 calc R . . C11 C 0.3402(7) 0.5289(4) 0.5197(5) 0.097(2) Uani 1 1 d . . . H11 H 0.3575 0.5508 0.5718 0.116 Uiso 1 1 calc R . . C12 C 0.2769(6) 0.5513(3) 0.4444(5) 0.085(2) Uani 1 1 d . . . H12 H 0.2531 0.5883 0.4450 0.102 Uiso 1 1 calc R . . C13 C 0.2477(5) 0.5178(2) 0.3655(4) 0.0681(15) Uani 1 1 d . . . C14 C 0.3970(6) 0.3852(3) 0.4485(4) 0.088(2) Uani 1 1 d . . . H14A H 0.4610 0.3827 0.4951 0.132 Uiso 1 1 calc R . . H14B H 0.4202 0.3762 0.3899 0.132 Uiso 1 1 calc R . . H14C H 0.3397 0.3594 0.4620 0.132 Uiso 1 1 calc R . . C15 C 0.1791(6) 0.5413(2) 0.2821(5) 0.0815(19) Uani 1 1 d . . . H15A H 0.2285 0.5529 0.2389 0.122 Uiso 1 1 calc R . . H15B H 0.1366 0.5728 0.2993 0.122 Uiso 1 1 calc R . . H15C H 0.1279 0.5132 0.2547 0.122 Uiso 1 1 calc R . . C16 C 0.2551(4) 0.3748(2) 0.0717(3) 0.0533(12) Uani 1 1 d . . . C17 C 0.1789(6) 0.3813(3) -0.0070(4) 0.0721(16) Uani 1 1 d . . . C18 C 0.2056(8) 0.3635(3) -0.0896(4) 0.098(3) Uani 1 1 d . . . H18 H 0.1536 0.3677 -0.1419 0.118 Uiso 1 1 calc R . . C19 C 0.3071(10) 0.3397(4) -0.0962(6) 0.111(3) Uani 1 1 d . . . H19 H 0.3253 0.3282 -0.1531 0.133 Uiso 1 1 calc R . . C20 C 0.3818(7) 0.3326(3) -0.0203(6) 0.093(3) Uani 1 1 d . . . H20 H 0.4506 0.3152 -0.0254 0.112 Uiso 1 1 calc R . . C21 C 0.3590(6) 0.3506(2) 0.0662(5) 0.0687(16) Uani 1 1 d . . . C22 C 0.4434(6) 0.3400(3) 0.1479(6) 0.095(2) Uani 1 1 d . . . H22A H 0.4938 0.3713 0.1577 0.142 Uiso 1 1 calc R . . H22B H 0.4861 0.3070 0.1377 0.142 Uiso 1 1 calc R . . H22C H 0.4049 0.3347 0.2009 0.142 Uiso 1 1 calc R . . C23 C 0.0658(6) 0.4074(4) -0.0016(4) 0.094(2) Uani 1 1 d . . . H23A H 0.0238 0.3848 0.0363 0.142 Uiso 1 1 calc R . . H23B H 0.0250 0.4100 -0.0621 0.142 Uiso 1 1 calc R . . H23C H 0.0760 0.4441 0.0245 0.142 Uiso 1 1 calc R . . C24 C 0.4178(8) 0.2085(4) 0.2941(8) 0.147(4) Uani 1 1 d . . . H24A H 0.3983 0.1847 0.2420 0.220 Uiso 1 1 calc R . . H24B H 0.4680 0.1890 0.3397 0.220 Uiso 1 1 calc R . . H24C H 0.4546 0.2415 0.2754 0.220 Uiso 1 1 calc R . . C25 C 0.2340(9) 0.1653(3) 0.3922(6) 0.111(3) Uani 1 1 d . . . H25A H 0.1782 0.1754 0.4310 0.167 Uiso 1 1 calc R . . H25B H 0.2951 0.1458 0.4277 0.167 Uiso 1 1 calc R . . H25C H 0.2001 0.1414 0.3438 0.167 Uiso 1 1 calc R . . C26 C 0.1996(9) 0.2180(3) 0.0780(6) 0.120(3) Uani 1 1 d . . . H26A H 0.2659 0.2411 0.0806 0.181 Uiso 1 1 calc R . . H26B H 0.1532 0.2236 0.0205 0.181 Uiso 1 1 calc R . . H26C H 0.2219 0.1795 0.0836 0.181 Uiso 1 1 calc R . . C27 C 0.0190(8) 0.1794(3) 0.1893(6) 0.112(3) Uani 1 1 d . . . H27A H 0.0576 0.1443 0.1879 0.168 Uiso 1 1 calc R . . H27B H -0.0430 0.1804 0.1408 0.168 Uiso 1 1 calc R . . H27C H -0.0092 0.1837 0.2473 0.168 Uiso 1 1 calc R . . C28 C -0.2248(7) 0.2908(4) 0.1582(5) 0.110(3) Uani 1 1 d . . . H28A H -0.2824 0.3161 0.1314 0.165 Uiso 1 1 calc R . . H28B H -0.2593 0.2568 0.1753 0.165 Uiso 1 1 calc R . . H28C H -0.1737 0.2827 0.1143 0.165 Uiso 1 1 calc R . . C29 C -0.2513(8) 0.3400(4) 0.3383(6) 0.107(3) Uani 1 1 d . . . H29A H -0.2139 0.3549 0.3947 0.161 Uiso 1 1 calc R . . H29B H -0.2914 0.3066 0.3507 0.161 Uiso 1 1 calc R . . H29C H -0.3038 0.3670 0.3096 0.161 Uiso 1 1 calc R . . C30 C -0.1278(7) 0.4892(3) 0.3004(5) 0.093(2) Uani 1 1 d . . . H30A H -0.1848 0.4728 0.3328 0.139 Uiso 1 1 calc R . . H30B H -0.1546 0.5242 0.2743 0.139 Uiso 1 1 calc R . . H30C H -0.0602 0.4952 0.3422 0.139 Uiso 1 1 calc R . . C31 C -0.2165(7) 0.4450(4) 0.1163(5) 0.105(3) Uani 1 1 d . . . H31A H -0.2013 0.4223 0.0653 0.158 Uiso 1 1 calc R . . H31B H -0.2277 0.4831 0.0966 0.158 Uiso 1 1 calc R . . H31C H -0.2835 0.4316 0.1394 0.158 Uiso 1 1 calc R . . C32 C 0.1001(7) 0.3027(2) 0.4828(4) 0.0791(18) Uani 1 1 d . . . H32A H 0.0600 0.2728 0.4481 0.095 Uiso 1 1 calc R . . H32B H 0.1747 0.2894 0.5074 0.095 Uiso 1 1 calc R . . C33 C 0.0388(11) 0.3207(3) 0.5554(7) 0.138(4) Uani 1 1 d . . . H33A H -0.0389 0.3078 0.5444 0.166 Uiso 1 1 calc R . . H33B H 0.0733 0.3056 0.6136 0.166 Uiso 1 1 calc R . . C34 C 0.0423(12) 0.3793(4) 0.5573(7) 0.160(5) Uani 1 1 d . . . H34A H 0.0985 0.3919 0.6066 0.192 Uiso 1 1 calc R . . H34B H -0.0308 0.3940 0.5680 0.192 Uiso 1 1 calc R . . C35 C 0.0705(6) 0.3987(2) 0.4717(4) 0.0756(17) Uani 1 1 d . . . H35A H 0.1298 0.4267 0.4810 0.091 Uiso 1 1 calc R . . H35B H 0.0048 0.4151 0.4357 0.091 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 Y1 0.0486(3) 0.0428(3) 0.0467(3) -0.00229(19) 0.0154(2) -0.00252(19) Si1 0.0925(14) 0.0529(8) 0.1064(14) 0.0173(9) 0.0365(11) 0.0140(8) Si2 0.1043(14) 0.0565(9) 0.0830(11) -0.0214(8) 0.0484(10) -0.0193(9) Si3 0.0669(11) 0.0843(11) 0.0682(9) -0.0107(9) 0.0123(8) -0.0068(9) Si4 0.0624(10) 0.0839(11) 0.0692(9) -0.0019(9) 0.0128(8) 0.0119(8) O1 0.072(2) 0.0543(19) 0.0475(18) -0.0003(15) 0.0174(17) -0.0006(16) N1 0.054(2) 0.045(2) 0.044(2) -0.0021(17) 0.0105(17) -0.0063(17) N2 0.046(2) 0.047(2) 0.048(2) -0.0083(18) 0.0141(17) -0.0042(17) N3 0.081(3) 0.043(2) 0.077(3) 0.000(2) 0.041(3) 0.001(2) N4 0.050(3) 0.071(3) 0.062(2) -0.008(2) 0.010(2) -0.001(2) C1 0.040(2) 0.044(2) 0.051(2) 0.009(2) 0.010(2) 0.0071(19) C2 0.051(3) 0.043(2) 0.061(3) -0.015(2) 0.018(2) -0.009(2) C3 0.050(3) 0.064(3) 0.059(3) 0.005(3) 0.015(2) -0.006(2) C4 0.045(3) 0.078(4) 0.075(4) -0.002(3) 0.005(3) -0.011(3) C5 0.060(3) 0.063(3) 0.076(4) -0.003(3) 0.024(3) -0.023(3) C6 0.065(4) 0.066(3) 0.063(3) 0.013(3) 0.019(3) -0.001(3) C7 0.055(3) 0.049(2) 0.047(2) 0.006(2) 0.012(2) -0.001(2) C8 0.059(3) 0.049(3) 0.053(3) -0.011(2) 0.019(2) -0.015(2) C9 0.074(4) 0.083(4) 0.049(3) -0.006(3) 0.012(3) -0.024(3) C10 0.088(5) 0.120(6) 0.066(4) -0.019(4) 0.012(3) -0.018(5) C11 0.086(5) 0.134(7) 0.073(4) -0.041(5) 0.020(4) -0.024(5) C12 0.082(5) 0.066(3) 0.114(6) -0.035(4) 0.048(4) -0.015(3) C13 0.071(4) 0.058(3) 0.081(4) -0.007(3) 0.034(3) -0.006(3) C14 0.100(5) 0.087(4) 0.072(4) 0.018(4) -0.006(4) -0.006(4) C15 0.085(4) 0.046(3) 0.120(5) 0.008(3) 0.037(4) 0.004(3) C16 0.061(3) 0.050(3) 0.053(3) -0.006(2) 0.024(2) -0.018(2) C17 0.082(4) 0.076(4) 0.062(3) -0.008(3) 0.023(3) -0.031(3) C18 0.130(7) 0.114(5) 0.058(4) -0.034(4) 0.043(4) -0.061(5) C19 0.152(9) 0.111(6) 0.084(5) -0.047(5) 0.072(6) -0.057(6) C20 0.109(6) 0.058(3) 0.129(7) -0.018(4) 0.082(6) -0.016(4) C21 0.081(4) 0.048(3) 0.085(4) -0.010(3) 0.046(3) -0.011(3) C22 0.078(5) 0.073(4) 0.143(7) 0.014(4) 0.052(5) 0.022(3) C23 0.078(5) 0.142(7) 0.061(3) 0.004(4) 0.003(3) -0.020(4) C24 0.120(8) 0.133(7) 0.200(11) 0.071(8) 0.073(7) 0.055(6) C25 0.156(8) 0.075(4) 0.111(6) 0.024(4) 0.048(6) 0.009(5) C26 0.183(9) 0.080(4) 0.118(6) -0.035(4) 0.096(6) -0.027(5) C27 0.133(7) 0.094(5) 0.121(6) -0.036(5) 0.065(5) -0.049(5) C28 0.085(5) 0.140(7) 0.108(6) -0.042(5) 0.027(4) -0.031(5) C29 0.111(6) 0.127(6) 0.093(5) -0.014(5) 0.051(5) -0.023(5) C30 0.109(6) 0.085(4) 0.083(4) -0.010(4) 0.008(4) 0.023(4) C31 0.119(6) 0.125(6) 0.066(4) 0.004(4) -0.010(4) 0.037(5) C32 0.114(5) 0.062(3) 0.065(3) 0.018(3) 0.028(4) 0.006(3) C33 0.215(11) 0.095(6) 0.128(7) 0.035(5) 0.113(8) 0.030(6) C34 0.285(15) 0.089(5) 0.138(8) -0.010(5) 0.146(10) 0.006(7) C35 0.106(5) 0.059(3) 0.066(3) -0.011(3) 0.030(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N4 2.254(4) . ? Y1 N3 2.265(4) . ? Y1 N1 2.358(4) . ? Y1 O1 2.363(3) . ? Y1 N2 2.372(4) . ? Y1 C1 2.815(5) . ? Y1 Si2 3.0654(16) . ? Y1 Si3 3.268(2) . ? Y1 H2 2.47(5) . ? Si1 N3 1.702(5) . ? Si1 C25 1.850(7) . ? Si1 C24 1.858(9) . ? Si1 H1 1.44(7) . ? Si2 N3 1.702(5) . ? Si2 C27 1.867(7) . ? Si2 C26 1.875(7) . ? Si2 H2 1.35(5) . ? Si3 N4 1.696(5) . ? Si3 C29 1.859(8) . ? Si3 C28 1.869(7) . ? Si3 H3 1.54(4) . ? Si4 N4 1.697(5) . ? Si4 C31 1.851(7) . ? Si4 C30 1.880(7) . ? Si4 H4 1.43(7) . ? O1 C32 1.450(6) . ? O1 C35 1.452(6) . ? N1 C1 1.337(6) . ? N1 C8 1.427(6) . ? N2 C1 1.334(6) . ? N2 C16 1.420(6) . ? C1 C2 1.485(6) . ? C2 C3 1.385(7) . ? C2 C7 1.394(7) . ? C3 C4 1.376(7) . ? C3 H3A 0.9400 . ? C4 C5 1.379(8) . ? C4 H4A 0.9400 . ? C5 C6 1.376(8) . ? C5 H5 0.9400 . ? C6 C7 1.387(7) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C8 C13 1.384(8) . ? C8 C9 1.417(8) . ? C9 C10 1.361(9) . ? C9 C14 1.519(10) . ? C10 C11 1.355(11) . ? C10 H10 0.9400 . ? C11 C12 1.381(11) . ? C11 H11 0.9400 . ? C12 C13 1.431(9) . ? C12 H12 0.9400 . ? C13 C15 1.510(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C21 1.391(8) . ? C16 C17 1.398(8) . ? C17 C18 1.376(9) . ? C17 C23 1.511(10) . ? C18 C19 1.364(13) . ? C18 H18 0.9400 . ? C19 C20 1.361(13) . ? C19 H19 0.9400 . ? C20 C21 1.415(9) . ? C20 H20 0.9400 . ? C21 C22 1.502(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 C33 1.446(10) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 C34 1.418(12) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 C35 1.435(10) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 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 N4 Y1 N3 127.76(18) . . ? N4 Y1 N1 113.49(15) . . ? N3 Y1 N1 118.75(16) . . ? N4 Y1 O1 89.36(14) . . ? N3 Y1 O1 93.71(14) . . ? N1 Y1 O1 85.91(12) . . ? N4 Y1 N2 108.70(15) . . ? N3 Y1 N2 100.20(14) . . ? N1 Y1 N2 56.37(13) . . ? O1 Y1 N2 141.98(12) . . ? N4 Y1 C1 115.10(15) . . ? N3 Y1 C1 110.94(15) . . ? N1 Y1 C1 28.23(13) . . ? O1 Y1 C1 113.91(13) . . ? N2 Y1 C1 28.17(13) . . ? N4 Y1 Si2 102.44(12) . . ? N3 Y1 Si2 33.12(14) . . ? N1 Y1 Si2 137.40(10) . . ? O1 Y1 Si2 117.58(9) . . ? N2 Y1 Si2 91.55(9) . . ? C1 Y1 Si2 115.05(10) . . ? N4 Y1 Si3 29.01(12) . . ? N3 Y1 Si3 100.31(13) . . ? N1 Y1 Si3 139.52(10) . . ? O1 Y1 Si3 81.12(10) . . ? N2 Y1 Si3 129.77(10) . . ? C1 Y1 Si3 143.59(9) . . ? Si2 Y1 Si3 81.75(5) . . ? N4 Y1 H2 81.7(12) . . ? N3 Y1 H2 58.5(11) . . ? N1 Y1 H2 140.6(11) . . ? O1 Y1 H2 132.1(11) . . ? N2 Y1 H2 84.6(11) . . ? C1 Y1 H2 112.5(11) . . ? Si2 Y1 H2 25.4(11) . . ? Si3 Y1 H2 68.6(12) . . ? N3 Si1 C25 113.7(4) . . ? N3 Si1 C24 115.1(4) . . ? C25 Si1 C24 107.2(4) . . ? N3 Si1 H1 109(3) . . ? C25 Si1 H1 109(3) . . ? C24 Si1 H1 103(3) . . ? N3 Si2 C27 115.8(3) . . ? N3 Si2 C26 117.7(4) . . ? C27 Si2 C26 108.4(3) . . ? N3 Si2 Y1 46.63(15) . . ? C27 Si2 Y1 125.2(3) . . ? C26 Si2 Y1 125.8(2) . . ? N3 Si2 H2 98(2) . . ? C27 Si2 H2 108(2) . . ? C26 Si2 H2 107(2) . . ? Y1 Si2 H2 52(2) . . ? N4 Si3 C29 115.3(3) . . ? N4 Si3 C28 115.8(3) . . ? C29 Si3 C28 106.1(4) . . ? N4 Si3 Y1 40.11(16) . . ? C29 Si3 Y1 133.3(3) . . ? C28 Si3 Y1 120.4(3) . . ? N4 Si3 H3 110.1(17) . . ? C29 Si3 H3 103.7(17) . . ? C28 Si3 H3 104.7(17) . . ? Y1 Si3 H3 70.7(17) . . ? N4 Si4 C31 114.6(3) . . ? N4 Si4 C30 115.0(3) . . ? C31 Si4 C30 107.1(3) . . ? N4 Si4 H4 104(2) . . ? C31 Si4 H4 107(2) . . ? C30 Si4 H4 108(3) . . ? C32 O1 C35 108.2(4) . . ? C32 O1 Y1 126.2(3) . . ? C35 O1 Y1 122.6(3) . . ? C1 N1 C8 124.0(4) . . ? C1 N1 Y1 95.3(3) . . ? C8 N1 Y1 140.4(3) . . ? C1 N2 C16 123.8(4) . . ? C1 N2 Y1 94.7(3) . . ? C16 N2 Y1 137.4(3) . . ? Si1 N3 Si2 126.6(3) . . ? Si1 N3 Y1 133.2(3) . . ? Si2 N3 Y1 100.2(2) . . ? Si3 N4 Si4 127.2(3) . . ? Si3 N4 Y1 110.9(2) . . ? Si4 N4 Y1 122.0(2) . . ? N2 C1 N1 113.5(4) . . ? N2 C1 C2 124.1(4) . . ? N1 C1 C2 122.4(4) . . ? N2 C1 Y1 57.1(2) . . ? N1 C1 Y1 56.5(2) . . ? C2 C1 Y1 177.2(3) . . ? C3 C2 C7 118.1(4) . . ? C3 C2 C1 121.6(5) . . ? C7 C2 C1 120.3(4) . . ? C4 C3 C2 121.2(5) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 120.4(5) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C6 C5 C4 119.5(5) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 120.3(5) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C2 120.6(5) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? C13 C8 C9 118.5(5) . . ? C13 C8 N1 123.7(5) . . ? C9 C8 N1 117.6(4) . . ? C10 C9 C8 122.2(6) . . ? C10 C9 C14 117.6(6) . . ? C8 C9 C14 120.2(5) . . ? C11 C10 C9 119.3(7) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C12 121.8(7) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C13 119.5(6) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C8 C13 C12 118.8(6) . . ? C8 C13 C15 120.6(5) . . ? C12 C13 C15 120.6(6) . