Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Glen Deacon' 'Craig M. Forsyth' 'Natalie M. Scott' _publ_contact_author_name 'Prof Glen Deacon' _publ_contact_author_address ; School of Chemistry Monash University Wellington Rd Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_email GLEN.DEACON@SCI.MONASH.EDU.AU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Mixed-Ligand Ytterbium(III) Complexes Incorporating One or Two Bidentate (N,O) Amide Ligands ; data_compound1 _database_code_CSD 207491 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(2,6-di-tert-butylphenoxo)(bis(N-(2-phenoxyphenyl)-N-trimethylsilyla mido)ytterbium(III)] ; _chemical_name_common ybphoar _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H57 N2 O3 Si2 Yb' _chemical_formula_weight 891.14 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8480(1) _cell_length_b 15.6557(2) _cell_length_c 20.1433(2) _cell_angle_alpha 77.7021(6) _cell_angle_beta 82.8115(6) _cell_angle_gamma 88.2532(4) _cell_volume 4233.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 59052 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 28.29 _exptl_crystal_description prismatic _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1828 _exptl_absorpt_coefficient_mu 2.305 _exptl_absorpt_correction_type empirical/multiscan _exptl_absorpt_correction_T_min 0.669 _exptl_absorpt_correction_T_max 0.712 _exptl_absorpt_process_details 'SORTAV (R. Blessing 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59052 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.29 _reflns_number_total 19744 _reflns_number_gt 15006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0192P)^2^+3.8736P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19744 _refine_ls_number_parameters 937 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0653 _refine_ls_wR_factor_gt 0.0581 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 Yb1 Yb 0.946385(9) 0.307142(8) 0.249432(6) 0.01519(4) Uani 1 1 d . . . Si1 Si 0.96410(6) 0.52931(6) 0.16502(4) 0.01946(19) Uani 1 1 d . . . O1 O 0.90721(15) 0.26124(13) 0.15111(10) 0.0189(5) Uani 1 1 d . . . N1 N 0.91804(18) 0.42493(16) 0.17193(12) 0.0173(6) Uani 1 1 d . . . Yb2 Yb 0.599561(9) 0.222740(8) -0.215501(6) 0.01587(4) Uani 1 1 d . . . Si2 Si 1.19144(6) 0.27965(6) 0.18454(4) 0.02057(19) Uani 1 1 d . . . O2 O 0.98826(15) 0.35030(13) 0.34761(10) 0.0186(5) Uani 1 1 d . . . N2 N 1.10433(18) 0.28460(16) 0.25391(12) 0.0171(5) Uani 1 1 d . . . O3 O 0.83880(16) 0.22642(13) 0.30894(10) 0.0217(5) Uani 1 1 d . . . Si4 Si 0.52980(7) 0.38470(6) -0.12174(4) 0.02030(19) Uani 1 1 d . . . O4 O 0.50115(15) 0.11450(13) -0.13893(10) 0.0190(5) Uani 1 1 d . . . N4 N 0.50496(18) 0.28776(16) -0.14510(12) 0.0175(6) Uani 1 1 d . . . Si5 Si 0.77903(6) 0.14421(6) -0.10779(4) 0.01951(19) Uani 1 1 d . . . O5 O 0.70498(15) 0.32562(13) -0.29162(10) 0.0205(5) Uani 1 1 d . . . N5 N 0.74958(18) 0.20166(16) -0.18635(12) 0.0187(6) Uani 1 1 d . . . O6 O 0.53118(15) 0.19739(14) -0.29392(10) 0.0218(5) Uani 1 1 d . . . C11 C 0.8604(2) 0.4109(2) 0.12288(15) 0.0178(7) Uani 1 1 d . . . C12 C 0.8536(2) 0.3267(2) 0.10958(14) 0.0176(7) Uani 1 1 d . . . C13 C 0.7981(2) 0.3065(2) 0.06341(15) 0.0229(7) Uani 1 1 d . . . H13 H 0.7964 0.2483 0.0567 0.028 Uiso 1 1 calc R . . C14 C 0.7443(2) 0.3721(2) 0.02657(16) 0.0273(8) Uani 1 1 d . . . H14 H 0.7058 0.3596 -0.0060 0.033 Uiso 1 1 calc R . . C15 C 0.7476(2) 0.4554(2) 0.03775(16) 0.0286(8) Uani 1 1 d . . . H15 H 0.7108 0.5005 0.0128 0.034 Uiso 1 1 calc R . . C16 C 0.8038(2) 0.4744(2) 0.08486(15) 0.0231(7) Uani 1 1 d . . . H16 H 0.8041 0.5326 0.0917 0.028 Uiso 1 1 calc R . . C17 C 1.0047(3) 0.5822(2) 0.07360(17) 0.0311(8) Uani 1 1 d . . . H17A H 0.9490 0.5883 0.0473 0.047 Uiso 1 1 calc R . . H17B H 1.0549 0.5459 0.0542 0.047 Uiso 1 1 calc R . . H17C H 1.0315 0.6401 0.0714 0.047 Uiso 1 1 calc R . . C18 C 0.8756(3) 0.6008(2) 0.20547(18) 0.0356(9) Uani 1 1 d . . . H18A H 0.8551 0.5721 0.2532 0.053 Uiso 1 1 calc R . . H18B H 0.8186 0.6111 0.1804 0.053 Uiso 1 1 calc R . . H18C H 0.9065 0.6568 0.2041 0.053 Uiso 1 1 calc R . . C19 C 1.0725(2) 0.5195(2) 0.21292(17) 0.0271(8) Uani 1 1 d . . . H19A H 1.0532 0.4920 0.2610 0.041 Uiso 1 1 calc R . . H19B H 1.0987 0.5778 0.2100 0.041 Uiso 1 1 calc R . . H19C H 1.1224 0.4836 0.1929 0.041 Uiso 1 1 calc R . . C21 C 1.1305(2) 0.26962(19) 0.32029(15) 0.0184(7) Uani 1 1 d . . . C22 C 1.0723(2) 0.30438(19) 0.37091(15) 0.0190(7) Uani 1 1 d . . . C23 C 1.0901(2) 0.2916(2) 0.43829(16) 0.0251(8) Uani 1 1 d . . . H23 H 1.0480 0.3164 0.4703 0.030 Uiso 1 1 calc R . . C24 C 1.1695(3) 0.2424(2) 0.45842(17) 0.0282(8) Uani 1 1 d . . . H24 H 1.1830 0.2331 0.5045 0.034 Uiso 1 1 calc R . . C25 C 1.2291(3) 0.2070(2) 0.41147(18) 0.0299(8) Uani 1 1 d . . . H25 H 1.2841 0.1733 0.4254 0.036 Uiso 1 1 calc R . . C26 C 1.2105(2) 0.2197(2) 0.34360(17) 0.0246(7) Uani 1 1 d . . . H26 H 1.2528 0.1940 0.3124 0.029 Uiso 1 1 calc R . . C27 C 1.3073(2) 0.3357(2) 0.18978(18) 0.0309(8) Uani 1 1 d . . . H27A H 1.3352 0.3066 0.2312 0.046 Uiso 1 1 calc R . . H27B H 1.2935 0.3970 0.1914 0.046 Uiso 1 1 calc R . . H27C H 1.3538 0.3327 0.1494 0.046 Uiso 1 1 calc R . . C28 C 1.2188(3) 0.1650(2) 0.17536(19) 0.0362(9) Uani 1 1 d . . . H28A H 1.2440 0.1321 0.2167 0.054 Uiso 1 1 calc R . . H28B H 1.2675 0.1653 0.1356 0.054 Uiso 1 1 calc R . . H28C H 1.1591 0.1373 0.1689 0.054 Uiso 1 1 calc R . . C29 C 1.1436(2) 0.3390(2) 0.10416(16) 0.0295(8) Uani 1 1 d . . . H29A H 1.0827 0.3119 0.0993 0.044 Uiso 1 1 calc R . . H29B H 1.1916 0.3358 0.0646 0.044 Uiso 1 1 calc R . . H29C H 1.1315 0.4004 0.1065 0.044 Uiso 1 1 calc R . . C31 C 0.7721(2) 0.16245(19) 0.33496(14) 0.0181(7) Uani 1 1 d . . . C32 C 0.8045(2) 0.0767(2) 0.36405(15) 0.0206(7) Uani 1 1 d . . . C33 C 0.7349(3) 0.0116(2) 0.38529(17) 0.0273(8) Uani 1 1 d . . . H33 H 0.7552 -0.0462 0.4035 0.033 Uiso 1 1 calc R . . C34 C 0.6370(3) 0.0278(2) 0.38094(18) 0.0322(9) Uani 