Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Michael F. Lappert' 'Anthony G. Avent' 'Peter B. Hitchcock' 'Alexei V. Khvostov' _publ_contact_author_name 'Prof Michael F. Lappert' _publ_contact_author_address ; The Chemistry Laboratory University of Sussex Falmer Brighton East Sussex BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_section_title ; Synthesis and structures of the ytterbium(II) b-diketiminates [Yb{N(SiMe3)C(R1)C(H)C(R2)N(SiMe3)}2] (R1 = R2 = Ph, C6H4Me-4, or C6H4Ph-4; or R1 = C6H4Me-4, R2 = 1-adamantyl) ; data_oct200 _database_code_CSD 191917 _audit_creation_date 2000-10-04T15:25:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [Yb{Me3SiNC(Ad)CHC(PhMe)NSiMe3}2] _chemical_formula_moiety 'C52 H82 N4 Si4 Yb1' _chemical_formula_structural 'C52 H82 N4 Si4 Yb' _chemical_formula_sum 'C52 H82 N4 Si4 Yb' _chemical_formula_weight 1048.62 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7363(5) _cell_length_b 13.1615(6) _cell_length_c 16.5277(11) _cell_angle_alpha 85.738(3) _cell_angle_beta 82.722(4) _cell_angle_gamma 82.784(4) _cell_volume 2721.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18834 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.28 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.4332 _exptl_absorpt_correction_T_max 0.4783 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 18527 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_unetI/netI 0.0944 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 9531 _reflns_number_gt 7645 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1095P)^2^+10.6867P] 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_number_reflns 9531 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.199 _refine_ls_wR_factor_gt 0.1854 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 5.905 _refine_diff_density_min -2.063 _refine_diff_density_rms 0.201 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Yb Yb -0.385 5.5486 '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' 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 Yb Yb 0.77708(3) 0.71712(3) 0.75434(2) 0.02745(16) Uani 1 1 d . . . Si1 Si 0.7768(2) 0.46186(19) 0.67028(16) 0.0322(6) Uani 1 1 d . . . Si2 Si 0.50110(19) 0.74028(19) 0.83355(17) 0.0326(6) Uani 1 1 d . . . Si3 Si 1.0509(2) 0.7258(2) 0.81581(17) 0.0343(6) Uani 1 1 d . . . Si4 Si 0.75648(18) 0.98597(19) 0.69463(15) 0.0273(5) Uani 1 1 d . . . N1 N 0.7764(6) 0.5372(5) 0.7530(4) 0.0294(16) Uani 1 1 d . . . N2 N 0.6282(5) 0.7013(5) 0.8550(4) 0.0276(16) Uani 1 1 d . . . N3 N 0.9669(6) 0.7238(6) 0.7398(5) 0.0314(17) Uani 1 1 d . . . N4 N 0.7840(5) 0.8638(5) 0.6630(4) 0.0269(16) Uani 1 1 d . . . C1 C 0.7906(7) 0.5092(6) 0.8309(6) 0.0292(19) Uani 1 1 d . . . C2 C 0.7655(7) 0.5741(7) 0.8981(6) 0.032(2) Uani 1 1 d . . . H2 H 0.8121 0.5603 0.9393 0.038 Uiso 1 1 calc R . . C3 C 0.6836(7) 0.6548(7) 0.9135(6) 0.0299(19) Uani 1 1 d . . . C4 C 0.6881(10) 0.5419(9) 0.6042(7) 0.054(3) Uani 1 1 d . . . H4A H 0.7162 0.6075 0.5888 0.081 Uiso 1 1 calc R . . H4B H 0.6165 0.5544 0.6339 0.081 Uiso 1 1 calc R . . H4C H 0.6846 0.5061 0.5548 0.081 Uiso 1 1 calc R . . C5 C 0.9108(9) 0.4380(9) 0.6073(8) 0.056(3) Uani 1 1 d . . . H5A H 0.9607 0.3956 0.6401 0.085 Uiso 1 1 calc R . . H5B H 0.9381 0.5036 0.5905 0.085 Uiso 1 1 calc R . . H5C H 0.9033 0.4022 0.5588 0.085 Uiso 1 1 calc R . . C6 C 0.7199(10) 0.3377(8) 0.6982(8) 0.054(3) Uani 1 1 d . . . H6A H 0.7658 0.2938 0.733 0.081 Uiso 1 1 calc R . . H6B H 0.7158 0.3031 0.6483 0.081 Uiso 1 1 calc R . . H6C H 0.6483 0.3514 0.7277 0.081 Uiso 1 1 calc R . . C7 C 0.8393(7) 0.4023(7) 0.8532(5) 0.031(2) Uani 1 1 d . . . C8 C 0.7867(8) 0.3406(8) 0.9086(6) 0.043(2) Uani 1 1 d . . . H8 H 0.7205 0.3666 0.9373 0.051 Uiso 1 1 calc R . . C9 C 0.8287(10) 0.2386(9) 0.9243(7) 0.054(3) Uani 1 1 d . . . H9 H 0.7903 0.1958 0.963 0.065 Uiso 1 1 calc R . . C10 C 0.9262(9) 0.1993(8) 0.8837(7) 0.046(3) Uani 1 1 d . . . C11 C 0.9801(8) 0.2627(8) 0.8305(7) 0.046(3) Uani 1 1 d . . . H11 H 1.0478 0.2371 0.804 0.056 Uiso 1 1 calc R . . C12 C 0.9401(8) 0.3643(8) 0.8130(7) 0.043(2) Uani 1 1 d . . . H12 H 0.9795 0.4071 0.775 0.052 Uiso 1 1 calc R . . C13 C 0.9695(12) 0.0880(8) 0.9002(10) 0.073(4) Uani 1 1 d . . . H13A H 0.9189 0.0548 0.9401 0.11 Uiso 0.5 1 calc PR . . H13B H 1.038 0.0847 0.922 0.11 Uiso 0.5 1 calc PR . . H13C H 0.9796 0.0526 0.8492 0.11 Uiso 0.5 1 calc PR . . H13D H 1.0387 0.0733 0.8675 0.11 Uiso 0.5 1 calc PR . . H13E H 0.9197 0.0434 0.8855 0.11 Uiso 0.5 1 calc PR . . H13F H 0.978 0.0754 0.9583 0.11 Uiso 0.5 1 calc PR . . C14 C 0.6598(7) 0.6919(7) 1.0018(6) 0.032(2) Uani 1 1 d . . . C15 C 0.7393(9) 0.6429(8) 1.0602(6) 0.045(3) Uani 1 1 d . . . H15A H 0.8121 0.6575 1.038 0.054 Uiso 1 1 calc R . . H15B H 0.7386 0.5676 1.0646 0.054 Uiso 1 1 calc R . . C16 C 0.7102(10) 0.6855(8) 1.1462(7) 0.051(3) Uani 1 1 d . . . H16 H 0.7625 0.6526 1.1834 0.061 Uiso 1 1 calc R . . C17 C 0.5989(12) 0.6620(11) 1.1802(7) 0.072(4) Uani 1 1 d . . . H17A H 0.5795 0.6892 1.235 0.086 Uiso 1 1 calc R . . H17B H 0.5969 0.5868 1.1857 0.086 Uiso 1 1 calc R . . C18 C 0.5190(10) 0.7112(12) 1.1227(7) 0.068(4) Uani 1 1 d . . . H18 H 0.4456 0.696 1.1453 0.082 Uiso 1 1 calc R . . C19 C 0.5481(9) 0.6684(10) 1.0381(7) 0.051(3) Uani 1 1 d . . . H19A H 0.4954 0.6995 1.0015 0.061 Uiso 1 1 calc R . . H19B H 0.5458 0.5933 1.0426 0.061 Uiso 1 1 calc R . . C20 C 0.6613(8) 0.8087(7) 0.9965(6) 0.036(2) Uani 1 1 d . . . H20A H 0.6093 0.8415 0.96 0.043 Uiso 1 1 calc R . . H20B H 0.733 0.8254 0.9731 0.043 Uiso 1 1 calc R . . C21 C 0.6332(9) 0.8502(8) 1.0819(7) 0.046(3) Uani 1 1 d . . . H21 H 0.6343 0.9263 1.0773 0.055 Uiso 1 1 calc R . . C22 C 0.5225(11) 0.8269(12) 1.1159(9) 0.074(4) Uani 1 1 d . . . H22A H 0.4704 0.8599 1.0796 0.088 Uiso 1 1 calc R . . H22B H 0.503 0.8548 1.1705 0.088 Uiso 1 1 calc R . . C23 C 0.7147(10) 0.8020(9) 1.1379(7) 0.052(3) Uani 1 1 d . . . H23A H 0.6983 0.831 1.1922 0.062 Uiso 1 1 calc R . . H23B H 0.787 0.8169 1.1145 0.062 Uiso 1 1 calc R . . C24 C 0.5110(8) 0.7759(9) 0.7219(6) 0.045(3) Uani 1 1 d . . . H24A H 0.5535 0.8334 0.7094 0.068 Uiso 1 1 calc R . . H24B H 0.4394 0.7961 0.706 0.068 Uiso 1 1 calc R . . H24C H 0.5453 0.717 0.6916 0.068 Uiso 1 1 calc R . . C25 C 0.4201(9) 0.6317(9) 0.8566(8) 0.054(3) Uani 1 1 d . . . H25A H 0.4145 0.6127 0.9153 0.082 Uiso 1 1 calc R . . H25B H 0.4543 0.5729 0.8262 0.082 Uiso 1 1 calc R . . H25C H 0.3487 0.6523 0.8405 0.082 Uiso 1 1 calc R . . C26 C 0.4274(9) 0.8575(9) 0.8816(9) 0.058(3) Uani 1 1 d . . . H26A H 0.4699 0.915 0.8693 0.087 Uiso 1 1 calc R . . H26B H 0.4148 0.8439 0.941 0.087 Uiso 1 1 calc R . . H26C H 0.3589 0.8748 0.8597 0.087 Uiso 1 1 calc R . . C27 C 0.9884(7) 0.7160(6) 0.6625(6) 0.029(2) Uani 1 1 d . . . C28 C 0.9141(7) 0.7370(6) 0.6013(6) 0.0288(19) Uani 1 1 d . . . H28 H 0.9253 0.6917 0.558 0.035 Uiso 1 1 calc R . . C29 C 0.8292(7) 0.8139(7) 0.5975(5) 0.0273(18) Uani 1 1 d . . . C30 C 1.1621(9) 