data_feb602 _audit_creation_date 2002-02-14T08:17:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Yb3(thf){Me3SiNCPhCHCPhNSiMe3}3]' _chemical_formula_moiety 'C67 H95 N6 O Si6 Yb3' _chemical_formula_sum 'C67 H95 N6 O Si6 Yb3' _chemical_formula_weight 1688.15 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4823(4) _cell_length_b 16.3546(5) _cell_length_c 20.0818(6) _cell_angle_alpha 65.993(2) _cell_angle_beta 84.086(2) _cell_angle_gamma 86.355(2) _cell_volume 4022.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13654 _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1682 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.587 _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 0.323 _exptl_absorpt_correction_T_max 0.358 #----------------------------------------------------------------------------# # 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_av_R_equivalents 0.0452 _diffrn_reflns_av_unetI/netI 0.0558 _diffrn_reflns_number 29430 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 14142 _reflns_number_gt 11516 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack' _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 ; The centroids of the C25 to C30 , and C4 to C9, rings were included as fixed positions M1 and M2 and for calculating the geometry were assumed to have the same positional esd as the C atoms of the ring. 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^)+(0.0465P)^2^+13.9786P] 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 'riding mode' _refine_ls_extinction_method none _refine_ls_number_reflns 14142 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.419 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.139 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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 Yb1 Yb 0.46224(2) 0.376422(18) 0.185839(14) 0.02880(8) Uani 1 1 d . . . Yb2 Yb 0.38499(2) 0.380346(18) 0.344563(14) 0.02847(8) Uani 1 1 d . . . Yb3 Yb 0.16505(2) 0.234580(18) 0.109586(15) 0.03089(8) Uani 1 1 d . . . Si1 Si 0.57713(16) 0.23322(16) 0.46751(11) 0.0502(6) Uani 1 1 d . A 1 Si2 Si 0.40544(14) 0.58395(12) 0.14958(10) 0.0328(4) Uani 1 1 d . A 1 Si3 Si 0.29845(15) 0.19347(12) 0.34138(10) 0.0372(4) Uani 1 1 d . B 1 Si4 Si 0.20513(15) 0.43367(14) 0.44557(10) 0.0400(5) Uani 1 1 d . B 1 Si5 Si 0.35035(15) 0.04409(13) 0.11168(11) 0.0394(5) Uani 1 1 d . C 1 Si6 Si 0.05777(17) 0.27440(14) -0.06875(11) 0.0449(5) Uani 1 1 d . C 1 O O 0.0060(4) 0.2715(4) 0.1607(3) 0.0577(15) Uani 1 1 d . D 1 N1 N 0.5134(4) 0.2920(4) 0.3925(3) 0.0350(13) Uani 1 1 d . A 1 N2 N 0.4426(4) 0.4991(3) 0.2291(3) 0.0287(11) Uani 1 1 d . A 1 N3 N 0.3366(4) 0.3010(3) 0.2842(3) 0.0301(12) Uani 1 1 d . B 1 N4 N 0.2270(4) 0.4174(4) 0.3658(3) 0.0346(13) Uani 1 1 d . B 1 N5 N 0.2350(4) 0.0925(3) 0.1262(3) 0.0335(12) Uani 1 1 d . C 1 N6 N 0.0753(4) 0.2096(3) 0.0233(3) 0.0356(13) Uani 1 1 d . C 1 C1 