# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dongmei Cui' _publ_contact_author_email DMCUI@CIAC.JL.CN _publ_section_title ; The Behavior of Pyrrolyl Ligands within the Rare-Earth Metal Alkyl Complexes. Insertion of C=N and C=O Double Bonds into Ln-C Bonds ; loop_ _publ_author_name 'Dongmei Cui' 'Xuesi Chen' 'Yi Yang' #===========END============= data_5 _database_code_depnum_ccdc_archive 'CCDC 298639' #TrackingRef 'complexes_1-61.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H61 N2 O Si2 Y' _chemical_formula_weight 694.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.1398(6) _cell_length_b 18.4371(11) _cell_length_c 20.6375(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3858.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 1.602 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6142 _exptl_absorpt_correction_T_max 0.8934 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23028 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0952 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.05 _reflns_number_total 7613 _reflns_number_gt 5760 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1364P)^2^+15.8970P] 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 -0.030(8) _refine_ls_number_reflns 7613 _refine_ls_number_parameters 402 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1439 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 0.582 _refine_ls_restrained_S_all 0.582 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y Y 1.00951(4) 1.04533(2) 0.927570(19) 0.02424(12) Uani 1 1 d . . . N1 N 0.9058(4) 0.9173(2) 0.9275(2) 0.0264(8) Uani 1 1 d . . . N2 N 0.8114(4) 1.0455(2) 0.98649(19) 0.0291(8) Uani 1 1 d . . . O O 1.1965(3) 0.97273(19) 0.90043(17) 0.0356(9) Uani 1 1 d . . . Si1 Si 1.12584(19) 1.05184(11) 1.10591(7) 0.0494(4) Uani 1 1 d . . . Si2 Si 0.70984(15) 1.13425(9) 0.82730(7) 0.0363(4) Uani 1 1 d . . . C1 C 0.9480(5) 0.8449(3) 0.9099(2) 0.0275(11) Uani 1 1 d . . . C2 C 0.9215(6) 0.8165(3) 0.8482(3) 0.0365(12) Uani 1 1 d . . . C3 C 0.9627(6) 0.7462(3) 0.8342(3) 0.0452(15) Uani 1 1 d . . . H3 H 0.9473 0.7273 0.7931 0.054 Uiso 1 1 calc R . . C4 C 1.0253(6) 0.7043(3) 0.8794(3) 0.0485(15) Uani 1 1 d . . . H4 H 1.0510 0.6572 0.8694 0.058 Uiso 1 1 calc R . . C5 C 1.0499(6) 0.7329(3) 0.9400(3) 0.0436(14) Uani 1 1 d . . . H5 H 1.0921 0.7040 0.9706 0.052 Uiso 1 1 calc R . . C6 C 1.0143(5) 0.8022(3) 0.9568(2) 0.0315(10) Uani 1 1 d . . . C7 C 0.8472(6) 0.8601(3) 0.7975(3) 0.0443(14) Uani 1 1 d . . . H7 H 0.8517 0.9113 0.8103 0.053 Uiso 1 1 calc R . . C8 C 0.9052(9) 0.8539(4) 0.7296(3) 0.065(2) Uani 1 1 d . . . H8A H 0.8924 0.8055 0.7137 0.098 Uiso 1 1 calc R . . H8B H 0.9978 0.8646 0.7311 0.098 Uiso 1 1 calc R . . H8C H 0.8619 0.8877 0.7014 0.098 Uiso 1 1 calc R . . C9 C 0.7009(7) 0.8378(4) 0.7975(4) 0.065(2) Uani 1 1 d . . . H9A H 0.6639 0.8463 0.8397 0.098 Uiso 1 1 calc R . . H9B H 0.6938 0.7872 0.7871 0.098 Uiso 1 1 calc R . . H9C H 0.6540 0.8659 0.7659 0.098 Uiso 1 1 calc R . . C10 C 1.0432(5) 0.8306(3) 1.0242(3) 0.0367(12) Uani 1 1 d . . . H10 H 1.0455 0.8837 1.0219 0.044 Uiso 1 1 calc R . . C11 C 0.9364(7) 0.8096(4) 1.0721(3) 0.0605(17) Uani 1 1 d . . . H11A H 0.9326 0.7578 1.0756 0.091 Uiso 1 1 calc R . . H11B H 0.8529 0.8277 1.0572 0.091 Uiso 1 1 calc R . . H11C H 0.9561 0.8302 1.1137 0.091 Uiso 1 1 calc R . . C12 C 1.1765(7) 0.8050(4) 1.0500(3) 0.066(2) Uani 1 1 d . . . H12A H 1.2447 0.8187 1.0201 0.099 Uiso 1 1 calc R . . H12B H 1.1756 0.7532 1.0547 0.099 Uiso 1 1 calc R . . H12C H 1.1931 0.8271 1.0913 0.099 Uiso 1 1 calc R . . C13 C 0.7934(5) 0.9195(3) 0.9588(2) 0.0310(11) Uani 1 1 d . . . H13 H 0.7451 0.8767 0.9618 0.037 Uiso 1 1 calc R . . C14 C 0.7405(5) 0.9817(3) 0.9883(2) 0.0296(11) Uani 1 1 d . . . C15 C 0.6286(5) 0.9889(3) 1.0277(3) 0.0391(13) Uani 1 1 d . . . H15 H 0.5656 0.9536 1.0365 0.047 Uiso 1 1 calc R . . C16 C 0.6309(6) 1.0585(3) 1.0506(3) 0.0474(15) Uani 1 1 d . . . H16 H 0.5693 1.0798 1.0780 0.057 Uiso 1 1 calc R . . C17 C 0.7425(6) 1.0912(3) 1.0251(3) 0.0435(14) Uani 1 1 d . . . H17 H 0.7672 1.1388 1.0335 0.052 Uiso 1 1 calc R . . C18 C 0.9880(5) 1.0991(3) 0.8077(2) 0.0303(10) Uani 1 1 d . . . C19 C 1.1146(5) 1.1242(3) 0.8279(2) 0.0316(12) Uani 1 1 d . . . C20 C 1.0962(5) 1.1741(3) 0.8784(2) 0.0328(12) Uani 1 1 d . . . C21 C 0.9600(5) 1.1820(3) 0.8901(2) 0.0300(11) Uani 1 1 d . . . C22 C 0.8900(5) 1.1350(3) 0.8468(2) 0.0298(11) Uani 1 1 d . . . C23 C 1.2448(6) 1.1088(4) 0.7948(3) 0.0475(15) Uani 1 1 d . . . H23A H 1.3092 1.0954 0.8267 0.071 Uiso 1 1 calc R . . H23B H 1.2740 1.1514 0.7723 0.071 Uiso 1 1 calc R . . H23C H 1.2337 1.0698 0.7645 0.071 Uiso 1 1 calc R . . C24 C 1.2059(6) 1.2172(3) 0.9104(3) 0.0453(15) Uani 1 1 d . . . H24A H 1.2277 1.2583 0.8839 0.068 Uiso 1 1 calc R . . H24B H 1.2823 1.1870 0.9153 0.068 Uiso 1 1 calc R . . H24C H 1.1771 1.2336 0.9522 0.068 Uiso 1 1 calc R . . C25 C 0.9053(6) 1.2368(3) 0.9364(3) 0.0419(13) Uani 1 1 d . . . H25A H 0.9046 1.2837 0.9161 0.063 Uiso 1 1 calc R . . H25B H 0.9592 1.2384 0.9746 0.063 Uiso 1 1 calc R . . H25C H 0.8169 1.2235 0.9480 0.063 Uiso 1 1 calc R . . C26 C 0.9653(5) 1.0508(3) 0.7502(2) 0.0393(12) Uani 1 1 d . . . H26A H 1.0130 1.0063 0.7558 0.059 Uiso 1 1 calc R . . H26B H 0.9954 1.0747 0.7116 0.059 Uiso 1 1 calc R . . H26C H 0.8728 1.0404 0.7463 0.059 Uiso 1 1 calc R . . C27 C 0.6859(7) 1.1824(4) 0.7489(3) 0.0557(17) Uani 1 1 d . . . H27A H 0.7298 1.2285 0.7504 0.084 Uiso 1 1 calc R . . H27B H 0.5934 1.1898 0.7415 0.084 Uiso 1 1 calc R . . H27C H 0.7221 1.1538 0.7143 0.084 Uiso 1 1 calc R . . C28 C 0.6025(6) 1.1797(5) 0.8886(3) 0.063(2) Uani 1 1 d . . . H28A H 0.5128 1.1796 0.8737 0.095 Uiso 1 1 calc R . . H28B H 0.6314 1.2289 0.8947 0.095 Uiso 1 1 calc R . . H28C H 0.6080 1.1541 0.9290 0.095 Uiso 1 1 calc R . . C29 C 0.6433(6) 1.0403(4) 0.8190(3) 0.0576(17) Uani 1 1 d . . . H29A H 0.6894 1.0155 0.7850 0.086 Uiso 1 1 calc R . . H29B H 0.5510 1.0425 0.8087 0.086 Uiso 1 1 calc R . . H29C H 0.6552 1.0147 0.8590 0.086 Uiso 1 1 calc R . . C30 C 1.1169(6) 1.0890(3) 1.0238(2) 0.0352(12) Uani 1 1 d . . . H30A H 1.2083 1.0952 1.0110 0.042 Uiso 1 1 calc R . . H30B H 1.0824 1.1376 1.0296 0.042 Uiso 1 1 calc R . . C31 C 1.1548(13) 1.1209(5) 1.1696(4) 0.118(5) Uani 1 1 d . . . H31A H 1.0926 1.1598 1.1647 0.177 Uiso 1 1 calc R . . H31B H 1.2428 1.1396 1.1656 0.177 Uiso 1 1 calc R . . H31C H 1.1440 1.0991 1.2115 0.177 Uiso 1 1 calc R . . C32 C 0.9742(7) 1.0023(4) 1.1313(3) 0.0623(19) Uani 1 1 d . . . H32A H 0.9531 0.9661 1.0995 0.094 Uiso 1 1 calc R . . H32B H 0.9022 1.0359 1.1350 0.094 Uiso 1 1 calc R . . H32C H 0.9891 0.9794 1.1724 0.094 Uiso 1 1 calc R . . C33 C 1.2707(8) 0.9867(5) 1.1128(4) 0.089(3) Uani 1 1 d . . . H33A H 1.3518 1.0135 1.1103 0.134 Uiso 1 1 calc R . . H33B H 1.2671 0.9522 1.0780 0.134 Uiso 1 1 calc R . . H33C H 1.2663 0.9617 1.1535 0.134 Uiso 1 1 calc R . . C34 C 1.3234(6) 0.9755(4) 0.9324(3) 0.0543(16) Uani 1 1 d . . . H34A H 1.3121 0.9753 0.9791 0.065 Uiso 1 1 calc R . . H34B H 1.3702 1.0194 0.9202 0.065 Uiso 1 1 calc R . . C35 C 1.3981(7) 0.9106(4) 0.9114(4) 0.0616(19) Uani 1 1 d . . . H35A H 1.4140 0.8783 0.9476 0.074 Uiso 1 1 calc R . . H35B H 1.4822 0.9243 0.8926 0.074 Uiso 1 1 calc R . . C36 C 1.3102(10) 0.8742(5) 0.8608(4) 0.097(3) Uani 1 1 d . . . H36A H 1.3612 0.8612 0.8227 0.117 Uiso 1 1 calc R . . H36B H 1.2705 0.8306 0.8784 0.117 Uiso 1 1 calc R . . C37 C 1.2117(6) 0.9254(4) 0.8445(3) 0.0492(15) Uani 1 1 d . . . H37A H 1.1292 0.9010 0.8349 0.059 Uiso 1 1 calc R . . H37B H 1.2381 0.9532 0.8067 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.0270(2) 0.0250(2) 0.02072(19) 0.00013(17) 0.00025(19) 0.0006(2) N1 0.0277(19) 0.028(2) 0.0240(19) 0.0011(17) 0.0038(19) 0.0029(16) N2 0.030(2) 0.027(2) 0.030(2) -0.0034(19) 0.0063(16) -0.001(2) O 0.0285(18) 0.042(2) 0.0365(19) -0.0043(16) 0.0036(15) 0.0064(15) Si1 0.0705(11) 0.0517(10) 0.0261(7) 0.0027(7) -0.0083(7) -0.0128(10) Si2 0.0283(8) 0.0473(9) 0.0334(8) 0.0048(7) -0.0046(6) 0.0037(7) C1 0.030(2) 0.024(2) 0.029(3) -0.0002(18) 0.0100(19) 0.0002(19) C2 0.044(3) 0.032(3) 0.033(3) -0.007(2) 0.006(2) 0.001(2) C3 0.052(4) 0.038(3) 0.045(3) -0.018(3) 0.012(3) -0.002(3) C4 0.056(4) 0.029(3) 0.061(4) -0.008(2) 0.007(3) 0.006(3) C5 0.046(3) 0.030(3) 0.055(4) 0.007(2) 0.004(3) 0.006(2) C6 0.027(3) 0.029(2) 0.039(3) -0.0021(19) 0.007(2) 0.001(2) C7 0.067(4) 0.033(3) 0.032(3) -0.007(2) -0.007(3) -0.002(3) C8 0.105(6) 0.059(4) 0.031(3) -0.014(3) 0.000(4) -0.003(4) C9 0.067(5) 0.062(4) 0.067(5) -0.001(4) -0.019(4) 0.003(4) C10 0.042(3) 0.028(3) 0.041(3) 0.003(2) 0.000(2) 0.007(2) C11 0.081(5) 0.060(4) 0.040(3) 0.004(3) 0.008(4) -0.015(4) C12 0.065(5) 0.073(5) 0.060(4) -0.007(4) -0.027(4) 0.023(4) C13 0.034(3) 0.029(3) 0.030(3) 0.005(2) 0.002(2) -0.007(2) C14 0.029(3) 0.031(3) 0.029(3) -0.004(2) 0.002(2) 0.004(2) C15 0.033(3) 0.039(3) 0.045(3) -0.001(3) 0.011(2) 0.000(2) C16 0.046(3) 0.053(4) 0.044(3) -0.010(3) 0.016(3) 0.009(3) C17 0.047(3) 0.036(3) 0.048(3) -0.011(3) 0.009(3) 0.005(3) C18 0.031(3) 0.038(2) 0.023(2) 0.0026(18) 0.000(2) 0.000(2) C19 0.028(3) 0.040(3) 0.028(3) 0.009(2) 0.004(2) -0.003(2) C20 0.038(3) 0.031(3) 0.029(3) 0.004(2) -0.008(2) -0.006(2) C21 0.039(3) 0.022(2) 0.029(3) 0.0022(19) -0.003(2) 0.001(2) C22 0.032(3) 0.031(3) 0.026(3) 0.011(2) -0.002(2) 0.001(2) C23 0.035(3) 0.058(4) 0.049(4) 0.018(3) 0.009(3) 0.002(3) C24 0.050(3) 0.043(3) 0.043(3) 0.006(3) -0.012(3) -0.016(3) C25 0.055(3) 0.030(3) 0.040(3) -0.003(2) -0.001(3) 0.008(2) C26 0.047(3) 0.039(3) 0.032(3) 0.000(2) 0.002(2) -0.002(3) C27 0.051(4) 0.072(4) 0.045(4) 0.012(3) -0.011(3) 0.012(3) C28 0.036(3) 0.104(6) 0.050(4) -0.001(4) 0.001(3) 0.018(4) C29 0.040(3) 0.061(4) 0.072(4) 0.013(4) -0.015(3) -0.010(3) C30 0.041(3) 0.038(3) 0.026(3) 0.004(2) -0.002(2) -0.008(2) C31 0.230(13) 0.084(6) 0.040(4) -0.003(4) -0.032(6) -0.061(8) C32 0.075(5) 0.074(4) 0.039(3) 0.009(3) 0.015(3) -0.002(4) C33 0.073(5) 0.124(8) 0.070(5) 0.055(5) -0.014(4) 0.008(5) C34 0.041(3) 0.064(4) 0.057(4) -0.010(3) -0.016(3) 0.012(3) C35 0.046(4) 0.053(4) 0.086(6) -0.001(4) -0.001(4) 0.010(3) C36 0.128(8) 0.094(6) 0.070(5) -0.039(5) -0.030(5) 0.067(6) C37 0.046(4) 0.054(4) 0.047(4) -0.016(3) 0.009(3) 0.003(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 Y N2 2.348(4) . ? Y O 2.388(3) . ? Y C30 2.404(5) . ? Y N1 2.585(4) . ? Y C22 2.642(5) . ? Y C18 2.675(4) . ? Y C21 2.682(5) . ? Y C20 2.728(5) . ? Y C19 2.736(5) . ? N1 C13 1.311(6) . ? N1 C1 1.448(6) . ? N2 C17 1.353(7) . ? N2 C14 1.379(6) . ? O C34 1.446(6) . ? O C37 1.456(7) . ? Si1 C30 1.830(5) . ? Si1 C32 1.864(7) . ? Si1 C31 1.854(8) . ? Si1 C33 1.902(9) . ? Si2 C27 1.862(6) . ? Si2 C29 1.866(7) . ? Si2 C28 1.869(7) . ? Si2 C22 1.871(5) . ? C1 C2 1.403(7) . ? C1 C6 1.417(7) . ? C2 C3 1.392(7) . ? C2 C7 1.519(8) . ? C3 C4 1.367(9) . ? C3 H3 0.9300 . ? C4 C5 1.380(8) . ? C4 H4 0.9300 . ? C5 C6 1.373(7) . ? C5 H5 0.9300 . ? C6 C10 1.516(7) . ? C7 C8 1.524(8) . ? C7 C9 1.540(10) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.515(8) . ? C10 C12 1.527(8) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.404(7) . ? C13 H13 0.9300 . ? C14 C15 1.403(7) . ? C15 C16 1.367(8) . ? C15 H15 0.9300 . ? C16 C17 1.386(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.427(7) . ? C18 C22 1.440(7) . ? C18 C26 1.502(7) . ? C19 C20 1.402(7) . ? C19 C23 1.513(8) . ? C20 C21 1.409(8) . ? C20 C24 1.518(7) . ? C21 C22 1.434(7) . ? C21 C25 1.498(7) . ? 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 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.482(9) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.528(11) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.414(10) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 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 N2 Y O 143.30(14) . . ? N2 Y C30 87.68(17) . . ? O Y C30 91.23(17) . . ? N2 Y N1 69.72(13) . . ? O Y N1 79.12(12) . . ? C30 Y N1 119.37(15) . . ? N2 Y C22 86.19(15) . . ? O Y C22 124.52(14) . . ? C30 Y C22 121.34(17) . . ? N1 Y C22 112.61(15) . . ? N2 Y C18 114.12(15) . . ? O Y C18 93.19(14) . . ? C30 Y C18 132.63(17) . . ? N1 Y C18 107.76(14) . . ? C22 Y C18 31.43(15) . . ? N2 Y C21 89.29(15) . . ? O Y C21 127.40(14) . . ? C30 Y C21 90.50(17) . . ? N1 Y C21 141.40(14) . . ? C22 Y C21 31.23(15) . . ? C18 Y C21 50.95(15) . . ? N2 Y C20 117.84(16) . . ? O Y C20 98.31(15) . . ? C30 Y C20 82.54(16) . . ? N1 Y C20 157.82(14) . . ? C22 Y C20 50.83(16) . . ? C18 Y C20 50.15(15) . . ? C21 Y C20 30.19(17) . . ? N2 Y C19 136.20(15) . . ? O Y C19 79.18(15) . . ? C30 Y C19 105.47(17) . . ? N1 Y C19 130.09(15) . . ? C22 Y C19 51.05(15) . . ? C18 Y C19 30.57(16) . . ? C21 Y C19 49.97(16) . . ? C20 Y C19 29.74(16) . . ? C13 N1 C1 114.2(4) . . ? C13 N1 Y 109.0(3) . . ? C1 N1 Y 136.2(3) . . ? C17 N2 C14 104.3(4) . . ? C17 N2 Y 138.4(4) . . ? C14 N2 Y 117.3(3) . . ? C34 O C37 106.8(4) . . ? C34 O Y 125.4(3) . . ? C37 O Y 127.3(3) . . ? C30 Si1 C32 113.7(3) . . ? C30 Si1 C31 114.1(3) . . ? C32 Si1 C31 105.6(4) . . ? C30 Si1 C33 110.0(3) . . ? C32 Si1 C33 107.9(4) . . ? C31 Si1 C33 105.0(5) . . ? C27 Si2 C29 108.4(3) . . ? C27 Si2 C28 107.4(3) . . ? C29 Si2 C28 105.5(4) . . ? C27 Si2 C22 108.1(3) . . ? C29 Si2 C22 112.3(3) . . ? C28 Si2 C22 114.9(3) . . ? C2 C1 C6 120.2(4) . . ? C2 C1 N1 121.0(4) . . ? C6 C1 N1 118.8(4) . . ? C3 C2 C1 118.6(5) . . ? C3 C2 C7 119.9(5) . . ? C1 C2 C7 121.5(5) . . ? C4 C3 C2 121.6(5) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 119.1(5) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 122.4(5) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C1 118.0(5) . . ? C5 C6 C10 120.2(5) . . ? C1 C6 C10 121.8(4) . . ? C2 C7 C8 113.7(6) . . ? C2 C7 C9 109.6(5) . . ? C8 C7 C9 110.6(6) . . ? C2 C7 H7 107.6 . . ? C8 C7 H7 107.6 . . ? C9 C7 H7 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C11 111.8(5) . . ? C6 C10 C12 112.5(5) . . ? C11 C10 C12 109.1(5) . . ? C6 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 124.8(5) . . ? N1 C13 H13 117.6 . . ? C14 C13 H13 117.6 . . ? N2 C14 C13 119.1(4) . . ? N2 C14 C15 110.8(4) . . ? C13 C14 C15 129.6(5) . . ? C16 C15 C14 106.0(5) . . ? C16 C15 H15 127.0 . . ? C14 C15 H15 127.0 . . ? C15 C16 C17 106.9(5) . . ? C15 C16 H16 126.5 . . ? C17 C16 H16 126.5 . . ? N2 C17 C16 112.0(5) . . ? N2 C17 H17 124.0 . . ? C16 C17 H17 124.0 . . ? C19 C18 C22 107.9(4) . . ? C19 C18 C26 124.2(5) . . ? C22 C18 C26 127.5(5) . . ? C19 C18 Y 77.1(3) . . ? C22 C18 Y 73.0(3) . . ? C26 C18 Y 121.6(3) . . ? C20 C19 C18 108.1(4) . . ? C20 C19 C23 125.1(5) . . ? C18 C19 C23 126.3(5) . . ? C20 C19 Y 74.8(3) . . ? C18 C19 Y 72.3(3) . . ? C23 C19 Y 125.4(4) . . ? C19 C20 C21 109.0(5) . . ? C19 C20 C24 124.7(5) . . ? C21 C20 C24 126.1(5) . . ? C19 C20 Y 75.5(3) . . ? C21 C20 Y 73.1(3) . . ? C24 C20 Y 122.0(3) . . ? C20 C21 C22 108.4(5) . . ? C20 C21 C25 122.8(5) . . ? C22 C21 C25 128.5(5) . . ? C20 C21 Y 76.7(3) . . ? C22 C21 Y 72.8(3) . . ? C25 C21 Y 121.3(3) . . ? C21 C22 C18 106.6(4) . . ? C21 C22 Si2 128.4(4) . . ? C18 C22 Si2 123.4(4) . . ? C21 C22 Y 75.9(3) . . ? C18 C22 Y 75.5(3) . . ? Si2 C22 Y 125.4(2) . