# 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_complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H108 N8 Si8 Y2' _chemical_formula_sum 'C56 H108 N8 Si8 Y2' _chemical_formula_weight 1296.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1103(18) _cell_length_b 11.4141(19) _cell_length_c 15.307(2) _cell_angle_alpha 92.761(4) _cell_angle_beta 92.247(3) _cell_angle_gamma 108.104(4) _cell_volume 1839.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6705 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description chip _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 690 _exptl_absorpt_coefficient_mu 1.736 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.432 _exptl_absorpt_correction_T_max 0.716 _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 14910 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6792 _reflns_number_gt 4974 _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^)+(0.0631P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6792 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1144 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.20166(3) 0.36396(3) 0.72251(2) 0.03145(13) Uani 1 1 d . . . Si1 Si 0.35475(11) 0.63232(10) 0.85755(8) 0.0470(3) Uani 1 1 d . . . Si2 Si 0.42386(10) 0.60568(9) 0.67053(8) 0.0408(3) Uani 1 1 d . . . Si3 Si 0.45151(10) 0.22792(10) 0.73245(7) 0.0399(3) Uani 1 1 d . . . Si4 Si 0.21513(10) 0.11457(9) 0.61665(7) 0.0384(3) Uani 1 1 d . . . N1 N 0.0452(3) 0.2626(3) 0.81151(19) 0.0350(7) Uani 1 1 d . . . N2 N 0.0312(3) 0.4344(3) 0.6738(2) 0.0382(7) Uani 1 1 d . . . N3 N 0.3405(3) 0.5487(3) 0.7593(2) 0.0378(7) Uani 1 1 d . . . N4 N 0.3041(3) 0.2261(3) 0.69300(19) 0.0338(7) Uani 1 1 d . . . C1 C -0.0721(5) 0.2930(4) 0.9398(3) 0.0623(13) Uani 1 1 d . . . H1A H -0.1532 0.2292 0.9280 0.093 Uiso 1 1 calc R . . H1B H -0.0848 0.3637 0.9712 0.093 Uiso 1 1 calc R . . H1C H -0.0164 0.2611 0.9751 0.093 Uiso 1 1 calc R . . C2 C -0.0132(4) 0.3316(3) 0.8547(3) 0.0411(9) Uani 1 1 d . . . C3 C -0.0265(4) 0.4411(4) 0.8242(3) 0.0480(10) Uani 1 1 d . . . H3 H -0.0403 0.4964 0.8672 0.058 Uiso 1 1 calc R . . C4 C -0.0221(4) 0.4798(4) 0.7371(3) 0.0451(10) Uani 1 1 d . . . C5 C -0.0880(5) 0.5749(4) 0.7200(3) 0.0649(14) Uani 1 1 d . . . H5A H -0.0254 0.6529 0.7096 0.097 Uiso 1 1 calc R . . H5B H -0.1346 0.5856 0.7705 0.097 Uiso 1 1 calc R . . H5C H -0.1464 0.5470 0.6689 0.097 Uiso 1 1 calc R . . C6 C 0.0096(4) 0.1336(3) 0.8294(3) 0.0405(9) Uani 1 1 d . . . C7 C -0.1047(4) 0.0542(4) 0.7920(3) 0.0556(12) Uani 1 1 d . . . C8 C -0.1361(6) -0.0707(5) 0.8075(4) 0.0793(17) Uani 1 1 d . . . H8 H -0.2127 -0.1261 0.7829 0.095 Uiso 1 1 calc R . . C9 C -0.0563(7) -0.1137(5) 0.8585(4) 0.088(2) Uani 1 1 d . . . H9 H -0.0782 -0.1984 0.8676 0.106 Uiso 1 1 calc R . . C10 C 0.0535(6) -0.0352(4) 0.8956(3) 0.0693(14) Uani 1 1 d . . . H10 H 0.1062 -0.0661 0.9309 0.083 Uiso 1 1 calc R . . C11 C 0.0895(4) 0.0894(4) 0.8826(3) 0.0467(10) Uani 1 1 d . . . C12 C -0.1937(4) 0.1014(5) 0.7386(4) 0.0777(16) Uani 1 1 d . . . H12A H -0.2332 0.1472 0.7768 0.117 Uiso 1 1 calc R . . H12B H -0.2586 0.0323 0.7084 0.117 Uiso 1 1 calc R . . H12C H -0.1469 0.1552 0.6959 0.117 Uiso 1 1 calc R . . C13 C 0.2089(4) 0.1745(4) 0.9270(3) 0.0613(12) Uani 1 1 d . . . H13A H 0.2507 0.1274 0.9611 0.092 Uiso 1 1 calc R . . H13B H 0.1889 0.2351 0.9653 0.092 Uiso 1 1 calc R . . H13C H 0.2648 0.2163 0.8832 0.092 Uiso 1 1 calc R . . C14 C 0.0140(3) 0.4684(3) 0.5865(3) 0.0392(9) Uani 1 1 d . . . C15 C -0.0692(3) 0.3859(4) 0.5258(3) 0.0457(10) Uani 1 1 d . . . H15 H -0.1177 0.3080 0.5428 0.055 Uiso 1 1 calc R . . C16 C -0.0820(4) 0.4166(3) 0.4405(3) 0.0426(10) Uani 1 1 d . . . H16 H -0.1378 0.3585 0.4000 0.051 Uiso 1 1 calc R . . C17 C 0.5221(5) 0.7284(5) 0.8898(4) 0.0847(18) Uani 1 1 d . . . H17A H 0.5750 0.6753 0.8941 0.127 Uiso 1 1 calc R . . H17B H 0.5245 0.7724 0.9460 0.127 Uiso 1 1 calc R . . H17C H 0.5533 0.7873 0.8459 0.127 Uiso 1 1 calc R . . C18 C 0.3008(4) 0.5254(4) 0.9467(3) 0.0576(12) Uani 1 1 d . . . H18A H 0.2158 0.4706 0.9312 0.086 Uiso 1 1 calc R . . H18B H 0.3006 0.5730 1.0009 0.086 Uiso 1 1 calc R . . H18C H 0.3580 0.4770 0.9544 0.086 Uiso 1 1 calc R . . C19 C 0.2571(5) 0.7398(4) 0.8578(3) 0.0641(13) Uani 1 1 d . . . H19A H 0.2783 0.7926 0.8092 0.096 Uiso 1 1 calc R . . H19B H 0.2747 0.7904 0.9124 0.096 Uiso 1 1 calc R . . H19C H 0.1678 0.6922 0.8519 0.096 Uiso 1 1 calc R . . C20 C 0.5965(4) 0.6188(4) 0.6797(3) 0.0588(12) Uani 1 1 d . . . H20A H 0.6375 0.6745 0.7297 0.088 Uiso 1 1 calc R . . H20B H 0.6361 0.6508 0.6267 0.088 Uiso 1 1 calc R . . H20C H 0.6053 0.5380 0.6876 0.088 Uiso 1 1 calc R . . C21 C 0.4178(4) 0.7624(4) 0.6423(3) 0.0576(12) Uani 1 1 d . . . H21A H 0.3324 0.7660 0.6479 0.086 Uiso 1 1 calc R . . H21B H 0.4419 0.7767 0.5826 0.086 Uiso 1 1 calc R . . H21C H 0.4761 0.8252 0.6820 0.086 Uiso 1 1 calc R . . C22 C 0.3542(4) 0.4944(4) 0.5728(3) 0.0481(10) Uani 1 1 d . . . H22A H 0.3729 0.4178 0.5803 0.072 Uiso 1 1 calc R . . H22B H 0.3910 0.5303 0.5201 0.072 Uiso 1 1 calc R . . H22C H 0.2631 0.4779 0.5679 0.072 Uiso 1 1 calc R . . C23 C 0.4491(5) 0.0770(4) 0.7765(3) 0.0652(13) Uani 1 1 d . . . H23A H 0.3795 0.0502 0.8147 0.098 Uiso 1 1 calc R . . H23B H 0.5286 0.0870 0.8092 0.098 Uiso 1 1 calc R . . H23C H 0.4380 0.0156 0.7282 0.098 Uiso 1 1 calc R . . C24 C 0.5174(4) 0.3475(4) 0.8249(3) 0.0533(11) Uani 1 1 d . . . H24A H 0.5062 0.4251 0.8095 0.080 Uiso 1 1 calc R . . H24B H 0.6070 0.3587 0.8357 0.080 Uiso 1 1 calc R . . H24C H 0.4730 0.3206 0.8773 0.080 Uiso 1 1 calc R . . C25 C 0.5720(4) 0.2625(4) 0.6469(3) 0.0619(13) Uani 1 1 d . . . H25A H 0.5623 0.1883 0.6100 0.093 Uiso 1 1 calc R . . H25B H 0.6566 0.2910 0.6751 0.093 Uiso 1 1 calc R . . H25C H 0.5594 0.3262 0.6112 0.093 Uiso 1 1 calc R . . C26 C 0.2981(5) 0.0946(5) 0.5155(3) 0.0676(14) Uani 1 1 d . . . H26A H 0.3393 0.1749 0.4936 0.101 Uiso 1 1 calc R . . H26B H 0.2368 0.0440 0.4711 0.101 Uiso 1 1 calc R . . H26C H 0.3613 0.0547 0.5293 0.101 Uiso 1 1 calc R . . C27 C 0.0798(4) 0.1689(4) 0.5782(3) 0.0524(11) Uani 1 1 d . . . H27A H 0.0358 0.1861 0.6283 0.079 Uiso 1 1 calc R . . H27B H 0.0214 0.1051 0.5393 0.079 Uiso 1 1 calc R . . H27C H 0.1124 0.2434 0.5472 0.079 Uiso 1 1 calc R . . C28 C 0.1439(4) -0.0417(3) 0.6578(3) 0.0523(11) Uani 1 1 d . . . H28A H 0.2109 -0.0726 0.6792 0.078 Uiso 1 1 calc R . . H28B H 0.0938 -0.0974 0.6106 0.078 Uiso 1 1 calc R . . H28C H 0.0899 -0.0363 0.7052 0.078 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 0.02972(19) 0.02998(19) 0.0349(2) 0.00459(15) 0.00225(14) 0.00923(14) Si1 0.0463(6) 0.0390(6) 0.0483(7) -0.0077(5) 0.0069(5) 0.0037(5) Si2 0.0366(6) 0.0319(5) 0.0531(7) 0.0035(5) 0.0129(5) 0.0084(4) Si3 0.0347(6) 0.0378(6) 0.0500(7) 0.0062(5) 0.0023(5) 0.0148(4) Si4 0.0402(6) 0.0345(6) 0.0398(6) -0.0002(5) 0.0029(5) 0.0106(4) N1 0.0321(16) 0.0362(16) 0.0375(18) 0.0052(14) 0.0065(13) 0.0108(13) N2 0.0403(17) 0.0377(17) 0.0396(19) 0.0030(15) -0.0001(14) 0.0169(14) N3 0.0356(17) 0.0322(16) 0.0442(19) -0.0019(14) 0.0066(14) 0.0085(13) N4 0.0352(16) 0.0296(15) 0.0379(18) 0.0019(13) 0.0056(13) 0.0119(12) C1 0.080(3) 0.065(3) 0.051(3) 0.009(2) 0.029(2) 0.033(3) C2 0.045(2) 0.039(2) 0.042(2) 0.0013(18) 0.0024(18) 0.0157(17) C3 0.058(3) 0.046(2) 0.046(3) -0.003(2) 0.005(2) 0.025(2) C4 0.042(2) 0.038(2) 0.055(3) 0.003(2) -0.004(2) 0.0129(17) C5 0.082(3) 0.063(3) 0.070(3) 0.007(3) 0.006(3) 0.052(3) C6 0.042(2) 0.0319(19) 0.048(2) 0.0078(18) 0.0196(18) 0.0095(17) C7 0.038(2) 0.057(3) 0.063(3) 0.002(2) 0.020(2) -0.001(2) C8 0.084(4) 0.049(3) 0.079(4) -0.007(3) 0.037(3) -0.017(3) C9 0.142(6) 0.038(3) 0.083(4) 0.017(3) 0.054(4) 0.016(3) C10 0.109(4) 0.050(3) 0.060(3) 0.023(2) 0.033(3) 0.035(3) C11 0.060(3) 0.045(2) 0.043(2) 0.0120(19) 0.023(2) 0.025(2) C12 0.037(3) 0.096(4) 0.082(4) -0.004(3) -0.002(3) -0.002(3) C13 0.059(3) 0.074(3) 0.058(3) 0.024(3) 0.002(2) 0.030(3) C14 0.035(2) 0.043(2) 0.044(2) 0.0116(18) -0.0035(17) 0.0179(17) C15 0.034(2) 0.042(2) 0.057(3) 0.015(2) -0.0082(19) 0.0062(17) C16 0.040(2) 0.041(2) 0.046(3) 0.0032(19) -0.0112(18) 0.0120(17) C17 0.062(3) 0.078(4) 0.084(4) -0.032(3) 0.000(3) -0.017(3) C18 0.066(3) 0.055(3) 0.047(3) -0.007(2) -0.001(2) 0.014(2) C19 0.088(4) 0.046(3) 0.061(3) 0.003(2) 0.030(3) 0.021(2) C20 0.044(2) 0.050(3) 0.080(3) 0.001(2) 0.016(2) 0.010(2) C21 0.057(3) 0.038(2) 0.078(3) 0.014(2) 0.025(2) 0.012(2) C22 0.051(2) 0.050(2) 0.046(3) 0.009(2) 0.016(2) 0.017(2) C23 0.059(3) 0.052(3) 0.090(4) 0.017(3) -0.002(3) 0.023(2) C24 0.044(2) 0.058(3) 0.057(3) 0.006(2) -0.008(2) 0.015(2) C25 0.045(2) 0.069(3) 0.075(3) 0.010(3) 0.014(2) 0.021(2) C26 0.075(3) 0.072(3) 0.051(3) -0.016(2) 0.013(2) 0.017(3) C27 0.052(3) 0.050(2) 0.054(3) -0.010(2) -0.009(2) 0.017(2) C28 0.054(3) 0.037(2) 0.060(3) -0.001(2) -0.001(2) 0.0075(19) _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 2.222(3) . ? Y1 N4 2.249(3) . ? Y1 N1 2.303(3) . ? Y1 N2 2.383(3) . ? Y1 Si2 3.2360(12) . ? Y1 Si4 3.2542(11) . ? Si1 N3 1.716(3) . ? Si1 C18 1.866(5) . ? Si1 C19 1.873(4) . ? Si1 C17 1.874(5) . ? Si2 N3 1.714(3) . ? Si2 C20 1.876(4) . ? Si2 C21 1.881(4) . ? Si2 C22 1.888(4) . ? Si3 N4 1.717(3) . ? Si3 C23 1.873(4) . ? Si3 C24 1.874(4) . ? Si3 C25 1.877(5) . ? Si4 N4 1.717(3) . ? Si4 C28 1.864(4) . ? Si4 C26 1.873(4) . ? Si4 C27 1.880(4) . ? N1 C2 1.333(4) . ? N1 C6 1.444(5) . ? N2 C4 1.321(5) . ? N2 C14 1.432(5) . ? C1 C2 1.504(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C3 1.403(5) . ? C3 C4 1.422(6) . ? C3 H3 0.9400 . ? C4 C5 1.513(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.392(6) . ? C6 C11 1.402(6) . ? C7 C8 1.393(7) . ? C7 C12 1.499(7) . ? C8 C9 1.375(8) . ? C8 H8 0.9400 . ? C9 C10 1.353(8) . ? C9 H9 0.9400 . ? C10 C11 1.378(6) . ? C10 H10 0.9400 . ? C11 C13 1.494(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 C15 1.382(5) . ? C14 C16 1.387(5) 2_566 ? C15 C16 1.382(5) . ? C15 H15 0.9400 . ? C16 C14 1.387(5) 2_566 ? C16 H16 0.9400 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? 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 . ? 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 N4 110.09(11) . . ? N3 Y1 N1 123.31(11) . . ? N4 Y1 N1 103.72(11) . . ? N3 Y1 N2 97.04(11) . . ? N4 Y1 N2 143.93(10) . . ? N1 Y1 N2 78.91(11) . . ? N3 Y1 Si2 29.87(8) . . ? N4 Y1 Si2 96.80(8) . . ? N1 Y1 Si2 152.34(7) . . ? N2 Y1 Si2 95.30(8) . . ? N3 Y1 Si4 134.63(8) . . ? N4 Y1 Si4 29.82(7) . . ? N1 Y1 Si4 95.21(7) . . ? N2 Y1 Si4 114.64(7) . . ? Si2 Y1 Si4 111.57(3) . . ? N3 Si1 C18 109.75(17) . . ? N3 Si1 C19 112.73(19) . . ? C18 Si1 C19 107.4(2) . . ? N3 Si1 C17 113.1(2) . . ? C18 Si1 C17 106.6(2) . . ? C19 Si1 C17 106.8(2) . . ? N3 Si2 C20 114.9(2) . . ? N3 Si2 C21 114.37(18) . . ? C20 Si2 C21 105.8(2) . . ? N3 Si2 C22 107.79(17) . . ? C20 Si2 C22 105.65(19) . . ? C21 Si2 C22 107.8(2) . . ? N3 Si2 Y1 40.21(10) . . ? C20 Si2 Y1 123.05(15) . . ? C21 Si2 Y1 130.64(14) . . ? C22 Si2 Y1 67.72(13) . . ? N4 Si3 C23 112.15(19) . . ? N4 Si3 C24 112.50(16) . . ? C23 Si3 C24 105.9(2) . . ? N4 Si3 C25 112.67(18) . . ? C23 Si3 C25 107.2(2) . . ? C24 Si3 C25 106.0(2) . . ? N4 Si4 C28 115.59(17) . . ? N4 Si4 C26 114.97(19) . . ? C28 Si4 C26 107.4(2) . . ? N4 Si4 C27 105.95(16) . . ? C28 Si4 C27 106.9(2) . . ? C26 Si4 C27 105.3(2) . . ? N4 Si4 Y1 40.63(9) . . ? C28 Si4 Y1 121.98(14) . . ? C26 Si4 Y1 130.50(17) . . ? C27 Si4 Y1 65.70(12) . . ? C2 N1 C6 116.8(3) . . ? C2 N1 Y1 116.6(2) . . ? C6 N1 Y1 126.5(2) . . ? C4 N2 C14 118.0(3) . . ? C4 N2 Y1 114.5(2) . . ? C14 N2 Y1 124.0(2) . . ? Si2 N3 Si1 123.25(18) . . ? Si2 N3 Y1 109.92(14) . . ? Si1 N3 Y1 126.53(17) . . ? Si4 N4 Si3 121.92(16) . . ? Si4 N4 Y1 109.55(14) . . ? Si3 N4 Y1 128.45(15) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.4(4) . . ? N1 C2 C1 120.7(4) . . ? C3 C2 C1 115.8(3) . . ? C2 C3 C4 128.9(3) . . ? C2 C3 H3 115.6 . . ? C4 C3 H3 115.6 . . ? N2 C4 C3 123.5(3) . . ? N2 C4 C5 121.3(4) . . ? C3 C4 C5 115.2(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 120.9(4) . . ? C7 C6 N1 118.6(4) . . ? C11 C6 N1 120.5(3) . . ? C6 C7 C8 118.1(5) . . ? C6 C7 C12 121.4(4) . . ? C8 C7 C12 120.5(5) . . ? C9 C8 C7 120.7(5) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 120.6(5) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 121.3(5) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 118.4(4) . . ? C10 C11 C13 120.1(4) . . ? C6 C11 C13 121.4(4) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 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 C16 118.0(4) . 2_566 ? C15 C14 N2 120.6(4) . . ? C16 C14 N2 121.3(3) 2_566 . ? C16 C15 C14 120.7(4) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C14 121.2(3) . 2_566 ? C15 C16 H16 119.4 . . ? C14 C16 H16 119.4 2_566 . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C24 H24A 109.5 . . ? Si3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si4 C27 H27A 109.5 . . ? Si4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? 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 -119.15(17) . . . . ? N1 Y1 Si2 N3 18.7(2) . . . . ? N2 Y1 Si2 N3 94.90(17) . . . . ? Si4 Y1 Si2 N3 -145.96(16) . . . . ? N3 Y1 Si2 C20 90.5(2) . . . . ? N4 Y1 Si2 C20 -28.65(19) . . . . ? N1 Y1 Si2 C20 109.2(2) . . . . ? N2 Y1 Si2 C20 -174.61(19) . . . . ? Si4 Y1 Si2 C20 -55.47(18) . . . . ? N3 Y1 Si2 C21 -80.0(3) . . . . ? N4 Y1 Si2 C21 160.8(2) . . . . ? N1 Y1 Si2 C21 -61.3(3) . . . . ? N2 Y1 Si2 C21 14.9(2) . . . . ? Si4 Y1 Si2 C21 134.0(2) . . . . ? N3 Y1 Si2 C22 -174.8(2) . . . . ? N4 Y1 Si2 C22 66.01(16) . . . . ? N1 Y1 Si2 C22 -156.1(2) . . . . ? N2 Y1 Si2 C22 -79.94(15) . . . . ? Si4 Y1 Si2 C22 39.20(14) . . . . ? N3 Y1 Si4 N4 41.2(2) . . . . ? N1 Y1 Si4 N4 -108.65(18) . . . . ? N2 Y1 Si4 N4 171.18(18) . . . . ? Si2 Y1 Si4 N4 64.28(16) . . . . ? N3 Y1 Si4 C28 134.3(2) . . . . ? N4 Y1 Si4 C28 93.1(2) . . . . ? N1 Y1 Si4 C28 -15.54(18) . . . . ? N2 Y1 Si4 C28 -95.71(18) . . . . ? Si2 Y1 Si4 C28 157.39(16) . . . . ? N3 Y1 Si4 C26 -40.6(2) . . . . ? N4 Y1 Si4 C26 -81.8(3) . . . . ? N1 Y1 Si4 C26 169.6(2) . . . . ? N2 Y1 Si4 C26 89.4(2) . . . . ? Si2 Y1 Si4 C26 -17.5(2) . . . . ? N3 Y1 Si4 C27 -130.3(2) . . . . ? N4 Y1 Si4 C27 -171.5(2) . . . . ? N1 Y1 Si4 C27 79.82(18) . . . . ? N2 Y1 Si4 C27 -0.35(19) . . . . ? Si2 Y1 Si4 C27 -107.25(17) . . . . ? N3 Y1 N1 C2 40.1(3) . . . . ? N4 Y1 N1 C2 165.8(3) . . . . ? N2 Y1 N1 C2 -51.1(3) . . . . ? Si2 Y1 N1 C2 29.1(4) . . . . ? Si4 Y1 N1 C2 -165.2(2) . . . . ? N3 Y1 N1 C6 -135.7(3) . . . . ? N4 Y1 N1 C6 -10.0(3) . . . . ? N2 Y1 N1 C6 133.1(3) . . . . ? Si2 Y1 N1 C6 -146.7(2) . . . . ? Si4 Y1 N1 C6 19.0(3) . . . . ? N3 Y1 N2 C4 -71.2(3) . . . . ? N4 Y1 N2 C4 149.6(3) . . . . ? N1 Y1 N2 C4 51.5(3) . . . . ? Si2 Y1 N2 C4 -101.2(3) . . . . ? Si4 Y1 N2 C4 142.2(2) . . . . ? N3 Y1 N2 C14 87.0(3) . . . . ? N4 Y1 N2 C14 -52.2(4) . . . . ? N1 Y1 N2 C14 -150.3(3) . . . . ? Si2 Y1 N2 C14 57.0(3) . . . . ? Si4 Y1 N2 C14 -59.7(3) . . . . ? C20 Si2 N3 Si1 73.5(3) . . . . ? C21 Si2 N3 Si1 -49.2(3) . . . . ? C22 Si2 N3 Si1 -169.0(2) . . . . ? Y1 Si2 N3 Si1 -174.1(3) . . . . ? C20 Si2 N3 Y1 -112.46(18) . . . . ? C21 Si2 N3 Y1 124.86(19) . . . . ? C22 Si2 N3 Y1 5.0(2) . . . . ? C18 Si1 N3 Si2 -158.6(2) . . . . ? C19 Si1 N3 Si2 81.7(3) . . . . ? C17 Si1 N3 Si2 -39.6(3) . . . . ? C18 Si1 N3 Y1 28.4(3) . . . . ? C19 Si1 N3 Y1 -91.3(2) . . . . ? C17 Si1 N3 Y1 147.3(3) . . . . ? N4 Y1 N3 Si2 67.43(17) . . . . ? N1 Y1 N3 Si2 -169.72(12) . . . . ? N2 Y1 N3 Si2 -88.40(16) . . . . ? Si4 Y1 N3 Si2 47.0(2) . . . . ? N4 Y1 N3 Si1 -118.76(19) . . . . ? N1 Y1 N3 Si1 4.1(3) . . . . ? N2 Y1 N3 Si1 85.4(2) . . . . ? Si2 Y1 N3 Si1 173.8(3) . . . . ? Si4 Y1 N3 Si1 -139.18(14) . . . . ? C28 Si4 N4 Si3 72.9(3) . . . . ? C26 Si4 N4 Si3 -53.1(3) . . . . ? C27 Si4 N4 Si3 -169.0(2) . . . . ? Y1 Si4 N4 Si3 -177.0(3) . . . . ? C28 Si4 N4 Y1 -110.10(19) . . . . ? C26 Si4 N4 Y1 123.9(2) . . . . ? C27 Si4 N4 Y1 8.0(2) . . . . ? C23 Si3 N4 Si4 -53.5(3) . . . . ? C24 Si3 N4 Si4 -172.7(2) . . . . ? C25 Si3 N4 Si4 67.5(3) . . . . ? C23 Si3 N4 Y1 130.1(2) . . . . ? C24 Si3 N4 Y1 10.9(3) . . . . ? C25 Si3 N4 Y1 -108.9(2) . . . . ? N3 Y1 N4 Si4 -150.05(15) . . . . ? N1 Y1 N4 Si4 76.24(17) . . . . ? N2 Y1 N4 Si4 -13.7(3) . . . . ? Si2 Y1 N4 Si4 -122.46(14) . . . . ? N3 Y1 N4 Si3 26.7(2) . . . . ? N1 Y1 N4 Si3 -107.0(2) . . . . ? N2 Y1 N4 Si3 163.07(17) . . . . ? Si2 Y1 N4 Si3 54.3(2) . . . . ? Si4 Y1 N4 Si3 176.8(3) . . . . ? C6 N1 C2 C3 -155.8(4) . . . . ? Y1 N1 C2 C3 28.0(5) . . . . ? C6 N1 C2 C1 22.8(5) . . . . ? Y1 N1 C2 C1 -153.5(3) . . . . ? N1 C2 C3 C4 22.2(7) . . . . ? C1 C2 C3 C4 -156.4(4) . . . . ? C14 N2 C4 C3 171.4(4) . . . . ? Y1 N2 C4 C3 -29.0(5) . . . . ? C14 N2 C4 C5 -6.1(5) . . . . ? Y1 N2 C4 C5 153.5(3) . . . . ? C2 C3 C4 N2 -20.3(7) . . . . ? C2 C3 C4 C5 157.4(4) . . . . ? C2 N1 C6 C7 76.9(5) . . . . ? Y1 N1 C6 C7 -107.3(4) . . . . ? C2 N1 C6 C11 -103.8(4) . . . . ? Y1 N1 C6 C11 72.0(4) . . . . ? C11 C6 C7 C8 -1.2(6) . . . . ? N1 C6 C7 C8 178.0(4) . . . . ? C11 C6 C7 C12 177.1(4) . . . . ? N1 C6 C7 C12 -3.7(6) . . . . ? C6 C7 C8 C9 0.1(7) . . . . ? C12 C7 C8 C9 -178.2(5) . . . . ? C7 C8 C9 C10 1.0(8) . . . . ? C8 C9 C10 C11 -0.9(8) . . . . ? C9 C10 C11 C6 -0.2(7) . . . . ? C9 C10 C11 C13 177.8(5) . . . . ? C7 C6 C11 C10 1.3(6) . . . . ? N1 C6 C11 C10 -177.9(4) . . . . ? C7 C6 C11 C13 -176.7(4) . . . . ? N1 C6 C11 C13 4.1(6) . . . . ? C4 N2 C14 C15 -104.4(4) . . . . ? Y1 N2 C14 C15 98.1(4) . . . . ? C4 N2 C14 C16 77.0(5) . . . 