0.8042(10) 0.7823(8) 0.056(3) Uani 1 1 d . . . H30A H 1.2083 0.7726 0.7367 0.084 Uiso 1 1 calc R . . H30B H 1.2036 0.8075 0.8279 0.084 Uiso 1 1 calc R . . H30C H 1.133 0.8737 0.7647 0.084 Uiso 1 1 calc R . . C31 C 0.9660(9) 0.7887(9) 0.9018(7) 0.052(3) Uani 1 1 d . . . H31A H 0.9066 0.7489 0.9207 0.078 Uiso 1 1 calc R . . H31B H 0.938 0.8582 0.8834 0.078 Uiso 1 1 calc R . . H31C H 1.0085 0.7924 0.9467 0.078 Uiso 1 1 calc R . . C32 C 1.1009(10) 0.5950(9) 0.8580(7) 0.054(3) Uani 1 1 d . . . H32A H 1.1469 0.558 0.815 0.081 Uiso 1 1 calc R . . H32B H 1.0403 0.557 0.8776 0.081 Uiso 1 1 calc R . . H32C H 1.1417 0.6017 0.9034 0.081 Uiso 1 1 calc R . . C33 C 1.1026(7) 0.6911(7) 0.6223(6) 0.031(2) Uani 1 1 d . . . C34 C 1.1670(8) 0.6039(8) 0.6437(7) 0.044(2) Uani 1 1 d . . . H34 H 1.1389 0.5538 0.682 0.053 Uiso 1 1 calc R . . C35 C 1.2728(8) 0.5885(9) 0.6098(7) 0.046(3) Uani 1 1 d . . . H35 H 1.316 0.5273 0.6242 0.056 Uiso 1 1 calc R . . C36 C 1.3157(8) 0.6613(9) 0.5554(7) 0.043(2) Uani 1 1 d . . . C37 C 1.2510(8) 0.7485(9) 0.5323(8) 0.051(3) Uani 1 1 d . . . H37 H 1.2795 0.7991 0.4947 0.062 Uiso 1 1 calc R . . C38 C 1.1437(8) 0.7618(8) 0.5645(6) 0.043(2) Uani 1 1 d . . . H38 H 1.0984 0.8198 0.5466 0.052 Uiso 1 1 calc R . . C39 C 1.4316(9) 0.6479(11) 0.5175(9) 0.064(3) Uani 1 1 d . . . H39A H 1.4461 0.7079 0.4809 0.096 Uiso 0.5 1 calc PR . . H39B H 1.4451 0.5861 0.4864 0.096 Uiso 0.5 1 calc PR . . H39C H 1.4783 0.6412 0.5609 0.096 Uiso 0.5 1 calc PR . . H39D H 1.4669 0.5822 0.5379 0.096 Uiso 0.5 1 calc PR . . H39E H 1.4679 0.704 0.5324 0.096 Uiso 0.5 1 calc PR . . H39F H 1.4346 0.6489 0.4579 0.096 Uiso 0.5 1 calc PR . . C40 C 0.7857(6) 0.8409(7) 0.5145(5) 0.0280(19) Uani 1 1 d . . . C41 C 0.8270(7) 0.7622(7) 0.4486(5) 0.033(2) Uani 1 1 d . . . H41A H 0.9057 0.7569 0.4387 0.04 Uiso 1 1 calc R . . H41B H 0.8069 0.6937 0.4688 0.04 Uiso 1 1 calc R . . C42 C 0.7806(7) 0.7942(8) 0.3683(6) 0.038(2) Uani 1 1 d . . . H42 H 0.8072 0.742 0.3273 0.046 Uiso 1 1 calc R . . C43 C 0.8147(8) 0.8995(9) 0.3360(6) 0.043(2) Uani 1 1 d . . . H43A H 0.8934 0.8945 0.3255 0.052 Uiso 1 1 calc R . . H43B H 0.7854 0.9209 0.2839 0.052 Uiso 1 1 calc R . . C44 C 0.7743(9) 0.9784(8) 0.3981(6) 0.043(2) Uani 1 1 d . . . H44 H 0.7963 1.0467 0.3771 0.052 Uiso 1 1 calc R . . C45 C 0.8193(7) 0.9455(7) 0.4797(5) 0.035(2) Uani 1 1 d . . . H45A H 0.7931 0.9981 0.5196 0.042 Uiso 1 1 calc R . . H45B H 0.8981 0.9409 0.4709 0.042 Uiso 1 1 calc R . . C46 C 0.6635(7) 0.8493(7) 0.5258(5) 0.0307(19) Uani 1 1 d . . . H46A H 0.6349 0.9004 0.5665 0.037 Uiso 1 1 calc R . . H46B H 0.6406 0.7822 0.5471 0.037 Uiso 1 1 calc R . . C47 C 0.6174(8) 0.8818(9) 0.4442(6) 0.042(2) Uani 1 1 d . . . H47 H 0.5378 0.8872 0.4535 0.051 Uiso 1 1 calc R . . C48 C 0.6514(8) 0.9850(8) 0.4121(7) 0.045(3) Uani 1 1 d . . . H48A H 0.623 1.0373 0.4519 0.054 Uiso 1 1 calc R . . H48B H 0.6219 1.0063 0.36 0.054 Uiso 1 1 calc R . . C49 C 0.6583(8) 0.8035(9) 0.3840(6) 0.044(3) Uani 1 1 d . . . H49A H 0.6279 0.8231 0.332 0.053 Uiso 1 1 calc R . . H49B H 0.6355 0.7363 0.405 0.053 Uiso 1 1 calc R . . C50 C 0.8770(8) 1.0553(8) 0.6673(7) 0.044(2) Uani 1 1 d . . . H50A H 0.8936 1.0616 0.6077 0.066 Uiso 1 1 calc R . . H50B H 0.9377 1.0168 0.6912 0.066 Uiso 1 1 calc R . . H50C H 0.8628 1.1238 0.6886 0.066 Uiso 1 1 calc R . . C51 C 0.7268(8) 0.9746(8) 0.8076(6) 0.041(2) Uani 1 1 d . . . H51A H 0.6636 0.9386 0.8227 0.062 Uiso 1 1 calc R . . H51B H 0.7132 1.0432 0.8288 0.062 Uiso 1 1 calc R . . H51C H 0.7878 0.9359 0.8311 0.062 Uiso 1 1 calc R . . C52 C 0.6358(7) 1.0671(7) 0.6603(6) 0.036(2) Uani 1 1 d . . . H52A H 0.6447 1.077 0.6006 0.054 Uiso 1 1 calc R . . H52B H 0.6275 1.1338 0.6844 0.054 Uiso 1 1 calc R . . H52C H 0.5722 1.0325 0.6781 0.054 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 Yb 0.0289(2) 0.0283(2) 0.0251(2) -0.00216(15) -0.00169(14) -0.00440(14) Si1 0.0420(14) 0.0307(13) 0.0240(13) -0.0070(10) -0.0018(10) -0.0043(11) Si2 0.0283(12) 0.0329(13) 0.0366(15) -0.0027(11) -0.0024(10) -0.0053(10) Si3 0.0307(13) 0.0424(15) 0.0323(15) -0.0031(12) -0.0125(11) -0.0044(11) Si4 0.0262(11) 0.0320(13) 0.0240(13) -0.0030(10) -0.0021(9) -0.0042(10) N1 0.039(4) 0.028(4) 0.021(4) -0.003(3) 0.000(3) -0.007(3) N2 0.030(4) 0.032(4) 0.020(4) -0.005(3) 0.004(3) -0.005(3) N3 0.034(4) 0.034(4) 0.027(4) -0.001(3) -0.010(3) -0.002(3) N4 0.031(4) 0.029(4) 0.022(4) -0.004(3) 0.000(3) -0.008(3) C1 0.032(4) 0.022(4) 0.035(5) -0.006(4) -0.012(4) -0.001(3) C2 0.040(5) 0.029(5) 0.026(5) -0.007(4) -0.006(4) 0.002(4) C3 0.034(5) 0.027(4) 0.028(5) -0.004(4) 0.001(4) -0.006(4) C4 0.080(8) 0.049(6) 0.037(6) -0.013(5) -0.024(6) -0.004(6) C5 0.062(7) 0.055(7) 0.048(7) -0.019(6) 0.011(6) 0.000(6) C6 0.073(8) 0.044(6) 0.050(7) -0.006(5) -0.012(6) -0.018(5) C7 0.045(5) 0.032(5) 0.020(5) -0.012(4) -0.007(4) -0.008(4) C8 0.050(6) 0.042(6) 0.033(6) -0.003(5) 0.004(5) -0.001(5) C9 0.078(8) 0.046(6) 0.040(7) 0.007(5) -0.016(6) -0.010(6) C10 0.060(7) 0.035(5) 0.045(7) -0.004(5) -0.022(5) 0.004(5) C11 0.044(6) 0.037(6) 0.056(7) -0.009(5) -0.014(5) 0.015(5) C12 0.038(5) 0.039(6) 0.053(7) -0.012(5) -0.007(5) 0.002(4) C13 0.104(11) 0.030(6) 0.085(11) 0.007(6) -0.033(9) 0.010(6) C14 0.041(5) 0.030(5) 0.025(5) -0.004(4) 0.007(4) -0.013(4) C15 0.073(7) 0.038(6) 0.026(5) -0.003(4) -0.013(5) -0.002(5) C16 0.084(8) 0.043(6) 0.027(6) -0.007(5) -0.008(5) -0.013(6) C17 0.116(11) 0.089(10) 0.017(6) -0.015(6) 0.019(6) -0.059(9) C18 0.066(8) 0.120(12) 0.022(6) -0.019(7) 0.019(5) -0.044(8) C19 0.063(7) 0.069(8) 0.026(6) -0.009(5) 0.004(5) -0.030(6) C20 0.043(5) 0.032(5) 0.031(5) -0.002(4) 0.004(4) -0.003(4) C21 0.065(7) 0.036(5) 0.037(6) -0.018(5) 0.002(5) -0.007(5) C22 0.068(8) 0.097(11) 0.055(9) -0.050(8) 0.012(6) 0.002(7) C23 0.081(8) 0.057(7) 0.023(5) -0.015(5) -0.004(5) -0.021(6) C24 0.042(5) 0.058(7) 0.033(6) 0.005(5) -0.005(4) -0.003(5) C25 0.054(7) 0.058(7) 0.058(8) 0.004(6) -0.015(6) -0.030(6) C26 0.039(6) 0.057(7) 0.075(9) -0.013(6) -0.008(6) 0.009(5) C27 0.028(4) 0.020(4) 0.041(6) -0.001(4) -0.006(4) -0.006(3) C28 0.032(4) 0.027(4) 0.027(5) -0.008(4) -0.006(4) 0.002(4) C29 0.030(4) 0.031(5) 0.022(5) -0.003(4) -0.003(3) -0.007(4) C30 0.046(6) 0.074(8) 0.053(7) 0.003(6) -0.010(5) -0.023(6) C31 0.049(6) 0.063(7) 0.046(7) -0.004(6) -0.016(5) -0.006(5) C32 0.066(7) 0.054(7) 0.044(7) 0.004(5) -0.023(6) 0.000(6) C33 0.029(4) 0.039(5) 0.026(5) -0.011(4) -0.002(4) -0.002(4) C34 0.043(6) 0.050(6) 0.035(6) -0.007(5) -0.003(4) 0.009(5) C35 0.038(5) 0.059(7) 0.044(6) -0.016(5) -0.010(5) 0.003(5) C36 0.034(5) 0.062(7) 0.038(6) -0.020(5) -0.002(4) -0.011(5) C37 0.042(6) 0.056(7) 0.056(8) -0.011(6) 0.002(5) -0.012(5) C38 0.038(5) 0.054(6) 0.035(6) -0.001(5) -0.001(4) 0.002(5) C39 0.038(6) 0.092(10) 0.062(9) -0.021(7) 0.003(5) -0.009(6) C40 0.027(4) 0.034(5) 0.024(5) -0.001(4) -0.003(3) -0.006(4) C41 0.041(5) 0.041(5) 0.020(5) -0.009(4) -0.005(4) -0.006(4) C42 0.039(5) 0.058(6) 