1 1 d . . . H34 H 0.5913 -0.0186 0.3951 0.039 Uiso 1 1 calc R . . C35 C 0.6064(2) 0.1114(2) 0.35594(16) 0.0259(8) Uani 1 1 d . . . H35 H 0.5387 0.1223 0.3547 0.031 Uiso 1 1 calc R . . C36 C 0.6712(2) 0.1808(2) 0.33231(15) 0.0199(7) Uani 1 1 d . . . C41 C 0.4187(2) 0.24300(19) -0.11699(15) 0.0172(7) Uani 1 1 d . . . C42 C 0.4140(2) 0.1517(2) -0.11106(15) 0.0179(7) Uani 1 1 d . . . C43 C 0.3327(2) 0.1023(2) -0.08234(15) 0.0215(7) Uani 1 1 d . . . H43 H 0.3337 0.0409 -0.0791 0.026 Uiso 1 1 calc R . . C44 C 0.2494(2) 0.1433(2) -0.05817(16) 0.0256(8) Uani 1 1 d . . . H44 H 0.1930 0.1101 -0.0378 0.031 Uiso 1 1 calc R . . C45 C 0.2494(2) 0.2334(2) -0.06414(17) 0.0277(8) Uani 1 1 d . . . H45 H 0.1926 0.2620 -0.0480 0.033 Uiso 1 1 calc R . . C46 C 0.3317(2) 0.2814(2) -0.09348(16) 0.0244(7) Uani 1 1 d . . . H46 H 0.3293 0.3431 -0.0979 0.029 Uiso 1 1 calc R . . C47 C 0.4687(3) 0.4824(2) -0.1704(2) 0.0373(9) Uani 1 1 d . . . H47A H 0.3979 0.4755 -0.1605 0.056 Uiso 1 1 calc R . . H47B H 0.4883 0.4878 -0.2195 0.056 Uiso 1 1 calc R . . H47C H 0.4879 0.5352 -0.1565 0.056 Uiso 1 1 calc R . . C48 C 0.4966(2) 0.3759(2) -0.02730(16) 0.0287(8) Uani 1 1 d . . . H48A H 0.5291 0.3248 -0.0022 0.043 Uiso 1 1 calc R . . H48B H 0.4260 0.3696 -0.0159 0.043 Uiso 1 1 calc R . . H48C H 0.5175 0.4288 -0.0145 0.043 Uiso 1 1 calc R . . C49 C 0.6635(2) 0.4043(2) -0.14344(16) 0.0229(7) Uani 1 1 d . . . H49A H 0.6990 0.3546 -0.1193 0.034 Uiso 1 1 calc R . . H49B H 0.6804 0.4577 -0.1295 0.034 Uiso 1 1 calc R . . H49C H 0.6812 0.4109 -0.1929 0.034 Uiso 1 1 calc R . . C51 C 0.8229(2) 0.2294(2) -0.24035(15) 0.0180(7) Uani 1 1 d . . . C52 C 0.8036(2) 0.2958(2) -0.29581(15) 0.0191(7) Uani 1 1 d . . . C53 C 0.8703(2) 0.3254(2) -0.35198(17) 0.0288(8) Uani 1 1 d . . . H53 H 0.8533 0.3705 -0.3884 0.035 Uiso 1 1 calc R . . C54 C 0.9625(3) 0.2889(2) -0.35485(18) 0.0336(9) Uani 1 1 d . . . H54 H 1.0097 0.3092 -0.3930 0.040 Uiso 1 1 calc R . . C55 C 0.9856(2) 0.2231(2) -0.30227(17) 0.0303(8) Uani 1 1 d . . . H55 H 1.0489 0.1979 -0.3041 0.036 Uiso 1 1 calc R . . C56 C 0.9168(2) 0.1931(2) -0.24636(17) 0.0261(8) Uani 1 1 d . . . H56 H 0.9339 0.1466 -0.2110 0.031 Uiso 1 1 calc R . . C57 C 0.6763(2) 0.1564(2) -0.04069(15) 0.0232(7) Uani 1 1 d . . . H57A H 0.6677 0.2183 -0.0390 0.035 Uiso 1 1 calc R . . H57B H 0.6911 0.1232 0.0039 0.035 Uiso 1 1 calc R . . H57C H 0.6164 0.1340 -0.0518 0.035 Uiso 1 1 calc R . . C58 C 0.7950(3) 0.0262(2) -0.1100(2) 0.0392(10) Uani 1 1 d . . . H58A H 0.8488 0.0193 -0.1451 0.059 Uiso 1 1 calc R . . H58B H 0.7349 0.0038 -0.1210 0.059 Uiso 1 1 calc R . . H58C H 0.8096 -0.0065 -0.0652 0.059 Uiso 1 1 calc R . . C59 C 0.8895(3) 0.1872(3) -0.08148(19) 0.0407(10) Uani 1 1 d . . . H59A H 0.8797 0.2491 -0.0803 0.061 Uiso 1 1 calc R . . H59B H 0.9462 0.1808 -0.1145 0.061 Uiso 1 1 calc R . . H59C H 0.9005 0.1542 -0.0359 0.061 Uiso 1 1 calc R . . C61 C 0.5093(2) 0.18903(19) -0.35584(15) 0.0181(7) Uani 1 1 d . . . C62 C 0.5740(2) 0.1462(2) -0.39841(16) 0.0215(7) Uani 1 1 d . . . C63 C 0.5514(3) 0.1477(2) -0.46424(16) 0.0287(8) Uani 1 1 d . . . H63 H 0.5951 0.1210 -0.4940 0.034 Uiso 1 1 calc R . . C64 C 0.4685(3) 0.1864(3) -0.48748(17) 0.0351(9) Uani 1 1 d . . . H64 H 0.4561 0.1875 -0.5330 0.042 Uiso 1 1 calc R . . C65 C 0.4029(2) 0.2239(2) -0.44417(15) 0.0258(8) Uani 1 1 d . . . H65 H 0.3446 0.2490 -0.4601 0.031 Uiso 1 1 calc R . . C66 C 0.4202(2) 0.22562(19) -0.37782(15) 0.0185(7) Uani 1 1 d . . . C111 C 0.8996(2) 0.1738(2) 0.14228(16) 0.0217(7) Uani 1 1 d . . . C112 C 0.9717(3) 0.1434(3) 0.09998(19) 0.0359(9) Uani 1 1 d . . . H112 H 1.0236 0.1800 0.0757 0.043 Uiso 1 1 calc R . . C113 C 0.9659(3) 0.0563(3) 0.0938(2) 0.0558(13) Uani 1 1 d . . . H113 H 1.0152 0.0329 0.0655 0.067 Uiso 1 1 calc R . . C114 C 0.8899(4) 0.0046(3) 0.1281(3) 0.0554(13) Uani 1 1 d . . . H114 H 0.8865 -0.0542 0.1232 0.067 Uiso 1 1 calc R . . C115 C 0.8186(3) 0.0376(2) 0.1696(2) 0.0432(11) Uani 1 1 d . . . H115 H 0.7662 0.0013 0.1935 0.052 Uiso 1 1 calc R . . C116 C 0.8225(3) 0.1235(2) 0.17676(17) 0.0281(8) Uani 1 1 d . . . H116 H 0.7729 0.1469 0.2049 0.034 Uiso 1 1 calc R . . C211 C 0.9279(2) 0.3901(2) 0.39495(15) 0.0210(7) Uani 1 1 d . . . C212 C 0.8486(2) 0.3461(2) 0.43174(16) 0.0270(8) Uani 1 1 d . . . H212 H 0.8354 0.2886 0.4273 0.032 Uiso 1 1 calc R . . C213 C 0.7875(3) 0.3866(2) 0.47580(17) 0.0328(9) Uani 1 1 d . . . H213 H 0.7311 0.3573 0.5011 0.039 Uiso 1 1 calc R . . C214 C 0.8088(3) 0.4692(2) 0.48266(17) 0.0358(9) Uani 1 1 d . . . H214 H 0.7673 0.4967 0.5131 0.043 Uiso 1 1 calc R . . C215 C 0.8894(3) 0.5121(2) 0.44589(18) 0.0427(10) Uani 1 1 d . . . H215 H 0.9036 0.5691 0.4510 0.051 Uiso 1 1 calc R . . C216 C 0.9504(3) 0.4726(2) 0.40110(18) 0.0348(9) Uani 1 1 d . . . H216 H 1.0065 0.5020 0.3753 0.042 Uiso 1 1 calc R . . C321 C 0.9121(2) 0.0541(2) 0.37296(16) 0.0231(7) Uani 1 1 d . . . C322 C 0.9254(3) -0.0418(2) 0.41008(19) 0.0348(9) Uani 1 1 d . . . H32A H 0.9945 -0.0534 0.4144 0.052 Uiso 1 1 calc R . . H32B H 0.9019 -0.0810 0.3836 0.052 Uiso 1 1 calc R . . H32C H 0.8882 -0.0518 0.4557 0.052 Uiso 1 1 calc R . . C323 C 0.9494(3) 0.1108(2) 0.41802(16) 0.0277(8) Uani 1 1 d . . . H32D H 0.9425 0.1727 0.3967 0.042 Uiso 1 1 calc R . . H32E H 1.0181 0.0973 0.4226 0.042 Uiso 1 1 calc R . . H32F H 0.9113 0.0984 0.4634 0.042 Uiso 1 1 calc R . . C324 C 0.9772(3) 0.0661(2) 0.30386(16) 0.0294(8) Uani 1 1 d . . . H32G H 0.9711 0.1263 0.2782 0.044 Uiso 1 1 calc R . . H32H H 0.9569 0.0254 0.2775 0.044 Uiso 1 1 calc R . . H32I H 1.0452 0.0544 0.3119 0.044 Uiso 1 1 calc R . . C361 C 0.6299(2) 0.2726(2) 0.30405(16) 0.0244(7) Uani 1 1 d . . . C362 C 0.6547(3) 0.3376(2) 0.3457(2) 0.0414(10) Uani 1 1 d . . . H36A H 0.6293 0.3164 0.3939 0.062 Uiso 1 1 calc R . . H36B H 0.6252 0.3945 0.3286 0.062 Uiso 1 1 calc R . . H36C H 0.7255 0.3439 0.3416 0.062 Uiso 1 1 calc R . . C363 C 0.5177(2) 0.2734(2) 0.30719(18) 0.0322(9) Uani 1 1 d . . . H36D H 0.4887 