2_566 ? Y1 N2 C14 C16 -80.5(4) . . . 2_566 ? C16 C14 C15 C16 1.3(6) 2_566 . . . ? N2 C14 C15 C16 -177.3(3) . . . . ? C14 C15 C16 C14 -1.3(6) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.703 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.072 _database_code_depnum_ccdc_archive 'CCDC 952927' ####################################################################### # # 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_complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H108 N8 Si8 Sm2' _chemical_formula_sum 'C56 H108 N8 Si8 Sm2' _chemical_formula_weight 1418.92 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2006(12) _cell_length_b 11.4482(11) _cell_length_c 15.2323(13) _cell_angle_alpha 92.946(2) _cell_angle_beta 93.603(2) _cell_angle_gamma 108.289(3) _cell_volume 1845.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8822 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 1.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.508 _exptl_absorpt_correction_T_max 0.819 _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 15907 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6812 _reflns_number_gt 6104 _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^)+(0.0258P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6812 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Sm1 Sm 0.300239(16) 0.132374(13) 0.273185(10) 0.02866(6) Uani 1 1 d . . . Si1 Si 0.28559(9) 0.38405(8) 0.38192(6) 0.0354(2) Uani 1 1 d . . . Si2 Si 0.04806(9) 0.26569(8) 0.26221(6) 0.0375(2) Uani 1 1 d . . . Si3 Si 0.07937(10) -0.11355(8) 0.33565(6) 0.0383(2) Uani 1 1 d . . . Si4 Si 0.14782(10) -0.14415(8) 0.14766(6) 0.0426(2) Uani 1 1 d . . . N1 N 0.4635(3) 0.2383(2) 0.18643(16) 0.0329(6) Uani 1 1 d . . . N2 N 0.4788(3) 0.0683(2) 0.32465(17) 0.0368(7) Uani 1 1 d . . . N3 N 0.1959(2) 0.2715(2) 0.30456(15) 0.0309(6) Uani 1 1 d . . . N4 N 0.1610(3) -0.0611(2) 0.24652(16) 0.0336(6) Uani 1 1 d . . . C1 C 0.5828(4) 0.2107(4) 0.0606(2) 0.0620(12) Uani 1 1 d . . . H1A H 0.5322 0.2507 0.0273 0.093 Uiso 1 1 calc R . . H1B H 0.5874 0.1392 0.0257 0.093 Uiso 1 1 calc R . . H1C H 0.6672 0.2680 0.0748 0.093 Uiso 1 1 calc R . . C2 C 0.5234(3) 0.1704(3) 0.1446(2) 0.0391(8) Uani 1 1 d . . . C3 C 0.5381(4) 0.0623(3) 0.1754(2) 0.0476(9) Uani 1 1 d . . . H3 H 0.5535 0.0080 0.1325 0.057 Uiso 1 1 calc R . . C4 C 0.5330(3) 0.0235(3) 0.2621(2) 0.0404(8) Uani 1 1 d . . . C5 C 0.5991(4) -0.0707(4) 0.2810(3) 0.0598(11) Uani 1 1 d . . . H5A H 0.6550 -0.0433 0.3345 0.090 Uiso 1 1 calc R . . H5B H 0.6479 -0.0794 0.2321 0.090 Uiso 1 1 calc R . . H5C H 0.5368 -0.1496 0.2885 0.090 Uiso 1 1 calc R . . C6 C 0.4946(3) 0.3667(3) 0.1683(2) 0.0383(8) Uani 1 1 d . . . C7 C 0.4114(4) 0.4061(3) 0.1143(2) 0.0444(9) Uani 1 1 d . . . C8 C 0.4421(5) 0.5307(4) 0.1012(3) 0.0668(13) Uani 1 1 d . . . H8 H 0.3876 0.5585 0.0644 0.080 Uiso 1 1 calc R . . C9 C 0.5497(6) 0.6131(4) 0.1407(3) 0.0824(17) Uani 1 1 d . . . H9 H 0.5681 0.6976 0.1324 0.099 Uiso 1 1 calc R . . C10 C 0.6319(5) 0.5737(4) 0.1927(3) 0.0756(15) Uani 1 1 d . . . H10 H 0.7064 0.6318 0.2192 0.091 Uiso 1 1 calc R . . C11 C 0.6074(4) 0.4495(3) 0.2073(2) 0.0524(10) Uani 1 1 d . . . C12 C 0.2930(4) 0.3176(4) 0.0689(2) 0.0585(11) Uani 1 1 d . . . H12A H 0.2508 0.3619 0.0321 0.088 Uiso 1 1 calc R . . H12B H 0.2378 0.2778 0.1127 0.088 Uiso 1 1 calc R . . H12C H 0.3136 0.2557 0.0326 0.088 Uiso 1 1 calc R . . C13 C 0.6983(4) 0.4073(4) 0.2636(3) 0.0768(14) Uani 1 1 d . . . H13A H 0.6528 0.3517 0.3049 0.115 Uiso 1 1 calc R . . H13B H 0.7599 0.4782 0.2959 0.115 Uiso 1 1 calc R . . H13C H 0.7412 0.3649 0.2264 0.115 Uiso 1 1 calc R . . C14 C 0.4923(3) 0.0331(3) 0.4132(2) 0.0378(8) Uani 1 1 d . . . C15 C 0.5692(3) 0.1155(3) 0.4783(2) 0.0403(8) Uani 1 1 d . . . H15 H 0.6174 0.1944 0.4640 0.048 Uiso 1 1 calc R . . C16 C 0.5761(3) 0.0835(3) 0.5636(2) 0.0412(8) Uani 1 1 d . . . H16 H 0.6280 0.1415 0.6072 0.049 Uiso 1 1 calc R . . C17 C 0.4228(4) 0.3328(3) 0.4210(2) 0.0510(10) Uani 1 1 d . . . H17A H 0.3917 0.2548 0.4474 0.076 Uiso 1 1 calc R . . H17B H 0.4776 0.3944 0.4644 0.076 Uiso 1 1 calc R . . H17C H 0.4697 0.3230 0.3713 0.076 Uiso 1 1 calc R . . C18 C 0.2038(4) 0.4040(4) 0.4826(2) 0.0691(13) Uani 1 1 d . . . H18A H 0.1368 0.4379 0.4669 0.104 Uiso 1 1 calc R . . H18B H 0.2641 0.4598 0.5266 0.104 Uiso 1 1 calc R . . H18C H 0.1683 0.3246 0.5064 0.104 Uiso 1 1 calc R . . C19 C 0.3526(4) 0.5400(3) 0.3403(2) 0.0508(10) Uani 1 1 d . . . H19A H 0.4040 0.5348 0.2923 0.076 Uiso 1 1 calc R . . H19B H 0.4041 0.5967 0.3877 0.076 Uiso 1 1 calc R . . H19C H 0.2843 0.5694 0.3194 0.076 Uiso 1 1 calc R . . C20 C -0.0144(4) 0.1404(3) 0.1707(2) 0.0507(10) Uani 1 1 d . . . H20A H 0.0274 0.1667 0.1179 0.076 Uiso 1 1 calc R . . H20B H -0.1045 0.1239 0.1590 0.076 Uiso 1 1 calc R . . H20C H 0.0018 0.0661 0.1880 0.076 Uiso 1 1 calc R . . C21 C 0.0470(4) 0.4123(3) 0.2133(3) 0.0601(11) Uani 1 1 d . . . H21A H 0.0675 0.4786 0.2596 0.090 Uiso 1 1 calc R . . H21B H -0.0361 0.4016 0.1848 0.090 Uiso 1 1 calc R . . H21C H 0.1089 0.4327 0.1701 0.090 Uiso 1 1 calc R . . C22 C -0.0711(4) 0.2343(4) 0.3463(3) 0.0581(11) Uani 1 1 d . . . H22A H -0.0634 0.1671 0.3801 0.087 Uiso 1 1 calc R . . H22B H -0.1553 0.2118 0.3167 0.087 Uiso 1 1 calc R . . H22C H -0.0562 0.3078 0.3856 0.087 Uiso 1 1 calc R . . C23 C 0.1484(4) 0.0027(3) 0.4322(2) 0.0431(9) Uani 1 1 d . . . H23A H 0.2382 0.0154 0.4417 0.065 Uiso 1 1 calc R . . H23B H 0.1076 -0.0277 0.4846 0.065 Uiso 1 1 calc R . . H23C H 0.1350 0.0802 0.4201 0.065 Uiso 1 1 calc R . . C24 C 0.0849(4) -0.2680(3) 0.3673(3) 0.0553(11) Uani 1 1 d . . . H24A H 0.0340 -0.3316 0.3235 0.083 Uiso 1 1 calc R . . H24B H 0.0522 -0.2837 0.4244 0.083 Uiso 1 1 calc R . . H24C H 0.1715 -0.2685 0.3702 0.083 Uiso 1 1 calc R . . C25 C -0.0919(4) -0.1262(3) 0.3220(3) 0.0567(10) Uani 1 1 d . . . H25A H -0.0998 -0.0449 0.3163 0.085 Uiso 1 1 calc R . . H25B H -0.1330 -0.1613 0.3731 0.085 Uiso 1 1 calc R . . H25C H -0.1315 -0.1791 0.2694 0.085 Uiso 1 1 calc R . . C26 C 0.2031(4) -0.0336(3) 0.0606(2) 0.0553(10) Uani 1 1 d . . . H26A H 0.1471 0.0156 0.0535 0.083 Uiso 1 1 calc R . . H26B H 0.2025 -0.0795 0.0052 0.083 Uiso 1 1 calc R . . H26C H 0.2881 0.0201 0.0783 0.083 Uiso 1 1 calc R . . C27 C -0.0179(4) -0.2406(4) 0.1104(3) 0.0814(15) Uani 1 1 d . . . H27A H -0.0501 -0.2996 0.1535 0.122 Uiso 1 1 calc R . . H27B H -0.0190 -0.2844 0.0539 0.122 Uiso 1 1 calc R . . H27C H -0.0704 -0.1879 0.1043 0.122 Uiso 1 1 calc R . . C28 C 0.2478(4) -0.2478(3) 0.1488(3) 0.0617(12) Uani 1 1 d . . . H28A H 0.3360 -0.1984 0.1588 0.093 Uiso 1 1 calc R . . H28B H 0.2338 -0.2957 0.0925 0.093 Uiso 1 1 calc R . . H28C H 0.2254 -0.3030 0.1956 0.093 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 Sm1 0.02868(11) 0.02788(9) 0.03172(10) 0.00487(6) 0.00313(7) 0.01175(7) Si1 0.0400(6) 0.0343(5) 0.0340(5) 0.0006(4) 0.0044(4) 0.0149(4) Si2 0.0342(6) 0.0384(5) 0.0444(5) 0.0071(4) 0.0030(4) 0.0173(4) Si3 0.0364(6) 0.0307(5) 0.0487(6) 0.0038(4) 0.0134(4) 0.0099(4) Si4 0.0434(7) 0.0364(5) 0.0433(5) -0.0053(4) 0.0058(5) 0.0067(5) N1 0.0328(17) 0.0342(14) 0.0342(14) 0.0073(11) 0.0036(12) 0.0133(13) N2 0.0336(18) 0.0360(15) 0.0434(16) 0.0121(12) -0.0021(13) 0.0143(13) N3 0.0325(17) 0.0315(14) 0.0323(14) 0.0036(11) 0.0056(12) 0.0147(12) N4 0.0301(17) 0.0318(14) 0.0385(15) 0.0020(11) 0.0053(12) 0.0087(12) C1 0.085(3) 0.067(3) 0.050(2) 0.0147(19) 0.031(2) 0.041(2) C2 0.039(2) 0.0410(19) 0.0395(19) 0.0059(15) 0.0029(16) 0.0157(17) C3 0.061(3) 0.045(2) 0.046(2) -0.0002(16) 0.0040(18) 0.0301(19) C4 0.035(2) 0.0352(18) 0.052(2) 0.0025(16) -0.0021(17) 0.0151(16) C5 0.071(3) 0.061(2) 0.065(3) 0.009(2) 0.003(2) 0.046(2) C6 0.041(2) 0.0346(18) 0.0432(19) 0.0087(15) 0.0213(16) 0.0130(16) C7 0.058(3) 0.045(2) 0.0396(19) 0.0144(16) 0.0191(18) 0.0248(19) C8 0.107(4) 0.052(3) 0.061(3) 0.026(2) 0.038(3) 0.044(3) C9 0.135(5) 0.038(2) 0.075(3) 0.012(2) 0.050(3) 0.021(3) C10 0.079(4) 0.049(3) 0.077(3) -0.007(2) 0.035(3) -0.014(3) C11 0.042(3) 0.053(2) 0.055(2) -0.0036(18) 0.018(2) 0.002(2) C12 0.059(3) 0.075(3) 0.052(2) 0.022(2) 0.006(2) 0.033(2) C13 0.035(3) 0.100(4) 0.081(3) -0.014(3) 0.001(2) 0.005(3) C14 0.034(2) 0.0383(18) 0.046(2) 0.0132(15) -0.0007(16) 0.0186(16) C15 0.034(2) 0.0322(17) 0.053(2) 0.0130(15) -0.0059(16) 0.0086(15) C16 0.036(2) 0.0368(18) 0.049(2) 0.0078(15) -0.0057(16) 0.0110(16) C17 0.051(3) 0.046(2) 0.054(2) -0.0076(17) -0.0150(19) 0.0182(19) C18 0.080(4) 0.072(3) 0.051(2) -0.013(2) 0.022(2) 0.018(3) C19 0.056(3) 0.0369(19) 0.055(2) -0.0016(16) -0.0039(19) 0.0113(18) C20 0.042(3) 0.057(2) 0.051(2) 0.0025(18) -0.0072(18) 0.0150(19) C21 0.053(3) 0.054(2) 0.080(3) 0.022(2) 0.000(2) 0.027(2) C22 0.045(3) 0.068(3) 0.068(3) 0.007(2) 0.013(2) 0.026(2) C23 0.048(2) 0.045(2) 0.0415(19) 0.0068(16) 0.0115(17) 0.0209(18) C24 0.061(3) 0.040(2) 0.069(3) 0.0126(18) 0.027(2) 0.0172(19) C25 0.040(3) 0.051(2) 0.077(3) 0.004(2) 0.017(2) 0.0103(19) C26 0.062(3) 0.056(2) 0.047(2) -0.0015(18) 0.006(2) 0.019(2) C27 0.065(3) 0.084(3) 0.068(3) -0.031(2) 0.001(2) -0.008(3) C28 0.086(4) 0.046(2) 0.061(2) 0.0036(19) 0.026(2) 0.030(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N4 2.272(2) . ? Sm1 N3 2.300(2) . ? Sm1 N1 2.375(3) . ? Sm1 N2 2.436(3) . ? Sm1 Si1 3.3034(9) . ? Sm1 Si3 3.3394(10) . ? Si1 N3 1.715(3) . ? Si1 C19 1.867(3) . ? Si1 C18 1.874(4) . ? Si1 C17 1.883(4) . ? Si2 N3 1.719(3) . ? Si2 C22 1.874(4) . ? Si2 C21 1.875(3) . ? Si2 C20 1.879(3) . ? Si3 N4 1.713(3) . ? Si3 C24 1.875(3) . ? Si3 C25 1.875(4) . ? Si3 C23 1.882(3) . ? Si4 N4 1.712(3) . ? Si4 C28 1.870(4) . ? Si4 C27 1.872(4) . ? Si4 C26 1.877(4) . ? N1 C2 1.337(4) . ? N1 C6 1.446(4) . ? N2 C4 1.326(4) . ? N2 C14 1.440(4) . ? C1 C2 1.506(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C3 1.399(4) . ? C3 C4 1.414(5) . ? C3 H3 0.9400 . ? C4 C5 1.516(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C11 1.394(5) . ? C6 C7 1.398(5) . ? C7 C8 1.387(5) . ? C7 C12 1.494(5) . ? C8 C9 1.358(7) . ? C8 H8 0.9400 . ? C9 C10 1.373(7) . ? C9 H9 0.9400 . ? C10 C11 1.393(6) . ? C10 H10 0.9400 . ? C11 C13 1.500(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 C15 1.378(4) . ? C14 C16 1.391(4) 2_656 ? C15 C16 1.372(5) . ? C15 H15 0.9400 . ? C16 C14 1.391(4) 2_656 ? C16 H16 0.9400 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? 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 . ? 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 Sm1 N3 110.45(9) . . ? N4 Sm1 N1 128.31(9) . . ? N3 Sm1 N1 104.65(9) . . ? N4 Sm1 N2 96.03(9) . . ? N3 Sm1 N2 142.53(9) . . ? N1 Sm1 N2 76.30(9) . . ? N4 Sm1 Si1 132.75(7) . . ? N3 Sm1 Si1 29.23(6) . . ? N1 Sm1 Si1 95.10(6) . . ? N2 Sm1 Si1 113.76(6) . . ? N4 Sm1 Si3 28.16(6) . . ? N3 Sm1 Si3 95.96(6) . . ? N1 Sm1 Si3 155.31(6) . . ? N2 Sm1 Si3 95.56(6) . . ? Si1 Sm1 Si3 109.44(2) . . ? N3 Si1 C19 115.13(14) . . ? N3 Si1 C18 114.54(17) . . ? C19 Si1 C18 107.18(18) . . ? N3 Si1 C17 106.14(14) . . ? C19 Si1 C17 107.11(18) . . ? C18 Si1 C17 106.14(19) . . ? N3 Si1 Sm1 40.91(8) . . ? C19 Si1 Sm1 121.70(12) . . ? C18 Si1 Sm1 130.88(14) . . ? C17 Si1 Sm1 65.63(11) . . ? N3 Si2 C22 113.11(16) . . ? N3 Si2 C21 112.58(16) . . ? C22 Si2 C21 106.97(18) . . ? N3 Si2 C20 111.17(15) . . ? C22 Si2 C20 106.64(18) . . ? C21 Si2 C20 105.90(18) . . ? N4 Si3 C24 114.33(15) . . ? N4 Si3 C25 114.07(16) . . ? C24 Si3 C25 106.21(18) . . ? N4 Si3 C23 107.88(14) . . ? C24 Si3 C23 108.53(17) . . ? C25 Si3 C23 105.35(17) . . ? N4 Si3 Sm1 38.75(8) . . ? C24 Si3 Sm1 132.03(13) . . ? C25 Si3 Sm1 120.82(12) . . ? C23 Si3 Sm1 69.38(11) . . ? N4 Si4 C28 112.64(16) . . ? N4 Si4 C27 113.56(17) . . ? C28 Si4 C27 107.8(2) . . ? N4 Si4 C26 108.59(14) . . ? C28 Si4 C26 107.14(18) . . ? C27 Si4 C26 106.7(2) . . ? C2 N1 C6 117.5(3) . . ? C2 N1 Sm1 116.8(2) . . ? C6 N1 Sm1 125.4(2) . . ? C4 N2 C14 118.5(3) . . ? C4 N2 Sm1 115.3(2) . . ? C14 N2 Sm1 121.5(2) . . ? Si1 N3 Si2 123.06(14) . . ? Si1 N3 Sm1 109.86(13) . . ? Si2 N3 Sm1 127.04(13) . . ? Si4 N4 Si3 125.27(15) . . ? Si4 N4 Sm1 121.58(13) . . ? Si3 N4 Sm1 113.09(12) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.8(3) . . ? N1 C2 C1 120.2(3) . . ? C3 C2 C1 116.0(3) . . ? C2 C3 C4 129.0(3) . . ? C2 C3 H3 115.5 . . ? C4 C3 H3 115.5 . . ? N2 C4 C3 123.3(3) . . ? N2 C4 C5 121.2(3) . . ? C3 C4 C5 115.5(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 121.3(3) . . ? C11 C6 N1 118.5(3) . . ? C7 C6 N1 120.2(3) . . ? C8 C7 C6 118.6(4) . . ? C8 C7 C12 119.5(4) . . ? C6 C7 C12 121.8(3) . . ? C9 C8 C7 120.8(5) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 120.3(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 121.6(4) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 117.4(4) . . ? C10 C11 C13 121.1(4) . . ? C6 C11 C13 121.5(4) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 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 C16 118.1(3) . 2_656 ? C15 C14 N2 121.0(3) . . ? C16 C14 N2 120.9(3) 2_656 . ? C16 C15 C14 120.7(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C14 121.2(3) . 2_656 ? C15 C16 H16 119.4 . . ? C14 C16 H16 119.4 2_656 . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C24 H24A 109.5 . . ? Si3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si4 C27 H27A 109.5 . . ? Si4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? 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 Sm1 Si1 N3 -47.35(16) . . . . ? N1 Sm1 Si1 N3 111.12(14) . . . . ? N2 Sm1 Si1 N3 -171.62(14) . . . . ? Si3 Sm1 Si1 N3 -66.09(13) . . . . ? N4 Sm1 Si1 C19 -140.18(17) . . . . ? N3 Sm1 Si1 C19 -92.83(19) . . . . ? N1 Sm1 Si1 C19 18.29(16) . . . . ? N2 Sm1 Si1 C19 95.55(16) . . . . ? Si3 Sm1 Si1 C19 -158.92(15) . . . . ? N4 Sm1 Si1 C18 33.4(2) . . . . ? N3 Sm1 Si1 C18 80.8(2) . . . . ? N1 Sm1 Si1 C18 -168.1(2) . . . . ? N2 Sm1 Si1 C18 -90.8(2) . . . . ? Si3 Sm1 Si1 C18 14.7(2) . . . . ? N4 Sm1 Si1 C17 124.10(16) . . . . ? N3 Sm1 Si1 C17 171.44(19) . . . . ? N1 Sm1 Si1 C17 -77.44(15) . . . . ? N2 Sm1 Si1 C17 -0.17(15) . . . . ? Si3 Sm1 Si1 C17 105.35(14) . . . . ? N3 Sm1 Si3 N4 123.33(16) . . . . ? N1 Sm1 Si3 N4 -23.3(2) . . . . ? N2 Sm1 Si3 N4 -92.38(16) . . . . ? Si1 Sm1 Si3 N4 150.00(14) . . . . ? N4 Sm1 Si3 C24 76.3(2) . . . . ? N3 Sm1 Si3 C24 -160.36(18) . . . . ? N1 Sm1 Si3 C24 53.0(2) . . . . ? N2 Sm1 Si3 C24 -16.07(18) . . . . ? Si1 Sm1 Si3 C24 -133.69(17) . . . . ? N4 Sm1 Si3 C25 -90.9(2) . . . . ? N3 Sm1 Si3 C25 32.44(16) . . . . ? N1 Sm1 Si3 C25 -114.2(2) . . . . ? N2 Sm1 Si3 C25 176.73(16) . . . . ? Si1 Sm1 Si3 C25 59.12(15) . . . . ? N4 Sm1 Si3 C23 173.09(19) . . . . ? N3 Sm1 Si3 C23 -63.58(13) . . . . ? N1 Sm1 Si3 C23 149.75(19) . . . . ? N2 Sm1 Si3 C23 80.71(14) . . . . ? Si1 Sm1 Si3 C23 -36.91(12) . . . . ? N4 Sm1 N1 C2 -35.4(3) . . . . ? N3 Sm1 N1 C2 -167.2(2) . . . . ? N2 Sm1 N1 C2 51.5(2) . . . . ? Si1 Sm1 N1 C2 164.7(2) . . . . ? Si3 Sm1 N1 C2 -21.6(3) . . . . ? N4 Sm1 N1 C6 138.1(2) . . . . ? N3 Sm1 N1 C6 6.3(3) . . . . ? N2 Sm1 N1 C6 -135.0(3) . . . . ? Si1 Sm1 N1 C6 -21.8(2) . . . . ? Si3 Sm1 N1 C6 151.9(2) . . . . ? N4 Sm1 N2 C4 75.3(2) . . . . ? N3 Sm1 N2 C4 -149.0(2) . . . . ? N1 Sm1 N2 C4 -52.7(2) . . . . ? Si1 Sm1 N2 C4 -142.3(2) . . . . ? Si3 Sm1 N2 C4 103.6(2) . . . . ? N4 Sm1 N2 C14 -80.1(2) . . . . ? N3 Sm1 N2 C14 55.6(3) . . . . ? N1 Sm1 N2 C14 151.9(2) . . . . ? Si1 Sm1 N2 C14 62.3(2) . . . . ? Si3 Sm1 N2 C14 -51.8(2) . . . . ? C19 Si1 N3 Si2 -71.9(2) . . . . ? C18 Si1 N3 Si2 53.0(2) . . . . ? C17 Si1 N3 Si2 169.81(18) . . . . ? Sm1 Si1 N3 Si2 177.9(2) . . . . ? C19 Si1 N3 Sm1 110.19(17) . . . . ? C18 Si1 N3 Sm1 -124.87(18) . . . . ? C17 Si1 N3 Sm1 -8.11(18) . . . . ? C22 Si2 N3 Si1 -66.1(2) . . . . ? C21 Si2 N3 Si1 55.3(2) . . . . ? C20 Si2 N3 Si1 173.90(18) . . . . ? C22 Si2 N3 Sm1 111.40(19) . . . . ? C21 Si2 N3 Sm1 -127.19(19) . . . . ? C20 Si2 N3 Sm1 -8.6(2) . . . . ? N4 Sm1 N3 Si1 144.80(12) . . . . ? N1 Sm1 N3 Si1 -73.81(13) . . . . ? N2 Sm1 N3 Si1 12.7(2) . . . . ? Si3 Sm1 N3 Si1 119.92(11) . . . . ? N4 Sm1 N3 Si2 -33.01(18) . . . . ? N1 Sm1 N3 Si2 108.38(16) . . . . ? N2 Sm1 N3 Si2 -165.14(13) . . . . ? Si1 Sm1 N3 Si2 -177.8(3) . . . . ? Si3 Sm1 N3 Si2 -57.90(15) . . . . ? C28 Si4 N4 Si3 -83.3(2) . . . . ? C27 Si4 N4 Si3 39.7(3) . . . . ? C26 Si4 N4 Si3 158.2(2) . . . . ? C28 Si4 N4 Sm1 93.84(19) . . . . ? C27 Si4 N4 Sm1 -143.2(2) . . . . ? C26 Si4 N4 Sm1 -24.7(2) . . . . ? C24 Si3 N4 Si4 49.7(3) . . . . ? C25 Si3 N4 Si4 -72.8(2) . . . . ? C23 Si3 N4 Si4 170.52(18) . . . . ? Sm1 Si3 N4 Si4 177.3(3) . . . . ? C24 Si3 N4 Sm1 -127.62(17) . . . . ? C25 Si3 N4 Sm1 109.87(17) . . . . ? C23 Si3 N4 Sm1 -6.79(19) . . . . ? N3 Sm1 N4 Si4 120.08(15) . . . . ? N1 Sm1 N4 Si4 -9.6(2) . . . . ? N2 Sm1 N4 Si4 -86.89(16) . . . . ? Si1 Sm1 N4 Si4 142.62(11) . . . . ? Si3 Sm1 N4 Si4 -177.4(3) . . . . ? N3 Sm1 N4 Si3 -62.49(15) . . . . ? N1 Sm1 N4 Si3 167.82(11) . . . . ? N2 Sm1 N4 Si3 90.54(14) . . . . ? Si1 Sm1 N4 Si3 -39.95(18) . . . . ? C6 N1 C2 C3 157.0(3) . . . . ? Sm1 N1 C2 C3 -29.0(4) . . . . ? C6 N1 C2 C1 -21.3(5) . . . . ? Sm1 N1 C2 C1 152.7(3) . . . . ? N1 C2 C3 C4 -21.9(6) . . . . ? C1 C2 C3 C4 156.5(4) . . . . ? C14 N2 C4 C3 -172.7(3) . . . . ? Sm1 N2 C4 C3 31.1(4) . . . . ? C14 N2 C4 C5 4.8(5) . . . . ? Sm1 N2 C4 C5 -151.4(3) . . . . ? C2 C3 C4 N2 19.6(6) . . . . ? C2 C3 C4 C5 -158.0(4) . . . . ? C2 N1 C6 C11 -76.9(4) . . . . ? Sm1 N1 C6 C11 109.7(3) . . . . ? C2 N1 C6 C7 104.5(4) . . . . ? Sm1 N1 C6 C7 -68.9(4) . . . . ? C11 C6 C7 C8 -1.1(5) . . . . ? N1 C6 C7 C8 177.5(3) . . . . ? C11 C6 C7 C12 177.3(3) . . . . ? N1 C6 C7 C12 -4.1(5) . . . . ? C6 C7 C8 C9 -0.8(6) . . . . ? C12 C7 C8 C9 -179.2(4) . . . . ? C7 C8 C9 C10 1.6(7) . . . . ? C8 C9 C10 C11 -0.6(7) . . . . ? C9 C10 C11 C6 -1.2(6) . . . . ? C9 C10 C11 C13 179.4(4) . . . . ? C7 C6 C11 C10 2.1(5) . . . . ? N1 C6 C11 C10 -176.5(3) . . . . ? C7 C6 C11 C13 -178.6(3) . . . . ? N1 C6 C11 C13 2.8(5) . . . . ? C4 N2 C14 C15 107.3(4) . . . . ? Sm1 N2 C14 C15 -98.0(3) . . . . ? C4 N2 C14 C16 -75.4(4) . . . 