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 119.8(5) . . ? C21 C16 N2 121.4(5) . . ? C17 C16 N2 118.6(5) . . ? C18 C17 C16 120.5(7) . . ? C18 C17 C23 119.4(7) . . ? C16 C17 C23 120.2(5) . . ? C19 C18 C17 120.5(8) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C18 119.8(6) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 121.9(7) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C16 C21 C20 117.4(7) . . ? C16 C21 C22 123.1(5) . . ? C20 C21 C22 119.3(7) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C17 C23 H23A 109.5 . . ? C17 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C17 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si3 C28 H28A 109.5 . . ? Si3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si3 C29 H29A 109.5 . . ? Si3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si4 C30 H30A 109.5 . . ? Si4 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si4 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si4 C31 H31A 109.5 . . ? Si4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 O1 106.1(5) . . ? C33 C32 H32A 110.5 . . ? O1 C32 H32A 110.5 . . ? C33 C32 H32B 110.5 . . ? O1 C32 H32B 110.5 . . ? H32A C32 H32B 108.7 . . ? C34 C33 C32 107.4(6) . . ? C34 C33 H33A 110.2 . . ? C32 C33 H33A 110.2 . . ? C34 C33 H33B 110.2 . . ? C32 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? C33 C34 C35 108.5(6) . . ? C33 C34 H34A 110.0 . . ? C35 C34 H34A 110.0 . . ? C33 C34 H34B 110.0 . . ? C35 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? C34 C35 O1 106.3(5) . . ? C34 C35 H35A 110.5 . . ? O1 C35 H35A 110.5 . . ? C34 C35 H35B 110.5 . . ? O1 C35 H35B 110.5 . . ? H35A C35 H35B 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Y1 Si2 N3 -144.0(2) . . . . ? N1 Y1 Si2 N3 68.5(3) . . . . ? O1 Y1 Si2 N3 -48.2(2) . . . . ? N2 Y1 Si2 N3 106.4(2) . . . . ? C1 Y1 Si2 N3 90.3(2) . . . . ? Si3 Y1 Si2 N3 -123.6(2) . . . . ? N4 Y1 Si2 C27 -50.2(4) . . . . ? N3 Y1 Si2 C27 93.8(5) . . . . ? N1 Y1 Si2 C27 162.3(4) . . . . ? O1 Y1 Si2 C27 45.6(4) . . . . ? N2 Y1 Si2 C27 -159.8(4) . . . . ? C1 Y1 Si2 C27 -175.9(4) . . . . ? Si3 Y1 Si2 C27 -29.8(4) . . . . ? N4 Y1 Si2 C26 119.8(5) . . . . ? N3 Y1 Si2 C26 -96.2(5) . . . . ? N1 Y1 Si2 C26 -27.7(5) . . . . ? O1 Y1 Si2 C26 -144.4(5) . . . . ? N2 Y1 Si2 C26 10.2(5) . . . . ? C1 Y1 Si2 C26 -5.9(5) . . . . ? Si3 Y1 Si2 C26 140.2(4) . . . . ? N3 Y1 Si3 N4 -162.8(3) . . . . ? N1 Y1 Si3 N4 32.1(3) . . . . ? O1 Y1 Si3 N4 105.0(2) . . . . ? N2 Y1 Si3 N4 -50.1(3) . . . . ? C1 Y1 Si3 N4 -13.6(3) . . . . ? Si2 Y1 Si3 N4 -135.3(2) . . . . ? N4 Y1 Si3 C29 -78.1(5) . . . . ? N3 Y1 Si3 C29 119.1(4) . . . . ? N1 Y1 Si3 C29 -46.0(4) . . . . ? O1 Y1 Si3 C29 26.9(4) . . . . ? N2 Y1 Si3 C29 -128.2(4) . . . . ? C1 Y1 Si3 C29 -91.7(4) . . . . ? Si2 Y1 Si3 C29 146.7(4) . . . . ? N4 Y1 Si3 C28 95.1(4) . . . . ? N3 Y1 Si3 C28 -67.8(4) . . . . ? N1 Y1 Si3 C28 127.2(4) . . . . ? O1 Y1 Si3 C28 -159.9(4) . . . . ? N2 Y1 Si3 C28 44.9(4) . . . . ? C1 Y1 Si3 C28 81.4(4) . . . . ? Si2 Y1 Si3 C28 -40.2(4) . . . . ? N4 Y1 O1 C32 104.1(5) . . . . ? N3 Y1 O1 C32 -23.7(5) . . . . ? N1 Y1 O1 C32 -142.3(5) . . . . ? N2 Y1 O1 C32 -135.5(5) . . . . ? C1 Y1 O1 C32 -138.6(5) . . . . ? Si2 Y1 O1 C32 0.4(5) . . . . ? Si3 Y1 O1 C32 76.2(5) . . . . ? N4 Y1 O1 C35 -54.0(4) . . . . ? N3 Y1 O1 C35 178.2(4) . . . . ? N1 Y1 O1 C35 59.6(4) . . . . ? N2 Y1 O1 C35 66.4(5) . . . . ? C1 Y1 O1 C35 63.3(5) . . . . ? Si2 Y1 O1 C35 -157.7(4) . . . . ? Si3 Y1 O1 C35 -81.9(4) . . . . ? N4 Y1 N1 C1 -99.7(3) . . . . ? N3 Y1 N1 C1 80.8(3) . . . . ? O1 Y1 N1 C1 172.8(3) . . . . ? N2 Y1 N1 C1 -2.2(2) . . . . ? Si2 Y1 N1 C1 45.3(3) . . . . ? Si3 Y1 N1 C1 -116.0(3) . . . . ? N4 Y1 N1 C8 73.0(5) . . . . ? N3 Y1 N1 C8 -106.5(5) . . . . ? O1 Y1 N1 C8 -14.5(5) . . . . ? N2 Y1 N1 C8 170.5(5) . . . . ? C1 Y1 N1 C8 172.7(7) . . . . ? Si2 Y1 N1 C8 -142.0(4) . . . . ? Si3 Y1 N1 C8 56.7(5) . . . . ? N4 Y1 N2 C1 108.5(3) . . . . ? N3 Y1 N2 C1 -115.7(3) . . . . ? N1 Y1 N2 C1 2.2(2) . . . . ? O1 Y1 N2 C1 -6.0(4) . . . . ? Si2 Y1 N2 C1 -147.8(3) . . . . ? Si3 Y1 N2 C1 131.6(2) . . . . ? N4 Y1 N2 C16 -95.4(5) . . . . ? N3 Y1 N2 C16 40.4(5) . . . . ? N1 Y1 N2 C16 158.3(5) . . . . ? O1 Y1 N2 C16 150.1(4) . . . . ? C1 Y1 N2 C16 156.1(6) . . . . ? Si2 Y1 N2 C16 8.3(5) . . . . ? Si3 Y1 N2 C16 -72.3(5) . . . . ? C25 Si1 N3 Si2 -59.3(5) . . . . ? C24 Si1 N3 Si2 64.9(6) . . . . ? C25 Si1 N3 Y1 121.7(4) . . . . ? C24 Si1 N3 Y1 -114.1(5) . . . . ? C27 Si2 N3 Si1 65.6(5) . . . . ? C26 Si2 N3 Si1 -65.0(5) . . . . ? Y1 Si2 N3 Si1 -179.3(4) . . . . ? C27 Si2 N3 Y1 -115.1(4) . . . . ? C26 Si2 N3 Y1 114.3(3) . . . . ? N4 Y1 N3 Si1 -134.3(3) . . . . ? N1 Y1 N3 Si1 45.2(4) . . . . ? O1 Y1 N3 Si1 -42.2(3) . . . . ? N2 Y1 N3 Si1 102.3(3) . . . . ? C1 Y1 N3 Si1 75.2(3) . . . . ? Si2 Y1 N3 Si1 179.2(5) . . . . ? Si3 Y1 N3 Si1 -123.8(3) . . . . ? N4 Y1 N3 Si2 46.5(3) . . . . ? N1 Y1 N3 Si2 -134.07(19) . . . . ? O1 Y1 N3 Si2 138.6(2) . . . . ? N2 Y1 N3 Si2 -77.0(2) . . . . ? C1 Y1 N3 Si2 -104.1(2) . . . . ? Si3 Y1 N3 Si2 56.93(19) . . . . ? C29 Si3 N4 Si4 -51.2(5) . . . . ? C28 Si3 N4 Si4 73.4(5) . . . . ? Y1 Si3 N4 Si4 -179.3(5) . . . . ? C29 Si3 N4 Y1 128.0(4) . . . . ? C28 Si3 N4 Y1 -107.3(4) . . . . ? C31 Si4 N4 Si3 -43.2(5) . . . . ? C30 Si4 N4 Si3 81.7(4) . . . . ? C31 Si4 N4 Y1 137.6(4) . . . . ? C30 Si4 N4 Y1 -97.5(4) . . . . ? N3 Y1 N4 Si3 21.6(3) . . . . ? N1 Y1 N4 Si3 -157.90(19) . . . . ? O1 Y1 N4 Si3 -72.6(2) . . . . ? N2 Y1 N4 Si3 141.5(2) . . . . ? C1 Y1 N4 Si3 171.11(19) . . . . ? Si2 Y1 N4 Si3 45.5(2) . . . . ? N3 Y1 N4 Si4 -159.1(2) . . . . ? N1 Y1 N4 Si4 21.4(3) . . . . ? O1 Y1 N4 Si4 106.7(3) . . . . ? N2 Y1 N4 Si4 -39.2(3) . . . . ? C1 Y1 N4 Si4 -9.6(3) . . . . ? Si2 Y1 N4 Si4 -135.2(2) . . . . ? Si3 Y1 N4 Si4 179.3(4) . . . . ? C16 N2 C1 N1 -164.2(4) . . . . ? Y1 N2 C1 N1 -3.5(4) . . . . ? C16 N2 C1 C2 16.3(7) . . . . ? Y1 N2 C1 C2 177.0(4) . . . . ? C16 N2 C1 Y1 -160.7(5) . . . . ? C8 N1 C1 N2 -170.9(4) . . . . ? Y1 N1 C1 N2 3.5(4) . . . . ? C8 N1 C1 C2 8.6(7) . . . . ? Y1 N1 C1 C2 -177.0(4) . . . . ? C8 N1 C1 Y1 -174.4(5) . . . . ? N4 Y1 C1 N2 -82.8(3) . . . . ? N3 Y1 C1 N2 71.8(3) . . . . ? N1 Y1 C1 N2 -176.2(4) . . . . ? O1 Y1 C1 N2 176.0(3) . . . . ? Si2 Y1 C1 N2 36.0(3) . . . . ? Si3 Y1 C1 N2 -75.6(3) . . . . ? N4 Y1 C1 N1 93.3(3) . . . . ? N3 Y1 C1 N1 -112.1(3) . . . . ? O1 Y1 C1 N1 -7.9(3) . . . . ? N2 Y1 C1 N1 176.2(4) . . . . ? Si2 Y1 C1 N1 -147.9(2) . . . . ? Si3 Y1 C1 N1 100.6(3) . . . . ? N4 Y1 C1 C2 160(7) . . . . ? N3 Y1 C1 C2 -46(7) . . . . ? N1 Y1 C1 C2 67(7) . . . . ? O1 Y1 C1 C2 59(7) . . . . ? N2 Y1 C1 C2 -117(7) . . . . ? Si2 Y1 C1 C2 -81(7) . . . . ? Si3 Y1 C1 C2 167(7) . . . . ? N2 C1 C2 C3 -137.8(5) . . . . ? N1 C1 C2 C3 42.8(7) . . . . ? Y1 C1 C2 C3 -22(7) . . . . ? N2 C1 C2 C7 43.1(7) . . . . ? N1 C1 C2 C7 -136.3(5) . . . . ? Y1 C1 C2 C7 159(7) . . . . ? C7 C2 C3 C4 -1.0(8) . . . . ? C1 C2 C3 C4 179.8(5) . . . . ? C2 C3 C4 C5 1.3(9) . . . . ? C3 C4 C5 C6 -0.4(9) . . . . ? C4 C5 C6 C7 -0.7(9) . . . . ? C5 C6 C7 C2 1.0(8) . . . . ? C3 C2 C7 C6 -0.1(7) . . . . ? C1 C2 C7 C6 179.1(5) . . . . ? C1 N1 C8 C13 69.7(7) . . . . ? Y1 N1 C8 C13 -101.5(6) . . . . ? C1 N1 C8 C9 -116.8(5) . . . . ? Y1 N1 C8 C9 72.0(7) . . . . ? C13 C8 C9 C10 1.6(9) . . . . ? N1 C8 C9 C10 -172.2(6) . . . . ? C13 C8 C9 C14 -176.4(5) . . . . ? N1 C8 C9 C14 9.7(8) . . . . ? C8 C9 C10 C11 0.3(10) . . . . ? C14 C9 C10 C11 178.3(7) . . . . ? C9 C10 C11 C12 -1.9(11) . . . . ? C10 C11 C12 C13 1.5(11) . . . . ? C9 C8 C13 C12 -1.9(8) . . . . ? N1 C8 C13 C12 171.5(5) . . . . ? C9 C8 C13 C15 178.2(5) . . . . ? N1 C8 C13 C15 -8.3(8) . . . . ? C11 C12 C13 C8 0.4(9) . . . . ? C11 C12 C13 C15 -179.7(6) . . . . ? C1 N2 C16 C21 59.1(6) . . . . ? Y1 N2 C16 C21 -91.8(6) . . . . ? C1 N2 C16 C17 -124.8(5) . . . . ? Y1 N2 C16 C17 84.2(6) . . . . ? C21 C16 C17 C18 0.5(8) . . . . ? N2 C16 C17 C18 -175.6(5) . . . . ? C21 C16 C17 C23 179.8(5) . . . . ? N2 C16 C17 C23 3.7(8) . . . . ? C16 C17 C18 C19 -0.5(10) . . . . ? C23 C17 C18 C19 -179.9(7) . . . . ? C17 C18 C19 C20 1.2(11) . . . . ? C18 C19 C20 C21 -1.8(11) . . . . ? C17 C16 C21 C20 -1.1(7) . . . . ? N2 C16 C21 C20 174.9(5) . . . . ? C17 C16 C21 C22 -177.3(5) . . . . ? N2 C16 C21 C22 -1.2(8) . . . . ? C19 C20 C21 C16 1.8(9) . . . . ? C19 C20 C21 C22 178.1(7) . . . . ? C35 O1 C32 C33 9.5(9) . . . . ? Y1 O1 C32 C33 -151.2(6) . . . . ? O1 C32 C33 C34 -17.4(12) . . . . ? C32 C33 C34 C35 18.9(14) . . . . ? C33 C34 C35 O1 -12.7(12) . . . . ? C32 O1 C35 C34 1.7(9) . . . . ? Y1 O1 C35 C34 163.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.252 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.085 data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 894306' #TrackingRef 'CCDC.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H77 N3 O3 Si2 Y, C24 B F20' _chemical_formula_sum 'C71 H77 B F20 N3 O3 Si2 Y' _chemical_formula_weight 1556.26 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' Y Y -2.7962 3.5667 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 21.1633(16) _cell_length_b 12.3731(9) _cell_length_c 27.746(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.515(3) _cell_angle_gamma 90.00 _cell_volume 7218.