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C18 C26 H26A 109.5 . . ? C18 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C18 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 . . ? Si1 C30 Y 131.5(3) . . ? Si1 C30 H30A 104.4 . . ? Y C30 H30A 104.4 . . ? Si1 C30 H30B 104.4 . . ? Y C30 H30B 104.4 . . ? H30A C30 H30B 105.6 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O C34 C35 107.0(5) . . ? O C34 H34A 110.3 . . ? C35 C34 H34A 110.3 . . ? O C34 H34B 110.3 . . ? C35 C34 H34B 110.3 . . ? H34A C34 H34B 108.6 . . ? C34 C35 C36 104.8(6) . . ? C34 C35 H35A 110.8 . . ? C36 C35 H35A 110.8 . . ? C34 C35 H35B 110.8 . . ? C36 C35 H35B 110.8 . . ? H35A C35 H35B 108.9 . . ? C37 C36 C35 106.4(6) . . ? C37 C36 H36A 110.5 . . ? C35 C36 H36A 110.5 . . ? C37 C36 H36B 110.4 . . ? C35 C36 H36B 110.4 . . ? H36A C36 H36B 108.6 . . ? C36 C37 O 106.6(6) . . ? C36 C37 H37A 110.4 . . ? O C37 H37A 110.4 . . ? C36 C37 H37B 110.4 . . ? O C37 H37B 110.4 . . ? H37A C37 H37B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.525 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.067 #===========END============= data_2 _database_code_depnum_ccdc_archive 'CCDC 642643' #TrackingRef 'complexes_1-61.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H84 N4 O4 Si4 Y2' _chemical_formula_weight 1107.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7862(13) _cell_length_b 21.816(2) _cell_length_c 21.621(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.421(2) _cell_angle_gamma 90.00 _cell_volume 5911.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 2.076 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6937 _exptl_absorpt_correction_T_max 0.7598 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33031 _diffrn_reflns_av_R_equivalents 0.1518 _diffrn_reflns_av_sigmaI/netI 0.2996 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.02 _reflns_number_total 11617 _reflns_number_gt 3952 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal data is not good, which results in high Rint and poor GOF. ; _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^)+(0.0227P)^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 11617 _refine_ls_number_parameters 603 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1849 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 0.671 _refine_ls_restrained_S_all 0.678 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.22006(5) 0.75110(3) 0.00091(3) 0.03781(17) Uani 1 1 d . . . Y2 Y 0.15270(5) 0.82623(3) 0.15196(3) 0.03455(17) Uani 1 1 d . . . Si1 Si 0.60210(16) 0.88879(12) 0.15018(10) 0.0781(8) Uani 1 1 d . . . Si2 Si 0.31665(16) 0.85391(10) -0.12617(9) 0.0593(6) Uani 1 1 d . . . Si3 Si 0.17370(16) 0.60704(9) -0.09808(9) 0.0575(6) Uani 1 1 d . . . Si4 Si -0.22759(14) 0.68591(9) 0.01440(9) 0.0532(6) Uani 1 1 d . . . O1 O 0.2152(3) 0.88807(18) 0.25164(18) 0.0468(12) Uani 1 1 d . . . O2 O 0.0122(3) 0.8410(2) 0.21918(19) 0.0513(12) Uani 1 1 d . . . O3 O 0.2125(3) 0.75333(19) 0.23736(16) 0.0409(10) Uani 1 1 d . . . O4 O 0.0685(3) 0.92480(17) 0.12171(17) 0.0393(11) Uani 1 1 d . . . N1 N 0.2622(4) 0.8929(2) 0.1094(2) 0.0337(13) Uani 1 1 d . . . N2 N 0.0701(3) 0.7305(2) 0.1337(2) 0.0343(13) Uani 1 1 d . . . N3 N 0.2996(4) 0.7751(2) 0.1214(2) 0.0358(14) Uani 1 1 d . . . N4 N 0.0725(3) 0.8126(2) 0.0441(2) 0.0328(13) Uani 1 1 d . . . C1 C 0.0825(4) 0.8422(3) -0.0097(3) 0.0408(17) Uani 1 1 d . . . H1 H 0.1147 0.8803 -0.0107 0.049 Uiso 1 1 calc R . . C2 C 0.0391(4) 0.8087(3) -0.0626(3) 0.0395(17) Uani 1 1 d . . . H2 H 0.0361 0.8200 -0.1044 0.047 Uiso 1 1 calc R . . C3 C 0.0007(4) 0.7543(3) -0.0411(3) 0.0398(16) Uani 1 1 d . . . H3 H -0.0318 0.7220 -0.0657 0.048 Uiso 1 1 calc R . . C4 C 0.0206(4) 0.7585(3) 0.0238(3) 0.0349(16) Uani 1 1 d . . . C5 C -0.0040(5) 0.7156(3) 0.0736(3) 0.0361(16) Uani 1 1 d . . . H5 H 0.0111 0.6737 0.0616 0.043 Uiso 1 1 calc R . . C6 C 0.0879(5) 0.6849(3) 0.1770(3) 0.0329(16) Uani 1 1 d . . . C7 C 0.0404(5) 0.6263(3) 0.1731(3) 0.0463(18) Uani 1 1 d . . . H7 H -0.0080 0.6157 0.1367 0.056 Uiso 1 1 calc R . . C8 C 0.0635(5) 0.5844(3) 0.2215(3) 0.0508(19) Uani 1 1 d . . . H8 H 0.0290 0.5467 0.2170 0.061 Uiso 1 1 calc R . . C9 C 0.1350(5) 0.5962(3) 0.2759(3) 0.057(2) Uani 1 1 d . . . H9 H 0.1501 0.5673 0.3080 0.068 Uiso 1 1 calc R . . C10 C 0.1847(5) 0.6534(3) 0.2816(3) 0.0456(18) Uani 1 1 d . . . H10 H 0.2328 0.6632 0.3184 0.055 Uiso 1 1 calc R . . C11 C 0.1636(5) 0.6951(3) 0.2336(3) 0.0376(17) Uani 1 1 d . . . C12 C 0.3172(5) 0.7572(3) 0.2755(3) 0.062(2) Uani 1 1 d . . . H12A H 0.3125 0.7564 0.3193 0.093 Uiso 1 1 calc R . . H12B H 0.3503 0.7947 0.2664 0.093 Uiso 1 1 calc R . . H12C H 0.3590 0.7230 0.2664 0.093 Uiso 1 1 calc R . . C13 C -0.1231(4) 0.7188(3) 0.0791(2) 0.0413(17) Uani 1 1 d . . . H13A H -0.1406 0.7616 0.0837 0.050 Uiso 1 1 calc R . . H13B H -0.1297 0.6983 0.1180 0.050 Uiso 1 1 calc R . . C14 C -0.3339(5) 0.6539(3) 0.0521(3) 0.084(3) Uani 1 1 d . . . H14A H -0.3543 0.6839 0.0799 0.126 Uiso 1 1 calc R . . H14B H -0.3077 0.6179 0.0757 0.126 Uiso 1 1 calc R . . H14C H -0.3946 0.6434 0.0201 0.126 Uiso 1 1 calc R . . C15 C -0.1726(5) 0.6216(3) -0.0269(3) 0.063(2) Uani 1 1 d . . . H15A H -0.2298 0.6015 -0.0551 0.094 Uiso 1 1 calc R . . H15B H -0.1372 0.5927 0.0037 0.094 Uiso 1 1 calc R . . H15C H -0.1226 0.6376 -0.0506 0.094 Uiso 1 1 calc R . . C16 C -0.2870(5) 0.7457(3) -0.0430(3) 0.079(2) Uani 1 1 d . . . H16A H -0.3434 0.7280 -0.0738 0.119 Uiso 1 1 calc R . . H16B H -0.2331 0.7618 -0.0637 0.119 Uiso 1 1 calc R . . H16C H -0.3152 0.7781 -0.0212 0.119 Uiso 1 1 calc R . . C17 C 0.3218(5) 0.7146(3) 0.1145(3) 0.0384(17) Uani 1 1 d . . . H17 H 0.2891 0.6823 0.1313 0.046 Uiso 1 1 calc R . . C18 C 0.4003(5) 0.7082(3) 0.0786(3) 0.0458(18) Uani 1 1 d . . . H18 H 0.4286 0.6718 0.0668 0.055 Uiso 1 1 calc R . . C19 C 0.4280(5) 0.7676(3) 0.0637(3) 0.0431(18) Uani 1 1 d . . . H19 H 0.4779 0.7782 0.0397 0.052 Uiso 1 1 calc R . . C20 C 0.3672(5) 0.8074(3) 0.0915(3) 0.0342(16) Uani 1 1 d . . . C21 C 0.3677(4) 0.8761(3) 0.0974(3) 0.0345(16) Uani 1 1 d . . . H21 H 0.3781 0.8948 0.0578 0.041 Uiso 1 1 calc R . . C22 C 0.2322(5) 0.9526(3) 0.0951(3) 0.0339(16) Uani 1 1 d . . . C23 C 0.2932(5) 0.9996(3) 0.0740(3) 0.0401(17) Uani 1 1 d . . . H23 H 0.3614 0.9903 0.0680 0.048 Uiso 1 1 calc R . . C24 C 0.2554(5) 1.0589(3) 0.0621(3) 0.0458(18) Uani 1 1 d . . . H24 H 0.2982 1.0885 0.0484 0.055 Uiso 1 1 calc R . . C25 C 0.1550(5) 1.0738(3) 0.0703(3) 0.0480(19) Uani 1 1 d . . . H25 H 0.1300 1.1137 0.0627 0.058 Uiso 1 1 calc R . . C26 C 0.0905(5) 1.0300(3) 0.0900(3) 0.0414(17) Uani 1 1 d . . . H26 H 0.0221 1.0401 0.0952 0.050 Uiso 1 1 calc R . . C27 C 0.1288(5) 0.9713(3) 0.1016(3) 0.0335(16) Uani 1 1 d . . . C28 C -0.0458(4) 0.9303(3) 0.1036(3) 0.056(2) Uani 1 1 d . . . H28A H -0.0706 0.9608 0.1292 0.085 Uiso 1 1 calc R . . H28B H -0.0783 0.8916 0.1095 0.085 Uiso 1 1 calc R . . H28C H -0.0647 0.9421 0.0600 0.085 Uiso 1 1 calc R . . C29 C 0.4583(4) 0.8964(3) 0.1523(3) 0.0394(17) Uani 1 1 d . . . H29A H 0.4472 0.8745 0.1895 0.047 Uiso 1 1 calc R . . H29B H 0.4461 0.9395 0.1598 0.047 Uiso 1 1 calc R . . C30 C 0.6504(6) 0.8090(4) 0.1772(4) 0.135(4) Uani 1 1 d U . . H30A H 0.5945 0.7798 0.1631 0.202 Uiso 1 1 calc R . . H30B H 0.6695 0.8081 0.2224 0.202 Uiso 1 1 calc R . . H30C H 0.7116 0.7987 0.1597 0.202 Uiso 1 1 calc R . . C31 C 0.6271(6) 0.9034(4) 0.0734(3) 0.133(3) Uani 1 1 d U . . H31A H 0.5929 0.8725 0.0447 0.199 Uiso 1 1 calc R . . H31B H 0.7026 0.9026 0.0748 0.199 Uiso 1 1 calc R . . H31C H 0.5993 0.9430 0.0593 0.199 Uiso 1 1 calc R . . C32 C 0.6754(5) 0.9454(3) 0.2065(3) 0.080(3) Uani 1 1 d . . . H32A H 0.7495 0.9450 0.2039 0.120 Uiso 1 1 calc R . . H32B H 0.6682 0.9349 0.2486 0.120 Uiso 1 1 calc R . . H32C H 0.6465 0.9855 0.1961 0.120 Uiso 1 1 calc R . . C33 C 0.2862(5) 0.7811(3) -0.0891(3) 0.0549(19) Uani 1 1 d . . . H33A H 0.3529 0.7588 -0.0843 0.066 Uiso 1 1 calc R . . H33B H 0.2383 0.7606 -0.1232 0.066 Uiso 1 1 calc R . . C34 C 0.3002(5) 0.8507(3) -0.2141(3) 0.087(3) Uani 1 1 d . . . H34A H 0.3512 0.8226 -0.2253 0.131 Uiso 1 1 calc R . . H34B H 0.3115 0.8907 -0.2300 0.131 Uiso 1 1 calc R . . H34C H 0.2293 0.8371 -0.2322 0.131 Uiso 1 1 calc R . . C35 C 0.2288(5) 0.9175(3) -0.1101(3) 0.077(2) Uani 1 1 d . . . H35A H 0.1555 0.9063 -0.1249 0.115 Uiso 1 1 calc R . . H35B H 0.2446 0.9539 -0.1315 0.115 Uiso 1 1 calc R . . H35C H 0.2409 0.9252 -0.0655 0.115 Uiso 1 1 calc R . . C36 C 0.4560(5) 0.8777(4) -0.0941(3) 0.114(3) Uani 1 1 d . . . H36A H 0.4630 0.8887 -0.0505 0.171 Uiso 1 1 calc R . . H36B H 0.4737 0.9124 -0.1174 0.171 Uiso 1 1 calc R . . H36C H 0.5034 0.8444 -0.0979 0.171 Uiso 1 1 calc R . . C37 C 0.1870(4) 0.6434(2) -0.0216(2) 0.0448(18) Uani 1 1 d . . . H37A H 0.2439 0.6216 0.0061 0.054 Uiso 1 1 calc R . . H37B H 0.1219 0.6337 -0.0070 0.054 Uiso 1 1 calc R . . C38 C 0.0590(5) 0.6403(3) -0.1572(3) 0.081(3) Uani 1 1 d . . . H38A H -0.0061 0.6352 -0.1420 0.121 Uiso 1 1 calc R . . H38B H 0.0534 0.6195 -0.1969 0.121 Uiso 1 1 calc R . . H38C H 0.0715 0.6832 -0.1628 0.121 Uiso 1 1 calc R . . C39 C 0.1460(5) 0.5228(3) -0.0968(3) 0.090(3) Uani 1 1 d . . . H39A H 0.2067 0.5022 -0.0724 0.135 Uiso 1 1 calc R . . H39B H 0.1323 0.5072 -0.1392 0.135 Uiso 1 1 calc R . . H39C H 0.0848 0.5159 -0.0782 0.135 Uiso 1 1 calc R . . C40 C 0.3001(5) 0.6152(3) -0.1281(3) 0.077(2) Uani 1 1 d . . . H40A H 0.3013 0.6544 -0.1481 0.115 Uiso 1 1 calc R . . H40B H 0.3042 0.5833 -0.1582 0.115 Uiso 1 1 calc R . . H40C H 0.3599 0.6120 -0.0936 0.115 Uiso 1 1 calc R . . C41 C -0.0439(5) 0.7921(3) 0.2423(3) 0.063(2) Uani 1 1 d . . . H41A H -0.0003 0.7752 0.2797 0.094 Uiso 1 1 calc R . . H41B H -0.0599 0.7607 0.2107 0.094 Uiso 1 1 calc R . . H41C H -0.1091 0.8074 0.2521 0.094 Uiso 1 1 calc R . . C42 C 0.0362(7) 0.8896(4) 0.2639(4) 0.094(3) Uani 1 1 d . . . H42A H -0.0096 0.8866 0.2946 0.113 Uiso 1 1 calc R . . H42B H 0.0226 0.9287 0.2424 0.113 Uiso 1 1 calc R . . C43 C 0.1472(7) 0.8864(3) 0.2959(3) 0.075(3) Uani 1 1 d . . . H43A H 0.1634 0.9206 0.3249 0.090 Uiso 1 1 calc R . . H43B H 0.1593 0.8488 0.3202 0.090 Uiso 1 1 calc R . . C44 C 0.2757(5) 0.9436(3) 0.2548(3) 0.065(2) Uani 1 1 d . . . H44A H 0.2280 0.9780 0.2482 0.097 Uiso 1 1 calc R . . H44B H 0.3180 0.9431 0.2227 0.097 Uiso 1 1 calc R . . H44C H 0.3217 0.9468 0.2955 0.097 Uiso 1 1 calc R . . C45 C 0.0516(17) 0.0623(5) 0.3102(7) 0.153(8) Uani 1 1 d . . . C46 C 0.1568(10) 0.0602(4) 0.3355(8) 0.099(4) Uani 1 1 d . . . H46 H 0.2070 0.0748 0.3133 0.119 Uiso 1 1 calc R . . C47 C 0.1867(12) 0.0367(6) 0.3931(9) 0.135(5) Uani 1 1 d . . . H47 H 0.2589 0.0360 0.4115 0.162 Uiso 1 1 calc R . . C48 C 0.1068(18) 0.0109(5) 0.4299(7) 0.167(7) Uani 1 1 d . . . H48 H 0.1223 -0.0059 0.4702 0.201 Uiso 1 1 calc R . . C49 C 0.0176(13) 0.0164(6) 0.3961(9) 0.159(8) Uani 1 1 d . . . H49 H -0.0332 0.0008 0.4173 0.191 Uiso 1 1 calc R . . C50 C -0.0329(10) 0.0377(6) 0.3378(8) 0.134(7) Uani 1 1 d . . . H50 H -0.1054 0.0364 0.3203 0.161 Uiso 1 1 calc R . . C51 C 0.0236(10) 0.0855(5) 0.2525(5) 0.188(6) Uani 1 1 d . . . H51A H 0.0269 0.1294 0.2547 0.282 Uiso 1 1 calc R . . H51B H -0.0478 0.0729 0.2343 0.282 Uiso 1 1 calc R . . H51C H 0.0716 0.0709 0.2268 0.282 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 0.0390(4) 0.0330(4) 0.0418(4) 0.0005(4) 0.0090(3) 0.0026(3) Y2 0.0384(4) 0.0288(4) 0.0361(4) 0.0004(3) 0.0064(3) -0.0010(3) Si1 0.0430(15) 0.122(2) 0.0689(16) -0.0261(16) 0.0097(12) -0.0166(14) Si2 0.0583(16) 0.0609(16) 0.0605(15) 0.0094(12) 0.0161(12) 0.0012(12) Si3 0.0660(16) 0.0472(15) 0.0554(14) -0.0085(12) 0.0029(12) 0.0027(11) Si4 0.0423(13) 0.0530(15) 0.0611(14) -0.0052(12) 0.0028(11) -0.0078(11) O1 0.066(3) 0.038(3) 0.036(3) -0.006(2) 0.010(2) -0.007(2) O2 0.057(3) 0.046(3) 0.055(3) -0.016(3) 0.023(2) -0.010(2) O3 0.042(3) 0.040(3) 0.035(2) 0.001(2) -0.006(2) -0.005(2) O4 0.031(3) 0.034(3) 0.054(3) 0.002(2) 0.012(2) 0.006(2) N1 0.034(3) 0.026(3) 0.040(3) -0.003(3) 0.007(3) 