2_656 ? Sm1 N2 C14 C16 79.3(4) . . . 2_656 ? C16 C14 C15 C16 -1.0(6) 2_656 . . . ? N2 C14 C15 C16 176.3(3) . . . . ? C14 C15 C16 C14 1.1(6) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.731 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.075 _database_code_depnum_ccdc_archive 'CCDC 952928' ####################################################################### # # 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_complex3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H108 N8 Si8 Y2' _chemical_formula_sum 'C56 H108 N8 Si8 Y2' _chemical_formula_weight 1296.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_space_group_name_Hall 'C 2c 2' _symmetry_Int_Tables_number 20 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, -z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 16.9447(7) _cell_length_b 18.8097(9) _cell_length_c 23.3593(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7445.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 5980 _cell_measurement_theta_min 3.3451 _cell_measurement_theta_max 29.3805 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.66 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 1.716 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73037 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4692 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23492 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6861 _reflns_number_gt 5924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _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^)+(0.0379P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.029(4) _refine_ls_number_reflns 6861 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.182653(15) 0.769596(14) 0.629902(12) 0.02301(8) Uani 1 1 d . . . Si1 Si 0.20813(5) 0.68915(5) 0.49307(4) 0.0323(2) Uani 1 1 d . . . Si2 Si 0.24236(6) 0.61173(5) 0.60344(4) 0.0337(2) Uani 1 1 d . . . Si3 Si 0.27080(5) 0.84511(5) 0.73919(4) 0.0309(2) Uani 1 1 d . . . Si4 Si 0.38652(5) 0.81174(5) 0.64635(4) 0.0374(2) Uani 1 1 d . . . N1 N 0.10966(15) 0.86834(13) 0.60639(11) 0.0300(6) Uani 1 1 d . . . N2 N 0.05476(13) 0.72925(14) 0.65417(10) 0.0263(5) Uani 1 1 d . . . N3 N 0.21768(14) 0.68676(14) 0.56641(10) 0.0271(6) Uani 1 1 d . . . N4 N 0.29116(14) 0.81447(13) 0.67166(10) 0.0263(6) Uani 1 1 d . . . C1 C 0.0332(2) 0.9028(2) 0.52079(16) 0.0497(10) Uani 1 1 d . . . H1A H -0.0102 0.9311 0.5354 0.075 Uiso 1 1 calc R . . H1B H 0.0164 0.8777 0.4866 0.075 Uiso 1 1 calc R . . H1C H 0.0773 0.9336 0.5116 0.075 Uiso 1 1 calc R . . C2 C 0.05834(18) 0.84955(17) 0.56577(14) 0.0329(8) Uani 1 1 d . . . C3 C 0.02469(19) 0.78184(17) 0.56279(14) 0.0352(8) Uani 1 1 d . . . H3 H 0.0091 0.7671 0.5260 0.042 Uiso 1 1 calc R . . C4 C 0.01075(17) 0.73223(18) 0.60727(13) 0.0302(7) Uani 1 1 d . . . C5 C -0.0602(2) 0.6846(2) 0.59884(17) 0.0520(10) Uani 1 1 d . . . H5A H -0.0437 0.6352 0.6002 0.078 Uiso 1 1 calc R . . H5B H -0.0841 0.6945 0.5620 0.078 Uiso 1 1 calc R . . H5C H -0.0984 0.6934 0.6290 0.078 Uiso 1 1 calc R . . C6 C 0.11473(19) 0.94333(16) 0.62061(15) 0.0359(8) Uani 1 1 d . . . C7 C 0.0531(2) 0.97255(18) 0.65237(16) 0.0440(9) Uani 1 1 d . . . C8 C 0.0590(3) 1.0441(2) 0.6681(2) 0.0657(12) Uani 1 1 d . . . H8 H 0.0184 1.0649 0.6898 0.079 Uiso 1 1 calc R . . C9 C 0.1225(3) 1.0840(2) 0.6526(2) 0.0745(14) Uani 1 1 d . . . H9 H 0.1252 1.1321 0.6633 0.089 Uiso 1 1 calc R . . C10 C 0.1824(3) 1.05437(19) 0.6215(2) 0.0672(12) Uani 1 1 d . . . H10 H 0.2260 1.0826 0.6115 0.081 Uiso 1 1 calc R . . C11 C 0.1804(2) 0.98367(17) 0.60443(16) 0.0452(9) Uani 1 1 d . . . C12 C -0.0178(2) 0.9297(2) 0.66992(18) 0.0525(10) Uani 1 1 d . . . H12A H -0.0515 0.9220 0.6369 0.079 Uiso 1 1 calc R . . H12B H -0.0469 0.9552 0.6992 0.079 Uiso 1 1 calc R . . H12C H -0.0007 0.8841 0.6850 0.079 Uiso 1 1 calc R . . C13 C 0.2454(2) 0.9519(2) 0.56986(19) 0.0603(12) Uani 1 1 d . . . H13A H 0.2717 0.9154 0.5921 0.090 Uiso 1 1 calc R . . H13B H 0.2831 0.9887 0.5597 0.090 Uiso 1 1 calc R . . H13C H 0.2237 0.9311 0.5353 0.090 Uiso 1 1 calc R . . C14 C 0.02650(17) 0.68796(16) 0.70187(13) 0.0274(7) Uani 1 1 d . . . C15 C 0.0000 0.7242(2) 0.7500 0.0257(9) Uani 1 2 d S . . H15 H 0.0000 0.7741 0.7500 0.031 Uiso 1 2 calc SR . . C16 C 0.02704(19) 0.61416(17) 0.70232(15) 0.0369(8) Uani 1 1 d . . . H16 H 0.0457 0.5888 0.6704 0.044 Uiso 1 1 calc R . . C17 C 0.0000 0.5781(2) 0.7500 0.0410(12) Uani 1 2 d S . . H17 H 0.0000 0.5282 0.7500 0.049 Uiso 1 2 calc SR . . C18 C 0.2914(2) 0.6440(2) 0.45528(16) 0.0493(10) Uani 1 1 d . . . H18A H 0.3410 0.6649 0.4673 0.074 Uiso 1 1 calc R . . H18B H 0.2852 0.6499 0.4143 0.074 Uiso 1 1 calc R . . H18C H 0.2912 0.5938 0.4646 0.074 Uiso 1 1 calc R . . C19 C 0.2083(2) 0.78355(19) 0.46640(16) 0.0518(10) Uani 1 1 d . . . H19A H 0.1623 0.8082 0.4811 0.078 Uiso 1 1 calc R . . H19B H 0.2070 0.7837 0.4249 0.078 Uiso 1 1 calc R . . H19C H 0.2558 0.8074 0.4795 0.078 Uiso 1 1 calc R . . C20 C 0.1146(2) 0.6466(2) 0.46797(16) 0.0481(10) Uani 1 1 d . . . H20A H 0.1173 0.5957 0.4744 0.072 Uiso 1 1 calc R . . H20B H 0.1076 0.6558 0.4274 0.072 Uiso 1 1 calc R . . H20C H 0.0703 0.6662 0.4891 0.072 Uiso 1 1 calc R . . C21 C 0.3446(2) 0.5770(2) 0.59016(18) 0.0580(11) Uani 1 1 d . . . H21A H 0.3471 0.5559 0.5523 0.087 Uiso 1 1 calc R . . H21B H 0.3574 0.5413 0.6187 0.087 Uiso 1 1 calc R . . H21C H 0.3821 0.6158 0.5926 0.087 Uiso 1 1 calc R . . C22 C 0.1734(3) 0.53532(18) 0.58988(16) 0.0540(10) Uani 1 1 d . . . H22A H 0.1193 0.5515 0.5936 0.081 Uiso 1 1 calc R . . H22B H 0.1834 0.4979 0.6175 0.081 Uiso 1 1 calc R . . H22C H 0.1818 0.5171 0.5515 0.081 Uiso 1 1 calc R . . C23 C 0.2370(2) 0.63351(17) 0.68234(14) 0.0390(8) Uani 1 1 d . . . H23A H 0.2733 0.6719 0.6910 0.058 Uiso 1 1 calc R . . H23B H 0.2511 0.5918 0.7045 0.058 Uiso 1 1 calc R . . H23C H 0.1837 0.6480 0.6920 0.058 Uiso 1 1 calc R . . C24 C 0.3331(2) 0.8050(2) 0.79667(16) 0.0598(11) Uani 1 1 d . . . H24A H 0.3264 0.7538 0.7965 0.090 Uiso 1 1 calc R . . H24B H 0.3171 0.8239 0.8335 0.090 Uiso 1 1 calc R . . H24C H 0.3880 0.8165 0.7898 0.090 Uiso 1 1 calc R . . C25 C 0.16725(19) 0.8184(2) 0.75566(15) 0.0469(9) Uani 1 1 d . . . H25A H 0.1319 0.8392 0.7277 0.070 Uiso 1 1 calc R . . H25B H 0.1531 0.8350 0.7936 0.070 Uiso 1 1 calc R . . H25C H 0.1629 0.7670 0.7543 0.070 Uiso 1 1 calc R . . C26 C 0.2743(3) 0.94406(19) 0.74838(19) 0.0627(12) Uani 1 1 d . . . H26A H 0.3289 0.9595 0.7504 0.094 Uiso 1 1 calc R . . H26B H 0.2473 0.9571 0.7834 0.094 Uiso 1 1 calc R . . H26C H 0.2486 0.9667 0.7161 0.094 Uiso 1 1 calc R . . C27 C 0.4439(2) 0.8945(2) 0.66360(19) 0.0617(12) Uani 1 1 d . . . H27A H 0.4161 0.9356 0.6488 0.093 Uiso 1 1 calc R . . H27B H 0.4958 0.8916 0.6462 0.093 Uiso 1 1 calc R . . H27C H 0.4495 0.8989 0.7048 0.093 Uiso 1 1 calc R . . C28 C 0.3900(2) 0.8015(2) 0.56656(15) 0.0556(11) Uani 1 1 d . . . H28A H 0.3604 0.7596 0.5554 0.083 Uiso 1 1 calc R . . H28B H 0.4444 0.7966 0.5543 0.083 Uiso 1 1 calc R . . H28C H 0.3669 0.8432 0.5487 0.083 Uiso 1 1 calc R . . C29 C 0.4437(2) 0.7351(3) 0.67575(19) 0.0647(12) Uani 1 1 d . . . H29A H 0.4477 0.7396 0.7170 0.097 Uiso 1 1 calc R . . H29B H 0.4962 0.7347 0.6592 0.097 Uiso 1 1 calc R . . H29C H 0.4169 0.6910 0.6663 0.097 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 0.02497(13) 0.02312(13) 0.02094(14) -0.00101(14) -0.00151(13) 0.00205(13) Si1 0.0355(5) 0.0378(5) 0.0237(5) -0.0053(4) -0.0020(4) 0.0045(4) Si2 0.0438(5) 0.0261(4) 0.0312(5) -0.0028(4) -0.0020(4) 0.0066(4) Si3 0.0317(5) 0.0352(5) 0.0259(5) -0.0080(4) -0.0022(4) -0.0007(4) Si4 0.0263(4) 0.0490(5) 0.0369(6) -0.0143(5) -0.0003(4) -0.0027(4) N1 0.0309(13) 0.0273(13) 0.0320(16) 0.0066(11) -0.0041(13) 0.0039(11) N2 0.0319(12) 0.0263(12) 0.0208(13) -0.0061(12) 0.0023(11) 0.0022(13) N3 0.0325(13) 0.0277(13) 0.0211(14) -0.0021(12) 0.0003(11) 0.0029(12) N4 0.0255(12) 0.0290(13) 0.0244(14) -0.0019(12) -0.0044(11) -0.0001(11) C1 0.055(2) 0.051(2) 0.044(2) 0.0178(19) -0.0101(19) 0.0025(19) C2 0.0352(17) 0.0375(19) 0.0260(19) 0.0048(15) -0.0019(16) 0.0121(16) C3 0.0439(18) 0.038(2) 0.0235(18) -0.0023(15) -0.0087(15) 0.0009(16) C4 0.0327(15) 0.0319(16) 0.0259(16) 0.0001(16) -0.0020(14) -0.0012(16) C5 0.050(2) 0.056(2) 0.050(2) 0.003(2) -0.0158(19) -0.012(2) C6 0.0452(19) 0.0260(16) 0.037(2) 0.0105(16) -0.0119(17) 0.0033(15) C7 0.051(2) 0.0337(19) 0.047(2) 0.0039(17) -0.0032(18) 0.0087(17) C8 0.086(3) 0.037(2) 0.074(3) -0.006(2) 0.000(3) 0.020(2) C9 0.104(4) 0.0233(19) 0.097(4) -0.003(2) -0.012(3) -0.004(2) C10 0.074(3) 0.0336(19) 0.094(4) 0.023(2) -0.013(3) -0.009(2) C11 0.048(2) 0.0370(19) 0.051(2) 0.0161(17) -0.011(2) -0.0036(19) C12 0.054(2) 0.044(2) 0.059(3) 0.002(2) 0.007(2) 0.0117(19) C13 0.059(2) 0.056(2) 0.067(3) 0.030(2) 0.005(2) -0.008(2) C14 0.0268(15) 0.0299(16) 0.0254(18) -0.0009(15) 0.0002(14) -0.0051(14) C15 0.0215(18) 0.023(2) 0.033(3) 0.000 0.0009(18) 0.000 C16 0.0464(19) 0.0273(17) 0.037(2) -0.0056(16) 0.0083(17) 0.0019(16) C17 0.055(3) 0.021(2) 0.047(3) 0.000 0.006(3) 0.000 C18 0.053(2) 0.062(2) 0.034(2) -0.0085(19) 0.0055(18) 0.0075(19) C19 0.065(2) 0.054(2) 0.037(2) 0.0026(18) 0.0021(18) 0.0072(19) C20 0.0433(19) 0.060(2) 0.041(2) -0.021(2) -0.0131(18) 0.0083(19) C21 0.058(2) 0.058(2) 0.058(3) 0.003(2) -0.001(2) 0.026(2) C22 0.083(3) 0.0332(18) 0.046(2) -0.0068(17) 0.000(2) -0.004(2) C23 0.051(2) 0.0301(17) 0.036(2) 0.0066(15) -0.0065(18) 0.0030(16) C24 0.057(3) 0.084(3) 0.038(2) 0.001(2) -0.0119(19) 0.010(2) C25 0.044(2) 0.065(2) 0.032(2) -0.0141(19) 0.0061(17) 0.0021(19) C26 0.087(3) 0.043(2) 0.058(3) -0.022(2) 0.003(3) -0.006(2) C27 0.042(2) 0.076(3) 0.067(3) -0.019(2) 0.006(2) -0.021(2) C28 0.0404(19) 0.086(3) 0.040(2) -0.017(2) 0.0147(18) -0.007(2) C29 0.0385(18) 0.081(3) 0.074(3) -0.026(3) -0.009(2) 0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N3 2.232(2) . ? Y1 N4 2.246(2) . ? Y1 N1 2.298(2) . ? Y1 N2 2.365(2) . ? Y1 C2 2.990(3) . ? Y1 C4 3.043(3) . ? Y1 Si2 3.1973(9) . ? Y1 Si3 3.2810(9) . ? Si1 N3 1.722(3) . ? Si1 C18 1.868(3) . ? Si1 C20 1.870(4) . ? Si1 C19 1.882(4) . ? Si2 N3 1.707(3) . ? Si2 C21 1.878(4) . ? Si2 C22 1.879(4) . ? Si2 C23 1.890(3) . ? Si3 N4 1.714(3) . ? Si3 C25 1.865(3) . ? Si3 C24 1.867(4) . ? Si3 C26 1.874(3) . ? Si4 N4 1.721(3) . ? Si4 C29 1.868(4) . ? Si4 C28 1.875(4) . ? Si4 C27 1.879(4) . ? N1 C2 1.335(4) . ? N1 C6 1.452(4) . ? N2 C4 1.326(4) . ? N2 C14 1.440(4) . ? C1 C2 1.512(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C3 1.397(4) . ? C3 C4 1.416(4) . ? C3 H3 0.9400 . ? C4 C5 1.513(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.394(5) . ? C6 C11 1.398(5) . ? C7 C8 1.398(5) . ? C7 C12 1.504(5) . ? C8 C9 1.361(6) . ? C8 H8 0.9400 . ? C9 C10 1.366(6) . ? C9 H9 0.9400 . ? C10 C11 1.389(5) . ? C10 H10 0.9400 . ? C11 C13 1.491(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 C16 1.388(4) . ? C14 C15 1.389(4) . ? C15 C14 1.389(4) 4_556 ? C15 H15 0.9400 . ? C16 C17 1.382(4) . ? C16 H16 0.9400 . ? C17 C16 1.382(4) 4_556 ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? 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 . ? 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 N4 109.47(9) . . ? N3 Y1 N1 123.27(9) . . ? N4 Y1 N1 103.93(9) . . ? N3 Y1 N2 100.31(9) . . ? N4 Y1 N2 140.05(9) . . ? N1 Y1 N2 79.83(9) . . ? N3 Y1 C2 101.86(9) . . ? N4 Y1 C2 127.24(9) . . ? N1 Y1 C2 25.14(9) . . ? N2 Y1 C2 68.66(9) . . ? N3 Y1 C4 88.73(9) . . ? N4 Y1 C4 161.07(9) . . ? N1 Y1 C4 68.28(9) . . ? N2 Y1 C4 24.54(8) . . ? C2 Y1 C4 49.82(9) . . ? N3 Y1 Si2 30.56(7) . . ? N4 Y1 Si2 100.02(6) . . ? N1 Y1 Si2 151.01(7) . . ? N2 Y1 Si2 92.19(6) . . ? C2 Y1 Si2 126.38(7) . . ? C4 Y1 Si2 93.14(6) . . ? N3 Y1 Si3 134.29(6) . . ? N4 Y1 Si3 29.16(7) . . ? N1 Y1 Si3 94.65(7) . . ? N2 Y1 Si3 111.69(6) . . ? C2 Y1 Si3 119.52(7) . . ? C4 Y1 Si3 132.14(6) . . ? Si2 Y1 Si3 114.11(2) . . ? N3 Si1 C18 112.79(15) . . ? N3 Si1 C20 112.37(16) . . ? C18 Si1 C20 107.29(17) . . ? N3 Si1 C19 110.73(15) . . ? C18 Si1 C19 105.73(18) . . ? C20 Si1 C19 107.57(18) . . ? N3 Si2 C21 115.47(16) . . ? N3 Si2 C22 113.23(16) . . ? C21 Si2 C22 106.3(2) . . ? N3 Si2 C23 107.64(13) . . ? C21 Si2 C23 106.32(17) . . ? C22 Si2 C23 107.46(16) . . ? N3 Si2 Y1 41.65(8) . . ? C21 Si2 Y1 130.33(14) . . ? C22 Si2 Y1 123.09(14) . . ? C23 Si2 Y1 66.11(10) . . ? N4 Si3 C25 106.77(14) . . ? N4 Si3 C24 114.34(15) . . ? C25 Si3 C24 105.91(18) . . ? N4 Si3 C26 115.64(17) . . ? C25 Si3 C26 105.90(18) . . ? C24 Si3 C26 107.5(2) . . ? N4 Si3 Y1 39.67(8) . . ? C25 Si3 Y1 67.39(11) . . ? C24 Si3 Y1 129.93(14) . . ? C26 Si3 Y1 122.24(15) . . ? N4 Si4 C29 112.55(16) . . ? N4 Si4 C28 111.94(14) . . ? C29 Si4 C28 105.7(2) . . ? N4 Si4 C27 112.80(16) . . ? C29 Si4 C27 107.00(19) . . ? C28 Si4 C27 106.4(2) . . ? C2 N1 C6 117.3(3) . . ? C2 N1 Y1 107.9(2) . . ? C6 N1 Y1 134.3(2) . . ? C4 N2 C14 118.4(2) . . ? C4 N2 Y1 107.68(18) . . ? C14 N2 Y1 131.54(18) . . ? Si2 N3 Si1 123.29(15) . . ? Si2 N3 Y1 107.80(12) . . ? Si1 N3 Y1 128.18(14) . . ? Si3 N4 Si4 120.99(14) . . ? Si3 N4 Y1 111.17(12) . . ? Si4 N4 Y1 127.45(13) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 122.9(3) . . ? N1 C2 C1 120.1(3) . . ? C3 C2 C1 117.0(3) . . ? N1 C2 Y1 47.01(14) . . ? C3 C2 Y1 81.61(18) . . ? C1 C2 Y1 151.5(2) . . ? C2 C3 C4 129.2(3) . . ? C2 C3 H3 115.4 . . ? C4 C3 H3 115.4 . . ? N2 C4 C3 122.7(3) . . ? N2 C4 C5 122.0(3) . . ? C3 C4 C5 115.3(3) . . ? N2 C4 Y1 47.78(14) . . ? C3 C4 Y1 79.38(18) . . ? C5 C4 Y1 157.0(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 121.7(3) . . ? C7 C6 N1 117.4(3) . . ? C11 C6 N1 120.8(3) . . ? C6 C7 C8 117.8(4) . . ? C6 C7 C12 122.1(3) . . ? C8 C7 C12 120.1(4) . . ? C9 C8 C7 121.1(4) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 120.2(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 121.7(4) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 117.5(4) . . ? C10 C11 C13 121.4(4) . . ? C6 C11 C13 121.1(3) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 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 . . ? C16 C14 C15 119.1(3) . . ? C16 C14 N2 122.9(3) . . ? C15 C14 N2 118.0(3) . . ? C14 C15 C14 121.3(4) . 4_556 ? C14 C15 H15 119.4 . . ? C14 C15 H15 119.4 4_556 . ? C17 C16 C14 119.6(3) . . ? C17 C16 H16 120.2 . . ? C14 C16 H16 120.2 . . ? C16 C17 C16 121.3(4) . 4_556 ? C16 C17 H17 119.4 . . ? C16 C17 H17 119.4 4_556 . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C24 H24A 109.5 . . ? Si3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si3 C26 H26A 109.5 . . ? Si3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si4 C27 H27A 109.5 . . ? Si4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si4 C29 H29A 109.5 . . ? Si4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? 