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23259 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3200 _exptl_absorpt_coefficient_mu 0.941 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_correction_T_max 0.849 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67717 _diffrn_reflns_av_R_equivalents 0.0998 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.35 _reflns_number_total 13099 _reflns_number_gt 9386 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+12.3111P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13099 _refine_ls_number_parameters 931 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1395 _refine_ls_R_factor_gt 0.0976 _refine_ls_wR_factor_ref 0.1608 _refine_ls_wR_factor_gt 0.1468 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.158 _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 Y1 Y 0.26247(2) 0.29305(4) 0.814394(19) 0.04104(15) Uani 1 1 d . . . Si1 Si 0.34284(10) 0.19838(17) 0.71506(7) 0.0710(5) Uani 1 1 d . . . H1 H 0.397(3) 0.178(4) 0.754(2) 0.075(18) Uiso 1 1 d . . . Si2 Si 0.20850(11) 0.28082(18) 0.70346(7) 0.0782(6) Uani 1 1 d . . . H2 H 0.170(2) 0.344(4) 0.7395(16) 0.043(13) Uiso 1 1 d . . . F1 F 0.21850(16) 0.8476(3) 0.66825(12) 0.0639(9) Uani 1 1 d . . . F2 F 0.33833(18) 0.7911(4) 0.69636(15) 0.0945(13) Uani 1 1 d . . . F3 F 0.39531(18) 0.6334(4) 0.64919(17) 0.1089(16) Uani 1 1 d . . . F4 F 0.3279(2) 0.5287(4) 0.57374(17) 0.1031(15) Uani 1 1 d . . . F5 F 0.20889(18) 0.5813(3) 0.54548(13) 0.0731(10) Uani 1 1 d . . . F6 F 0.08021(17) 0.8986(3) 0.66821(12) 0.0679(10) Uani 1 1 d . . . F7 F 0.03167(19) 0.8178(3) 0.74381(13) 0.0883(12) Uani 1 1 d . . . F8 F 0.02628(19) 0.6016(4) 0.75776(14) 0.0924(13) Uani 1 1 d . . . F9 F 0.06543(19) 0.4646(3) 0.69006(15) 0.0880(12) Uani 1 1 d . . . F10 F 0.11104(17) 0.5441(3) 0.61163(13) 0.0698(10) Uani 1 1 d . . . F11 F 0.18790(16) 0.7899(3) 0.49768(11) 0.0625(9) Uani 1 1 d . . . F12 F 0.1365(2) 0.7384(3) 0.40894(13) 0.0838(12) Uani 1 1 d . . . F13 F 0.0224(2) 0.6357(3) 0.39496(14) 0.0973(14) Uani 1 1 d . . . F14 F -0.03985(18) 0.5882(3) 0.47291(15) 0.0798(11) Uani 1 1 d . . . F15 F 0.00701(15) 0.6449(3) 0.56060(13) 0.0634(9) Uani 1 1 d . . . F16 F 0.24029(15) 0.9336(3) 0.57926(12) 0.0594(9) Uani 1 1 d . . . F17 F 0.22139(18) 1.1368(3) 0.55679(15) 0.0803(11) Uani 1 1 d . . . F18 F 0.1023(2) 1.2192(3) 0.53797(18) 0.1027(15) Uani 1 1 d . . . F19 F 0.00030(18) 1.0878(3) 0.54594(15) 0.0798(11) Uani 1 1 d . . . F20 F 0.01732(15) 0.8828(3) 0.57094(12) 0.0612(9) Uani 1 1 d . . . O1 O 0.19095(17) 0.1416(3) 0.80632(15) 0.0575(11) Uani 1 1 d . . . O2 O 0.17308(17) 0.3640(3) 0.85011(15) 0.0559(10) Uani 1 1 d . . . O3 O 0.26243(19) 0.4865(3) 0.79827(14) 0.0578(11) Uani 1 1 d . . . N1 N 0.35512(19) 0.3400(3) 0.86647(15) 0.0390(10) Uani 1 1 d . . . N2 N 0.31503(19) 0.1741(3) 0.87400(15) 0.0377(10) Uani 1 1 d . . . N3 N 0.2777(2) 0.2518(4) 0.73880(17) 0.0594(13) Uani 1 1 d . . . C1 C 0.3615(2) 0.2437(4) 0.88906(17) 0.0383(12) Uani 1 1 d . . . C2 C 0.3941(2) 0.4317(4) 0.8811(2) 0.0430(13) Uani 1 1 d . . . C3 C 0.4311(3) 0.4787(5) 0.8470(2) 0.0516(15) Uani 1 1 d . . . C4 C 0.4675(3) 0.5692(6) 0.8614(3) 0.075(2) Uani 1 1 d . . . H4 H 0.4925 0.6000 0.8396 0.090 Uiso 1 1 calc R . . C5 C 0.4679(3) 0.6143(5) 0.9060(3) 0.078(2) Uani 1 1 d . . . H5 H 0.4934 0.6742 0.9145 0.094 Uiso 1 1 calc R . . C6 C 0.4307(3) 0.5716(5) 0.9386(2) 0.0633(18) Uani 1 1 d . . . H6 H 0.4307 0.6038 0.9689 0.076 Uiso 1 1 calc R . . C7 C 0.3929(3) 0.4809(4) 0.9273(2) 0.0483(14) Uani 1 1 d . . . C8 C 0.4326(3) 0.4340(5) 0.7965(2) 0.0628(17) Uani 1 1 d . . . H7 H 0.3927 0.3950 0.7878 0.075 Uiso 1 1 calc R . . C9 C 0.4364(4) 0.5237(7) 0.7588(3) 0.104(3) Uani 1 1 d . . . H9A H 0.4044 0.5770 0.7624 0.156 Uiso 1 1 calc R . . H9B H 0.4297 0.4933 0.7268 0.156 Uiso 1 1 calc R . . H9C H 0.4777 0.5570 0.7635 0.156 Uiso 1 1 calc R . . C10 C 0.4862(4) 0.3544(6) 0.7940(3) 0.093(2) Uani 1 1 d . . . H10A H 0.5259 0.3883 0.8054 0.140 Uiso 1 1 calc R . . H10B H 0.4871 0.3315 0.7610 0.140 Uiso 1 1 calc R . . H10C H 0.4797 0.2928 0.8139 0.140 Uiso 1 1 calc R . . C11 C 0.3505(3) 0.4432(5) 0.9644(2) 0.0545(16) Uani 1 1 d . . . H11 H 0.3274 0.3789 0.9516 0.065 Uiso 1 1 calc R . . C12 C 0.3021(3) 0.5299(5) 0.9736(2) 0.075(2) Uani 1 1 d . . . H12A H 0.3237 0.5918 0.9883 0.112 Uiso 1 1 calc R . . H12B H 0.2733 0.5017 0.9949 0.112 Uiso 1 1 calc R . . H12C H 0.2786 0.5507 0.9434 0.112 Uiso 1 1 calc R . . C13 C 0.3891(4) 0.4130(5) 1.0125(2) 0.078(2) Uani 1 1 d . . . H13A H 0.4209 0.3608 1.0067 0.117 Uiso 1 1 calc R . . H13B H 0.3613 0.3827 1.0340 0.117 Uiso 1 1 calc R . . H13C H 0.4092 0.4764 1.0270 0.117 Uiso 1 1 calc R . . C14 C 0.3144(2) 0.0648(4) 0.89174(18) 0.0370(12) Uani 1 1 d . . . C15 C 0.3571(2) -0.0136(4) 0.87823(18) 0.0398(13) Uani 1 1 d . . . C16 C 0.3529(3) -0.1182(4) 0.8959(2) 0.0496(14) Uani 1 1 d . . . H16 H 0.3812 -0.1702 0.8872 0.059 Uiso 1 1 calc R . . C17 C 0.3084(3) -0.1469(5) 0.9258(2) 0.0580(16) Uani 1 1 d . . . H17 H 0.3071 -0.2169 0.9378 0.070 Uiso 1 1 calc R . . C18 C 0.2659(3) -0.0705(4) 0.9377(2) 0.0527(15) Uani 1 1 d . . . H18 H 0.2352 -0.0903 0.9575 0.063 Uiso 1 1 calc R . . C19 C 0.2670(3) 0.0353(4) 0.92114(19) 0.0420(13) Uani 1 1 d . . . C20 C 0.4072(3) 0.0084(5) 0.8446(2) 0.0523(15) Uani 1 1 d . . . H20 H 0.4050 0.0850 0.8355 0.063 Uiso 1 1 calc R . . C21 C 0.4745(3) -0.0159(6) 0.8683(3) 0.0712(19) Uani 1 1 d . . . H21A H 0.4815 0.0203 0.8990 0.107 Uiso 1 1 calc R . . H21B H 0.5049 0.0092 0.8476 0.107 Uiso 1 1 calc R . . H21C H 0.4794 -0.0924 0.8730 0.107 Uiso 1 1 calc R . . C22 C 0.3942(3) -0.0597(6) 0.7984(2) 0.075(2) Uani 1 1 d . . . H22A H 0.4007 -0.1348 0.8063 0.112 Uiso 1 1 calc R . . H22B H 0.4226 -0.0383 0.7755 0.112 Uiso 1 1 calc R . . H22C H 0.3510 -0.0488 0.7844 0.112 Uiso 1 1 calc R . . C23 C 0.2179(3) 0.1156(4) 0.9349(2) 0.0538(15) Uani 1 1 d . . . H23 H 0.2122 0.1701 0.9092 0.065 Uiso 1 1 calc R . . C24 C 0.2412(3) 0.1741(5) 0.9820(2) 0.075(2) Uani 1 1 d . . . H24A H 0.2503 0.1222 1.0076 0.113 Uiso 1 1 calc R . . H24B H 0.2089 0.2229 0.9903 0.113 Uiso 1 1 calc R . . H24C H 0.2791 0.2140 0.9778 0.113 Uiso 1 1 calc R . . C25 C 0.1527(3) 0.0668(5) 0.9397(3) 0.075(2) Uani 1 1 d . . . H25A H 0.1550 0.0231 0.9684 0.112 Uiso 1 1 calc R . . H25B H 0.1397 0.0229 0.9118 0.112 Uiso 1 1 calc R . . H25C H 0.1224 0.1238 0.9418 0.112 Uiso 1 1 calc R . . C26 C 0.4170(2) 0.2163(4) 0.92576(19) 0.0422(13) Uani 1 1 d . . . C27 C 0.4781(3) 0.2530(5) 0.9199(2) 0.0569(16) Uani 1 1 d . . . H27 H 0.4844 0.2963 0.8935 0.068 Uiso 1 1 calc R . . C28 C 0.5293(3) 0.2254(5) 0.9533(3) 0.072(2) Uani 1 1 d . . . H28 H 0.5700 0.2486 0.9486 0.086 Uiso 1 1 calc R . . C29 C 0.5207(4) 0.1644(6) 0.9932(3) 0.080(2) Uani 1 1 d . . . H29 H 0.5552 0.1466 1.0157 0.096 Uiso 1 1 calc R . . C30 C 0.4612(4) 0.1300(5) 0.9996(2) 0.070(2) Uani 1 1 d . . . H30 H 0.4553 0.0889 1.0268 0.084 Uiso 1 1 calc R . . C31 C 0.4095(3) 0.1545(4) 0.96688(19) 0.0519(15) Uani 1 1 d . . . H31 H 0.3694 0.1298 0.9721 0.062 Uiso 1 1 calc R . . C32 C 0.3265(4) 0.0708(6) 0.6810(3) 0.094(2) Uani 1 1 d . . . H32A H 0.3081 0.0192 0.7012 0.141 Uiso 1 1 calc R . . H32B H 0.3655 0.0424 0.6716 0.141 Uiso 1 1 calc R . . H32C H 0.2974 0.0845 0.6525 0.141 Uiso 1 1 calc R . . C33 C 0.3797(4) 0.2896(7) 0.6732(3) 0.113(3) Uani 1 1 d . . . H33A H 0.3537 0.2918 0.6425 0.169 Uiso 1 1 calc R . . H33B H 0.4213 0.2634 0.6686 0.169 Uiso 1 1 calc R . . H33C H 0.3831 0.3610 0.6868 0.169 Uiso 1 1 calc R . . C34 C 0.1534(4) 0.1698(7) 0.6813(3) 0.113(3) Uani 1 1 d . . . H34A H 0.1755 0.1191 0.6630 0.170 Uiso 1 1 calc R . . H34B H 0.1179 0.1994 0.6609 0.170 Uiso 1 1 calc R . . H34C H 0.1384 0.1338 0.7084 0.170 Uiso 1 1 calc R . . C35 C 0.2169(4) 0.3655(7) 0.6492(3) 0.112(3) Uani 1 1 d . . . H35A H 0.2389 0.4310 0.6590 0.168 Uiso 1 1 calc R . . H35B H 0.1755 0.3826 0.6332 0.168 Uiso 1 1 calc R . . H35C H 0.2406 0.3264 0.6273 0.168 Uiso 1 1 calc R . . C36 C 0.2141(3) 0.0373(5) 0.7908(2) 0.0655(18) Uani 1 1 d . . . H36A H 0.2561 0.0222 0.8072 0.079 Uiso 1 1 calc R . . H36B H 0.2163 0.0370 0.7561 0.079 Uiso 1 1 calc R . . C37 C 0.1681(3) -0.0433(6) 0.8039(3) 0.090(2) Uani 1 1 d . . . H37A H 0.1796 -0.0693 0.8367 0.108 Uiso 1 1 calc R . . H37B H 0.1662 -0.1043 0.7818 0.108 Uiso 1 1 calc R . . C38 C 0.1067(3) 0.0142(6) 0.7999(3) 0.090(2) Uani 1 1 d . . . H38A H 0.0801 -0.0132 0.8234 0.108 Uiso 1 1 calc R . . H38B H 0.0842 0.0060 0.7676 0.108 Uiso 1 1 calc R . . C39 C 0.1239(3) 0.1315(5) 0.8101(3) 0.0681(18) Uani 1 1 d . . . H39A H 0.0997 0.1782 0.7867 0.082 Uiso 1 1 calc R . . H39B H 0.1146 0.1516 0.8423 0.082 Uiso 1 1 calc R . . C40 C 0.1172(3) 0.4192(6) 0.8246(3) 0.078(2) Uani 1 1 d . . . H40A H 0.1302 0.4660 0.7995 0.093 Uiso 1 1 calc R . . H40B H 0.0872 0.3665 0.8096 0.093 Uiso 1 1 calc R . . C41 C 0.0874(4) 0.4834(7) 0.8606(3) 0.097(3) Uani 1 1 d . . . H41A H 0.0452 0.4561 0.8641 0.117 Uiso 1 1 calc R . . H41B H 0.0838 0.5585 0.8506 0.117 Uiso 1 1 calc R . . C42 C 0.1294(3) 0.4734(6) 0.9077(3) 0.082(2) Uani 1 1 d . . . H42A H 0.1567 0.5362 0.9134 0.099 Uiso 1 1 calc R . . H42B H 0.1043 0.4654 0.9347 0.099 Uiso 1 1 calc R . . C43 C 0.1673(3) 0.3752(5) 0.9015(2) 0.074(2) Uani 1 1 d . . . H43A H 0.2091 0.3817 0.9197 0.089 Uiso 1 1 calc R . . H43B H 0.1463 0.3123 0.9132 0.089 Uiso 1 1 calc R . . C44 C 0.2505(4) 0.5452(6) 0.7523(2) 0.089(2) Uani 1 1 d . . . H44A H 0.2867 0.5391 0.7340 0.107 Uiso 1 1 calc R . . H44B H 0.2133 0.5162 0.7329 0.107 Uiso 1 1 calc R . . C45 C 0.2400(6) 0.6576(7) 0.7648(3) 0.134(4) Uani 1 1 d . . . H45A H 0.2729 0.7026 0.7536 0.161 Uiso 1 1 calc R . . H45B H 0.1992 0.6818 0.7489 0.161 Uiso 1 1 calc R . . C46 C 0.2410(5) 0.6679(6) 0.8153(3) 0.119(3) Uani 1 1 d . . . H46A H 0.1983 0.6780 0.8240 0.143 Uiso 1 1 calc R . . H46B H 0.2668 0.7293 0.8271 0.143 Uiso 1 1 calc R . . C47 C 0.2682(4) 0.5684(5) 0.8360(2) 0.073(2) Uani 1 1 d . . . H47A H 0.2457 0.5456 0.8629 0.087 Uiso 1 1 calc R . . H47B H 0.3126 0.5792 0.8481 0.087 Uiso 1 1 calc R . . C48 C 0.2079(3) 0.7231(4) 0.6037(2) 0.0493(14) Uani 1 1 d . . . C49 C 0.2445(3) 0.7691(5) 0.6430(2) 0.0535(15) Uani 1 1 d . . . C50 C 0.3055(3) 0.7406(6) 0.6582(2) 0.0648(18) Uani 1 1 d . . . C51 C 0.3344(3) 0.6611(7) 0.6348(3) 0.078(2) Uani 1 1 d . . . C52 C 0.3004(3) 0.6089(6) 0.5969(3) 0.0677(19) Uani 1 1 d . . . C53 C 0.2391(3) 0.6404(5) 0.5827(2) 0.0557(16) Uani 1 1 d . . . C54 C 0.0976(2) 0.7252(4) 0.63508(19) 0.0459(14) Uani 1 1 d . . . C55 C 0.0766(3) 0.7891(5) 