0.020(5) -0.007(4) -0.001(4) -0.012(5) C43 0.036(5) 0.073(7) 0.021(5) 0.000(5) 0.000(4) -0.017(5) C44 0.060(6) 0.045(6) 0.024(5) 0.004(4) -0.006(5) -0.010(5) C45 0.040(5) 0.046(6) 0.018(5) -0.004(4) 0.001(4) -0.010(4) C46 0.029(4) 0.044(5) 0.021(5) -0.004(4) -0.004(3) -0.006(4) C47 0.033(5) 0.066(7) 0.027(5) -0.004(5) -0.004(4) -0.003(5) C48 0.053(6) 0.049(6) 0.034(6) -0.002(5) -0.017(5) 0.003(5) C49 0.042(5) 0.074(7) 0.023(5) -0.004(5) -0.012(4) -0.020(5) C50 0.040(5) 0.045(6) 0.050(7) -0.008(5) -0.002(5) -0.013(4) C51 0.051(6) 0.048(6) 0.024(5) -0.010(4) -0.005(4) 0.001(5) C52 0.035(5) 0.037(5) 0.033(5) -0.006(4) -0.002(4) 0.008(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Yb N4 2.364(7) . ? Yb N1 2.371(7) . ? Yb N2 2.378(7) . ? Yb N3 2.412(7) . ? Si1 N1 1.746(8) . ? Si1 C4 1.850(11) . ? Si1 C6 1.873(11) . ? Si1 C5 1.886(11) . ? Si2 N2 1.709(7) . ? Si2 C25 1.855(10) . ? Si2 C24 1.862(10) . ? Si2 C26 1.877(11) . ? Si3 N3 1.753(7) . ? Si3 C31 1.853(12) . ? Si3 C30 1.860(11) . ? Si3 C32 1.874(11) . ? Si4 N4 1.708(7) . ? Si4 C51 1.856(10) . ? Si4 C50 1.873(10) . ? Si4 C52 1.882(9) . ? N1 C1 1.341(12) . ? N2 C3 1.336(11) . ? N3 C27 1.282(12) . ? N4 C29 1.337(11) . ? C1 C2 1.432(13) . ? C1 C7 1.503(12) . ? C2 C3 1.406(12) . ? C3 C14 1.554(13) . ? C7 C8 1.349(14) . ? C7 C12 1.419(14) . ? C8 C9 1.399(15) . ? C9 C10 1.392(17) . ? C10 C11 1.351(16) . ? C10 C13 1.516(14) . ? C11 C12 1.392(14) . ? C14 C19 1.532(14) . ? C14 C20 1.535(13) . ? C14 C15 1.538(13) . ? C15 C16 1.550(14) . ? C16 C17 1.518(17) . ? C16 C23 1.537(15) . ? C17 C18 1.53(2) . ? C18 C22 1.52(2) . ? C18 C19 1.531(15) . ? C20 C21 1.536(14) . ? C21 C22 1.510(17) . ? C21 C23 1.526(16) . ? C27 C28 1.460(12) . ? C27 C33 1.527(12) . ? C28 C29 1.390(12) . ? C29 C40 1.545(12) . ? C33 C34 1.376(13) . ? C33 C38 1.383(14) . ? C34 C35 1.388(14) . ? C35 C36 1.380(16) . ? C36 C37 1.387(16) . ? C36 C39 1.523(14) . ? C37 C38 1.397(14) . ? C40 C46 1.534(12) . ? C40 C45 1.543(13) . ? C40 C41 1.557(12) . ? C41 C42 1.529(13) . ? C42 C49 1.537(13) . ? C42 C43 1.543(15) . ? C43 C44 1.512(15) . ? C44 C45 1.542(13) . ? C44 C48 1.545(15) . ? C46 C47 1.549(12) . ? C47 C49 1.487(15) . ? C47 C48 1.516(15) . ? 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 Yb N1 140.2(2) . . ? N4 Yb N2 121.0(2) . . ? N1 Yb N2 82.4(2) . . ? N4 Yb N3 81.7(2) . . ? N1 Yb N3 99.2(2) . . ? N2 Yb N3 141.8(3) . . ? N1 Si1 C4 103.5(4) . . ? N1 Si1 C6 114.0(5) . . ? C4 Si1 C6 107.9(6) . . ? N1 Si1 C5 114.0(5) . . ? C4 Si1 C5 106.6(6) . . ? C6 Si1 C5 110.1(6) . . ? N2 Si2 C25 109.3(5) . . ? N2 Si2 C24 106.3(4) . . ? C25 Si2 C24 109.1(5) . . ? N2 Si2 C26 118.4(5) . . ? C25 Si2 C26 109.4(6) . . ? C24 Si2 C26 104.0(6) . . ? N3 Si3 C31 105.3(4) . . ? N3 Si3 C30 112.2(5) . . ? C31 Si3 C30 107.8(6) . . ? N3 Si3 C32 113.6(5) . . ? C31 Si3 C32 105.8(6) . . ? C30 Si3 C32 111.5(6) . . ? N4 Si4 C51 106.6(4) . . ? N4 Si4 C50 109.5(4) . . ? C51 Si4 C50 108.8(5) . . ? N4 Si4 C52 117.8(4) . . ? C51 Si4 C52 103.9(5) . . ? C50 Si4 C52 109.8(5) . . ? C1 N1 Si1 130.0(6) . . ? C1 N1 Yb 100.2(5) . . ? Si1 N1 Yb 129.3(4) . . ? C3 N2 Si2 142.4(6) . . ? C3 N2 Yb 96.3(5) . . ? Si2 N2 Yb 121.2(4) . . ? C27 N3 Si3 130.9(6) . . ? C27 N3 Yb 99.8(5) . . ? Si3 N3 Yb 129.1(4) . . ? C29 N4 Si4 139.9(6) . . ? C29 N4 Yb 96.3(5) . . ? Si4 N4 Yb 122.8(4) . . ? N1 C1 C2 125.6(8) . . ? N1 C1 C7 120.1(8) . . ? C2 C1 C7 114.4(8) . . ? N1 C1 Yb 53.0(4) . . ? C2 C1 Yb 75.7(5) . . ? C7 C1 Yb 158.1(6) . . ? C3 C2 C1 130.8(8) . . ? C3 C2 Yb 73.3(5) . . ? C1 C2 Yb 75.9(5) . . ? N2 C3 C2 122.4(8) . . ? N2 C3 C14 119.6(7) . . ? C2 C3 C14 118.0(8) . . ? N2 C3 Yb 55.9(4) . . ? C2 C3 Yb 78.6(5) . . ? C14 C3 Yb 140.9(6) . . ? C8 C7 C12 119.4(9) . . ? C8 C7 C1 120.9(9) . . ? C12 C7 C1 119.6(9) . . ? C7 C8 C9 120.6(10) . . ? C10 C9 C8 120.7(11) . . ? C11 C10 C9 118.3(9) . . ? C11 C10 C13 121.7(11) . . ? C9 C10 C13 120.0(11) . . ? C10 C11 C12 122.5(10) . . ? C11 C12 C7 118.5(10) . . ? C19 C14 C20 108.4(8) . . ? C19 C14 C15 108.1(8) . . ? C20 C14 C15 108.7(8) . . ? C19 C14 C3 109.2(8) . . ? C20 C14 C3 107.8(7) . . ? C15 C14 C3 114.4(8) . . ? C14 C15 C16 110.8(9) . . ? C17 C16 C23 110.4(10) . . ? C17 C16 C15 109.2(10) . . ? C23 C16 C15 108.3(9) . . ? C16 C17 C18 109.6(10) . . ? C22 C18 C19 109.6(10) . . ? C22 C18 C17 108.8(11) . . ? C19 C18 C17 109.9(11) . . ? C18 C19 C14 110.4(9) . . ? C14 C20 C21 110.0(8) . . ? C22 C21 C23 110.7(11) . . ? C22 C21 C20 109.2(9) . . ? C23 C21 C20 110.0(8) . . ? C21 C22 C18 109.7(10) . . ? C21 C23 C16 108.5(9) . . ? N3 C27 C28 127.0(8) . . ? N3 C27 C33 121.7(8) . . ? C28 C27 C33 111.1(8) . . ? N3 C27 Yb 54.6(5) . . ? C28 C27 Yb 74.8(5) . . ? C33 C27 Yb 167.3(6) . . ? C29 C28 C27 129.0(8) . . ? C29 C28 Yb 73.6(5) . . ? C27 C28 Yb 76.1(5) . . ? N4 C29 C28 122.3(8) . . ? N4 C29 C40 119.6(7) . . ? C28 C29 C40 118.1(8) . . ? N4 C29 Yb 55.8(4) . . ? C28 C29 Yb 78.4(5) . . ? C40 C29 Yb 141.8(6) . . ? C34 C33 C38 119.2(9) . . ? C34 C33 C27 122.7(9) . . ? C38 C33 C27 118.1(8) . . ? C33 C34 C35 120.5(11) . . ? C36 C35 C34 120.7(10) . . ? C35 C36 C37 119.3(9) . . ? C35 C36 C39 122.3(10) . . ? C37 C36 C39 118.4(11) . . ? C36 C37 C38 119.7(11) . . ? C33 C38 C37 120.6(10) . . ? C46 C40 C45 108.4(7) . . ? C46 C40 C29 110.3(7) . . ? C45 C40 C29 109.0(7) . . ? C46 C40 C41 107.6(7) . . ? C45 C40 C41 107.0(7) . . ? C29 C40 C41 114.4(7) . . ? C42 C41 C40 111.3(8) . . ? C41 C42 C49 109.3(8) . . ? C41 C42 C43 109.0(8) . . ? C49 C42 C43 108.9(9) . . ? C44 C43 C42 109.8(8) . . ? C43 C44 C45 110.1(8) . . ? C43 C44 C48 108.2(9) . . ? C45 C44 C48 109.1(8) . . ? C44 C45 C40 111.3(8) . . ? C40 C46 C47 111.4(7) . . ? C49 C47 C48 109.8(9) . . ? C49 C47 C46 109.1(8) . . ? C48 C47 C46 109.3(8) . . ? C47 C48 C44 110.2(8) . . ? C47 C49 C42 110.5(8) . . ? data_sep501 _database_code_CSD 191918 _audit_creation_date 2001-09-11T14:37:11-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common sep501 _chemical_formula_moiety 'C42 H58 N4 Si4 Yb1' _chemical_formula_sum 'C42 H58 N4 Si4 Yb' _chemical_formula_weight 904.32 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1217(14) _cell_length_b 13.6826(15) _cell_length_c 14.1141(16) _cell_angle_alpha 103.340(5) _cell_angle_beta 108.799(5) _cell_angle_gamma 100.987(6) _cell_volume 2235.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11519 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_T_max 0.767 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 10932 _diffrn_reflns_av_R_equivalents 0.0793 _diffrn_reflns_av_unetI/netI 0.1128 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 21.94 _diffrn_reflns_theta_full 21.94 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 5369 _reflns_number_gt 4096 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; An initial refinement with all atoms anisotropic showed elongated ellipsoids for the carbon atoms of the phenyl groups, suggesting some disorder. For two of the phenyl groups (C16- C21) and (C31 - C36) this disorder could be resolved. All phenyl groups were finally refined as rigid bodies with isotropic carbon atoms,; two ordered rings and two disordered rings. 