0.2536 0.3547 0.048 Uiso 1 1 calc R . . H36E H 0.4981 0.2342 0.2793 0.048 Uiso 1 1 calc R . . H36F H 0.4953 0.3329 0.2895 0.048 Uiso 1 1 calc R . . C364 C 0.6673(3) 0.3041(2) 0.22875(17) 0.0346(9) Uani 1 1 d . . . H36G H 0.6407 0.3624 0.2120 0.052 Uiso 1 1 calc R . . H36H H 0.6467 0.2634 0.2025 0.052 Uiso 1 1 calc R . . H36I H 0.7385 0.3069 0.2232 0.052 Uiso 1 1 calc R . . C411 C 0.5008(2) 0.02300(19) -0.13674(15) 0.0175(7) Uani 1 1 d . . . C412 C 0.5385(2) -0.0325(2) -0.08333(15) 0.0201(7) Uani 1 1 d . . . H412 H 0.5638 -0.0101 -0.0488 0.024 Uiso 1 1 calc R . . C413 C 0.5387(2) -0.1220(2) -0.08097(16) 0.0235(7) Uani 1 1 d . . . H413 H 0.5646 -0.1614 -0.0447 0.028 Uiso 1 1 calc R . . C414 C 0.5015(2) -0.1532(2) -0.13117(17) 0.0279(8) Uani 1 1 d . . . H414 H 0.5011 -0.2144 -0.1291 0.034 Uiso 1 1 calc R . . C415 C 0.4646(2) -0.0967(2) -0.18453(17) 0.0280(8) Uani 1 1 d . . . H415 H 0.4393 -0.1190 -0.2191 0.034 Uiso 1 1 calc R . . C416 C 0.4644(2) -0.0071(2) -0.18780(16) 0.0247(7) Uani 1 1 d . . . H416 H 0.4396 0.0323 -0.2245 0.030 Uiso 1 1 calc R . . C511 C 0.6811(2) 0.4064(2) -0.33280(15) 0.0187(7) Uani 1 1 d . . . C512 C 0.6098(2) 0.4062(2) -0.37410(16) 0.0233(7) Uani 1 1 d . . . H512 H 0.5828 0.3530 -0.3785 0.028 Uiso 1 1 calc R . . C513 C 0.5780(3) 0.4867(2) -0.40950(17) 0.0320(9) Uani 1 1 d . . . H513 H 0.5278 0.4885 -0.4379 0.038 Uiso 1 1 calc R . . C514 C 0.6190(3) 0.5636(2) -0.40351(18) 0.0313(9) Uani 1 1 d . . . H514 H 0.5968 0.6179 -0.4277 0.038 Uiso 1 1 calc R . . C515 C 0.6917(3) 0.5621(2) -0.36289(17) 0.0314(9) Uani 1 1 d . . . H515 H 0.7200 0.6152 -0.3595 0.038 Uiso 1 1 calc R . . C516 C 0.7237(3) 0.4834(2) -0.32689(16) 0.0261(8) Uani 1 1 d . . . H516 H 0.7739 0.4818 -0.2986 0.031 Uiso 1 1 calc R . . C621 C 0.6676(2) 0.0953(2) -0.37914(17) 0.0241(7) Uani 1 1 d . . . C622 C 0.6608(5) 0.0041(4) -0.3907(4) 0.138(4) Uani 1 1 d . . . H62A H 0.6035 -0.0249 -0.3624 0.207 Uiso 1 1 calc R . . H62B H 0.7195 -0.0289 -0.3782 0.207 Uiso 1 1 calc R . . H62C H 0.6551 0.0066 -0.4391 0.207 Uiso 1 1 calc R . . C623 C 0.7558(3) 0.1415(4) -0.4218(3) 0.089(2) Uani 1 1 d . . . H62D H 0.8147 0.1091 -0.4091 0.134 Uiso 1 1 calc R . . H62E H 0.7589 0.2008 -0.4134 0.134 Uiso 1 1 calc R . . H62F H 0.7510 0.1448 -0.4704 0.134 Uiso 1 1 calc R . . C624 C 0.6888(3) 0.0847(3) -0.3045(2) 0.0602(14) Uani 1 1 d . . . H62G H 0.6336 0.0558 -0.2734 0.090 Uiso 1 1 calc R . . H62H H 0.6986 0.1424 -0.2949 0.090 Uiso 1 1 calc R . . H62I H 0.7476 0.0491 -0.2976 0.090 Uiso 1 1 calc R . . C661 C 0.3412(2) 0.2629(2) -0.33007(15) 0.0200(7) Uani 1 1 d . . . C662 C 0.3089(2) 0.1908(2) -0.26733(16) 0.0263(8) Uani 1 1 d . . . H66A H 0.3651 0.1702 -0.2431 0.039 Uiso 1 1 calc R . . H66B H 0.2816 0.1420 -0.2822 0.039 Uiso 1 1 calc R . . H66C H 0.2594 0.2141 -0.2366 0.039 Uiso 1 1 calc R . . C663 C 0.2497(2) 0.2921(2) -0.36516(17) 0.0292(8) Uani 1 1 d . . . H66D H 0.2669 0.3385 -0.4057 0.044 Uiso 1 1 calc R . . H66E H 0.2011 0.3142 -0.3332 0.044 Uiso 1 1 calc R . . H66F H 0.2229 0.2423 -0.3789 0.044 Uiso 1 1 calc R . . C664 C 0.3759(2) 0.3432(2) -0.30710(18) 0.0300(8) Uani 1 1 d . . . H66G H 0.3964 0.3890 -0.3474 0.045 Uiso 1 1 calc R . . H66H H 0.4310 0.3266 -0.2808 0.045 Uiso 1 1 calc R . . H66I H 0.3226 0.3652 -0.2785 0.045 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 Yb1 0.01518(7) 0.01616(7) 0.01473(7) -0.00308(5) -0.00410(5) 0.00010(6) Si1 0.0212(5) 0.0156(4) 0.0224(5) -0.0058(4) -0.0028(4) 0.0002(4) O1 0.0238(12) 0.0151(11) 0.0198(11) -0.0047(9) -0.0085(9) 0.0000(9) N1 0.0159(13) 0.0188(14) 0.0176(13) -0.0033(11) -0.0047(11) 0.0006(11) Yb2 0.01411(7) 0.01549(7) 0.01786(7) -0.00311(6) -0.00178(5) -0.00134(5) Si2 0.0170(5) 0.0206(5) 0.0261(5) -0.0103(4) -0.0013(4) 0.0017(4) O2 0.0195(11) 0.0223(12) 0.0159(11) -0.0083(9) -0.0034(9) 0.0034(9) N2 0.0176(14) 0.0160(13) 0.0203(13) -0.0077(11) -0.0056(11) 0.0016(11) O3 0.0270(13) 0.0156(11) 0.0204(11) -0.0001(9) -0.0011(10) -0.0017(10) Si4 0.0233(5) 0.0133(4) 0.0253(5) -0.0043(4) -0.0067(4) 0.0015(4) O4 0.0215(12) 0.0118(11) 0.0230(11) -0.0042(9) 0.0020(9) -0.0028(9) N4 0.0173(13) 0.0144(13) 0.0199(13) -0.0016(11) -0.0016(11) -0.0008(11) Si5 0.0205(5) 0.0179(4) 0.0194(4) -0.0016(4) -0.0040(4) 0.0020(4) O5 0.0169(11) 0.0206(12) 0.0210(11) 0.0040(9) -0.0037(9) -0.0041(9) N5 0.0163(13) 0.0196(14) 0.0190(13) -0.0021(11) -0.0014(11) 0.0016(11) O6 0.0195(12) 0.0243(12) 0.0230(12) -0.0043(10) -0.0098(9) 0.0016(10) C11 0.0157(16) 0.0215(17) 0.0153(15) -0.0034(13) 0.0016(13) -0.0019(13) C12 0.0162(16) 0.0227(17) 0.0123(15) 0.0000(13) -0.0011(12) -0.0014(13) C13 0.0261(18) 0.0247(18) 0.0194(16) -0.0063(14) -0.0053(14) -0.0021(15) C14 0.0245(18) 0.039(2) 0.0203(17) -0.0058(16) -0.0117(14) -0.0011(16) C15 0.0256(19) 0.033(2) 0.0248(18) 0.0010(16) -0.0095(15) 0.0070(16) C16 0.0246(18) 0.0211(17) 0.0228(17) -0.0023(14) -0.0050(14) 0.0032(14) C17 0.034(2) 0.028(2) 0.0306(19) -0.0046(16) -0.0014(16) -0.0056(16) C18 0.042(2) 0.031(2) 0.037(2) -0.0153(17) -0.0073(18) 0.0079(18) C19 0.0291(19) 0.0228(18) 0.0319(19) -0.0088(15) -0.0072(16) -0.0030(15) C21 0.0220(17) 0.0084(14) 0.0261(17) -0.0037(13) -0.0076(14) -0.0021(13) C22 0.0212(17) 0.0154(16) 0.0217(16) -0.0028(13) -0.0090(14) -0.0025(13) C23 0.0303(19) 0.0263(18) 0.0201(17) -0.0058(14) -0.0055(15) -0.0062(16) C24 0.039(2) 0.0232(18) 0.0244(18) 0.0010(15) -0.0184(16) -0.0048(16) C25 0.031(2) 0.0188(18) 0.042(2) 0.0004(16) -0.0226(17) 0.0006(15) C26 0.0251(18) 0.0167(16) 0.0333(19) -0.0045(14) -0.0102(15) 0.0001(14) C27 0.0220(18) 0.031(2) 0.040(2) -0.0088(17) -0.0027(16) -0.0006(16) C28 0.034(2) 0.029(2) 0.047(2) -0.0196(18) 0.0051(18) 0.0015(17) C29 0.0250(19) 0.040(2) 0.0247(18) -0.0127(16) 0.0018(15) -0.0036(16) C31 0.0245(17) 0.0150(16) 0.0144(15) -0.0031(13) -0.0003(13) -0.0045(13) C32 0.0259(18) 0.0174(16) 0.0187(16) -0.0016(13) -0.0065(14) -0.0009(14) C33 0.034(2) 0.0154(17) 0.0313(19) 0.0023(14) -0.0115(16) -0.0030(15) C34 