0.6702(2) 0.0545(15) Uani 1 1 d . . . C56 C 0.0521(3) 0.7491(6) 0.7109(2) 0.0609(17) Uani 1 1 d . . . C57 C 0.0487(3) 0.6414(6) 0.7175(2) 0.0638(18) Uani 1 1 d . . . C58 C 0.0687(3) 0.5727(5) 0.6838(3) 0.0622(17) Uani 1 1 d . . . C59 C 0.0923(3) 0.6150(5) 0.6433(2) 0.0541(15) Uani 1 1 d . . . C60 C 0.1017(3) 0.7165(4) 0.5352(2) 0.0455(13) Uani 1 1 d . . . C61 C 0.1307(3) 0.7390(4) 0.4937(2) 0.0509(15) Uani 1 1 d . . . C62 C 0.1048(3) 0.7127(5) 0.4473(2) 0.0587(16) Uani 1 1 d . . . C63 C 0.0476(4) 0.6616(5) 0.4404(2) 0.0642(18) Uani 1 1 d . . . C64 C 0.0168(3) 0.6394(5) 0.4793(3) 0.0565(16) Uani 1 1 d . . . C65 C 0.0432(3) 0.6676(4) 0.5248(2) 0.0508(15) Uani 1 1 d . . . C66 C 0.1295(3) 0.8964(4) 0.57782(18) 0.0431(13) Uani 1 1 d . . . C67 C 0.1788(3) 0.9659(5) 0.57223(19) 0.0481(14) Uani 1 1 d . . . C68 C 0.1697(3) 1.0731(5) 0.5595(2) 0.0543(16) Uani 1 1 d . . . C69 C 0.1106(3) 1.1141(5) 0.5503(2) 0.0620(17) Uani 1 1 d . . . C70 C 0.0599(3) 1.0483(5) 0.5546(2) 0.0575(16) Uani 1 1 d . . . C71 C 0.0701(3) 0.9433(4) 0.5681(2) 0.0477(14) Uani 1 1 d . . . B1 B 0.1342(3) 0.7642(5) 0.5880(2) 0.0450(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0397(3) 0.0423(3) 0.0402(3) 0.0018(3) 0.0005(2) 0.0026(3) Si1 0.0827(14) 0.0714(13) 0.0585(12) -0.0005(10) 0.0071(10) -0.0011(11) Si2 0.0944(15) 0.0867(15) 0.0514(11) -0.0048(11) -0.0005(11) 0.0195(13) F1 0.067(2) 0.067(2) 0.055(2) -0.0021(18) -0.0039(17) 0.0009(19) F2 0.071(3) 0.115(3) 0.090(3) 0.011(3) -0.026(2) -0.006(3) F3 0.052(2) 0.154(4) 0.119(4) 0.039(3) 0.001(2) 0.036(3) F4 0.090(3) 0.109(3) 0.114(4) 0.005(3) 0.026(3) 0.057(3) F5 0.081(3) 0.065(2) 0.074(3) -0.011(2) 0.013(2) 0.021(2) F6 0.087(3) 0.059(2) 0.061(2) -0.0086(18) 0.0203(19) -0.003(2) F7 0.099(3) 0.113(3) 0.056(2) -0.016(2) 0.025(2) -0.018(3) F8 0.090(3) 0.128(4) 0.061(3) 0.028(2) 0.012(2) -0.027(3) F9 0.091(3) 0.069(3) 0.104(3) 0.035(2) 0.011(2) -0.006(2) F10 0.084(3) 0.048(2) 0.079(3) 0.0082(19) 0.017(2) 0.0085(19) F11 0.066(2) 0.066(2) 0.058(2) 0.0012(18) 0.0161(17) -0.0018(19) F12 0.110(3) 0.090(3) 0.054(2) 0.001(2) 0.019(2) 0.015(2) F13 0.117(3) 0.099(3) 0.067(3) -0.023(2) -0.026(2) 0.013(3) F14 0.069(2) 0.057(2) 0.106(3) -0.014(2) -0.019(2) -0.002(2) F15 0.056(2) 0.062(2) 0.073(2) 0.0004(18) 0.0071(19) -0.0062(17) F16 0.052(2) 0.059(2) 0.068(2) 0.0144(17) 0.0075(17) 0.0006(17) F17 0.079(3) 0.062(2) 0.103(3) 0.022(2) 0.026(2) -0.005(2) F18 0.105(3) 0.055(2) 0.153(4) 0.037(3) 0.036(3) 0.021(2) F19 0.073(3) 0.067(2) 0.101(3) 0.018(2) 0.013(2) 0.027(2) F20 0.050(2) 0.055(2) 0.079(3) 0.0007(18) 0.0084(18) 0.0037(17) O1 0.043(2) 0.052(2) 0.076(3) -0.007(2) -0.002(2) 0.0005(19) O2 0.048(2) 0.058(3) 0.061(3) -0.001(2) 0.006(2) 0.005(2) O3 0.072(3) 0.049(2) 0.051(3) 0.006(2) 0.006(2) 0.011(2) N1 0.042(3) 0.036(2) 0.038(3) 0.003(2) 0.002(2) -0.003(2) N2 0.037(2) 0.035(2) 0.041(3) -0.0012(19) 0.005(2) -0.002(2) N3 0.066(3) 0.062(3) 0.050(3) -0.001(2) 0.006(3) 0.002(3) C1 0.042(3) 0.048(3) 0.027(3) 0.000(2) 0.008(2) 0.008(3) C2 0.040(3) 0.039(3) 0.048(4) 0.004(3) -0.002(3) 0.005(3) C3 0.040(3) 0.061(4) 0.053(4) 0.010(3) 0.002(3) -0.007(3) C4 0.056(4) 0.069(5) 0.100(6) 0.015(4) 0.009(4) -0.028(4) C5 0.075(5) 0.055(4) 0.100(6) -0.004(4) -0.010(5) -0.029(4) C6 0.071(4) 0.053(4) 0.063(4) -0.017(3) 0.000(4) -0.015(4) C7 0.049(3) 0.042(3) 0.052(4) -0.003(3) -0.002(3) 0.000(3) C8 0.060(4) 0.071(4) 0.061(4) 0.009(3) 0.022(3) -0.010(3) C9 0.127(7) 0.109(7) 0.081(6) 0.023(5) 0.032(5) -0.011(6) C10 0.100(6) 0.108(6) 0.075(5) -0.010(5) 0.023(5) 0.003(5) C11 0.071(4) 0.052(4) 0.039(3) -0.006(3) 0.002(3) 0.002(3) C12 0.092(5) 0.075(5) 0.059(4) -0.009(4) 0.017(4) 0.016(4) C13 0.111(6) 0.072(5) 0.048(4) -0.004(3) -0.007(4) 0.011(4) C14 0.038(3) 0.032(3) 0.039(3) 0.002(2) -0.003(2) 0.001(2) C15 0.038(3) 0.040(3) 0.039(3) 0.001(2) -0.003(2) -0.001(3) C16 0.053(4) 0.039(3) 0.056(4) -0.007(3) 0.006(3) 0.006(3) C17 0.071(4) 0.037(3) 0.066(4) 0.008(3) 0.009(3) 0.005(3) C18 0.059(4) 0.044(3) 0.057(4) 0.010(3) 0.013(3) -0.011(3) C19 0.048(3) 0.038(3) 0.041(3) 0.002(2) 0.012(3) 0.001(3) C20 0.055(4) 0.052(4) 0.052(4) -0.002(3) 0.015(3) 0.011(3) C21 0.046(4) 0.078(5) 0.091(5) -0.012(4) 0.016(4) 0.002(3) C22 0.072(5) 0.090(5) 0.063(5) -0.014(4) 0.015(4) 0.014(4) C23 0.062(4) 0.045(3) 0.058(4) 0.007(3) 0.023(3) 0.007(3) C24 0.090(5) 0.070(5) 0.072(5) -0.012(4) 0.034(4) 0.003(4) C25 0.065(4) 0.077(5) 0.088(5) 0.008(4) 0.031(4) -0.002(4) C26 0.045(3) 0.038(3) 0.043(3) -0.007(3) -0.002(3) 0.003(3) C27 0.051(4) 0.055(4) 0.063(4) -0.007(3) -0.002(3) 0.002(3) C28 0.048(4) 0.067(5) 0.092(5) -0.009(4) -0.021(4) 0.010(3) C29 0.084(6) 0.065(5) 0.079(5) -0.017(4) -0.040(5) 0.023(4) C30 0.093(6) 0.055(4) 0.056(4) 0.003(3) -0.020(4) 0.009(4) C31 0.066(4) 0.045(3) 0.041(3) -0.001(3) -0.010(3) 0.001(3) C32 0.109(6) 0.096(6) 0.076(5) -0.022(4) 0.007(5) 0.011(5) C33 0.128(7) 0.114(7) 0.105(7) 0.013(6) 0.056(6) 0.002(6) C34 0.099(6) 0.157(9) 0.076(6) -0.022(6) -0.022(5) -0.009(6) C35 0.148(8) 0.122(7) 0.065(5) 0.021(5) 0.007(5) 0.050(6) C36 0.059(4) 0.058(4) 0.076(5) -0.014(3) -0.004(3) 0.004(3) C37 0.074(5) 0.054(4) 0.137(7) -0.006(4) -0.007(5) 0.004(4) C38 0.076(5) 0.067(5) 0.122(7) -0.014(5) -0.005(5) -0.021(4) C39 0.048(4) 0.072(5) 0.084(5) -0.003(4) 0.007(3) -0.009(3) C40 0.058(4) 0.090(5) 0.083(5) -0.007(4) -0.003(4) 0.022(4) C41 0.089(6) 0.129(7) 0.078(6) 0.016(5) 0.029(5) 0.053(5) C42 0.083(5) 0.085(5) 0.082(5) 0.000(4) 0.023(4) 0.029(4) C43 0.089(5) 0.070(5) 0.064(5) 0.003(4) 0.015(4) 0.018(4) C44 0.142(7) 0.072(5) 0.056(5) 0.015(4) 0.024(5) 0.008(5) C45 0.254(13) 0.073(6) 0.076(6) 0.016(5) 0.019(7) 0.037(7) C46 0.201(11) 0.057(5) 0.096(7) 0.003(5) -0.001(7) 0.031(6) C47 0.093(5) 0.057(4) 0.065(5) 0.005(4) -0.006(4) 0.011(4) C48 0.051(3) 0.044(3) 0.055(4) 0.012(3) 0.014(3) 0.009(3) C49 0.056(4) 0.055(4) 0.049(4) 0.009(3) 0.004(3) -0.003(3) C50 0.052(4) 0.081(5) 0.059(4) 0.013(4) -0.005(3) -0.003(4) C51 0.046(4) 0.098(6) 0.089(6) 0.038(5) 0.002(4) 0.019(4) C52 0.056(4) 0.075(5) 0.074(5) 0.014(4) 0.015(4) 0.025(4) C53 0.059(4) 0.059(4) 0.049(4) 0.009(3) 0.010(3) 0.010(3) C54 0.040(3) 0.052(4) 0.044(3) 0.004(3) 0.001(3) 0.004(3) C55 0.056(4) 0.058(4) 0.049(4) 0.000(3) 0.001(3) -0.001(3) C56 0.060(4) 0.084(5) 0.039(4) -0.007(3) 0.008(3) -0.011(4) C57 0.053(4) 0.085(5) 0.053(4) 0.020(4) 0.005(3) -0.015(4) C58 0.054(4) 0.059(4) 0.071(5) 0.019(4) -0.005(3) -0.001(3) C59 0.054(4) 0.052(4) 0.055(4) 0.008(3) -0.002(3) 0.001(3) C60 0.052(3) 0.038(3) 0.047(3) 0.002(3) 0.007(3) 0.009(3) C61 0.055(4) 0.041(3) 0.056(4) -0.004(3) 0.002(3) 0.001(3) C62 0.077(5) 0.050(4) 0.049(4) -0.003(3) 0.009(3) 0.012(4) C63 0.085(5) 0.051(4) 0.053(4) -0.013(3) -0.010(4) 0.016(4) C64 0.055(4) 0.043(3) 0.069(5) -0.009(3) -0.007(3) 0.001(3) C65 0.051(4) 0.043(3) 0.058(4) -0.002(3) 0.005(3) 0.006(3) C66 0.049(3) 0.046(3) 0.034(3) 0.001(2) 0.005(3) 0.003(3) C67 0.054(4) 0.053(4) 0.037(3) 0.000(3) 0.004(3) 0.004(3) C68 0.062(4) 0.049(4) 0.056(4) 0.006(3) 0.023(3) -0.006(3) C69 0.078(5) 0.045(4) 0.066(4) 0.016(3) 0.023(4) 0.016(4) C70 0.063(4) 0.056(4) 0.055(4) 0.010(3) 0.013(3) 0.017(4) C71 0.049(4) 0.046(3) 0.049(4) 0.001(3) 0.012(3) 0.007(3) B1 0.053(4) 0.047(4) 0.037(4) -0.003(3) 0.011(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N3 2.217(5) . ? Y1 N1 2.372(4) . ? Y1 N2 2.392(4) . ? Y1 O2 2.400(4) . ? Y1 O1 2.403(4) . ? Y1 O3 2.436(4) . ? Y1 C1 2.841(5) . ? Y1 Si2 3.163(2) . ? Si1 N3 1.726(5) . ? Si1 C32 1.853(7) . ? Si1 C33 1.854(8) . ? Si1 H1 1.50(6) . ? Si2 N3 1.705(5) . ? Si2 C35 1.860(8) . ? Si2 C34 1.860(8) . ? Si2 H2 1.56(4) . ? F1 C49 1.350(7) . ? F2 C50 1.350(7) . ? F3 C51 1.349(7) . ? F4 C52 1.350(7) . ? F5 C53 1.364(7) . ? F6 C55 1.358(7) . ? F7 C56 1.355(7) . ? F8 C57 1.355(7) . ? F9 C58 1.351(7) . ? F10 C59 1.334(7) . ? F11 C61 1.358(6) . ? F12 C62 1.359(7) . ? F13 C63 1.351(7) . ? F14 C64 1.350(7) . ? F15 C65 1.352(6) . ? F16 C67 1.355(6) . ? F17 C68 1.358(6) . ? F18 C69 1.351(6) . ? F19 C70 1.349(7) . ? F20 C71 1.355(6) . ? O1 C39 1.441(7) . ? O1 C36 1.463(7) . ? O2 C43 1.452(7) . ? O2 C40 1.475(7) . ? O3 C47 1.452(7) . ? O3 C44 1.464(7) . ? N1 C1 1.346(6) . ? N1 C2 1.434(6) . ? N2 C1 1.338(6) . ? N2 C14 1.439(6) . ? C1 C26 1.504(7) . ? C2 C3 1.419(7) . ? C2 C7 1.422(7) . ? C3 C4 1.392(8) . ? C3 C8 1.510(8) . ? C4 C5 1.358(9) . ? C4 H4 0.9300 . ? C5 C6 1.371(9) . ? C5 H5 0.9300 . ? C6 C7 1.392(8) . ? C6 H6 0.9300 . ? C7 C11 1.514(8) . ? C8 C10 1.510(9) . ? C8 C9 1.534(9) . ? C8 H7 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.525(8) . ? C11 C13 1.529(8) . ? C11 H11 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.406(7) . ? C14 C19 1.411(7) . ? C15 C16 1.390(7) . ? C15 C20 1.516(7) . ? C16 C17 1.370(8) . ? C16 H16 0.9300 . ? C17 C18 1.370(8) . ? C17 H17 0.9300 . ? C18 C19 1.388(7) . ? C18 H18 0.9300 . ? C19 C23 1.517(7) . ? C20 C21 1.528(8) . ? C20 C22 1.533(8) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C25 1.525(8) . ? C23 C24 1.525(8) . ? C23 H23 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.397(7) . ? C26 C31 1.398(7) . ? C27 C28 1.387(8) . ? C27 H27 0.9300 . ? C28 C29 1.369(10) . ? C28 H28 0.9300 . ? C29 C30 1.360(9) . ? C29 H29 0.9300 . ? C30 C31 1.373(8) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.468(9) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.475(9) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.516(9) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.473(9) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.499(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.477(8) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.456(10) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.406(10) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.449(9) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C53 1.382(8) . ? C48 C49 1.388(8) . ? C48 B1 1.650(8) . ? C49 C50 1.358(8) . ? C50 C51 1.363(10) . ? C51 C52 1.368(10) . ? C52 C53 1.369(8) . ? C54 C55 1.369(8) . ? C54 C59 1.390(8) . ? C54 B1 1.664(8) . ? C55 C56 1.385(8) . ? C56 C57 1.348(9) . ? C57 C58 1.366(9) . ? C58 C59 1.383(8) . ? C60 C65 1.379(8) . ? C60 C61 1.390(8) . ? C60 B1 1.656(8) . ? C61 C62 1.380(8) . ? C62 C63 1.360(9) . ? C63 C64 1.349(9) . ? C64 C65 1.367(8) . ? C66 C67 1.373(7) . ? C66 C71 1.383(7) . ? C66 B1 1.660(8) . ? C67 C68 1.381(8) . ? C68 C69 1.347(8) . ? C69 C70 1.362(8) . ? C70 C71 1.362(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Y1 N1 115.73(17) . . ? N3 Y1 N2 113.98(16) . . ? N1 Y1 N2 56.09(14) . . ? N3 Y1 O2 132.89(16) . . ? N1 