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^)+(0.0614P)^2^+14.6008P] 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_number_reflns 5369 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.05 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.867 _refine_diff_density_min -1.278 _refine_diff_density_rms 0.159 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Yb Yb -0.385 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Yb Yb 0.89054(5) 0.62549(4) 0.74134(4) 0.0349(2) Uani 1 1 d . . . Si1 Si 0.8426(3) 0.3631(3) 0.6240(3) 0.0374(9) Uani 1 1 d . . . Si2 Si 0.8540(3) 0.7984(3) 0.9419(3) 0.0400(9) Uani 1 1 d . . . Si3 Si 0.6927(3) 0.6786(3) 0.5453(3) 0.0403(9) Uani 1 1 d . . . Si4 Si 1.1741(3) 0.6664(3) 0.8578(3) 0.0363(9) Uani 1 1 d . . . N1 N 0.8174(7) 0.4429(7) 0.7240(7) 0.032(2) Uani 1 1 d . . . N2 N 0.8159(8) 0.6647(8) 0.8770(7) 0.036(3) Uani 1 1 d . A . N3 N 0.8387(8) 0.7128(9) 0.6119(9) 0.050(3) Uani 1 1 d . B . N4 N 1.0809(8) 0.7052(7) 0.7654(7) 0.031(2) Uani 1 1 d . B . C1 C 0.7548(10) 0.4143(10) 0.7755(9) 0.036(3) Uani 1 1 d . . . C2 C 0.7210(10) 0.4803(10) 0.8453(9) 0.036(3) Uani 1 1 d . A . H2 H 0.6688 0.4423 0.8667 0.043 Uiso 1 1 calc R . . C3 C 0.7474(9) 0.5889(10) 0.8897(8) 0.033(3) Uani 1 1 d . . . C4 C 0.7149(10) 0.2552(10) 0.5253(9) 0.045(4) Uani 1 1 d . . . H4A H 0.652 0.2844 0.5021 0.068 Uiso 1 1 calc R . . H4B H 0.6951 0.2024 0.5578 0.068 Uiso 1 1 calc R . . H4C H 0.7311 0.2225 0.4643 0.068 Uiso 1 1 calc R . . C5 C 0.9623(11) 0.3091(11) 0.6681(11) 0.054(4) Uani 1 1 d . . . H5A H 0.9457 0.2609 0.7064 0.081 Uiso 1 1 calc R . . H5B H 1.0302 0.3666 0.7147 0.081 Uiso 1 1 calc R . . H5C H 0.9745 0.2713 0.6066 0.081 Uiso 1 1 calc R . . C6 C 0.8843(12) 0.4528(10) 0.5518(10) 0.052(4) Uani 1 1 d . . . H6A H 0.8241 0.4844 0.5262 0.079 Uiso 1 1 calc R . . H6B H 0.8973 0.4126 0.4918 0.079 Uiso 1 1 calc R . . H6C H 0.9534 0.5082 0.5996 0.079 Uiso 1 1 calc R . . C7 C 0.913(2) 0.8378(14) 1.0878(13) 0.118(9) Uani 1 1 d . . . H7A H 0.9715 0.804 1.1114 0.177 Uiso 1 1 calc R . . H7B H 0.8529 0.8161 1.1124 0.177 Uiso 1 1 calc R . . H7C H 0.9451 0.9141 1.1168 0.177 Uiso 1 1 calc R . . C8 C 0.7449(18) 0.8656(17) 0.9052(16) 0.129(9) Uani 1 1 d . . . H8A H 0.7113 0.8476 0.8282 0.194 Uiso 1 1 calc R . . H8B H 0.779 0.9417 0.9364 0.194 Uiso 1 1 calc R . . H8C H 0.6866 0.8434 0.9313 0.194 Uiso 1 1 calc R . . C9 C 0.967(2) 0.8558(13) 0.902(2) 0.179(15) Uani 1 1 d . . . H9A H 0.9387 0.8369 0.8254 0.268 Uiso 1 1 calc R . . H9B H 1.0308 0.8286 0.9277 0.268 Uiso 1 1 calc R . . H9C H 0.9905 0.9323 0.9333 0.268 Uiso 1 1 calc R . . C10 C 0.7110(6) 0.2992(4) 0.7612(6) 0.027(3) Uiso 1 1 d G . . C11 C 0.7852(4) 0.2408(6) 0.7883(6) 0.040(3) Uiso 1 1 d G . . H11 H 0.8639 0.274 0.82 0.048 Uiso 1 1 calc R . . C12 C 0.7442(6) 0.1336(6) 0.7690(7) 0.052(4) Uiso 1 1 d G . . H12 H 0.7949 0.0937 0.7875 0.062 Uiso 1 1 calc R . . C13 C 0.6291(7) 0.0850(4) 0.7225(7) 0.061(4) Uiso 1 1 d G . . H13 H 0.6011 0.0118 0.7093 0.073 Uiso 1 1 calc R . . C14 C 0.5549(5) 0.1435(6) 0.6954(7) 0.057(4) Uiso 1 1 d G . . H14 H 0.4762 0.1102 0.6636 0.068 Uiso 1 1 calc R . . C15 C 0.5959(5) 0.2506(6) 0.7147(6) 0.043(3) Uiso 1 1 d G . . H15 H 0.5452 0.2905 0.6962 0.051 Uiso 1 1 calc R . . C22 C 0.9136(10) 0.7909(11) 0.6058(11) 0.048(4) Uani 1 1 d . . . C23 C 1.0310(10) 0.8215(11) 0.6593(11) 0.051(4) Uani 1 1 d . B . H23 H 1.0684 0.8799 0.6455 0.061 Uiso 1 1 calc R . . C24 C 1.1059(9) 0.7834(10) 0.7300(9) 0.034(3) Uani 1 1 d . . . C25 C 0.6369(10) 0.5909(11) 0.6108(10) 0.053(4) Uani 1 1 d . . . H25A H 0.6693 0.5319 0.6068 0.079 Uiso 1 1 calc R . . H25B H 0.5549 0.5642 0.5753 0.079 Uiso 1 1 calc R . . H25C H 0.6571 0.6302 0.6849 0.079 Uiso 1 1 calc R . . C26 C 0.6431(13) 0.6008(14) 0.4039(11) 0.074(5) Uani 1 1 d . . . H26A H 0.6771 0.543 0.3974 0.111 Uiso 1 1 calc R . . H26B H 0.6649 0.646 0.3648 0.111 Uiso 1 1 calc R . . H26C H 0.561 0.5724 0.3749 0.111 Uiso 1 1 calc R . . C27 C 0.6271(11) 0.7869(12) 0.5561(12) 0.061(4) Uani 1 1 d . . . H27A H 0.653 0.8285 0.6304 0.092 Uiso 1 1 calc R . . H27B H 0.5452 0.7578 0.5271 0.092 Uiso 1 1 calc R . . H27C H 0.6485 0.8318 0.5165 0.092 Uiso 1 1 calc R . . C28 C 1.0844(10) 0.5901(11) 0.9127(10) 0.044(3) Uani 1 1 d . . . H28A H 1.0249 0.5319 0.855 0.067 Uiso 1 1 calc R . . H28B H 1.0504 0.6365 0.9484 0.067 Uiso 1 1 calc R . . H28C H 1.1312 0.5624 0.9631 0.067 Uiso 1 1 calc R . . C29 C 1.2383(11) 0.5748(10) 0.7926(11) 0.050(4) Uani 1 1 d . . . H29A H 1.1789 0.5189 0.7324 0.074 Uiso 1 1 calc R . . H29B H 1.2797 0.5439 0.8432 0.074 Uiso 1 1 calc R . . H29C H 1.29 0.6135 0.768 0.074 Uiso 1 1 calc R . . C30 C 1.2844(11) 0.7751(10) 0.9739(9) 0.044(3) Uani 1 1 d . . . H30A H 1.2485 0.8219 1.0063 0.066 Uiso 1 1 calc R . . H30B H 1.3366 0.8148 0.9505 0.066 Uiso 1 1 calc R . . H30C H 1.3258 0.7453 1.0257 0.066 Uiso 1 1 calc R . . C37 C 1.2271(5) 0.8501(6) 0.7678(6) 0.031(3) Uiso 1 1 d G B . C38 C 1.3051(6) 0.8060(5) 0.7411(6) 0.038(3) Uiso 1 1 d G . . H38 H 1.282 0.7356 0.6965 0.046 Uiso 1 1 calc R B . C39 C 1.4170(5) 0.8650(6) 0.7797(7) 0.052(4) Uiso 1 1 d G B . H39 H 1.4703 0.8348 0.7614 0.062 Uiso 1 1 calc R . . C40 C 1.4508(5) 0.9680(6) 0.8450(7) 0.051(4) Uiso 1 1 d G . . H40 H 1.5272 1.0083 0.8713 0.061 Uiso 1 1 calc R B . C41 C 1.3728(6) 1.0121(5) 0.8717(6) 0.055(4) Uiso 1 1 d G B . H41 H 1.3959 1.0825 0.9163 0.066 Uiso 1 1 calc R . . C42 C 1.2610(6) 0.9531(6) 0.8331(6) 0.050(4) Uiso 1 1 d G . . H42 H 1.2077 0.9833 0.8513 0.06 Uiso 1 1 calc R B . C16 C 0.6759(14) 0.6222(13) 0.9526(13) 0.027(8) Uiso 0.53(2) 1 d PG A 1 C17 C 0.5940(14) 0.6707(15) 0.9164(10) 0.049(8) Uiso 0.53(2) 1 d PG A 1 H17 H 0.5806 0.6844 0.8512 0.059 Uiso 0.53(2) 1 calc PR A 1 C18 C 0.5318(12) 0.6993(15) 0.9758(13) 0.049(8) Uiso 0.53(2) 1 d PG A 1 H18 H 0.4758 0.7324 0.9511 0.059 Uiso 0.53(2) 1 calc PR A 1 C19 C 0.5515(14) 0.6792(13) 1.0713(13) 0.053(8) Uiso 0.53(2) 1 d PG A 1 H19 H 0.509 0.6987 1.1119 0.064 Uiso 0.53(2) 1 calc PR A 1 C20 C 0.6334(17) 0.6307(14) 1.1075(12) 0.042(7) Uiso 0.53(2) 1 d PG A 1 H20 H 0.6469 0.617 1.1728 0.05 Uiso 0.53(2) 1 calc PR A 1 C21 C 0.6956(15) 0.6022(13) 1.0481(14) 0.047(7) Uiso 0.53(2) 1 d PG A 1 H21 H 0.7516 0.569 1.0728 0.056 Uiso 0.53(2) 1 calc PR A 1 C31 C 0.8750(16) 0.8743(19) 0.5538(17) 0.037(8) Uiso 0.50(4) 1 d PG B 1 C32 C 0.848(2) 0.9611(16) 0.6017(13) 0.064(10) Uiso 0.50(4) 1 d PG B 1 H32 H 0.8607 0.9785 0.6745 0.077 Uiso 0.50(4) 1 calc PR B 1 C33 C 0.803(2) 1.0225(13) 0.5431(16) 0.064(10) Uiso 0.50(4) 1 d PG B 1 H33 H 0.7849 1.0818 0.5759 0.076 Uiso 0.50(4) 1 calc PR B 1 C34 C 0.7850(15) 0.9971(17) 0.4366(17) 0.035(8) Uiso 0.50(4) 1 d PG B 1 H34 H 0.7542 1.039 0.3966 0.043 Uiso 0.50(4) 1 calc PR B 1 C35 C 0.812(2) 0.910(2) 0.3887(17) 0.052(9) Uiso 0.50(4) 1 