C 0.5660(5) 0.3567(5) 0.3283(3) 0.0348(15) Uani 1 1 d . A 1 C2 C 0.5570(5) 0.4486(5) 0.3248(4) 0.0360(15) Uani 1 1 d . A 1 H2 H 0.5931 0.4627 0.3567 0.043 Uiso 1 1 calc R A 1 C3 C 0.4991(5) 0.5153(4) 0.2777(4) 0.0327(14) Uani 1 1 d . A 1 C4 C 0.6066(5) 0.3403(4) 0.2679(3) 0.0328(15) Uani 1 1 d . A 1 C5 C 0.5990(5) 0.2548(5) 0.2636(4) 0.0381(16) Uani 1 1 d . A 1 H5 H 0.584 0.2031 0.3071 0.046 Uiso 1 1 calc R A 1 C6 C 0.6133(6) 0.2469(5) 0.1971(4) 0.0449(18) Uani 1 1 d . A 1 H6 H 0.6058 0.1901 0.196 0.054 Uiso 1 1 calc R A 1 C7 C 0.6382(6) 0.3193(5) 0.1321(4) 0.0461(19) Uani 1 1 d . A 1 H7 H 0.6403 0.3144 0.0864 0.055 Uiso 1 1 calc R A 1 C8 C 0.6603(5) 0.3999(5) 0.1355(4) 0.0396(17) Uani 1 1 d . A 1 H8 H 0.6853 0.448 0.0924 0.048 Uiso 1 1 calc R A 1 C9 C 0.6461(5) 0.4105(5) 0.2009(4) 0.0373(16) Uani 1 1 d . A 1 H9 H 0.6629 0.4657 0.2017 0.045 Uiso 1 1 calc R A 1 C10 C 0.4880(6) 0.6023(5) 0.2850(4) 0.0418(17) Uani 1 1 d . A 1 C11 C 0.5723(8) 0.6472(6) 0.2865(5) 0.072(3) Uani 1 1 d . A 1 H11 H 0.6374 0.6234 0.2816 0.087 Uiso 1 1 calc R A 1 C12 C 0.5584(13) 0.7285(8) 0.2954(7) 0.109(5) Uani 1 1 d . A 1 H12 H 0.6148 0.7599 0.2964 0.13 Uiso 1 1 calc R A 1 C13 C 0.4632(14) 0.7631(8) 0.3026(6) 0.100(5) Uani 1 1 d . A 1 H13 H 0.4539 0.8178 0.3087 0.12 Uiso 1 1 calc R A 1 C14 C 0.3868(10) 0.7195(6) 0.3009(5) 0.074(3) Uani 1 1 d . A 1 H14 H 0.3218 0.7436 0.3056 0.089 Uiso 1 1 calc R A 1 C15 C 0.3960(7) 0.6395(5) 0.2925(4) 0.051(2) Uani 1 1 d . A 1 H15 H 0.3378 0.61 0.2919 0.061 Uiso 1 1 calc R A 1 C16 C 0.4912(7) 0.1581(6) 0.5428(4) 0.060(2) Uani 1 1 d . A 1 H16A H 0.437 0.1938 0.5549 0.09 Uiso 1 1 calc R A 1 H16B H 0.5279 0.1253 0.5859 0.09 Uiso 1 1 calc R A 1 H16C H 0.4633 0.1155 0.5272 0.09 Uiso 1 1 calc R A 1 C17 C 0.6768(9) 0.1612(9) 0.4481(5) 0.114(5) Uani 1 1 d . A 1 H17A H 0.7241 0.1984 0.4085 0.171 Uiso 1 1 calc R A 1 H17B H 0.6474 0.1186 0.4332 0.171 Uiso 1 1 calc R A 1 H17C H 0.7118 0.1284 0.4921 0.171 Uiso 1 1 calc R A 1 C18 C 0.6306(8) 0.3097(7) 0.5022(5) 0.078(3) Uani 1 1 d . A 1 H18A H 0.5771 0.3474 0.5125 0.116 Uiso 1 1 calc R A 1 H18B H 0.6802 0.3476 0.4651 0.116 Uiso 1 1 calc R A 1 H18C H 0.6626 0.2741 0.5471 0.116 Uiso 1 1 calc R A 1 C19 C 0.4246(6) 0.5406(4) 0.0742(3) 0.0388(16) Uani 1 1 d . A 1 H19A H 0.3849 0.4871 0.088 0.058 Uiso 1 1 calc R A 1 H19B H 0.4953 0.5254 0.0674 0.058 Uiso 1 1 calc R A 1 H19C H 0.4034 0.587 0.0285 0.058 Uiso 1 1 calc R A 1 C20 C 0.4851(6) 0.6844(5) 0.1138(4) 0.0460(18) Uani 1 1 d . A 1 H20A H 0.5555 0.6656 0.1115 0.069 Uiso 1 1 calc R A 1 H20B H 0.4743 0.7159 0.1463 0.069 Uiso 1 1 calc R A 1 H20C H 0.4676 0.7244 0.0646 0.069 Uiso 1 1 calc R A 1 C21 C 0.2718(6) 0.6196(5) 0.1537(4) 0.0499(19) Uani 1 1 d . A 1 H21A H 0.2299 0.5668 0.1725 0.075 Uiso 1 1 calc R A 1 H21B H 0.2544 0.6596 0.1045 0.075 Uiso 1 1 calc R A 1 H21C H 0.2608 0.6513 0.1862 0.075 Uiso 1 1 calc R A 1 C22 C 0.2627(5) 0.3534(4) 0.2347(3) 