Y1 O2 107.14(14) . . ? N2 Y1 O2 105.44(14) . . ? N3 Y1 O1 83.67(16) . . ? N1 Y1 O1 135.73(14) . . ? N2 Y1 O1 79.82(13) . . ? O2 Y1 O1 78.82(13) . . ? N3 Y1 O3 92.85(16) . . ? N1 Y1 O3 81.62(14) . . ? N2 Y1 O3 136.26(14) . . ? O2 Y1 O3 74.46(13) . . ? O1 Y1 O3 139.65(13) . . ? N3 Y1 C1 117.79(16) . . ? N1 Y1 C1 28.13(14) . . ? N2 Y1 C1 27.98(14) . . ? O2 Y1 C1 109.17(14) . . ? O1 Y1 C1 107.76(14) . . ? O3 Y1 C1 109.28(15) . . ? N3 Y1 Si2 31.07(13) . . ? N1 Y1 Si2 141.89(11) . . ? N2 Y1 Si2 137.02(10) . . ? O2 Y1 Si2 101.82(10) . . ? O1 Y1 Si2 73.61(11) . . ? O3 Y1 Si2 82.86(10) . . ? C1 Y1 Si2 148.70(11) . . ? N3 Si1 C32 114.2(3) . . ? N3 Si1 C33 114.6(3) . . ? C32 Si1 C33 105.5(4) . . ? N3 Si1 H1 112(2) . . ? C32 Si1 H1 108(2) . . ? C33 Si1 H1 102(2) . . ? N3 Si2 C35 115.5(4) . . ? N3 Si2 C34 120.0(3) . . ? C35 Si2 C34 105.1(4) . . ? N3 Si2 Y1 42.17(17) . . ? C35 Si2 Y1 134.8(3) . . ? C34 Si2 Y1 120.1(3) . . ? N3 Si2 H2 102.0(16) . . ? C35 Si2 H2 109.8(16) . . ? C34 Si2 H2 103.5(16) . . ? Y1 Si2 H2 60.6(16) . . ? C39 O1 C36 108.1(4) . . ? C39 O1 Y1 132.6(3) . . ? C36 O1 Y1 119.2(3) . . ? C43 O2 C40 105.9(5) . . ? C43 O2 Y1 126.8(3) . . ? C40 O2 Y1 126.8(4) . . ? C47 O3 C44 105.9(5) . . ? C47 O3 Y1 123.7(3) . . ? C44 O3 Y1 130.1(4) . . ? C1 N1 C2 123.0(4) . . ? C1 N1 Y1 95.7(3) . . ? C2 N1 Y1 140.8(3) . . ? C1 N2 C14 122.2(4) . . ? C1 N2 Y1 95.0(3) . . ? C14 N2 Y1 142.5(3) . . ? Si2 N3 Si1 122.2(3) . . ? Si2 N3 Y1 106.8(2) . . ? Si1 N3 Y1 131.1(3) . . ? N2 C1 N1 113.2(4) . . ? N2 C1 C26 123.8(5) . . ? N1 C1 C26 122.9(5) . . ? N2 C1 Y1 57.0(2) . . ? N1 C1 Y1 56.2(3) . . ? C26 C1 Y1 175.8(3) . . ? C3 C2 C7 119.5(5) . . ? C3 C2 N1 118.6(5) . . ? C7 C2 N1 121.7(5) . . ? C4 C3 C2 117.9(6) . . ? C4 C3 C8 119.4(6) . . ? C2 C3 C8 122.7(5) . . ? C5 C4 C3 122.6(6) . . ? C5 C4 H4 118.7 . . ? C3 C4 H4 118.7 . . ? C4 C5 C6 119.9(6) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 121.3(6) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C6 C7 C2 118.7(6) . . ? C6 C7 C11 117.6(5) . . ? C2 C7 C11 123.6(5) . . ? C10 C8 C3 112.2(6) . . ? C10 C8 C9 110.0(6) . . ? C3 C8 C9 112.1(6) . . ? C10 C8 H7 107.4 . . ? C3 C8 H7 107.4 . . ? C9 C8 H7 107.4 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 C12 111.0(5) . . ? C7 C11 C13 111.7(5) . . ? C12 C11 C13 109.2(5) . . ? C7 C11 H11 108.3 . . ? C12 C11 H11 108.3 . . ? C13 C11 H11 108.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 119.7(5) . . ? C15 C14 N2 121.7(5) . . ? C19 C14 N2 118.4(4) . . ? C16 C15 C14 118.7(5) . . ? C16 C15 C20 117.5(5) . . ? C14 C15 C20 123.8(5) . . ? C17 C16 C15 122.0(5) . . ? C17 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C18 C17 C16 118.8(5) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C17 C18 C19 122.4(5) . . ? C17 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C18 C19 C14 118.3(5) . . ? C18 C19 C23 119.8(5) . . ? C14 C19 C23 121.9(5) . . ? C15 C20 C21 112.5(5) . . ? C15 C20 C22 110.1(5) . . ? C21 C20 C22 108.8(5) . . ? C15 C20 H20 108.5 . . ? C21 C20 H20 108.5 . . ? C22 C20 H20 108.5 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 C25 114.5(5) . . ? C19 C23 C24 111.3(5) . . ? C25 C23 C24 108.8(5) . . ? C19 C23 H23 107.3 . . ? C25 C23 H23 107.3 . . ? C24 C23 H23 107.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 117.7(5) . . ? C27 C26 C1 120.7(5) . . ? C31 C26 C1 121.6(5) . . ? C28 C27 C26 120.4(6) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C29 C28 C27 120.7(7) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C28 119.2(6) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C29 C30 C31 121.7(7) . . ? C29 C30 H30 119.1 . . ? C31 C30 H30 119.1 . . ? C30 C31 C26 120.3(6) . . ? C30 C31 H31 119.9 . . ? C26 C31 H31 119.9 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O1 C36 C37 105.9(5) . . ? O1 C36 H36A 110.6 . . ? C37 C36 H36A 110.6 . . ? O1 C36 H36B 110.6 . . ? C37 C36 H36B 110.6 . . ? H36A C36 H36B 108.7 . . ? C36 C37 C38 104.9(6) . . ? C36 C37 H37A 110.8 . . ? C38 C37 H37A 110.8 . . ? C36 C37 H37B 110.8 . . ? C38 C37 H37B 110.8 . . ? H37A C37 H37B 108.8 . . ? C37 C38 C39 104.9(6) . . ? C37 C38 H38A 110.8 . . ? C39 C38 H38A 110.8 . . ? C37 C38 H38B 110.8 . . ? C39 C38 H38B 110.8 . . ? H38A C38 H38B 108.8 . . ? O1 C39 C38 106.7(5) . . ? O1 C39 H39A 110.4 . . ? C38 C39 H39A 110.4 . . ? O1 C39 H39B 110.4 . . ? C38 C39 H39B 110.4 . . ? H39A C39 H39B 108.6 . . ? C41 C40 O2 107.8(6) . . ? C41 C40 H40A 110.1 . . ? O2 C40 H40A 110.1 . . ? C41 C40 H40B 110.1 . . ? O2 C40 H40B 110.1 . . ? H40A C40 H40B 108.5 . . ? C40 C41 C42 106.8(6) . . ? C40 C41 H41A 110.4 . . ? C42 C41 H41A 110.4 . . ? C40 C41 H41B 110.4 . . ? C42 C41 H41B 110.4 . . ? H41A C41 H41B 108.6 . . ? C43 C42 C41 104.1(6) . . ? C43 C42 H42A 110.9 . . ? C41 C42 H42A 110.9 . . ? C43 C42 H42B 110.9 . . ? C41 C42 H42B 110.9 . . ? H42A C42 H42B 109.0 . . ? O2 C43 C42 107.4(5) . . ? O2 C43 H43A 110.2 . . ? C42 C43 H43A 110.2 . . ? O2 C43 H43B 110.2 . . ? C42 C43 H43B 110.2 . . ? H43A C43 H43B 108.5 . . ? C45 C44 O3 106.4(6) . . ? C45 C44 H44A 110.4 . . ? O3 C44 H44A 110.4 . . ? C45 C44 H44B 110.4 . . ? O3 C44 H44B 110.4 . . ? H44A C44 H44B 108.6 . . ? C46 C45 C44 109.7(7) . . ? C46 C45 H45A 109.7 . . ? C44 C45 H45A 109.7 . . ? C46 C45 H45B 109.7 . . ? C44 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? C45 C46 C47 106.2(7) . . ? C45 C46 H46A 110.5 . . ? C47 C46 H46A 110.5 . . ? C45 C46 H46B 110.5 . . ? C47 C46 H46B 110.5 . . ? H46A C46 H46B 108.7 . . ? C46 C47 O3 108.0(6) . . ? C46 C47 H47A 110.1 . . ? O3 C47 H47A 110.1 . . ? C46 C47 H47B 110.1 . . ? O3 C47 H47B 110.1 . . ? H47A C47 H47B 108.4 . . ? C53 C48 C49 112.5(5) . . ? C53 C48 B1 126.8(5) . . ? C49 C48 B1 120.6(5) . . ? F1 C49 C50 117.1(6) . . ? F1 C49 C48 118.5(5) . . ? C50 C49 C48 124.4(6) . . ? F2 C50 C49 120.7(7) . . ? F2 C50 C51 119.2(6) . . ? C49 C50 C51 120.1(7) . . ? F3 C51 C50 120.5(8) . . ? F3 C51 C52 120.7(8) . . ? C50 C51 C52 118.8(6) . . ? F4 C52 C51 119.6(6) . . ? F4 C52 C53 121.3(7) . . ? C51 C52 C53 119.1(7) . . ? F5 C53 C52 114.3(6) . . ? F5 C53 C48 120.7(5) . . ? C52 C53 C48 124.9(6) . . ? C55 C54 C59 114.2(5) . . ? C55 C54 B1 127.6(5) . . ? C59 C54 B1 117.9(5) . . ? F6 C55 C54 121.5(5) . . ? F6 C55 C56 114.7(5) . . ? C54 C55 C56 123.7(6) . . ? C57 C56 F7 120.2(6) . . ? C57 C56 C55 119.7(6) . . ? F7 C56 C55 120.1(6) . . ? C56 C57 F8 120.1(7) . . ? C56 C57 C58 119.8(6) . . ? F8 C57 C58 120.2(7) . . ? F9 C58 C57 120.3(6) . . ? F9 C58 C59 120.4(7) . . ? C57 C58 C59 119.3(6) . . ? F10 C59 C58 116.7(6) . . ? F10 C59 C54 120.0(5) . . ? C58 C59 C54 123.3(6) . . ? C65 C60 C61 112.6(5) . . ? C65 C60 B1 127.9(5) . . ? C61 C60 B1 118.9(5) . . ? F11 C61 C62 116.1(6) . . ? F11 C61 C60 119.9(5) . . ? C62 C61 C60 124.0(6) . . ? F12 C62 C63 120.6(6) . . ? F12 C62 C61 119.8(6) . . ? C63 C62 C61 119.6(6) . . ? C64 C63 F13 121.5(7) . . ? C64 C63 C62 119.1(6) . . ? F13 C63 C62 119.5(7) . . ? C63 C64 F14 119.6(6) . . ? C63 C64 C65 120.1(6) . . ? F14 C64 C65 120.3(6) . . ? F15 C65 C64 114.8(6) . . ? F15 C65 C60 120.5(5) . . ? C64 C65 C60 124.6(6) . . ? C67 C66 C71 113.6(5) . . ? C67 C66 B1 127.2(5) . . ? C71 C66 B1 118.8(5) . . ? F16 C67 C66 121.9(5) . . ? F16 C67 C68 115.1(5) . . ? C66 C67 C68 123.0(6) . . ? C69 C68 F17 120.5(5) . . ? C69 C68 C67 120.6(6) . . ? F17 C68 C67 118.8(6) . . ? C68 C69 F18 120.1(6) . . ? C68 C69 C70 118.8(6) . . ? F18 C69 C70 121.2(6) . . ? F19 C70 C69 119.8(5) . . ? F19 C70 C71 120.7(6) . . ? C69 C70 C71 119.5(6) . . ? F20 C71 C70 115.9(5) . . ? F20 C71 C66 119.6(5) . . ? C70 C71 C66 124.5(6) . . ? C48 B1 C60 114.1(5) . . ? C48 B1 C66 112.6(5) . . ? C60 B1 C66 101.0(4) . . ? C48 B1 C54 102.3(4) . . ? C60 B1 C54 114.1(5) . . ? C66 B1 C54 113.3(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Y1 Si2 N3 41.2(3) . . . . ? N2 Y1 Si2 N3 -51.3(3) . . . . ? O2 Y1 Si2 N3 -179.8(3) . . . . ? O1 Y1 Si2 N3 -105.4(3) . . . . ? O3 Y1 Si2 N3 107.7(3) . . . . ? C1 Y1 Si2 N3 -8.0(4) . . . . ? N3 Y1 Si2 C35 -78.9(5) . . . . ? N1 Y1 Si2 C35 -37.7(4) . . . . ? N2 Y1 Si2 C35 -130.1(4) . . . . ? O2 Y1 Si2 C35 101.3(4) . . . . ? O1 Y1 Si2 C35 175.8(4) . . . . ? O3 Y1 Si2 C35 28.9(4) . . . . ? C1 Y1 Si2 C35 -86.9(4) . . . . ? N3 Y1 Si2 C34 102.8(4) . . . . ? N1 Y1 Si2 C34 143.9(4) . . . . ? N2 Y1 Si2 C34 51.5(4) . . . . ? O2 Y1 Si2 C34 -77.1(4) . . . . ? O1 Y1 Si2 C34 -2.6(3) . . . . ? O3 Y1 Si2 C34 -149.5(4) . . . . ? C1 Y1 Si2 C34 94.8(4) . . . . ? N3 Y1 O1 C39 -120.6(5) . . . . ? N1 Y1 O1 C39 118.6(5) . . . . ? N2 Y1 O1 C39 123.6(5) . . . . ? O2 Y1 O1 C39 15.4(5) . . . . ? O3 Y1 O1 C39 -33.7(6) . . . . ? C1 Y1 O1 C39 122.2(5) . . . . ? Si2 Y1 O1 C39 -90.6(5) . . . . ? N3 Y1 O1 C36 53.4(4) . . . . ? N1 Y1 O1 C36 -67.4(5) . . . . ? N2 Y1 O1 C36 -62.4(4) . . . . ? O2 Y1 O1 C36 -170.5(4) . . . . ? O3 Y1 O1 C36 140.3(4) . . . . ? C1 Y1 O1 C36 -63.8(4) . . . . ? Si2 Y1 O1 C36 83.5(4) . . . . ? N3 Y1 O2 C43 172.0(4) . . . . ? N1 Y1 O2 C43 -32.9(5) . . . . ? N2 Y1 O2 C43 25.7(5) . . . . ? O1 Y1 O2 C43 101.7(5) . . . . ? O3 Y1 O2 C43 -108.8(5) . . . . ? C1 Y1 O2 C43 -3.4(5) . . . . ? Si2 Y1 O2 C43 172.1(4) . . . . ? N3 Y1 O2 C40 -17.5(5) . . . . ? N1 Y1 O2 C40 137.5(5) . . . . ? N2 Y1 O2 C40 -163.8(5) . . . . ? O1 Y1 O2 C40 -87.8(5) . . . . ? O3 Y1 O2 C40 61.7(5) . . . . ? C1 Y1 O2 C40 167.1(5) . . . . ? Si2 Y1 O2 C40 -17.4(5) . . . . ? N3 Y1 O3 C47 -166.0(5) . . . . ? N1 Y1 O3 C47 -50.4(5) . . . . ? N2 Y1 O3 C47 -36.1(5) . . . . ? O2 Y1 O3 C47 60.1(4) . . . . ? O1 Y1 O3 C47 110.5(5) . . . . ? C1 Y1 O3 C47 -45.2(5) . . . . ? Si2 Y1 O3 C47 164.6(5) . . . . ? N3 Y1 O3 C44 21.2(6) . . . . ? N1 Y1 O3 C44 136.8(6) . . . . ? N2 Y1 O3 C44 151.1(5) . . . . ? O2 Y1 O3 C44 -112.7(6) . . . . ? O1 Y1 O3 C44 -62.3(6) . . . . ? C1 Y1 O3 C44 142.0(5) . . . . ? Si2 Y1 O3 C44 -8.3(5) . . . . ? N3 Y1 N1 C1 -101.3(3) . . . . ? N2 Y1 N1 C1 1.4(3) . . . . ? O2 Y1 N1 C1 98.7(3) . . . . ? O1 Y1 N1 C1 7.3(4) . . . . ? O3 Y1 N1 C1 169.5(3) . . . . ? Si2 Y1 N1 C1 -123.5(3) . . . . ? N3 Y1 N1 C2 87.3(5) . . . . ? N2 Y1 N1 C2 -170.1(6) . . . . ? O2 Y1 N1 C2 -72.7(5) . . . . ? O1 Y1 N1 C2 -164.1(5) . . . . ? O3 Y1 N1 C2 -1.9(5) . . . . ? C1 Y1 N1 C2 -171.4(7) . . . . ? Si2 Y1 N1 C2 65.1(6) . . . . ? N3 Y1 N2 C1 104.5(3) . . . . ? N1 Y1 N2 C1 -1.4(3) . . . . ? O2 Y1 N2 C1 -101.9(3) . . . . ? O1 Y1 N2 C1 -177.2(3) . . . . ? O3 Y1 N2 C1 -18.4(4) . . . . ? Si2 Y1 N2 C1 130.7(3) . . . . ? N3 Y1 N2 C14 -68.2(6) . . . . ? N1 Y1 N2 C14 -174.1(6) . . . . ? O2 Y1 N2 C14 85.4(5) . . . . ? O1 Y1 N2 C14 10.1(5) . . . . ? O3 Y1 N2 C14 