0.003(3) N2 0.038(3) 0.036(4) 0.028(3) 0.007(3) 0.004(3) -0.006(2) N3 0.038(4) 0.028(3) 0.040(3) 0.003(3) 0.003(3) -0.001(3) N4 0.034(3) 0.029(4) 0.038(3) 0.006(3) 0.013(3) 0.004(3) C1 0.040(4) 0.036(5) 0.046(4) 0.005(4) 0.008(4) 0.006(3) C2 0.042(4) 0.048(5) 0.028(4) 0.009(4) 0.003(3) 0.013(3) C3 0.040(4) 0.036(4) 0.044(4) -0.005(4) 0.009(3) -0.005(4) C4 0.032(4) 0.041(5) 0.031(4) -0.006(4) 0.005(3) 0.002(3) C5 0.046(5) 0.021(4) 0.041(4) 0.004(3) 0.010(4) 0.005(3) C6 0.042(4) 0.034(5) 0.024(4) -0.004(3) 0.010(3) -0.001(3) C7 0.053(5) 0.039(5) 0.044(5) 0.006(4) 0.002(4) -0.004(4) C8 0.061(5) 0.034(5) 0.059(5) 0.009(4) 0.017(4) -0.011(4) C9 0.079(6) 0.036(5) 0.050(5) 0.014(4) -0.001(4) 0.001(4) C10 0.065(5) 0.047(5) 0.026(4) 0.002(4) 0.010(4) 0.000(4) C11 0.048(5) 0.034(5) 0.032(4) 0.000(4) 0.010(4) -0.005(3) C12 0.058(5) 0.055(5) 0.059(5) 0.009(4) -0.017(4) -0.020(4) C13 0.043(5) 0.037(4) 0.045(4) 0.003(3) 0.013(4) 0.006(3) C14 0.053(5) 0.086(7) 0.116(6) -0.031(5) 0.026(5) -0.020(4) C15 0.066(5) 0.058(5) 0.060(5) -0.012(4) 0.001(4) -0.015(4) C16 0.063(5) 0.087(6) 0.077(5) 0.009(5) -0.012(4) 0.016(5) C17 0.039(5) 0.028(4) 0.045(4) 0.004(4) 0.001(4) 0.002(3) C18 0.037(5) 0.035(5) 0.061(5) -0.006(4) 0.000(4) 0.010(3) C19 0.030(4) 0.047(5) 0.054(4) 0.002(4) 0.013(3) 0.000(3) C20 0.028(4) 0.031(4) 0.041(4) -0.002(3) 0.002(3) 0.003(3) C21 0.032(4) 0.024(4) 0.045(4) 0.001(3) 0.002(3) 0.003(3) C22 0.036(4) 0.032(4) 0.031(4) -0.010(3) 0.000(3) -0.010(3) C23 0.038(4) 0.034(4) 0.048(4) -0.003(4) 0.007(3) 0.006(4) C24 0.051(5) 0.031(5) 0.054(5) -0.002(4) 0.006(4) -0.006(4) C25 0.054(5) 0.033(5) 0.052(5) 0.002(4) -0.003(4) 0.007(4) C26 0.037(5) 0.037(5) 0.051(4) -0.006(4) 0.011(4) 0.003(4) C27 0.033(4) 0.032(4) 0.033(4) 0.001(3) 0.003(3) 0.000(4) C28 0.040(5) 0.052(5) 0.078(5) 0.011(4) 0.015(4) 0.004(4) C29 0.034(4) 0.033(4) 0.050(4) 0.000(3) 0.005(3) 0.002(3) C30 0.105(6) 0.125(6) 0.159(6) -0.038(5) -0.011(5) 0.053(5) C31 0.107(6) 0.190(7) 0.107(6) -0.034(5) 0.035(5) -0.057(5) C32 0.058(5) 0.109(7) 0.071(5) 0.004(5) 0.007(4) -0.034(5) C33 0.043(5) 0.048(5) 0.074(5) 0.001(4) 0.011(4) 0.008(3) C34 0.099(7) 0.083(7) 0.085(6) 0.006(5) 0.032(5) 0.012(5) C35 0.102(6) 0.047(5) 0.089(6) 0.015(5) 0.036(5) -0.001(4) C36 0.066(6) 0.160(9) 0.114(7) 0.051(6) 0.011(5) -0.034(6) C37 0.048(5) 0.039(4) 0.045(4) 0.007(3) 0.004(3) 0.007(3) C38 0.072(6) 0.102(7) 0.060(5) -0.037(5) -0.008(4) 0.019(5) C39 0.125(7) 0.057(6) 0.079(6) -0.020(5) -0.002(5) -0.023(5) C40 0.065(6) 0.080(6) 0.089(6) -0.026(5) 0.024(5) 0.012(4) C41 0.059(5) 0.068(6) 0.068(5) -0.007(4) 0.030(4) -0.009(4) C42 0.106(8) 0.088(7) 0.106(8) -0.052(6) 0.063(6) -0.029(6) C43 0.117(8) 0.066(6) 0.046(5) -0.023(4) 0.025(5) -0.033(5) C44 0.070(6) 0.057(6) 0.070(5) -0.023(4) 0.020(4) -0.026(4) C45 0.176(15) 0.075(9) 0.149(14) -0.062(9) -0.108(14) 0.058(10) C46 0.097(11) 0.039(7) 0.152(12) -0.026(7) 0.001(10) 0.006(6) C47 0.148(13) 0.057(10) 0.201(17) -0.075(10) 0.033(14) -0.004(9) C48 0.25(2) 0.066(9) 0.150(14) -0.031(9) -0.043(15) 0.002(12) C49 0.146(16) 0.122(13) 0.187(18) -0.097(14) -0.022(12) 0.031(10) C50 0.097(11) 0.085(9) 0.24(2) -0.063(11) 0.081(13) -0.031(8) C51 0.195(14) 0.172(14) 0.166(12) -0.085(11) -0.039(11) 0.043(10) _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 C33 2.363(6) . ? Y1 C37 2.420(5) . ? Y1 C1 2.633(5) . ? Y1 N4 2.632(4) . ? Y1 N3 2.654(5) . ? Y1 C17 2.662(5) . ? Y1 C4 2.696(5) . ? Y1 C20 2.725(6) . ? Y1 C18 2.734(6) . ? Y1 C2 2.749(5) . ? Y1 C19 2.759(6) . ? Y1 C3 2.773(5) . ? Y2 N1 2.332(5) . ? Y2 N2 2.339(4) . ? Y2 N4 2.373(5) . ? Y2 N3 2.388(5) . ? Y2 O4 2.436(4) . ? Y2 O3 2.442(4) . ? Y2 O1 2.534(4) . ? Y2 O2 2.545(4) . ? Si1 C31 1.780(7) . ? Si1 C32 1.852(6) . ? Si1 C29 1.856(5) . ? Si1 C30 1.900(8) . ? Si2 C36 1.853(6) . ? Si2 C33 1.854(6) . ? Si2 C35 1.861(6) . ? Si2 C34 1.873(6) . ? Si3 C37 1.811(5) . ? Si3 C40 1.866(6) . ? Si3 C39 1.872(6) . ? Si3 C38 1.890(6) . ? Si4 C16 1.856(6) . ? Si4 C14 1.854(6) . ? Si4 C15 1.874(6) . ? Si4 C13 1.875(5) . ? O1 C43 1.416(7) . ? O1 C44 1.431(6) . ? O2 C42 1.426(7) . ? O2 C41 1.431(6) . ? O3 C11 1.411(6) . ? O3 C12 1.429(5) . ? O4 C27 1.394(6) . ? O4 C28 1.441(5) . ? N1 C22 1.375(6) . ? N1 C21 1.469(6) . ? N2 C6 1.354(6) . ? N2 C5 1.484(6) . ? N3 C17 1.364(6) . ? N3 C20 1.371(6) . ? N4 C1 1.357(6) . ? N4 C4 1.384(6) . ? C1 C2 1.379(7) . ? C1 H1 0.9300 . ? C2 C3 1.397(7) . ? C2 H2 0.9300 . ? C3 C4 1.379(7) . ? C3 H3 0.9300 . ? C4 C5 1.506(7) . ? C5 C13 1.552(6) . ? C5 H5 0.9800 . ? C6 C7 1.410(7) . ? C6 C11 1.418(7) . ? C7 C8 1.378(7) . ? C7 H7 0.9300 . ? C8 C9 1.364(7) . ? C8 H8 0.9300 . ? C9 C10 1.394(7) . ? C9 H9 0.9300 . ? C10 C11 1.366(7) . ? C10 H10 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.392(7) . ? C17 H17 0.9300 . ? C18 C19 1.396(7) . ? C18 H18 0.9300 . ? C19 C20 1.380(7) . ? C19 H19 0.9300 . ? C20 C21 1.505(7) . ? C21 C29 1.551(7) . ? C21 H21 0.9800 . ? C22 C27 1.418(7) . ? C22 C23 1.417(7) . ? C23 C24 1.387(7) . ? C23 H23 0.9300 . ? C24 C25 1.371(7) . ? C24 H24 0.9300 . ? C25 C26 1.383(7) . ? C25 H25 0.9300 . ? C26 C27 1.376(7) . ? C26 H26 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? 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 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.453(8) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C51 1.329(14) . ? C45 C46 1.348(15) . ? C45 C50 1.44(2) . ? C46 C47 1.331(13) . ? C46 H46 0.9300 . ? C47 C48 1.522(16) . ? C47 H47 0.9300 . ? C48 C49 1.232(14) . ? C48 H48 0.9300 . ? C49 C50 1.379(18) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 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 C33 Y1 C37 100.38(19) . . ? C33 Y1 C1 93.51(19) . . ? C37 Y1 C1 128.92(19) . . ? C33 Y1 N4 123.32(17) . . ? C37 Y1 N4 117.23(17) . . ? C1 Y1 N4 29.87(13) . . ? C33 Y1 N3 128.56(18) . . ? C37 Y1 N3 114.01(16) . . ? C1 Y1 N3 93.20(17) . . ? N4 Y1 N3 73.35(14) . . ? C33 Y1 C17 130.8(2) . . ? C37 Y1 C17 85.94(18) . . ? C1 Y1 C17 120.10(19) . . ? N4 Y1 C17 94.53(17) . . ? N3 Y1 C17 29.74(14) . . ? C33 Y1 C4 129.82(19) . . ? C37 Y1 C4 87.75(19) . . ? C1 Y1 C4 48.05(18) . . ? N4 Y1 C4 30.07(14) . . ? N3 Y1 C4 90.04(16) . . ? C17 Y1 C4 98.95(19) . . ? C33 Y1 C20 99.1(2) . . ? C37 Y1 C20 130.59(18) . . ? C1 Y1 C20 94.38(18) . . ? N4 Y1 C20 87.50(16) . . ? N3 Y1 C20 29.51(13) . . ? C17 Y1 C20 47.95(18) . . ? C4 Y1 C20 112.62(18) . . ? C33 Y1 C18 101.8(2) . . ? C37 Y1 C18 83.33(18) . . ? C1 Y1 C18 141.15(19) . . ? N4 Y1 C18 122.20(17) . . ? N3 Y1 C18 49.62(16) . . ? C17 Y1 C18 29.87(15) . . ? C4 Y1 C18 128.36(19) . . ? C20 Y1 C18 48.29(18) . . ? C33 Y1 C2 82.25(18) . . ? C37 Y1 C2 104.29(19) . . ? C1 Y1 C2 29.59(14) . . ? N4 Y1 C2 49.68(15) . . ? N3 Y1 C2 121.41(16) . . ? C17 Y1 C2 143.74(18) . . ? C4 Y1 C2 48.06(17) . . ? C20 Y1 C2 123.10(18) . . ? C18 Y1 C2 170.71(18) . . ? C33 Y1 C19 84.38(19) . . ? C37 Y1 C19 109.78(19) . . ? C1 Y1 C19 120.42(19) . . ? N4 Y1 C19 116.58(16) . . ? N3 Y1 C19 49.20(16) . . ? C17 Y1 C19 48.53(18) . . ? C4 Y1 C19 139.11(18) . . ? C20 Y1 C19 29.15(15) . . ? C18 Y1 C19 29.43(15) . . ? C2 Y1 C19 145.10(19) . . ? C33 Y1 C3 103.11(19) . . ? C37 Y1 C3 80.42(19) . . ? C1 Y1 C3 48.51(18) . . ? N4 Y1 C3 49.75(15) . . ? N3 Y1 C3 118.88(16) . . ? C17 Y1 C3 125.99(19) . . ? C4 Y1 C3 29.17(14) . . ? C20 Y1 C3 137.20(18) . . ? C18 Y1 C3 152.27(19) . . ? C2 Y1 C3 29.30(15) . . ? C19 Y1 C3 166.33(18) . . ? N1 Y2 N2 141.02(15) . . ? N1 Y2 N4 82.33(16) . . ? N2 Y2 N4 68.26(16) . . ? N1 Y2 N3 67.38(17) . . ? N2 Y2 N3 83.68(16) . . ? N4 Y2 N3 83.08(15) . . ? N1 Y2 O4 67.10(15) . . ? N2 Y2 O4 125.61(15) . . ? N4 Y2 O4 76.39(14) . . ? N3 Y2 O4 131.92(15) . . ? N1 Y2 O3 125.62(15) . . ? N2 Y2 O3 67.01(15) . . ? N4 Y2 O3 132.16(15) . . ? N3 Y2 O3 76.10(14) . . ? O4 Y2 O3 146.46(12) . . ? N1 Y2 O1 83.71(15) . . ? N2 Y2 O1 132.45(15) . . ? N4 Y2 O1 154.76(15) . . ? N3 Y2 O1 110.58(15) . . ? O4 Y2 O1 78.84(13) . . ? O3 Y2 O1 72.84(13) . . ? N1 Y2 O2 133.89(15) . . ? N2 Y2 O2 82.14(14) . . ? N4 Y2 O2 111.15(14) . . ? N3 Y2 O2 154.20(15) . . ? O4 Y2 O2 73.56(13) . . ? O3 Y2 O2 78.54(13) . . ? O1 Y2 O2 65.55(14) . . ? C31 Si1 C32 109.4(3) . . ? C31 Si1 C29 111.6(3) . . ? C32 Si1 C29 107.4(3) . . ? C31 Si1 C30 110.1(4) . . ? C32 Si1 C30 108.5(3) . . ? C29 Si1 C30 109.8(3) . . ? C36 Si2 C33 110.3(3) . . ? C36 Si2 C35 107.0(3) . . ? C33 Si2 C35 111.8(3) . . ? C36 Si2 C34 107.3(3) . . ? C33 Si2 C34 114.6(3) . . ? C35 Si2 C34 105.5(3) . . ? C37 Si3 C40 110.2(3) . . ? C37 Si3 C39 113.6(3) . . ? C40 Si3 C39 106.1(3) . . ? C37 Si3 C38 111.7(3) . . ? C40 Si3 C38 109.7(3) . . ? C39 Si3 C38 105.3(3) . . ? C16 Si4 C14 108.7(3) . . ? C16 Si4 C15 110.5(3) . . ? C14 Si4 C15 107.7(3) . . ? C16 Si4 C13 111.5(3) . . ? C14 Si4 C13 107.0(3) . . ? C15 Si4 C13 111.3(3) . . ? C43 O1 C44 112.9(5) . . ? C43 O1 Y2 115.4(4) . . ? C44 O1 Y2 124.5(3) . . ? C42 O2 C41 111.9(5) . . ? C42 O2 Y2 113.6(4) . . ? C41 O2 Y2 124.4(4) . . ? C11 O3 C12 116.1(5) . . ? C11 O3 Y2 118.3(3) . . ? C12 O3 Y2 121.0(3) . . ? C27 O4 C28 116.6(4) . . ? C27 O4 Y2 118.9(4) . . ? C28 O4 Y2 121.1(3) . . ? C22 N1 C21 114.9(5) . . ? C22 N1 Y2 121.1(4) . . ? C21 N1 Y2 123.9(3) . . ? C6 N2 C5 115.9(5) . . ? C6 N2 Y2 122.0(4) . . ? C5 N2 Y2 122.1(3) . . ? C17 N3 C20 106.3(5) . . ? C17 N3 Y2 132.4(4) . . ? C20 N3 Y2 119.6(4) . . ? C17 N3 Y1 75.5(3) . . ? C20 N3 Y1 78.1(3) . . ? Y2 N3 Y1 101.22(16) . . ? C1 N4 C4 104.8(5) . . ? C1 N4 Y2 133.4(4) . . ? C4 N4 Y2 120.4(4) . . ? C1 N4 Y1 75.1(3) . . ? C4 N4 Y1 77.5(3) . . ? Y2 N4 Y1 102.24(15) . . ? N4 C1 C2 111.6(5) . . ? N4 C1 Y1 75.0(3) . . ? C2 C1 Y1 79.9(3) . . ? N4 C1 H1 124.2 . . ? C2 C1 H1 124.2 . . ? Y1 C1 H1 112.7 . . ? C1 C2 C3 106.5(5) . . ? C1 C2 Y1 70.6(3) . . ? C3 C2 Y1 76.3(3) . . ? C1 C2 H2 126.7 . . ? C3 C2 H2 126.7 . . ? Y1 C2 H2 118.4 . . ? C4 C3 C2 106.1(6) . . ? C4 C3 Y1 72.3(3) . . ? C2 C3 Y1 74.4(3) . . ? C4 C3 H3 127.0 . . ? C2 C3 H3 127.0 . . ? Y1 C3 H3 118.4 . . ? C3 C4 N4 111.0(6) . . ? C3 C4 C5 131.7(6) . . ? N4 C4 C5 117.3(5) . . ? C3 C4 Y1 78.5(3) . . ? N4 C4 Y1 72.4(3) . . ? C5 C4 Y1 115.7(4) . . ? N2 C5 C4 107.6(5) . . ? N2 C5 C13 112.9(4) . . ? C4 C5 C13 112.0(4) . . ? N2 C5 H5 108.0 . . ? C4 C5 H5 108.0 . . ? C13 C5 H5 108.0 . . ? N2 C6 C7 127.7(6) . . ? N2 C6 C11 118.3(6) . . ? C7 C6 C11 113.9(6) . . ? C8 C7 C6 122.1(6) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C9 C8 C7 122.4(6) . . ? C9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? C8 C9 C10 117.4(6) . . ? C8 C9 H9 121.3 . . ? C10 C9 H9 121.3 . . ? C11 C10 C9 120.8(6) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 O3 122.5(6) . . ? C10 C11 C6 123.3(6) . . ? O3 C11 C6 114.2(5) . . ? O3 C12 H12A 109.5 . . ? O3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 Si4 119.4(4) . . ? C5 C13 H13A 107.5 . . ? Si4 C13 H13A 107.5 . . ? C5 C13 H13B 107.5 . . ? Si4 C13 H13B 107.5 . . ? H13A C13 H13B 107.0 . . ? Si4 C14 H14A 109.5 . . ? Si4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si4 C15 H15A 109.5 . . ? Si4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si4 C16 H16A 109.5 . . ? Si4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C18 110.3(6) . . ? N3 C17 Y1 74.8(3) . . ? C18 C17 Y1 77.9(3) . . ? N3 C17 H17 124.9 . . ? C18 C17 H17 124.9 . . ? Y1 C17 H17 114.4 . . ? C19 C18 C17 106.2(6) . . ? C19 C18 Y1 76.3(3) . . ? C17 C18 Y1 72.2(3) . . ? C19 C18 H18 126.9 . . ? C17 C18 H18 126.9 . . ? Y1 C18 H18 116.8 . . ? C20 C19 C18 107.1(6) . . ? C20 C19 Y1 74.1(3) . . ? C18 C19 Y1 74.3(3) . . ? C20 C19 H19 126.5 . . ? C18 C19 H19 126.5 . . ? Y1 C19 H19 117.3 . . ? N3 C20 C19 110.1(6) . . ? N3 C20 C21 117.7(5) . . ? C19 C20 C21 132.1(6) . . ? N3 C20 Y1 72.4(3) . . ? C19 C20 Y1 76.8(4) . . ? C21 C20 Y1 120.0(4) . . ? N1 C21 C20 106.0(5) . . ? N1 C21 C29 111.5(5) . . ? C20 C21 C29 109.9(5) . . ? N1 C21 H21 109.8 . . ? C20 C21 H21 109.8 . . ? C29 C21 H21 109.8 . . ? N1 C22 C27 118.3(6) . . ? N1 C22 C23 127.7(6) . . ? C27 C22 C23 114.0(6) . . ? C24 C23 C22 122.9(6) . . ? C24 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? C25 C24 C23 119.8(6) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 120.5(6) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 119.1(6) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 O4 122.4(6) . . ? C26 C27 C22 123.7(6) . . ? O4 C27 C22 113.9(6) . . ? O4 C28 H28A 109.5 . . ? O4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C21 C29 Si1 123.3(4) . . ? C21 C29 H29A 106.5 . . ? Si1 C29 H29A 106.5 . . ? C21 C29 H29B 106.5 . . ? Si1 C29 H29B 106.5 . . ? H29A C29 H29B 106.5 . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 Y1 137.2(3) . . ? Si2 C33 H33A 102.8 . . ? Y1 C33 H33A 102.8 . . ? Si2 C33 H33B 102.8 . . ? Y1 C33 H33B 102.8 . . ? H33A C33 H33B 105.0 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si2 C36 H36A 109.5 . . ? Si2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si3 C37 Y1 126.2(3) . . ? Si3 C37 H37A 105.8 . . ? Y1 C37 H37A 105.8 . . ? Si3 C37 H37B 105.8 . . ? Y1 C37 H37B 105.8 . . ? H37A C37 H37B 106.2 . . ? Si3 C38 H38A 109.5 . . ? Si3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si3 C39 H39A 109.5 . . ? Si3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si3 C40 H40A 109.5 . . ? Si3 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si3 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O2 C41 H41A 109.5 . . ? O2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O2 C42 C43 110.3(6) . . ? O2 C42 H42A 109.6 . . ? C43 C42 H42A 109.6 . . ? O2 C42 H42B 109.6 . . ? C43 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? O1 C43 C42 110.4(6) . . ? O1 C43 H43A 109.6 . . ? C42 C43 H43A 109.6 . . ? O1 C43 H43B 109.6 . . ? C42 C43 H43B 109.6 . . ? H43A C43 H43B 108.1 . . ? O1 C44 H44A 109.5 . . ? O1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C51 C45 C46 117(2) . . ? C51 C45 C50 116.5(18) . . ? C46 C45 C50 126.2(15) . . ? C47 C46 C45 118.1(17) . . ? C47 C46 H46 120.9 . . ? C45 C46 H46 120.9 . . ? C46 C47 C48 122.2(17) . . ? C46 C47 H47 118.9 . . ? C48 C47 H47 118.9 . . ? C49 C48 C47 107.1(18) . . ? C49 C48 H48 126.5 . . ? C47 C48 H48 126.5 . . ? C48 C49 C50 142(2) . . ? C48 C49 H49 109.1 . . ? C50 C49 H49 109.1 . . ? C49 C50 C45 104.6(14) . . ? C49 C50 H50 127.7 . . ? C45 C50 H50 127.7 . . ? C45 C51 H51A 109.5 . . ? C45 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C45 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.485 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.069 # Attachment 'complexes_1-61.