0.030(2) 0.0262(19) 0.039(2) 0.0005(16) -0.0100(17) -0.0078(16) C35 0.0223(18) 0.0304(19) 0.0233(17) -0.0002(15) -0.0059(14) -0.0004(15) C36 0.0257(18) 0.0204(17) 0.0142(15) -0.0048(13) -0.0022(13) 0.0005(14) C41 0.0198(16) 0.0164(16) 0.0171(15) -0.0042(13) -0.0080(13) 0.0028(13) C42 0.0168(16) 0.0206(17) 0.0165(15) -0.0048(13) -0.0026(13) 0.0028(13) C43 0.0233(18) 0.0200(17) 0.0202(16) -0.0010(14) -0.0039(14) -0.0026(14) C44 0.0209(18) 0.032(2) 0.0217(17) -0.0003(15) -0.0009(14) -0.0059(15) C45 0.0166(17) 0.037(2) 0.0295(19) -0.0095(16) 0.0003(15) 0.0046(15) C46 0.0221(18) 0.0213(17) 0.0316(19) -0.0089(15) -0.0054(15) 0.0041(14) C47 0.037(2) 0.0188(18) 0.055(2) -0.0015(17) -0.0145(19) 0.0051(16) C48 0.0260(19) 0.031(2) 0.035(2) -0.0181(16) -0.0040(16) 0.0014(16) C49 0.0312(19) 0.0189(17) 0.0196(16) -0.0040(13) -0.0059(14) -0.0038(15) C51 0.0182(16) 0.0181(16) 0.0193(16) -0.0070(13) -0.0023(13) -0.0044(13) C52 0.0163(16) 0.0239(17) 0.0185(16) -0.0057(14) -0.0041(13) -0.0042(14) C53 0.028(2) 0.032(2) 0.0240(18) -0.0009(16) -0.0009(15) -0.0060(16) C54 0.0235(19) 0.040(2) 0.032(2) -0.0050(18) 0.0116(16) -0.0048(17) C55 0.0189(18) 0.035(2) 0.036(2) -0.0075(17) 0.0038(16) -0.0008(16) C56 0.0223(18) 0.0279(19) 0.0268(18) -0.0031(15) -0.0033(15) 0.0011(15) C57 0.0304(19) 0.0188(17) 0.0197(16) -0.0022(14) -0.0035(14) 0.0001(15) C58 0.033(2) 0.024(2) 0.052(2) 0.0034(18) 0.0062(19) 0.0071(17) C59 0.031(2) 0.061(3) 0.035(2) -0.018(2) -0.0091(17) 0.001(2) C61 0.0186(16) 0.0136(15) 0.0194(16) 0.0039(13) -0.0030(13) -0.0054(13) C62 0.0197(17) 0.0149(16) 0.0261(18) 0.0035(14) -0.0009(14) -0.0015(13) C63 0.0278(19) 0.032(2) 0.0224(18) -0.0028(15) 0.0045(15) 0.0025(16) C64 0.035(2) 0.052(2) 0.0158(17) -0.0037(17) -0.0020(16) 0.0052(19) C65 0.0231(18) 0.033(2) 0.0189(17) 0.0022(15) -0.0060(14) 0.0042(15) C66 0.0185(16) 0.0164(16) 0.0177(16) 0.0017(13) 0.0000(13) -0.0026(13) C111 0.0274(18) 0.0190(17) 0.0236(17) -0.0091(14) -0.0145(15) 0.0028(14) C112 0.026(2) 0.046(2) 0.046(2) -0.0282(19) -0.0106(17) 0.0044(18) C113 0.043(3) 0.060(3) 0.089(3) -0.059(3) -0.033(2) 0.025(2) C114 0.063(3) 0.026(2) 0.097(4) -0.036(2) -0.053(3) 0.020(2) C115 0.056(3) 0.024(2) 0.054(3) -0.0023(19) -0.032(2) -0.008(2) C116 0.035(2) 0.0232(18) 0.0295(19) -0.0070(15) -0.0128(16) -0.0018(16) C211 0.0279(18) 0.0218(17) 0.0146(16) -0.0070(13) -0.0028(14) 0.0038(15) C212 0.034(2) 0.0266(19) 0.0222(17) -0.0093(15) -0.0024(15) 0.0013(16) C213 0.036(2) 0.041(2) 0.0217(18) -0.0088(16) 0.0017(16) 0.0018(18) C214 0.047(2) 0.039(2) 0.0211(18) -0.0102(17) -0.0012(17) 0.0202(19) C215 0.070(3) 0.024(2) 0.035(2) -0.0147(17) 0.006(2) -0.002(2) C216 0.044(2) 0.029(2) 0.030(2) -0.0125(16) 0.0100(17) -0.0062(18) C321 0.0262(18) 0.0175(17) 0.0250(17) -0.0010(14) -0.0070(15) 0.0010(14) C322 0.037(2) 0.0232(19) 0.042(2) 0.0011(17) -0.0124(18) 0.0046(17) C323 0.0300(19) 0.0264(19) 0.0260(18) -0.0002(15) -0.0089(15) -0.0042(16) C324 0.032(2) 0.0257(19) 0.0290(19) -0.0033(15) -0.0064(16) 0.0098(16) C361 0.0225(18) 0.0232(18) 0.0250(18) -0.0030(15) 0.0024(14) 0.0046(14) C362 0.042(2) 0.033(2) 0.057(3) -0.022(2) -0.018(2) 0.0095(19) C363 0.027(2) 0.035(2) 0.032(2) -0.0042(17) -0.0010(16) 0.0057(16) C364 0.030(2) 0.032(2) 0.035(2) 0.0049(17) -0.0014(17) 0.0053(17) C411 0.0168(16) 0.0151(16) 0.0195(16) -0.0043(13) 0.0034(13) -0.0022(13) C412 0.0192(17) 0.0237(17) 0.0169(16) -0.0052(14) 0.0018(13) -0.0024(14) C413 0.0236(18) 0.0187(17) 0.0259(18) -0.0016(14) 0.0009(15) 0.0002(14) C414 0.031(2) 0.0147(17) 0.036(2) -0.0070(15) 0.0060(16) -0.0012(15) C415 0.031(2) 0.0231(18) 0.034(2) -0.0129(16) -0.0052(16) -0.0066(16) C416 0.0287(19) 0.0232(18) 0.0222(17) -0.0041(14) -0.0034(15) -0.0001(15) C511 0.0216(17) 0.0179(16) 0.0140(15) 0.0011(13) 0.0001(13) -0.0021(14) C512 0.0193(17) 0.0257(18) 0.0229(17) -0.0007(14) -0.0014(14) -0.0047(14) C513 0.0234(19) 0.037(2) 0.0307(19) 0.0057(17) -0.0084(16) 0.0024(17) C514 0.034(2) 0.0200(18) 0.034(2) 0.0017(16) 0.0072(17) 0.0074(16) C515 0.048(2) 0.0207(18) 0.0235(18) -0.0061(15) 0.0086(17) -0.0070(17) C516 0.034(2) 0.0272(19) 0.0172(16) -0.0041(14) -0.0025(15) -0.0089(16) C621 0.0197(17) 0.0220(17) 0.0308(18) -0.0075(15) -0.0007(15) 0.0024(14) C622 0.159(7) 0.064(4) 0.257(9) -0.104(5) -0.172(7) 0.075(4) C623 0.026(2) 0.110(5) 0.103(4) 0.037(4) 0.000(3) 0.004(3) C624 0.045(3) 0.081(4) 0.047(3) -0.004(2) -0.004(2) 0.033(3) C661 0.0181(16) 0.0220(17) 0.0182(16) -0.0005(13) -0.0024(13) 0.0000(14) C662 0.0255(18) 0.0310(19) 0.0208(17) -0.0039(15) 0.0013(15) -0.0025(16) C663 0.0177(17) 0.041(2) 0.0286(19) -0.0063(16) -0.0040(15) 0.0025(16) C664 0.0212(18) 0.0273(19) 0.043(2) -0.0109(17) -0.0033(16) 0.0033(15) _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 Yb1 O3 2.068(2) . ? Yb1 N1 2.208(2) . ? Yb1 N2 2.215(3) . ? Yb1 O2 2.363(2) . ? Yb1 O1 2.373(2) . ? Yb1 C21 3.057(3) . ? Yb1 C11 3.071(3) . ? Yb1 C22 3.170(3) . ? Yb1 C12 3.193(3) . ? Yb1 Si2 3.5285(13) . ? Yb1 Si1 3.5323(14) . ? Si1 N1 1.744(3) . ? Si1 C18 1.864(4) . ? Si1 C19 1.869(3) . ? Si1 C17 1.874(3) . ? O1 C111 1.427(4) . ? O1 C12 1.430(4) . ? N1 C11 1.401(4) . ? Yb2 O6 2.053(2) . ? Yb2 N4 2.198(3) . ? Yb2 N5 2.225(3) . ? Yb2 O5 2.368(2) . ? Yb2 O4 2.368(2) . ? Yb2 C41 3.047(3) . ? Yb2 C51 3.072(3) . ? Yb2 C42 3.177(3) . ? Yb2 C52 3.189(3) . ? Yb2 Si4 3.5162(13) . ? Yb2 Si5 3.5245(14) . ? Si2 N2 1.741(3) . ? Si2 C28 1.866(4) . ? Si2 C29 1.875(3) . ? Si2 C27 1.877(3) . ? O2 C211 1.421(4) . ? O2 C22 1.426(4) . ? N2 C21 1.399(4) . ? O3 C31 1.357(3) . ? Si4 N4 1.738(3) . ? Si4 C49 1.868(3) . ? Si4 C47 1.873(3) . ? Si4 C48 1.877(3) . ? O4 C411 1.424(3) . ? O4 C42 1.428(4) . ? N4 C41 1.396(4) . ? Si5 N5 1.736(3) . ? Si5 C58 1.863(4) . ? Si5 C59 1.869(4) . ? Si5 C57 1.870(3) . ? O5 C511 1.412(4) . ? O5 C52 1.428(4) . ? N5 C51 1.397(4) . ? O6 C61 1.353(4) . ? C11 C16 1.402(4) . ? C11 C12 1.409(4) . ? C12 C13 1.369(4) . ? C13 C14 1.389(5) . ? C14 C15 