168.9(5) . . . . ? C1 Y1 N2 C14 -172.7(7) . . . . ? Si2 Y1 N2 C14 -42.1(6) . . . . ? C35 Si2 N3 Si1 -51.5(5) . . . . ? C34 Si2 N3 Si1 76.0(5) . . . . ? Y1 Si2 N3 Si1 179.0(5) . . . . ? C35 Si2 N3 Y1 129.5(3) . . . . ? C34 Si2 N3 Y1 -103.0(4) . . . . ? C32 Si1 N3 Si2 -56.1(5) . . . . ? C33 Si1 N3 Si2 65.8(5) . . . . ? C32 Si1 N3 Y1 122.6(4) . . . . ? C33 Si1 N3 Y1 -115.5(4) . . . . ? N1 Y1 N3 Si2 -153.2(2) . . . . ? N2 Y1 N3 Si2 144.4(2) . . . . ? O2 Y1 N3 Si2 0.2(4) . . . . ? O1 Y1 N3 Si2 68.5(2) . . . . ? O3 Y1 N3 Si2 -71.1(2) . . . . ? C1 Y1 N3 Si2 175.3(2) . . . . ? N1 Y1 N3 Si1 27.9(4) . . . . ? N2 Y1 N3 Si1 -34.5(4) . . . . ? O2 Y1 N3 Si1 -178.7(3) . . . . ? O1 Y1 N3 Si1 -110.4(4) . . . . ? O3 Y1 N3 Si1 110.0(4) . . . . ? C1 Y1 N3 Si1 -3.6(4) . . . . ? Si2 Y1 N3 Si1 -178.9(6) . . . . ? C14 N2 C1 N1 176.9(4) . . . . ? Y1 N2 C1 N1 2.2(4) . . . . ? C14 N2 C1 C26 -0.4(7) . . . . ? Y1 N2 C1 C26 -175.1(4) . . . . ? C14 N2 C1 Y1 174.8(5) . . . . ? C2 N1 C1 N2 171.4(4) . . . . ? Y1 N1 C1 N2 -2.2(4) . . . . ? C2 N1 C1 C26 -11.3(7) . . . . ? Y1 N1 C1 C26 175.1(4) . . . . ? C2 N1 C1 Y1 173.5(5) . . . . ? N3 Y1 C1 N2 -89.3(3) . . . . ? N1 Y1 C1 N2 177.6(5) . . . . ? O2 Y1 C1 N2 86.9(3) . . . . ? O1 Y1 C1 N2 2.9(3) . . . . ? O3 Y1 C1 N2 166.6(3) . . . . ? Si2 Y1 C1 N2 -84.6(3) . . . . ? N3 Y1 C1 N1 93.1(3) . . . . ? N2 Y1 C1 N1 -177.6(5) . . . . ? O2 Y1 C1 N1 -90.7(3) . . . . ? O1 Y1 C1 N1 -174.7(3) . . . . ? O3 Y1 C1 N1 -11.0(3) . . . . ? Si2 Y1 C1 N1 97.8(3) . . . . ? N3 Y1 C1 C26 14(5) . . . . ? N1 Y1 C1 C26 -80(5) . . . . ? N2 Y1 C1 C26 103(5) . . . . ? O2 Y1 C1 C26 -170(5) . . . . ? O1 Y1 C1 C26 106(5) . . . . ? O3 Y1 C1 C26 -91(5) . . . . ? Si2 Y1 C1 C26 18(5) . . . . ? C1 N1 C2 C3 121.0(5) . . . . ? Y1 N1 C2 C3 -69.2(7) . . . . ? C1 N1 C2 C7 -63.7(7) . . . . ? Y1 N1 C2 C7 106.1(6) . . . . ? C7 C2 C3 C4 3.1(8) . . . . ? N1 C2 C3 C4 178.5(5) . . . . ? C7 C2 C3 C8 -177.4(5) . . . . ? N1 C2 C3 C8 -2.0(8) . . . . ? C2 C3 C4 C5 -1.1(10) . . . . ? C8 C3 C4 C5 179.3(6) . . . . ? C3 C4 C5 C6 -1.0(11) . . . . ? C4 C5 C6 C7 1.1(11) . . . . ? C5 C6 C7 C2 0.9(9) . . . . ? C5 C6 C7 C11 -176.5(6) . . . . ? C3 C2 C7 C6 -3.0(8) . . . . ? N1 C2 C7 C6 -178.2(5) . . . . ? C3 C2 C7 C11 174.2(5) . . . . ? N1 C2 C7 C11 -1.0(8) . . . . ? C4 C3 C8 C10 87.1(7) . . . . ? C2 C3 C8 C10 -92.5(7) . . . . ? C4 C3 C8 C9 -37.4(8) . . . . ? C2 C3 C8 C9 143.1(6) . . . . ? C6 C7 C11 C12 61.8(7) . . . . ? C2 C7 C11 C12 -115.4(6) . . . . ? C6 C7 C11 C13 -60.4(7) . . . . ? C2 C7 C11 C13 122.4(6) . . . . ? C1 N2 C14 C15 -71.9(6) . . . . ? Y1 N2 C14 C15 99.6(6) . . . . ? C1 N2 C14 C19 111.9(5) . . . . ? Y1 N2 C14 C19 -76.7(7) . . . . ? C19 C14 C15 C16 -2.5(7) . . . . ? N2 C14 C15 C16 -178.7(5) . . . . ? C19 C14 C15 C20 176.5(5) . . . . ? N2 C14 C15 C20 0.3(8) . . . . ? C14 C15 C16 C17 0.4(8) . . . . ? C20 C15 C16 C17 -178.7(5) . . . . ? C15 C16 C17 C18 1.4(9) . . . . ? C16 C17 C18 C19 -1.0(9) . . . . ? C17 C18 C19 C14 -1.1(9) . . . . ? C17 C18 C19 C23 179.0(5) . . . . ? C15 C14 C19 C18 2.9(8) . . . . ? N2 C14 C19 C18 179.1(5) . . . . ? C15 C14 C19 C23 -177.3(5) . . . . ? N2 C14 C19 C23 -1.0(7) . . . . ? C16 C15 C20 C21 -59.3(7) . . . . ? C14 C15 C20 C21 121.7(6) . . . . ? C16 C15 C20 C22 62.2(7) . . . . ? C14 C15 C20 C22 -116.8(6) . . . . ? C18 C19 C23 C25 -33.8(8) . . . . ? C14 C19 C23 C25 146.3(5) . . . . ? C18 C19 C23 C24 90.0(6) . . . . ? C14 C19 C23 C24 -89.9(6) . . . . ? N2 C1 C26 C27 139.8(5) . . . . ? N1 C1 C26 C27 -37.2(7) . . . . ? Y1 C1 C26 C27 40(5) . . . . ? N2 C1 C26 C31 -40.7(7) . . . . ? N1 C1 C26 C31 142.3(5) . . . . ? Y1 C1 C26 C31 -141(5) . . . . ? C31 C26 C27 C28 2.0(8) . . . . ? C1 C26 C27 C28 -178.5(5) . . . . ? C26 C27 C28 C29 -1.8(10) . . . . ? C27 C28 C29 C30 0.6(10) . . . . ? C28 C29 C30 C31 0.4(10) . . . . ? C29 C30 C31 C26 -0.1(9) . . . . ? C27 C26 C31 C30 -1.1(8) . . . . ? C1 C26 C31 C30 179.5(5) . . . . ? C39 O1 C36 C37 -21.9(7) . . . . ? Y1 O1 C36 C37 162.7(4) . . . . ? O1 C36 C37 C38 31.1(8) . . . . ? C36 C37 C38 C39 -28.2(8) . . . . ? C36 O1 C39 C38 4.1(7) . . . . ? Y1 O1 C39 C38 178.6(4) . . . . ? C37 C38 C39 O1 15.0(8) . . . . ? C43 O2 C40 C41 13.0(8) . . . . ? Y1 O2 C40 C41 -159.1(5) . . . . ? O2 C40 C41 C42 4.6(9) . . . . ? C40 C41 C42 C43 -20.0(9) . . . . ? C40 O2 C43 C42 -26.0(7) . . . . ? Y1 O2 C43 C42 146.0(5) . . . . ? C41 C42 C43 O2 28.5(8) . . . . ? C47 O3 C44 C45 -8.4(9) . . . . ? Y1 O3 C44 C45 165.4(6) . . . . ? O3 C44 C45 C46 -3.7(12) . . . . ? C44 C45 C46 C47 14.4(13) . . . . ? C45 C46 C47 O3 -19.7(11) . . . . ? C44 O3 C47 C46 17.4(8) . . . . ? Y1 O3 C47 C46 -156.9(6) . . . . ? C53 C48 C49 F1 -176.9(5) . . . . ? B1 C48 C49 F1 0.4(8) . . . . ? C53 C48 C49 C50 3.1(8) . . . . ? B1 C48 C49 C50 -179.6(6) . . . . ? F1 C49 C50 F2 -1.3(9) . . . . ? C48 C49 C50 F2 178.7(5) . . . . ? F1 C49 C50 C51 179.2(6) . . . . ? C48 C49 C50 C51 -0.8(10) . . . . ? F2 C50 C51 F3 -0.5(10) . . . . ? C49 C50 C51 F3 179.0(6) . . . . ? F2 C50 C51 C52 178.6(6) . . . . ? C49 C50 C51 C52 -1.9(10) . . . . ? F3 C51 C52 F4 0.2(10) . . . . ? C50 C51 C52 F4 -178.9(6) . . . . ? F3 C51 C52 C53 -178.9(6) . . . . ? C50 C51 C52 C53 2.0(10) . . . . ? F4 C52 C53 F5 2.6(9) . . . . ? C51 C52 C53 F5 -178.4(6) . . . . ? F4 C52 C53 C48 -178.5(6) . . . . ? C51 C52 C53 C48 0.6(10) . . . . ? C49 C48 C53 F5 175.9(5) . . . . ? B1 C48 C53 F5 -1.2(9) . . . . ? C49 C48 C53 C52 -3.0(9) . . . . ? B1 C48 C53 C52 179.9(6) . . . . ? C59 C54 C55 F6 178.2(5) . . . . ? B1 C54 C55 F6 4.6(9) . . . . ? C59 C54 C55 C56 0.2(9) . . . . ? B1 C54 C55 C56 -173.4(5) . . . . ? F6 C55 C56 C57 -177.4(6) . . . . ? C54 C55 C56 C57 0.7(10) . . . . ? F6 C55 C56 F7 2.6(8) . . . . ? C54 C55 C56 F7 -179.3(5) . . . . ? F7 C56 C57 F8 -1.6(10) . . . . ? C55 C56 C57 F8 178.4(5) . . . . ? F7 C56 C57 C58 179.2(6) . . . . ? C55 C56 C57 C58 -0.9(10) . . . . ? C56 C57 C58 F9 -179.9(6) . . . . ? F8 C57 C58 F9 0.9(9) . . . . ? C56 C57 C58 C59 0.1(10) . . . . ? F8 C57 C58 C59 -179.1(5) . . . . ? F9 C58 C59 F10 0.0(8) . . . . ? C57 C58 C59 F10 -180.0(5) . . . . ? F9 C58 C59 C54 -179.2(5) . . . . ? C57 C58 C59 C54 0.9(9) . . . . ? C55 C54 C59 F10 179.9(5) . . . . ? B1 C54 C59 F10 -5.8(8) . . . . ? C55 C54 C59 C58 -1.0(8) . . . . ? B1 C54 C59 C58 173.3(5) . . . . ? C65 C60 C61 F11 178.2(5) . . . . ? B1 C60 C61 F11 6.5(7) . . . . ? C65 C60 C61 C62 -1.8(8) . . . . ? B1 C60 C61 C62 -173.5(5) . . . . ? F11 C61 C62 F12 -0.3(8) . . . . ? C60 C61 C62 F12 179.7(5) . . . . ? F11 C61 C62 C63 -180.0(5) . . . . ? C60 C61 C62 C63 0.0(9) . . . . ? F12 C62 C63 C64 -178.6(5) . . . . ? C61 C62 C63 C64 1.1(9) . . . . ? F12 C62 C63 F13 0.5(9) . . . . ? C61 C62 C63 F13 -179.9(5) . . . . ? F13 C63 C64 F14 1.3(9) . . . . ? C62 C63 C64 F14 -179.7(5) . . . . ? F13 C63 C64 C65 -179.4(5) . . . . ? C62 C63 C64 C65 -0.3(9) . . . . ? C63 C64 C65 F15 177.6(5) . . . . ? F14 C64 C65 F15 -3.0(8) . . . . ? C63 C64 C65 C60 -1.7(9) . . . . ? F14 C64 C65 C60 177.6(5) . . . . ? C61 C60 C65 F15 -176.7(5) . . . . ? B1 C60 C65 F15 -5.9(8) . . . . ? C61 C60 C65 C64 2.6(8) . . . . ? B1 C60 C65 C64 173.4(5) . . . . ? C71 C66 C67 F16 -178.6(5) . . . . ? B1 C66 C67 F16 -6.6(8) . . . . ? C71 C66 C67 C68 1.9(8) . . . . ? B1 C66 C67 C68 173.9(5) . . . . ? F16 C67 C68 C69 178.3(5) . . . . ? C66 C67 C68 C69 -2.2(9) . . . . ? F16 C67 C68 F17 -2.2(8) . . . . ? C66 C67 C68 F17 177.3(5) . . . . ? F17 C68 C69 F18 0.4(9) . . . . ? C67 C68 C69 F18 179.9(6) . . . . ? F17 C68 C69 C70 -178.3(6) . . . . ? C67 C68 C69 C70 1.2(10) . . . . ? C68 C69 C70 F19 179.5(6) . . . . ? F18 C69 C70 F19 0.8(10) . . . . ? C68 C69 C70 C71 0.0(10) . . . . ? F18 C69 C70 C71 -178.7(6) . . . . ? F19 C70 C71 F20 1.3(8) . . . . ? C69 C70 C71 F20 -179.2(5) . . . . ? F19 C70 C71 C66 -179.8(5) . . . . ? C69 C70 C71 C66 -0.2(9) . . . . ? C67 C66 C71 F20 178.3(5) . . . . ? B1 C66 C71 F20 5.5(8) . . . . ? C67 C66 C71 C70 -0.7(8) . . . . ? B1 C66 C71 C70 -173.5(5) . . . . ? C53 C48 B1 C60 -13.1(8) . . . . ? C49 C48 B1 C60 170.0(5) . . . . ? C53 C48 B1 C66 -127.5(6) . . . . ? C49 C48 B1 C66 55.6(7) . . . . ? C53 C48 B1 C54 110.6(6) . . . . ? C49 C48 B1 C54 -66.3(6) . . . . ? C65 C60 B1 C48 130.5(6) . . . . ? C61 C60 B1 C48 -59.3(7) . . . . ? C65 C60 B1 C66 -108.5(6) . . . . ? C61 C60 B1 C66 61.8(6) . . . . ? C65 C60 B1 C54 13.4(8) . . . . ? C61 C60 B1 C54 -176.4(5) . . . . ? C67 C66 B1 C48 13.3(8) . . . . ? C71 C66 B1 C48 -175.0(5) . . . . ? C67 C66 B1 C60 -108.8(6) . . . . ? C71 C66 B1 C60 62.9(6) . . . . ? C67 C66 B1 C54 128.8(6) . . . . ? C71 C66 B1 C54 -59.5(7) . . . . ? C55 C54 B1 C48 107.5(6) . . . . ? C59 C54 B1 C48 -65.9(6) . . . . ? C55 C54 B1 C60 -128.7(6) . . . . ? C59 C54 B1 C60 57.9(7) . . . . ? C55 C54 B1 C66 -13.9(8) . . . . ? C59 C54 B1 C66 172.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.270 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.055 data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 894307' #TrackingRef 'CCDC.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H47 Al2 N2 Y' _chemical_formula_sum 'C31 H47 Al2 N2 Y' _chemical_formula_weight 590.58 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' Y Y -2.7962 3.5667 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.094(3) _cell_length_b 14.327(3) _cell_length_c 16.524(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.951(6) _cell_angle_gamma 90.00 _cell_volume 3296.