0.0290(14) Uani 1 1 d . B 1 C23 C 0.1775(5) 0.3960(4) 0.2597(3) 0.0294(14) Uani 1 1 d . B 1 H23 H 0.124 0.411 0.2292 0.035 Uiso 1 1 calc R B 1 C24 C 0.1591(5) 0.4188(4) 0.3183(3) 0.0317(14) Uani 1 1 d . B 1 C25 C 0.2682(5) 0.3528(4) 0.1651(3) 0.0283(14) Uani 1 1 d . B 1 C26 C 0.3374(5) 0.2944(4) 0.1420(3) 0.0313(14) Uani 1 1 d . B 1 H26 H 0.3724 0.2478 0.178 0.038 Uiso 1 1 calc R B 1 C27 C 0.3538(5) 0.3048(4) 0.0695(4) 0.0363(16) Uani 1 1 d . B 1 H27 H 0.4063 0.2714 0.0562 0.044 Uiso 1 1 calc R B 1 C28 C 0.2955(5) 0.3627(5) 0.0162(4) 0.0398(17) Uani 1 1 d . B 1 H28 H 0.305 0.3674 -0.0327 0.048 Uiso 1 1 calc R B 1 C29 C 0.2207(5) 0.4150(4) 0.0373(4) 0.0367(16) Uani 1 1 d . B 1 H29 H 0.1799 0.4553 0.0015 0.044 Uiso 1 1 calc R B 1 C30 C 0.2057(5) 0.4091(4) 0.1077(4) 0.0343(15) Uani 1 1 d . B 1 H30 H 0.1524 0.443 0.1196 0.041 Uiso 1 1 calc R B 1 C31 C 0.0540(5) 0.4523(6) 0.3281(4) 0.0455(19) Uani 1 1 d . B 1 C32 C 0.0289(7) 0.5422(7) 0.3013(5) 0.073(3) Uani 1 1 d . B 1 H32 H 0.0784 0.5857 0.2767 0.088 Uiso 1 1 calc R B 1 C33 C -0.0711(10) 0.5685(10) 0.3107(6) 0.113(5) Uani 1 1 d . B 1 H33 H -0.0885 0.6305 0.2922 0.135 Uiso 1 1 calc R B 1 C34 C -0.1423(8) 0.5089(15) 0.3448(7) 0.120(7) Uani 1 1 d . B 1 H34 H -0.2096 0.5281 0.3497 0.144 Uiso 1 1 calc R B 1 C35 C -0.1174(9) 0.4216(13) 0.3720(10) 0.136(7) Uani 1 1 d . B 1 H35 H -0.1675 0.3789 0.3973 0.164 Uiso 1 1 calc R B 1 C36 C -0.0204(7) 0.3925(9) 0.3641(7) 0.097(4) Uani 1 1 d . B 1 H36 H -0.0048 0.3301 0.3838 0.116 Uiso 1 1 calc R B 1 C37 C 0.3967(6) 0.1047(5) 0.3533(5) 0.054(2) Uani 1 1 d . B 1 H37A H 0.4223 0.1063 0.3053 0.081 Uiso 1 1 calc R B 1 H37B H 0.3683 0.046 0.3834 0.081 Uiso 1 1 calc R B 1 H37C H 0.4513 0.1149 0.3774 0.081 Uiso 1 1 calc R B 1 C38 C 0.2550(7) 0.1856(5) 0.4344(4) 0.056(2) Uani 1 1 d . B 1 H38A H 0.2025 0.2311 0.4309 0.084 Uiso 1 1 calc R B 1 H38B H 0.311 0.1955 0.4574 0.084 Uiso 1 1 calc R B 1 H38C H 0.2284 0.126 0.4639 0.084 Uiso 1 1 calc R B 1 C39 C 0.1905(6) 0.1637(5) 0.3033(5) 0.056(2) Uani 1 1 d . B 1 H39A H 0.2111 0.1673 0.254 0.085 Uiso 1 1 calc R B 1 H39B H 0.1346 0.2057 0.3012 0.085 Uiso 1 1 calc R B 1 H39C H 0.1699 0.1027 0.335 0.085 Uiso 1 1 calc R B 1 C40 C 0.3339(6) 0.4175(6) 0.4785(4) 0.060(2) Uani 1 1 d . B 1 H40A H 0.379 0.4604 0.4409 0.09 Uiso 1 1 calc R B 1 H40B H 0.3585 0.3564 0.488 0.09 Uiso 1 1 calc R B 1 H40C H 0.3312 0.4274 0.5236 0.09 Uiso 1 1 calc R B 1 C41 C 0.1605(7) 0.5479(6) 0.4362(5) 0.065(2) Uani 1 1 d . B 1 H41A H 0.2031 0.5928 0.3982 0.097 Uiso 1 1 calc R B 1 H41B H 0.1632 0.5531 0.4829 0.097 Uiso 1 1 calc R B 1 H41C H 0.0916 0.5577 0.4226 0.097 Uiso 1 1 calc R B 1 C42 C 0.1213(8) 0.3507(7) 0.5188(5) 0.076(3) Uani 1 1 d . B 1 H42A H 0.1433 0.2899 0.5252 0.114 Uiso 1 1 calc R B 1 H42B H 0.0527 0.3613 0.5046 0.114 Uiso 1 1 calc R B 1 H42C H 0.124 0.3574 0.5649 0.114 Uiso 1 1 calc R B 1 C43 C 0.1522(5) 0.0484(4) 0.1613(4) 0.0355(15) Uani 1 1 