d PG B 1 H35 H 0.7993 0.893 0.316 0.063 Uiso 0.50(4) 1 calc PR B 1 C36 C 0.857(2) 0.849(2) 0.447(2) 0.040(8) Uiso 0.50(4) 1 d PG B 1 H36 H 0.875 0.7896 0.4145 0.048 Uiso 0.50(4) 1 calc PR B 1 C16A C 0.6947(15) 0.6138(15) 0.9687(13) 0.041(11) Uiso 0.47(2) 1 d PG A 2 C17A C 0.5830(15) 0.6140(18) 0.9309(11) 0.056(9) Uiso 0.47(2) 1 d PG A 2 H17A H 0.5417 0.5949 0.8571 0.067 Uiso 0.47(2) 1 calc PR A 2 C18A C 0.5316(12) 0.6420(18) 1.0009(15) 0.055(9) Uiso 0.47(2) 1 d PG A 2 H18A H 0.4553 0.6421 0.9751 0.066 Uiso 0.47(2) 1 calc PR A 2 C19A C 0.5920(16) 0.6700(16) 1.1089(14) 0.064(10) Uiso 0.47(2) 1 d PG A 2 H19A H 0.5569 0.6891 1.1567 0.077 Uiso 0.47(2) 1 calc PR A 2 C20A C 0.7038(16) 0.6698(16) 1.1467(11) 0.044(8) Uiso 0.47(2) 1 d PG A 2 H20A H 0.7451 0.6889 1.2205 0.053 Uiso 0.47(2) 1 calc PR A 2 C21A C 0.7551(14) 0.6417(15) 1.0766(14) 0.035(7) Uiso 0.47(2) 1 d PG A 2 H21A H 0.8315 0.6416 1.1025 0.043 Uiso 0.47(2) 1 calc PR A 2 C31A C 0.8727(14) 0.8456(15) 0.5285(14) 0.021(7) Uiso 0.50(4) 1 d PG B 2 C32A C 0.8793(16) 0.9483(13) 0.5778(13) 0.029(8) Uiso 0.50(4) 1 d PG B 2 H32A H 0.913 0.9767 0.6525 0.035 Uiso 0.50(4) 1 calc PR B 2 C33A C 0.8365(17) 1.0095(11) 0.5179(16) 0.040(8) Uiso 0.50(4) 1 d PG B 2 H33A H 0.841 1.0797 0.5516 0.048 Uiso 0.50(4) 1 calc PR B 2 C34A C 0.7871(15) 0.9680(16) 0.4086(16) 0.042(8) Uiso 0.50(4) 1 d PG B 2 H34A H 0.7579 1.0098 0.3676 0.05 Uiso 0.50(4) 1 calc PR B 2 C35A C 0.7806(17) 0.8652(19) 0.3593(12) 0.044(8) Uiso 0.50(4) 1 d PG B 2 H35A H 0.7469 0.8368 0.2846 0.053 Uiso 0.50(4) 1 calc PR B 2 C36A C 0.8234(18) 0.8040(17) 0.4193(13) 0.026(7) Uiso 0.50(4) 1 d PG B 2 H36A H 0.8189 0.7338 0.3856 0.031 Uiso 0.50(4) 1 calc PR B 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 Yb 0.0365(3) 0.0393(4) 0.0352(4) 0.0187(3) 0.0181(3) 0.0086(2) Si1 0.041(2) 0.040(2) 0.032(2) 0.0092(17) 0.0209(17) 0.0056(17) Si2 0.049(2) 0.036(2) 0.043(2) 0.0168(18) 0.0238(19) 0.0124(18) Si3 0.0283(18) 0.056(2) 0.037(2) 0.0227(19) 0.0111(17) 0.0075(18) Si4 0.0344(19) 0.043(2) 0.029(2) 0.0156(17) 0.0067(16) 0.0090(17) N1 0.034(5) 0.039(6) 0.020(5) 0.007(5) 0.013(5) 0.000(5) N2 0.042(6) 0.040(6) 0.029(6) 0.012(5) 0.019(5) 0.004(5) N3 0.030(6) 0.059(7) 0.071(8) 0.042(7) 0.018(6) 0.010(6) N4 0.036(6) 0.032(6) 0.026(6) 0.015(5) 0.012(5) 0.007(5) C1 0.035(7) 0.045(8) 0.032(7) 0.017(7) 0.014(6) 0.009(6) C2 0.038(7) 0.036(8) 0.028(7) 0.007(6) 0.014(6) -0.001(6) C3 0.032(7) 0.044(8) 0.015(6) 0.005(6) 0.005(5) 0.001(6) C4 0.052(8) 0.053(9) 0.016(7) 0.003(6) 0.007(6) 0.005(7) C5 0.053(8) 0.054(9) 0.065(10) 0.014(8) 0.038(8) 0.013(7) C6 0.072(10) 0.045(9) 0.035(8) 0.008(7) 0.023(7) 0.005(8) C7 0.19(2) 0.057(12) 0.048(11) -0.002(9) -0.016(13) 0.039(13) C8 0.134(18) 0.117(18) 0.083(15) -0.020(13) -0.015(14) 0.079(16) C9 0.27(3) 0.035(11) 0.30(4) -0.004(16) 0.25(3) 0.014(15) C22 0.035(8) 0.065(10) 0.055(9) 0.039(8) 0.019(7) 0.011(7) C23 0.029(7) 0.058(9) 0.074(10) 0.044(8) 0.023(7) -0.001(7) C24 0.028(6) 0.055(8) 0.031(7) 0.025(7) 0.016(6) 0.019(6) C25 0.039(8) 0.057(9) 0.043(9) 0.023(8) 0.002(7) -0.014(7) C26 0.079(11) 0.119(15) 0.040(9) 0.041(10) 0.027(8) 0.035(11) C27 0.047(8) 0.073(11) 0.056(10) 0.024(9) 0.008(8) 0.015(8) C28 0.040(7) 0.061(9) 0.027(7) 0.018(7) 0.000(6) 0.018(7) C29 0.039(7) 0.051(9) 0.062(10) 0.023(8) 0.021(7) 0.010(7) C30 0.058(8) 0.048(8) 0.028(7) 0.013(7) 0.017(7) 0.015(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Yb N3 2.396(10) . ? Yb N4 2.405(9) . ? Yb N2 2.418(9) . ? Yb N1 2.423(9) . ? Si1 N1 1.738(10) . ? Si1 C5 1.851(14) . ? Si1 C6 1.878(12) . ? Si1 C4 1.879(12) . ? Si2 N2 1.738(11) . ? Si2 C9 1.845(18) . ? Si2 C8 1.845(18) . ? Si2 C7 1.852(17) . ? Si3 N3 1.751(10) . ? Si3 C27 1.851(15) . ? Si3 C25 1.857(12) . ? Si3 C26 1.859(15) . ? Si4 N4 1.737(10) . ? Si4 C29 1.871(14) . ? Si4 C30 1.876(13) . ? Si4 C28 1.890(12) . ? N1 C1 1.323(14) . ? N2 C3 1.323(14) . ? N3 C22 1.347(15) . ? N4 C24 1.311(14) . ? C1 C2 1.416(17) . ? C1 C10 1.512(13) . ? C2 C3 1.398(17) . ? C3 C16A 1.500(17) . ? C3 C16 1.545(16) . ? C10 C11 1.39 . ? C10 C15 1.39 . ? C11 C12 1.39 . ? C12 C13 1.39 . ? C13 C14 1.39 . ? C14 C15 1.39 . ? C22 C23 1.406(17) . ? C22 C31A 1.480(16) . ? C22 C31 1.571(19) . ? C23 C24 1.427(16) . ? C24 C37 1.524(12) . ? C37 C38 1.39 . ? C37 C42 1.39 . ? C38 C39 1.39 . ? C39 C40 1.39 . ? C40 C41 1.39 . ? C41 C42 1.39 . ? C16 C17 1.39 . ? C16 C21 1.39 . ? C17 C18 1.39 . ? C18 C19 1.39 . ? C19 C20 1.39 . ? C20 C21 1.39 . ? C31 C32 1.39 . ? C31 C36 1.39 . ? C32 C33 1.39 . ? C33 C34 1.39 . ? C34 C35 1.39 . ? C35 C36 1.39 . ? C16A C17A 1.39 . ? C16A C21A 1.39 . ? C17A C18A 1.39 . ? C18A C19A 1.39 . ? C19A C20A 1.39 . ? C20A C21A 1.39 . ? C31A C32A 1.39 . ? C31A C36A 1.39 . ? C32A C33A 1.39 . ? C33A C34A 1.39 . ? C34A C35A 1.39 . ? C35A C36A 1.39 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Yb N4 85.4(3) . . ? N3 Yb N2 114.0(4) . . ? N4 Yb N2 123.6(3) . . ? N3 Yb N1 128.2(3) . . ? N4 Yb N1 124.0(3) . . ? N2 Yb N1 86.0(3) . . ? N1 Si1 C5 115.5(6) . . ? N1 Si1 C6 104.5(6) . . ? C5 Si1 C6 105.2(6) . . ? N1 Si1 C4 113.9(5) . . ? C5 Si1 C4 110.0(6) . . ? C6 Si1 C4 106.8(6) . . ? N2 Si2 C9 104.4(6) . . ? N2 Si2 C8 116.6(8) . . ? C9 Si2 C8 106.2(13) . . ? N2 Si2 C7 115.7(7) . . ? C9 Si2 C7 107.0(13) . . ? C8 Si2 C7 106.3(10) . . ? N3 Si3 C27 116.5(6) . . ? N3 Si3 C25 103.8(5) . . ? C27 Si3 C25 106.5(7) . . ? N3 Si3 C26 113.6(7) . . ? C27 Si3 C26 108.9(7) . . ? C25 Si3 C26 106.7(7) . . ? N4 Si4 C29 110.7(6) . . ? N4 Si4 C30 115.8(5) . . ? C29 Si4 C30 111.2(6) . . ? N4 Si4 C28 104.9(5) . . ? C29 Si4 C28 107.6(6) . . ? C30 Si4 C28 106.0(6) . . ? C1 N1 Si1 127.9(8) . . ? C1 N1 Yb 121.6(8) . . ? Si1 N1 Yb 109.8(4) . . ? C3 N2 Si2 127.2(8) . . ? C3 N2 Yb 120.3(8) . . ? Si2 N2 Yb 112.3(4) . . ? C22 N3 Si3 125.1(9) . . ? C22 N3 Yb 122.1(8) . . ? Si3 N3 Yb 111.9(5) . . ? C24 N4 Si4 126.6(8) . . ? C24 N4 Yb 121.5(7) . . ? Si4 N4 Yb 110.3(4) . . ? N1 C1 C2 127.4(11) . . ? N1 C1 C10 119.3(10) . . ? C2 C1 C10 113.3(9) . . ? C3 C2 C1 134.3(11) . . ? N2 C3 C2 129.1(11) . . ? N2 C3 C16A 120.4(12) . . ? C2 C3 C16A 110.2(12) . . ? N2 C3 C16 117.0(11) . . ? C2 C3 C16 113.6(11) . . ? C16A C3 C16 12.5(10) . . ? C11 C10 C15 120 . . ? C11 C10 C1 120.4(6) . . ? C15 C10 C1 119.5(6) . . ? C12 C11 C10 120 . . ? C13 C12 C11 120 . . ? C12 C13 C14 120 . . ? C15 C14 C13 120 . . ? C14 C15 C10 120 . . ? N3 C22 C23 126.6(11) . . ? N3 C22 C31A 118.5(12) . . ? C23 C22 C31A 114.7(12) . . ? N3 C22 C31 121.2(12) . . ? C23 C22 C31 111.0(12) . . ? C31A C22 C31 16.8(9) . . ? C22 C23 C24 133.6(11) . . ? N4 C24 C23 128.1(10) . . ? N4 C24 C37 120.8(9) . . ? C23 C24 C37 111.1(9) . . ? C38 C37 C42 120 . . ? C38 C37 C24 119.8(7) . . ? C42 C37 C24 120.2(7) . . ? C37 C38 C39 120 . . ? C38 C39 C40 120 . . ? C39 C40 C41 120 . . ? C42 C41 C40 120 . . ? C41 C42 C37 120 . . ? C17 C16 C21 120 . . ? C17 C16 C3 122.1(12) . . ? C21 C16 C3 117.9(12) . . ? C16 C17 C18 120 . . ? C17 C18 C19 120 . . ? C20 C19 C18 120 . . ? C19 C20 C21 120 . . ? C20 C21 C16 120 . . ? C32 C31 C36 120 . . ? C32 C31 C22 125.9(14) . . ? C36 C31 C22 113.8(14) . . ? C31 C32 C33 120 . . ? C34 C33 C32 120 . . ? C35 C34 C33 120 . . ? C34 C35 C36 120 . . ? C35 C36 C31 120 . . ? C17A C16A C21A 120 . . ? C17A C16A C3 117.5(13) . . ? C21A C16A C3 122.4(13) . . ? C18A C17A C16A 120 . . ? C17A C18A C19A 120 . . ? C18A C19A C20A 120 . . ? C19A C20A C21A 120 . . ? C20A C21A C16A 120 . . ? C32A C31A C36A 120 . . ? C32A C31A C22 111.8(12) . . ? C36A C31A C22 128.0(12) . . ? C31A C32A C33A 120 . . ? C34A C33A C32A 120 . . ? C33A C34A C35A 120 . . ? C36A C35A C34A 120 . . ? C35A C36A C31A 120 . . ? data_jul701 _database_code_CSD 192428 _audit_creation_date 2001-07-05T13:39:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Yb{Me3SiNC(C6H4Ph)CHC(C6H4Ph)NSiMe3)}2]]' ; _chemical_formula_moiety 'C66 H74 N4 Si4 Yb1' _chemical_formula_sum 'C66 H74 N4 Si4 Yb' _chemical_formula_weight 1208.69 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 12.1373(3) _cell_length_b 22.1348(5) _cell_length_c 23.2872(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6256.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28940 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.613 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.508 _exptl_absorpt_correction_T_max 0.530 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 38043 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_av_unetI/netI 0.0637 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 13613 _reflns_number_gt 10281 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0266P)^2^+3.2824P] 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_number_reflns 13613 _refine_ls_number_parameters 676 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.030(7) _refine_diff_density_max 0.921 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.075 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Yb Yb -0.385 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Yb Yb 0.507053(14) 0.457186(8) 0.118502(19) 0.03325(6) Uani 1 1 d . . . Si1 Si 0.77782(11) 0.48623(8) 0.14260(6) 0.0403(4) Uani 1 1 d . . . Si2 Si 0.25588(11) 0.43235(7) 0.18568(6) 0.0392(3) Uani 1 1 d . . . Si3 Si 0.52621(11) 0.31270(6) 0.06125(6) 0.0353(3) Uani 1 1 d . . . Si4 Si 0.45677(15) 0.60824(9) 0.08266(7) 0.0457(4) Uani 1 1 d . . . N1 N 0.6617(3) 0.46646(18) 0.18188(16) 0.0342(9) Uani 1 1 d . . . N2 N 0.3979(3) 0.43584(19) 0.20125(15) 0.0374(10) Uani 1 1 d . . . N3 N 0.4860(3) 0.38530(18) 0.04255(15) 0.0329(9) Uani 1 1 d . . . N4 N 0.4600(3) 0.53634(18) 0.05213(16) 0.0364(9) Uani 1 1 d . . . C1 C 0.6446(4) 0.4715(2) 0.23815(19) 0.0338(11) Uani 1 1 d . . . C2 C 0.5492(4) 0.4559(2) 0.2692(2) 0.0368(12) Uani 1 1 d . . . H2 H 0.5599 0.457 0.3095 0.044 Uiso 1 1 calc R . . C3 C 0.4417(5) 0.4390(3) 0.2536(2) 0.0389(13) Uani 1 1 d . . . C4 C 0.7330(4) 0.4977(2) 0.27664(18) 0.0335(11) Uani 1 1 d . . . C5 C 0.7086(4) 0.5510(2) 0.3059(2) 0.0413(13) Uani 1 1 d . . . H5 H 0.6391 0.57 0.3004 0.05 Uiso 1 1 calc R . . C6 C 0.7851(4) 0.5766(3) 0.3430(2) 0.0432(14) Uani 1 1 d . . . H6 H 0.768 0.6132 0.3623 0.052 Uiso 1 1 calc R . . C7 C 0.8863(4) 0.5489(2) 0.35209(19) 0.0344(11) Uani 1 1 d . . . C8 C 0.9108(4) 0.4967(2) 0.32225(19) 0.0355(12) Uani 1 1 d . . . H8 H 0.9805 0.4779 0.3273 0.043 Uiso 1 1 calc R . . C9 C 0.8341(4) 0.4713(2) 0.28469(18) 0.0335(11) Uani 1 1 d . . . H9 H 0.8521 0.4354 0.2645 0.04 Uiso 1 1 calc R . . C10 C 0.9643(4) 0.5750(2) 0.3945(2) 0.0395(12) Uani 1 1 d . . . C11 C 1.0752(4) 0.5815(3) 0.3827(3) 0.0532(15) Uani 1 1 d . . . H11 H 1.1031 0.5701 0.3461 0.064 Uiso 1 1 calc R . . C12 C 1.1473(5) 0.6051(3) 0.4249(3) 0.0643(18) Uani 1 1 d . . . H12 H 1.2235 0.6095 0.4166 0.077 Uiso 1 1 calc R . . C13 C 1.1076(5) 0.6218(3) 0.4777(3) 0.0601(17) Uani 1 1 d . . . H13 H 1.1562 0.6379 0.5058 0.072 Uiso 1 1 calc R . . C14 C 0.9981(5) 0.6152(3) 0.4899(2) 0.0564(16) Uani 1 1 d . . . H14 H 0.9706 0.6262 0.5266 0.068 Uiso 1 1 calc R . . C15 C 0.9270(5) 0.5923(3) 0.4484(2) 0.0474(14) Uani 1 1 d . . . H15 H 0.8509 0.5885 0.4572 0.057 Uiso 1 1 calc R . . C16 C 0.3707(4) 0.4239(2) 0.30509(17) 0.0312(11) Uani 1 1 d . . . C17 C 0.3270(4) 0.3668(2) 0.31217(19) 0.0384(12) Uani 1 1 d . . . H17 H 0.3426 0.3366 0.2843 0.046 Uiso 1 1 calc R . . C18 C 0.2612(4) 0.3523(2) 0.35866(19) 0.0405(12) Uani 1 1 d . . . H18 H 0.2334 0.3124 0.3626 0.049 Uiso 1 1 calc R . . C19 C 0.2354(4) 0.3958(2) 0.3997(2) 0.0360(12) Uani 1 1 d . . . C20 C 0.2801(4) 0.4528(2) 0.3938(2) 0.0388(12) Uani 1 1 d . . . H20 H 0.2646 0.4829 0.4217 0.047 Uiso 1 1 calc R . . C21 C 0.3478(4) 0.4663(2) 0.3474(2) 0.0403(12) Uani 1 1 d . . . H21 H 0.3791 0.5055 0.3446 0.048 Uiso 1 1 calc R . . C22 C 0.1575(4) 0.3809(3) 0.44807(19) 0.0404(13) Uani 1 1 d . . . C23 C 0.1553(5) 0.3238(3) 0.4710(2) 0.0616(17) Uani 1 1 d . . . H23 H 0.2036 0.2934 0.4571 0.074 Uiso 1 1 calc R . . C24 C 0.0798(7) 0.3110(4) 0.5157(3) 0.085(2) Uani 1 1 d . . . H24 H 0.0773 0.2715 0.5315 0.102 Uiso 1 1 calc R . . C25 C 0.0114(5) 0.3538(5) 0.5363(3) 0.079(3) Uani 1 1 d . . . H25 H -0.0395 0.3442 0.5659 0.095 Uiso 1 1 calc R . . C26 C 0.0154(4) 0.4108(4) 0.5147(2) 0.068(2) Uani 1 1 d . . . H26 H -0.0313 0.4412 0.53 0.082 Uiso 1 1 calc R . . C27 C 0.0878(4) 0.4248(3) 0.4699(2) 0.0513(15) Uani 1 1 d . . . H27 H 0.0892 0.4645 0.4544 0.062 Uiso 1 1 calc R . . C28 C 0.8900(4) 0.4278(3) 0.1440(2) 0.0555(16) Uani 1 1 d . . . H28A H 0.8587 0.3881 0.1352 0.083 Uiso 1 1 calc R . . H28B H 0.9236 0.4268 0.1823 0.083 Uiso 1 1 calc R . . H28C H 0.9462 0.438 0.1154 0.083 Uiso 1 1 calc R . . C29 C 0.8352(5) 0.5618(3) 0.1597(2) 0.0696(19) Uani 1 1 d . . . H29A H 0.7759 0.5918 0.1589 0.104 Uiso 1 1 calc R . . H29B H 0.8913 0.5725 0.1312 0.104 Uiso 1 1 calc R . . H29C H 0.8686 0.5609 0.198 0.104 Uiso 1 1 calc R . . C30 C 0.7283(4) 0.4869(3) 0.06566(19) 0.0436(13) Uani 1 1 d . . . H30A H 0.6979 0.4472 0.0559 0.065 Uiso 1 1 calc R . . H30B H 0.7903 0.4961 0.0401 0.065 Uiso 1 1 calc R . . H30C H 0.6711 0.5178 0.0611 0.065 Uiso 1 1 calc R . . C31 C 0.1928(5) 0.3558(3) 0.1864(3) 0.0608(16) Uani 1 1 d . . . H31A H 0.2373 0.3284 0.1629 0.091 Uiso 1 1 calc R . . H31B H 0.118 0.358 0.1708 0.091 Uiso 1 1 calc R . . H31C H 0.19 0.3407 0.2259 0.091 Uiso 1 1 calc R . . C32 C 0.1728(5) 0.4844(3) 0.2308(3) 0.073(2) Uani 1 1 d . . . H32A H 0.2062 0.5247 0.2303 0.11 Uiso 1 1 calc R . . H32B H 0.1707 0.4693 0.2704 0.11 Uiso 1 1 calc R . . H32C H 0.0976 0.4867 0.2156 0.11 Uiso 1 1 calc R . . C33 C 0.2431(4) 0.4578(3) 0.1091(3) 0.0690(19) Uani 1 1 d . . . H33A H 0.2861 0.4309 0.0843 0.103 Uiso 1 1 calc R . . H33B H 0.2711 0.4992 0.1055 0.103 Uiso 1 1 calc R . . H33C H 0.1656 0.4566 0.0975 0.103 Uiso 1 1 calc R . . C34 C 0.4569(4) 0.4059(3) -0.00960(19) 0.0363(12) Uani 1 1 d . . . C35 C 0.4301(5) 0.4644(2) -0.0271(2) 0.0377(14) Uani 1 1 d . . . H35 H 0.4079 0.466 -0.0662 0.045 Uiso 