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13700 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 1.843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.368 _exptl_absorpt_correction_T_max 0.692 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16494 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.0854 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6115 _reflns_number_gt 4230 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6115 _refine_ls_number_parameters 370 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.1755 _refine_ls_wR_factor_gt 0.1568 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.106 _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 Y1 Y 0.38175(4) 0.69818(3) 0.69717(3) 0.03943(19) Uani 1 1 d . . . Al1 Al 0.26428(13) 0.78883(12) 0.81869(11) 0.0513(5) Uani 1 1 d . . . Al2 Al 0.23347(12) 0.62151(11) 0.55580(10) 0.0479(4) Uani 1 1 d . . . N1 N 0.5278(3) 0.6478(3) 0.7657(2) 0.0397(10) Uani 1 1 d . . . N2 N 0.5247(3) 0.7338(3) 0.6524(3) 0.0406(10) Uani 1 1 d . . . C1 C 0.5805(4) 0.6885(3) 0.7144(3) 0.0398(12) Uani 1 1 d . . . C2 C 0.5676(4) 0.5815(3) 0.8274(3) 0.0409(12) Uani 1 1 d . . . C3 C 0.6001(4) 0.4935(4) 0.8061(3) 0.0461(13) Uani 1 1 d . . . C4 C 0.6329(4) 0.4312(4) 0.8690(4) 0.0576(16) Uani 1 1 d . . . H4 H 0.6547 0.3718 0.8560 0.069 Uiso 1 1 calc R . . C5 C 0.6339(5) 0.4550(4) 0.9494(4) 0.0657(18) Uani 1 1 d . . . H5 H 0.6577 0.4125 0.9910 0.079 Uiso 1 1 calc R . . C6 C 0.6007(4) 0.5400(5) 0.9694(4) 0.0588(16) Uani 1 1 d . . . H6 H 0.6011 0.5549 1.0248 0.071 Uiso 1 1 calc R . . C7 C 0.5665(4) 0.6044(4) 0.9101(3) 0.0472(13) Uani 1 1 d . . . C8 C 0.6008(4) 0.4653(4) 0.7187(4) 0.0580(16) Uani 1 1 d . . . H8A H 0.6576 0.4903 0.7001 0.087 Uiso 1 1 calc R . . H8B H 0.5439 0.4896 0.6846 0.087 Uiso 1 1 calc R . . H8C H 0.6012 0.3977 0.7148 0.087 Uiso 1 1 calc R . . C9 C 0.5303(4) 0.6978(4) 0.9330(4) 0.0580(16) Uani 1 1 d . . . H9A H 0.5403 0.7040 0.9921 0.087 Uiso 1 1 calc R . . H9B H 0.4622 0.7029 0.9120 0.087 Uiso 1 1 calc R . . H9C H 0.5649 0.7468 0.9095 0.087 Uiso 1 1 calc R . . C10 C 0.5598(4) 0.7963(3) 0.5956(3) 0.0401(12) Uani 1 1 d . . . C11 C 0.5976(4) 0.8837(4) 0.6208(4) 0.0485(14) Uani 1 1 d . . . C12 C 0.6202(4) 0.9442(4) 0.5607(4) 0.0615(17) Uani 1 1 d . . . H12 H 0.6451 1.0035 0.5765 0.074 Uiso 1 1 calc R . . C13 C 0.6075(5) 0.9205(5) 0.4802(4) 0.0666(18) Uani 1 1 d . . . H13 H 0.6224 0.9633 0.4409 0.080 Uiso 1 1 calc R . . C14 C 0.5726(4) 0.8328(5) 0.4565(4) 0.0613(17) Uani 1 1 d . . . H14 H 0.5645 0.8160 0.4008 0.074 Uiso 1 1 calc R . . C15 C 0.5492(4) 0.7687(4) 0.5144(3) 0.0459(13) Uani 1 1 d . . . C16 C 0.6148(5) 0.9146(4) 0.7088(4) 0.0625(17) Uani 1 1 d . . . H16A H 0.6217 0.9819 0.7113 0.094 Uiso 1 1 calc R . . H16B H 0.6730 0.8856 0.7369 0.094 Uiso 1 1 calc R . . H16C H 0.5608 0.8961 0.7351 0.094 Uiso 1 1 calc R . . C17 C 0.5126(4) 0.6740(4) 0.4872(3) 0.0587(16) Uani 1 1 d . . . H17A H 0.5494 0.6267 0.5205 0.088 Uiso 1 1 calc R . . H17B H 0.5194 0.6648 0.4302 0.088 Uiso 1 1 calc R . . H17C H 0.4455 0.6689 0.4932 0.088 Uiso 1 1 calc R . . C18 C 0.6867(4) 0.6851(3) 0.7251(3) 0.0401(12) Uani 1 1 d . . . C19 C 0.7412(4) 0.6968(3) 0.8016(3) 0.0428(12) Uani 1 1 d . . . H19 H 0.7102 0.7078 0.8470 0.051 Uiso 1 1 calc R . . C20 C 0.8397(4) 0.6925(4) 0.8124(4) 0.0520(14) Uani 1 1 d . . . H20 H 0.8757 0.7011 0.8647 0.062 Uiso 1 1 calc R . . C21 C 0.8855(4) 0.6752(4) 0.7452(4) 0.0552(15) Uani 1 1 d . . . H21 H 0.9529 0.6714 0.7526 0.066 Uiso 1 1 calc R . . C22 C 0.8344(4) 0.6636(4) 0.6688(4) 0.0522(14) Uani 1 1 d . . . H22 H 0.8658 0.6520 0.6237 0.063 Uiso 1 1 calc R . . C23 C 0.7344(4) 0.6693(4) 0.6590(3) 0.0459(13) Uani 1 1 d . . . H23 H 0.6985 0.6623 0.6064 0.055 Uiso 1 1 calc R . . C24 C 0.2809(5) 0.6467(5) 0.8049(4) 0.0554(15) Uani 1 1 d D . . H24A H 0.247(4) 0.603(4) 0.766(3) 0.083 Uiso 1 1 d D . . H24B H 0.340(3) 0.613(4) 0.824(4) 0.083 Uiso 1 1 d D . . H24C H 0.247(4) 0.631(4) 0.850(3) 0.083 Uiso 1 1 d D . . C25 C 0.3716(5) 0.8548(4) 0.7661(4) 0.0577(16) Uani 1 1 d D . . H25A H 0.378(5) 0.883(4) 0.713(2) 0.087 Uiso 1 1 d D . . H25B H 0.433(2) 0.837(5) 0.796(4) 0.087 Uiso 1 1 d D . . H25C H 0.363(5) 0.912(2) 0.794(3) 0.087 Uiso 1 1 d D . . C26 C 0.1393(5) 0.8231(5) 0.7564(4) 0.0688(18) Uani 1 1 d . . . H26A H 0.0923 0.8281 0.7933 0.103 Uiso 1 1 calc R . . H26B H 0.1190 0.7756 0.7155 0.103 Uiso 1 1 calc R . . H26C H 0.1446 0.8827 0.7295 0.103 Uiso 1 1 calc R . . C27 C 0.2911(5) 0.8165(4) 0.9364(4) 0.0645(17) Uani 1 1 d . . . H27A H 0.2314 0.8307 0.9561 0.097 Uiso 1 1 calc R . . H27B H 0.3340 0.8696 0.9456 0.097 Uiso 1 1 calc R . . H27C H 0.3210 0.7627 0.9655 0.097 Uiso 1 1 calc R . . C28 C 0.3447(5) 0.5458(4) 0.6243(4) 0.0530(15) Uani 1 1 d D . . H28A H 0.356(4) 0.545(4) 0.6835(8) 0.080 Uiso 1 1 d D . . H28B H 0.403(3) 0.553(4) 0.601(4) 0.080 Uiso 1 1 d D . . H28C H 0.320(4) 0.489(3) 0.596(3) 0.080 Uiso 1 1 d D . . C29 C 0.2728(5) 0.7608(4) 0.5709(4) 0.0512(14) Uani 1 1 d D . . H29A H 0.334(2) 0.785(4) 0.561(4) 0.077 Uiso 1 1 d D . . H29B H 0.247(4) 0.805(3) 0.606(3) 0.077 Uiso 1 1 d D . . H29C H 0.229(4) 0.788(4) 0.526(3) 0.077 Uiso 1 1 d D . . C30 C 0.2378(5) 0.5853(5) 0.4411(4) 0.0751(19) Uani 1 1 d . . . H30A H 0.2324 0.5180 0.4358 0.113 Uiso 1 1 calc R . . H30B H 0.2982 0.6056 0.4257 0.113 Uiso 1 1 calc R . . H30C H 0.1850 0.6146 0.4055 0.113 Uiso 1 1 calc R . . C31 C 0.1114(4) 0.6002(4) 0.5963(4) 0.0628(16) Uani 1 1 d . . . H31A H 0.0694 0.6533 0.5826 0.094 Uiso 1 1 calc R . . H31B H 0.1236 0.5923 0.6554 0.094 Uiso 1 1 calc R . . H31C H 0.0810 0.5444 0.5711 0.094 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 Y1 0.0363(3) 0.0402(3) 0.0412(3) -0.0031(2) 0.0040(2) 0.0016(2) Al1 0.0480(11) 0.0551(10) 0.0522(10) -0.0089(8) 0.0126(9) 0.0050(8) Al2 0.0462(11) 0.0490(9) 0.0460(10) -0.0038(8) -0.0003(8) -0.0015(8) N1 0.038(3) 0.043(2) 0.037(2) 0.003(2) 0.003(2) 0.0014(19) N2 0.040(3) 0.043(2) 0.039(2) 0.001(2) 0.005(2) -0.002(2) C1 0.037(3) 0.040(3) 0.041(3) -0.009(2) -0.001(2) -0.002(2) C2 0.033(3) 0.045(3) 0.044(3) 0.008(2) 0.004(2) -0.002(2) C3 0.042(3) 0.043(3) 0.054(3) -0.006(3) 0.008(3) 0.000(2) C4 0.046(4) 0.050(3) 0.076(5) 0.015(3) 0.007(3) 0.005(3) C5 0.056(4) 0.065(4) 0.073(5) 0.033(4) 0.000(3) 0.009(3) C6 0.046(4) 0.083(4) 0.046(3) 0.011(3) 0.001(3) -0.004(3) C7 0.033(3) 0.062(3) 0.047(3) 0.002(3) 0.005(3) -0.003(3) C8 0.049(4) 0.051(3) 0.072(4) -0.007(3) 0.006(3) 0.011(3) C9 0.048(4) 0.079(4) 0.046(3) -0.016(3) 0.002(3) 0.004(3) C10 0.036(3) 0.044(3) 0.040(3) 0.003(2) 0.004(2) 0.011(2) C11 0.045(3) 0.045(3) 0.057(4) 0.004(3) 0.012(3) 0.001(3) C12 0.046(4) 0.058(4) 0.080(5) 0.010(4) 0.009(3) -0.002(3) C13 0.055(4) 0.071(4) 0.074(5) 0.028(4) 0.013(3) 0.001(3) C14 0.046(4) 0.093(5) 0.044(3) 0.015(3) 0.005(3) 0.011(3) C15 0.029(3) 0.062(3) 0.045(3) 0.008(3) 0.001(2) 0.002(3) C16 0.075(5) 0.050(3) 0.062(4) -0.009(3) 0.008(3) -0.006(3) C17 0.048(4) 0.091(5) 0.037(3) -0.012(3) 0.007(3) -0.006(3) C18 0.035(3) 0.038(3) 0.048(3) -0.005(2) 0.008(2) -0.001(2) C19 0.039(3) 0.044(3) 0.044(3) -0.004(3) 0.002(2) -0.007(2) C20 0.043(4) 0.057(3) 0.052(3) 0.002(3) -0.005(3) -0.007(3) C21 0.031(3) 0.058(3) 0.075(4) 0.005(3) 0.002(3) 0.000(3) C22 0.040(3) 0.057(3) 0.060(4) 0.001(3) 0.009(3) 0.001(3) C23 0.042(3) 0.052(3) 0.044(3) 0.000(3) 0.006(3) 0.001(3) C24 0.046(4) 0.068(4) 0.055(4) -0.008(3) 0.016(3) -0.003(3) C25 0.066(4) 0.047(3) 0.061(4) -0.008(3) 0.013(3) -0.001(3) C26 0.055(4) 0.084(5) 0.066(4) -0.014(4) 0.007(3) 0.015(3) C27 0.056(4) 0.074(4) 0.064(4) -0.013(3) 0.011(3) 0.009(3) C28 0.052(4) 0.044(3) 0.061(4) -0.016(3) 0.003(3) 0.002(3) C29 0.057(4) 0.042(3) 0.054(4) 0.002(3) 0.007(3) 0.002(3) C30 0.089(5) 0.075(4) 0.057(4) -0.010(3) 0.000(4) -0.009(4) C31 0.048(4) 0.066(4) 0.073(4) 0.005(3) 0.001(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N1 2.305(4) . ? Y1 N2 2.309(4) . ? Y1 C28 2.509(6) . ? Y1 C25 2.531(6) . ? Y1 C24 2.553(6) . ? Y1 C29 2.554(6) . ? Y1 C1 2.775(5) . ? Y1 Al1 3.0813(18) . ? Y1 Al2 3.0841(18) . ? Y1 H24B 2.58(6) . ? Y1 H28A 2.23(6) . ? Y1 H29A 2.56(6) . ? Al1 C26 1.960(7) . ? Al1 C27 1.962(6) . ? Al1 C24 2.066(7) . ? Al1 C25 2.084(7) . ? Al2 C31 1.965(6) . ? Al2 C30 1.975(6) . ? Al2 C29 2.075(6) . ? Al2 C28 2.089(7) . ? N1 C1 1.344(6) . ? N1 C2 1.442(6) . ? N2 C1 1.356(7) . ? N2 C10 1.440(6) . ? C1 C18 1.481(7) . ? C2 C3 1.405(7) . ? C2 C7 1.409(7) . ? C3 C4 1.393(8) . ? C3 C8 1.501(8) . ? C4 C5 1.370(9) . ? C4 H4 0.9400 . ? C5 C6 1.364(8) . ? C5 H5 0.9400 . ? C6 C7 1.377(8) . ? C6 H6 0.9400 . ? C7 C9 1.501(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C15 1.384(7) . ? C10 C11 1.398(7) . ? C11 C12 1.391(8) . ? C11 C16 1.504(8) . ? C12 C13 1.358(9) . ? C12 H12 0.9400 . ? C13 C14 1.383(9) . ? C13 H13 0.9400 . ? C14 C15 1.403(8) . ? C14 H14 0.9400 . ? C15 C17 1.496(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C19 1.383(7) . ? C18 C23 1.386(7) . ? C19 C20 1.373(8) . ? C19 H19 0.9400 . ? C20 C21 1.391(8) . ? C20 H20 0.9400 . ? C21 C22 1.363(8) . ? C21 H21 0.9400 . ? C22 C23 1.396(8) . ? C22 H22 0.9400 . ? C23 H23 0.9400 . ? C24 H24A 0.970(10) . ? C24 H24B 0.969(10) . ? C24 H24C 0.970(10) . ? C25 H25A 0.978(10) . ? C25 H25B 0.970(10) . ? C25 H25C 0.967(10) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.967(10) . ? C28 H28B 0.968(10) . ? C28 H28C 0.971(10) . ? C29 H29A 0.970(10) . ? C29 H29B 0.973(10) . ? C29 H29C 0.968(10) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? 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 N1 Y1 N2 57.98(15) . . ? N1 Y1 C28 93.80(18) . . ? N2 Y1 C28 99.51(18) . . ? N1 Y1 C25 99.55(19) . . ? N2 Y1 C25 93.53(18) . . ? C28 Y1 C25 164.9(2) . . ? N1 Y1 C24 96.81(19) . . ? N2 Y1 C24 153.56(19) . . ? C28 Y1 C24 89.2(2) . . ? C25 Y1 C24 82.3(2) . . ? N1 Y1 C29 152.72(18) . . ? N2 Y1 C29 95.98(18) . . ? C28 Y1 C29 81.9(2) . . ? C25 Y1 C29 89.3(2) . . ? C24 Y1 C29 110.0(2) . . ? N1 Y1 C1 28.84(14) . . ? N2 Y1 C1 29.14(15) . . ? C28 Y1 C1 97.88(17) . . ? C25 Y1 C1 97.19(18) . . ? C24 Y1 C1 125.22(19) . . ? C29 Y1 C1 124.78(18) . . ? N1 Y1 Al1 109.95(11) . . ? N2 Y1 Al1 134.41(11) . . ? C28 Y1 Al1 125.94(15) . . ? C25 Y1 Al1 42.20(15) . . ? C24 Y1 Al1 41.71(15) . . ? C29 Y1 Al1 93.95(14) . . ? C1 Y1 Al1 126.18(11) . . ? N1 Y1 Al2 135.10(11) . . ? N2 Y1 Al2 110.99(11) . . ? C28 Y1 Al2 42.31(15) . . ? C25 Y1 Al2 125.27(16) . . ? C24 Y1 Al2 92.30(15) . . ? C29 Y1 Al2 41.89(14) . . ? C1 Y1 Al2 127.90(11) . . ? Al1 Y1 Al2 105.92(5) . . ? N1 Y1 H24B 75.7(5) . . ? N2 Y1 H24B 133.6(6) . . ? C28 Y1 H24B 85.5(14) . . ? C25 Y1 H24B 91.0(13) . . ? C24 Y1 H24B 21.8(4) . . ? C29 Y1 H24B 130.3(7) . . ? C1 Y1 H24B 104.5(6) . . ? Al1 Y1 H24B 56.9(10) . . ? Al2 Y1 H24B 103.5(13) . . ? N1 Y1 H28A 82.1(14) . . ? N2 Y1 H28A 108.9(15) . . ? C28 Y1 H28A 22.6(3) . . ? C25 Y1 H28A 153.9(10) . . ? C24 Y1 H28A 71.7(11) . . ? C29 Y1 H28A 101.2(9) . . ? C1 Y1 H28A 96.3(16) . . ? Al1 Y1 H28A 112.5(12) . . ? Al2 Y1 H28A 59.4(10) . . ? H24B Y1 H28A 63.9(15) . . ? N1 Y1 H29A 132.3(5) . . ? N2 Y1 H29A 74.5(5) . . ? C28 Y1 H29A 89.8(13) . . ? C25 Y1 H29A 86.4(13) . . ? C24 Y1 H29A 130.8(6) . . ? C29 Y1 H29A 21.9(4) . . ? C1 Y1 H29A 103.6(5) . . ? Al1 Y1 H29A 105.8(11) . . ? Al2 Y1 H29A 57.0(9) . . ? H24B Y1 H29A 151.9(7) . . ? H28A Y1 H29A 111.9(13) . . ? C26 Al1 C27 119.2(3) . . ? C26 Al1 C24 107.3(3) . . ? C27 Al1 C24 107.5(3) . . ? C26 Al1 C25 108.5(3) . . ? C27 Al1 C25 106.4(3) . . ? C24 Al1 C25 107.4(2) . . ? C26 Al1 Y1 107.1(2) . . ? C27 Al1 Y1 133.7(2) . . ? C24 Al1 Y1 55.32(17) . . ? C25 Al1 Y1 54.63(17) . . ? C31 Al2 C30 116.5(3) . . ? C31 Al2 C29 109.9(3) . . ? C30 Al2 C29 108.6(3) . . ? C31 Al2 C28 111.0(3) . . ? C30 Al2 C28 104.5(3) . . ? C29 