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 -111.51(14) . . . . ? N1 Y1 Si2 N3 33.88(19) . . . . ? N2 Y1 Si2 N3 106.70(14) . . . . ? C2 Y1 Si2 N3 41.80(15) . . . . ? C4 Y1 Si2 N3 82.15(14) . . . . ? Si3 Y1 Si2 N3 -138.32(13) . . . . ? N3 Y1 Si2 C21 83.9(2) . . . . ? N4 Y1 Si2 C21 -27.58(19) . . . . ? N1 Y1 Si2 C21 117.8(2) . . . . ? N2 Y1 Si2 C21 -169.37(19) . . . . ? C2 Y1 Si2 C21 125.73(19) . . . . ? C4 Y1 Si2 C21 166.08(19) . . . . ? Si3 Y1 Si2 C21 -54.39(18) . . . . ? N3 Y1 Si2 C22 -88.60(19) . . . . ? N4 Y1 Si2 C22 159.89(16) . . . . ? N1 Y1 Si2 C22 -54.7(2) . . . . ? N2 Y1 Si2 C22 18.10(16) . . . . ? C2 Y1 Si2 C22 -46.80(17) . . . . ? C4 Y1 Si2 C22 -6.45(16) . . . . ? Si3 Y1 Si2 C22 133.08(15) . . . . ? N3 Y1 Si2 C23 175.48(18) . . . . ? N4 Y1 Si2 C23 63.98(13) . . . . ? N1 Y1 Si2 C23 -150.63(18) . . . . ? N2 Y1 Si2 C23 -77.82(13) . . . . ? C2 Y1 Si2 C23 -142.72(14) . . . . ? C4 Y1 Si2 C23 -102.37(13) . . . . ? Si3 Y1 Si2 C23 37.16(12) . . . . ? N3 Y1 Si3 N4 37.57(15) . . . . ? N1 Y1 Si3 N4 -110.47(15) . . . . ? N2 Y1 Si3 N4 168.64(15) . . . . ? C2 Y1 Si3 N4 -114.36(15) . . . . ? C4 Y1 Si3 N4 -175.18(16) . . . . ? Si2 Y1 Si3 N4 65.75(13) . . . . ? N3 Y1 Si3 C25 -135.03(16) . . . . ? N4 Y1 Si3 C25 -172.59(19) . . . . ? N1 Y1 Si3 C25 76.94(14) . . . . ? N2 Y1 Si3 C25 -3.96(15) . . . . ? C2 Y1 Si3 C25 73.04(15) . . . . ? C4 Y1 Si3 C25 12.23(16) . . . . ? Si2 Y1 Si3 C25 -106.84(13) . . . . ? N3 Y1 Si3 C24 -42.8(2) . . . . ? N4 Y1 Si3 C24 -80.4(2) . . . . ? N1 Y1 Si3 C24 169.16(18) . . . . ? N2 Y1 Si3 C24 88.27(18) . . . . ? C2 Y1 Si3 C24 165.27(18) . . . . ? C4 Y1 Si3 C24 104.45(19) . . . . ? Si2 Y1 Si3 C24 -14.62(17) . . . . ? N3 Y1 Si3 C26 129.91(19) . . . . ? N4 Y1 Si3 C26 92.3(2) . . . . ? N1 Y1 Si3 C26 -18.12(18) . . . . ? N2 Y1 Si3 C26 -99.02(18) . . . . ? C2 Y1 Si3 C26 -22.02(18) . . . . ? C4 Y1 Si3 C26 -82.84(19) . . . . ? Si2 Y1 Si3 C26 158.10(16) . . . . ? N3 Y1 N1 C2 34.9(2) . . . . ? N4 Y1 N1 C2 159.9(2) . . . . ? N2 Y1 N1 C2 -60.8(2) . . . . ? C4 Y1 N1 C2 -38.20(19) . . . . ? Si2 Y1 N1 C2 15.1(3) . . . . ? Si3 Y1 N1 C2 -172.0(2) . . . . ? N3 Y1 N1 C6 -136.2(3) . . . . ? N4 Y1 N1 C6 -11.2(3) . . . . ? N2 Y1 N1 C6 128.1(3) . . . . ? C2 Y1 N1 C6 -171.1(4) . . . . ? C4 Y1 N1 C6 150.7(3) . . . . ? Si2 Y1 N1 C6 -156.0(2) . . . . ? Si3 Y1 N1 C6 16.9(3) . . . . ? N3 Y1 N2 C4 -63.1(2) . . . . ? N4 Y1 N2 C4 158.76(19) . . . . ? N1 Y1 N2 C4 59.2(2) . . . . ? C2 Y1 N2 C4 35.7(2) . . . . ? Si2 Y1 N2 C4 -92.8(2) . . . . ? Si3 Y1 N2 C4 150.16(19) . . . . ? N3 Y1 N2 C14 98.4(2) . . . . ? N4 Y1 N2 C14 -39.7(3) . . . . ? N1 Y1 N2 C14 -139.3(3) . . . . ? C2 Y1 N2 C14 -162.8(3) . . . . ? C4 Y1 N2 C14 161.5(4) . . . . ? Si2 Y1 N2 C14 68.7(2) . . . . ? Si3 Y1 N2 C14 -48.3(3) . . . . ? C21 Si2 N3 Si1 66.2(2) . . . . ? C22 Si2 N3 Si1 -56.6(2) . . . . ? C23 Si2 N3 Si1 -175.24(17) . . . . ? Y1 Si2 N3 Si1 -170.9(2) . . . . ? C21 Si2 N3 Y1 -122.90(17) . . . . ? C22 Si2 N3 Y1 114.30(16) . . . . ? C23 Si2 N3 Y1 -4.33(17) . . . . ? C18 Si1 N3 Si2 -46.1(2) . . . . ? C20 Si1 N3 Si2 75.3(2) . . . . ? C19 Si1 N3 Si2 -164.40(18) . . . . ? C18 Si1 N3 Y1 144.88(18) . . . . ? C20 Si1 N3 Y1 -93.7(2) . . . . ? C19 Si1 N3 Y1 26.6(2) . . . . ? N4 Y1 N3 Si2 76.35(14) . . . . ? N1 Y1 N3 Si2 -161.14(11) . . . . ? N2 Y1 N3 Si2 -76.61(13) . . . . ? C2 Y1 N3 Si2 -146.75(12) . . . . ? C4 Y1 N3 Si2 -98.36(13) . . . . ? Si3 Y1 N3 Si2 57.99(16) . . . . ? N4 Y1 N3 Si1 -113.32(16) . . . . ? N1 Y1 N3 Si1 9.2(2) . . . . ? N2 Y1 N3 Si1 93.72(17) . . . . ? C2 Y1 N3 Si1 23.58(18) . . . . ? C4 Y1 N3 Si1 71.97(17) . . . . ? Si2 Y1 N3 Si1 170.3(3) . . . . ? Si3 Y1 N3 Si1 -131.68(13) . . . . ? C25 Si3 N4 Si4 -166.24(18) . . . . ? C24 Si3 N4 Si4 -49.5(2) . . . . ? C26 Si3 N4 Si4 76.2(2) . . . . ? Y1 Si3 N4 Si4 -173.4(2) . . . . ? C25 Si3 N4 Y1 7.14(18) . . . . ? C24 Si3 N4 Y1 123.93(18) . . . . ? C26 Si3 N4 Y1 -110.37(18) . . . . ? C29 Si4 N4 Si3 77.5(2) . . . . ? C28 Si4 N4 Si3 -163.7(2) . . . . ? C27 Si4 N4 Si3 -43.7(2) . . . . ? C29 Si4 N4 Y1 -94.7(2) . . . . ? C28 Si4 N4 Y1 24.1(2) . . . . ? C27 Si4 N4 Y1 144.1(2) . . . . ? N3 Y1 N4 Si3 -152.43(11) . . . . ? N1 Y1 N4 Si3 74.16(14) . . . . ? N2 Y1 N4 Si3 -16.6(2) . . . . ? C2 Y1 N4 Si3 84.71(15) . . . . ? C4 Y1 N4 Si3 11.1(4) . . . . ? Si2 Y1 N4 Si3 -122.31(11) . . . . ? N3 Y1 N4 Si4 20.4(2) . . . . ? N1 Y1 N4 Si4 -112.99(17) . . . . ? N2 Y1 N4 Si4 156.28(14) . . . . ? C2 Y1 N4 Si4 -102.44(17) . . . . ? C4 Y1 N4 Si4 -176.1(2) . . . . ? Si2 Y1 N4 Si4 50.53(17) . . . . ? Si3 Y1 N4 Si4 172.8(3) . . . . ? C6 N1 C2 C3 -154.3(3) . . . . ? Y1 N1 C2 C3 32.9(4) . . . . ? C6 N1 C2 C1 24.8(4) . . . . ? Y1 N1 C2 C1 -148.1(3) . . . . ? C6 N1 C2 Y1 172.9(3) . . . . ? N3 Y1 C2 N1 -150.7(2) . . . . ? N4 Y1 C2 N1 -24.7(2) . . . . ? N2 Y1 C2 N1 112.7(2) . . . . ? C4 Y1 C2 N1 131.2(2) . . . . ? Si2 Y1 C2 N1 -170.96(18) . . . . ? Si3 Y1 C2 N1 9.2(2) . . . . ? N3 Y1 C2 C3 56.7(2) . . . . ? N4 Y1 C2 C3 -177.28(18) . . . . ? N1 Y1 C2 C3 -152.6(3) . . . . ? N2 Y1 C2 C3 -39.82(19) . . . . ? C4 Y1 C2 C3 -21.32(18) . . . . ? Si2 Y1 C2 C3 36.5(2) . . . . ? Si3 Y1 C2 C3 -143.40(17) . . . . ? N3 Y1 C2 C1 -76.9(5) . . . . ? N4 Y1 C2 C1 49.1(5) . . . . ? N1 Y1 C2 C1 73.8(5) . . . . ? N2 Y1 C2 C1 -173.5(5) . . . . ? C4 Y1 C2 C1 -155.0(5) . . . . ? Si2 Y1 C2 C1 -97.2(5) . . . . ? Si3 Y1 C2 C1 83.0(5) . . . . ? N1 C2 C3 C4 26.7(5) . . . . ? C1 C2 C3 C4 -152.4(3) . . . . ? Y1 C2 C3 C4 50.4(3) . . . . ? C14 N2 C4 C3 167.0(3) . . . . ? Y1 N2 C4 C3 -28.6(4) . . . . ? C14 N2 C4 C5 -10.3(4) . . . . ? Y1 N2 C4 C5 154.0(3) . . . . ? C14 N2 C4 Y1 -164.3(3) . . . . ? C2 C3 C4 N2 -28.5(5) . . . . ? C2 C3 C4 C5 149.1(3) . . . . ? C2 C3 C4 Y1 -49.6(3) . . . . ? N3 Y1 C4 N2 118.6(2) . . . . ? N4 Y1 C4 N2 -45.8(4) . . . . ? N1 Y1 C4 N2 -114.5(2) . . . . ? C2 Y1 C4 N2 -134.6(2) . . . . ? Si2 Y1 C4 N2 88.4(2) . . . . ? Si3 Y1 C4 N2 -38.6(2) . . . . ? N3 Y1 C4 C3 -85.57(19) . . . . ? N4 Y1 C4 C3 110.0(3) . . . . ? N1 Y1 C4 C3 41.27(18) . . . . ? N2 Y1 C4 C3 155.8(3) . . . . ? C2 Y1 C4 C3 21.16(17) . . . . ? Si2 Y1 C4 C3 -115.82(18) . . . . ? Si3 Y1 C4 C3 117.22(17) . . . . ? N3 Y1 C4 C5 46.6(6) . . . . ? N4 Y1 C4 C5 -117.9(6) . . . . ? N1 Y1 C4 C5 173.4(6) . . . . ? N2 Y1 C4 C5 -72.1(6) . . . . ? C2 Y1 C4 C5 153.3(6) . . . . ? Si2 Y1 C4 C5 16.3(6) . . . . ? Si3 Y1 C4 C5 -110.6(6) . . . . ? C2 N1 C6 C7 74.1(4) . . . . ? Y1 N1 C6 C7 -115.4(3) . . . . ? C2 N1 C6 C11 -107.9(3) . . . . ? Y1 N1 C6 C11 62.6(4) . . . . ? C11 C6 C7 C8 -0.4(5) . . . . ? N1 C6 C7 C8 177.6(3) . . . . ? C11 C6 C7 C12 179.9(3) . . . . ? N1 C6 C7 C12 -2.1(5) . . . . ? C6 C7 C8 C9 0.5(6) . . . . ? C12 C7 C8 C9 -179.8(4) . . . . ? C7 C8 C9 C10 -0.6(7) . . . . ? C8 C9 C10 C11 0.6(7) . . . . ? C9 C10 C11 C6 -0.5(6) . . . . ? C9 C10 C11 C13 179.2(4) . . . . ? C7 C6 C11 C10 0.4(5) . . . . ? N1 C6 C11 C10 -177.5(3) . . . . ? C7 C6 C11 C13 -179.3(3) . . . . ? N1 C6 C11 C13 2.8(5) . . . . ? C4 N2 C14 C16 73.9(4) . . . . ? Y1 N2 C14 C16 -86.0(4) . . . . ? C4 N2 C14 C15 -108.2(3) . . . . ? Y1 N2 C14 C15 91.9(3) . . . . ? C16 C14 C15 C14 -0.6(2) . . . 4_556 ? N2 C14 C15 C14 -178.6(3) . . . 4_556 ? C15 C14 C16 C17 1.2(4) . . . . ? N2 C14 C16 C17 179.1(2) . . . . ? C14 C16 C17 C16 -0.6(2) . . . 4_556 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.528 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.055 _database_code_depnum_ccdc_archive 'CCDC 952929' ####################################################################### # # 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_complex4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H108 N8 Si8 Y2' _chemical_formula_weight 1296.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.5762(8) _cell_length_b 20.4287(10) _cell_length_c 34.9745(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.853(6) _cell_angle_gamma 90.00 _cell_volume 7517.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2887 _cell_measurement_theta_min 3.4840 _cell_measurement_theta_max 25.0310 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 1.700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4549 _exptl_absorpt_correction_T_max 0.8484 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3818 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19022 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0987 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6980 _reflns_number_gt 4464 _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^)+(0.1206P)^2^+17.2690P] 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 6980 _refine_ls_number_parameters 300 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1340 _refine_ls_R_factor_gt 0.0843 _refine_ls_wR_factor_ref 0.2386 _refine_ls_wR_factor_gt 0.2142 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.227 _refine_ls_shift/su_max 0.006 _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 0.96197(6) 0.39030(3) 0.360568(19) 0.0326(3) Uani 1 1 d . . . N1 N 0.8506(6) 0.3267(3) 0.40057(16) 0.0371(15) Uani 1 1 d . . . N2 N 0.8664(6) 0.3179(3) 0.31639(16) 0.0364(14) Uani 1 1 d . . . N3 N 1.1727(6) 0.3789(3) 0.37190(18) 0.0407(16) Uani 1 1 d . . . N4 N 0.8908(6) 0.4883(3) 0.33919(17) 0.0422(16) Uani 1 1 d . . . Si1 Si 1.2891(3) 0.33844(19) 0.35117(10) 0.0879(10) Uani 1 1 d D . . H111 H 1.3553 0.3321 0.3726 0.132 Uiso 1 1 calc RD . . Si2 Si 1.2087(2) 0.42721(11) 0.41106(6) 0.0425(6) Uani 1 1 d D . . H112 H 1.1270 0.4454 0.4169 0.064 Uiso 1 1 calc RD . . Si3 Si 0.9752(3) 0.55608(12) 0.32972(8) 0.0570(7) Uani 1 1 d . . . Si4 Si 0.7291(3) 0.48622(13) 0.33256(7) 0.0568(7) Uani 1 1 d D . . H114 H 0.7042 0.4454 0.3445 0.085 Uiso 1 1 calc RD . . C1 C 0.6629(9) 0.2685(5) 0.4201(2) 0.063(3) Uani 1 1 d . . . H1A H 0.6881 0.2245 0.4269 0.094 Uiso 1 1 calc R . . H1B H 0.5752 0.2689 0.4098 0.094 Uiso 1 1 calc R . . H1C H 0.6739 0.2957 0.4426 0.094 Uiso 1 1 calc R . . C2 C 0.7431(8) 0.2941(4) 0.3906(2) 0.044(2) Uani 1 1 d . . . C3 C 0.6963(8) 0.2815(4) 0.3519(2) 0.045(2) Uani 1 1 d . . . H3 H 0.6134 0.2658 0.3485 0.054 Uiso 1 1 calc R . . C4 C 0.7531(8) 0.2887(4) 0.3184(2) 0.0395(18) Uani 1 1 d . . . C5 C 0.6789(9) 0.2630(5) 0.2818(2) 0.061(3) Uani 1 1 d . . . H5A H 0.6893 0.2924 0.2610 0.092 Uiso 1 1 calc R . . H5B H 0.5904 0.2599 0.2856 0.092 Uiso 1 1 calc R . . H5C H 0.7102 0.2205 0.2759 0.092 Uiso 1 1 calc R . . C6 C 0.8973(7) 0.3275(4) 0.4407(2) 0.041(2) Uani 1 1 d . . . C7 C 0.9806(9) 0.2767(4) 0.4550(2) 0.050(2) Uani 1 1 d . . . C8 C 1.0272(10) 0.2788(5) 0.4941(3) 0.062(3) Uani 1 1 d . . . H8 H 1.0798 0.2454 0.5044 0.075 Uiso 1 1 calc R . . C9 C 0.9967(9) 0.3287(5) 0.5170(2) 0.060(3) Uani 1 1 d . . . H9 H 1.0293 0.3291 0.5428 0.072 Uiso 1 1 calc R . . C10 C 0.9188(9) 0.3785(5) 0.5030(2) 0.060(3) Uani 1 1 d . . . H10 H 0.8999 0.4124 0.5193 0.072 Uiso 1 1 calc R . . C11 C 0.8668(8) 0.3795(4) 0.4644(2) 0.049(2) Uani 1 1 d . . . C12 C 1.0193(14) 0.2219(6) 0.4294(4) 0.105(3) Uani 1 1 d . . . H12 H 0.9922 0.2331 0.4025 0.126 Uiso 1 1 calc R . . C13 C 1.1577(13) 0.2077(6) 0.4333(4) 0.105(3) Uani 1 1 d . . . H13A H 1.2044 0.2481 0.4341 0.158 Uiso 1 1 calc R . . H13B H 1.1783 0.1821 0.4118 0.158 Uiso 1 1 calc R . . H13C H 1.1800 0.1837 0.4567 0.158 Uiso 1 1 calc R . . C14 C 0.9539(13) 0.1570(5) 0.4395(4) 0.105(3) Uani 1 1 d . . . H14A H 1.0176 0.1252 0.4479 0.158 Uiso 1 1 calc R . . H14B H 0.9031 0.1408 0.4172 0.158 Uiso 1 1 calc R . . H14C H 0.9007 0.1648 0.4597 0.158 Uiso 1 1 calc R . . C15 C 0.7804(11) 0.4358(6) 0.4497(4) 0.090(2) Uani 1 1 d . . . H15 H 0.7597 0.4307 0.4219 0.108 Uiso 1 1 calc R . . C16 C 0.6555(11) 0.4344(6) 0.4691(4) 0.090(2) Uani 1 1 d . . . H16A H 0.6741 0.4409 0.4963 0.134 Uiso 1 1 calc R . . H16B H 0.6145 0.3928 0.4645 0.134 Uiso 1 1 calc R . . H16C H 0.6001 0.4686 0.4586 0.134 Uiso 1 1 calc R . . C17 C 0.8397(11) 0.5022(6) 0.4574(4) 0.090(2) Uani 1 1 d . . . H17A H 0.8643 0.5069 0.4845 0.134 Uiso 1 1 calc R . . H17B H 0.7793 0.5356 0.4491 0.134 Uiso 1 1 calc R . . H17C H 0.9133 0.5063 0.4437 0.134 Uiso 1 1 calc R . . C18 C 0.9287(7) 0.3156(4) 0.28201(19) 0.0344(17) Uani 1 1 d . . . C19 C 0.9664(9) 0.2582(4) 0.2658(2) 0.049(2) Uani 1 1 d . . . H19 H 0.9458 0.2185 0.2766 0.059 Uiso 1 1 calc R . . C20 C 0.9647(8) 0.3730(4) 0.2658(2) 0.0426(19) Uani 1 1 d . . . H20 H 0.9416 0.4127 0.2761 0.051 Uiso 1 1 calc R . . C21 C 1.2544(11) 0.2572(6) 0.3348(3) 0.0879(10) Uani 1 1 d . . . H21A H 1.2204 0.2326 0.3547 0.132 Uiso 1 1 calc R . . H21B H 1.3309 0.2366 0.3282 0.132 Uiso 1 1 calc R . . H21C H 1.1932 0.2586 0.3125 0.132 Uiso 1 1 calc R . . C22 C 1.3676(11) 0.3870(6) 0.3176(3) 0.0879(10) Uani 1 1 d . . . H22A H 1.3051 0.4090 0.3003 0.132 Uiso 1 1 calc R . . H22B H 1.4182 0.3591 0.3031 0.132 Uiso 1 1 calc R . . H22C H 1.4213 0.4188 0.3313 0.132 Uiso 1 1 calc R . . C23 C 1.2751(9) 0.3866(5) 0.4563(3) 0.062(3) Uani 1 1 d . . . H23A H 1.2179 0.3529 0.4629 0.093 Uiso 1 1 calc R . . H23B H 1.2856 0.4184 0.4766 0.093 Uiso 1 1 calc R . . H23C H 1.3559 0.3675 0.4526 0.093 Uiso 1 1 calc R . . C24 C 1.3108(11) 0.4994(5) 0.4051(3) 0.082(4) Uani 1 1 d . . . H24A H 1.3962 0.4852 0.4027 0.124 Uiso 1 1 calc R . . H24B H 1.3103 0.5275 0.4270 0.124 Uiso 1 1 calc R . . H24C H 1.2790 0.5230 0.3823 0.124 Uiso 1 1 calc R . . C25 C 1.1207(9) 0.5390(5) 0.3057(3) 0.0568(7) Uani 1 1 d . . . H25A H 1.1696 0.5055 0.3196 0.085 Uiso 1 1 calc R . . H25B H 1.1706 0.5782 0.3052 0.085 Uiso 1 1 calc R . . H25C H 1.0968 0.5246 0.2798 0.085 Uiso 1 1 calc R . . C26 C 1.0137(9) 0.6078(4) 0.3728(3) 0.0568(7) Uani 1 1 d . . . H26A H 0.9365 0.6245 0.3814 0.085 Uiso 1 1 calc R . . H26B H 1.0663 0.6437 0.3665 0.085 Uiso 1 1 calc R . . H26C H 1.0582 0.5822 0.3928 0.085 Uiso 1 1 calc R . . C27 C 0.6624(10) 0.4815(7) 0.2818(3) 0.089(4) Uani 1 1 d . . . H27A H 0.6919 0.5180 0.2679 0.133 Uiso 1 1 calc R . . H27B H 0.5713 0.4824 0.2804 0.133 Uiso 1 1 calc R . . H27C H 0.6893 0.4414 0.2707 0.133 Uiso 1 1 calc R . . C28 C 0.6462(11) 0.5530(5) 0.3564(3) 0.082(3) Uani 1 1 d . . . H28A H 0.6695 0.5514 0.3836 0.123 Uiso 1 1 calc R . . H28B H 0.5559 0.5474 0.3512 0.123 Uiso 1 1 calc R . . H28C H 0.6704 0.5945 0.3465 0.123 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 0.0334(4) 0.0346(4) 0.0303(4) -0.0010(3) 0.0059(3) -0.0100(3) N1 0.039(4) 0.046(4) 0.027(3) -0.002(3) 0.005(3) -0.019(3) N2 0.046(4) 0.034(3) 0.030(3) 0.001(3) 0.004(3) -0.008(3) N3 0.037(4) 0.043(4) 0.044(4) -0.004(3) 0.011(3) -0.008(3) N4 0.047(4) 0.039(4) 0.039(4) -0.008(3) 0.001(3) -0.001(3) Si1 0.073(2) 0.102(2) 0.095(2) -0.0239(19) 0.0386(17) 0.0063(17) Si2 0.0360(13) 0.0456(14) 0.0457(13) -0.0028(11) 0.0032(9) -0.0097(10) Si3 0.0671(18) 0.0467(14) 0.0580(16) -0.0047(12) 0.0105(13) -0.0054(12) Si4 0.0578(16) 0.0576(15) 0.0540(14) -0.0013(12) 0.0008(11) 0.0010(12) C1 0.062(6) 0.085(7) 0.042(5) -0.005(5) 0.012(4) -0.044(5) C2 0.048(5) 0.050(5) 0.034(4) 0.001(4) 0.010(3) -0.019(4) C3 0.043(5) 0.056(5) 0.036(4) -0.002(4) 0.006(4) -0.025(4) C4 0.048(5) 0.036(4) 0.032(4) 0.001(3) -0.007(3) -0.014(4) C5 0.060(6) 0.078(7) 0.044(5) -0.012(5) 0.002(4) -0.023(5) C6 0.043(5) 0.055(5) 0.026(4) 0.004(4) 0.007(3) -0.027(4) C7 0.069(6) 0.045(5) 0.034(4) 0.006(4) -0.006(4) -0.023(4) C8 0.077(7) 0.061(6) 0.046(5) 0.014(5) -0.010(5) -0.021(5) C9 0.065(6) 0.088(7) 0.026(4) 0.005(5) 0.001(4) -0.035(6) C10 0.060(6) 0.086(7) 0.034(4) -0.011(5) 0.011(4) -0.023(5) C11 0.045(5) 0.070(6) 0.033(4) -0.013(4) 0.010(3) -0.017(4) C12 0.122(6) 0.055(4) 0.137(7) -0.014(4) 0.004(6) -0.014(4) C13 0.122(6) 0.055(4) 0.137(7) -0.014(4) 0.004(6) -0.014(4) C14 0.122(6) 0.055(4) 0.137(7) -0.014(4) 0.004(6) -0.014(4) C15 0.065(4) 0.100(5) 0.103(5) -0.020(4) 0.006(4) 0.014(4) C16 0.065(4) 0.100(5) 0.103(5) -0.020(4) 0.006(4) 0.014(4) C17 0.065(4) 0.100(5) 0.103(5) -0.020(4) 0.006(4) 0.014(4) C18 0.040(4) 0.037(4) 0.025(4) -0.001(3) -0.002(3) -0.002(3) C19 0.074(6) 0.030(4) 0.047(5) 0.003(4) 0.018(4) -0.004(4) C20 0.066(6) 0.031(4) 0.033(4) -0.004(3) 0.016(4) 0.003(4) C21 0.073(2) 0.102(2) 0.095(2) -0.0239(19) 0.0386(17) 0.0063(17) C22 0.073(2) 0.102(2) 0.095(2) -0.0239(19) 0.0386(17) 0.0063(17) C23 0.058(6) 0.073(7) 0.054(6) 0.000(5) -0.006(4) -0.013(5) C24 0.083(8) 0.077(7) 0.081(7) 0.008(6) -0.018(6) -0.041(6) C25 0.0578(16) 0.0576(15) 0.0540(14) -0.0013(12) 0.0008(11) 0.0010(12) C26 0.0578(16) 0.0576(15) 0.0540(14) -0.0013(12) 0.0008(11) 0.0010(12) C27 0.059(7) 0.144(12) 0.059(6) 0.011(7) -0.016(5) 0.002(7) C28 0.070(7) 0.078(7) 0.100(9) -0.005(6) 0.021(6) 0.018(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. The H atom bound to Si3 could not be located despite many efforts. ; 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 2.236(6) . ? Y1 N4 2.239(6) . ? Y1 N2 2.298(6) . ? Y1 N1 2.317(6) . ? N1 C2 1.334(9) . ? N1 C6 1.439(9) . ? N2 C4 1.347(9) . ? N2 C18 1.430(9) . ? N3 Si2 1.699(7) . ? N3 Si1 1.705(7) . ? N4 Si3 1.699(7) . ? N4 Si4 1.703(7) . ? Si1 C21 1.783(12) . ? Si1 C22 1.804(12) . ? Si1 H111 0.9800 . ? Si2 C24 1.853(10) . ? Si2 C23 1.859(9) . ? Si2 H112 0.9800 . ? Si3 C26 1.851(9) . ? Si3 C25 1.859(9) . ? Si4 C27 1.844(10) . ? Si4 C28 1.863(10) . ? Si4 H114 0.9800 . ? C1 C2 1.496(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.416(10) . ? C3 C4 1.378(10) . ? C3 H3 0.9300 . ? C4 C5 1.523(10) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C11 1.405(11) . ? C6 C7 1.419(12) . ? C7 C8 1.408(11) . ? C7 C12 1.515(15) . ? C8 C9 1.355(13) . ? C8 H8 0.9300 . ? C9 C10 1.370(13) . ? C9 H9 0.9300 . ? C10 C11 1.405(12) . ? C10 H10 0.9300 . ? C11 C15 1.525(14) . ? C12 C13 1.485(17) . ? C12 C14 1.554(16) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C17 1.507(16) . ? C15 C16 1.546(16) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C20 1.372(10) . ? C18 C19 1.379(10) . ? C19 C19 1.374(16) 2_755 ? C19 H19 0.9300 . ? C20 C20 1.398(15) 2_755 ? C20 H20 0.9300 . ? 