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 753704' #TrackingRef 'complexes_1-61.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H66 N4 O2 Si4 Y2' _chemical_formula_weight 925.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3031(9) _cell_length_b 37.091(3) _cell_length_c 12.1407(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.7270(10) _cell_angle_gamma 90.00 _cell_volume 5087.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 2.397 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5856 _exptl_absorpt_correction_T_max 0.6722 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28025 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.07 _reflns_number_total 9889 _reflns_number_gt 6778 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disordered solvents were possibly in the void and couldn't be defined correctly. ; _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^)+(0.0878P)^2^+0.1915P] 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 9889 _refine_ls_number_parameters 497 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.1296 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.33471(3) 0.185367(10) 0.53133(3) 0.02895(13) Uani 1 1 d . . . Y2 Y 0.28095(4) 0.083001(11) 0.47201(4) 0.03347(14) Uani 1 1 d . . . Si1 Si 0.64610(11) 0.22223(4) 0.50247(12) 0.0416(3) Uani 1 1 d . . . Si2 Si 0.43521(15) 0.04001(5) 0.22988(13) 0.0688(5) Uani 1 1 d D . . Si3 Si -0.03026(12) 0.11639(4) 0.21765(13) 0.0523(4) Uani 1 1 d . . . Si4 Si 0.46055(12) 0.15421(4) 0.88957(11) 0.0421(3) Uani 1 1 d . . . N1 N 0.2759(3) 0.13858(9) 0.3758(3) 0.0327(8) Uani 1 1 d . . . N2 N 0.0974(3) 0.10655(10) 0.4782(3) 0.0388(9) Uani 1 1 d . . . N3 N 0.4155(3) 0.12877(9) 0.5888(3) 0.0311(8) Uani 1 1 d . . . N4 N 0.2387(3) 0.16590(9) 0.6819(3) 0.0305(8) Uani 1 1 d . . . O1 O 0.1496(3) 0.04184(8) 0.5499(3) 0.0527(9) Uani 1 1 d . . . O2 O 0.1988(2) 0.22878(7) 0.5910(2) 0.0353(7) Uani 1 1 d . . . C1 C 0.3561(4) 0.16074(12) 0.3244(3) 0.0386(11) Uani 1 1 d . . . H1 H 0.4320 0.1539 0.3056 0.046 Uiso 1 1 calc R . . C2 C 0.3085(5) 0.19401(14) 0.3051(4) 0.0499(13) Uani 1 1 d . . . H2 H 0.3448 0.2135 0.2714 0.060 Uiso 1 1 calc R . . C3 C 0.1935(5) 0.19300(13) 0.3464(4) 0.0474(13) Uani 1 1 d . . . H3 H 0.1401 0.2121 0.3464 0.057 Uiso 1 1 calc R . . C4 C 0.1738(4) 0.15871(12) 0.3869(4) 0.0367(10) Uani 1 1 d . . . C5 C 0.0658(4) 0.14247(12) 0.4348(4) 0.0403(11) Uani 1 1 d . . . H5A H 0.0431 0.1575 0.4971 0.048 Uiso 1 1 calc R . . C6 C 0.0149(4) 0.09038(14) 0.5448(4) 0.0495(13) Uani 1 1 d . . . C7 C -0.0908(5) 0.10551(18) 0.5815(5) 0.0692(17) Uani 1 1 d . . . H7 H -0.1110 0.1290 0.5615 0.083 Uiso 1 1 calc R . . C8 C -0.1663(6) 0.0855(3) 0.6482(7) 0.098(3) Uani 1 1 d . . . H8 H -0.2346 0.0963 0.6733 0.117 Uiso 1 1 calc R . . C9 C -0.1427(7) 0.0516(3) 0.6763(7) 0.105(3) Uani 1 1 d . . . H9 H -0.1971 0.0385 0.7161 0.126 Uiso 1 1 calc R . . C10 C -0.0366(6) 0.03537(18) 0.6462(6) 0.083(2) Uani 1 1 d . . . H10 H -0.0176 0.0120 0.6683 0.100 Uiso 1 1 calc R . . C11 C 0.0392(5) 0.05532(14) 0.5823(5) 0.0547(14) Uani 1 1 d . . . C12 C 0.1830(6) 0.00604(14) 0.5860(6) 0.0764(19) Uani 1 1 d . . . H12A H 0.1788 0.0046 0.6647 0.115 Uiso 1 1 calc R . . H12B H 0.2624 0.0010 0.5646 0.115 Uiso 1 1 calc R . . H12C H 0.1299 -0.0113 0.5526 0.115 Uiso 1 1 calc R . . C13 C 0.3395(7) 0.03780(15) 0.3456(6) 0.078(2) Uani 1 1 d . A . H13A H 0.3729 0.0188 0.3917 0.094 Uiso 1 1 calc R . . H13B H 0.2656 0.0282 0.3152 0.094 Uiso 1 1 calc R . . C17 C -0.0369(4) 0.14336(16) 0.3479(5) 0.0588(15) Uani 1 1 d . . . H17A H -0.0483 0.1684 0.3266 0.071 Uiso 1 1 calc R . . H17B H -0.1078 0.1360 0.3848 0.071 Uiso 1 1 calc R . . C18 C -0.0213(8) 0.06824(19) 0.2455(7) 0.105(2) Uani 1 1 d U . . H18A H -0.0418 0.0551 0.1795 0.158 Uiso 1 1 calc R . . H18B H -0.0754 0.0621 0.3020 0.158 Uiso 1 1 calc R . . H18C H 0.0578 0.0621 0.2695 0.158 Uiso 1 1 calc R . . C19 C -0.1701(7) 0.1268(3) 0.1363(8) 0.124(3) Uani 1 1 d U . . H19A H -0.1772 0.1524 0.1265 0.186 Uiso 1 1 calc R . . H19B H -0.2369 0.1180 0.1752 0.186 Uiso 1 1 calc R . . H19C H -0.1677 0.1153 0.0655 0.186 Uiso 1 1 calc R . . C20 C 0.0923(7) 0.1305(2) 0.1291(6) 0.096(2) Uani 1 1 d U . . H20A H 0.0683 0.1512 0.0866 0.145 Uiso 1 1 calc R . . H20B H 0.1115 0.1111 0.0803 0.145 Uiso 1 1 calc R . . H20C H 0.1606 0.1364 0.1744 0.145 Uiso 1 1 calc R . . C21 C 0.4953(4) 0.10394(13) 0.5499(4) 0.0401(11) Uani 1 1 d . . . H21 H 0.5507 0.1087 0.4966 0.048 Uiso 1 1 calc R . . C22 C 0.4815(4) 0.07115(13) 0.6008(4) 0.0468(12) Uani 1 1 d . . . H22 H 0.5243 0.0502 0.5881 0.056 Uiso 1 1 calc R . . C23 C 0.3900(4) 0.07553(13) 0.6757(4) 0.0435(12) Uani 1 1 d . . . H23 H 0.3604 0.0579 0.7217 0.052 Uiso 1 1 calc R . . C24 C 0.3519(4) 0.11126(12) 0.6684(4) 0.0336(10) Uani 1 1 d . . . C25 C 0.2637(4) 0.13116(11) 0.7351(3) 0.0329(10) Uani 1 1 d . . . H25A H 0.1902 0.1171 0.7344 0.039 Uiso 1 1 calc R . . C26 C 0.1416(4) 0.18440(12) 0.7172(4) 0.0336(10) Uani 1 1 d . . . C27 C 0.0600(4) 0.17266(13) 0.7965(4) 0.0402(11) Uani 1 1 d . . . H27 H 0.0703 0.1502 0.8295 0.048 Uiso 1 1 calc R . . C28 C -0.0354(4) 0.19418(14) 0.8258(4) 0.0474(12) Uani 1 1 d . . . H28 H -0.0869 0.1858 0.8783 0.057 Uiso 1 1 calc R . . C29 C -0.0546(4) 0.22713(15) 0.7792(4) 0.0501(13) Uani 1 1 d . . . H29 H -0.1179 0.2413 0.8004 0.060 Uiso 1 1 calc R . . C30 C 0.0221(4) 0.23952(13) 0.6988(4) 0.0429(12) Uani 1 1 d . . . H30 H 0.0093 0.2618 0.6652 0.051 Uiso 1 1 calc R . . C31 C 0.1169(4) 0.21840(12) 0.6701(4) 0.0338(10) Uani 1 1 d . . . C32 C 0.1808(4) 0.26299(12) 0.5365(4) 0.0460(12) Uani 1 1 d . . . H32A H 0.1046 0.2632 0.4995 0.069 Uiso 1 1 calc R . . H32B H 0.2413 0.2665 0.4837 0.069 Uiso 1 1 calc R . . H32C H 0.1847 0.2820 0.5901 0.069 Uiso 1 1 calc R . . C33 C 0.4899(4) 0.22920(12) 0.5322(4) 0.0376(10) Uani 1 1 d . . . H33A H 0.4627 0.2479 0.4815 0.045 Uiso 1 1 calc R . . H33B H 0.4899 0.2400 0.6050 0.045 Uiso 1 1 calc R . . C34 C 0.7154(5) 0.18760(16) 0.5949(6) 0.076(2) Uani 1 1 d . . . H34A H 0.7090 0.1950 0.6702 0.114 Uiso 1 1 calc R . . H34B H 0.7974 0.1850 0.5781 0.114 Uiso 1 1 calc R . . H34C H 0.6756 0.1650 0.5840 0.114 Uiso 1 1 calc R . . C35 C 0.6611(5) 0.20649(17) 0.3555(5) 0.0645(16) Uani 1 1 d . . . H35A H 0.6192 0.1842 0.3450 0.097 Uiso 1 1 calc R . . H35B H 0.7432 0.2030 0.3407 0.097 Uiso 1 1 calc R . . H35C H 0.6284 0.2243 0.3061 0.097 Uiso 1 1 calc R . . C36 C 0.7411(4) 0.26355(14) 0.5223(4) 0.0512(13) Uani 1 1 d . . . H36A H 0.7169 0.2816 0.4697 0.077 Uiso 1 1 calc R . . H36B H 0.8224 0.2574 0.5119 0.077 Uiso 1 1 calc R . . H36C H 0.7323 0.2727 0.5956 0.077 Uiso 1 1 calc R . . C37 C 0.3107(4) 0.13402(12) 0.8563(4) 0.0383(10) Uani 1 1 d . . . H37A H 0.3108 0.1098 0.8868 0.046 Uiso 1 1 calc R . . H37B H 0.2532 0.1478 0.8964 0.046 Uiso 1 1 calc R . . C38 C 0.4805(5) 0.19642(15) 0.8103(4) 0.0612(15) Uani 1 1 d . . . H38A H 0.4110 0.2111 0.8154 0.092 Uiso 1 1 calc R . . H38B H 0.4930 0.1907 0.7344 0.092 Uiso 1 1 calc R . . H38C H 0.5478 0.2093 0.8400 0.092 Uiso 1 1 calc R . . C39 C 0.4649(5) 0.16467(14) 1.0399(4) 0.0543(13) Uani 1 1 d . . . H39A H 0.4568 0.1428 1.0810 0.081 Uiso 1 1 calc R . . H39B H 0.4011 0.1807 1.0562 0.081 Uiso 1 1 calc R . . H39C H 0.5389 0.1759 1.0597 0.081 Uiso 1 1 calc R . . C40 C 0.5836(5) 0.12254(17) 0.8595(5) 0.0664(16) Uani 1 1 d . . . H40A H 0.6574 0.1328 0.8850 0.100 Uiso 1 1 calc R . . H40B H 0.5858 0.1185 0.7815 0.100 Uiso 1 1 calc R . . H40C H 0.5710 0.1001 0.8965 0.100 Uiso 1 1 calc R . . C14 C 0.3509(11) 0.0687(3) 0.1230(8) 0.071(3) Uani 0.636(12) 1 d PDU A 1 H14A H 0.2804 0.0563 0.0987 0.106 Uiso 0.636(12) 1 calc PR A 1 H14B H 0.4000 0.0730 0.0612 0.106 Uiso 0.636(12) 1 calc PR A 1 H14C H 0.3299 0.0913 0.1554 0.106 Uiso 0.636(12) 1 calc PR A 1 C15 C 0.4353(12) -0.0077(3) 0.1558(9) 0.076(3) Uani 0.636(12) 1 d PDU A 1 H15A H 0.3555 -0.0165 0.1480 0.114 Uiso 0.636(12) 1 calc PR A 1 H15B H 0.4818 -0.0244 0.1994 0.114 Uiso 0.636(12) 1 calc PR A 1 H15C H 0.4686 -0.0054 0.0844 0.114 Uiso 0.636(12) 1 calc PR A 1 C16 C 0.5737(9) 0.0711(4) 0.2658(12) 0.107(5) Uani 0.636(12) 1 d PDU A 1 H16A H 0.5478 0.0926 0.3015 0.161 Uiso 0.636(12) 1 calc PR A 1 H16B H 0.6125 0.0773 0.1991 0.161 Uiso 0.636(12) 1 calc PR A 1 H16C H 0.6280 0.0583 0.3140 0.161 Uiso 0.636(12) 1 calc PR A 1 C16B C 0.5810(11) 0.0359(5) 0.3081(14) 0.071(6) Uani 0.364(12) 1 d PDU A 2 H16D H 0.5882 0.0122 0.3390 0.106 Uiso 0.364(12) 1 calc PR A 2 H16E H 0.5846 0.0535 0.3663 0.106 Uiso 0.364(12) 1 calc PR A 2 H16F H 0.6446 0.0401 0.2590 0.106 Uiso 0.364(12) 1 calc PR A 2 C15B C 0.5126(17) 0.0020(4) 0.1643(14) 0.059(5) Uani 0.364(12) 1 d PDU A 2 H15D H 0.4558 -0.0158 0.1405 0.088 Uiso 0.364(12) 1 calc PR A 2 H15E H 0.5679 -0.0085 0.2165 0.088 Uiso 0.364(12) 1 calc PR A 2 H15F H 0.5543 0.0107 0.1019 0.088 Uiso 0.364(12) 1 calc PR A 2 C14B C 0.429(2) 0.0735(5) 0.1168(16) 0.090(7) Uani 0.364(12) 1 d PDU A 2 H14D H 0.3624 0.0683 0.0683 0.134 Uiso 0.364(12) 1 calc PR A 2 H14E H 0.5005 0.0722 0.0764 0.134 Uiso 0.364(12) 1 calc PR A 2 H14F H 0.4205 0.0972 0.1471 0.134 Uiso 0.364(12) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0319(2) 0.0277(2) 0.0272(2) 0.00171(17) 0.00089(16) -0.00188(17) Y2 0.0345(2) 0.0273(2) 0.0390(3) -0.00167(18) 0.00797(18) 0.00113(17) Si1 0.0348(7) 0.0435(8) 0.0464(8) 0.0008(6) 0.0011(6) -0.0058(6) Si2 0.0650(10) 0.0996(14) 0.0425(9) 0.0068(9) 0.0139(8) 0.0314(10) Si3 0.0487(8) 0.0545(9) 0.0528(9) -0.0018(7) -0.0158(7) -0.0055(7) Si4 0.0491(8) 0.0466(8) 0.0306(7) -0.0008(6) 0.0010(6) -0.0024(6) N1 0.0361(19) 0.033(2) 0.0288(19) -0.0022(15) 0.0016(15) -0.0033(16) N2 0.0299(19) 0.041(2) 0.045(2) -0.0077(18) 0.0059(16) -0.0041(17) N3 0.0275(18) 0.034(2) 0.031(2) 0.0007(15) 0.0017(14) 0.0014(15) N4 0.0314(18) 0.034(2) 0.0261(19) -0.0008(15) 0.0013(14) 0.0035(15) O1 0.065(2) 0.0366(19) 0.058(2) 0.0001(16) 0.0218(18) -0.0114(16) O2 0.0411(17) 0.0284(16) 0.0362(18) 0.0019(13) -0.0009(14) 0.0019(13) C1 0.049(3) 0.041(3) 0.025(2) -0.0016(19) 0.002(2) -0.008(2) C2 0.073(4) 0.045(3) 0.031(3) 0.005(2) -0.007(2) -0.017(3) C3 0.065(3) 0.033(3) 0.043(3) -0.005(2) -0.019(2) 0.009(2) C4 0.041(3) 0.034(2) 0.034(3) -0.0059(19) -0.011(2) 0.007(2) C5 0.032(2) 0.043(3) 0.045(3) -0.015(2) -0.005(2) 0.007(2) C6 0.038(3) 0.056(3) 0.055(3) -0.021(3) 0.014(2) -0.016(2) C7 0.041(3) 0.082(4) 0.086(5) -0.021(4) 0.022(3) -0.011(3) C8 0.046(4) 0.144(8) 0.105(6) -0.046(6) 0.038(4) -0.029(4) C9 0.091(6) 0.119(7) 0.107(6) -0.026(6) 0.060(5) -0.049(5) C10 0.098(5) 0.070(4) 0.083(5) -0.014(3) 0.042(4) -0.039(4) C11 0.060(3) 0.047(3) 0.059(3) -0.015(3) 0.025(3) -0.026(3) C12 0.121(6) 0.037(3) 0.074(4) 0.008(3) 0.034(4) -0.005(3) C13 0.120(5) 0.045(3) 0.072(4) -0.007(3) 0.043(4) 0.004(3) C17 0.037(3) 0.068(4) 0.071(4) -0.014(3) -0.014(3) 0.009(3) C18 0.145(5) 0.080(4) 0.090(4) -0.001(3) -0.008(4) -0.021(4) C19 0.105(4) 0.143(5) 0.121(5) -0.027(4) -0.037(4) 0.005(4) C20 0.102(4) 0.111(4) 0.076(4) 0.001(3) 0.001(3) -0.025(3) C21 0.031(2) 0.049(3) 0.040(3) 0.001(2) 0.004(2) 0.007(2) C22 0.041(3) 0.041(3) 0.059(3) 0.005(2) 0.006(2) 0.017(2) C23 0.045(3) 0.039(3) 0.046(3) 0.014(2) 0.003(2) 0.008(2) C24 0.032(2) 0.035(2) 0.034(2) 0.0081(19) -0.0020(18) 0.0024(19) C25 0.031(2) 0.035(2) 0.033(2) 0.0033(19) 0.0036(18) 0.0007(18) C26 0.030(2) 0.039(3) 0.031(2) -0.0070(19) -0.0016(18) 0.0001(19) C27 0.036(2) 0.044(3) 0.041(3) -0.001(2) 0.008(2) 0.001(2) C28 0.032(2) 0.063(3) 0.048(3) -0.009(3) 0.007(2) 0.002(2) C29 0.035(3) 0.060(3) 0.055(3) -0.018(3) 0.001(2) 0.013(2) C30 0.040(3) 0.039(3) 0.049(3) -0.011(2) -0.011(2) 0.007(2) C31 0.033(2) 0.037(3) 0.031(2) -0.0077(19) -0.0045(18) 0.0003(19) C32 0.058(3) 0.031(3) 0.048(3) 0.006(2) -0.005(2) 0.007(2) C33 0.040(2) 0.035(3) 0.038(3) 0.004(2) 0.006(2) -0.004(2) C34 0.051(3) 0.060(4) 0.115(6) 0.021(4) -0.021(3) -0.004(3) C35 0.049(3) 0.087(4) 0.058(4) -0.016(3) 0.010(3) -0.007(3) C36 0.040(3) 0.057(3) 0.056(3) 0.008(3) 0.004(2) -0.010(2) C37 0.046(3) 0.039(3) 0.029(2) 0.009(2) 0.0038(19) 0.003(2) C38 0.084(4) 0.065(4) 0.035(3) 0.002(3) -0.002(3) -0.031(3) C39 0.070(4) 0.057(3) 0.035(3) 0.000(2) -0.002(2) -0.004(3) C40 0.049(3) 0.080(4) 0.070(4) -0.019(3) -0.006(3) 0.004(3) C14 0.090(7) 0.061(6) 0.061(6) 0.007(4) -0.004(5) 0.001(5) C15 0.083(7) 0.083(6) 0.062(6) 0.002(5) 0.023(5) 0.038(5) C16 0.080(7) 0.142(9) 0.102(8) -0.004(7) 0.025(6) 0.002(6) C16B 0.057(8) 0.075(9) 0.081(9) -0.016(7) 0.009(7) 0.006(7) C15B 0.062(8) 0.062(8) 0.052(8) 0.003(6) 0.010(7) 0.015(7) C14B 0.097(10) 0.078(10) 0.094(10) 0.006(8) 0.020(8) -0.008(8) _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 