d . C 1 C44 C 0.0558(5) 0.0805(4) 0.1404(4) 0.0401(16) Uani 1 1 d . C 1 H44 H 0.0035 0.057 0.178 0.048 Uiso 1 1 calc R C 1 C45 C 0.0240(5) 0.1426(4) 0.0717(4) 0.0351(15) Uani 1 1 d . C 1 C46 C 0.1553(5) -0.0368(4) 0.2281(4) 0.0355(15) Uani 1 1 d . C 1 C47 C 0.2169(6) -0.0436(5) 0.2814(4) 0.0427(17) Uani 1 1 d . C 1 H47 H 0.2593 0.0043 0.2732 0.051 Uiso 1 1 calc R C 1 C48 C 0.2178(7) -0.1193(6) 0.3464(5) 0.059(2) Uani 1 1 d . C 1 H48 H 0.2614 -0.1234 0.382 0.071 Uiso 1 1 calc R C 1 C49 C 0.1539(8) -0.1900(6) 0.3594(5) 0.068(3) Uani 1 1 d . C 1 H49 H 0.1512 -0.2405 0.4049 0.081 Uiso 1 1 calc R C 1 C50 C 0.0959(8) -0.1853(6) 0.3061(5) 0.071(3) Uani 1 1 d . C 1 H50 H 0.0556 -0.2343 0.3135 0.086 Uiso 1 1 calc R C 1 C51 C 0.0955(6) -0.1077(5) 0.2396(4) 0.052(2) Uani 1 1 d . C 1 H51 H 0.054 -0.1044 0.2031 0.063 Uiso 1 1 calc R C 1 C52 C -0.0788(5) 0.1237(5) 0.0589(4) 0.0368(16) Uani 1 1 d . C 1 C53 C -0.0954(6) 0.0437(6) 0.0549(5) 0.060(2) Uani 1 1 d . C 1 H53 H -0.0419 0.0013 0.0608 0.071 Uiso 1 1 calc R C 1 C54 C -0.1876(8) 0.0237(7) 0.0426(7) 0.084(3) Uani 1 1 d . C 1 H54 H -0.1963 -0.0309 0.038 0.1 Uiso 1 1 calc R C 1 C55 C -0.2680(7) 0.0829(7) 0.0370(6) 0.072(3) Uani 1 1 d . C 1 H55 H -0.3326 0.0685 0.0307 0.086 Uiso 1 1 calc R C 1 C56 C -0.2515(6) 0.1623(6) 0.0407(5) 0.062(2) Uani 1 1 d . C 1 H56 H -0.3056 0.2039 0.0364 0.074 Uiso 1 1 calc R C 1 C57 C -0.1581(6) 0.1838(5) 0.0506(4) 0.049(2) Uani 1 1 d . C 1 H57 H -0.1485 0.2403 0.0516 0.059 Uiso 1 1 calc R C 1 C58 C 0.3428(7) -0.0770(5) 0.1327(5) 0.059(2) Uani 1 1 d . C 1 H58A H 0.2913 -0.0858 0.1053 0.089 Uiso 1 1 calc R C 1 H58B H 0.3257 -0.11 0.1852 0.089 Uiso 1 1 calc R C 1 H58C H 0.4073 -0.099 0.1186 0.089 Uiso 1 1 calc R C 1 C59 C 0.3904(6) 0.1027(5) 0.0121(4) 0.053(2) Uani 1 1 d . C 1 H59A H 0.3956 0.1668 -0.0005 0.079 Uiso 1 1 calc R C 1 H59B H 0.3411 0.0936 -0.0167 0.079 Uiso 1 1 calc R C 1 H59C H 0.4554 0.0783 0.0013 0.079 Uiso 1 1 calc R C 1 C60 C 0.4488(6) 0.0605(6) 0.1634(5) 0.062(2) Uani 1 1 d . C 1 H60A H 0.4533 0.1244 0.1522 0.093 Uiso 1 1 calc R C 1 H60B H 0.5131 0.038 0.1492 0.093 Uiso 1 1 calc R C 1 H60C H 0.4319 0.0276 0.216 0.093 Uiso 1 1 calc R C 1 C61 C 0.1834(8) 0.2908(8) -0.1164(5) 0.090(4) Uani 1 1 d . C 1 H61A H 0.2251 0.3181 -0.0942 0.135 Uiso 1 1 calc R C 1 H61B H 0.1792 0.3303 -0.1682 0.135 Uiso 1 1 calc R C 1 H61C H 0.213 0.2329 -0.1124 0.135 Uiso 1 1 calc R C 1 C62 C -0.0004(8) 0.3841(5) -0.0772(5) 0.076(3) Uani 1 1 d . C 1 H62A H -0.0675 0.3747 -0.0518 0.114 Uiso 1 1 calc R C 1 H62B H -0.0048 0.423 -0.1291 0.114 Uiso 1 1 calc R C 1 H62C H 0.0404 0.4124 -0.0553 0.114 Uiso 1 1 calc R C 1 C63 C -0.0193(7) 0.2226(5) -0.1130(4) 0.056(2) Uani 1 1 d . C 1 H63A H -0.0868 0.2131 -0.0883 0.083 Uiso 1 1 calc R C 1 H63B H 0.0112 0.165 -0.1092 0.083 Uiso 1 1 calc R C 1 H63C H -0.0226 0.2626 -0.1647 0.083 Uiso 1 1 calc R C 1 C64 C -0.0485(6) 0.3564(6) 0.1334(6) 0.065(3) Uani 