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 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? 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 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? 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 N4 116.6(2) . . ? N3 Y1 N2 114.5(2) . . ? N4 Y1 N2 103.9(2) . . ? N3 Y1 N1 113.2(2) . . ? N4 Y1 N1 121.9(2) . . ? N2 Y1 N1 80.2(2) . . ? C2 N1 C6 117.4(6) . . ? C2 N1 Y1 126.4(5) . . ? C6 N1 Y1 115.9(4) . . ? C4 N2 C18 121.2(6) . . ? C4 N2 Y1 125.7(5) . . ? C18 N2 Y1 112.1(4) . . ? Si2 N3 Si1 120.8(4) . . ? Si2 N3 Y1 102.7(3) . . ? Si1 N3 Y1 136.5(4) . . ? Si3 N4 Si4 122.3(4) . . ? Si3 N4 Y1 128.9(4) . . ? Si4 N4 Y1 108.8(3) . . ? N3 Si1 C21 117.1(4) . . ? N3 Si1 C22 114.2(5) . . ? C21 Si1 C22 113.3(5) . . ? N3 Si1 H111 103.3 . . ? C21 Si1 H111 103.3 . . ? C22 Si1 H111 103.3 . . ? N3 Si2 C24 117.1(4) . . ? N3 Si2 C23 117.4(4) . . ? C24 Si2 C23 106.1(4) . . ? N3 Si2 H112 104.9 . . ? C24 Si2 H112 104.9 . . ? C23 Si2 H112 104.9 . . ? N4 Si3 C26 112.5(4) . . ? N4 Si3 C25 114.3(4) . . ? C26 Si3 C25 110.6(4) . . ? N4 Si4 C27 114.4(4) . . ? N4 Si4 C28 115.7(4) . . ? C27 Si4 C28 108.5(6) . . ? N4 Si4 H114 105.8 . . ? C27 Si4 H114 105.8 . . ? C28 Si4 H114 105.8 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.2(6) . . ? N1 C2 C1 121.4(7) . . ? C3 C2 C1 115.4(7) . . ? C4 C3 C2 130.8(7) . . ? C4 C3 H3 114.6 . . ? C2 C3 H3 114.6 . . ? N2 C4 C3 123.9(7) . . ? N2 C4 C5 119.6(7) . . ? C3 C4 C5 116.5(7) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 121.2(7) . . ? C11 C6 N1 120.5(7) . . ? C7 C6 N1 118.3(7) . . ? C8 C7 C6 117.6(8) . . ? C8 C7 C12 120.6(10) . . ? C6 C7 C12 121.9(8) . . ? C9 C8 C7 121.2(9) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 121.1(8) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C9 C10 C11 121.2(9) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C6 C11 C10 117.7(9) . . ? C6 C11 C15 122.5(8) . . ? C10 C11 C15 119.8(9) . . ? C13 C12 C7 114.4(10) . . ? C13 C12 C14 105.6(11) . . ? C7 C12 C14 110.0(11) . . ? C13 C12 H12 108.9 . . ? C7 C12 H12 108.9 . . ? C14 C12 H12 108.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C11 113.2(10) . . ? C17 C15 C16 107.3(10) . . ? C11 C15 C16 110.3(10) . . ? C17 C15 H15 108.6 . . ? C11 C15 H15 108.6 . . ? C16 C15 H15 108.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 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 . . ? C20 C18 C19 116.9(7) . . ? C20 C18 N2 119.4(7) . . ? C19 C18 N2 123.4(7) . . ? C19 C19 C18 121.7(4) 2_755 . ? C19 C19 H19 119.1 2_755 . ? C18 C19 H19 119.1 . . ? C18 C20 C20 121.3(4) . 2_755 ? C18 C20 H20 119.3 . . ? C20 C20 H20 119.3 2_755 . ? Si1 C21 H21A 109.5 . . ? Si1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si2 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si3 C26 H26A 109.5 . . ? Si3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si4 C27 H27A 109.5 . . ? Si4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? 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 N3 Y1 N1 C2 -140.2(7) . . . . ? N4 Y1 N1 C2 72.7(7) . . . . ? N2 Y1 N1 C2 -27.7(7) . . . . ? N3 Y1 N1 C6 45.4(6) . . . . ? N4 Y1 N1 C6 -101.7(6) . . . . ? N2 Y1 N1 C6 157.9(6) . . . . ? N3 Y1 N2 C4 141.6(6) . . . . ? N4 Y1 N2 C4 -90.1(6) . . . . ? N1 Y1 N2 C4 30.5(6) . . . . ? N3 Y1 N2 C18 -49.5(5) . . . . ? N4 Y1 N2 C18 78.8(5) . . . . ? N1 Y1 N2 C18 -160.6(5) . . . . ? N4 Y1 N3 Si2 69.3(4) . . . . ? N2 Y1 N3 Si2 -169.1(3) . . . . ? N1 Y1 N3 Si2 -79.6(3) . . . . ? N4 Y1 N3 Si1 -108.9(5) . . . . ? N2 Y1 N3 Si1 12.7(6) . . . . ? N1 Y1 N3 Si1 102.1(5) . . . . ? N3 Y1 N4 Si3 0.7(5) . . . . ? N2 Y1 N4 Si3 -126.2(4) . . . . ? N1 Y1 N4 Si3 146.8(4) . . . . ? N3 Y1 N4 Si4 -179.9(3) . . . . ? N2 Y1 N4 Si4 53.1(3) . . . . ? N1 Y1 N4 Si4 -33.9(4) . . . . ? Si2 N3 Si1 C21 140.4(6) . . . . ? Y1 N3 Si1 C21 -41.6(8) . . . . ? Si2 N3 Si1 C22 -83.8(6) . . . . ? Y1 N3 Si1 C22 94.2(7) . . . . ? Si1 N3 Si2 C24 62.7(6) . . . . ? Y1 N3 Si2 C24 -115.9(5) . . . . ? Si1 N3 Si2 C23 -65.4(6) . . . . ? Y1 N3 Si2 C23 116.0(4) . . . . ? Si4 N4 Si3 C26 94.0(5) . . . . ? Y1 N4 Si3 C26 -86.8(5) . . . . ? Si4 N4 Si3 C25 -138.8(4) . . . . ? Y1 N4 Si3 C25 40.4(6) . . . . ? Si3 N4 Si4 C27 74.3(6) . . . . ? Y1 N4 Si4 C27 -105.0(5) . . . . ? Si3 N4 Si4 C28 -52.8(6) . . . . ? Y1 N4 Si4 C28 127.8(5) . . . . ? C6 N1 C2 C3 -170.8(8) . . . . ? Y1 N1 C2 C3 14.9(12) . . . . ? C6 N1 C2 C1 9.7(12) . . . . ? Y1 N1 C2 C1 -164.6(7) . . . . ? N1 C2 C3 C4 11.6(15) . . . . ? C1 C2 C3 C4 -168.8(9) . . . . ? C18 N2 C4 C3 171.0(8) . . . . ? Y1 N2 C4 C3 -21.0(11) . . . . ? C18 N2 C4 C5 -10.7(11) . . . . ? Y1 N2 C4 C5 157.3(6) . . . . ? C2 C3 C4 N2 -8.3(15) . . . . ? C2 C3 C4 C5 173.4(9) . . . . ? C2 N1 C6 C11 -94.4(9) . . . . ? Y1 N1 C6 C11 80.6(8) . . . . ? C2 N1 C6 C7 89.2(9) . . . . ? Y1 N1 C6 C7 -95.8(7) . . . . ? C11 C6 C7 C8 2.6(11) . . . . ? N1 C6 C7 C8 178.9(7) . . . . ? C11 C6 C7 C12 -177.2(9) . . . . ? N1 C6 C7 C12 -0.8(12) . . . . ? C6 C7 C8 C9 -2.0(13) . . . . ? C12 C7 C8 C9 177.8(9) . . . . ? C7 C8 C9 C10 0.5(14) . . . . ? C8 C9 C10 C11 0.5(14) . . . . ? C7 C6 C11 C10 -1.6(11) . . . . ? N1 C6 C11 C10 -177.9(7) . . . . ? C7 C6 C11 C15 178.4(8) . . . . ? N1 C6 C11 C15 2.1(12) . . . . ? C9 C10 C11 C6 0.1(12) . . . . ? C9 C10 C11 C15 -180.0(9) . . . . ? C8 C7 C12 C13 -46.6(15) . . . . ? C6 C7 C12 C13 133.1(11) . . . . ? C8 C7 C12 C14 72.0(13) . . . . ? C6 C7 C12 C14 -108.3(12) . . . . ? C6 C11 C15 C17 -126.2(10) . . . . ? C10 C11 C15 C17 53.9(13) . . . . ? C6 C11 C15 C16 113.6(10) . . . . ? C10 C11 C15 C16 -66.3(12) . . . . ? C4 N2 C18 C20 125.3(8) . . . . ? Y1 N2 C18 C20 -44.1(8) . . . . ? C4 N2 C18 C19 -61.1(10) . . . . ? Y1 N2 C18 C19 129.4(7) . . . . ? C20 C18 C19 C19 -1.9(15) . . . 2_755 ? N2 C18 C19 C19 -175.6(10) . . . 2_755 ? C19 C18 C20 C20 0.5(15) . . . 2_755 ? N2 C18 C20 C20 174.5(9) . . . 2_755 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.587 _refine_diff_density_min -2.061 _refine_diff_density_rms 0.112 _database_code_depnum_ccdc_archive 'CCDC 952930' ####################################################################### # # 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_complex6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H65 N4 Si4 Y' _chemical_formula_sum 'C35 H65 N4 Si4 Y' _chemical_formula_weight 743.18 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' 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 orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 20.0835(9) _cell_length_b 20.5924(12) _cell_length_c 20.6268(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8530.6(8) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 20411 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 1.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.534 _exptl_absorpt_correction_T_max 0.745 _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 25980 _diffrn_reflns_av_R_equivalents 0.0738 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7897 _reflns_number_gt 5961 _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^)+(0.0330P)^2^+4.6202P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7897 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1245 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _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 0.28560(2) 0.60549(2) 0.404122(19) 0.03725(14) Uani 1 1 d . . . Si1 Si 0.22726(7) 0.62901(7) 0.55166(6) 0.0505(4) Uani 1 1 d . . . Si2 Si 0.37561(8) 0.62098(7) 0.55285(7) 0.0548(4) Uani 1 1 d . . . Si3 Si 0.38593(7) 0.71476(7) 0.35227(7) 0.0487(4) Uani 1 1 d . . . Si4 Si 0.42945(7) 0.58284(8) 0.30584(7) 0.0506(4) Uani 1 1 d . . . N1 N 0.23529(17) 0.50481(18) 0.39048(16) 0.0383(9) Uani 1 1 d . . . N2 N 0.20610(16) 0.63307(18) 0.32507(16) 0.0381(9) Uani 1 1 d . . . N3 N 0.30103(18) 0.61476(18) 0.51202(16) 0.0434(9) Uani 1 1 d . . . N4 N 0.37855(16) 0.63197(18) 0.35170(16) 0.0412(9) Uani 1 1 d . . . C1 C 0.2449(3) 0.4179(3) 0.3081(2) 0.0651(15) Uani 1 1 d . . . H1A H 0.2192 0.3921 0.3385 0.098 Uiso 1 1 calc R . . H1B H 0.2906 0.4027 0.3077 0.098 Uiso 1 1 calc R . . H1C H 0.2259 0.4138 0.2651 0.098 Uiso 1 1 calc R . . C2 C 0.2432(2) 0.4884(2) 0.3288(2) 0.0434(11) Uani 1 1 d . . . C3 C 0.2496(2) 0.5345(2) 0.2780(2) 0.0434(11) Uani 1 1 d . . . H3 H 0.2754 0.5210 0.2424 0.052 Uiso 1 1 calc R . . C4 C 0.2229(2) 0.5975(2) 0.2734(2) 0.0408(11) Uani 1 1 d . . . C5 C 0.2117(2) 0.6207(3) 0.2047(2) 0.0550(14) Uani 1 1 d . . . H5A H 0.1652 0.6326 0.1992 0.082 Uiso 1 1 calc R . . H5B H 0.2230 0.5863 0.1746 0.082 Uiso 1 1 calc R . . H5C H 0.2395 0.6583 0.1963 0.082 Uiso 1 1 calc R . . C6 C 0.2047(2) 0.4586(2) 0.4344(2) 0.0423(11) Uani 1 1 d . . . C7 C 0.2434(2) 0.4220(2) 0.4775(2) 0.0423(11) Uani 1 1 d . . . C8 C 0.2099(3) 0.3834(2) 0.5227(2) 0.0520(13) Uani 1 1 d . . . H8 H 0.2348 0.3588 0.5524 0.062 Uiso 1 1 calc R . . C9 C 0.1416(3) 0.3802(2) 0.5248(2) 0.0525(13) Uani 1 1 d . . . H9 H 0.1203 0.3549 0.5565 0.063 Uiso 1 1 calc R . . C10 C 0.1048(3) 0.4142(3) 0.4804(2) 0.0544(13) Uani 1 1 d . . . H10 H 0.0581 0.4101 0.4807 0.065 Uiso 1 1 calc R . . C11 C 0.1346(2) 0.4548(2) 0.4347(2) 0.0475(12) Uani 1 1 d . . . C12 C 0.3183(2) 0.4199(3) 0.4758(2) 0.0500(13) Uani 1 1 d . . . H12 H 0.3334 0.4551 0.4467 0.060 Uiso 1 1 calc R . . C13 C 0.3494(3) 0.4318(3) 0.5419(2) 0.0681(16) Uani 1 1 d . . . H13A H 0.3299 0.4703 0.5611 0.102 Uiso 1 1 calc R . . H13B H 0.3970 0.4379 0.5370 0.102 Uiso 1 1 calc R . . H13C H 0.3412 0.3947 0.5697 0.102 Uiso 1 1 calc R . . C14 C 0.3450(3) 0.3559(3) 0.4486(3) 0.086(2) Uani 1 1 d . . . H14A H 0.3328 0.3206 0.4773 0.128 Uiso 1 1 calc R . . H14B H 0.3931 0.3582 0.4452 0.128 Uiso 1 1 calc R . . H14C H 0.3260 0.3483 0.4060 0.128 Uiso 1 1 calc R . . C15 C 0.0913(2) 0.4913(3) 0.3858(2) 0.0553(13) Uani 1 1 d . . . H15 H 0.1193 0.5252 0.3654 0.066 Uiso 1 1 calc R . . C16 C 0.0324(2) 0.5255(3) 0.4193(2) 0.0636(15) Uani 1 1 d . . . H16A H 0.0014 0.4932 0.4354 0.095 Uiso 1 1 calc R . . H16B H 0.0100 0.5535 0.3883 0.095 Uiso 1 1 calc R . . H16C H 0.0488 0.5515 0.4552 0.095 Uiso 1 1 calc R . . C17 C 0.0657(3) 0.4470(3) 0.3322(3) 0.090(2) Uani 1 1 d . . . H17A H 0.1031 0.4266 0.3105 0.135 Uiso 1 1 calc R . . H17B H 0.0404 0.4723 0.3012 0.135 Uiso 1 1 calc R . . H17C H 0.0373 0.4138 0.3508 0.135 Uiso 1 1 calc R . . C18 C 0.1607(2) 0.6864(2) 0.3145(2) 0.0414(11) Uani 1 1 d . . . C19 C 0.0965(2) 0.6800(2) 0.3388(2) 0.0489(12) Uani 1 1 d . . . H19 H 0.0843 0.6419 0.3610 0.059 Uiso 1 1 calc R . . C20 C 0.0504(3) 0.7293(3) 0.3306(3) 0.0624(15) Uani 1 1 d . . . H20 H 0.0071 0.7244 0.3472 0.075 Uiso 1 1 calc R . . C21 C 0.0673(3) 0.7849(3) 0.2983(3) 0.0616(15) Uani 1 1 d . . . H21 H 0.0358 0.8182 0.2927 0.074 Uiso 1 1 calc R . . C22 C 0.1307(3) 0.7917(3) 0.2744(2) 0.0607(14) Uani 1 1 d . . . H22 H 0.1421 0.8297 0.2516 0.073 Uiso 1 1 calc R . . C23 C 0.1780(2) 0.7437(2) 0.2832(2) 0.0506(13) Uani 1 1 d . . . H23 H 0.2217 0.7498 0.2680 0.061 Uiso 1 1 calc R . . C24 C 0.1629(2) 0.6444(3) 0.4874(2) 0.0603(15) Uani 1 1 d . . . H24A H 0.1756 0.6822 0.4621 0.090 Uiso 1 1 calc R . . H24B H 0.1201 0.6522 0.5077 0.090 Uiso 1 1 calc R . . H24C H 0.1597 0.6069 0.4592 0.090 Uiso 1 1 calc R . . C25 C 0.2273(3) 0.7034(3) 0.6051(2) 0.0724(17) Uani 1 1 d . . . H25A H 0.2560 0.6960 0.6422 0.109 Uiso 1 1 calc R . . H25B H 0.1823 0.7120 0.6199 0.109 Uiso 1 1 calc R . . H25C H 0.2436 0.7403 0.5806 0.109 Uiso 1 1 calc R . . C26 C 0.1962(3) 0.5598(3) 0.6015(3) 0.0752(17) Uani 1 1 d . . . H26A H 0.1893 0.5223 0.5739 0.113 Uiso 1 1 calc R . . H26B H 0.1544 0.5718 0.6218 0.113 Uiso 1 1 calc R . . H26C H 0.2287 0.5494 0.6347 0.113 Uiso 1 1 calc R . . C27 C 0.4441(3) 0.5803(3) 0.5066(2) 0.0685(16) Uani 1 1 d . . . H27A H 0.4310 0.5362 0.4962 0.103 Uiso 1 1 calc R . . H27B H 0.4842 0.5796 0.5329 0.103 Uiso 1 1 calc R . . H27C H 0.4526 0.6042 0.4669 0.103 Uiso 1 1 calc R . . C28 C 0.3749(3) 0.5856(3) 0.6371(2) 0.0762(18) Uani 1 1 d . . . H28A H 0.3457 0.6111 0.6645 0.114 Uiso 1 1 calc R . . H28B H 0.4196 0.5863 0.6547 0.114 Uiso 1 1 calc R . . H28C H 0.3590 0.5411 0.6353 0.114 Uiso 1 1 calc R . . C29 C 0.4021(3) 0.7069(3) 0.5656(3) 0.0802(18) Uani 1 1 d . . . H29A H 0.4014 0.7298 0.5244 0.120 Uiso 1 1 calc R . . H29B H 0.4469 0.7077 0.5832 0.120 Uiso 1 1 calc R . . H29C H 0.3719 0.7279 0.5956 0.120 Uiso 1 1 calc R . . C30 C 0.3139(2) 0.7481(2) 0.4015(2) 0.0494(12) Uani 1 1 d . . . H30A H 0.2722 0.7377 0.3800 0.074 Uiso 1 1 calc R . . H30B H 0.3182 0.7949 0.4053 0.074 Uiso 1 1 calc R . . H30C H 0.3143 0.7288 0.4444 0.074 Uiso 1 1 calc R . . C31 C 0.3798(3) 0.7532(3) 0.2700(2) 0.0675(16) Uani 1 1 d . . . H31A H 0.4194 0.7430 0.2451 0.101 Uiso 1 1 calc R . . H31B H 0.3760 0.7999 0.2747 0.101 Uiso 1 1 calc R . . H31C H 0.3409 0.7366 0.2477 0.101 Uiso 1 1 calc R . . C32 C 0.4646(3) 0.7463(3) 0.3900(3) 0.0730(17) Uani 1 1 d . . . H32A H 0.4760 0.7198 0.4273 0.110 Uiso 1 1 calc R . . H32B H 0.4580 0.7909 0.4038 0.110 Uiso 1 1 calc R . . H32C H 0.5004 0.7445 0.3586 0.110 Uiso 1 1 calc R . . C33 C 0.4229(3) 0.4959(3) 0.3321(3) 0.0643(15) Uani 1 1 d . . . H33A H 0.4337 0.4925 0.3778 0.096 Uiso 1 1 calc R . . H33B H 0.4537 0.4696 0.3071 0.096 Uiso 1 1 calc R . . H33C H 0.3778 0.4806 0.3251 0.096 Uiso 1 1 calc R . . C34 C 0.4088(3) 0.5863(3) 0.2172(2) 0.0625(15) Uani 1 1 d . . . H34A H 0.3608 0.5857 0.2117 0.094 Uiso 1 1 calc R . . H34B H 0.4281 0.5491 0.1954 0.094 Uiso 1 1 calc R . . H34C H 0.4267 0.6259 0.1987 0.094 Uiso 1 1 calc R . . C35 C 0.5200(2) 0.6038(3) 0.3137(3) 0.0692(16) Uani 1 1 d . . . H35A H 0.5275 0.6473 0.2972 0.104 Uiso 1 1 calc R . . H35B H 0.5463 0.5730 0.2891 0.104 Uiso 1 1 calc R . . H35C H 0.5329 0.6019 0.3590 0.104 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 0.0436(2) 0.0387(3) 0.0295(2) 0.00002(19) -0.00092(19) 0.0024(2) Si1 0.0701(9) 0.0498(9) 0.0316(7) -0.0025(6) 0.0041(6) 0.0032(7) Si2 0.0714(9) 0.0506(10) 0.0425(8) -0.0006(7) -0.0168(7) 0.0030(8) Si3 0.0487(8) 0.0478(9) 0.0496(8) 0.0042(7) -0.0002(6) 0.0000(7) Si4 0.0466(7) 0.0575(10) 0.0477(8) 0.0014(7) 0.0068(6) 0.0087(7) N1 0.049(2) 0.036(2) 0.030(2) -0.0011(16) 0.0032(16) -0.0019(17) N2 0.044(2) 0.041(2) 0.029(2) 0.0000(17) 0.0010(16) 0.0069(18) N3 0.056(2) 0.041(2) 0.033(2) 0.0020(17) -0.0039(17) 0.0021(19) N4 0.042(2) 0.042(2) 0.039(2) 0.0004(18) 0.0003(17) 0.0030(18) C1 0.097(4) 0.049(4) 0.050(3) -0.008(3) 0.010(3) 0.005(3) C2 0.050(3) 0.042(3) 0.038(3) -0.004(2) 0.000(2) 0.002(2) C3 0.049(3) 0.046(3) 0.035(3) -0.001(2) 0.003(2) 0.003(2) C4 0.041(2) 0.049(3) 0.032(2) 0.008(2) -0.001(2) -0.003(2) C5 0.068(3) 0.064(4) 0.032(3) 0.003(2) -0.002(2) 0.003(3) C6 0.059(3) 0.037(3) 0.031(2) -0.003(2) 0.004(2) 0.003(2) C7 0.058(3) 0.037(3) 0.032(2) 0.000(2) 0.003(2) 0.001(2) C8 0.069(3) 0.047(3) 0.040(3) 0.003(2) 0.004(3) 0.003(3) C9 0.076(4) 0.036(3) 0.046(3) 0.006(2) 0.015(3) -0.005(3) C10 0.057(3) 0.050(3) 0.056(3) 0.003(3) 0.014(3) -0.006(3) C11 0.058(3) 0.040(3) 0.044(3) 0.000(2) 0.005(2) 0.005(2) C12 0.064(3) 0.049(3) 0.037(3) 0.011(2) 0.001(2) -0.003(3) C13 0.075(4) 0.073(4) 0.056(4) -0.002(3) -0.011(3) 0.004(3) C14 0.071(4) 0.099(6) 0.087(4) -0.034(4) 0.007(3) 0.015(4) C15 0.052(3) 0.056(4) 0.058(3) 0.013(3) 0.003(3) 0.008(3) C16 0.054(3) 0.063(4) 0.074(4) 0.017(3) 0.004(3) 0.007(3) C17 0.107(5) 0.094(6) 0.069(4) -0.003(4) -0.017(4) 0.016(4) C18 0.048(3) 0.045(3) 0.031(2) -0.006(2) -0.009(2) 0.004(2) C19 0.045(3) 0.051(3) 0.050(3) -0.003(2) -0.001(2) 0.009(2) C20 0.050(3) 0.066(4) 0.072(4) -0.014(3) -0.007(3) 0.008(3) C21 0.062(4) 0.048(4) 0.074(4) -0.010(3) -0.019(3) 0.016(3) C22 0.075(4) 0.039(3) 0.068(4) 0.004(3) -0.014(3) -0.003(3) C23 0.050(3) 0.050(3) 0.051(3) 0.007(3) -0.009(2) 0.000(3) C24 0.059(3) 0.073(4) 0.049(3) -0.008(3) 0.003(3) 0.011(3) C25 0.100(4) 0.065(4) 0.052(3) -0.019(3) 0.006(3) 0.005(3) C26 0.100(4) 0.069(4) 0.057(4) 0.013(3) 0.016(3) -0.002(4) C27 0.066(3) 0.075(4) 0.064(4) 0.008(3) -0.012(3) 0.010(3) C28 0.107(5) 0.073(4) 0.048(3) -0.003(3) -0.022(3) 0.016(4) C29 0.099(5) 0.067(4) 0.074(4) -0.007(3) -0.032(3) -0.013(4) C30 0.059(3) 0.044(3) 0.045(3) 0.003(2) -0.003(2) 0.004(2) C31 0.084(4) 0.061(4) 0.057(3) 0.018(3) 0.017(3) 0.008(3) C32 0.061(3) 0.064(4) 0.095(4) -0.001(3) -0.004(3) -0.009(3) C33 0.068(3) 0.057(4) 0.067(4) 0.004(3) 0.010(3) 0.019(3) C34 0.070(3) 0.071(4) 0.047(3) -0.004(3) 0.013(3) 0.008(3) C35 0.046(3) 0.088(5) 0.074(4) 0.012(3) 0.006(3) 0.011(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 2.225(3) . ? Y1 N3 2.255(3) . ? Y1 N1 2.323(4) . ? Y1 N2 2.352(3) . ? Y1 C4 2.980(4) . ? Y1 C2 2.993(5) . ? Y1 Si3 3.2043(15) . ? Y1 Si1 3.2969(13) . ? Si1 N3 1.717(4) . ? Si1 C26 1.864(5) . ? Si1 C24 1.879(5) . ? Si1 C25 1.886(5) . ? Si2 N3 1.723(4) . ? Si2 C29 1.867(6) . ? Si2 C27 1.871(5) . ? Si2 C28 1.884(5) . ? Si3 N4 1.711(4) . ? Si3 C31 1.876(5) . ? Si3 C32 1.877(5) . ? Si3 C30 1.897(5) . ? Si4 N4 1.721(4) . ? Si4 C33 1.875(5) . ? Si4 C35 1.876(5) . ? Si4 C34 1.877(5) . ? N1 C2 1.327(5) . ? N1 C6 1.450(6) . ? N2 C4 1.337(5) . ? N2 C18 1.444(5) . ? C1 C2 1.513(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C3 1.418(6) . ? C3 C4 1.408(6) . ? C3 H3 0.9400 . ? C4 C5 1.512(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.400(6) . ? C6 C11 1.410(6) . ? C7 C8 1.399(6) . ? C7 C12 1.505(6) . ? C8 C9 1.374(6) . ? C8 H8 0.9400 . ? C9 C10 1.370(6) . ? C9 H9 0.9400 . ? C10 C11 1.395(6) . ? C10 H10 0.9400 . ? C11 C15 1.529(6) . ? C12 C13 1.519(6) . ? C12 C14 1.529(7) . ? C12 H12 0.9900 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C17 1.524(7) . ? C15 C16 1.540(7) . ? C15 H15 0.9900 . ? 