Al2 C28 105.7(3) . . ? C31 Al2 Y1 108.9(2) . . ? C30 Al2 Y1 134.6(2) . . ? C29 Al2 Y1 55.25(18) . . ? C28 Al2 Y1 53.96(16) . . ? C1 N1 C2 122.6(4) . . ? C1 N1 Y1 95.4(3) . . ? C2 N1 Y1 140.7(3) . . ? C1 N2 C10 124.9(4) . . ? C1 N2 Y1 94.8(3) . . ? C10 N2 Y1 138.8(3) . . ? N1 C1 N2 111.8(4) . . ? N1 C1 C18 124.0(5) . . ? N2 C1 C18 124.2(5) . . ? N1 C1 Y1 55.8(3) . . ? N2 C1 Y1 56.0(3) . . ? C18 C1 Y1 178.6(4) . . ? C3 C2 C7 120.4(5) . . ? C3 C2 N1 121.3(4) . . ? C7 C2 N1 118.1(4) . . ? C4 C3 C2 118.1(5) . . ? C4 C3 C8 119.6(5) . . ? C2 C3 C8 122.3(5) . . ? C5 C4 C3 121.1(6) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C6 C5 C4 120.4(6) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 121.5(6) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C6 C7 C2 118.6(5) . . ? C6 C7 C9 120.9(5) . . ? C2 C7 C9 120.5(5) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 121.6(5) . . ? C15 C10 N2 117.2(5) . . ? C11 C10 N2 121.1(5) . . ? C12 C11 C10 117.7(5) . . ? C12 C11 C16 119.1(5) . . ? C10 C11 C16 123.3(5) . . ? C13 C12 C11 122.2(6) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C14 119.4(6) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C13 C14 C15 120.8(6) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C10 C15 C14 118.2(5) . . ? C10 C15 C17 122.1(5) . . ? C14 C15 C17 119.7(5) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 118.1(5) . . ? C19 C18 C1 120.8(5) . . ? C23 C18 C1 121.1(5) . . ? C20 C19 C18 121.4(5) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 119.2(5) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C22 C21 C20 121.2(6) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 118.6(6) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C18 C23 C22 121.5(5) . . ? C18 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? Al1 C24 Y1 83.0(2) . . ? Al1 C24 H24A 131(4) . . ? Y1 C24 H24A 90(4) . . ? Al1 C24 H24B 124(4) . . ? Y1 C24 H24B 80(4) . . ? H24A C24 H24B 102(5) . . ? Al1 C24 H24C 94(4) . . ? Y1 C24 H24C 174(4) . . ? H24A C24 H24C 96(5) . . ? H24B C24 H24C 98(5) . . ? Al1 C25 Y1 83.2(2) . . ? Al1 C25 H25A 137(4) . . ? Y1 C25 H25A 87(4) . . ? Al1 C25 H25B 109(4) . . ? Y1 C25 H25B 84(4) . . ? H25A C25 H25B 111(6) . . ? Al1 C25 H25C 92(4) . . ? Y1 C25 H25C 175(4) . . ? H25A C25 H25C 97(5) . . ? H25B C25 H25C 98(5) . . ? Al1 C26 H26A 109.5 . . ? Al1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Al1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Al1 C27 H27A 109.5 . . ? Al1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Al1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Al2 C28 Y1 83.73(19) . . ? Al2 C28 H28A 123(4) . . ? Y1 C28 H28A 62(4) . . ? Al2 C28 H28B 110(4) . . ? Y1 C28 H28B 88(4) . . ? H28A C28 H28B 113(5) . . ? Al2 C28 H28C 89(4) . . ? Y1 C28 H28C 171(4) . . ? H28A C28 H28C 117(5) . . ? H28B C28 H28C 100(5) . . ? Al2 C29 Y1 82.9(2) . . ? Al2 C29 H29A 124(4) . . ? Y1 C29 H29A 80(4) . . ? Al2 C29 H29B 126(4) . . ? Y1 C29 H29B 88(4) . . ? H29A C29 H29B 107(5) . . ? Al2 C29 H29C 99(4) . . ? Y1 C29 H29C 176(4) . . ? H29A C29 H29C 102(5) . . ? H29B C29 H29C 87(5) . . ? Al2 C30 H30A 109.5 . . ? Al2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Al2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Al2 C31 H31A 109.5 . . ? Al2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Al2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Y1 Al1 C26 -177.0(2) . . . . ? N2 Y1 Al1 C26 118.8(3) . . . . ? C28 Y1 Al1 C26 -66.5(3) . . . . ? C25 Y1 Al1 C26 101.0(3) . . . . ? C24 Y1 Al1 C26 -99.5(3) . . . . ? C29 Y1 Al1 C26 16.4(3) . . . . ? C1 Y1 Al1 C26 155.8(3) . . . . ? Al2 Y1 Al1 C26 -24.4(2) . . . . ? N1 Y1 Al1 C27 3.6(3) . . . . ? N2 Y1 Al1 C27 -60.6(3) . . . . ? C28 Y1 Al1 C27 114.1(3) . . . . ? C25 Y1 Al1 C27 -78.4(4) . . . . ? C24 Y1 Al1 C27 81.1(4) . . . . ? C29 Y1 Al1 C27 -163.0(3) . . . . ? C1 Y1 Al1 C27 -23.6(3) . . . . ? Al2 Y1 Al1 C27 156.2(3) . . . . ? N1 Y1 Al1 C24 -77.4(3) . . . . ? N2 Y1 Al1 C24 -141.7(3) . . . . ? C28 Y1 Al1 C24 33.1(3) . . . . ? C25 Y1 Al1 C24 -159.5(3) . . . . ? C29 Y1 Al1 C24 116.0(3) . . . . ? C1 Y1 Al1 C24 -104.7(3) . . . . ? Al2 Y1 Al1 C24 75.1(2) . . . . ? N1 Y1 Al1 C25 82.1(3) . . . . ? N2 Y1 Al1 C25 17.8(3) . . . . ? C28 Y1 Al1 C25 -167.4(3) . . . . ? C24 Y1 Al1 C25 159.5(3) . . . . ? C29 Y1 Al1 C25 -84.5(3) . . . . ? C1 Y1 Al1 C25 54.8(3) . . . . ? Al2 Y1 Al1 C25 -125.4(2) . . . . ? N1 Y1 Al2 C31 118.3(2) . . . . ? N2 Y1 Al2 C31 -176.5(2) . . . . ? C28 Y1 Al2 C31 102.7(3) . . . . ? C25 Y1 Al2 C31 -65.9(3) . . . . ? C24 Y1 Al2 C31 16.3(2) . . . . ? C29 Y1 Al2 C31 -101.6(3) . . . . ? C1 Y1 Al2 C31 156.0(2) . . . . ? Al1 Y1 Al2 C31 -23.7(2) . . . . ? N1 Y1 Al2 C30 -58.0(3) . . . . ? N2 Y1 Al2 C30 7.2(3) . . . . ? C28 Y1 Al2 C30 -73.6(4) . . . . ? C25 Y1 Al2 C30 117.8(3) . . . . ? C24 Y1 Al2 C30 -160.0(3) . . . . ? C29 Y1 Al2 C30 82.1(4) . . . . ? C1 Y1 Al2 C30 -20.3(3) . . . . ? Al1 Y1 Al2 C30 160.0(3) . . . . ? N1 Y1 Al2 C29 -140.1(3) . . . . ? N2 Y1 Al2 C29 -74.9(2) . . . . ? C28 Y1 Al2 C29 -155.8(3) . . . . ? C25 Y1 Al2 C29 35.7(3) . . . . ? C24 Y1 Al2 C29 117.9(3) . . . . ? C1 Y1 Al2 C29 -102.4(3) . . . . ? Al1 Y1 Al2 C29 77.8(2) . . . . ? N1 Y1 Al2 C28 15.7(3) . . . . ? N2 Y1 Al2 C28 80.9(3) . . . . ? C25 Y1 Al2 C28 -168.5(3) . . . . ? C24 Y1 Al2 C28 -86.3(3) . . . . ? C29 Y1 Al2 C28 155.8(3) . . . . ? C1 Y1 Al2 C28 53.4(3) . . . . ? Al1 Y1 Al2 C28 -126.4(2) . . . . ? N2 Y1 N1 C1 0.6(3) . . . . ? C28 Y1 N1 C1 99.5(3) . . . . ? C25 Y1 N1 C1 -87.6(3) . . . . ? C24 Y1 N1 C1 -170.8(3) . . . . ? C29 Y1 N1 C1 19.8(5) . . . . ? Al1 Y1 N1 C1 -130.0(3) . . . . ? Al2 Y1 N1 C1 89.0(3) . . . . ? N2 Y1 N1 C2 -165.0(5) . . . . ? C28 Y1 N1 C2 -66.2(5) . . . . ? C25 Y1 N1 C2 106.8(5) . . . . ? C24 Y1 N1 C2 23.5(5) . . . . ? C29 Y1 N1 C2 -145.9(5) . . . . ? C1 Y1 N1 C2 -165.6(7) . . . . ? Al1 Y1 N1 C2 64.4(5) . . . . ? Al2 Y1 N1 C2 -76.7(5) . . . . ? N1 Y1 N2 C1 -0.6(3) . . . . ? C28 Y1 N2 C1 -89.2(3) . . . . ? C25 Y1 N2 C1 98.4(3) . . . . ? C24 Y1 N2 C1 18.7(5) . . . . ? C29 Y1 N2 C1 -171.9(3) . . . . ? Al1 Y1 N2 C1 86.6(3) . . . . ? Al2 Y1 N2 C1 -131.5(3) . . . . ? N1 Y1 N2 C10 -166.2(5) . . . . ? C28 Y1 N2 C10 105.3(5) . . . . ? C25 Y1 N2 C10 -67.1(5) . . . . ? C24 Y1 N2 C10 -146.9(5) . . . . ? C29 Y1 N2 C10 22.5(5) . . . . ? C1 Y1 N2 C10 -165.6(7) . . . . ? Al1 Y1 N2 C10 -79.0(5) . . . . ? Al2 Y1 N2 C10 62.9(5) . . . . ? C2 N1 C1 N2 168.3(4) . . . . ? Y1 N1 C1 N2 -1.0(4) . . . . ? C2 N1 C1 C18 -12.4(7) . . . . ? Y1 N1 C1 C18 178.4(4) . . . . ? C2 N1 C1 Y1 169.2(5) . . . . ? C10 N2 C1 N1 169.4(4) . . . . ? Y1 N2 C1 N1 1.0(4) . . . . ? C10 N2 C1 C18 -9.9(7) . . . . ? Y1 N2 C1 C18 -178.4(4) . . . . ? C10 N2 C1 Y1 168.4(5) . . . . ? N2 Y1 C1 N1 -178.9(5) . . . . ? C28 Y1 C1 N1 -83.5(3) . . . . ? C25 Y1 C1 N1 96.8(3) . . . . ? C24 Y1 C1 N1 11.2(4) . . . . ? C29 Y1 C1 N1 -169.1(3) . . . . ? Al1 Y1 C1 N1 63.1(3) . . . . ? Al2 Y1 C1 N1 -116.6(3) . . . . ? N1 Y1 C1 N2 178.9(5) . . . . ? C28 Y1 C1 N2 95.4(3) . . . . ? C25 Y1 C1 N2 -84.3(3) . . . . ? C24 Y1 C1 N2 -169.9(3) . . . . ? C29 Y1 C1 N2 9.8(4) . . . . ? Al1 Y1 C1 N2 -117.9(3) . . . . ? Al2 Y1 C1 N2 62.3(3) . . . . ? N1 Y1 C1 C18 -81(17) . . . . ? N2 Y1 C1 C18 101(17) . . . . ? C28 Y1 C1 C18 -164(17) . . . . ? C25 Y1 C1 C18 16(17) . . . . ? C24 Y1 C1 C18 -69(17) . . . . ? C29 Y1 C1 C18 110(17) . . . . ? Al1 Y1 C1 C18 -17(17) . . . . ? Al2 Y1 C1 C18 163(17) . . . . ? C1 N1 C2 C3 -66.9(7) . . . . ? Y1 N1 C2 C3 96.1(6) . . . . ? C1 N1 C2 C7 117.9(5) . . . . ? Y1 N1 C2 C7 -79.2(6) . . . . ? C7 C2 C3 C4 -1.5(8) . . . . ? N1 C2 C3 C4 -176.6(5) . . . . ? C7 C2 C3 C8 178.7(5) . . . . ? N1 C2 C3 C8 3.6(8) . . . . ? C2 C3 C4 C5 -0.3(8) . . . . ? C8 C3 C4 C5 179.5(6) . . . . ? C3 C4 C5 C6 1.4(9) . . . . ? C4 C5 C6 C7 -0.8(10) . . . . ? C5 C6 C7 C2 -0.9(9) . . . . ? C5 C6 C7 C9 -179.9(6) . . . . ? C3 C2 C7 C6 2.1(8) . . . . ? N1 C2 C7 C6 177.4(5) . . . . ? C3 C2 C7 C9 -179.0(5) . . . . ? N1 C2 C7 C9 -3.7(7) . . . . ? C1 N2 C10 C15 113.9(6) . . . . ? Y1 N2 C10 C15 -83.7(6) . . . . ? C1 N2 C10 C11 -69.8(6) . . . . ? Y1 N2 C10 C11 92.6(6) . . . . ? C15 C10 C11 C12 3.1(8) . . . . ? N2 C10 C11 C12 -173.0(5) . . . . ? C15 C10 C11 C16 -176.9(5) . . . . ? N2 C10 C11 C16 7.0(8) . . . . ? C10 C11 C12 C13 -0.7(9) . . . . ? C16 C11 C12 C13 179.3(6) . . . . ? C11 C12 C13 C14 -1.2(9) . . . . ? C12 C13 C14 C15 0.7(9) . . . . ? C11 C10 C15 C14 -3.5(8) . . . . ? N2 C10 C15 C14 172.8(5) . . . . ? C11 C10 C15 C17 177.4(5) . . . . ? N2 C10 C15 C17 -6.3(7) . . . . ? C13 C14 C15 C10 1.5(8) . . . . ? C13 C14 C15 C17 -179.3(5) . . . . ? N1 C1 C18 C19 -42.3(7) . . . . ? N2 C1 C18 C19 137.0(5) . . . . ? Y1 C1 C18 C19 37(18) . . . . ? N1 C1 C18 C23 137.0(5) . . . . ? N2 C1 C18 C23 -43.7(7) . . . . ? Y1 C1 C18 C23 -143(17) . . . . ? C23 C18 C19 C20 -0.3(8) . . . . ? C1 C18 C19 C20 179.1(5) . . . . ? C18 C19 C20 C21 -0.6(8) . . . . ? C19 C20 C21 C22 0.8(8) . . . . ? C20 C21 C22 C23 -0.1(9) . . . . ? C19 C18 C23 C22 1.0(8) . . . . ? C1 C18 C23 C22 -178.3(5) . . . . ? C21 C22 C23 C18 -0.9(8) . . . . ? C26 Al1 C24 Y1 99.1(3) . . . . ? C27 Al1 C24 Y1 -131.5(2) . . . . ? C25 Al1 C24 Y1 -17.4(3) . . . . ? N1 Y1 C24 Al1 112.5(2) . . . . ? N2 Y1 C24 Al1 96.1(4) . . . . ? C28 Y1 C24 Al1 -153.8(2) . . . . ? C25 Y1 C24 Al1 13.7(2) . . . . ? C29 Y1 C24 Al1 -72.7(2) . . . . ? C1 Y1 C24 Al1 107.1(2) . . . . ? Al2 Y1 C24 Al1 -111.56(18) . . . . ? C26 Al1 C25 Y1 -98.1(2) . . . . ? C27 Al1 C25 Y1 132.4(2) . . . . ? C24 Al1 C25 Y1 17.6(3) . . . . ? N1 Y1 C25 Al1 -109.2(2) . . . . ? N2 Y1 C25 Al1 -167.4(2) . . . . ? C28 Y1 C25 Al1 42.7(9) . . . . ? C24 Y1 C25 Al1 -13.6(2) . . . . ? C29 Y1 C25 Al1 96.7(2) . . . . ? C1 Y1 C25 Al1 -138.3(2) . . . . ? Al2 Y1 C25 Al1 73.8(2) . . . . ? C31 Al2 C28 Y1 -98.6(3) . . . . ? C30 Al2 C28 Y1 135.1(2) . . . . ? C29 Al2 C28 Y1 20.5(3) . . . . ? N1 Y1 C28 Al2 -168.98(19) . . . . ? N2 Y1 C28 Al2 -110.8(2) . . . . ? C25 Y1 C28 Al2 38.7(9) . . . . ? C24 Y1 C28 Al2 94.2(2) . . . . ? C29 Y1 C28 Al2 -16.1(2) . . . . ? C1 Y1 C28 Al2 -140.27(19) . . . . ? Al1 Y1 C28 Al2 73.0(2) . . . . ? C31 Al2 C29 Y1 99.6(2) . . . . ? C30 Al2 C29 Y1 -131.9(3) . . . . ? C28 Al2 C29 Y1 -20.2(3) . . . . ? N1 Y1 C29 Al2 98.8(4) . . . . ? N2 Y1 C29 Al2 115.00(19) . . . . ? C28 Y1 C29 Al2 16.2(2) . . . . ? C25 Y1 C29 Al2 -151.5(2) . . . . ? C24 Y1 C29 Al2 -70.0(2) . . . . ? C1 Y1 C29 Al2 110.2(2) . . . . ? Al1 Y1 C29 Al2 -109.56(16) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.796 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.077