1 1 d . D 1 H64A H -0.102 0.3548 0.1037 0.078 Uiso 1 1 calc R D 1 H64B H -0.0034 0.4059 0.1032 0.078 Uiso 1 1 calc R D 1 C65 C -0.0915(7) 0.3676(8) 0.2013(7) 0.086(4) Uani 1 1 d . D 1 H65A H -0.1543 0.4038 0.1925 0.103 Uiso 1 1 calc R D 1 H65B H -0.0437 0.3965 0.2186 0.103 Uiso 1 1 calc R D 1 C66 C -0.1106(8) 0.2722(9) 0.2559(7) 0.093(4) Uani 1 1 d . D 1 H66A H -0.0856 0.2619 0.3034 0.111 Uiso 1 1 calc R D 1 H66B H -0.1829 0.2604 0.2639 0.111 Uiso 1 1 calc R D 1 C67 C -0.0554(7) 0.2123(7) 0.2232(5) 0.073(3) Uani 1 1 d . D 1 H67A H -0.0135 0.1672 0.2591 0.087 Uiso 1 1 calc R D 1 H67B H -0.1027 0.1809 0.2078 0.087 Uiso 1 1 calc R D 1 M1 C 0.2803 0.3565 0.0896 0.01 Uiso 0 1 d P D 2 M2 C 0.6272 0.3286 0.1995 0.01 Uiso 0 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.02523(15) 0.03484(16) 0.02548(15) -0.01148(12) -0.00308(11) 0.00207(11) Yb2 0.02403(15) 0.03699(16) 0.02384(15) -0.01153(12) -0.00484(11) 0.00261(11) Yb3 0.02746(16) 0.03073(15) 0.03435(16) -0.01304(13) -0.00211(12) -0.00120(11) Si1 0.0385(12) 0.0700(15) 0.0287(10) -0.0069(10) -0.0100(9) 0.0150(11) Si2 0.0293(10) 0.0351(10) 0.0288(9) -0.0069(8) -0.0059(8) 0.0004(8) Si3 0.0394(11) 0.0323(10) 0.0349(10) -0.0088(8) -0.0003(8) -0.0024(8) Si4 0.0390(11) 0.0544(12) 0.0331(10) -0.0250(10) -0.0035(8) 0.0051(9) Si5 0.0385(11) 0.0385(10) 0.0449(11) -0.0209(9) -0.0058(9) 0.0054(9) Si6 0.0497(13) 0.0423(11) 0.0391(11) -0.0092(10) -0.0183(10) -0.0025(10) O 0.039(3) 0.065(4) 0.072(4) -0.035(3) 0.013(3) -0.003(3) N1 0.028(3) 0.048(3) 0.024(3) -0.009(3) -0.006(2) 0.006(3) N2 0.020(3) 0.039(3) 0.026(3) -0.012(2) -0.007(2) 0.001(2) N3 0.027(3) 0.030(3) 0.030(3) -0.009(2) -0.007(2) 0.005(2) N4 0.029(3) 0.050(3) 0.031(3) -0.024(3) -0.001(2) 0.000(3) N5 0.033(3) 0.031(3) 0.037(3) -0.013(3) -0.009(3) 0.002(2) N6 0.034(3) 0.029(3) 0.039(3) -0.007(3) -0.011(3) -0.002(2) C1 0.028(4) 0.048(4) 0.028(3) -0.014(3) -0.009(3) 0.005(3) C2 0.021(3) 0.053(4) 0.037(4) -0.020(3) -0.007(3) -0.005(3) C3 0.023(3) 0.043(4) 0.034(4) -0.018(3) -0.008(3) 0.001(3) C4 0.023(3) 0.042(4) 0.029(3) -0.010(3) -0.006(3) 0.008(3) C5 0.030(4) 0.042(4) 0.034(4) -0.008(3) -0.003(3) 0.008(3) C6 0.042(4) 0.047(4) 0.044(4) -0.020(4) 0.002(3) 0.009(3) C7 0.044(5) 0.060(5) 0.036(4) -0.025(4) 0.003(3) 0.010(4) C8 0.029(4) 0.052(4) 0.029(4) -0.009(3) 0.003(3) 0.007(3) C9 0.021(3) 0.043(4) 0.042(4) -0.011(3) -0.002(3) 0.001(3) C10 0.046(5) 0.043(4) 0.038(4) -0.016(3) -0.012(3) -0.006(3) C11 0.083(7) 0.061(6) 0.082(7) -0.032(5) -0.032(6) -0.005(5) C12 0.162(14) 0.067(7) 0.117(10) -0.042(7) -0.058(10) -0.033(8) C13 0.179(15) 0.060(7) 0.080(8) -0.042(6) -0.039(9) 0.013(8) C14 0.121(10) 0.060(6) 0.043(5) -0.026(5) 0.000(5) 0.012(6) C15 0.068(6) 0.042(4) 0.040(4) -0.017(4) 0.005(4) 0.001(4) C16 0.075(6) 0.058(5) 0.033(4) -0.006(4) -0.008(4) 0.003(4) C17 0.100(9) 0.170(12) 0.047(6) -0.026(7) -0.029(6) 0.092(9) C18 0.067(6) 0.107(8) 