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 1.388(6) . ? C18 C23 1.389(6) . ? C19 C20 1.385(6) . ? C19 H19 0.9400 . ? C20 C21 1.367(7) . ? C20 H20 0.9400 . ? C21 C22 1.374(7) . ? C21 H21 0.9400 . ? C22 C23 1.384(7) . ? C22 H22 0.9400 . ? C23 H23 0.9400 . ? 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 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 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 N4 Y1 N3 110.09(13) . . ? N4 Y1 N1 121.65(13) . . ? N3 Y1 N1 104.76(13) . . ? N4 Y1 N2 99.99(12) . . ? N3 Y1 N2 139.21(13) . . ? N1 Y1 N2 80.58(12) . . ? N4 Y1 C4 85.89(12) . . ? N3 Y1 C4 162.85(12) . . ? N1 Y1 C4 69.97(12) . . ? N2 Y1 C4 25.74(12) . . ? N4 Y1 C2 100.60(13) . . ? N3 Y1 C2 128.31(13) . . ? N1 Y1 C2 25.09(11) . . ? N2 Y1 C2 68.97(13) . . ? C4 Y1 C2 50.61(13) . . ? N4 Y1 Si3 30.47(10) . . ? N3 Y1 Si3 100.58(10) . . ? N1 Y1 Si3 149.28(9) . . ? N2 Y1 Si3 91.48(9) . . ? C4 Y1 Si3 90.14(9) . . ? C2 Y1 Si3 124.85(9) . . ? N4 Y1 Si1 135.29(9) . . ? N3 Y1 Si1 29.00(10) . . ? N1 Y1 Si1 95.07(9) . . ? N2 Y1 Si1 111.30(8) . . ? C4 Y1 Si1 133.88(9) . . ? C2 Y1 Si1 119.78(9) . . ? Si3 Y1 Si1 115.37(4) . . ? N3 Si1 C26 114.9(2) . . ? N3 Si1 C24 106.67(19) . . ? C26 Si1 C24 106.7(3) . . ? N3 Si1 C25 114.6(2) . . ? C26 Si1 C25 107.4(3) . . ? C24 Si1 C25 106.0(3) . . ? N3 Si1 Y1 39.54(12) . . ? C26 Si1 Y1 121.03(19) . . ? C24 Si1 Y1 67.56(15) . . ? C25 Si1 Y1 131.17(19) . . ? N3 Si2 C29 112.8(2) . . ? N3 Si2 C27 110.9(2) . . ? C29 Si2 C27 106.6(3) . . ? N3 Si2 C28 114.5(2) . . ? C29 Si2 C28 103.9(3) . . ? C27 Si2 C28 107.6(3) . . ? N4 Si3 C31 114.1(2) . . ? N4 Si3 C32 114.9(2) . . ? C31 Si3 C32 106.5(3) . . ? N4 Si3 C30 107.4(2) . . ? C31 Si3 C30 106.3(2) . . ? C32 Si3 C30 107.1(2) . . ? N4 Si3 Y1 41.26(12) . . ? C31 Si3 Y1 123.85(19) . . ? C32 Si3 Y1 129.31(19) . . ? C30 Si3 Y1 66.16(15) . . ? N4 Si4 C33 111.1(2) . . ? N4 Si4 C35 113.1(2) . . ? C33 Si4 C35 105.2(2) . . ? N4 Si4 C34 112.4(2) . . ? C33 Si4 C34 107.6(3) . . ? C35 Si4 C34 106.9(2) . . ? C2 N1 C6 118.9(4) . . ? C2 N1 Y1 107.0(3) . . ? C6 N1 Y1 134.0(3) . . ? C4 N2 C18 117.1(3) . . ? C4 N2 Y1 104.4(3) . . ? C18 N2 Y1 135.8(3) . . ? Si1 N3 Si2 120.3(2) . . ? Si1 N3 Y1 111.46(18) . . ? Si2 N3 Y1 127.45(19) . . ? Si3 N4 Si4 122.5(2) . . ? Si3 N4 Y1 108.27(17) . . ? Si4 N4 Y1 128.4(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.3(4) . . ? N1 C2 C1 121.1(4) . . ? C3 C2 C1 115.6(4) . . ? N1 C2 Y1 48.0(2) . . ? C3 C2 Y1 79.5(3) . . ? C1 C2 Y1 155.9(3) . . ? C4 C3 C2 129.2(4) . . ? C4 C3 H3 115.4 . . ? C2 C3 H3 115.4 . . ? N2 C4 C3 123.2(4) . . ? N2 C4 C5 122.4(4) . . ? C3 C4 C5 114.3(4) . . ? N2 C4 Y1 49.8(2) . . ? C3 C4 Y1 80.1(2) . . ? C5 C4 Y1 153.3(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 121.4(4) . . ? C7 C6 N1 121.0(4) . . ? C11 C6 N1 117.5(4) . . ? C8 C7 C6 117.5(4) . . ? C8 C7 C12 118.6(4) . . ? C6 C7 C12 123.8(4) . . ? C9 C8 C7 121.9(5) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C10 C9 C8 119.6(5) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 121.7(5) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C10 C11 C6 117.8(4) . . ? C10 C11 C15 119.7(4) . . ? C6 C11 C15 122.5(4) . . ? C7 C12 C13 112.7(4) . . ? C7 C12 C14 112.6(4) . . ? C13 C12 C14 108.9(4) . . ? C7 C12 H12 107.4 . . ? C13 C12 H12 107.4 . . ? C14 C12 H12 107.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C11 112.0(5) . . ? C17 C15 C16 109.8(4) . . ? C11 C15 C16 111.5(4) . . ? C17 C15 H15 107.7 . . ? C11 C15 H15 107.7 . . ? C16 C15 H15 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 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 118.8(4) . . ? C19 C18 N2 117.4(4) . . ? C23 C18 N2 123.9(4) . . ? C20 C19 C18 120.5(5) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 120.5(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 119.4(5) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C23 121.1(5) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 119.7(5) . . ? C22 C23 H23 120.1 . . ? C18 C23 H23 120.1 . . ? 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 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 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 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si3 C30 H30A 109.5 . . ? Si3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si3 C31 H31A 109.5 . . ? Si3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si4 C33 H33A 109.5 . . ? Si4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si4 C34 H34A 109.5 . . ? Si4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si4 C35 H35A 109.5 . . ? Si4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 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 N4 Y1 Si1 N3 -35.4(2) . . . . ? N1 Y1 Si1 N3 111.6(2) . . . . ? N2 Y1 Si1 N3 -166.6(2) . . . . ? C4 Y1 Si1 N3 178.5(2) . . . . ? C2 Y1 Si1 N3 116.2(2) . . . . ? Si3 Y1 Si1 N3 -64.1(2) . . . . ? N4 Y1 Si1 C26 -127.8(3) . . . . ? N3 Y1 Si1 C26 -92.4(3) . . . . ? N1 Y1 Si1 C26 19.1(2) . . . . ? N2 Y1 Si1 C26 101.0(3) . . . . ? C4 Y1 Si1 C26 86.1(3) . . . . ? C2 Y1 Si1 C26 23.7(3) . . . . ? Si3 Y1 Si1 C26 -156.6(2) . . . . ? N4 Y1 Si1 C24 135.6(2) . . . . ? N3 Y1 Si1 C24 171.0(3) . . . . ? N1 Y1 Si1 C24 -77.4(2) . . . . ? N2 Y1 Si1 C24 4.4(2) . . . . ? C4 Y1 Si1 C24 -10.5(2) . . . . ? C2 Y1 Si1 C24 -72.9(2) . . . . ? Si3 Y1 Si1 C24 106.86(19) . . . . ? N4 Y1 Si1 C25 43.6(3) . . . . ? N3 Y1 Si1 C25 79.0(3) . . . . ? N1 Y1 Si1 C25 -169.4(3) . . . . ? N2 Y1 Si1 C25 -87.5(3) . . . . ? C4 Y1 Si1 C25 -102.5(3) . . . . ? C2 Y1 Si1 C25 -164.8(3) . . . . ? Si3 Y1 Si1 C25 14.9(3) . . . . ? N3 Y1 Si3 N4 111.8(2) . . . . ? N1 Y1 Si3 N4 -33.4(3) . . . . ? N2 Y1 Si3 N4 -107.35(19) . . . . ? C4 Y1 Si3 N4 -81.6(2) . . . . ? C2 Y1 Si3 N4 -42.1(2) . . . . ? Si1 Y1 Si3 N4 138.17(18) . . . . ? N4 Y1 Si3 C31 88.9(3) . . . . ? N3 Y1 Si3 C31 -159.2(2) . . . . ? N1 Y1 Si3 C31 55.5(3) . . . . ? N2 Y1 Si3 C31 -18.4(2) . . . . ? C4 Y1 Si3 C31 7.3(2) . . . . ? C2 Y1 Si3 C31 46.8(2) . . . . ? Si1 Y1 Si3 C31 -132.9(2) . . . . ? N4 Y1 Si3 C32 -83.7(3) . . . . ? N3 Y1 Si3 C32 28.1(3) . . . . ? N1 Y1 Si3 C32 -117.1(3) . . . . ? N2 Y1 Si3 C32 168.9(3) . . . . ? C4 Y1 Si3 C32 -165.4(3) . . . . ? C2 Y1 Si3 C32 -125.9(3) . . . . ? Si1 Y1 Si3 C32 54.5(2) . . . . ? N4 Y1 Si3 C30 -176.8(2) . . . . ? N3 Y1 Si3 C30 -64.99(18) . . . . ? N1 Y1 Si3 C30 149.8(2) . . . . ? N2 Y1 Si3 C30 75.83(17) . . . . ? C4 Y1 Si3 C30 101.54(18) . . . . ? C2 Y1 Si3 C30 141.04(18) . . . . ? Si1 Y1 Si3 C30 -38.65(16) . . . . ? N4 Y1 N1 C2 -36.2(3) . . . . ? N3 Y1 N1 C2 -161.6(3) . . . . ? N2 Y1 N1 C2 59.8(3) . . . . ? C4 Y1 N1 C2 35.5(3) . . . . ? Si3 Y1 N1 C2 -17.1(4) . . . . ? Si1 Y1 N1 C2 170.6(3) . . . . ? N4 Y1 N1 C6 138.0(4) . . . . ? N3 Y1 N1 C6 12.5(4) . . . . ? N2 Y1 N1 C6 -126.0(4) . . . . ? C4 Y1 N1 C6 -150.3(4) . . . . ? C2 Y1 N1 C6 174.2(6) . . . . ? Si3 Y1 N1 C6 157.1(3) . . . . ? Si1 Y1 N1 C6 -15.3(4) . . . . ? N4 Y1 N2 C4 57.8(3) . . . . ? N3 Y1 N2 C4 -164.6(3) . . . . ? N1 Y1 N2 C4 -62.9(3) . . . . ? C2 Y1 N2 C4 -39.8(3) . . . . ? Si3 Y1 N2 C4 87.2(3) . . . . ? Si1 Y1 N2 C4 -154.7(3) . . . . ? N4 Y1 N2 C18 -102.3(4) . . . . ? N3 Y1 N2 C18 35.3(5) . . . . ? N1 Y1 N2 C18 137.0(4) . . . . ? C4 Y1 N2 C18 -160.1(6) . . . . ? C2 Y1 N2 C18 160.1(4) . . . . ? Si3 Y1 N2 C18 -72.8(4) . . . . ? Si1 Y1 N2 C18 45.2(4) . . . . ? C26 Si1 N3 Si2 -80.2(3) . . . . ? C24 Si1 N3 Si2 161.8(3) . . . . ? C25 Si1 N3 Si2 44.9(3) . . . . ? Y1 Si1 N3 Si2 170.5(4) . . . . ? C26 Si1 N3 Y1 109.3(3) . . . . ? C24 Si1 N3 Y1 -8.7(3) . . . . ? C25 Si1 N3 Y1 -125.6(2) . . . . ? C29 Si2 N3 Si1 -77.1(3) . . . . ? C27 Si2 N3 Si1 163.4(3) . . . . ? C28 Si2 N3 Si1 41.4(3) . . . . ? C29 Si2 N3 Y1 91.8(3) . . . . ? C27 Si2 N3 Y1 -27.7(3) . . . . ? C28 Si2 N3 Y1 -149.7(3) . . . . ? N4 Y1 N3 Si1 154.29(18) . . . . ? N1 Y1 N3 Si1 -73.3(2) . . . . ? N2 Y1 N3 Si1 19.3(3) . . . . ? C4 Y1 N3 Si1 -3.6(6) . . . . ? C2 Y1 N3 Si1 -83.1(2) . . . . ? Si3 Y1 N3 Si1 124.20(17) . . . . ? N4 Y1 N3 Si2 -15.4(3) . . . . ? N1 Y1 N3 Si2 117.0(2) . . . . ? N2 Y1 N3 Si2 -150.3(2) . . . . ? C4 Y1 N3 Si2 -173.3(3) . . . . ? C2 Y1 N3 Si2 107.2(2) . . . . ? Si3 Y1 N3 Si2 -45.5(2) . . . . ? Si1 Y1 N3 Si2 -169.7(4) . . . . ? C31 Si3 N4 Si4 56.0(3) . . . . ? C32 Si3 N4 Si4 -67.4(3) . . . . ? C30 Si3 N4 Si4 173.6(2) . . . . ? Y1 Si3 N4 Si4 170.6(3) . . . . ? C31 Si3 N4 Y1 -114.5(2) . . . . ? C32 Si3 N4 Y1 122.0(2) . . . . ? C30 Si3 N4 Y1 3.0(2) . . . . ? C33 Si4 N4 Si3 165.5(2) . . . . ? C35 Si4 N4 Si3 47.4(3) . . . . ? C34 Si4 N4 Si3 -73.8(3) . . . . ? C33 Si4 N4 Y1 -25.9(3) . . . . ? C35 Si4 N4 Y1 -144.0(2) . . . . ? C34 Si4 N4 Y1 94.8(3) . . . . ? N3 Y1 N4 Si3 -76.34(19) . . . . ? N1 Y1 N4 Si3 160.69(15) . . . . ? N2 Y1 N4 Si3 75.67(18) . . . . ? C4 Y1 N4 Si3 97.29(18) . . . . ? C2 Y1 N4 Si3 145.93(17) . . . . ? Si1 Y1 N4 Si3 -58.9(2) . . . . ? N3 Y1 N4 Si4 113.8(2) . . . . ? N1 Y1 N4 Si4 -9.2(3) . . . . ? N2 Y1 N4 Si4 -94.2(2) . . . . ? C4 Y1 N4 Si4 -72.6(2) . . . . ? C2 Y1 N4 Si4 -23.9(2) . . . . ? Si3 Y1 N4 Si4 -169.9(4) . . . . ? Si1 Y1 N4 Si4 131.21(18) . . . . ? C6 N1 C2 C3 156.9(4) . . . . ? Y1 N1 C2 C3 -27.8(5) . . . . ? C6 N1 C2 C1 -22.2(6) . . . . ? Y1 N1 C2 C1 153.0(4) . . . . ? C6 N1 C2 Y1 -175.2(5) . . . . ? N4 Y1 C2 N1 149.2(3) . . . . ? N3 Y1 C2 N1 22.8(3) . . . . ? N2 Y1 C2 N1 -114.0(3) . . . . ? C4 Y1 C2 N1 -135.1(3) . . . . ? Si3 Y1 C2 N1 169.5(2) . . . . ? Si1 Y1 C2 N1 -10.8(3) . . . . ? N4 Y1 C2 C3 -54.2(3) . . . . ? N3 Y1 C2 C3 179.4(2) . . . . ? N1 Y1 C2 C3 156.6(4) . . . . ? N2 Y1 C2 C3 42.6(3) . . . . ? C4 Y1 C2 C3 21.5(2) . . . . ? Si3 Y1 C2 C3 -33.9(3) . . . . ? Si1 Y1 C2 C3 145.8(2) . . . . ? N4 Y1 C2 C1 77.3(8) . . . . ? N3 Y1 C2 C1 -49.1(8) . . . . ? N1 Y1 C2 C1 -71.9(8) . . . . ? N2 Y1 C2 C1 174.0(8) . . . . ? C4 Y1 C2 C1 152.9(8) . . . . ? Si3 Y1 C2 C1 97.6(8) . . . . ? Si1 Y1 C2 C1 -82.8(8) . . . . ? N1 C2 C3 C4 -29.9(7) . . . . ? C1 C2 C3 C4 149.3(5) . . . . ? Y1 C2 C3 C4 -50.6(5) . . . . ? C18 N2 C4 C3 -160.6(4) . . . . ? Y1 N2 C4 C3 34.9(5) . . . . ? C18 N2 C4 C5 16.4(6) . . . . ? Y1 N2 C4 C5 -148.1(4) . . . . ? C18 N2 C4 Y1 164.5(5) . . . . ? C2 C3 C4 N2 24.4(7) . . . . ? C2 C3 C4 C5 -152.9(5) . . . . ? C2 C3 C4 Y1 50.7(5) . . . . ? N4 Y1 C4 N2 -123.3(3) . . . . ? N3 Y1 C4 N2 35.9(6) . . . . ? N1 Y1 C4 N2 110.8(3) . . . . ? C2 Y1 C4 N2 129.4(3) . . . . ? Si3 Y1 C4 N2 -93.1(3) . . . . ? Si1 Y1 C4 N2 33.5(3) . . . . ? N4 Y1 C4 C3 85.7(3) . . . . ? N3 Y1 C4 C3 -115.0(5) . . . . ? N1 Y1 C4 C3 -40.2(2) . . . . ? N2 Y1 C4 C3 -150.9(4) . . . . ? C2 Y1 C4 C3 -21.6(2) . . . . ? Si3 Y1 C4 C3 115.9(2) . . . . ? Si1 Y1 C4 C3 -117.4(2) . . . . ? N4 Y1 C4 C5 -40.0(7) . . . . ? N3 Y1 C4 C5 119.2(7) . . . . ? N1 Y1 C4 C5 -165.9(7) . . . . ? N2 Y1 C4 C5 83.3(8) . . . . ? C2 Y1 C4 C5 -147.4(8) . . . . ? Si3 Y1 C4 C5 -9.8(7) . . . . ? Si1 Y1 C4 C5 116.8(7) . . . . ? C2 N1 C6 C7 102.1(5) . . . . ? Y1 N1 C6 C7 -71.5(5) . . . . ? C2 N1 C6 C11 -81.6(5) . . . . ? Y1 N1 C6 C11 104.8(4) . . . . ? C11 C6 C7 C8 -2.4(7) . . . . ? N1 C6 C7 C8 173.7(4) . . . . ? C11 C6 C7 C12 174.8(4) . . . . ? N1 C6 C7 C12 -9.1(7) . . . . ? C6 C7 C8 C9 0.8(7) . . . . ? C12 C7 C8 C9 -176.6(4) . . . . ? C7 C8 C9 C10 2.0(8) . . . . ? C8 C9 C10 C11 -3.2(8) . . . . ? C9 C10 C11 C6 1.6(8) . . . . ? C9 C10 C11 C15 179.6(5) . . . . ? C7 C6 C11 C10 1.3(7) . . . . ? N1 C6 C11 C10 -175.0(4) . . . . ? C7 C6 C11 C15 -176.6(4) . . . . ? N1 C6 C11 C15 7.1(7) . . . . ? C8 C7 C12 C13 -52.5(6) . . . . ? C6 C7 C12 C13 130.3(5) . . . . ? C8 C7 C12 C14 71.2(6) . . . . ? C6 C7 C12 C14 -105.9(6) . . . . ? C10 C11 C15 C17 -75.6(6) . . . . ? C6 C11 C15 C17 102.2(6) . . . . ? C10 C11 C15 C16 48.0(7) . . . . ? C6 C11 C15 C16 -134.1(5) . . . . ? C4 N2 C18 C19 109.2(5) . . . . ? Y1 N2 C18 C19 -92.5(5) . . . . ? C4 N2 C18 C23 -72.4(6) . . . . ? Y1 N2 C18 C23 85.9(5) . . . . ? C23 C18 C19 C20 1.4(7) . . . . ? N2 C18 C19 C20 179.9(4) . . . . ? C18 C19 C20 C21 0.1(8) . . . . ? C19 C20 C21 C22 -0.3(8) . . . . ? C20 C21 C22 C23 -1.0(8) . . . . ? C21 C22 C23 C18 2.5(8) . . . . ? C19 C18 C23 C22 -2.7(7) . . . . ? N2 C18 C23 C22 178.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.253 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.059 _database_code_depnum_ccdc_archive 'CCDC 952931' ####################################################################### # # 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_complex7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H65 N4 O Si4 Y' _chemical_formula_weight 759.18 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 18.189(2) _cell_length_b 14.5123(12) _cell_length_c 16.414(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4332.