2.272(3) . ? Y1 O2 2.355(3) . ? Y1 N3 2.385(3) . ? Y1 C33 2.391(4) . ? Y1 N1 2.635(3) . ? Y1 C4 2.677(4) . ? Y1 C1 2.691(4) . ? Y1 C3 2.730(5) . ? Y1 C2 2.772(5) . ? Y1 Y2 3.9087(6) . ? Y2 N2 2.255(3) . ? Y2 O1 2.348(3) . ? Y2 N1 2.369(3) . ? Y2 C13 2.380(5) . ? Y2 N3 2.660(3) . ? Y2 C21 2.689(4) . ? Y2 C24 2.704(4) . ? Y2 C23 2.744(5) . ? Y2 C22 2.750(5) . ? Si1 C33 1.831(4) . ? Si1 C34 1.863(6) . ? Si1 C36 1.883(5) . ? Si1 C35 1.890(6) . ? Si2 C13 1.801(6) . ? Si2 C14B 1.850(13) . ? Si2 C15B 1.851(11) . ? Si2 C16B 1.883(12) . ? Si2 C14 1.911(9) . ? Si2 C16 1.982(10) . ? Si2 C15 1.986(9) . ? Si3 C18 1.820(7) . ? Si3 C20 1.855(7) . ? Si3 C17 1.875(6) . ? Si3 C19 1.879(8) . ? Si4 C38 1.855(5) . ? Si4 C39 1.865(5) . ? Si4 C40 1.865(6) . ? Si4 C37 1.884(5) . ? N1 C4 1.385(5) . ? N1 C1 1.386(5) . ? N2 C6 1.388(6) . ? N2 C5 1.473(6) . ? N3 C24 1.383(5) . ? N3 C21 1.383(5) . ? N4 C26 1.374(5) . ? N4 C25 1.465(5) . ? O1 C11 1.411(6) . ? O1 C12 1.445(6) . ? O2 C31 1.407(5) . ? O2 C32 1.442(5) . ? C1 C2 1.363(7) . ? C1 H1 0.9300 . ? C2 C3 1.408(7) . ? C2 H2 0.9300 . ? C3 C4 1.385(6) . ? C3 H3 0.9300 . ? C4 C5 1.494(6) . ? C5 C17 1.545(6) . ? C5 H5A 0.9800 . ? C6 C11 1.402(7) . ? C6 C7 1.405(7) . ? C7 C8 1.405(10) . ? C7 H7 0.9300 . ? C8 C9 1.330(11) . ? C8 H8 0.9300 . ? C9 C10 1.400(10) . ? C9 H9 0.9300 . ? C10 C11 1.387(7) . ? C10 H10 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.375(7) . ? C21 H21 0.9300 . ? C22 C23 1.407(7) . ? C22 H22 0.9300 . ? C23 C24 1.396(6) . ? C23 H23 0.9300 . ? C24 C25 1.498(6) . ? C25 C37 1.553(6) . ? C25 H25A 0.9800 . ? C26 C31 1.409(6) . ? C26 C27 1.422(6) . ? C27 C28 1.395(6) . ? C27 H27 0.9300 . ? C28 C29 1.362(7) . ? C28 H28 0.9300 . ? C29 C30 1.402(7) . ? C29 H29 0.9300 . ? C30 C31 1.381(6) . ? C30 H30 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 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 N4 Y1 O2 68.77(11) . . ? N4 Y1 N3 70.89(12) . . ? O2 Y1 N3 139.40(11) . . ? N4 Y1 C33 125.49(14) . . ? O2 Y1 C33 91.08(13) . . ? N3 Y1 C33 108.84(13) . . ? N4 Y1 N1 104.55(11) . . ? O2 Y1 N1 121.19(10) . . ? N3 Y1 N1 73.52(11) . . ? C33 Y1 N1 128.33(13) . . ? N4 Y1 C4 94.47(13) . . ? O2 Y1 C4 90.99(12) . . ? N3 Y1 C4 96.49(12) . . ? C33 Y1 C4 137.54(15) . . ? N1 Y1 C4 30.20(11) . . ? N4 Y1 C1 134.59(13) . . ? O2 Y1 C1 126.66(13) . . ? N3 Y1 C1 86.00(13) . . ? C33 Y1 C1 98.54(15) . . ? N1 Y1 C1 30.14(11) . . ? C4 Y1 C1 48.82(14) . . ? N4 Y1 C3 114.42(15) . . ? O2 Y1 C3 79.13(13) . . ? N3 Y1 C3 122.76(13) . . ? C33 Y1 C3 110.10(16) . . ? N1 Y1 C3 49.48(12) . . ? C4 Y1 C3 29.65(14) . . ? C1 Y1 C3 48.24(15) . . ? N4 Y1 C2 142.64(14) . . ? O2 Y1 C2 100.05(13) . . ? N3 Y1 C2 114.85(14) . . ? C33 Y1 C2 88.98(15) . . ? N1 Y1 C2 49.39(13) . . ? C4 Y1 C2 48.99(14) . . ? C1 Y1 C2 28.85(14) . . ? C3 Y1 C2 29.63(15) . . ? N4 Y1 Y2 76.36(9) . . ? O2 Y1 Y2 128.44(7) . . ? N3 Y1 Y2 41.84(8) . . ? C33 Y1 Y2 140.46(11) . . ? N1 Y1 Y2 36.27(7) . . ? C4 Y1 Y2 54.67(9) . . ? C1 Y1 Y2 61.06(9) . . ? C3 Y1 Y2 82.27(10) . . ? C2 Y1 Y2 85.32(10) . . ? N2 Y2 O1 69.21(13) . . ? N2 Y2 N1 70.77(13) . . ? O1 Y2 N1 139.30(12) . . ? N2 Y2 C13 124.6(2) . . ? O1 Y2 C13 89.61(17) . . ? N1 Y2 C13 107.33(17) . . ? N2 Y2 N3 104.30(12) . . ? O1 Y2 N3 123.93(11) . . ? N1 Y2 N3 73.30(11) . . ? C13 Y2 N3 128.9(2) . . ? N2 Y2 C21 134.19(13) . . ? O1 Y2 C21 128.31(14) . . ? N1 Y2 C21 86.00(13) . . ? C13 Y2 C21 99.5(2) . . ? N3 Y2 C21 29.96(11) . . ? N2 Y2 C24 93.98(13) . . ? O1 Y2 C24 94.08(13) . . ? N1 Y2 C24 95.72(12) . . ? C13 Y2 C24 139.5(2) . . ? N3 Y2 C24 29.87(11) . . ? C21 Y2 C24 48.53(13) . . ? N2 Y2 C23 113.47(14) . . ? O1 Y2 C23 81.00(14) . . ? N1 Y2 C23 122.40(13) . . ? C13 Y2 C23 112.6(2) . . ? N3 Y2 C23 49.44(12) . . ? C21 Y2 C23 48.44(14) . . ? C24 Y2 C23 29.67(13) . . ? N2 Y2 C22 141.89(14) . . ? O1 Y2 C22 100.80(14) . . ? N1 Y2 C22 115.26(13) . . ? C13 Y2 C22 90.8(2) . . ? N3 Y2 C22 49.52(13) . . ? C21 Y2 C22 29.26(14) . . ? C24 Y2 C22 48.95(13) . . ? C23 Y2 C22 29.68(14) . . ? N2 Y2 Y1 75.86(9) . . ? O1 Y2 Y1 130.84(8) . . ? N1 Y2 Y1 41.15(8) . . ? C13 Y2 Y1 139.32(15) . . ? N3 Y2 Y1 36.73(7) . . ? C21 Y2 Y1 61.40(10) . . ? C24 Y2 Y1 54.59(9) . . ? C23 Y2 Y1 82.46(10) . . ? C22 Y2 Y1 85.96(10) . . ? C33 Si1 C34 111.7(3) . . ? C33 Si1 C36 114.2(2) . . ? C34 Si1 C36 104.9(2) . . ? C33 Si1 C35 110.1(2) . . ? C34 Si1 C35 107.9(3) . . ? C36 Si1 C35 107.8(3) . . ? C13 Si2 C14B 126.8(8) . . ? C13 Si2 C15B 127.1(6) . . ? C14B Si2 C15B 101.5(9) . . ? C13 Si2 C16B 98.1(6) . . ? C14B Si2 C16B 116.2(10) . . ? C15B Si2 C16B 74.8(9) . . ? C13 Si2 C14 104.8(5) . . ? C14B Si2 C14 27.8(7) . . ? C15B Si2 C14 111.4(7) . . ? C16B Si2 C14 143.0(7) . . ? C13 Si2 C16 110.2(5) . . ? C14B Si2 C16 77.6(9) . . ? C15B Si2 C16 99.0(8) . . ? C16B Si2 C16 42.5(6) . . ? C14 Si2 C16 101.5(6) . . ? C13 Si2 C15 108.7(4) . . ? C14B Si2 C15 105.2(8) . . ? C15B Si2 C15 28.4(6) . . ? C16B Si2 C15 98.3(7) . . ? C14 Si2 C15 101.3(5) . . ? C16 Si2 C15 127.4(6) . . ? C18 Si3 C20 110.3(4) . . ? C18 Si3 C17 111.7(3) . . ? C20 Si3 C17 112.8(3) . . ? C18 Si3 C19 109.9(4) . . ? C20 Si3 C19 105.6(4) . . ? C17 Si3 C19 106.3(3) . . ? C38 Si4 C39 109.4(2) . . ? C38 Si4 C40 109.1(3) . . ? C39 Si4 C40 108.9(3) . . ? C38 Si4 C37 110.3(2) . . ? C39 Si4 C37 106.8(2) . . ? C40 Si4 C37 112.2(2) . . ? C4 N1 C1 106.4(4) . . ? C4 N1 Y2 115.4(3) . . ? C1 N1 Y2 137.0(3) . . ? C4 N1 Y1 76.6(2) . . ? C1 N1 Y1 77.2(2) . . ? Y2 N1 Y1 102.57(12) . . ? C6 N2 C5 116.1(4) . . ? C6 N2 Y2 119.1(3) . . ? C5 N2 Y2 123.5(3) . . ? C24 N3 C21 106.5(4) . . ? C24 N3 Y1 114.5(3) . . ? C21 N3 Y1 137.2(3) . . ? C24 N3 Y2 76.8(2) . . ? C21 N3 Y2 76.2(2) . . ? Y1 N3 Y2 101.43(11) . . ? C26 N4 C25 116.5(3) . . ? C26 N4 Y1 119.9(3) . . ? C25 N4 Y1 123.0(2) . . ? C11 O1 C12 117.8(4) . . ? C11 O1 Y2 117.2(3) . . ? C12 O1 Y2 123.9(3) . . ? C31 O2 C32 117.9(3) . . ? C31 O2 Y1 118.1(2) . . ? C32 O2 Y1 123.0(3) . . ? C2 C1 N1 110.8(4) . . ? C2 C1 Y1 78.9(3) . . ? N1 C1 Y1 72.7(2) . . ? C2 C1 H1 124.6 . . ? N1 C1 H1 124.6 . . ? Y1 C1 H1 115.5 . . ? C1 C2 C3 106.2(4) . . ? C1 C2 Y1 72.3(3) . . ? C3 C2 Y1 73.5(3) . . ? C1 C2 H2 126.9 . . ? C3 C2 H2 126.9 . . ? Y1 C2 H2 119.3 . . ? C4 C3 C2 108.1(4) . . ? C4 C3 Y1 73.1(2) . . ? C2 C3 Y1 76.9(3) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Y1 C3 H3 116.2 . . ? N1 C4 C3 108.5(4) . . ? N1 C4 C5 120.9(4) . . ? C3 C4 C5 130.6(4) . . ? N1 C4 Y1 73.2(2) . . ? C3 C4 Y1 77.3(3) . . ? C5 C4 Y1 116.2(3) . . ? N2 C5 C4 108.2(3) . . ? N2 C5 C17 115.6(4) . . ? C4 C5 C17 109.4(4) . . ? N2 C5 H5A 107.8 . . ? C4 C5 H5A 107.8 . . ? C17 C5 H5A 107.8 . . ? N2 C6 C11 117.5(4) . . ? N2 C6 C7 127.2(5) . . ? C11 C6 C7 115.3(5) . . ? C6 C7 C8 120.6(7) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C9 C8 C7 121.8(7) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C10 120.4(7) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 117.7(7) . . ? C11 C10 H10 121.1 . . ? C9 C10 H10 121.1 . . ? C10 C11 C6 123.9(6) . . ? C10 C11 O1 122.2(6) . . ? C6 C11 O1 113.8(4) . . ? O1 C12 H12A 109.5 . . ? O1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 Y2 131.0(3) . . ? Si2 C13 H13A 104.5 . . ? Y2 C13 H13A 104.5 . . ? Si2 C13 H13B 104.5 . . ? Y2 C13 H13B 104.5 . . ? H13A C13 H13B 105.7 . . ? C5 C17 Si3 121.1(3) . . ? C5 C17 H17A 107.1 . . ? Si3 C17 H17A 107.1 . . ? C5 C17 H17B 107.1 . . ? Si3 C17 H17B 107.1 . . ? H17A C17 H17B 106.8 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si3 C19 H19A 109.5 . . ? Si3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N3 110.6(4) . . ? C22 C21 Y2 77.8(3) . . ? N3 C21 Y2 73.9(2) . . ? C22 C21 H21 124.7 . . ? N3 C21 H21 124.7 . . ? Y2 C21 H21 115.4 . . ? C21 C22 C23 106.5(4) . . ? C21 C22 Y2 72.9(3) . . ? C23 C22 Y2 74.9(3) . . ? C21 C22 H22 126.8 . . ? C23 C22 H22 126.8 . . ? Y2 C22 H22 117.6 . . ? C24 C23 C22 107.4(4) . . ? C24 C23 Y2 73.6(3) . . ? C22 C23 Y2 75.4(3) . . ? C24 C23 H23 126.3 . . ? C22 C23 H23 126.3 . . ? Y2 C23 H23 116.9 . . ? N3 C24 C23 109.0(4) . . ? N3 C24 C25 121.0(4) . . ? C23 C24 C25 130.0(4) . . ? N3 C24 Y2 73.3(2) . . ? C23 C24 Y2 76.8(3) . . ? C25 C24 Y2 118.9(3) . . ? N4 C25 C24 108.5(3) . . ? N4 C25 C37 114.4(3) . . ? C24 C25 C37 109.4(3) . . ? N4 C25 H25A 108.1 . . ? C24 C25 H25A 108.1 . . ? C37 C25 H25A 108.1 . . ? N4 C26 C31 118.0(4) . . ? N4 C26 C27 126.8(4) . . ? C31 C26 C27 115.2(4) . . ? C28 C27 C26 121.3(5) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C29 C28 C27 121.5(5) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C30 119.3(4) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 119.4(5) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 O2 123.3(4) . . ? C30 C31 C26 123.4(4) . . ? O2 C31 C26 113.3(4) . . ? O2 C32 H32A 109.5 . . ? O2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si1 C33 Y1 127.9(2) . . ? Si1 C33 H33A 105.3 . . ? Y1 C33 H33A 105.3 . . ? Si1 C33 H33B 105.3 . . ? Y1 C33 H33B 105.3 . . ? H33A C33 H33B 106.0 . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C25 C37 Si4 120.7(3) . . ? C25 C37 H37A 107.2 . . ? Si4 C37 H37A 107.2 . . ? C25 C37 H37B 107.2 . . ? Si4 C37 H37B 107.2 . . ? H37A C37 H37B 106.8 . . ? Si4 C38 H38A 109.5 . . ? Si4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si4 C39 H39A 109.5 . . ? Si4 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si4 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si4 C40 H40A 109.5 . . ? Si4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C16B H16D 109.5 . . ? Si2 C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? Si2 C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? Si2 C15B H15D 109.5 . . ? Si2 C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? Si2 C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? Si2 C14B H14D 109.5 . . ? Si2 C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? Si2 C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.201 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.095 #===========END============= data_1b _database_code_depnum_ccdc_archive 'CCDC 753705' #TrackingRef 'complexes_1-61.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H66 Lu2 N4 O2 Si4' _chemical_formula_weight 1097.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3018(5) _cell_length_b 35.7385(17) _cell_length_c 12.1937(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.5500(10) _cell_angle_gamma 90.00 _cell_volume 4924.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 4.117 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5085 _exptl_absorpt_correction_T_max 0.6379 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27545 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.04 _reflns_number_total 9673 _reflns_number_gt 7986 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0322P)^2^+4.5374P] 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 9673 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.948 _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 Lu1 Lu 0.731645(15) 0.592760(5) 0.894942(14) 0.02808(6) Uani 1 1 d . . . Lu2 Lu 0.748093(15) 0.697566(5) 0.942548(14) 0.02721(6) Uani 1 1 d . . . N1 N 0.8629(3) 0.64520(9) 0.9804(3) 0.0280(8) Uani 1 1 d . . . N2 N 0.6857(3) 0.67329(9) 1.0978(3) 0.0291(8) Uani 1 1 d . . . N3 N 0.6975(3) 0.64724(9) 0.7966(3) 0.0295(8) Uani 1 1 d . . . N4 N 0.5441(3) 0.60868(10) 0.9192(3) 0.0332(8) Uani 1 1 d . . . O1 O 0.5979(3) 0.73356(8) 1.0154(2) 0.0378(7) Uani 1 1 d . . . O2 O 0.6416(3) 0.54959(9) 1.0061(3) 0.0437(8) Uani 1 1 d . . . Si1 Si 0.88722(12) 0.52193(3) 0.71522(10) 0.0369(3) Uani 1 1 d . . . Si2 Si 1.04856(12) 0.73636(4) 0.94081(12) 0.0464(3) Uani 1 1 d . . . Si3 Si 0.88450(12) 0.62043(4) 1.35300(10) 0.0400(3) Uani 1 1 d . . . Si4 Si 0.39320(14) 0.60702(4) 0.67061(14) 0.0540(4) Uani 1 1 d . . . C1 C 0.9425(4) 0.62312(12) 0.9242(4) 0.0340(10) Uani 1 1 d . . . H1 H 0.9799 0.6302 0.8598 0.041 Uiso 1 1 calc R . . C2 C 0.9589(4) 0.58970(13) 0.9758(4) 0.0387(11) Uani 1 1 d . . . H2 H 1.0088 0.5704 0.9543 0.046 Uiso 1 1 calc R . . C3 C 0.8849(4) 0.59013(12) 1.0690(4) 0.0365(10) Uani 1 1 d . . . H3 H 0.8750 0.5709 1.1194 0.044 Uiso 1 1 calc R . . C4 C 0.8298(4) 0.62494(11) 1.0702(3) 0.0289(9) Uani 1 1 d . . . C5 C 0.7457(4) 0.64202(11) 1.1519(3) 0.0302(9) Uani 1 1 d . . . H5 H 0.6865 0.6232 1.1717 0.036 Uiso 1 1 calc R . . C6 C 0.5821(4) 0.68539(12) 1.1453(3) 0.0327(10) Uani 1 1 d . . . C7 C 0.5193(4) 0.66878(14) 1.2308(4) 0.0421(11) Uani 1 1 d . . . H7 H 0.5503 0.6476 1.2651 0.051 Uiso 1 1 calc R . . C8 C 0.4120(4) 0.68309(16) 1.2656(4) 0.0509(14) Uani 1 1 d . . . H8 H 0.3723 0.6713 1.3223 0.061 Uiso 1 1 calc R . . C9 C 0.3637(4) 0.71411(17) 1.2184(4) 0.0530(14) Uani 1 1 d . . . H9 H 0.2915 0.7233 1.2425 0.064 Uiso 1 1 calc R . . C10 C 0.4228(4) 0.73182(14) 1.1344(4) 0.0464(13) Uani 1 1 d . . . H10 H 0.3909 0.7531 1.1016 0.056 Uiso 1 1 calc R . . C11 C 0.5295(4) 0.71762(12) 1.0998(3) 0.0342(10) Uani 1 1 d . . . C12 C 0.5586(5) 0.76832(14) 0.9686(4) 0.0587(15) Uani 1 1 d . . . H12A H 0.4820 0.7649 0.9354 0.088 Uiso 1 1 calc R . . H12B H 0.6137 0.7763 0.9140 0.088 Uiso 1 1 calc R . . H12C H 0.5537 0.7869 1.0251 0.088 Uiso 1 1 calc R . . C13 C 0.8897(4) 0.74487(13) 0.9533(4) 0.0448(12) Uani 1 1 d . . . H13A H 0.8689 0.7630 0.8973 0.054 Uiso 1 1 calc R . . H13B H 0.8786 0.7572 1.0234 0.054 Uiso 1 1 calc R . . C14 C 1.1423(5) 0.77960(16) 0.9583(5) 0.0667(17) Uani 1 1 d . . . H14A H 1.1179 0.7981 0.9058 0.100 Uiso 1 1 calc R . . H14B H 1.2239 0.7734 0.9469 0.100 Uiso 1 1 calc R . . H14C H 1.1328 0.7893 1.0311 0.100 Uiso 1 1 calc R . . C15 C 