0.041(5) -0.003(5) -0.026(4) -0.021(6) C19 0.050(5) 0.034(4) 0.028(3) -0.005(3) -0.009(3) -0.008(3) C20 0.058(5) 0.036(4) 0.039(4) -0.012(3) 0.011(4) -0.013(3) C21 0.038(4) 0.055(5) 0.046(4) -0.009(4) -0.011(3) 0.014(4) C22 0.023(3) 0.034(3) 0.034(3) -0.019(3) -0.002(3) -0.004(3) C23 0.023(3) 0.036(3) 0.029(3) -0.012(3) -0.007(3) 0.002(3) C24 0.022(3) 0.044(4) 0.029(3) -0.016(3) -0.001(3) -0.001(3) C25 0.028(3) 0.032(3) 0.028(3) -0.016(3) 0.000(3) -0.001(3) C26 0.022(3) 0.038(4) 0.034(4) -0.014(3) -0.004(3) -0.003(3) C27 0.029(4) 0.040(4) 0.049(4) -0.028(4) 0.005(3) -0.008(3) C28 0.045(4) 0.046(4) 0.031(4) -0.018(3) 0.005(3) -0.012(3) C29 0.040(4) 0.035(4) 0.031(4) -0.008(3) -0.005(3) -0.014(3) C30 0.033(4) 0.041(4) 0.035(4) -0.020(3) -0.009(3) 0.002(3) C31 0.036(4) 0.080(6) 0.034(4) -0.038(4) -0.003(3) 0.007(4) C32 0.049(5) 0.106(8) 0.047(5) -0.017(5) -0.007(4) 0.046(5) C33 0.082(9) 0.181(13) 0.053(6) -0.036(8) -0.014(6) 0.091(9) C34 0.027(6) 0.28(2) 0.089(9) -0.116(12) -0.011(6) 0.046(9) C35 0.036(7) 0.230(19) 0.194(17) -0.146(17) 0.044(9) -0.027(9) C36 0.040(6) 0.132(10) 0.148(11) -0.095(9) 0.040(6) -0.028(6) C37 0.060(5) 0.035(4) 0.058(5) -0.010(4) -0.007(4) 0.004(4) C38 0.068(6) 0.047(5) 0.040(4) -0.007(4) 0.007(4) -0.011(4) C39 0.055(5) 0.040(4) 0.073(6) -0.020(4) -0.001(4) -0.014(4) C40 0.052(5) 0.097(7) 0.048(5) -0.045(5) -0.014(4) 0.015(5) C41 0.073(6) 0.072(6) 0.061(5) -0.042(5) -0.005(5) 0.022(5) C42 0.089(8) 0.089(7) 0.052(5) -0.037(5) 0.036(5) -0.019(6) C43 0.039(4) 0.031(3) 0.037(4) -0.014(3) -0.007(3) -0.003(3) C44 0.032(4) 0.038(4) 0.046(4) -0.013(3) -0.006(3) 0.002(3) C45 0.031(4) 0.034(4) 0.042(4) -0.016(3) -0.010(3) 0.005(3) C46 0.042(4) 0.027(3) 0.031(4) -0.004(3) -0.004(3) 0.000(3) C47 0.050(5) 0.038(4) 0.039(4) -0.014(3) -0.015(3) 0.009(3) C48 0.071(6) 0.057(5) 0.050(5) -0.021(4) -0.019(4) 0.017(5) C49 0.083(7) 0.051(5) 0.051(5) -0.003(4) -0.012(5) 0.009(5) C50 0.073(7) 0.047(5) 0.080(7) -0.008(5) -0.017(5) -0.006(5) C51 0.051(5) 0.041(4) 0.052(5) -0.002(4) -0.015(4) -0.004(4) C52 0.028(4) 0.046(4) 0.042(4) -0.022(3) -0.003(3) -0.003(3) C53 0.042(5) 0.054(5) 0.093(7) -0.037(5) -0.017(5) 0.001(4) C54 0.071(7) 0.069(6) 0.133(10) -0.055(7) -0.040(7) -0.002(5) C55 0.043(5) 0.093(7) 0.103(8) -0.060(7) -0.018(5) -0.007(5) C56 0.037(5) 0.085(6) 0.078(6) -0.047(6) -0.023(4) 0.021(4) C57 0.037(4) 0.057(5) 0.068(5) -0.036(4) -0.021(4) 0.011(4) C58 0.078(6) 0.045(4) 0.056(5) -0.024(4) -0.001(4) 0.011(4) C59 0.052(5) 0.048(4) 0.061(5) -0.028(4) 0.013(4) -0.013(4) C60 0.044(5) 0.076(6) 0.079(6) -0.045(5) -0.025(4) 0.023(4) C61 0.084(8) 0.134(10) 0.039(5) -0.018(6) -0.005(5) -0.029(7) C62 0.115(9) 0.041(5) 0.075(6) -0.018(5) -0.051(6) 0.011(5) C63 0.067(6) 0.056(5) 0.041(4) -0.012(4) -0.023(4) 0.004(4) C64 0.038(5) 0.070(6) 0.102(7) -0.051(6) -0.013(5) 0.010(4) C65 0.032(5) 0.122(9) 0.146(11) -0.097(9) -0.013(6) 0.014(5) C66 0.062(7) 0.125(10) 