1.372(5) . ? C15 C16 1.384(5) . ? C21 C26 1.406(4) . ? C21 C22 1.410(4) . ? C22 C23 1.381(4) . ? C23 C24 1.376(5) . ? C24 C25 1.372(5) . ? C25 C26 1.394(5) . ? C31 C36 1.423(4) . ? C31 C32 1.428(4) . ? C32 C33 1.386(4) . ? C32 C321 1.545(5) . ? C33 C34 1.381(5) . ? C34 C35 1.373(5) . ? C35 C36 1.395(4) . ? C36 C361 1.550(4) . ? C41 C46 1.405(4) . ? C41 C42 1.412(4) . ? C42 C43 1.378(4) . ? C43 C44 1.389(5) . ? C44 C45 1.390(5) . ? C45 C46 1.382(4) . ? C51 C52 1.402(4) . ? C51 C56 1.405(4) . ? C52 C53 1.375(4) . ? C53 C54 1.383(5) . ? C54 C55 1.373(5) . ? C55 C56 1.389(5) . ? C61 C62 1.416(4) . ? C61 C66 1.425(4) . ? C62 C63 1.395(5) . ? C62 C621 1.549(4) . ? C63 C64 1.368(5) . ? C64 C65 1.385(5) . ? C65 C66 1.393(4) . ? C66 C661 1.549(4) . ? C111 C116 1.370(5) . ? C111 C112 1.371(5) . ? C112 C113 1.400(5) . ? C113 C114 1.368(6) . ? C114 C115 1.373(6) . ? C115 C116 1.385(5) . ? C211 C212 1.361(5) . ? C211 C216 1.373(5) . ? C212 C213 1.387(5) . ? C213 C214 1.374(5) . ? C214 C215 1.368(5) . ? C215 C216 1.387(5) . ? C321 C323 1.538(5) . ? C321 C324 1.540(4) . ? C321 C322 1.544(4) . ? C361 C364 1.521(4) . ? C361 C362 1.522(5) . ? C361 C363 1.547(5) . ? C411 C416 1.373(4) . ? C411 C412 1.378(4) . ? C412 C413 1.392(4) . ? C413 C414 1.373(5) . ? C414 C415 1.380(5) . ? C415 C416 1.389(5) . ? C511 C512 1.369(4) . ? C511 C516 1.391(4) . ? C512 C513 1.397(5) . ? C513 C514 1.382(5) . ? C514 C515 1.370(5) . ? C515 C516 1.381(5) . ? C621 C622 1.503(6) . ? C621 C623 1.510(5) . ? C621 C624 1.542(5) . ? C661 C662 1.534(4) . ? C661 C663 1.538(4) . ? C661 C664 1.538(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Yb1 N1 124.14(9) . . ? O3 Yb1 N2 124.22(9) . . ? N1 Yb1 N2 111.62(9) . . ? O3 Yb1 O2 90.49(8) . . ? N1 Yb1 O2 109.05(8) . . ? N2 Yb1 O2 71.51(8) . . ? O3 Yb1 O1 89.61(8) . . ? N1 Yb1 O1 71.97(8) . . ? N2 Yb1 O1 107.35(8) . . ? O2 Yb1 O1 178.66(7) . . ? O3 Yb1 C21 106.88(8) . . ? N1 Yb1 C21 126.07(9) . . ? N2 Yb1 C21 24.78(8) . . ? O2 Yb1 C21 50.05(8) . . ? O1 Yb1 C21 128.67(8) . . ? O3 Yb1 C11 108.02(8) . . ? N1 Yb1 C11 24.46(8) . . ? N2 Yb1 C11 123.71(9) . . ? O2 Yb1 C11 131.33(8) . . ? O1 Yb1 C11 49.85(8) . . ? C21 Yb1 C11 145.04(8) . . ? O3 Yb1 C22 94.73(8) . . ? N1 Yb1 C22 124.57(9) . . ? N2 Yb1 C22 49.78(9) . . ? O2 Yb1 C22 24.81(8) . . ? O1 Yb1 C22 153.85(8) . . ? C21 Yb1 C22 26.10(8) . . ? C11 Yb1 C22 149.02(8) . . ? O3 Yb1 C12 95.60(8) . . ? N1 Yb1 C12 49.57(9) . . ? N2 Yb1 C12 121.61(8) . . ? O2 Yb1 C12 156.70(8) . . ? O1 Yb1 C12 24.57(7) . . ? C21 Yb1 C12 146.21(8) . . ? C11 Yb1 C12 25.89(8) . . ? C22 Yb1 C12 169.49(8) . . ? O3 Yb1 Si2 135.40(6) . . ? N1 Yb1 Si2 96.32(7) . . ? N2 Yb1 Si2 23.59(6) . . ? O2 Yb1 Si2 93.23(6) . . ? O1 Yb1 Si2 85.76(6) . . ? C21 Yb1 Si2 48.36(6) . . ? C11 Yb1 Si2 102.43(6) . . ? C22 Yb1 Si2 73.09(6) . . ? C12 Yb1 Si2 98.03(6) . . ? O3 Yb1 Si1 136.15(6) . . ? N1 Yb1 Si1 23.44(7) . . ? N2 Yb1 Si1 96.48(7) . . ? O2 Yb1 Si1 87.57(6) . . ? O1 Yb1 Si1 93.29(5) . . ? C21 Yb1 Si1 105.06(6) . . ? C11 Yb1 Si1 47.88(6) . . ? C22 Yb1 Si1 101.15(6) . . ? C12 Yb1 Si1 72.49(6) . . ? Si2 Yb1 Si1 88.44(4) . . ? N1 Si1 C18 112.27(15) . . ? N1 Si1 C19 108.52(14) . . ? C18 Si1 C19 106.01(16) . . ? N1 Si1 C17 111.35(14) . . ? C18 Si1 C17 110.62(17) . . ? C19 Si1 C17 107.81(16) . . ? N1 Si1 Yb1 30.24(8) . . ? C18 Si1 Yb1 112.98(12) . . ? C19 Si1 Yb1 79.81(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C12 C21 C22 54.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.179 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.106 #===END data_compound2 _database_code_CSD 207492 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichlorobis(methylcyclopentadienyl)bis(N-(2-methoxyphenyl)-N-trimethy lsilylamido)diytterbium(III)] ; _chemical_name_common ybcacl _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H23 Cl N O Si Yb' _chemical_formula_weight 481.93 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5538(1) _cell_length_b 9.7537(2) _cell_length_c 12.0433(2) _cell_angle_alpha 76.953(1) _cell_angle_beta 78.027(1) _cell_angle_gamma 64.868(1) _cell_volume 879.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8975 _cell_measurement_theta_min 3.50 _cell_measurement_theta_max 28.28 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 470 _exptl_absorpt_coefficient_mu 5.537 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.380 _exptl_absorpt_correction_T_max 0.740 _exptl_absorpt_process_details Face-indexed/Gaussian _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8975 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4293 _reflns_number_gt 3834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0343P)^2^+0.3207P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4293 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.88531(2) 0.960347(18) 0.663009(13) 0.01212(7) Uani 1 1 d . . . Cl1 Cl 1.19604(13) 0.87281(12) 0.53979(8) 0.0169(2) Uani 1 1 d . . . Si1 Si 0.59987(15) 1.31326(13) 0.74243(9) 0.0149(2) Uani 1 1 d . . . O1 O 1.0683(4) 0.9002(3) 0.8020(2) 0.0166(6) Uani 1 1 d . . . N1 N 0.8028(5) 1.1620(4) 0.7489(3) 0.0140(7) Uani 1 1 d . . . C1 C 0.8235(6) 0.7509(5) 0.5956(4) 0.0192(9) Uani 1 1 d . . . C2 C 0.6642(6) 0.8521(5) 0.6460(4) 0.0220(9) Uani 1 1 d . . . H2 H 0.5674 0.9200 0.6068 0.026 Uiso 1 1 calc R . . C3 C 0.6721(6) 0.8358(5) 0.7641(4) 0.0222(9) Uani 1 1 d . . . H3 H 0.5820 0.8907 0.8180 0.027 Uiso 1 1 calc R . . C4 C 0.8365(6) 0.7242(5) 0.7883(4) 0.0215(9) Uani 1 1 d . . . H4 H 0.8769 0.6896 0.8615 0.026 Uiso 1 1 calc R . . C5 C 0.9312(6) 0.6725(5) 0.6837(4) 0.0204(9) Uani 1 1 d . . . H5 H 1.0471 0.5980 0.6744 0.024 Uiso 1 1 calc R . . C6 C 0.8734(7) 0.7268(6) 0.4716(4) 0.0243(10) Uani 1 1 d . . . H6A H 0.9929 0.6500 0.4612 0.036 Uiso 1 1 calc R . . H6B H 0.8657 0.8237 0.4224 0.036 Uiso 1 1 calc R . . H6C H 0.7940 0.6909 0.4506 0.036 Uiso 1 1 calc R . . C10 C 1.2126(6) 0.7550(5) 0.8264(4) 0.0227(10) Uani 1 1 d . . . H10A