1.0831(5) 0.71682(18) 0.8018(5) 0.0738(18) Uani 1 1 d . . . H15A H 1.0503 0.6921 0.7952 0.111 Uiso 1 1 calc R . . H15B H 1.1674 0.7156 0.7929 0.111 Uiso 1 1 calc R . . H15C H 1.0495 0.7327 0.7462 0.111 Uiso 1 1 calc R . . C16 C 1.1021(5) 0.70210(16) 1.0466(5) 0.0734(19) Uani 1 1 d . . . H16A H 1.0904 0.7123 1.1185 0.110 Uiso 1 1 calc R . . H16B H 1.1848 0.6973 1.0361 0.110 Uiso 1 1 calc R . . H16C H 1.0585 0.6792 1.0394 0.110 Uiso 1 1 calc R . . C17 C 0.8108(4) 0.65462(12) 1.2567(3) 0.0316(10) Uani 1 1 d . . . H17A H 0.7543 0.6687 1.2996 0.038 Uiso 1 1 calc R . . H17B H 0.8712 0.6722 1.2342 0.038 Uiso 1 1 calc R . . C18 C 1.0407(5) 0.61182(16) 1.3123(5) 0.0597(15) Uani 1 1 d . . . H18A H 1.0822 0.6352 1.3085 0.090 Uiso 1 1 calc R . . H18B H 1.0419 0.5999 1.2418 0.090 Uiso 1 1 calc R . . H18C H 1.0784 0.5959 1.3656 0.090 Uiso 1 1 calc R . . C19 C 0.7980(5) 0.57597(15) 1.3593(4) 0.0608(15) Uani 1 1 d . . . H19A H 0.7990 0.5639 1.2889 0.091 Uiso 1 1 calc R . . H19B H 0.7177 0.5814 1.3789 0.091 Uiso 1 1 calc R . . H19C H 0.8327 0.5597 1.4133 0.091 Uiso 1 1 calc R . . C20 C 0.8843(6) 0.64243(15) 1.4917(4) 0.0624(16) Uani 1 1 d . . . H20A H 0.9292 0.6272 1.5419 0.094 Uiso 1 1 calc R . . H20B H 0.8043 0.6445 1.5170 0.094 Uiso 1 1 calc R . . H20C H 0.9191 0.6669 1.4877 0.094 Uiso 1 1 calc R . . C21 C 0.7646(4) 0.67330(13) 0.7403(3) 0.0383(11) Uani 1 1 d . . . H21 H 0.8412 0.6693 0.7157 0.046 Uiso 1 1 calc R . . C22 C 0.7015(5) 0.70596(13) 0.7258(3) 0.0433(12) Uani 1 1 d . . . H22 H 0.7273 0.7275 0.6907 0.052 Uiso 1 1 calc R . . C23 C 0.5905(4) 0.70036(13) 0.7744(4) 0.0411(11) Uani 1 1 d . . . H23 H 0.5293 0.7177 0.7783 0.049 Uiso 1 1 calc R . . C24 C 0.5894(4) 0.66424(12) 0.8154(3) 0.0344(10) Uani 1 1 d . . . C25 C 0.4933(4) 0.64311(12) 0.8734(4) 0.0404(11) Uani 1 1 d . . . H25 H 0.4672 0.6586 0.9350 0.049 Uiso 1 1 calc R . . C26 C 0.4833(4) 0.59222(13) 1.0043(4) 0.0416(12) Uani 1 1 d . . . C27 C 0.3755(5) 0.60461(16) 1.0505(5) 0.0601(16) Uani 1 1 d . . . H27 H 0.3361 0.6251 1.0206 0.072 Uiso 1 1 calc R . . C28 C 0.3287(6) 0.5860(2) 1.1409(6) 0.082(2) Uani 1 1 d . . . H28 H 0.2581 0.5945 1.1706 0.098 Uiso 1 1 calc R . . C29 C 0.3829(6) 0.5560(2) 1.1868(6) 0.086(2) Uani 1 1 d . . . H29 H 0.3499 0.5444 1.2476 0.103 Uiso 1 1 calc R . . C30 C 0.4876(5) 0.54248(17) 1.1432(5) 0.0656(17) Uani 1 1 d . . . H30 H 0.5251 0.5217 1.1737 0.079 Uiso 1 1 calc R . . C31 C 0.5347(5) 0.56037(14) 1.0542(4) 0.0462(12) Uani 1 1 d . . . C32 C 0.6942(5) 0.51473(14) 1.0415(5) 0.0603(15) Uani 1 1 d . . . H32A H 0.7180 0.5167 1.1171 0.090 Uiso 1 1 calc R . . H32B H 0.7620 0.5094 0.9975 0.090 Uiso 1 1 calc R . . H32C H 0.6374 0.4949 1.0336 0.090 Uiso 1 1 calc R . . C33 C 0.7587(4) 0.54991(13) 0.7547(4) 0.0414(11) Uani 1 1 d . . . H33A H 0.6962 0.5317 0.7649 0.050 Uiso 1 1 calc R . . H33B H 0.7374 0.5635 0.6886 0.050 Uiso 1 1 calc R . . C34 C 1.0129(5) 0.55325(16) 0.6786(5) 0.0621(16) Uani 1 1 d . . . H34A H 0.9888 0.5696 0.6201 0.093 Uiso 1 1 calc R . . H34B H 1.0788 0.5384 0.6554 0.093 Uiso 1 1 calc R . . H34C H 1.0356 0.5678 0.7414 0.093 Uiso 1 1 calc R . . C35 C 0.9416(5) 0.49119(14) 0.8288(4) 0.0539(14) Uani 1 1 d . . . H35A H 0.9624 0.5063 0.8912 0.081 Uiso 1 1 calc R . . H35B H 1.0098 0.4776 0.8049 0.081 Uiso 1 1 calc R . . H35C H 0.8804 0.4739 0.8487 0.081 Uiso 1 1 calc R . . C36 C 0.8587(5) 0.49050(14) 0.5950(4) 0.0511(13) Uani 1 1 d . . . H36A H 0.8029 0.4715 0.6151 0.077 Uiso 1 1 calc R . . H36B H 0.9315 0.4790 0.5732 0.077 Uiso 1 1 calc R . . H36C H 0.8271 0.5049 0.5351 0.077 Uiso 1 1 calc R . . C37 C 0.3856(4) 0.63790(14) 0.7947(5) 0.0546(14) Uani 1 1 d . . . H37A H 0.3632 0.6626 0.7692 0.065 Uiso 1 1 calc R . . H37B H 0.3207 0.6288 0.8388 0.065 Uiso 1 1 calc R . . C38 C 0.3899(6) 0.55673(15) 0.7118(6) 0.080(2) Uani 1 1 d . . . H38A H 0.3850 0.5413 0.6474 0.119 Uiso 1 1 calc R . . H38B H 0.3223 0.5522 0.7570 0.119 Uiso 1 1 calc R . . H38C H 0.4608 0.5508 0.7522 0.119 Uiso 1 1 calc R . . C39 C 0.2564(5) 0.61816(19) 0.5874(5) 0.083(2) Uani 1 1 d . . . H39A H 0.2660 0.6419 0.5520 0.124 Uiso 1 1 calc R . . H39B H 0.1891 0.6191 0.6348 0.124 Uiso 1 1 calc R . . H39C H 0.2443 0.5991 0.5329 0.124 Uiso 1 1 calc R . . C40 C 0.5239(5) 0.61623(17) 0.5832(4) 0.0657(16) Uani 1 1 d . . . H40A H 0.5948 0.6096 0.6226 0.099 Uiso 1 1 calc R . . H40B H 0.5264 0.6423 0.5644 0.099 Uiso 1 1 calc R . . H40C H 0.5181 0.6015 0.5175 0.099 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.02750(10) 0.02680(10) 0.02997(10) -0.00259(8) 0.00166(7) 0.00115(7) Lu2 0.02987(10) 0.02539(10) 0.02634(10) -0.00028(7) -0.00126(7) 0.00059(7) N1 0.0238(18) 0.031(2) 0.0297(19) -0.0035(15) 0.0006(14) 0.0012(14) N2 0.0288(19) 0.0298(19) 0.0287(18) 0.0021(15) -0.0001(14) 0.0077(15) N3 0.031(2) 0.032(2) 0.0262(18) -0.0049(15) -0.0020(15) -0.0005(15) N4 0.0264(19) 0.035(2) 0.038(2) -0.0049(17) 0.0057(16) -0.0028(15) O1 0.0439(19) 0.0330(18) 0.0364(17) -0.0010(14) -0.0078(14) 0.0119(14) O2 0.049(2) 0.0353(18) 0.0469(19) 0.0083(15) 0.0080(16) -0.0002(15) Si1 0.0430(8) 0.0324(7) 0.0353(7) -0.0019(6) 0.0043(6) 0.0085(5) Si2 0.0390(8) 0.0447(8) 0.0555(9) -0.0008(7) 0.0021(6) -0.0122(6) Si3 0.0547(9) 0.0378(7) 0.0273(6) 0.0009(6) -0.0043(6) 0.0110(6) Si4 0.0489(9) 0.0415(8) 0.0710(10) 0.0038(8) -0.0284(8) -0.0073(7) C1 0.027(2) 0.038(3) 0.037(2) -0.009(2) 0.0013(19) -0.0024(19) C2 0.038(3) 0.034(3) 0.044(3) -0.015(2) -0.007(2) 0.014(2) C3 0.045(3) 0.027(2) 0.038(3) -0.004(2) -0.004(2) 0.009(2) C4 0.032(2) 0.028(2) 0.027(2) -0.0056(18) -0.0085(17) 0.0005(18) C5 0.035(2) 0.029(2) 0.026(2) -0.0028(18) 0.0007(18) 0.0020(18) C6 0.029(2) 0.038(3) 0.031(2) -0.014(2) -0.0057(18) 0.0049(18) C7 0.039(3) 0.049(3) 0.038(3) -0.008(2) 0.006(2) -0.004(2) C8 0.039(3) 0.074(4) 0.041(3) -0.019(3) 0.009(2) -0.009(3) C9 0.026(3) 0.080(4) 0.053(3) -0.030(3) 0.002(2) 0.003(3) C10 0.038(3) 0.048(3) 0.053(3) -0.027(2) -0.017(2) 0.014(2) C11 0.036(3) 0.037(3) 0.030(2) -0.013(2) -0.0058(19) 0.005(2) C12 0.080(4) 0.047(3) 0.050(3) 0.001(3) -0.012(3) 0.031(3) C13 0.047(3) 0.036(3) 0.052(3) -0.002(2) -0.001(2) -0.010(2) C14 0.050(4) 0.064(4) 0.086(4) -0.003(3) 0.005(3) -0.021(3) C15 0.064(4) 0.077(4) 0.080(4) -0.011(4) 0.025(3) -0.017(3) C16 0.067(4) 0.057(4) 0.095(5) 0.010(3) -0.040(4) -0.014(3) C17 0.042(3) 0.030(2) 0.023(2) -0.0009(18) -0.0020(18) 0.0086(19) C18 0.054(3) 0.061(4) 0.064(4) -0.017(3) -0.012(3) 0.020(3) C19 0.086(4) 0.051(3) 0.046(3) 0.008(3) 0.009(3) 0.000(3) C20 0.092(5) 0.064(4) 0.031(3) -0.003(3) -0.006(3) 0.020(3) C21 0.050(3) 0.040(3) 0.024(2) -0.002(2) 0.002(2) -0.005(2) C22 0.067(3) 0.038(3) 0.025(2) 0.007(2) -0.007(2) -0.002(2) C23 0.052(3) 0.036(3) 0.035(3) 0.002(2) -0.014(2) 0.010(2) C24 0.032(2) 0.037(3) 0.034(2) -0.007(2) -0.0109(19) 0.0032(19) C25 0.031(3) 0.036(3) 0.055(3) -0.011(2) 0.001(2) 0.0042(19) C26 0.039(3) 0.040(3) 0.046(3) -0.015(2) 0.009(2) -0.010(2) C27 0.041(3) 0.059(4) 0.080(4) -0.014(3) 0.025(3) -0.013(3) C28 0.067(4) 0.077(5) 0.102(5) -0.021(4) 0.049(4) -0.018(4) C29 0.093(5) 0.083(5) 0.083(5) -0.009(4) 0.055(4) -0.031(4) C30 0.078(4) 0.059(4) 0.060(4) 0.009(3) 0.022(3) -0.019(3) C31 0.052(3) 0.043(3) 0.044(3) 0.000(2) 0.013(2) -0.012(2) C32 0.082(4) 0.036(3) 0.063(4) 0.011(3) 0.005(3) 0.001(3) C33 0.044(3) 0.040(3) 0.040(3) -0.009(2) -0.004(2) 0.006(2) C34 0.061(4) 0.066(4) 0.060(4) -0.003(3) 0.018(3) -0.007(3) C35 0.067(4) 0.041(3) 0.053(3) 0.000(3) -0.003(3) 0.017(3) C36 0.067(4) 0.045(3) 0.042(3) -0.009(2) 0.012(2) 0.008(3) C37 0.034(3) 0.046(3) 0.084(4) 0.000(3) -0.011(3) 0.006(2) C38 0.090(5) 0.046(4) 0.103(5) 0.006(4) -0.030(4) -0.008(3) C39 0.065(4) 0.075(5) 0.107(5) 0.015(4) -0.049(4) -0.012(3) C40 0.070(4) 0.068(4) 0.059(4) -0.012(3) -0.016(3) -0.005(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 Lu1 N4 2.217(3) . ? Lu1 O2 2.298(3) . ? Lu1 N3 2.317(3) . ? Lu1 C33 2.318(4) . ? Lu1 N1 2.601(3) . ? Lu1 C1 2.640(4) . ? Lu1 C4 2.659(4) . ? Lu1 C3 2.728(4) . ? Lu1 C2 2.745(4) . ? Lu1 Lu2 3.7946(3) . ? Lu2 N2 2.204(3) . ? Lu2 O1 2.314(3) . ? Lu2 N1 2.321(3) . ? Lu2 C13 2.331(4) . ? Lu2 N3 2.590(3) . ? Lu2 C21 2.623(4) . ? Lu2 C24 2.643(4) . ? Lu2 C23 2.704(4) . ? Lu2 C22 2.706(4) . ? N1 C4 1.368(5) . ? N1 C1 1.383(5) . ? N2 C6 1.381(5) . ? N2 C5 1.461(5) . ? N3 C24 1.385(5) . ? N3 C21 1.387(5) . ? N4 C26 1.381(6) . ? N4 C25 1.466(6) . ? O1 C11 1.413(5) . ? O1 C12 1.436(5) . ? O2 C31 1.402(6) . ? O2 C32 1.444(6) . ? Si1 C33 1.831(4) . ? Si1 C34 1.866(5) . ? Si1 C35 1.867(5) . ? Si1 C36 1.872(5) . ? Si2 C13 1.829(5) . ? Si2 C16 1.875(6) . ? Si2 C15 1.878(6) . ? Si2 C14 1.885(5) . ? Si3 C18 1.864(5) . ? Si3 C20 1.865(5) . ? Si3 C19 1.868(6) . ? Si3 C17 1.884(4) . ? Si4 C40 1.860(6) . ? Si4 C38 1.867(6) . ? Si4 C39 1.884(5) . ? Si4 C37 1.876(6) . ? C1 C2 1.362(6) . ? C2 C3 1.417(6) . ? C3 C4 1.391(6) . ? C4 C5 1.513(6) . ? C5 C17 1.535(6) . ? C6 C7 1.399(6) . ? C6 C11 1.408(6) . ? C7 C8 1.386(6) . ? C8 C9 1.361(8) . ? C9 C10 1.382(7) . ? C10 C11 1.379(6) . ? C21 C22 1.378(6) . ? C22 C23 1.407(7) . ? C23 C24 1.384(6) . ? C24 C25 1.506(6) . ? C25 C37 1.554(7) . ? C26 C31 1.413(7) . ? C26 C27 1.418(6) . ? C27 C28 1.396(8) . ? C28 C29 1.354(9) . ? C29 C30 1.389(8) . ? C30 C31 1.371(7) . ? 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 Lu1 O2 70.38(12) . . ? N4 Lu1 N3 72.47(12) . . ? O2 Lu1 N3 142.85(12) . . ? N4 Lu1 C33 113.65(15) . . ? O2 Lu1 C33 93.09(15) . . ? N3 Lu1 C33 101.30(14) . . ? N4 Lu1 N1 107.69(11) . . ? O2 Lu1 N1 120.10(11) . . ? N3 Lu1 N1 72.14(11) . . ? C33 Lu1 N1 133.83(14) . . ? N4 Lu1 C1 137.69(13) . . ? O2 Lu1 C1 126.91(13) . . ? N3 Lu1 C1 82.55(13) . . ? C33 Lu1 C1 104.22(15) . . ? N1 Lu1 C1 30.60(11) . . ? N4 Lu1 C4 99.99(13) . . ? O2 Lu1 C4 90.00(12) . . ? N3 Lu1 C4 96.81(12) . . ? C33 Lu1 C4 145.23(15) . . ? N1 Lu1 C4 30.12(11) . . ? C1 Lu1 C4 49.06(13) . . ? N4 Lu1 C3 120.37(13) . . ? O2 Lu1 C3 78.42(13) . . ? N3 Lu1 C3 122.20(12) . . ? C33 Lu1 C3 117.63(14) . . ? N1 Lu1 C3 50.06(12) . . ? C1 Lu1 C3 48.95(14) . . ? C4 Lu1 C3 29.90(12) . . ? N4 Lu1 C2 148.73(13) . . ? O2 Lu1 C2 100.34(13) . . ? N3 Lu1 C2 111.72(13) . . ? C33 Lu1 C2 96.26(14) . . ? N1 Lu1 C2 49.97(11) . . ? C1 Lu1 C2 29.21(13) . . ? C4 Lu1 C2 49.22(12) . . ? C3 Lu1 C2 30.01(13) . . ? N4 Lu1 Lu2 76.81(9) . . ? O2 Lu1 Lu2 126.43(8) . . ? N3 Lu1 Lu2 42.05(8) . . ? C33 Lu1 Lu2 139.32(12) . . ? N1 Lu1 Lu2 36.94(7) . . ? C1 Lu1 Lu2 62.02(9) . . ? C4 Lu1 Lu2 55.30(9) . . ? C3 Lu1 Lu2 83.41(9) . . ? C2 Lu1 Lu2 86.56(9) . . ? N2 Lu2 O1 69.34(11) . . ? N2 Lu2 N1 72.23(12) . . ? O1 Lu2 N1 141.51(11) . . ? N2 Lu2 C13 117.52(15) . . ? O1 Lu2 C13 94.65(14) . . ? N1 Lu2 C13 101.03(15) . . ? N2 Lu2 N3 104.27(12) . . ? O1 Lu2 N3 119.47(11) . . ? N1 Lu2 N3 72.30(11) . . ? C13 Lu2 N3 133.58(14) . . ? N2 Lu2 C21 134.72(14) . . ? O1 Lu2 C21 127.16(13) . . ? N1 Lu2 C21 82.85(13) . . ? C13 Lu2 C21 103.76(16) . . ? N3 Lu2 C21 30.85(12) . . ? N2 Lu2 C24 96.06(14) . . ? O1 Lu2 C24 88.84(12) . . ? N1 Lu2 C24 97.35(13) . . ? C13 Lu2 C24 145.25(16) . . ? N3 Lu2 C24 30.68(12) . . ? C21 Lu2 C24 49.71(14) . . ? N2 Lu2 C23 116.86(14) . . ? O1 Lu2 C23 77.90(13) . . ? N1 Lu2 C23 122.90(13) . . ? C13 Lu2 C23 117.57(16) . . ? N3 Lu2 C23 50.61(12) . . ? C21 Lu2 C23 49.58(15) . . ? C24 Lu2 C23 29.98(13) . . ? N2 Lu2 C22 145.22(14) . . ? O1 Lu2 C22 100.19(13) . . ? N1 Lu2 C22 112.73(13) . . ? C13 Lu2 C22 95.84(17) . . ? N3 Lu2 C22 50.68(12) . . ? C21 Lu2 C22 29.92(14) . . ? C24 Lu2 C22 49.65(15) . . ? C23 Lu2 C22 30.14(14) . . ? N2 Lu2 Lu1 74.17(9) . . ? O1 Lu2 Lu1 124.92(8) . . ? N1 Lu2 Lu1 42.35(8) . . ? C13 Lu2 Lu1 139.21(12) . . ? N3 Lu2 Lu1 36.81(7) . . ? C21 Lu2 Lu1 62.20(10) . . ? C24 Lu2 Lu1 55.49(10) . . ? C23 Lu2 Lu1 83.66(10) . . ? C22 Lu2 Lu1 87.20(10) . . ? C4 N1 C1 106.2(3) . . ? C4 N1 Lu2 115.4(3) . . ? C1 N1 Lu2 136.6(3) . . ? C4 N1 Lu1 77.3(2) . . ? C1 N1 Lu1 76.2(2) . . ? Lu2 N1 Lu1 100.71(12) . . ? C6 N2 C5 116.2(3) . . ? C6 N2 Lu2 121.1(3) . . ? C5 N2 Lu2 122.6(2) . . ? C24 N3 C21 105.9(4) . . ? C24 N3 Lu1 115.2(3) . . ? C21 N3 Lu1 137.0(3) . . ? C24 N3 Lu2 76.7(2) . . ? C21 N3 Lu2 75.9(2) . . ? Lu1 N3 Lu2 101.14(12) . . ? C26 N4 C25 116.6(4) . . ? C26 N4 Lu1 118.3(3) . . ? C25 N4 Lu1 122.4(3) . . ? C11 O1 C12 118.0(4) . . ? C11 O1 Lu2 117.7(2) . . ? C12 O1 Lu2 123.6(3) . . ? C31 O2 C32 117.8(4) . . ? C31 O2 Lu1 116.8(3) . . ? C32 O2 Lu1 124.9(3) . . ? C33 Si1 C34 110.0(2) . . ? C33 Si1 C35 112.5(2) . . ? C34 Si1 C35 106.6(3) . . ? C33 Si1 C36 113.7(2) . . ? C34 Si1 C36 107.3(2) . . ? C35 Si1 C36 106.3(2) . . ? C13 Si2 C16 111.2(3) . . ? C13 Si2 C15 110.5(3) . . ? C16 Si2 C15 108.0(3) . . ? C13 Si2 C14 113.9(2) . . ? C16 Si2 C14 106.3(3) . . ? C15 Si2 C14 106.6(3) . . ? C18 Si3 C20 108.7(3) . . ? C18 Si3 C19 111.6(3) . . ? C20 Si3 C19 108.4(3) . . ? C18 Si3 C17 110.8(2) . . ? C20 Si3 C17 106.7(2) . . ? C19 Si3 C17 110.4(2) . . ? C40 Si4 C38 110.0(3) . . ? C40 Si4 C39 107.9(3) . . ? C38 Si4 C39 109.3(3) . . ? C40 Si4 C37 113.6(2) . . ? C38 Si4 C37 110.4(3) . . ? C39 Si4 C37 105.5(3) . . ? C2 C1 N1 110.9(4) . . ? C2 C1 Lu1 79.7(3) . . ? N1 C1 Lu1 73.2(2) . . ? C1 C2 C3 106.4(4) . . ? C1 C2 Lu1 71.1(2) . . ? C3 C2 Lu1 74.3(3) . . ? C4 C3 C2 106.6(4) . . ? C4 C3 Lu1 72.3(2) . . ? C2 C3 Lu1 75.7(3) . . ? N1 C4 C3 109.8(4) . . ? N1 C4 C5 119.5(3) . . ? C3 C4 C5 130.7(4) . . ? N1 C4 Lu1 72.6(2) . . ? C3 C4 Lu1 77.8(2) . . ? C5 C4 Lu1 116.4(3) . . ? N2 C5 C4 107.6(3) . . ? N2 C5 C17 111.6(3) . . ? C4 C5 C17 111.6(3) . . ? N2 C6 C7 128.2(4) . . ? N2 C6 C11 116.6(4) . . ? C7 C6 C11 115.2(4) . . ? C8 C7 C6 121.5(5) . . ? C9 C8 C7 121.4(5) . . ? C8 C9 C10 119.4(5) . . ? C11 C10 C9 119.3(5) . . ? C10 C11 C6 123.2(4) . . ? C10 C11 O1 124.1(4) . . ? C6 C11 O1 112.7(4) . . ? Si2 C13 Lu2 123.3(2) . . ? C5 C17 Si3 122.3(3) . . ? C22 C21 N3 110.3(4) . . ? C22 C21 Lu2 78.4(3) . . ? N3 C21 Lu2 73.3(2) . . ? C21 C22 C23 106.7(4) . . ? C21 C22 Lu2 71.7(2) . . ? C23 C22 Lu2 74.8(2) . . ? C24 C23 C22 107.2(4) . . ? C24 C23 Lu2 72.5(2) . . ? C22 C23 Lu2 75.0(3) . . ? N3 C24 C23 109.8(4) . . ? N3 C24 C25 120.0(4) . . ? C23 C24 C25 130.3(4) . . ? N3 C24 Lu2 72.6(2) . . ? C23 C24 Lu2 77.5(3) . . ? C25 C24 Lu2 116.0(3) . . ? N4 C25 C24 108.6(4) . . ? N4 C25 C37 115.8(4) . . ? C24 C25 C37 109.5(4) . . ? N4 C26 C31 117.5(4) . . ? N4 C26 C27 126.9(5) . . ? C31 C26 C27 115.6(5) . . ? C28 C27 C26 119.9(6) . . ? C29 C28 C27 122.0(6) . . ? C28 C29 C30 120.0(6) . . ? C31 C30 C29 118.7(6) . . ? C30 C31 O2 123.0(5) . . ? C30 C31 C26 123.7(5) . . ? O2 C31 C26 113.2(4) . . ? Si1 C33 Lu1 131.7(2) . . ? C25 C37 Si4 121.8(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.190 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.100 #===========END============= data_3 _database_code_depnum_ccdc_archive 'CCDC 753711' #TrackingRef 'complexes_1-61.