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5763 _cell_measurement_theta_min 3.8890 _cell_measurement_theta_max 25.8750 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.7500 _exptl_crystal_size_mid 0.6000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 1.486 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.52291 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24412 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 26.39 _reflns_number_total 8388 _reflns_number_gt 6598 _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^)+(0.0587P)^2^+1.3792P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.023(6) _refine_ls_number_reflns 8388 _refine_ls_number_parameters 396 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 0.97044(2) 0.27482(2) 0.24899(3) 0.03051(10) Uani 1 1 d . B . O1 O 1.02345(18) 0.4259(2) 0.22577(17) 0.0464(8) Uani 1 1 d . . . N1 N 0.88090(18) 0.1615(2) 0.28015(19) 0.0308(8) Uani 1 1 d . . . N2 N 0.8745(2) 0.3638(2) 0.3036(2) 0.0374(8) Uani 1 1 d . . . N3 N 0.9990(2) 0.2539(2) 0.1154(2) 0.0391(8) Uani 1 1 d . B . N4 N 1.0505(2) 0.2581(3) 0.3526(2) 0.0425(9) Uani 1 1 d . B . Si1 Si 1.08458(10) 0.24863(12) 0.07398(11) 0.0639(4) Uani 1 1 d . . . H111 H 1.1191 0.2602 0.1187 0.077 Uiso 1 1 calc R A 1 Si2 Si 0.91846(8) 0.25549(9) 0.06314(8) 0.0446(3) Uani 1 1 d . . . H112 H 0.8805 0.2667 0.1043 0.067 Uiso 1 1 calc R B . Si3 Si 1.05107(10) 0.31290(12) 0.44471(9) 0.0637(4) Uani 1 1 d . . . H113 H 1.0156 0.3636 0.4419 0.096 Uiso 1 1 calc R . . Si4 Si 1.10948(8) 0.17292(10) 0.32800(9) 0.0525(4) Uani 1 1 d . . . H114 H 1.0942 0.1522 0.2738 0.079 Uiso 1 1 calc R B . C1 C 0.8370(3) 0.0779(3) 0.4018(3) 0.0533(13) Uani 1 1 d . . . H1A H 0.7945 0.0528 0.3750 0.080 Uiso 1 1 calc R . . H1B H 0.8248 0.0926 0.4572 0.080 Uiso 1 1 calc R . . H1C H 0.8761 0.0335 0.4010 0.080 Uiso 1 1 calc R . . C2 C 0.8614(2) 0.1645(3) 0.3580(2) 0.0368(10) Uani 1 1 d . . . C3 C 0.8578(3) 0.2469(3) 0.4036(3) 0.0431(11) Uani 1 1 d . . . H3 H 0.8590 0.2395 0.4599 0.052 Uiso 1 1 calc R . . C4 C 0.8526(3) 0.3377(3) 0.3765(3) 0.0425(11) Uani 1 1 d . . . C5 C 0.8162(4) 0.4042(3) 0.4353(3) 0.0645(16) Uani 1 1 d . . . H5A H 0.8524 0.4458 0.4567 0.097 Uiso 1 1 calc R . . H5B H 0.7943 0.3702 0.4793 0.097 Uiso 1 1 calc R . . H5C H 0.7789 0.4385 0.4073 0.097 Uiso 1 1 calc R . . C6 C 0.8490(2) 0.0885(3) 0.2311(2) 0.0354(10) Uani 1 1 d . . . C7 C 0.7785(2) 0.1051(3) 0.1979(2) 0.0364(10) Uani 1 1 d . . . C8 C 0.7473(3) 0.0353(3) 0.1516(3) 0.0505(12) Uani 1 1 d . . . H8 H 0.7005 0.0442 0.1303 0.061 Uiso 1 1 calc R . . C9 C 0.7826(3) -0.0460(4) 0.1359(3) 0.0642(16) Uani 1 1 d . . . H9 H 0.7603 -0.0911 0.1042 0.077 Uiso 1 1 calc R . . C10 C 0.8524(3) -0.0602(3) 0.1681(3) 0.0515(13) Uani 1 1 d . . . H10 H 0.8769 -0.1151 0.1574 0.062 Uiso 1 1 calc R . . C11 C 0.8858(3) 0.0061(3) 0.2159(3) 0.0412(11) Uani 1 1 d . . . C12 C 0.7368(3) 0.1940(3) 0.2135(3) 0.0430(11) Uani 1 1 d . . . H12 H 0.7728 0.2408 0.2298 0.052 Uiso 1 1 calc R . . C13 C 0.6977(3) 0.2294(4) 0.1383(3) 0.0621(14) Uani 1 1 d . . . H13A H 0.7319 0.2329 0.0939 0.093 Uiso 1 1 calc R . . H13B H 0.6781 0.2896 0.1491 0.093 Uiso 1 1 calc R . . H13C H 0.6584 0.1882 0.1244 0.093 Uiso 1 1 calc R . . C14 C 0.6816(3) 0.1836(4) 0.2833(3) 0.0618(14) Uani 1 1 d . . . H14A H 0.6456 0.1380 0.2691 0.093 Uiso 1 1 calc R . . H14B H 0.6576 0.2415 0.2927 0.093 Uiso 1 1 calc R . . H14C H 0.7069 0.1648 0.3318 0.093 Uiso 1 1 calc R . . C15 C 0.9615(2) -0.0149(3) 0.2487(4) 0.0438(9) Uani 1 1 d . . . H15 H 0.9751 0.0347 0.2863 0.053 Uiso 1 1 calc R . . C16 C 1.0181(3) -0.0169(4) 0.1808(4) 0.0624(15) Uani 1 1 d . . . H16A H 1.0088 -0.0687 0.1459 0.094 Uiso 1 1 calc R . . H16B H 1.0664 -0.0222 0.2038 0.094 Uiso 1 1 calc R . . H16C H 1.0149 0.0390 0.1497 0.094 Uiso 1 1 calc R . . C17 C 0.9651(3) -0.1062(4) 0.2958(4) 0.0728(17) Uani 1 1 d . . . H17A H 0.9241 -0.1102 0.3324 0.109 Uiso 1 1 calc R . . H17B H 1.0101 -0.1089 0.3263 0.109 Uiso 1 1 calc R . . H17C H 0.9634 -0.1568 0.2581 0.109 Uiso 1 1 calc R . . C18 C 0.8552(3) 0.4539(3) 0.2727(3) 0.0507(13) Uani 1 1 d . . . C19 C 0.8114(3) 0.4593(4) 0.2056(3) 0.0612(15) Uani 1 1 d . . . H19 H 0.7920 0.4061 0.1823 0.073 Uiso 1 1 calc R . . C20 C 0.7956(4) 0.5465(5) 0.1718(4) 0.084(2) Uani 1 1 d . . . H20 H 0.7654 0.5501 0.1262 0.101 Uiso 1 1 calc R . . C21 C 0.8229(5) 0.6233(5) 0.2035(5) 0.095(3) Uani 1 1 d . . . H21 H 0.8116 0.6799 0.1801 0.114 Uiso 1 1 calc R . . C22 C 0.8669(5) 0.6196(4) 0.2696(5) 0.095(3) Uani 1 1 d . . . H22 H 0.8850 0.6740 0.2918 0.114 Uiso 1 1 calc R . . C23 C 0.8860(4) 0.5342(3) 0.3061(4) 0.0742(19) Uani 1 1 d . . . H23 H 0.9178 0.5316 0.3504 0.089 Uiso 1 1 calc R . . C24 C 1.1057(5) 0.3338(6) -0.0048(6) 0.128(2) Uani 1 1 d . B 1 H24A H 1.0810 0.3173 -0.0545 0.192 Uiso 1 1 calc R B 1 H24B H 1.1578 0.3353 -0.0140 0.192 Uiso 1 1 calc R B 1 H24C H 1.0892 0.3935 0.0126 0.192 Uiso 1 1 calc R B 1 C25 C 1.1101(5) 0.1362(6) 0.0306(6) 0.128(2) Uani 1 1 d . B . H25A H 1.1195 0.0933 0.0739 0.192 Uiso 1 1 calc R . . H25B H 1.1536 0.1429 -0.0021 0.192 Uiso 1 1 calc R . . H25C H 1.0706 0.1137 -0.0027 0.192 Uiso 1 1 calc R . . C26 C 0.9060(5) 0.3492(4) -0.0145(4) 0.090(2) Uani 1 1 d . B . H26A H 0.9190 0.4074 0.0092 0.135 Uiso 1 1 calc R . . H26B H 0.8556 0.3508 -0.0317 0.135 Uiso 1 1 calc R . . H26C H 0.9370 0.3372 -0.0606 0.135 Uiso 1 1 calc R . . C27 C 0.8917(3) 0.1459(4) 0.0129(3) 0.0628(15) Uani 1 1 d . B . H27A H 0.9273 0.1306 -0.0282 0.094 Uiso 1 1 calc R . . H27B H 0.8442 0.1529 -0.0119 0.094 Uiso 1 1 calc R . . H27C H 0.8898 0.0975 0.0527 0.094 Uiso 1 1 calc R . . C28 C 1.1427(4) 0.3635(5) 0.4713(5) 0.105(3) Uani 1 1 d . . . H28A H 1.1756 0.3152 0.4875 0.158 Uiso 1 1 calc R . . H28B H 1.1370 0.4064 0.5153 0.158 Uiso 1 1 calc R . . H28C H 1.1625 0.3948 0.4247 0.158 Uiso 1 1 calc R . . C29 C 1.0252(5) 0.2389(6) 0.5329(4) 0.104(3) Uani 1 1 d . . . H29A H 1.0580 0.1872 0.5360 0.156 Uiso 1 1 calc R . . H29B H 0.9757 0.2173 0.5260 0.156 Uiso 1 1 calc R . . H29C H 1.0285 0.2742 0.5823 0.156 Uiso 1 1 calc R . . C30 C 1.2074(4) 0.2070(6) 0.3166(5) 0.106(3) Uani 1 1 d . B . H30A H 1.2339 0.1586 0.2897 0.159 Uiso 1 1 calc R . . H30B H 1.2284 0.2177 0.3694 0.159 Uiso 1 1 calc R . . H30C H 1.2105 0.2624 0.2848 0.159 Uiso 1 1 calc R . . C31 C 1.1067(5) 0.0682(4) 0.3929(4) 0.100(3) Uani 1 1 d . B . H31A H 1.1264 0.0824 0.4457 0.150 Uiso 1 1 calc R . . H31B H 1.1356 0.0205 0.3681 0.150 Uiso 1 1 calc R . . H31C H 1.0568 0.0478 0.3984 0.150 Uiso 1 1 calc R . . C32 C 1.0115(4) 0.4840(4) 0.1542(4) 0.0779(9) Uani 1 1 d . . . H32A H 0.9652 0.5169 0.1584 0.093 Uiso 1 1 calc R . . H32B H 1.0110 0.4472 0.1048 0.093 Uiso 1 1 calc R . . C33 C 1.0756(4) 0.5501(4) 0.1543(4) 0.0779(9) Uani 1 1 d . . . H33A H 1.1159 0.5258 0.1221 0.093 Uiso 1 1 calc R . . H33B H 1.0611 0.6092 0.1320 0.093 Uiso 1 1 calc R . . C34 C 1.0971(4) 0.5595(4) 0.2392(4) 0.0779(9) Uani 1 1 d . . . H34A H 1.0691 0.6079 0.2656 0.093 Uiso 1 1 calc R . . H34B H 1.1491 0.5738 0.2437 0.093 Uiso 1 1 calc R . . C35 C 1.0805(4) 0.4677(4) 0.2763(4) 0.0779(9) Uani 1 1 d . . . H35A H 1.1242 0.4293 0.2770 0.093 Uiso 1 1 calc R . . H35B H 1.0632 0.4751 0.3319 0.093 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 0.03726(19) 0.02801(17) 0.02625(17) 0.0012(2) 0.0016(2) -0.00235(16) O1 0.062(2) 0.0338(15) 0.043(2) 0.0052(12) -0.0033(14) -0.0138(14) N1 0.0302(19) 0.0289(17) 0.0333(18) 0.0019(13) 0.0013(13) -0.0011(14) N2 0.049(2) 0.0263(17) 0.037(2) 0.0010(15) 0.0073(16) 0.0016(15) N3 0.052(2) 0.0351(18) 0.030(2) 0.0003(15) 0.0078(17) 0.0035(18) N4 0.043(2) 0.045(2) 0.039(2) 0.0064(17) -0.0057(18) -0.0046(18) Si1 0.0583(10) 0.0725(10) 0.0610(10) 0.0075(8) 0.0216(8) -0.0046(8) Si2 0.0540(8) 0.0506(7) 0.0292(6) -0.0021(5) -0.0011(6) 0.0034(6) Si3 0.0801(12) 0.0719(10) 0.0391(8) -0.0042(8) -0.0146(7) 0.0153(9) Si4 0.0582(9) 0.0511(8) 0.0483(8) -0.0032(6) -0.0121(6) 0.0016(7) C1 0.082(4) 0.038(3) 0.040(3) 0.010(2) 0.007(2) -0.001(3) C2 0.045(3) 0.035(2) 0.030(2) 0.0022(18) 0.0002(18) -0.002(2) C3 0.055(3) 0.046(3) 0.028(2) 0.0048(19) 0.001(2) -0.006(2) C4 0.049(3) 0.044(3) 0.034(2) -0.009(2) 0.012(2) -0.008(2) C5 0.100(5) 0.042(3) 0.051(3) -0.004(2) 0.029(3) 0.000(3) C6 0.036(2) 0.033(2) 0.036(3) 0.0040(18) 0.0024(17) -0.0053(17) C7 0.039(3) 0.038(2) 0.032(2) -0.0019(18) 0.0033(18) -0.0041(19) C8 0.038(3) 0.058(3) 0.055(3) -0.008(2) -0.007(2) -0.009(2) C9 0.071(4) 0.050(3) 0.072(4) -0.026(3) -0.005(3) -0.017(3) C10 0.054(3) 0.037(3) 0.063(3) -0.017(2) 0.008(3) -0.008(2) C11 0.041(3) 0.035(2) 0.048(2) -0.001(2) 0.0087(19) -0.001(2) C12 0.038(3) 0.048(3) 0.043(2) -0.001(2) -0.002(2) 0.003(2) C13 0.058(4) 0.070(4) 0.059(3) 0.004(3) -0.002(3) 0.013(3) C14 0.052(3) 0.067(3) 0.066(3) -0.004(3) 0.018(3) 0.008(3) C15 0.042(2) 0.0345(19) 0.055(2) -0.003(3) -0.001(3) 0.0019(17) C16 0.052(4) 0.056(3) 0.079(4) -0.009(3) 0.010(3) 0.007(3) C17 0.076(4) 0.060(3) 0.083(4) 0.019(3) -0.001(3) 0.007(3) C18 0.062(3) 0.037(3) 0.053(3) 0.001(2) 0.029(2) 0.008(2) C19 0.060(4) 0.061(3) 0.062(4) 0.019(3) 0.021(3) 0.018(3) C20 0.085(5) 0.070(4) 0.098(5) 0.043(4) 0.031(4) 0.032(4) C21 0.133(7) 0.059(4) 0.093(6) 0.040(4) 0.058(5) 0.042(4) C22 0.151(7) 0.039(3) 0.096(6) -0.007(3) 0.063(5) -0.001(4) C23 0.120(5) 0.039(3) 0.064(4) -0.003(3) 0.032(3) 0.001(3) C24 0.136(6) 0.105(4) 0.142(5) 0.017(4) 0.076(5) 0.025(4) C25 0.136(6) 0.105(4) 0.142(5) 0.017(4) 0.076(5) 0.025(4) C26 0.135(7) 0.071(4) 0.063(4) 0.016(3) -0.034(4) 0.004(4) C27 0.073(4) 0.069(4) 0.046(3) -0.012(3) 0.000(3) -0.016(3) C28 0.108(6) 0.117(6) 0.090(5) -0.035(4) -0.037(4) -0.008(5) C29 0.133(7) 0.132(7) 0.046(4) 0.030(4) 0.007(4) 0.053(5) C30 0.059(4) 0.162(8) 0.097(5) -0.030(5) 0.003(4) -0.010(5) C31 0.161(7) 0.048(3) 0.091(5) 0.006(3) -0.049(5) 0.021(4) C32 0.094(2) 0.0608(17) 0.079(2) 0.0140(16) -0.0097(17) -0.0342(16) C33 0.094(2) 0.0608(17) 0.079(2) 0.0140(16) -0.0097(17) -0.0342(16) C34 0.094(2) 0.0608(17) 0.079(2) 0.0140(16) -0.0097(17) -0.0342(16) C35 0.094(2) 0.0608(17) 0.079(2) 0.0140(16) -0.0097(17) -0.0342(16) _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 2.252(4) . ? Y1 N3 2.275(4) . ? Y1 N2 2.349(3) . ? Y1 N1 2.370(3) . ? Y1 O1 2.425(3) . ? Y1 Si4 3.2038(15) . ? Y1 Si2 3.2061(16) . ? O1 C35 1.461(6) . ? O1 C32 1.463(6) . ? N1 C2 1.327(5) . ? N1 C6 1.452(5) . ? N2 C4 1.316(5) . ? N2 C18 1.445(6) . ? N3 Si2 1.698(4) . ? N3 Si1 1.699(4) . ? N4 Si4 1.685(4) . ? N4 Si3 1.709(4) . ? Si1 C25 1.840(8) . ? Si1 C24 1.830(8) . ? Si1 H111 0.9800 . ? Si2 C27 1.857(5) . ? Si2 C26 1.877(6) . ? Si2 H112 0.9800 . ? Si3 C29 1.863(7) . ? Si3 C28 1.873(7) . ? Si3 H113 0.9800 . ? Si4 C30 1.858(7) . ? Si4 C31 1.856(6) . ? Si4 H114 0.9800 . ? C1 C2 1.514(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.413(6) . ? C3 C4 1.394(6) . ? C3 H3 0.9300 . ? C4 C5 1.518(6) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C11 1.393(6) . ? C6 C7 1.414(6) . ? C7 C8 1.388(6) . ? C7 C12 1.518(6) . ? C8 C9 1.368(7) . ? C8 H8 0.9300 . ? C9 C10 1.390(8) . ? C9 H9 0.9300 . ? C10 C11 1.382(6) . ? C10 H10 0.9300 . ? C11 C15 1.510(6) . ? C12 C13 1.514(7) . ? C12 C14 1.532(6) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.517(7) . ? C15 C17 1.536(7) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.363(7) . ? C18 C23 1.405(7) . ? C19 C20 1.411(7) . ? C19 H19 0.9300 . ? C20 C21 1.327(11) . ? C20 H20 0.9300 . ? C21 C22 1.350(10) . ? C21 H21 0.9300 . ? C22 C23 1.419(9) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? 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 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.510(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.454(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.497(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 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 N4 Y1 N3 124.45(17) . . ? N4 Y1 N2 104.60(14) . . ? N3 Y1 N2 127.68(13) . . ? N4 Y1 N1 101.92(13) . . ? N3 Y1 N1 105.83(13) . . ? N2 Y1 N1 77.77(12) . . ? N4 Y1 O1 87.66(12) . . ? N3 Y1 O1 82.99(12) . . ? N2 Y1 O1 81.88(11) . . ? N1 Y1 O1 159.11(11) . . ? N4 Y1 Si4 30.01(11) . . ? N3 Y1 Si4 98.52(11) . . ? N2 Y1 Si4 133.31(9) . . ? N1 Y1 Si4 97.75(8) . . ? O1 Y1 Si4 99.61(8) . . ? N4 Y1 Si2 154.12(11) . . ? N3 Y1 Si2 30.49(11) . . ? N2 Y1 Si2 101.06(9) . . ? N1 Y1 Si2 86.67(8) . . ? O1 Y1 Si2 92.68(7) . . ? Si4 Y1 Si2 125.28(4) . . ? C35 O1 C32 108.8(4) . . ? C35 O1 Y1 124.7(3) . . ? C32 O1 Y1 126.0(3) . . ? C2 N1 C6 116.8(3) . . ? C2 N1 Y1 111.7(3) . . ? C6 N1 Y1 131.4(2) . . ? C4 N2 C18 120.4(4) . . ? C4 N2 Y1 114.4(3) . . ? C18 N2 Y1 122.9(3) . . ? Si2 N3 Si1 126.1(2) . . ? Si2 N3 Y1 106.7(2) . . ? Si1 N3 Y1 126.9(2) . . ? Si4 N4 Si3 123.3(2) . . ? Si4 N4 Y1 108.07(19) . . ? Si3 N4 Y1 128.5(2) . . ? N3 Si1 C25 115.2(3) . . ? N3 Si1 C24 116.4(3) . . ? C25 Si1 C24 105.8(4) . . ? N3 Si1 H111 106.2 . . ? C25 Si1 H111 106.2 . . ? C24 Si1 H111 106.2 . . ? N3 Si2 C27 116.0(2) . . ? N3 Si2 C26 117.2(3) . . ? C27 Si2 C26 106.7(3) . . ? N3 Si2 Y1 42.81(13) . . ? C27 Si2 Y1 125.11(19) . . ? C26 Si2 Y1 128.2(2) . . ? N3 Si2 H112 105.3 . . ? C27 Si2 H112 105.3 . . ? C26 Si2 H112 105.3 . . ? Y1 Si2 H112 62.5 . . ? N4 Si3 C29 114.7(3) . . ? N4 Si3 C28 113.2(3) . . ? C29 Si3 C28 105.6(4) . . ? N4 Si3 H113 107.6 . . ? C29 Si3 H113 107.6 . . ? C28 Si3 H113 107.6 . . ? N4 Si4 C30 116.0(3) . . ? N4 Si4 C31 116.5(3) . . ? C30 Si4 C31 107.6(4) . . ? N4 Si4 Y1 41.92(13) . . ? C30 Si4 Y1 126.4(3) . . ? C31 Si4 Y1 126.1(3) . . ? N4 Si4 H114 105.2 . . ? C30 Si4 H114 105.2 . . ? C31 Si4 H114 105.2 . . ? Y1 Si4 H114 63.3 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.4(4) . . ? N1 C2 C1 120.6(4) . . ? C3 C2 C1 115.9(4) . . ? C4 C3 C2 129.3(4) . . ? C4 C3 H3 115.3 . . ? C2 C3 H3 115.3 . . ? N2 C4 C3 122.9(4) . . ? N2 C4 C5 121.8(4) . . ? C3 C4 C5 115.3(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 120.9(4) . . ? C11 C6 N1 122.3(4) . . ? C7 C6 N1 116.8(3) . . ? C8 C7 C6 117.2(4) . . ? C8 C7 C12 120.5(4) . . ? C6 C7 C12 122.2(4) . . ? C9 C8 C7 122.7(5) . . ? C9 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? C8 C9 C10 119.0(5) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C11 C10 C9 120.9(5) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C6 119.2(4) . . ? C10 C11 C15 117.6(4) . . ? C6 C11 C15 123.2(4) . . ? C13 C12 C7 112.7(4) . . ? C13 C12 C14 109.5(4) . . ? C7 C12 C14 111.7(4) . . ? C13 C12 H12 107.5 . . ? C7 C12 H12 107.5 . . ? C14 C12 H12 107.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 111.1(5) . . ? C11 C15 C17 113.1(4) . . ? C16 C15 C17 108.9(4) . . ? C11 C15 H15 107.8 . . ? C16 C15 H15 107.8 . . ? C17 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 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 120.1(5) . . ? C19 C18 N2 118.5(4) . . ? C23 C18 N2 121.2(5) . . ? C18 C19 C20 119.2(6) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C21 C20 C19 121.6(7) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 120.2(6) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 121.3(7) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C18 117.5(7) . . ? C22 C23 H23 121.2 . . ? C18 C23 H23 121.2 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? Si1 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 . . ? O1 C32 C33 104.5(5) . . ? O1 C32 H32A 110.9 . . ? C33 C32 H32A 110.9 . . ? O1 C32 H32B 110.9 . . ? C33 C32 H32B 110.9 . . ? H32A C32 H32B 108.9 . . ? C34 C33 C32 105.6(5) . . ? C34 C33 H33A 110.6 . . ? C32 C33 H33A 110.6 . . ? C34 C33 H33B 110.6 . . ? C32 C33 H33B 110.6 . . ? H33A C33 H33B 108.7 . . ? C33 C34 C35 104.6(5) . . ? C33 C34 H34A 110.8 . . ? C35 C34 H34A 110.8 . . ? C33 C34 H34B 110.8 . . ? C35 C34 H34B 110.8 . . ? H34A C34 H34B 108.9 . . ? O1 C35 C34 106.4(5) . . ? O1 C35 H35A 110.5 . . ? C34 C35 H35A 110.5 . . ? O1 C35 H35B 110.5 . . ? C34 C35 H35B 110.5 . . ? H35A C35 H35B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.554 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.058 _database_code_depnum_ccdc_archive 'CCDC 952932' ####################################################################### # # 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_complex8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H53 Al2 N2 Y' _chemical_formula_weight 596.62 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 1 21/n 1' 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 12.6433(12) _cell_length_b 20.8974(18) _cell_length_c 13.2484(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.252(3) _cell_angle_gamma 90.00 _cell_volume 3464.