H 1.1998 0.6762 0.7954 0.034 Uiso 1 1 calc R . . H10B H 1.2137 0.7258 0.9097 0.034 Uiso 1 1 calc R . . H10C H 1.3220 0.7647 0.7907 0.034 Uiso 1 1 calc R . . C11 C 0.9254(5) 1.1637(5) 0.8085(3) 0.0140(8) Uani 1 1 d . . . C12 C 1.0657(6) 1.0268(5) 0.8398(3) 0.0150(8) Uani 1 1 d . . . C13 C 1.1885(6) 1.0155(5) 0.9041(3) 0.0191(9) Uani 1 1 d . . . H13 H 1.2781 0.9191 0.9261 0.023 Uiso 1 1 calc R . . C14 C 1.1785(6) 1.1474(6) 0.9359(4) 0.0230(10) Uani 1 1 d . . . H14 H 1.2615 1.1422 0.9800 0.028 Uiso 1 1 calc R . . C15 C 1.0470(6) 1.2865(6) 0.9029(4) 0.0227(10) Uani 1 1 d . . . H15 H 1.0410 1.3773 0.9235 0.027 Uiso 1 1 calc R . . C16 C 0.9240(6) 1.2949(5) 0.8402(4) 0.0193(9) Uani 1 1 d . . . H16 H 0.8357 1.3921 0.8178 0.023 Uiso 1 1 calc R . . C17 C 0.6061(6) 1.4891(5) 0.6428(4) 0.0239(10) Uani 1 1 d . . . H17A H 0.6824 1.5246 0.6681 0.036 Uiso 1 1 calc R . . H17B H 0.4883 1.5698 0.6435 0.036 Uiso 1 1 calc R . . H17C H 0.6508 1.4649 0.5647 0.036 Uiso 1 1 calc R . . C18 C 0.4538(6) 1.2534(5) 0.6871(4) 0.0211(9) Uani 1 1 d . . . H18A H 0.4466 1.1610 0.7367 0.032 Uiso 1 1 calc R . . H18B H 0.5008 1.2316 0.6087 0.032 Uiso 1 1 calc R . . H18C H 0.3373 1.3360 0.6871 0.032 Uiso 1 1 calc R . . C19 C 0.4954(6) 1.3605(6) 0.8909(4) 0.0261(10) Uani 1 1 d . . . H19A H 0.4934 1.2675 0.9420 0.039 Uiso 1 1 calc R . . H19B H 0.3760 1.4373 0.8870 0.039 Uiso 1 1 calc R . . H19C H 0.5625 1.4013 0.9206 0.039 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 Yb1 0.01244(10) 0.01116(10) 0.01130(9) -0.00152(6) -0.00130(6) -0.00352(7) Cl1 0.0118(5) 0.0186(5) 0.0136(4) 0.0000(4) -0.0010(4) -0.0012(4) Si1 0.0125(6) 0.0129(6) 0.0162(5) -0.0028(4) -0.0028(4) -0.0014(4) O1 0.0157(15) 0.0141(15) 0.0159(14) -0.0024(11) -0.0044(12) -0.0010(12) N1 0.0136(18) 0.0141(17) 0.0141(16) -0.0007(13) -0.0052(14) -0.0044(14) C1 0.027(2) 0.016(2) 0.021(2) -0.0040(17) -0.0046(19) -0.0128(19) C2 0.019(2) 0.022(2) 0.028(2) -0.0018(19) -0.0013(19) -0.0126(19) C3 0.020(2) 0.021(2) 0.025(2) -0.0058(18) 0.0072(18) -0.0110(19) C4 0.030(3) 0.017(2) 0.018(2) 0.0004(17) 0.0024(19) -0.014(2) C5 0.023(2) 0.018(2) 0.022(2) -0.0028(17) -0.0035(19) -0.0102(19) C6 0.033(3) 0.025(3) 0.021(2) -0.0057(19) -0.005(2) -0.015(2) C10 0.022(2) 0.017(2) 0.022(2) 0.0010(18) -0.0078(19) -0.0010(19) C11 0.015(2) 0.017(2) 0.0090(17) -0.0012(15) 0.0004(15) -0.0066(17) C12 0.016(2) 0.017(2) 0.0092(17) -0.0027(15) 0.0024(15) -0.0054(17) C13 0.015(2) 0.025(2) 0.0122(19) -0.0015(17) -0.0012(16) -0.0041(18) C14 0.018(2) 0.037(3) 0.018(2) -0.0063(19) -0.0033(18) -0.013(2) C15 0.028(3) 0.025(2) 0.019(2) -0.0073(18) -0.0036(19) -0.013(2) C16 0.018(2) 0.017(2) 0.018(2) -0.0012(17) 0.0008(17) -0.0052(18) C17 0.026(3) 0.017(2) 0.028(2) 0.0031(18) -0.007(2) -0.009(2) C18 0.013(2) 0.025(2) 0.020(2) -0.0042(18) 0.0000(17) -0.0038(19) C19 0.023(3) 0.025(3) 0.024(2) -0.0089(19) -0.004(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N1 2.207(3) . ? Yb1 O1 2.337(3) . ? Yb1 C3 2.564(5) . ? Yb1 C2 2.587(4) . ? Yb1 C4 2.597(4) . ? Yb1 C5 2.624(4) . ? Yb1 C1 2.637(4) . ? Yb1 Cl1 2.6464(14) . ? Yb1 Cl1 2.6545(13) 2_776 ? Yb1 C11 3.085(4) . ? Yb1 C12 3.189(4) . ? Yb1 Si1 3.4791(18) . ? Cl1 Yb1 2.6545(13) 2_776 ? Si1 N1 1.740(4) . ? Si1 C18 1.867(4) . ? Si1 C17 1.872(5) . ? Si1 C19 1.888(5) . ? O1 C12 1.400(5) . ? O1 C10 1.446(5) . ? N1 C11 1.396(5) . ? C1 C2 1.408(7) . ? C1 C5 1.414(6) . ? C1 C6 1.510(6) . ? C2 C3 1.407(6) . ? C3 C4 1.405(7) . ? C4 C5 1.419(6) . ? C11 C12 1.402(6) . ? C11 C16 1.410(6) . ? C12 C13 1.384(6) . ? C13 C14 1.387(7) . ? C14 C15 1.382(7) . ? C15 C16 1.383(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 N1 Yb1 O1 71.30(11) . . ? N1 Yb1 C3 103.44(14) . . ? O1 Yb1 C3 102.68(13) . . ? N1 Yb1 C2 120.89(14) . . ? O1 Yb1 C2 131.56(13) . . ? C3 Yb1 C2 31.71(14) . . ? N1 Yb1 C4 115.98(13) . . ? O1 Yb1 C4 79.83(13) . . ? C3 Yb1 C4 31.58(15) . . ? C2 Yb1 C4 52.13(15) . . ? N1 Yb1 C5 147.19(13) . . ? O1 Yb1 C5 91.52(12) . . ? C3 Yb1 C5 52.08(15) . . ? C2 Yb1 C5 51.70(15) . . ? C4 Yb1 C5 31.54(13) . . ? N1 Yb1 C1 152.11(14) . . ? O1 Yb1 C1 122.65(12) . . ? C3 Yb1 C1 52.16(14) . . ? C2 Yb1 C1 31.26(15) . . ? C4 Yb1 C1 52.05(13) . . ? C5 Yb1 C1 31.17(14) . . ? N1 Yb1 Cl1 117.35(10) . . ? O1 Yb1 Cl1 78.22(8) . . ? C3 Yb1 Cl1 136.48(11) . . ? C2 Yb1 Cl1 120.42(11) . . ? C4 Yb1 Cl1 110.36(11) . . ? C5 Yb1 Cl1 84.48(11) . . ? C1 Yb1 Cl1 90.13(11) . . ? N1 Yb1 Cl1 93.92(9) . 2_776 ? O1 Yb1 Cl1 143.31(8) . 2_776 ? C3 Yb1 Cl1 113.52(11) . 2_776 ? C2 Yb1 Cl1 85.00(11) . 2_776 ? C4 Yb1 Cl1 135.70(11) . 2_776 ? C5 Yb1 Cl1 115.00(10) . 2_776 ? C1 Yb1 Cl1 86.09(10) . 2_776 ? Cl1 Yb1 Cl1 79.60(5) . 2_776 ? N1 Yb1 C11 23.99(12) . . ? O1 Yb1 C11 48.85(11) . . ? C3 Yb1 C11 113.28(12) . . ? C2 Yb1 C11 139.42(13) . . ? C4 Yb1 C11 112.26(12) . . ? C5 Yb1 C11 136.93(12) . . ? C1 Yb1 C11 163.95(12) . . ? Cl1 Yb1 C11 99.94(8) . . ? Cl1 Yb1 C11 107.89(8) 2_776 . ? N1 Yb1 C12 49.20(12) . . ? O1 Yb1 C12 23.47(10) . . ? C3 Yb1 C12 112.50(13) . . ? C2 Yb1 C12 144.21(13) . . ? C4 Yb1 C12 97.89(13) . . ? C5 Yb1 C12 114.54(12) . . ? C1 Yb1 C12 145.68(12) . . ? Cl1 Yb1 C12 85.71(8) . . ? Cl1 Yb1 C12 126.27(8) 2_776 . ? C11 Yb1 C12 25.75(11) . . ? N1 Yb1 Si1 24.73(9) . . ? O1 Yb1 Si1 94.99(8) . . ? C3 Yb1 Si1 91.71(11) . . ? C2 Yb1 Si1 99.86(11) . . ? C4 Yb1 Si1 115.29(11) . . ? C5 Yb1 Si1 143.71(11) . . ? C1 Yb1 Si1 130.32(11) . . ? Cl1 Yb1 Si1 131.79(4) . . ? Cl1 Yb1 Si1 78.68(4) 2_776 . ? C11 Yb1 Si1 48.72(8) . . ? C12 Yb1 Si1 73.74(8) . . ? Yb1 Cl1 Yb1 100.40(5) . 