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H96 Lu2 N4 O4 Si4' _chemical_formula_weight 1639.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/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 25.9197(9) _cell_length_b 14.7975(5) _cell_length_c 21.2559(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.8190(10) _cell_angle_gamma 90.00 _cell_volume 7881.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 2.600 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6519 _exptl_absorpt_correction_T_max 0.7286 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21515 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.04 _reflns_number_total 7786 _reflns_number_gt 6845 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0350P)^2^+18.7039P] 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 7786 _refine_ls_number_parameters 420 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.009 _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 Lu Lu 0.955605(5) 0.219775(9) 0.811653(6) 0.02359(6) Uani 1 1 d . . . N1 N 0.93625(11) 0.34797(19) 0.75801(13) 0.0271(6) Uani 1 1 d . . . N2 N 0.94670(11) 0.18914(19) 0.70239(14) 0.0263(6) Uani 1 1 d . . . O1 O 0.94511(10) 0.33343(17) 0.88177(11) 0.0329(5) Uani 1 1 d . . . O2 O 0.89516(9) 0.14563(16) 0.82556(11) 0.0304(5) Uani 1 1 d . . . Si1 Si 0.83661(4) 0.39395(8) 0.56837(5) 0.0346(2) Uani 1 1 d . . . Si2 Si 0.86903(5) -0.07468(8) 0.83965(6) 0.0443(3) Uani 1 1 d . . . C1 C 1.04159(14) 0.1163(2) 0.83299(18) 0.0318(8) Uani 1 1 d . . . C2 C 1.04055(14) 0.1456(3) 0.89489(18) 0.0355(8) Uani 1 1 d . . . C3 C 1.05217(14) 0.2398(3) 0.89775(17) 0.0319(8) Uani 1 1 d . . . C4 C 1.06058(13) 0.2634(2) 0.83766(17) 0.0271(7) Uani 1 1 d . . . C5 C 0.94370(17) 0.3194(3) 0.94816(18) 0.0411(9) Uani 1 1 d . . . H5A H 0.9751 0.3448 0.9767 0.062 Uiso 1 1 calc R . . H5B H 0.9424 0.2557 0.9564 0.062 Uiso 1 1 calc R . . H5C H 0.9126 0.3481 0.9557 0.062 Uiso 1 1 calc R . . C6 C 0.94367(13) 0.4230(2) 0.85907(18) 0.0311(8) Uani 1 1 d . . . C7 C 0.94779(16) 0.4967(3) 0.8991(2) 0.0420(9) Uani 1 1 d . . . H7 H 0.9515 0.4896 0.9435 0.050 Uiso 1 1 calc R . . C8 C 0.94624(18) 0.5825(3) 0.8718(2) 0.0510(11) Uani 1 1 d . . . H8 H 0.9489 0.6336 0.8979 0.061 Uiso 1 1 calc R . . C9 C 0.94081(17) 0.5913(3) 0.8064(2) 0.0477(10) Uani 1 1 d . . . H9 H 0.9399 0.6488 0.7884 0.057 Uiso 1 1 calc R . . C10 C 0.93655(15) 0.5162(2) 0.7663(2) 0.0372(8) Uani 1 1 d . . . H10 H 0.9326 0.5246 0.7220 0.045 Uiso 1 1 calc R . . C11 C 0.93808(13) 0.4284(2) 0.79091(17) 0.0287(7) Uani 1 1 d . . . C12 C 0.92348(13) 0.3527(2) 0.68694(16) 0.0274(7) Uani 1 1 d . . . H12 H 0.9444 0.4013 0.6742 0.033 Uiso 1 1 calc R . . C13 C 0.86349(13) 0.3718(3) 0.65786(17) 0.0313(8) Uani 1 1 d . . . H13A H 0.8543 0.4237 0.6807 0.038 Uiso 1 1 calc R . . H13B H 0.8440 0.3207 0.6687 0.038 Uiso 1 1 calc R . . C14 C 0.88431(18) 0.4669(4) 0.5384(2) 0.0563(12) Uani 1 1 d . . . H14A H 0.9184 0.4374 0.5466 0.085 Uiso 1 1 calc R . . H14B H 0.8882 0.5238 0.5608 0.085 Uiso 1 1 calc R . . H14C H 0.8708 0.4768 0.4925 0.085 Uiso 1 1 calc R . . C15 C 0.77133(17) 0.4542(3) 0.5574(2) 0.0541(12) Uani 1 1 d . . . H15A H 0.7542 0.4594 0.5118 0.081 Uiso 1 1 calc R . . H15B H 0.7775 0.5135 0.5762 0.081 Uiso 1 1 calc R . . H15C H 0.7488 0.4207 0.5785 0.081 Uiso 1 1 calc R . . C16 C 0.82258(19) 0.2877(3) 0.5199(2) 0.0570(12) Uani 1 1 d . . . H16A H 0.8019 0.3015 0.4766 0.086 Uiso 1 1 calc R . . H16B H 0.8029 0.2469 0.5401 0.086 Uiso 1 1 calc R . . H16C H 0.8556 0.2601 0.5179 0.086 Uiso 1 1 calc R . . C17 C 0.81912(17) 0.2843(3) 0.8400(2) 0.0429(9) Uani 1 1 d . . . H17 H 0.8235 0.2887 0.7981 0.051 Uiso 1 1 calc R . . C18 C 0.80402(18) 0.3598(3) 0.8694(2) 0.0561(12) Uani 1 1 d . . . H18 H 0.7986 0.4146 0.8473 0.067 Uiso 1 1 calc R . . C19 C 0.79701(18) 0.3539(4) 0.9314(3) 0.0620(14) Uani 1 1 d . . . H19 H 0.7867 0.4046 0.9511 0.074 Uiso 1 1 calc R . . C20 C 0.80514(18) 0.2733(4) 0.9641(2) 0.0556(12) Uani 1 1 d . . . H20 H 0.8004 0.2692 1.0059 0.067 Uiso 1 1 calc R . . C21 C 0.82063(16) 0.1973(3) 0.9346(2) 0.0430(9) Uani 1 1 d . . . H21 H 0.8262 0.1427 0.9570 0.052 Uiso 1 1 calc R . . C22 C 0.82771(14) 0.2021(3) 0.87248(18) 0.0334(8) Uani 1 1 d . . . C23 C 0.84582(13) 0.1218(2) 0.83706(17) 0.0302(7) Uani 1 1 d . . . C24 C 0.81365(18) 0.1186(3) 0.71297(19) 0.0467(10) Uani 1 1 d . . . H24 H 0.8486 0.1285 0.7107 0.056 Uiso 1 1 calc R . . C25 C 0.7729(2) 0.1128(4) 0.6560(2) 0.0638(14) Uani 1 1 d . . . H25 H 0.7809 0.1194 0.6160 0.077 Uiso 1 1 calc R . . C26 C 0.7216(2) 0.0976(3) 0.6581(2) 0.0652(14) Uani 1 1 d . . . H26 H 0.6946 0.0944 0.6197 0.078 Uiso 1 1 calc R . . C27 C 0.70974(18) 0.0870(3) 0.7169(3) 0.0569(12) Uani 1 1 d . . . H27 H 0.6749 0.0756 0.7188 0.068 Uiso 1 1 calc R . . C28 C 0.75031(16) 0.0934(3) 0.7735(2) 0.0468(10) Uani 1 1 d . . . H28 H 0.7421 0.0866 0.8133 0.056 Uiso 1 1 calc R . . C29 C 0.80268(14) 0.1097(2) 0.77257(17) 0.0332(8) Uani 1 1 d . . . C30 C 0.85342(15) 0.0340(2) 0.87691(18) 0.0342(8) Uani 1 1 d . . . H30A H 0.8211 0.0242 0.8910 0.041 Uiso 1 1 calc R . . H30B H 0.8819 0.0445 0.9158 0.041 Uiso 1 1 calc R . . C31 C 0.8977(3) -0.1501(4) 0.9103(3) 0.0798(18) Uani 1 1 d . . . H31A H 0.9013 -0.2102 0.8949 0.120 Uiso 1 1 calc R . . H31B H 0.8744 -0.1512 0.9389 0.120 Uiso 1 1 calc R . . H31C H 0.9321 -0.1279 0.9334 0.120 Uiso 1 1 calc R . . C32 C 0.9185(2) -0.0620(3) 0.7905(2) 0.0552(12) Uani 1 1 d . . . H32A H 0.9509 -0.0369 0.8171 0.083 Uiso 1 1 calc R . . H32B H 0.9044 -0.0225 0.7544 0.083 Uiso 1 1 calc R . . H32C H 0.9258 -0.1201 0.7746 0.083 Uiso 1 1 calc R . . C33 C 0.8072(2) -0.1282(4) 0.7893(3) 0.0781(17) Uani 1 1 d . . . H33A H 0.7945 -0.0943 0.7498 0.117 Uiso 1 1 calc R . . H33B H 0.7804 -0.1288 0.8132 0.117 Uiso 1 1 calc R . . H33C H 0.8149 -0.1891 0.7789 0.117 Uiso 1 1 calc R . . C34 C 0.9237(2) 0.2631(4) 0.1304(3) 0.124(3) Uani 1 1 d GD . . H34 H 0.9352 0.3215 0.1428 0.149 Uiso 1 1 calc R . . C35 C 0.95630(17) 0.2048(4) 0.1066(3) 0.113(3) Uani 1 1 d G . . H35 H 0.9896 0.2241 0.1032 0.136 Uiso 1 1 calc R . . C36 C 0.9391(2) 0.1175(4) 0.0880(3) 0.160(5) Uani 1 1 d G . . H36 H 0.9609 0.0785 0.0721 0.192 Uiso 1 1 calc R . . C37 C 0.8893(3) 0.0886(4) 0.0931(3) 0.225(8) Uani 1 1 d G . . H37 H 0.8778 0.0302 0.0806 0.269 Uiso 1 1 calc R . . C38 C 0.85672(17) 0.1470(5) 0.1169(3) 0.117(3) Uani 1 1 d GD . . H38 H 0.8234 0.1276 0.1203 0.140 Uiso 1 1 calc R . . C39 C 0.87391(19) 0.2342(4) 0.1355(2) 0.127(4) Uani 1 1 d GD . . C40 C 0.8409(4) 0.2949(6) 0.1552(5) 0.166(5) Uani 1 1 d D . . H40A H 0.8118 0.3106 0.1188 0.248 Uiso 1 1 calc R . . H40B H 0.8607 0.3483 0.1718 0.248 Uiso 1 1 calc R . . H40C H 0.8271 0.2680 0.1887 0.248 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 Lu 0.02261(8) 0.02779(9) 0.02129(8) -0.00004(5) 0.00730(6) -0.00215(5) N1 0.0281(14) 0.0304(15) 0.0248(14) -0.0011(12) 0.0105(11) 0.0011(12) N2 0.0220(13) 0.0304(14) 0.0271(15) -0.0027(12) 0.0076(11) -0.0014(11) O1 0.0373(13) 0.0383(14) 0.0259(12) -0.0031(11) 0.0132(10) -0.0026(11) O2 0.0282(12) 0.0340(13) 0.0304(13) -0.0003(10) 0.0099(10) -0.0075(10) Si1 0.0264(5) 0.0484(6) 0.0305(5) 0.0079(5) 0.0099(4) 0.0081(4) Si2 0.0493(7) 0.0359(6) 0.0502(7) 0.0054(5) 0.0175(5) -0.0043(5) C1 0.0262(17) 0.0366(19) 0.0325(18) 0.0098(15) 0.0075(14) 0.0032(15) C2 0.0277(18) 0.047(2) 0.0301(18) 0.0072(16) 0.0039(14) 0.0004(16) C3 0.0252(17) 0.046(2) 0.0237(17) 0.0014(15) 0.0054(14) -0.0040(15) C4 0.0228(16) 0.0333(18) 0.0253(17) -0.0013(14) 0.0064(13) -0.0029(14) C5 0.045(2) 0.055(2) 0.0257(19) -0.0049(17) 0.0140(16) -0.0061(19) C6 0.0243(17) 0.0365(19) 0.0349(19) -0.0063(15) 0.0121(14) -0.0011(14) C7 0.042(2) 0.045(2) 0.041(2) -0.0157(18) 0.0138(18) -0.0024(18) C8 0.053(3) 0.038(2) 0.062(3) -0.017(2) 0.015(2) 0.0003(19) C9 0.044(2) 0.030(2) 0.069(3) -0.0020(19) 0.015(2) 0.0007(17) C10 0.0349(19) 0.0321(19) 0.046(2) 0.0001(17) 0.0138(17) 0.0024(16) C11 0.0203(15) 0.0338(18) 0.0338(18) -0.0032(15) 0.0106(14) 0.0007(14) C12 0.0263(17) 0.0334(18) 0.0248(17) 0.0018(14) 0.0108(13) 0.0011(14) C13 0.0273(17) 0.040(2) 0.0296(18) 0.0050(15) 0.0125(14) 0.0044(15) C14 0.045(2) 0.076(3) 0.050(3) 0.024(2) 0.016(2) -0.001(2) C15 0.040(2) 0.070(3) 0.053(3) 0.014(2) 0.013(2) 0.023(2) C16 0.040(2) 0.074(3) 0.049(3) -0.011(2) -0.003(2) 0.007(2) C17 0.038(2) 0.044(2) 0.046(2) 0.0024(18) 0.0086(18) 0.0033(17) C18 0.049(3) 0.049(3) 0.064(3) -0.007(2) 0.004(2) 0.012(2) C19 0.040(2) 0.073(3) 0.071(3) -0.030(3) 0.011(2) 0.009(2) C20 0.042(2) 0.080(4) 0.048(3) -0.016(3) 0.018(2) -0.002(2) C21 0.036(2) 0.058(2) 0.036(2) -0.0023(19) 0.0116(17) -0.0078(19) C22 0.0248(17) 0.043(2) 0.0329(19) -0.0007(16) 0.0072(15) -0.0048(15) C23 0.0269(17) 0.0368(19) 0.0285(18) 0.0029(15) 0.0099(14) -0.0063(15) C24 0.051(2) 0.054(3) 0.033(2) 0.0028(19) 0.0066(18) -0.021(2) C25 0.077(3) 0.075(3) 0.032(2) 0.005(2) 0.000(2) -0.033(3) C26 0.065(3) 0.064(3) 0.049(3) 0.009(2) -0.018(2) -0.020(3) C27 0.036(2) 0.060(3) 0.065(3) 0.002(2) -0.005(2) -0.012(2) C28 0.035(2) 0.058(3) 0.046(2) 0.001(2) 0.0061(18) -0.0085(19) C29 0.0344(19) 0.0318(19) 0.0301(19) 0.0021(15) 0.0025(15) -0.0063(15) C30 0.0320(18) 0.040(2) 0.0312(19) 0.0059(16) 0.0101(15) -0.0060(16) C31 0.116(5) 0.055(3) 0.081(4) 0.030(3) 0.048(4) 0.025(3) C32 0.063(3) 0.050(3) 0.059(3) 0.000(2) 0.027(2) -0.001(2) C33 0.071(4) 0.061(3) 0.103(5) -0.028(3) 0.022(3) -0.022(3) C34 0.069(5) 0.193(9) 0.111(6) 0.070(6) 0.023(4) 0.016(5) C35 0.067(4) 0.125(7) 0.142(8) 0.049(6) 0.019(5) -0.019(5) C36 0.094(6) 0.202(11) 0.167(10) 0.085(9) 0.003(6) -0.049(7) C37 0.311(19) 0.258(16) 0.077(7) 0.072(8) 0.000(9) 0.160(15) C38 0.091(5) 0.142(7) 0.089(5) 0.068(5) -0.026(4) -0.040(5) C39 0.082(5) 0.208(11) 0.090(6) 0.076(7) 0.021(4) 0.053(6) C40 0.215(13) 0.163(10) 0.110(8) 0.005(7) 0.025(8) 0.056(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu O2 1.996(2) . ? Lu N1 2.204(3) . ? Lu O1 2.309(2) . ? Lu N2 2.319(3) . ? Lu C1 2.646(3) . ? Lu N2 2.663(3) 2_756 ? Lu C2 2.681(4) . ? Lu C4 2.712(3) . ? Lu C3 2.713(3) . ? Lu Lu 3.9053(3) 2_756 ? N1 C11 1.375(4) . ? N1 C12 1.463(4) . ? N2 C4 1.374(5) 2_756 ? N2 C1 1.391(4) 2_756 ? N2 Lu 2.663(3) 2_756 ? O1 C6 1.407(4) . ? O1 C5 1.436(4) . ? O2 C23 1.407(4) . ? Si1 C16 1.864(5) . ? Si1 C14 1.871(4) . ? Si1 C15 1.874(4) . ? Si1 C13 1.880(4) . ? Si2 C32 1.860(5) . ? Si2 C33 1.862(5) . ? Si2 C31 1.866(5) . ? Si2 C30 1.882(4) . ? C1 N2 1.391(4) 2_756 ? C1 C2 1.392(5) . ? C2 C3 1.424(5) . ? C3 C4 1.394(5) . ? C4 N2 1.373(5) 2_756 ? C4 C12 1.516(5) 2_756 ? C6 C7 1.371(5) . ? C6 C11 1.421(5) . ? C7 C8 1.392(6) . ? C8 C9 1.367(6) . ? C9 C10 1.386(6) . ? C10 C11 1.397(5) . ? C12 C4 1.517(5) 2_756 ? C12 C13 1.545(5) . ? C17 C18 1.385(6) . ? C17 C22 1.388(5) . ? C18 C19 1.378(7) . ? C19 C20 1.368(7) . ? C20 C21 1.396(6) . ? C21 C22 1.380(5) . ? C22 C23 1.543(5) . ? C23 C30 1.536(5) . ? C23 C29 1.542(5) . ? C24 C29 1.374(5) . ? C24 C25 1.391(6) . ? C25 C26 1.361(7) . ? C26 C27 1.372(7) . ? C27 C28 1.383(6) . ? C28 C29 1.384(5) . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.377(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Lu N1 117.80(10) . . ? O2 Lu O1 94.49(9) . . ? N1 Lu O1 70.01(9) . . ? O2 Lu N2 99.21(10) . . ? N1 Lu N2 72.48(10) . . ? O1 Lu N2 142.26(9) . . ? O2 Lu C1 108.38(11) . . ? N1 Lu C1 131.08(10) . . ? O1 Lu C1 122.96(10) . . ? N2 Lu C1 85.54(10) . . ? O2 Lu N2 136.72(9) . 2_756 ? N1 Lu N2 100.70(9) . 2_756 ? O1 Lu N2 117.94(9) . 2_756 ? N2 Lu N2 73.05(10) . 2_756 ? C1 Lu N2 30.38(10) . 2_756 ? O2 Lu C2 102.74(11) . . ? N1 Lu C2 137.18(11) . . ? O1 Lu C2 94.85(11) . . ? N2 Lu C2 115.81(11) . . ? C1 Lu C2 30.29(11) . . ? N2 Lu C2 50.24(10) 2_756 . ? O2 Lu C4 152.30(10) . . ? N1 Lu C4 89.10(10) . . ? O1 Lu C4 88.43(10) . . ? N2 Lu C4 95.07(10) . . ? C1 Lu C4 49.14(11) . . ? N2 Lu C4 29.59(10) 2_756 . ? C2 Lu C4 49.56(11) . . ? O2 Lu C3 125.73(10) . . ? N1 Lu C3 107.68(11) . . ? O1 Lu C3 74.08(10) . . ? N2 Lu C3 122.37(10) . . ? C1 Lu C3 49.92(12) . . ? N2 Lu C3 49.80(10) 2_756 . ? C2 Lu C3 30.61(11) . . ? C4 Lu C3 29.78(10) . . ? O2 Lu Lu 135.98(7) . 2_756 ? N1 Lu Lu 75.41(7) . 2_756 ? O1 Lu Lu 128.32(6) . 2_756 ? N2 Lu Lu 41.64(7) . 2_756 ? C1 Lu Lu 59.99(8) . 2_756 ? N2 Lu Lu 35.36(6) 2_756 2_756 ? C2 Lu Lu 85.27(8) . 2_756 ? C4 Lu Lu 53.43(7) . 2_756 ? C3 Lu Lu 81.51(7) . 