1 1 calc R . . C36 C 0.4281(4) 0.5215(2) -0.00056(19) 0.0360(11) Uani 1 1 d . . . C37 C 0.4452(4) 0.3602(2) -0.05772(18) 0.0322(11) Uani 1 1 d . . . C38 C 0.5141(4) 0.3641(2) -0.1060(2) 0.0437(13) Uani 1 1 d . . . H38 H 0.5692 0.3945 -0.1076 0.052 Uiso 1 1 calc R . . C39 C 0.5024(4) 0.3238(3) -0.1513(2) 0.0488(14) Uani 1 1 d . . . H39 H 0.5502 0.3266 -0.1835 0.059 Uiso 1 1 calc R . . C40 C 0.4215(5) 0.2793(3) -0.1501(2) 0.0460(13) Uani 1 1 d . . . C41 C 0.3532(4) 0.2759(2) -0.1023(2) 0.0449(13) Uani 1 1 d . . . H41 H 0.2976 0.2457 -0.1007 0.054 Uiso 1 1 calc R . . C42 C 0.3650(4) 0.3155(2) -0.0574(2) 0.0392(12) Uani 1 1 d . . . H42 H 0.317 0.3123 -0.0253 0.047 Uiso 1 1 calc R . . C43 C 0.4080(5) 0.2368(3) -0.1997(2) 0.0590(17) Uani 1 1 d . . . C44 C 0.3081(8) 0.2167(5) -0.2156(4) 0.120(4) Uani 1 1 d . . . H44 H 0.2452 0.2289 -0.1943 0.144 Uiso 1 1 calc R . . C45 C 0.2946(10) 0.1782(6) -0.2624(4) 0.167(5) Uani 1 1 d . . . H45 H 0.2226 0.1661 -0.2735 0.2 Uiso 1 1 calc R . . C46 C 0.3835(11) 0.1579(5) -0.2923(4) 0.130(4) Uani 1 1 d . . . H46 H 0.3757 0.133 -0.3252 0.156 Uiso 1 1 calc R . . C47 C 0.4797(11) 0.1744(6) -0.2732(5) 0.156(6) Uani 1 1 d . . . H47 H 0.5436 0.1592 -0.2918 0.188 Uiso 1 1 calc R . . C48 C 0.4928(8) 0.2129(5) -0.2274(4) 0.124(4) Uani 1 1 d . . . H48 H 0.5653 0.2226 -0.2152 0.149 Uiso 1 1 calc R . . C49 C 0.3720(4) 0.5679(2) -0.03848(18) 0.0359(11) Uani 1 1 d . . . C50 C 0.4288(4) 0.6097(2) -0.0714(2) 0.0382(12) Uani 1 1 d . . . H50 H 0.5065 0.6133 -0.0678 0.046 Uiso 1 1 calc R . . C51 C 0.3718(4) 0.6466(2) -0.1098(2) 0.0400(12) Uani 1 1 d . . . H51 H 0.4115 0.6749 -0.1324 0.048 Uiso 1 1 calc R . . C52 C 0.2588(4) 0.6428(2) -0.11547(19) 0.0375(12) Uani 1 1 d . . . C53 C 0.2018(4) 0.6013(3) -0.0808(2) 0.0427(13) Uani 1 1 d . . . H53 H 0.1238 0.5992 -0.0827 0.051 Uiso 1 1 calc R . . C54 C 0.2580(4) 0.5637(3) -0.0442(2) 0.0417(12) Uani 1 1 d . . . H54 H 0.2187 0.5344 -0.0225 0.05 Uiso 1 1 calc R . . C55 C 0.1956(4) 0.6765(2) -0.1605(2) 0.0360(11) Uani 1 1 d . . . C56 C 0.2401(4) 0.6844(2) -0.21473(19) 0.0384(12) Uani 1 1 d . . . H56 H 0.3139 0.6726 -0.2221 0.046 Uiso 1 1 calc R . . C57 C 0.1769(5) 0.7098(2) -0.2585(2) 0.0446(13) Uani 1 1 d . . . H57 H 0.2092 0.7166 -0.2951 0.053 Uiso 1 1 calc R . . C58 C 0.0680(5) 0.7251(2) -0.2493(2) 0.0465(13) Uani 1 1 d . . . H58 H 0.0247 0.7412 -0.2797 0.056 Uiso 1 1 calc R . . C59 C 0.0228(4) 0.7169(3) -0.1956(2) 0.0478(14) Uani 1 1 d . . . H59 H -0.0518 0.7276 -0.1887 0.057 Uiso 1 1 calc R . . C60 C 0.0863(4) 0.6927(2) -0.1513(2) 0.0421(12) Uani 1 1 d . . . H60 H 0.0546 0.6873 -0.1144 0.051 Uiso 1 1 calc R . . C61 C 0.6176(4) 0.2735(3) 0.0084(2) 0.0507(14) Uani 1 1 d . . . H61A H 0.5781 0.2682 -0.028 0.076 Uiso 1 1 calc R . . H61B H 0.6387 0.2338 0.0236 0.076 Uiso 1 1 calc R . . H61C H 0.6839 0.2978 0.0019 0.076 Uiso 1 1 calc R . . C62 C 0.4089(4) 0.2611(2) 0.0796(2) 0.0433(13) Uani 1 1 d . . . H62A H 0.3638 0.2542 0.0453 0.065 Uiso 1 1 calc R . . H62B H 0.3635 0.2797 0.1096 0.065 Uiso 1 1 calc R . . H62C H 0.4379 0.2225 0.0935 0.065 Uiso 1 1 calc R . . C63 C 0.6046(5) 0.3216(2) 0.1301(2) 0.0598(17) Uani 1 1 d . . . H63A H 0.558 0.342 0.1586 0.09 Uiso 1 1 calc R . . H63B H 0.6709 0.3458 0.1232 0.09 Uiso 1 1 calc R . . H63C H 0.6258 0.2817 0.1447 0.09 Uiso 1 1 calc R . . C64 C 0.4775(6) 0.5956(4) 0.1614(3) 0.063(2) Uani 1 1 d . . . H64A H 0.4179 0.5703 0.1764 0.094 Uiso 1 1 calc R . . H64B H 0.4772 0.6346 0.1814 0.094 Uiso 1 1 calc R . . H64C H 0.5483 0.5755 0.1678 0.094 Uiso 1 1 calc R . . C65 C 0.3223(5) 0.6487(3) 0.0750(3) 0.0612(16) Uani 1 1 d . . . H65A H 0.2625 0.6225 0.0885 0.092 Uiso 1 1 calc R . . H65B H 0.3102 0.6589 0.0346 0.092 Uiso 1 1 calc R . . H65C H 0.3237 0.6858 0.098 0.092 Uiso 1 1 calc R . . C66 C 0.5734(5) 0.6570(3) 0.0573(3) 0.0613(16) Uani 1 1 d . . . H66A H 0.6431 0.635 0.0616 0.092 Uiso 1 1 calc R . . H66B H 0.5759 0.6941 0.0802 0.092 Uiso 1 1 calc R . . H66C H 0.5623 0.6673 0.0168 0.092 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 Yb 0.03121(9) 0.04422(10) 0.02430(8) -0.00072(15) -0.00228(12) -0.00168(9) Si1 0.0294(8) 0.0613(10) 0.0302(6) -0.0036(7) 0.0041(5) -0.0106(7) Si2 0.0257(7) 0.0542(9) 0.0378(7) -0.0010(7) 0.0001(5) -0.0015(7) Si3 0.0322(7) 0.0387(8) 0.0349(7) 0.0051(6) -0.0055(5) -0.0003(6) Si4 0.0469(9) 0.0443(10) 0.0459(9) -0.0067(7) -0.0056(8) 0.0032(9) N1 0.022(2) 0.049(3) 0.032(2) -0.0017(18) 0.0014(15) -0.0026(18) N2 0.027(2) 0.056(3) 0.029(2) -0.0047(19) 0.0003(15) 0.0018(19) N3 0.034(2) 0.036(2) 0.029(2) 0.0009(16) -0.0028(15) 0.0002(18) N4 0.035(2) 0.040(3) 0.035(2) -0.0017(19) -0.0010(17) 0.0006(18) C1 0.029(3) 0.044(3) 0.028(2) -0.004(2) -0.0004(18) -0.002(2) C2 0.028(2) 0.063(4) 0.020(2) -0.003(2) 0.0001(18) -0.003(3) C3 0.029(3) 0.053(4) 0.035(3) -0.004(3) 0.005(2) 0.001(3) C4 0.027(3) 0.051(3) 0.022(2) -0.008(2) 0.0021(17) -0.006(2) C5 0.026(3) 0.056(4) 0.042(3) -0.009(3) -0.006(2) 0.007(2) C6 0.034(3) 0.059(4) 0.036(3) -0.019(3) -0.004(2) 0.008(3) C7 0.028(3) 0.043(3) 0.032(2) -0.005(2) -0.0017(18) -0.005(2) C8 0.024(3) 0.045(3) 0.037(3) -0.004(2) 0.0011(19) 0.003(2) C9 0.033(3) 0.043(3) 0.025(2) -0.009(2) 0.0003(18) -0.002(2) C10 0.035(3) 0.037(3) 0.047(3) -0.005(2) -0.005(2) 0.002(2) C11 0.038(3) 0.058(4) 0.064(4) -0.022(3) 0.003(3) -0.008(3) C12 0.034(3) 0.063(4) 0.096(5) -0.006(4) -0.015(3) -0.005(3) C13 0.057(4) 0.055(4) 0.069(4) -0.015(3) -0.029(3) -0.002(3) C14 0.067(4) 0.061(4) 0.041(3) -0.014(3) -0.018(3) 0.004(3) C15 0.043(3) 0.057(4) 0.042(3) -0.008(3) -0.007(2) -0.004(3) C16 0.025(2) 0.046(3) 0.022(2) -0.002(2) 0.0014(17) -0.002(2) C17 0.040(3) 0.040(3) 0.036(3) -0.010(2) 0.001(2) 0.004(2) C18 0.042(3) 0.036(3) 0.043(3) 0.004(2) 0.001(2) -0.008(2) C19 0.023(3) 0.046(3) 0.039(3) -0.002(2) 0.002(2) -0.001(2) C20 0.036(3) 0.045(3) 0.036(3) -0.006(2) 0.007(2) 0.001(3) C21 0.035(3) 0.047(3) 0.038(3) -0.009(2) 0.008(2) -0.011(2) C22 0.032(3) 0.061(4) 0.029(3) 0.001(2) -0.0022(19) -0.011(3) C23 0.061(4) 0.073(5) 0.051(4) 0.018(3) 0.004(3) -0.011(3) C24 0.073(5) 0.111(7) 0.072(5) 0.044(5) 0.002(4) -0.030(5) C25 0.047(4) 0.143(8) 0.048(4) 0.022(5) 0.010(3) -0.022(5) C26 0.027(3) 0.140(7) 0.039(3) -0.009(4) 0.001(2) -0.006(4) C27 0.034(3) 0.090(5) 0.030(3) -0.002(3) -0.002(2) -0.009(3) C28 0.027(3) 0.097(5) 0.042(3) -0.004(3) 0.003(2) 0.003(3) C29 0.070(4) 0.087(5) 0.052(4) -0.003(3) 0.005(3) -0.038(4) C30 0.038(3) 0.063(4) 0.030(3) 0.000(2) 0.008(2) -0.004(3) C31 0.043(3) 0.073(4) 0.066(4) 0.001(3) -0.007(3) -0.011(3) C32 0.038(4) 0.101(5) 0.081(5) -0.028(4) -0.008(3) 0.011(4) C33 0.033(3) 0.118(5) 0.056(4) 0.019(4) -0.010(3) -0.010(3) C34 0.027(3) 0.051(4) 0.031(3) -0.007(2) -0.0002(19) -0.003(3) C35 0.043(3) 0.038(4) 0.032(3) 0.003(2) -0.007(2) 0.005(3) C36 0.025(3) 0.045(3) 0.038(3) 0.006(2) -0.0002(19) -0.004(2) C37 0.039(3) 0.032(3) 0.026(2) -0.002(2) -0.0040(19) 0.006(2) C38 0.044(3) 0.045(3) 0.042(3) -0.001(2) -0.004(2) -0.005(3) C39 