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13388 _cell_measurement_theta_min 3.0957 _cell_measurement_theta_max 25.3491 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 1.754 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3344 _exptl_absorpt_correction_T_max 0.5406 _exptl_absorpt_process_details ? _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 33231 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6331 _reflns_number_gt 5521 _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^)+(0.0660P)^2^+2.9367P] 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 6331 _refine_ls_number_parameters 384 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1386 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 H292 H 0.973(5) 0.871(3) 0.466(5) 0.10(2) Uiso 1 1 d . . . Y1 Y 0.93337(3) 0.785297(15) 0.60998(3) 0.03921(14) Uani 1 1 d . . . Al1 Al 0.89236(11) 0.72148(6) 0.39417(9) 0.0528(3) Uani 1 1 d . . . Al2 Al 1.08448(10) 0.90373(6) 0.63413(10) 0.0556(3) Uani 1 1 d . . . N1 N 0.9241(2) 0.69861(13) 0.7200(2) 0.0392(7) Uani 1 1 d . . . N2 N 0.8228(2) 0.82797(14) 0.7136(2) 0.0444(7) Uani 1 1 d . . . C1 C 0.9516(4) 0.6570(2) 0.8973(3) 0.0664(12) Uani 1 1 d . . . H1A H 0.9456 0.6163 0.8635 0.100 Uiso 1 1 calc R . . H1B H 0.9008 0.6593 0.9445 0.100 Uiso 1 1 calc R . . H1C H 1.0225 0.6619 0.9335 0.100 Uiso 1 1 calc R . . C2 C 0.9293(3) 0.70992(17) 0.8189(3) 0.0432(9) Uani 1 1 d . . . C3 C 0.9118(3) 0.77050(19) 0.8596(3) 0.0516(10) Uani 1 1 d . . . H3 H 0.9448 0.7773 0.9261 0.062 Uiso 1 1 calc R . . C4 C 0.8525(3) 0.82169(18) 0.8150(3) 0.0502(10) Uani 1 1 d . . . C5 C 0.8198(4) 0.8718(2) 0.8875(4) 0.0747(14) Uani 1 1 d . . . H5A H 0.8393 0.9135 0.8660 0.112 Uiso 1 1 calc R . . H5B H 0.8555 0.8636 0.9552 0.112 Uiso 1 1 calc R . . H5C H 0.7439 0.8700 0.8872 0.112 Uiso 1 1 calc R . . C6 C 0.9140(3) 0.63233(16) 0.6853(3) 0.0406(8) Uani 1 1 d . . . C7 C 1.0039(3) 0.59493(17) 0.6767(3) 0.0453(9) Uani 1 1 d . . . C8 C 0.9870(4) 0.53242(18) 0.6407(3) 0.0588(11) Uani 1 1 d . . . H8 H 1.0456 0.5065 0.6349 0.071 Uiso 1 1 calc R . . C9 C 0.8868(4) 0.5085(2) 0.6140(4) 0.0663(12) Uani 1 1 d . . . H9 H 0.8778 0.4668 0.5895 0.080 Uiso 1 1 calc R . . C10 C 0.7989(4) 0.5456(2) 0.6230(3) 0.0618(11) Uani 1 1 d . . . H10 H 0.7309 0.5285 0.6049 0.074 Uiso 1 1 calc R . . C11 C 0.8100(3) 0.60796(18) 0.6587(3) 0.0492(9) Uani 1 1 d . . . C12 C 1.1191(3) 0.61630(19) 0.7083(3) 0.0516(10) Uani 1 1 d . . . H12 H 1.1188 0.6622 0.7234 0.062 Uiso 1 1 calc R . . C13 C 1.1886(4) 0.6055(2) 0.6245(4) 0.0708(13) Uani 1 1 d . . . H13A H 1.1992 0.5605 0.6160 0.106 Uiso 1 1 calc R . . H13B H 1.2566 0.6261 0.6432 0.106 Uiso 1 1 calc R . . H13C H 1.1538 0.6234 0.5616 0.106 Uiso 1 1 calc R . . C14 C 1.1718(4) 0.5811(3) 0.8046(4) 0.0773(14) Uani 1 1 d . . . H14A H 1.1329 0.5900 0.8601 0.116 Uiso 1 1 calc R . . H14B H 1.2443 0.5955 0.8219 0.116 Uiso 1 1 calc R . . H14C H 1.1712 0.5358 0.7919 0.116 Uiso 1 1 calc R . . C15 C 0.7104(3) 0.6454(2) 0.6739(3) 0.0595(11) Uani 1 1 d . . . H15 H 0.7295 0.6909 0.6761 0.071 Uiso 1 1 calc R . . C16 C 0.6166(4) 0.6366(3) 0.5873(5) 0.0920(18) Uani 1 1 d . . . H16A H 0.6419 0.6415 0.5227 0.138 Uiso 1 1 calc R . . H16B H 0.5629 0.6683 0.5935 0.138 Uiso 1 1 calc R . . H16C H 0.5867 0.5947 0.5915 0.138 Uiso 1 1 calc R . . C17 C 0.6745(4) 0.6288(3) 0.7761(4) 0.0922(18) Uani 1 1 d . . . H17A H 0.6556 0.5843 0.7767 0.138 Uiso 1 1 calc R . . H17B H 0.6136 0.6544 0.7854 0.138 Uiso 1 1 calc R . . H17C H 0.7317 0.6373 0.8303 0.138 Uiso 1 1 calc R . . C18 C 0.7302(3) 0.86729(18) 0.6817(3) 0.0468(9) Uani 1 1 d . . . C19 C 0.7397(4) 0.9297(2) 0.6478(4) 0.0624(11) Uani 1 1 d . . . H19 H 0.8069 0.9475 0.6462 0.075 Uiso 1 1 calc R . . C20 C 0.6488(4) 0.9650(2) 0.6163(4) 0.0718(13) Uani 1 1 d . . . H20 H 0.6554 1.0065 0.5925 0.086 Uiso 1 1 calc R . . C21 C 0.5497(4) 0.9405(2) 0.6194(3) 0.0665(12) Uani 1 1 d . . . H21 H 0.4891 0.9649 0.5982 0.080 Uiso 1 1 calc R . . C22 C 0.5403(4) 0.8793(2) 0.6543(3) 0.0655(12) Uani 1 1 d . . . H22 H 0.4729 0.8623 0.6572 0.079 Uiso 1 1 calc R . . C23 C 0.6298(3) 0.8428(2) 0.6849(3) 0.0567(10) Uani 1 1 d . . . H23 H 0.6222 0.8013 0.7079 0.068 Uiso 1 1 calc R . . C24 C 0.7767(4) 0.7610(3) 0.4718(4) 0.0536(10) Uani 1 1 d . . . C25 C 1.0406(4) 0.7338(3) 0.4802(4) 0.0685(14) Uani 1 1 d . . . C26 C 0.8716(4) 0.6286(2) 0.3833(4) 0.0748(14) Uani 1 1 d . . . H26A H 0.7967 0.6190 0.3773 0.112 Uiso 1 1 calc R . . H26B H 0.9086 0.6083 0.4431 0.112 Uiso 1 1 calc R . . H26C H 0.8993 0.6131 0.3241 0.112 Uiso 1 1 calc R . . C27 C 0.8907(4) 0.7701(2) 0.2669(3) 0.0673(12) Uani 1 1 d . . . H27A H 0.9468 0.7551 0.2314 0.101 Uiso 1 1 calc R . . H27B H 0.9014 0.8147 0.2825 0.101 Uiso 1 1 calc R . . H27C H 0.8230 0.7644 0.2247 0.101 Uiso 1 1 calc R . . C28 C 1.1081(4) 0.8189(3) 0.7150(4) 0.0605(12) Uani 1 1 d . . . C29 C 0.9578(5) 0.8943(2) 0.5184(4) 0.0623(12) Uani 1 1 d . . . C30 C 1.0529(5) 0.9695(3) 0.7322(4) 0.0891(16) Uani 1 1 d . . . H30A H 1.1140 0.9751 0.7835 0.134 Uiso 1 1 calc R . . H30B H 0.9928 0.9562 0.7638 0.134 Uiso 1 1 calc R . . H30C H 1.0366 1.0092 0.6971 0.134 Uiso 1 1 calc R . . C31 C 1.2115(4) 0.9160(3) 0.5675(4) 0.0871(16) Uani 1 1 d . . . H31A H 1.2005 0.9517 0.5216 0.131 Uiso 1 1 calc R . . H31B H 1.2241 0.8781 0.5300 0.131 Uiso 1 1 calc R . . H31C H 1.2722 0.9242 0.6182 0.131 Uiso 1 1 calc R . . H241 H 0.762(3) 0.802(2) 0.478(3) 0.061(14) Uiso 1 1 d . . . H291 H 0.883(4) 0.894(2) 0.517(4) 0.082(16) Uiso 1 1 d . . . H281 H 1.072(5) 0.809(3) 0.769(5) 0.10(2) Uiso 1 1 d . . . H243 H 0.754(5) 0.743(3) 0.524(5) 0.10(2) Uiso 1 1 d . . . H242 H 0.723(4) 0.750(3) 0.420(4) 0.087(16) Uiso 1 1 d . . . H282 H 1.127(5) 0.782(3) 0.686(5) 0.10(2) Uiso 1 1 d . . . H293 H 0.967(4) 0.940(3) 0.500(4) 0.083(15) Uiso 1 1 d . . . H283 H 1.173(4) 0.837(3) 0.752(4) 0.091(17) Uiso 1 1 d . . . H252 H 1.076(5) 0.776(3) 0.496(5) 0.11(2) Uiso 1 1 d . . . H251 H 1.074(4) 0.717(2) 0.433(5) 0.083(17) Uiso 1 1 d . . . H253 H 1.063(6) 0.710(3) 0.547(6) 0.15(3) Uiso 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 0.0400(2) 0.0344(2) 0.0439(2) 0.00226(15) 0.00838(14) 0.00267(15) Al1 0.0668(8) 0.0461(7) 0.0462(7) -0.0005(5) 0.0103(6) 0.0112(6) Al2 0.0547(8) 0.0467(7) 0.0666(8) 0.0003(6) 0.0130(6) -0.0097(6) N1 0.0426(17) 0.0292(15) 0.0463(18) 0.0040(12) 0.0082(13) 0.0032(12) N2 0.0472(18) 0.0366(16) 0.0513(19) -0.0005(14) 0.0134(14) 0.0070(14) C1 0.087(3) 0.061(3) 0.052(2) 0.011(2) 0.012(2) 0.012(2) C2 0.046(2) 0.044(2) 0.040(2) 0.0040(16) 0.0067(16) 0.0055(16) C3 0.060(3) 0.054(2) 0.041(2) -0.0075(17) 0.0057(18) 0.0059(19) C4 0.055(2) 0.042(2) 0.056(2) -0.0103(18) 0.0162(19) 0.0030(18) C5 0.093(4) 0.070(3) 0.060(3) -0.019(2) 0.010(2) 0.025(3) C6 0.050(2) 0.0301(18) 0.042(2) 0.0065(15) 0.0082(16) 0.0013(16) C7 0.055(2) 0.0352(19) 0.045(2) 0.0028(16) 0.0049(17) 0.0005(17) C8 0.076(3) 0.033(2) 0.069(3) -0.0002(19) 0.015(2) 0.003(2) C9 0.086(3) 0.037(2) 0.076(3) -0.010(2) 0.014(3) -0.014(2) C10 0.065(3) 0.048(2) 0.071(3) 0.002(2) 0.008(2) -0.016(2) C11 0.055(2) 0.046(2) 0.046(2) 0.0084(18) 0.0076(17) -0.0050(18) C12 0.049(2) 0.038(2) 0.068(3) -0.0037(18) 0.0074(19) 0.0058(17) C13 0.063(3) 0.064(3) 0.089(3) -0.003(3) 0.020(2) 0.007(2) C14 0.070(3) 0.080(3) 0.078(3) 0.004(3) -0.001(3) 0.010(3) C15 0.048(2) 0.057(3) 0.073(3) 0.012(2) 0.008(2) -0.004(2) C16 0.061(3) 0.096(4) 0.111(4) 0.012(3) -0.013(3) -0.004(3) C17 0.073(4) 0.117(5) 0.093(4) 0.028(3) 0.035(3) 0.013(3) C18 0.051(2) 0.040(2) 0.051(2) -0.0034(17) 0.0145(17) 0.0062(17) C19 0.060(3) 0.044(2) 0.086(3) -0.003(2) 0.020(2) 0.005(2) C20 0.075(3) 0.051(3) 0.090(3) 0.009(2) 0.016(3) 0.019(2) C21 0.062(3) 0.076(3) 0.060(3) -0.001(2) 0.004(2) 0.025(3) C22 0.049(3) 0.082(3) 0.066(3) -0.007(2) 0.010(2) 0.004(2) C23 0.053(3) 0.054(2) 0.065(3) 0.002(2) 0.016(2) 0.005(2) C24 0.056(3) 0.055(3) 0.049(3) -0.001(2) 0.006(2) 0.002(2) C25 0.064(3) 0.084(4) 0.059(3) -0.004(3) 0.015(2) 0.027(3) C26 0.109(4) 0.049(3) 0.064(3) 0.001(2) 0.006(3) 0.012(3) C27 0.077(3) 0.068(3) 0.059(3) 0.007(2) 0.015(2) 0.006(2) C28 0.051(3) 0.060(3) 0.066(3) 0.007(2) -0.006(2) -0.007(2) C29 0.065(3) 0.047(3) 0.074(3) 0.013(2) 0.009(2) -0.002(2) C30 0.093(4) 0.069(3) 0.107(4) -0.023(3) 0.018(3) -0.013(3) C31 0.077(4) 0.095(4) 0.094(4) -0.001(3) 0.029(3) -0.024(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 N2 2.277(3) . ? Y1 N1 2.339(3) . ? Y1 C28 2.535(5) . ? Y1 C24 2.548(5) . ? Y1 C25 2.573(5) . ? Y1 C29 2.621(5) . ? Y1 H241 2.61(4) . ? Y1 H291 2.62(5) . ? Y1 H243 2.54(6) . ? Y1 H282 2.51(6) . ? Y1 H252 2.52(6) . ? Y1 H253 2.50(7) . ? Al1 C26 1.960(5) . ? Al1 C27 1.966(5) . ? Al1 C25 2.065(6) . ? Al1 C24 2.075(5) . ? Al2 C30 1.971(5) . ? Al2 C31 1.958(5) . ? Al2 C28 2.071(5) . ? Al2 C29 2.061(5) . ? N1 C2 1.324(5) . ? N1 C6 1.459(4) . ? N2 C4 1.349(5) . ? N2 C18 1.443(5) . ? C1 C2 1.515(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.405(5) . ? C3 C4 1.389(6) . ? C3 H3 0.9300 . ? C4 C5 1.519(5) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.398(5) . ? C6 C11 1.407(5) . ? C7 C8 1.396(5) . ? C7 C12 1.523(5) . ? C8 C9 1.361(6) . ? C8 H8 0.9300 . ? C9 C10 1.374(6) . ? C9 H9 0.9300 . ? C10 C11 1.387(6) . ? C10 H10 0.9300 . ? C11 C15 1.520(6) . ? C12 C13 1.528(6) . ? C12 C14 1.540(6) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C17 1.527(6) . ? C15 C16 1.539(6) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C23 1.375(6) . ? C18 C19 1.390(6) . ? C19 C20 1.379(6) . ? C19 H19 0.9300 . ? C20 C21 1.359(7) . ? C20 H20 0.9300 . ? C21 C22 1.371(7) . ? C21 H21 0.9300 . ? C22 C23 1.376(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H241 0.89(5) . ? C24 H243 0.87(6) . ? C24 H242 0.92(6) . ? C25 H252 1.01(6) . ? C25 H251 0.88(6) . ? C25 H253 1.02(8) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H281 0.92(6) . ? C28 H282 0.91(6) . ? C28 H283 0.97(6) . ? C29 H292 0.90(6) . ? C29 H291 0.95(5) . ? C29 H293 0.99(5) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 N2 Y1 N1 80.66(10) . . ? N2 Y1 C28 97.05(17) . . ? N1 Y1 C28 89.44(13) . . ? N2 Y1 C24 91.72(13) . . ? N1 Y1 C24 100.94(14) . . ? C28 Y1 C24 167.40(17) . . ? N2 Y1 C25 174.00(15) . . ? N1 Y1 C25 99.86(16) . . ? C28 Y1 C25 88.9(2) . . ? C24 Y1 C25 82.31(17) . . ? N2 Y1 C29 93.55(16) . . ? N1 Y1 C29 169.09(14) . . ? C28 Y1 C29 82.07(16) . . ? C24 Y1 C29 88.39(17) . . ? C25 Y1 C29 86.9(2) . . ? N2 Y1 H241 80.0(10) . . ? N1 Y1 H241 114.3(10) . . ? C28 Y1 H241 154.9(11) . . ? C24 Y1 H241 19.8(10) . . ? C25 Y1 H241 94.4(10) . . ? C29 Y1 H241 73.3(10) . . ? N2 Y1 H291 79.4(12) . . ? N1 Y1 H291 159.1(12) . . ? C28 Y1 H291 98.9(12) . . ? C24 Y1 H291 73.7(11) . . ? C25 Y1 H291 99.4(12) . . ? C29 Y1 H291 20.9(12) . . ? H241 Y1 H291 56.0(15) . . ? N2 Y1 H243 79.7(14) . . ? N1 Y1 H243 83.7(15) . . ? C28 Y1 H243 172.8(15) . . ? C24 Y1 H243 19.6(14) . . ? C25 Y1 H243 94.4(14) . . ? C29 Y1 H243 104.5(15) . . ? H241 Y1 H243 31.2(16) . . ? H291 Y1 H243 86.9(18) . . ? N2 Y1 H282 114.7(14) . . ? N1 Y1 H282 82.0(13) . . ? C28 Y1 H282 20.8(13) . . ? C24 Y1 H282 153.5(14) . . ? C25 Y1 H282 71.2(14) . . ? C29 Y1 H282 92.2(13) . . ? H241 Y1 H282 160.4(17) . . ? H291 Y1 H282 112.0(18) . . ? H243 Y1 H282 157.6(19) . . ? N2 Y1 H252 160.8(14) . . ? N1 Y1 H252 114.9(14) . . ? C28 Y1 H252 73.0(15) . . ? C24 Y1 H252 96.0(15) . . ? C25 Y1 H252 22.7(14) . . ? C29 Y1 H252 69.2(14) . . ? H241 Y1 H252 101.9(17) . . ? H291 Y1 H252 85.9(18) . . ? H243 Y1 H252 112(2) . . ? H282 Y1 H252 60(2) . . ? N2 Y1 H253 159.5(18) . . ? N1 Y1 H253 79.3(18) . . ? C28 Y1 H253 78.3(17) . . ? C24 Y1 H253 96.5(18) . . ? C25 Y1 H253 23.1(18) . . ? C29 Y1 H253 105.4(18) . . ? H241 Y1 H253 113(2) . . ? H291 Y1 H253 121(2) . . ? H243 Y1 H253 102(2) . . ? H282 Y1 H253 58(2) . . ? H252 Y1 H253 36(2) . . ? C26 Al1 C27 117.6(2) . . ? C26 Al1 C25 105.4(2) . . ? C27 Al1 C25 107.8(2) . . ? C26 Al1 C24 109.5(2) . . ? C27 Al1 C24 107.3(2) . . ? C25 Al1 C24 109.0(2) . . ? C30 Al2 C31 117.6(3) . . ? C30 Al2 C28 106.5(3) . . ? C31 Al2 C28 106.2(3) . . ? C30 Al2 C29 110.3(3) . . ? C31 Al2 C29 106.1(3) . . ? C28 Al2 C29 110.0(2) . . ? C2 N1 C6 118.1(3) . . ? C2 N1 Y1 118.6(2) . . ? C6 N1 Y1 123.3(2) . . ? C4 N2 C18 116.4(3) . . ? C4 N2 Y1 117.0(2) . . ? C18 N2 Y1 126.1(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.5(3) . . ? N1 C2 C1 121.7(3) . . ? C3 C2 C1 114.8(3) . . ? C4 C3 C2 129.5(4) . . ? C4 C3 H3 115.3 . . ? C2 C3 H3 115.3 . . ? N2 C4 C3 123.7(3) . . ? N2 C4 C5 120.1(4) . . ? C3 C4 C5 116.2(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 121.3(3) . . ? C7 C6 N1 121.4(3) . . ? C11 C6 N1 117.3(3) . . ? C8 C7 C6 117.7(4) . . ? C8 C7 C12 117.5(4) . . ? C6 C7 C12 124.8(3) . . ? C9 C8 C7 121.6(4) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C10 120.3(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 121.1(4) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 118.1(4) . . ? C10 C11 C15 119.0(4) . . ? C6 C11 C15 122.8(4) . . ? C7 C12 C13 112.6(3) . . ? C7 C12 C14 111.8(4) . . ? C13 C12 C14 107.8(4) . . ? C7 C12 H12 108.2 . . ? C13 C12 H12 108.2 . . ? C14 C12 H12 108.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 111.0(4) . . ? C11 C15 C16 113.8(4) . . ? C17 C15 C16 109.8(4) . . ? C11 C15 H15 107.3 . . ? C17 C15 H15 107.3 . . ? C16 C15 H15 107.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 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 . . ? C23 C18 C19 118.8(4) . . ? C23 C18 N2 119.6(3) . . ? C19 C18 N2 121.6(4) . . ? C20 C19 C18 119.5(4) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C21 C20 C19 121.4(5) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 119.1(4) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C21 C22 C23 120.6(4) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C18 120.5(4) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? Al1 C24 Y1 84.56(16) . . ? Al1 C24 H241 127(3) . . ? Y1 C24 H241 84(3) . . ? Al1 C24 H243 124(4) . . ? Y1 C24 H243 80(4) . . ? H241 C24 H243 104(5) . . ? Al1 C24 H242 92(3) . . ? Y1 C24 H242 176(3) . . ? H241 C24 H242 99(4) . . ? H243 C24 H242 102(5) . . ? Al1 C25 Y1 84.13(17) . . ? Al1 C25 H252 125(4) . . ? Y1 C25 H252 76(4) . . ? Al1 C25 H251 93(4) . . ? Y1 C25 H251 176(4) . . ? H252 C25 H251 104(5) . . ? Al1 C25 H253 122(4) . . ? Y1 C25 H253 74(4) . . ? H252 C25 H253 101(5) . . ? H251 C25 H253 109(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 84.45(16) . . ? Al2 C28 H281 123(4) . . ? Y1 C28 H281 83(4) . . ? Al2 C28 H282 122(4) . . ? Y1 C28 H282 78(4) . . ? H281 C28 H282 109(5) . . ? Al2 C28 H283 89(3) . . ? Y1 C28 H283 173(3) . . ? H281 C28 H283 99(4) . . ? H282 C28 H283 107(5) . . ? Al2 C29 Y1 82.47(16) . . ? Al2 C29 H292 114(4) . . ? Y1 C29 H292 86(4) . . ? Al2 C29 H291 134(3) . . ? Y1 C29 H291 79(3) . . ? H292 C29 H291 107(5) . . ? Al2 C29 H293 89(3) . . ? Y1 C29 H293 166(3) . . ? H292 C29 H293 107(5) . . ? H291 C29 H293 99(4) . . ? 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 N2 Y1 N1 C2 -42.3(3) . . . . ? C28 Y1 N1 C2 55.0(3) . . . . ? C24 Y1 N1 C2 -132.2(3) . . . . ? C25 Y1 N1 C2 143.8(3) . . . . ? C29 Y1 N1 C2 16.2(9) . . . . ? N2 Y1 N1 C6 138.5(3) . . . . ? C28 Y1 N1 C6 -124.3(3) . . . . ? C24 Y1 N1 C6 48.5(3) . . . . ? C25 Y1 N1 C6 -35.5(3) . . . . ? C29 Y1 N1 C6 -163.0(7) . . . . ? N1 Y1 N2 C4 47.8(3) . . . . ? C28 Y1 N2 C4 -40.5(3) . . . . ? C24 Y1 N2 C4 148.6(3) . . . . ? C25 Y1 N2 C4 143.2(15) . . . . ? C29 Y1 N2 C4 -122.9(3) . . . . ? N1 Y1 N2 C18 -139.7(3) . . . . ? C28 Y1 N2 C18 132.1(3) . . . . ? C24 Y1 N2 C18 -38.9(3) . . . . ? C25 Y1 N2 C18 -44.2(16) . . . . ? C29 Y1 N2 C18 49.6(3) . . . . ? C6 N1 C2 C3 -163.2(4) . . . . ? Y1 N1 C2 C3 17.5(5) . . . . ? C6 N1 C2 C1 14.9(5) . . . . ? Y1 N1 C2 C1 -164.5(3) . . . . ? N1 C2 C3 C4 25.4(7) . . . . ? C1 C2 C3 C4 -152.8(5) . . . . ? C18 N2 C4 C3 156.2(4) . . . . ? Y1 N2 C4 C3 -30.5(5) . . . . ? C18 N2 C4 C5 -22.8(6) . . . . ? Y1 N2 C4 C5 150.4(3) . . . . ? C2 C3 C4 N2 -18.0(7) . . . . ? C2 C3 C4 C5 161.1(4) . . . . ? C2 N1 C6 C7 -90.8(4) . . . . ? Y1 N1 C6 C7 88.5(4) . . . . ? C2 N1 C6 C11 90.7(4) . . . . ? Y1 N1 C6 C11 -90.0(3) . . . . ? C11 C6 C7 C8 -0.1(5) . . . . ? N1 C6 C7 C8 -178.6(3) . . . . ? C11 C6 C7 C12 -177.1(3) . . . . ? N1 C6 C7 C12 4.4(6) . . . . ? C6 C7 C8 C9 0.6(6) . . . . ? C12 C7 C8 C9 177.8(4) . . . . ? C7 C8 C9 C10 -0.8(7) . . . . ? C8 C9 C10 C11 0.4(7) . . . . ? C9 C10 C11 C6 0.0(6) . . . . ? C9 C10 C11 C15 -175.9(4) . . . . ? C7 C6 C11 C10 -0.2(6) . . . . ? N1 C6 C11 C10 178.4(3) . . . . ? C7 C6 C11 C15 175.6(3) . . . . ? N1 C6 C11 C15 -5.9(5) . . . . ? C8 C7 C12 C13 53.6(5) . . . . ? C6 C7 C12 C13 -129.5(4) . . . . ? C8 C7 C12 C14 -68.0(5) . . . . ? C6 C7 C12 C14 109.0(4) . . . . ? C10 C11 C15 C17 82.0(5) . . . . ? C6 C11 C15 C17 -93.7(5) . . . . ? C10 C11 C15 C16 -42.5(5) . . . . ? C6 C11 C15 C16 141.8(4) . . . . ? C4 N2 C18 C23 -78.2(5) . . . . ? Y1 N2 C18 C23 109.2(4) . . . . ? C4 N2 C18 C19 101.8(4) . . . . ? Y1 N2 C18 C19 -70.8(5) . . . . ? C23 C18 C19 C20 -1.2(6) . . . . ? N2 C18 C19 C20 178.8(4) . . . . ? C18 C19 C20 C21 1.1(7) . . . . ? C19 C20 C21 C22 -0.2(7) . . . . ? C20 C21 C22 C23 -0.6(7) . . . . ? C21 C22 C23 C18 0.4(7) . . . . ? C19 C18 C23 C22 0.4(6) . . . . ? N2 C18 C23 C22 -179.5(4) . . . . ? C26 Al1 C24 Y1 112.82(19) . . . . ? C27 Al1 C24 Y1 -118.45(19) . . . . ? C25 Al1 C24 Y1 -2.0(3) . . . . ? N2 Y1 C24 Al1 -177.91(16) . . . . ? N1 Y1 C24 Al1 -97.10(16) . . . . ? C28 Y1 C24 Al1 47.9(9) . . . . ? C25 Y1 C24 Al1 1.5(2) . . . . ? C29 Y1 C24 Al1 88.6(2) . . . . ? C26 Al1 C25 Y1 -115.4(2) . . . . ? C27 Al1 C25 Y1 118.11(19) . . . . ? C24 Al1 C25 Y1 2.0(3) . . . . ? N2 Y1 C25 Al1 3.9(17) . . . . ? N1 Y1 C25 Al1 98.32(18) . . . . ? C28 Y1 C25 Al1 -172.4(2) . . . . ? C24 Y1 C25 Al1 -1.5(2) . . . . ? C29 Y1 C25 Al1 -90.3(2) . . . . ? C30 Al2 C28 Y1 110.8(2) . . . . ? C31 Al2 C28 Y1 -123.1(2) . . . . ? C29 Al2 C28 Y1 -8.7(3) . . . . ? N2 Y1 C28 Al2 -86.12(19) . . . . ? N1 Y1 C28 Al2 -166.63(19) . . . . ? C24 Y1 C28 Al2 47.6(9) . . . . ? C25 Y1 C28 Al2 93.5(2) . . . . ? C29 Y1 C28 Al2 6.5(2) . . . . ? C30 Al2 C29 Y1 -108.7(2) . . . . ? C31 Al2 C29 Y1 122.9(2) . . . . ? C28 Al2 C29 Y1 8.5(3) . . . . ? N2 Y1 C29 Al2 90.07(18) . . . . ? N1 Y1 C29 Al2 32.6(9) . . . . ? C28 Y1 C29 Al2 -6.6(2) . . . . ? C24 Y1 C29 Al2 -178.3(2) . . . . ? C25 Y1 C29 Al2 -95.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.431 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.051 #======================================================end of cif _database_code_depnum_ccdc_archive 'CCDC 952933'