2_756 ? C11 N1 C12 116.9(3) . . ? C11 N1 Lu 120.6(2) . . ? C12 N1 Lu 122.5(2) . . ? C4 N2 C1 107.4(3) 2_756 2_756 ? C4 N2 Lu 115.3(2) 2_756 . ? C1 N2 Lu 135.5(2) 2_756 . ? C4 N2 Lu 77.19(18) 2_756 2_756 ? C1 N2 Lu 74.12(18) 2_756 2_756 ? Lu N2 Lu 103.00(10) . 2_756 ? C6 O1 C5 117.9(3) . . ? C6 O1 Lu 117.50(19) . . ? C5 O1 Lu 124.4(2) . . ? C23 O2 Lu 161.2(2) . . ? C16 Si1 C14 110.5(2) . . ? C16 Si1 C15 106.9(2) . . ? C14 Si1 C15 109.7(2) . . ? C16 Si1 C13 112.5(2) . . ? C14 Si1 C13 109.79(19) . . ? C15 Si1 C13 107.35(18) . . ? C32 Si2 C33 109.6(3) . . ? C32 Si2 C31 108.8(3) . . ? C33 Si2 C31 108.4(3) . . ? C32 Si2 C30 113.82(19) . . ? C33 Si2 C30 111.1(2) . . ? C31 Si2 C30 104.9(2) . . ? N2 C1 C2 109.2(3) 2_756 . ? N2 C1 Lu 75.50(18) 2_756 . ? C2 C1 Lu 76.3(2) . . ? C1 C2 C3 106.9(3) . . ? C1 C2 Lu 73.4(2) . . ? C3 C2 Lu 75.9(2) . . ? C4 C3 C2 106.7(3) . . ? C4 C3 Lu 75.1(2) . . ? C2 C3 Lu 73.5(2) . . ? N2 C4 C3 109.8(3) 2_756 . ? N2 C4 C12 119.3(3) 2_756 2_756 ? C3 C4 C12 130.9(3) . 2_756 ? N2 C4 Lu 73.23(17) 2_756 . ? C3 C4 Lu 75.1(2) . . ? C12 C4 Lu 119.0(2) 2_756 . ? C7 C6 O1 123.1(3) . . ? C7 C6 C11 124.0(4) . . ? O1 C6 C11 112.9(3) . . ? C6 C7 C8 118.6(4) . . ? C9 C8 C7 119.7(4) . . ? C8 C9 C10 121.3(4) . . ? C9 C10 C11 121.7(4) . . ? N1 C11 C10 128.4(3) . . ? N1 C11 C6 116.8(3) . . ? C10 C11 C6 114.8(3) . . ? N1 C12 C4 107.7(3) . 2_756 ? N1 C12 C13 111.1(3) . . ? C4 C12 C13 110.9(3) 2_756 . ? C12 C13 Si1 120.7(2) . . ? C18 C17 C22 120.7(4) . . ? C19 C18 C17 120.1(5) . . ? C20 C19 C18 120.0(4) . . ? C19 C20 C21 119.9(5) . . ? C22 C21 C20 120.8(4) . . ? C21 C22 C17 118.5(4) . . ? C21 C22 C23 123.9(4) . . ? C17 C22 C23 117.6(3) . . ? O2 C23 C30 108.3(3) . . ? O2 C23 C29 111.1(3) . . ? C30 C23 C29 110.7(3) . . ? O2 C23 C22 107.2(3) . . ? C30 C23 C22 113.2(3) . . ? C29 C23 C22 106.4(3) . . ? C29 C24 C25 120.5(4) . . ? C26 C25 C24 120.8(4) . . ? C25 C26 C27 119.9(4) . . ? C26 C27 C28 119.1(4) . . ? C27 C28 C29 122.1(4) . . ? C24 C29 C28 117.7(4) . . ? C24 C29 C23 122.3(3) . . ? C28 C29 C23 119.9(3) . . ? C23 C30 Si2 120.1(3) . . ? C35 C34 C39 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C37 120.0 . . ? C38 C37 C36 120.0 . . ? C37 C38 C39 120.0 . . ? C40 C39 C38 120.9(5) . . ? C40 C39 C34 119.0(5) . . ? C38 C39 C34 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.309 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.112 #===========END============= data_6 _database_code_depnum_ccdc_archive 'CCDC 753712' #TrackingRef 'complexes_1-61.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H43 N4 Si Y' _chemical_formula_weight 528.64 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 P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.3180(6) _cell_length_b 13.6148(9) _cell_length_c 21.6514(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2746.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 2.186 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7351 _exptl_absorpt_correction_T_max 0.8110 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15476 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.04 _reflns_number_total 5430 _reflns_number_gt 4086 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1030P)^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 -0.001(12) _refine_ls_number_reflns 5430 _refine_ls_number_parameters 300 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1657 _refine_ls_wR_factor_gt 0.1522 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.73961(6) 1.03510(4) 0.12897(2) 0.02900(18) Uani 1 1 d . . . Si1 Si 0.6525(2) 0.74117(13) 0.12030(10) 0.0499(6) Uani 1 1 d . . . N1 N 0.5598(6) 0.9829(4) 0.1955(2) 0.0372(13) Uani 1 1 d . . . N2 N 0.8268(6) 1.0590(4) 0.2388(2) 0.0399(14) Uani 1 1 d . . . N4 N 0.5647(6) 1.1587(5) 0.0879(3) 0.0497(16) Uani 1 1 d U . . C1 C 0.4156(7) 0.9626(6) 0.1939(3) 0.0462(17) Uani 1 1 d . . . H1 H 0.3605 0.9621 0.1581 0.055 Uiso 1 1 calc R . . C2 C 0.3639(7) 0.9434(5) 0.2508(3) 0.0445(17) Uani 1 1 d . . . H2 H 0.2695 0.9279 0.2607 0.053 Uiso 1 1 calc R . . C3 C 0.4790(7) 0.9513(5) 0.2923(3) 0.0440(17) Uani 1 1 d . . . H3 H 0.4762 0.9415 0.3347 0.053 Uiso 1 1 calc R . . C4 C 0.5958(7) 0.9761(5) 0.2578(3) 0.0372(15) Uani 1 1 d . . . C5 C 0.7472(8) 0.9830(5) 0.2755(3) 0.0449(15) Uani 1 1 d . . . H5A H 0.7926 0.9196 0.2696 0.054 Uiso 1 1 calc R . . H5B H 0.7534 0.9993 0.3190 0.054 Uiso 1 1 calc R . . C6 C 0.7761(8) 1.1569(5) 0.2579(3) 0.0496(18) Uani 1 1 d . . . H6A H 0.7986 1.1672 0.3007 0.074 Uiso 1 1 calc R . . H6B H 0.6742 1.1610 0.2521 0.074 Uiso 1 1 calc R . . H6C H 0.8226 1.2063 0.2334 0.074 Uiso 1 1 calc R . . C7 C 0.9806(8) 1.0519(7) 0.2513(4) 0.061(2) Uani 1 1 d . . . H7A H 0.9974 1.0607 0.2947 0.091 Uiso 1 1 calc R . . H7B H 1.0305 1.1019 0.2286 0.091 Uiso 1 1 calc R . . H7C H 1.0149 0.9885 0.2388 0.091 Uiso 1 1 calc R . . N3 N 0.8659(7) 1.1809(4) 0.1107(3) 0.0531(17) Uani 1 1 d . . . C8 C 0.9923(10) 1.2230(7) 0.1277(5) 0.075(3) Uani 1 1 d U . . H8 H 1.0743 1.1891 0.1397 0.090 Uiso 1 1 calc R . . C9 C 0.9802(11) 1.3226(8) 0.1244(5) 0.085(3) Uani 1 1 d U . . H9 H 1.0522 1.3673 0.1342 0.102 Uiso 1 1 calc R . . C10 C 0.8566(12) 1.3444(8) 0.1059(5) 0.093(3) Uani 1 1 d U . . H10 H 0.8215 1.4081 0.1027 0.112 Uiso 1 1 calc R . . C11 C 0.7752(12) 1.2559(8) 0.0903(5) 0.087(3) Uani 1 1 d DU . . C12 C 0.6448(14) 1.2265(10) 0.0497(6) 0.119(4) Uani 1 1 d DU . . H12A H 0.5873 1.2836 0.0394 0.142 Uiso 1 1 calc R . . H12B H 0.6761 1.1951 0.0118 0.142 Uiso 1 1 calc R . . C13 C 0.4374(13) 1.1209(11) 0.0525(6) 0.129(5) Uani 1 1 d U . . H13A H 0.3593 1.1665 0.0563 0.194 Uiso 1 1 calc R . . H13B H 0.4089 1.0584 0.0690 0.194 Uiso 1 1 calc R . . H13C H 0.4626 1.1135 0.0098 0.194 Uiso 1 1 calc R . . C14 C 0.4841(12) 1.2037(9) 0.1388(6) 0.104(4) Uani 1 1 d U . . H14A H 0.5423 1.2528 0.1584 0.156 Uiso 1 1 calc R . . H14B H 0.4588 1.1541 0.1684 0.156 Uiso 1 1 calc R . . H14C H 0.3984 1.2336 0.1229 0.156 Uiso 1 1 calc R . . C15 C 0.8414(7) 0.9670(5) 0.0231(3) 0.0375(15) Uani 1 1 d . . . C16 C 0.9500(7) 0.9473(5) 0.0665(3) 0.0373(16) Uani 1 1 d . . . C17 C 0.8973(7) 0.8759(4) 0.1071(3) 0.0355(15) Uani 1 1 d . . . C18 C 0.7518(7) 0.8515(4) 0.0892(3) 0.0327(13) Uani 1 1 d . . . C19 C 0.7213(7) 0.9080(5) 0.0360(3) 0.0352(15) Uani 1 1 d . . . C15A C 0.8621(10) 1.0332(7) -0.0334(3) 0.065(2) Uani 1 1 d . . . H20A H 0.8911 1.0975 -0.0201 0.098 Uiso 1 1 calc R . . H20B H 0.7734 1.0378 -0.0558 0.098 Uiso 1 1 calc R . . H20C H 0.9347 1.0057 -0.0597 0.098 Uiso 1 1 calc R . . C21 C 1.0992(8) 0.9890(6) 0.0652(5) 0.069(3) Uani 1 1 d . . . H21A H 1.1651 0.9395 0.0513 0.104 Uiso 1 1 calc R . . H21B H 1.1257 1.0100 0.1060 0.104 Uiso 1 1 calc R . . H21C H 1.1022 1.0440 0.0375 0.104 Uiso 1 1 calc R . . C22 C 0.9883(8) 0.8245(6) 0.1556(4) 0.058(2) Uani 1 1 d . . . H22A H 1.0113 0.7595 0.1417 0.086 Uiso 1 1 calc R . . H22B H 0.9359 0.8208 0.1936 0.086 Uiso 1 1 calc R . . H22C H 1.0753 0.8610 0.1620 0.086 Uiso 1 1 calc R . . C23 C 0.5923(8) 0.9000(7) -0.0036(4) 0.061(2) Uani 1 1 d . . . H23A H 0.5964 0.8399 -0.0268 0.091 Uiso 1 1 calc R . . H23B H 0.5892 0.9547 -0.0316 0.091 Uiso 1 1 calc R . . H23C H 0.5078 0.9002 0.0217 0.091 Uiso 1 1 calc R . . C24 C 0.7449(10) 0.6295(5) 0.0906(4) 0.073(2) Uani 1 1 d . . . H24A H 0.7717 0.6396 0.0483 0.109 Uiso 1 1 calc R . . H24B H 0.6814 0.5742 0.0935 0.109 Uiso 1 1 calc R . . H24C H 0.8294 0.6172 0.1148 0.109 Uiso 1 1 calc R . . C25 C 0.6481(10) 0.7318(6) 0.2064(4) 0.071(3) Uani 1 1 d . . . H25A H 0.6152 0.6676 0.2181 0.106 Uiso 1 1 calc R . . H25B H 0.5840 0.7805 0.2227 0.106 Uiso 1 1 calc R . . H25C H 0.7427 0.7424 0.2226 0.106 Uiso 1 1 calc R . . C26 C 0.4628(9) 0.7334(7) 0.0928(4) 0.073(3) Uani 1 1 d . . . H26A H 0.4617 0.7222 0.0490 0.109 Uiso 1 1 calc R . . H26B H 0.4142 0.7939 0.1018 0.109 Uiso 1 1 calc R . . H26C H 0.4150 0.6803 0.1134 0.109 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 0.0312(3) 0.0270(3) 0.0289(3) 0.0004(3) -0.0019(3) -0.0010(3) Si1 0.0633(12) 0.0279(10) 0.0584(14) -0.0045(10) 0.0197(11) -0.0105(9) N1 0.039(3) 0.040(3) 0.033(3) 0.004(3) 0.000(2) -0.004(3) N2 0.041(3) 0.043(4) 0.035(3) -0.006(3) -0.009(2) -0.010(3) N4 0.0506(18) 0.0493(18) 0.0493(18) 0.0001(10) 0.0003(10) 0.0018(10) C1 0.037(3) 0.050(4) 0.051(4) 0.016(4) -0.008(3) -0.001(4) C2 0.040(3) 0.038(4) 0.055(5) -0.004(3) 0.017(3) -0.002(3) C3 0.051(4) 0.038(4) 0.043(4) 0.009(3) 0.012(3) -0.003(3) C4 0.051(4) 0.024(3) 0.037(4) -0.002(3) -0.005(3) 0.006(3) C5 0.054(4) 0.046(4) 0.034(3) -0.004(3) -0.003(4) -0.004(4) C6 0.062(5) 0.047(4) 0.039(4) -0.012(3) -0.009(4) -0.014(4) C7 0.044(4) 0.082(7) 0.056(5) -0.019(5) -0.017(3) -0.003(4) N3 0.056(4) 0.040(3) 0.064(4) -0.005(3) 0.011(3) -0.012(3) C8 0.076(3) 0.075(3) 0.075(3) 0.0000(10) -0.0004(10) -0.0025(10) C9 0.087(3) 0.085(3) 0.084(3) -0.0006(10) -0.0001(10) -0.0024(10) C10 0.094(3) 0.092(3) 0.094(3) -0.0005(10) 0.0022(10) 0.0002(10) C11 0.087(3) 0.086(3) 0.088(3) 0.0004(10) 0.0008(10) -0.0003(10) C12 0.118(4) 0.118(4) 0.119(4) 0.0010(10) 0.0006(10) 0.0006(10) C13 0.129(5) 0.129(5) 0.130(5) 0.0005(10) -0.0004(10) 0.0001(10) C14 0.104(4) 0.104(4) 0.104(4) 0.0004(10) 0.0008(10) 0.0011(10) C15 0.050(4) 0.029(3) 0.033(3) -0.005(3) 0.009(3) 0.002(3) C16 0.035(3) 0.035(4) 0.042(4) -0.010(3) 0.005(3) -0.005(3) C17 0.039(4) 0.027(3) 0.040(4) -0.001(3) 0.000(3) 0.004(3) C18 0.026(3) 0.033(3) 0.039(3) -0.001(2) 0.001(3) -0.002(3) C19 0.046(4) 0.032(3) 0.028(3) -0.012(3) -0.002(3) 0.003(3) C15A 0.091(6) 0.060(5) 0.044(4) 0.023(4) 0.010(4) -0.002(5) C21 0.038(4) 0.076(6) 0.094(6) -0.002(5) 0.009(4) -0.013(4) C22 0.049(4) 0.058(5) 0.066(5) -0.001(4) -0.007(4) 0.022(4) C23 0.060(5) 0.066(5) 0.056(5) -0.008(4) -0.016(4) -0.010(4) C24 0.088(6) 0.039(4) 0.092(6) -0.010(4) 0.032(6) -0.012(5) C25 0.093(6) 0.046(5) 0.073(6) 0.012(4) 0.041(5) -0.002(5) C26 0.065(5) 0.064(6) 0.090(7) -0.026(5) 0.021(5) -0.033(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N1 2.321(5) . ? Y1 N3 2.341(6) . ? Y1 N4 2.506(6) . ? Y1 N2 2.533(5) . ? Y1 C15 2.649(6) . ? Y1 C18 2.646(5) . ? Y1 C16 2.664(6) . ? Y1 C17 2.661(6) . ? Y1 C19 2.660(6) . ? Si1 C24 1.862(8) . ? Si1 C25 1.869(8) . ? Si1 C26 1.868(9) . ? Si1 C18 1.889(6) . ? N1 C1 1.372(8) . ? N1 C4 1.392(8) . ? N2 C7 1.462(9) . ? N2 C6 1.474(9) . ? N2 C5 1.501(8) . ? N4 C12 1.447(13) . ? N4 C14 1.468(12) . ? N4 C13 1.503(13) . ? C1 C2 1.348(9) . ? C2 C3 1.402(10) . ? C3 C4 1.362(9) . ? C4 C5 1.465(10) . ? N3 C8 1.361(11) . ? N3 C11 1.397(12) . ? C8 C9 1.362(13) . ? C9 C10 1.255(14) . ? C10 C11 1.464(14) . ? C11 C12 1.551(12) . ? C15 C19 1.407(9) . ? C15 C16 1.408(9) . ? C15 C15A 1.530(9) . ? C16 C17 1.399(9) . ? C16 C21 1.502(9) . ? C17 C18 1.448(9) . ? C17 C22 1.520(9) . ? C18 C19 1.414(8) . ? C19 C23 1.481(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y1 N3 136.7(2) . . ? N1 Y1 N4 87.52(19) . . ? N3 Y1 N4 72.4(2) . . ? N1 Y1 N2 71.84(18) . . ? N3 Y1 N2 83.6(2) . . ? N4 Y1 N2 117.1(2) . . ? N1 Y1 C15 133.5(2) . . ? N3 Y1 C15 88.3(2) . . ? N4 Y1 C15 99.2(2) . . ? N2 Y1 C15 137.9(2) . . ? N1 Y1 C18 86.76(19) . . ? N3 Y1 C18 136.4(2) . . ? N4 Y1 C18 123.2(2) . . ? N2 Y1 C18 114.36(18) . . ? C15 Y1 C18 51.14(19) . . ? N1 Y1 C16 135.1(2) . . ? N3 Y1 C16 85.7(2) . . ? N4 Y1 C16 126.8(2) . . ? N2 Y1 C16 107.3(2) . . ? C15 Y1 C16 30.7(2) . . ? C18 Y1 C16 51.66(19) . . ? N1 Y1 C17 105.0(2) . . ? N3 Y1 C17 112.52(19) . . ? N4 Y1 C17 147.4(2) . . ? N2 Y1 C17 95.42(19) . . ? C15 Y1 C17 50.5(2) . . ? C18 Y1 C17 31.67(19) . . ? C16 Y1 C17 30.47(19) . . ? N1 Y1 C19 102.9(2) . . ? N3 Y1 C19 117.2(2) . . ? N4 Y1 C19 97.3(2) . . ? N2 Y1 C19 144.49(19) . . ? C15 Y1 C19 30.7(2) . . ? C18 Y1 C19 30.90(18) . . ? C16 Y1 C19 51.06(19) . . ? C17 Y1 C19 51.00(19) . . ? C24 Si1 C25 107.4(4) . . ? C24 Si1 C26 106.4(4) . . ? C25 Si1 C26 107.1(4) . . ? C24 Si1 C18 107.4(3) . . ? C25 Si1 C18 114.9(3) . . ? C26 Si1 C18 113.3(4) . . ? C1 N1 C4 104.3(5) . . ? C1 N1 Y1 138.8(4) . . ? C4 N1 Y1 116.6(4) . . ? C7 N2 C6 108.7(6) . . ? C7 N2 C5 109.9(6) . . ? C6 N2 C5 108.4(5) . . ? C7 N2 Y1 118.7(4) . . ? C6 N2 Y1 106.1(4) . . ? C5 N2 Y1 104.5(4) . . ? C12 N4 C14 115.3(9) . . ? C12 N4 C13 109.6(8) . . ? C14 N4 C13 97.0(8) . . ? C12 N4 Y1 107.2(6) . . ? C14 N4 Y1 110.2(6) . . ? C13 N4 Y1 117.6(7) . . ? C2 C1 N1 111.5(6) . . ? C1 C2 C3 107.2(6) . . ? C4 C3 C2 106.2(6) . . ? C3 C4 N1 110.8(6) . . ? C3 C4 C5 129.9(6) . . ? N1 C4 C5 118.8(6) . . ? C4 C5 N2 112.4(5) . . ? C8 N3 C11 107.5(7) . . ? C8 N3 Y1 138.3(6) . . ? C11 N3 Y1 111.7(6) . . ? N3 C8 C9 109.5(9) . . ? C10 C9 C8 109.2(11) . . ? C9 C10 C11 110.8(11) . . ? N3 C11 C10 102.4(9) . . ? N3 C11 C12 117.7(9) . . ? C10 C11 C12 138.5(10) . . ? N4 C12 C11 104.2(9) . . ? C19 C15 C16 109.2(5) . . ? C19 C15 C15A 126.6(6) . . ? C16 C15 C15A 123.7(7) . . ? C19 C15 Y1 75.1(3) . . ? C16 C15 Y1 75.2(4) . . ? C15A C15 Y1 122.1(5) . . ? C17 C16 C15 107.4(6) . . ? C17 C16 C21 126.8(7) . . ? C15 C16 C21 125.5(7) . . ? C17 C16 Y1 74.6(4) . . ? C15 C16 Y1 74.0(4) . . ? C21 C16 Y1 121.4(5) . . ? C16 C17 C18 108.7(6) . . ? C16 C17 C22 123.9(6) . . ? C18 C17 C22 127.0(6) . . ? C16 C17 Y1 74.9(4) . . ? C18 C17 Y1 73.6(3) . . ? C22 C17 Y1 124.1(4) . . ? C19 C18 C17 106.4(5) . . ? C19 C18 Si1 128.6(5) . . ? C17 C18 Si1 123.1(4) . . ? C19 C18 Y1 75.1(3) . . ? C17 C18 Y1 74.7(3) . . ? Si1 C18 Y1 127.9(3) . . ? C15 C19 C18 108.3(5) . . ? C15 C19 C23 124.9(6) . . ? C18 C19 C23 126.6(6) . . ? C15 C19 Y1 74.2(3) . . ? C18 C19 Y1 74.0(3) . . ? C23 C19 Y1 122.6(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.289 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.097