0.114(9) -0.079(9) 0.032(6) -0.014(7) C67 0.046(5) 0.099(7) 0.073(6) -0.037(6) 0.017(5) -0.021(5) #----------------------------------------------------------------------------# # 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 Yb1 M2 2.317(6) . ? Yb1 N3 2.426(5) . ? Yb1 N2 2.481(5) . ? Yb2 N1 2.215(5) . ? Yb2 N4 2.224(5) . ? Yb2 N3 2.264(5) . ? Yb2 N2 2.431(5) . ? Yb2 C1 2.456(7) . ? Yb2 C2 2.561(6) . ? Yb3 N5 2.357(5) . ? Yb3 N6 2.388(5) . ? Yb3 O 2.430(5) . ? Yb3 M1 2.483(6) . ? Si1 N1 1.707(5) . ? Si1 C17 1.847(10) . ? Si1 C16 1.856(9) . ? Si1 C18 1.869(10) . ? Si2 N2 1.732(5) . ? Si2 C21 1.862(7) . ? Si2 C20 1.864(7) . ? Si2 C19 1.905(7) . ? Si3 N3 1.740(5) . ? Si3 C38 1.854(8) . ? Si3 C37 1.860(8) . ? Si3 C39 1.887(8) . ? Si4 N4 1.721(5) . ? Si4 C41 1.866(8) . ? Si4 C42 1.874(9) . ? Si4 C40 1.886(8) . ? Si5 N5 1.752(6) . ? Si5 C58 1.856(8) . ? Si5 C60 1.862(8) . ? Si5 C59 1.869(8) . ? Si6 N6 1.749(6) . ? Si6 C61 1.837(11) . ? Si6 C62 1.861(9) . ? Si6 C63 1.871(8) . ? O C67 1.448(10) . ? O C64 1.450(10) . ? N1 C1 1.443(9) . ? N2 C3 1.411(8) . ? N3 C22 1.455(8) . ? N4 C24 1.382(8) . ? N5 C43 1.337(9) . ? N6 C45 1.310(9) . ? C1 C4 1.397(9) . ? C1 C2 1.473(9) . ? C2 C3 1.377(9) . ? C3 C10 1.486(9) . ? C4 C9 1.444(9) . ? C4 C5 1.448(10) . ? C5 C6 1.386(10) . ? C6 C7 1.386(10) . ? C7 C8 1.399(10) . ? C8 C9 1.386(9) . ? C10 C15 1.367(11) . ? C10 C11 1.401(11) . ? C11 C12 1.411(14) . ? C12 C13 1.388(18) . ? C13 C14 1.300(17) . ? C14 C15 1.382(12) . ? C22 C25 1.396(8) . ? C22 C23 1.458(8) . ? C23 C24 1.367(8) . ? C24 C31 1.510(9) . ? C25 C30 1.457(9) . ? C25 C26 1.468(8) . ? C26 C27 1.392(9) . ? C27 C28 1.383(10) . ? C28 C29 1.423(10) . ? C29 C30 1.372(9) . ? C31 C36 1.373(13) . ? C31 C32 1.376(12) . ? C32 C33 1.407(13) . ? C33 C34 1.34(2) . ? C34 C35 1.34(2) . ? C35 C36 1.380(16) . ? C43 C44 1.411(9) . ? C43 C46 1.493(9) . ? C44 C45 1.429(9) . ? C45 C52 1.508(9) . ? C46 C51 1.383(10) . ? C46 C47 1.385(10) . ? C47 C48 1.386(11) . ? C48 C49 1.408(13) . ? C49 C50 1.364(13) . ? C50 C51 1.419(11) . ? C52 C53 1.376(10) . ? C52 C57 1.381(10) . ? C53 C54 1.377(12) . ? C54 C55 1.388(13) . ? C55 C56 1.365(12) . ? C56 C57 1.383(11) . ? C64 C65 1.501(13) . ? C65 C66 1.517(16) . ? C66 C67 1.508(13) . ? 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 M2 Yb1 N3 118.9(2) . . ? M2 Yb1 N2 104.9(2) . . ? N3 Yb1 N2 85.56(17) . . ? N1 Yb2 N4 145.1(2) . . ? N1 Yb2 N3 96.65(19) . . ? N4 Yb2 N3 90.58(18) . . ? N1 Yb2 N2 109.14(18) . . ? N4 Yb2 N2 104.94(19) . . ? N3 Yb2 N2 90.37(17) . . ? N5 Yb3 N6 82.26(18) . . ? N5 Yb3 O 128.86(19) . . ? N6 Yb3 O 87.7(2) . . ? N5 Yb3 M1 118.0(2) . . ? N6 Yb3 M1 129.4(2) . . ? O Yb3 M1 106.99(13) . . ? N1 Si1 C17 111.5(4) . . ? N1 Si1 C16 109.8(3) . . ? C17 Si1 C16 106.8(5) . . ? N1 Si1 C18 111.3(4) . . ? C17 Si1 C18 110.1(6) . . ? C16 Si1 C18 107.1(4) . . ? N2 Si2 C21 115.0(3) . . ? N2 Si2 C20 114.1(3) . . ? C21 Si2 