0.052(4) 0.056(4) 0.038(3) -0.008(2) 0.004(2) 0.006(3) C40 0.048(3) 0.047(3) 0.043(3) -0.009(3) -0.011(2) 0.009(3) C41 0.047(3) 0.042(3) 0.045(3) -0.003(3) -0.012(2) -0.005(3) C42 0.039(3) 0.048(3) 0.030(2) 0.002(2) -0.005(2) -0.001(3) C43 0.061(4) 0.066(4) 0.050(3) -0.025(3) -0.006(3) 0.011(3) C44 0.090(7) 0.172(10) 0.098(6) -0.072(6) -0.004(5) -0.008(6) C45 0.152(11) 0.232(14) 0.116(8) -0.115(9) -0.017(7) -0.022(9) C46 0.178(12) 0.126(8) 0.087(6) -0.067(6) 0.004(7) -0.022(8) C47 0.139(10) 0.167(12) 0.163(11) -0.127(10) 0.000(8) 0.022(8) C48 0.115(8) 0.133(9) 0.124(7) -0.086(7) -0.025(6) 0.037(6) C49 0.042(3) 0.036(3) 0.029(2) -0.002(2) 0.000(2) 0.003(2) C50 0.028(3) 0.044(3) 0.042(3) 0.006(2) 0.004(2) -0.001(2) C51 0.036(3) 0.040(3) 0.044(3) 0.011(2) 0.005(2) 0.000(2) C52 0.038(3) 0.042(3) 0.032(2) 0.002(2) 0.001(2) 0.001(2) C53 0.033(3) 0.061(4) 0.035(3) 0.006(2) 0.005(2) -0.001(3) C54 0.041(3) 0.050(3) 0.035(3) 0.010(2) 0.001(2) -0.007(3) C55 0.033(3) 0.035(3) 0.040(3) -0.001(2) 0.000(2) 0.000(2) C56 0.036(3) 0.036(3) 0.043(3) 0.008(2) 0.004(2) -0.001(2) C57 0.052(4) 0.041(3) 0.041(3) 0.006(2) -0.001(2) 0.000(3) C58 0.050(4) 0.042(3) 0.047(3) 0.007(2) -0.010(3) -0.003(3) C59 0.034(3) 0.049(4) 0.060(4) 0.000(3) -0.004(2) 0.007(3) C60 0.038(3) 0.045(3) 0.044(3) 0.004(2) 0.004(2) 0.001(2) C61 0.034(3) 0.053(4) 0.066(3) 0.007(3) 0.004(3) 0.004(3) C62 0.039(3) 0.043(3) 0.048(3) 0.003(2) 0.003(2) -0.004(2) C63 0.078(4) 0.051(3) 0.050(4) 0.004(3) -0.031(3) -0.006(3) C64 0.078(5) 0.066(5) 0.045(4) -0.023(3) -0.004(3) 0.005(4) C65 0.061(4) 0.053(4) 0.070(4) -0.013(3) -0.002(3) 0.011(3) C66 0.059(4) 0.044(4) 0.081(4) 0.007(3) -0.003(3) -0.010(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Yb N2 2.386(4) . ? Yb N3 2.393(4) . ? Yb N1 2.396(4) . ? Yb N4 2.405(4) . ? Si1 N1 1.736(4) . ? Si1 C29 1.854(6) . ? Si1 C28 1.878(6) . ? Si1 C30 1.890(5) . ? Si2 N2 1.764(4) . ? Si2 C32 1.858(6) . ? Si2 C31 1.859(6) . ? Si2 C33 1.877(7) . ? Si3 N3 1.735(4) . ? Si3 C61 1.871(5) . ? Si3 C62 1.874(5) . ? Si3 C63 1.876(5) . ? Si4 N4 1.744(4) . ? Si4 C65 1.870(6) . ? Si4 C64 1.873(6) . ? Si4 C66 1.876(6) . ? N1 C1 1.331(6) . ? N2 C3 1.331(6) . ? N3 C34 1.345(6) . ? N4 C36 1.327(6) . ? C1 C2 1.408(6) . ? C1 C4 1.514(6) . ? C2 C3 1.404(8) . ? C3 C16 1.514(6) . ? C4 C9 1.372(6) . ? C4 C5 1.394(7) . ? C5 C6 1.389(7) . ? C6 C7 1.389(7) . ? C7 C8 1.381(6) . ? C7 C10 1.485(6) . ? C8 C9 1.396(6) . ? C10 C11 1.381(7) . ? C10 C15 1.388(7) . ? C11 C12 1.417(8) . ? C12 C13 1.371(9) . ? C13 C14 1.367(8) . ? C14 C15 1.390(7) . ? C16 C17 1.381(7) . ? C16 C21 1.389(6) . ? C17 C18 1.383(6) . ? C18 C19 1.393(7) . ? C19 C20 1.379(7) . ? C19 C22 1.506(6) . ? C20 C21 1.390(6) . ? C22 C23 1.373(8) . ? C22 C27 1.385(8) . ? C23 C24 1.416(9) . ? C24 C25 1.348(11) . ? C25 C26 1.358(11) . ? C26 C27 1.398(7) . ? C34 C35 1.396(7) . ? C34 C37 1.517(6) . ? C35 C36 1.408(7) . ? C36 C49 1.516(7) . ? C37 C42 1.387(7) . ? C37 C38 1.404(7) . ? C38 C39 1.390(7) . ? C39 C40 1.391(8) . ? C40 C41 1.390(7) . ? C40 C43 1.498(7) . ? C41 C42 1.372(7) . ? C43 C48 1.326(9) . ? C43 C44 1.343(10) . ? C44 C45 1.392(11) . ? C45 C46 1.361(13) . ? C46 C47 1.302(13) . ? C47 C48 1.374(12) . ? C49 C50 1.385(7) . ? C49 C54 1.394(6) . ? C50 C51 1.395(6) . ? C51 C52 1.381(7) . ? C52 C53 1.406(7) . ? C52 C55 1.498(6) . ? C53 C54 1.372(7) . ? C55 C56 1.384(6) . ? C55 C60 1.390(7) . ? C56 C57 1.393(7) . ? C57 C58 1.382(7) . ? C58 C59 1.378(7) . ? C59 C60 1.393(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 N2 Yb N3 113.97(13) . . ? N2 Yb N1 87.38(12) . . ? N3 Yb N1 126.57(13) . . ? N2 Yb N4 122.10(14) . . ? N3 Yb N4 89.08(13) . . ? N1 Yb N4 121.30(13) . . ? N1 Si1 C29 114.8(2) . . ? N1 Si1 C28 113.9(2) . . ? C29 Si1 C28 110.2(3) . . ? N1 Si1 C30 104.1(2) . . ? C29 Si1 C30 108.4(3) . . ? C28 Si1 C30 104.6(2) . . ? N2 Si2 C32 112.8(2) . . ? N2 Si2 C31 116.1(2) . . ? C32 Si2 C31 109.7(3) . . ? N2 Si2 C33 105.2(2) . . ? C32 Si2 C33 107.9(3) . . ? C31 Si2 C33 104.4(3) . . ? N3 Si3 C61 115.5(2) . . ? N3 Si3 C62 114.1(2) . . ? C61 Si3 C62 108.6(2) . . ? N3 Si3 C63 105.1(2) . . ? C61 Si3 C63 108.1(3) . . ? C62 Si3 C63 104.7(2) . . ? N4 Si4 C65 114.7(2) . . ? N4 Si4 C64 105.1(3) . . ? C65 Si4 C64 106.4(3) . . ? N4 Si4 C66 112.3(3) . . ? C65 Si4 C66 110.7(3) . . ? C64 Si4 C66 107.0(3) . . ? C1 N1 Si1 128.6(3) . . ? C1 N1 Yb 119.4(3) . . ? Si1 N1 Yb 109.45(18) . . ? C3 N2 Si2 125.5(3) . . ? C3 N2 Yb 120.5(3) . . ? Si2 N2 Yb 112.66(18) . . ? C34 N3 Si3 128.0(3) . . ? C34 N3 Yb 118.0(3) . . ? Si3 N3 Yb 113.60(17) . . ? C36 N4 Si4 126.6(4) . . ? C36 N4 Yb 118.9(3) . . ? Si4 N4 Yb 114.09(19) . . ? N1 C1 C2 127.8(4) . . ? N1 C1 C4 120.3(4) . . ? C2 C1 C4 111.9(4) . . ? C3 C2 C1 134.2(4) . . ? N2 C3 C2 128.4(5) . . ? N2 C3 C16 119.1(5) . . ? C2 C3 C16 112.5(4) . . ? C9 C4 C5 118.9(4) . . ? C9 C4 C1 123.5(4) . . ? C5 C4 C1 117.6(4) . . ? C6 C5 C4 120.4(5) . . ? C7 C6 C5 120.5(5) . . ? C8 C7 C6 118.8(4) . . ? C8 C7 C10 121.5(4) . . ? C6 C7 C10 119.6(4) . . ? C7 C8 C9 120.6(4) . . ? C4 C9 C8 120.7(4) . . ? C11 C10 C15 118.1(5) . . ? C11 C10 C7 121.9(4) . . ? C15 C10 C7 120.1(5) . . ? C10 C11 C12 120.1(5) . . ? C13 C12 C11 120.3(6) . . ? C14 C13 C12 119.9(5) . . ? C13 C14 C15 119.9(5) . . ? C10 C15 C14 121.7(5) . . ? C17 C16 C21 117.2(4) . . ? C17 C16 C3 121.0(4) . . ? C21 C16 C3 121.8(5) . . ? C16 C17 C18 121.8(4) . . ? C17 C18 C19 120.5(5) . . ? C20 C19 C18 118.3(4) . . ? C20 C19 C22 121.5(5) . . ? C18 C19 C22 120.2(5) . . ? C19 C20 C21 120.5(5) . . ? C16 C21 C20 121.6(5) . . ? C23 C22 C27 119.4(5) . . ? C23 C22 C19 120.3(5) . . ? C27 C22 C19 120.3(5) . . ? C22 C23 C24 118.8(7) . . ? C25 C24 C23 121.4(7) . . ? C24 C25 C26 119.8(6) . . ? C25 C26 C27 120.4(7) . . ? C22 C27 C26 120.1(6) . . ? N3 C34 C35 129.8(5) . . ? N3 C34 C37 117.7(5) . . ? C35 C34 C37 112.4(4) . . ? C34 C35 C36 135.1(5) . . ? N4 C36 C35 128.5(5) . . ? N4 C36 C49 120.2(5) . . ? C35 C36 C49 111.1(4) . . ? C42 C37 C38 117.8(4) . . ? C42 C37 C34 122.5(4) . . ? C38 C37 C34 119.6(4) . . ? C39 C38 C37 120.5(5) . . ? C38 C39 C40 120.8(5) . . ? C41 C40 C39 118.4(5) . . ? C41 C40 C43 121.2(5) . . ? C39 C40 C43 120.4(5) . . ? C42 C41 C40 120.9(5) . . ? C41 C42 C37 121.6(5) . . ? C48 C43 C44 115.7(7) . . ? C48 C43 C40 122.7(6) . . ? C44 C43 C40 121.3(6) . . ? C43 C44 C45 121.7(9) . . ? C46 C45 C44 120.6(10) . . ? C47 C46 C45 116.3(9) . . ? C46 C47 C48 122.8(10) . . ? C43 C48 C47 122.4(9) . . ? C50 C49 C54 119.1(4) . . ? C50 C49 C36 123.5(4) . . ? C54 C49 C36 117.2(4) . . ? C49 C50 C51 119.9(5) . . ? C52 C51 C50 121.3(5) . . ? C51 C52 C53 118.2(4) . . ? C51 C52 C55 123.1(4) . . ? C53 C52 C55 118.4(4) . . ? C54 C53 C52 120.6(5) . . ? C53 C54 C49 120.8(5) . . ? C56 C55 C60 118.7(4) . . ? C56 C55 C52 120.1(4) . . ? C60 C55 C52 120.6(4) . . ? C55 C56 C57 120.2(5) . . ? C58 C57 C56 120.8(5) . . ? C59 C58 C57 119.2(5) . . ? C58 C59 C60 120.2(5) . . ? C55 C60 C59 120.8(5) . . ?