2_776 ? N1 Si1 C18 108.95(19) . . ? N1 Si1 C17 113.6(2) . . ? C18 Si1 C17 106.4(2) . . ? N1 Si1 C19 110.50(19) . . ? C18 Si1 C19 106.7(2) . . ? C17 Si1 C19 110.4(2) . . ? N1 Si1 Yb1 32.06(11) . . ? C18 Si1 Yb1 77.80(14) . . ? C17 Si1 Yb1 117.24(16) . . ? C19 Si1 Yb1 128.61(16) . . ? C12 O1 C10 117.4(3) . . ? C12 O1 Yb1 114.8(2) . . ? C10 O1 Yb1 125.3(2) . . ? C11 N1 Si1 120.8(3) . . ? C11 N1 Yb1 116.0(3) . . ? Si1 N1 Yb1 123.21(17) . . ? C2 C1 C5 107.2(4) . . ? C2 C1 C6 127.5(4) . . ? C5 C1 C6 125.3(4) . . ? C2 C1 Yb1 72.4(2) . . ? C5 C1 Yb1 73.9(2) . . ? C6 C1 Yb1 119.7(3) . . ? C3 C2 C1 108.7(4) . . ? C3 C2 Yb1 73.3(2) . . ? C1 C2 Yb1 76.4(2) . . ? C4 C3 C2 108.2(4) . . ? C4 C3 Yb1 75.5(3) . . ? C2 C3 Yb1 75.0(3) . . ? C3 C4 C5 107.6(4) . . ? C3 C4 Yb1 72.9(3) . . ? C5 C4 Yb1 75.3(3) . . ? C1 C5 C4 108.3(4) . . ? C1 C5 Yb1 74.9(2) . . ? C4 C5 Yb1 73.2(2) . . ? N1 C11 C12 119.6(4) . . ? N1 C11 C16 125.5(4) . . ? C12 C11 C16 114.9(4) . . ? N1 C11 Yb1 40.02(18) . . ? C12 C11 Yb1 81.3(2) . . ? C16 C11 Yb1 159.7(3) . . ? C13 C12 O1 122.6(4) . . ? C13 C12 C11 123.8(4) . . ? O1 C12 C11 113.5(4) . . ? C13 C12 Yb1 161.6(3) . . ? O1 C12 Yb1 41.68(17) . . ? C11 C12 Yb1 73.0(2) . . ? C12 C13 C14 118.9(4) . . ? C15 C14 C13 119.6(4) . . ? C14 C15 C16 120.6(4) . . ? C15 C16 C11 122.1(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 O1 C12 C13 -3.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.741 _refine_diff_density_min -2.261 _refine_diff_density_rms 0.184 #===END data_compound3 _database_code_CSD 207493 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichlorobis(methylcyclopentadienyl)bis(N-(2-phenoxyphenyl)-N-trimethy lsilylamido)diytterbium(III) ; _chemical_name_common ybcph _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H25 Cl N O Si Yb' _chemical_formula_weight 544.00 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6568(1) _cell_length_b 8.7267(1) _cell_length_c 25.3241(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.9972(4) _cell_angle_gamma 90.00 _cell_volume 2107.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 20656 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 28.31 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 4.630 _exptl_absorpt_correction_type empirical/multiscan _exptl_absorpt_correction_T_min 0.458 _exptl_absorpt_correction_T_max 0.518 _exptl_absorpt_process_details 'SORTAV (R. Blessing 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20656 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 28.31 _reflns_number_total 5202 _reflns_number_gt 4876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0159P)^2^+3.8701P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5202 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0511 _refine_ls_wR_factor_gt 0.0501 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.478919(10) 0.091582(12) 0.072751(4) 0.00992(4) Uani 1 1 d . . . Cl1 Cl 0.46816(6) -0.17459(7) 0.02261(2) 0.01460(12) Uani 1 1 d . . . Si1 Si 0.77283(7) 0.33025(8) 0.09954(3) 0.01429(14) Uani 1 1 d . . . O1 O 0.54299(18) -0.0719(2) 0.14669(7) 0.0142(4) Uani 1 1 d . . . N1 N 0.6906(2) 0.1580(3) 0.11188(8) 0.0122(4) Uani 1 1 d . . . C1 C 0.2176(3) 0.1648(3) 0.03553(11) 0.0170(5) Uani 1 1 d . . . C2 C 0.2129(3) 0.0639(3) 0.07878(11) 0.0191(6) Uani 1 1 d . . . H2 H 0.1740 -0.0363 0.0764 0.023 Uiso 1 1 calc R . . C3 C 0.2757(3) 0.1373(4) 0.12636(11) 0.0206(6) Uani 1 1 d . . . H3 H 0.2852 0.0956 0.1614 0.025 Uiso 1 1 calc R . . C4 C 0.3218(3) 0.2826(3) 0.11265(11) 0.0204(6) Uani 1 1 d . . . H4 H 0.3686 0.3563 0.1367 0.024 Uiso 1 1 calc R . . C5 C 0.2859(3) 0.2996(3) 0.05649(11) 0.0180(5) Uani 1 1 d . . . H5 H 0.3047 0.3870 0.0364 0.022 Uiso 1 1 calc R . . C6 C 0.1571(3) 0.1360(4) -0.02214(12) 0.0249(6) Uani 1 1 d . . . H6A H 0.1158 0.0332 -0.0257 0.037 Uiso 1 1 calc R . . H6B H 0.2316 0.1436 -0.0442 0.037 Uiso 1 1 calc R . . H6C H 0.0845 0.2125 -0.0340 0.037 Uiso 1 1 calc R . . C11 C 0.7638(3) 0.0414(3) 0.14190(9) 0.0115(5) Uani 1 1 d . . . C12 C 0.6908(3) -0.0799(3) 0.16188(10) 0.0131(5) Uani 1 1 d . . . C13 C 0.7550(3) -0.1989(3) 0.19247(11) 0.0173(5) Uani 1 1 d . . . H13 H 0.7005 -0.2790 0.2042 0.021 Uiso 1 1 calc R . . C14 C 0.9001(3) -0.1999(3) 0.20574(11) 0.0206(6) Uani 1 1 d . . . H14 H 0.9457 -0.2783 0.2280 0.025 Uiso 1 1 calc R . . C15 C 0.9776(3) -0.0853(3) 0.18619(12) 0.0203(6) Uani 1 1 d . . . H15 H 1.0770 -0.0865 0.1946 0.024 Uiso 1 1 calc R . . C16 C 0.9114(3) 0.0312(3) 0.15448(10) 0.0159(5) Uani 1 1 d . . . H16 H 0.9671 0.1067 0.1408 0.019 Uiso 1 1 calc R . . C17 C 0.6311(3) 0.4759(3) 0.08159(12) 0.0219(6) Uani 1 1 d . . . H17A H 0.5751 0.4837 0.1106 0.033 Uiso 1 1 calc R . . H17B H 0.5706 0.4446 0.0486 0.033 Uiso 1 1 calc R . . H17C H 0.6732 0.5757 0.0762 0.033 Uiso 1 1 calc R . . C18 C 0.8772(3) 0.3192(4) 0.04346(13) 0.0251(6) Uani 1 1 d . . . H18A H 0.8180 0.2797 0.0114 0.038 Uiso 1 1 calc R . . H18B H 0.9573 0.2505 0.0534 0.038 Uiso 1 1 calc R . . H18C H 0.9111 0.4217 0.0361 0.038 Uiso 1 1 calc R . . C19 C 0.8924(3) 0.4070(3) 0.15913(13) 0.0281(7) Uani 1 1 d . . . H19B H 0.8411 0.4150 0.1895 0.042 Uiso 1 1 calc R . . H19A H 0.9263 0.5086 0.1507 0.042 Uiso 1 1 calc R . . H19C H 0.9723 0.3376 0.1683 0.042 Uiso 1 1 calc R . . C111 C 0.4579(3) -0.1620(3) 0.17540(10) 0.0146(5) Uani 1 1 d . . . C112 C 0.4626(3) -0.1400(4) 0.22973(11) 0.0217(6) Uani 1 1 d . . . H112 H 0.5263 -0.0687 0.2486 0.026 Uiso 1 1 calc R . . C113 C 0.3726(3) -0.2239(4) 0.25620(11) 0.0244(6) Uani 1 1 d . . . H113 H 0.3756 -0.2111 0.2936 0.029 Uiso 1 1 calc R . . C114 C 0.2786(3) -0.3262(4) 0.22851(12) 0.0230(6) Uani 1 1 d . . . H114 H 0.2164 -0.3822 0.2469 0.028 Uiso 1 1 calc R . . C115 C 0.2749(3) -0.3473(3) 0.17400(12) 0.0201(6) Uani 1 1 d . . . H115 H 0.2098 -0.4171 0.1550 0.024 Uiso 1 1 calc R . . C116 C 0.3673(3) -0.2657(3) 0.14712(11) 0.0163(5) Uani 1 1 d . . . H116 H 0.3675 -0.2813 0.1100 0.020 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 Yb1 0.00915(6) 0.01195(7) 0.00902(6) 0.00018(4) 0.00255(4) 0.00206(4) Cl1 0.0210(3) 0.0123(3) 0.0114(3) 0.0008(2) 0.0054(2) 0.0013(2) Si1 0.0127(3) 0.0119(4) 0.0184(3) 0.0019(3) 0.0030(3) 0.0003(3) O1 0.0115(8) 0.0170(10) 0.0139(8) 0.0049(7) 0.0017(7) -0.0020(7) N1 0.0124(9) 0.0123(11) 0.0120(10) 0.0000(8) 0.0017(7) 0.0010(8) C1 0.0095(11) 0.0214(15) 0.0203(13) -0.0008(11) 0.0027(9) 0.0050(10) C2 0.0115(11) 0.0212(14) 0.0260(14) 0.0015(11) 0.0077(10) 0.0011(10) C3 0.0173(12) 0.0296(16) 0.0168(13) 0.0020(11) 0.0082(10) 0.0078(11) C4 0.0174(12) 0.0244(15) 0.0197(13) -0.0081(11) 0.0044(10) 0.0061(11) C5 0.0160(12) 0.0164(14) 0.0224(13) -0.0006(11) 0.0060(10) 0.0041(10) C6 0.0163(13) 0.0355(17) 0.0221(14) -0.0043(13) 0.0001(11) 0.0026(12) C11 0.0146(11) 0.0111(12) 0.0093(10) -0.0023(9) 0.0029(8) 0.0023(9) C12 0.0123(11) 0.0156(13) 0.0110(11) -0.0028(9) 0.0010(9) 0.0007(9) C13 0.0214(13) 0.0130(13) 0.0171(12) 0.0025(10) 0.0017(10) 0.0004(10) C14 0.0223(13) 0.0155(14) 0.0220(13) 0.0012(11) -0.0023(10) 0.0059(11) C15 0.0152(12) 0.0204(15) 0.0240(14) -0.0006(11) -0.0014(10) 0.0048(10) C16 0.0138(11) 0.0147(13) 0.0193(12) -0.0010(10) 0.0033(9) 0.0001(10) C17 0.0204(13) 0.0146(14) 0.0314(15) 0.0041(12) 0.0056(11) 0.0037(11) C18 0.0219(14) 0.0250(16) 0.0314(16) 0.0056(12) 0.0134(12) -0.0006(11) C19 0.0292(16) 0.0215(16) 0.0310(17) -0.0009(12) -0.0039(13) -0.0058(12) C111 0.0134(11) 0.0148(13) 0.0169(12) 0.0054(10) 0.0065(9) 0.0011(9) C112 0.0249(14) 0.0266(16) 0.0134(12) 0.0040(11) 0.0024(10) 0.0001(12) C113 0.0263(14) 0.0320(17) 0.0167(13) 0.0090(12) 0.0094(11) 0.0035(13) C114 0.0207(13) 0.0237(16) 0.0271(15) 0.0150(12) 0.0116(11) 0.0068(11) C115 0.0184(12) 0.0143(14) 0.0290(15) 0.0046(11) 0.0076(11) 0.0018(10) C116 0.0165(11) 0.0158(13) 0.0178(12) 0.0012(10) 0.0065(9) 0.0015(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 Yb1 N1 2.205(2) . ? Yb1 O1 2.3586(18) . ? Yb1 C4 2.566(3) . ? Yb1 C3 2.586(3) . ? Yb1 C5 2.588(3) . ? Yb1 C2 2.609(3) . ? Yb1 C1 2.630(3) . ? Yb1 Cl1 2.6414(7) . ? Yb1 Cl1 2.6466(8) 3_655 ? Yb1 C11 3.053(3) . ? Yb1 C12 3.174(3) . ? Yb1 Si1 3.5002(9) . ? Cl1 Yb1 2.6466(8) 3_655 ? Si1 N1 1.751(2) . ? Si1 C18 1.868(3) . ? Si1 C17 1.871(3) . ? Si1 C19 1.875(3) . ? O1 C111 1.417(3) . ? O1 C12 1.420(3) . ? N1 C11 1.395(3) . ? C1 C2 1.411(4) . ? C1 C5 1.412(4) . ? C1 C6 1.507(4) . ? C2 C3 1.414(4) . ? C3 C4 1.406(4) . ? C4 C5 1.418(4) . ? C11 C12 1.409(4) . ? C11 C16 1.414(3) . ? C12 C13 1.383(4) . ? C13 C14 1.389(4) . ? C14 C15 1.386(4) . ? C15 C16 1.388(4) . ? C111 C116 1.379(4) . ? C111 C112 1.383(4) . ? C112 C113 1.387(4) . ? C113 C114 1.383(4) . ? C114 C115 1.388(4) . ? C115 C116 1.399(4) . ? 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 Yb1 O1 72.10(7) . . ? N1 Yb1 C4 102.47(8) . . ? O1 Yb1 C4 100.27(8) . . ? N1 Yb1 C3 116.73(9) . . ? O1 Yb1 C3 78.63(8) . . ? C4 Yb1 C3 31.67(10) . . ? N1 Yb1 C5 118.74(8) . . ? O1 Yb1 C5 130.07(8) . . ? C4 Yb1 C5 31.94(8) . . ? C3 Yb1 C5 52.32(9) . . ? N1 Yb1 C2 148.23(8) . . ? O1 Yb1 C2 92.07(8) . . ? C4 Yb1 C2 52.30(9) . . ? C3 Yb1 C2 31.60(9) . . ? C5 Yb1 C2 51.90(9) . . ? N1 Yb1 C1 150.12(9) . . ? O1 Yb1 C1 123.31(8) . . ? C4 Yb1 C1 52.42(9) . . ? C3 Yb1 C1 52.16(9) . . ? C5 Yb1 C1 31.37(9) . . ? C2 Yb1 C1 31.25(9) . . ? N1 Yb1 Cl1 114.28(6) . . ? O1 Yb1 Cl1 80.52(5) . . ? C4 Yb1 Cl1 141.22(7) . . ? C3 Yb1 Cl1 114.32(7) . . ? C5 Yb1 Cl1 124.55(6) . . ? C2 Yb1 Cl1 88.96(7) . . ? C1 Yb1 Cl1 94.46(6) . . ? N1 Yb1 Cl1 92.32(6) . 3_655 ? O1 Yb1 Cl1 145.69(5) . 3_655 ? C4 Yb1 Cl1 113.08(7) . 3_655 ? C3 Yb1 Cl1 135.04(7) . 3_655 ? C5 Yb1 Cl1 84.25(7) . 3_655 ? C2 Yb1 Cl1 114.28(7) . 3_655 ? C1 Yb1 Cl1 85.29(7) . 3_655 ? Cl1 Yb1 Cl1 78.51(2) . 3_655 ? N1 Yb1 C11 24.64(7) . . ? O1 Yb1 C11 49.97(7) . . ? C4 Yb1 C11 113.75(8) . . ? C3 Yb1 C11 114.25(8) . . ? C5 Yb1 C11 138.92(8) . . ? C2 Yb1 C11 139.52(8) . . ? C1 Yb1 C11 165.53(7) . . ? Cl1 Yb1 C11 96.53(5) . . ? Cl1 Yb1 C11 106.10(5) 3_655 . ? N1 Yb1 C12 49.86(7) . . ? O1 Yb1 C12 24.54(6) . . ? C4 Yb1 C12 112.42(8) . . ? C3 Yb1 C12 99.03(8) . . ? C5 Yb1 C12 144.28(8) . . ? C2 Yb1 C12 116.48(8) . . ? C1 Yb1 C12 147.64(8) . . ? Cl1 Yb1 C12 84.25(5) . . ? Cl1 Yb1 C12 125.66(5) 3_655 . ? C11 Yb1 C12 26.07(7) . . ? N1 Yb1 Si1 24.49(6) . . ? O1 Yb1 Si1 95.86(5) . . ? C4 Yb1 Si1 92.78(7) . . ? C3 Yb1 Si1 117.74(7) . . ? C5 Yb1 Si1 98.93(7) . . ? C2 Yb1 Si1 145.07(7) . . ? C1 Yb1 Si1 128.93(7) . . ? Cl1 Yb1 Si1 125.89(2) . . ? Cl1 Yb1 Si1 75.38(3) 3_655 . ? C11 Yb1 Si1 48.97(5) . . ? C12 Yb1 Si1 74.33(5) . . ? Yb1 Cl1 Yb1 101.49(2) . 3_655 ? N1 Si1 C18 113.91(13) . . ? N1 Si1 C17 106.94(12) . . ? C18 Si1 C17 108.15(14) . . ? N1 Si1 C19 113.74(13) . . ? C18 Si1 C19 107.01(15) . . ? C17 Si1 C19 106.73(14) . . ? N1 Si1 Yb1 31.46(7) . . ? C18 Si1 Yb1 109.86(10) . . ? C17 Si1 Yb1 79.45(10) . . ? C19 Si1 Yb1 138.37(11) . . ? C111 O1 C12 118.20(19) . . ? C111 O1 Yb1 129.91(15) . . ? C12 O1 Yb1 111.86(14) . . ? C11 N1 Si1 121.21(17) . . ? C11 N1 Yb1 114.11(16) . . ? Si1 N1 Yb1 124.05(11) . . ? C2 C1 C5 107.3(2) . . ? C2 C1 C6 126.4(3) . . ? C5 C1 C6 126.2(3) . . ? C2 C1 Yb1 73.53(15) . . ? C5 C1 Yb1 72.66(14) . . ? C6 C1 Yb1 120.79(18) . . ? C1 C2 C3 108.5(3) . . ? C1 C2 Yb1 75.22(15) . . ? C3 C2 Yb1 73.29(15) . . ? C4 C3 C2 107.9(2) . . ? C4 C3 Yb1 73.39(15) . . ? C2 C3 Yb1 75.11(15) . . ? C3 C4 C5 107.7(2) . . ? C3 C4 Yb1 74.94(16) . . ? C5 C4 Yb1 74.90(15) . . ? C1 C5 C4 108.5(3) . . ? C1 C5 Yb1 75.97(15) . . ? C4 C5 Yb1 73.16(15) . . ? N1 C11 C12 120.3(2) . . ? N1 C11 C16 125.2(2) . . ? C12 C11 C16 114.5(2) . . ? N1 C11 Yb1 41.24(11) . . ? C12 C11 Yb1 81.78(14) . . ? C16 C11 Yb1 157.61(18) . . ? C13 C12 C11 124.0(2) . . ? C13 C12 O1 122.1(2) . . ? C11 C12 O1 113.8(2) . . ? C13 C12 Yb1 159.20(18) . . ? C11 C12 Yb1 72.15(14) . . ? O1 C12 Yb1 43.60(10) . . ? C12 C13 C14 119.1(3) . . ? C15 C14 C13 119.4(2) . . ? C14 C15 C16 120.6(3) . . ? C15 C16 C11 122.3(3) . . ? C116 C111 C112 121.8(2) . . ? C116 C111 O1 118.0(2) . . ? C112 C111 O1 120.1(2) . . ? C111 C112 C113 118.8(3) . . ? C114 C113 C112 120.5(3) . . ? C113 C114 C115 120.2(3) . . ? C114 C115 C116 119.8(3) . . ? C111 C116 C115 118.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C111 O1 C12 C13 18.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.954 _refine_diff_density_min -1.678 _refine_diff_density_rms 0.116