C20 109.5(4) . . ? N2 Si2 C19 107.5(3) . . ? C21 Si2 C19 106.6(3) . . ? C20 Si2 C19 103.2(3) . . ? N3 Si3 C38 111.4(3) . . ? N3 Si3 C37 114.5(3) . . ? C38 Si3 C37 106.5(4) . . ? N3 Si3 C39 109.5(3) . . ? C38 Si3 C39 107.4(4) . . ? C37 Si3 C39 107.3(4) . . ? N4 Si4 C41 116.5(3) . . ? N4 Si4 C42 115.3(4) . . ? C41 Si4 C42 107.7(4) . . ? N4 Si4 C40 102.0(3) . . ? C41 Si4 C40 106.5(4) . . ? C42 Si4 C40 108.1(5) . . ? N5 Si5 C58 112.9(4) . . ? N5 Si5 C60 112.9(3) . . ? C58 Si5 C60 109.3(4) . . ? N5 Si5 C59 106.4(3) . . ? C58 Si5 C59 107.6(4) . . ? C60 Si5 C59 107.4(4) . . ? N6 Si6 C61 105.4(4) . . ? N6 Si6 C62 108.9(4) . . ? C61 Si6 C62 110.1(5) . . ? N6 Si6 C63 115.5(3) . . ? C61 Si6 C63 108.1(4) . . ? C62 Si6 C63 108.9(4) . . ? C67 O C64 105.9(7) . . ? C67 O Yb3 127.0(5) . . ? C64 O Yb3 127.1(5) . . ? C1 N1 Si1 118.7(4) . . ? C1 N1 Yb2 81.4(3) . . ? Si1 N1 Yb2 148.8(3) . . ? C3 N2 Si2 122.4(4) . . ? C3 N2 Yb2 79.4(3) . . ? Si2 N2 Yb2 144.7(3) . . ? C3 N2 Yb1 129.0(4) . . ? Si2 N2 Yb1 98.4(2) . . ? Yb2 N2 Yb1 83.62(16) . . ? C22 N3 Si3 113.4(4) . . ? C22 N3 Yb2 109.3(3) . . ? Si3 N3 Yb2 113.8(3) . . ? C22 N3 Yb1 86.9(3) . . ? Si3 N3 Yb1 140.2(3) . . ? Yb2 N3 Yb1 88.49(18) . . ? C24 N4 Si4 128.4(4) . . ? C24 N4 Yb2 118.3(4) . . ? Si4 N4 Yb2 113.1(3) . . ? C43 N5 Si5 126.1(4) . . ? C43 N5 Yb3 94.5(4) . . ? Si5 N5 Yb3 139.2(3) . . ? C45 N6 Si6 130.0(5) . . ? C45 N6 Yb3 95.8(4) . . ? Si6 N6 Yb3 132.3(3) . . ? C4 C1 N1 124.8(6) . . ? C4 C1 C2 120.7(6) . . ? N1 C1 C2 113.5(5) . . ? C4 C1 Yb2 119.4(4) . . ? N1 C1 Yb2 63.1(3) . . ? C2 C1 Yb2 76.9(4) . . ? C3 C2 C1 123.8(6) . . ? C3 C2 Yb2 75.0(4) . . ? C1 C2 Yb2 69.1(4) . . ? C2 C3 N2 121.3(6) . . ? C2 C3 C10 118.3(6) . . ? N2 C3 C10 120.0(5) . . ? C1 C4 C9 122.5(6) . . ? C1 C4 C5 122.4(6) . . ? C9 C4 C5 114.4(6) . . ? C1 C4 Yb1 104.0(4) . . ? C9 C4 Yb1 77.1(4) . . ? C5 C4 Yb1 80.1(4) . . ? C6 C5 C4 121.1(7) . . ? C5 C6 C7 122.1(7) . . ? C6 C7 C8 118.2(6) . . ? C9 C8 C7 121.0(7) . . ? C8 C9 C4 122.0(7) . . ? C15 C10 C11 118.3(8) . . ? C15 C10 C3 121.4(7) . . ? C11 C10 C3 120.4(7) . . ? C10 C11 C12 118.6(11) . . ? C13 C12 C11 120.6(11) . . ? C14 C13 C12 119.0(11) . . ? C13 C14 C15 122.9(11) . . ? C10 C15 C14 120.7(9) . . ? C25 C22 N3 118.4(5) . . ? C25 C22 C23 120.1(6) . . ? N3 C22 C23 121.0(5) . . ? C24 C23 C22 132.9(6) . . ? C23 C24 N4 126.7(6) . . ? C23 C24 C31 114.7(5) . . ? N4 C24 C31 118.6(5) . . ? C22 C25 C30 124.0(5) . . ? C22 C25 C26 123.4(6) . . ? C30 C25 C26 112.6(5) . . ? C27 C26 C25 122.5(6) . . ? C28 C27 C26 121.6(6) . . ? C27 C28 C29 117.7(6) . . ? C30 C29 C28 122.1(7) . . ? C29 C30 C25 122.6(6) . . ? C36 C31 C32 117.9(8) . . ? C36 C31 C24 120.0(8) . . ? C32 C31 C24 122.1(8) . . ? C31 C32 C33 119.0(11) . . ? C34 C33 C32 121.9(13) . . ? C33 C34 C35 119.0(10) . . ? C34 C35 C36 121.3(14) . . ? C31 C36 C35 120.9(13) . . ? N5 C43 C44 123.0(6) . . ? N5 C43 C46 122.0(6) . . ? C44 C43 C46 115.0(6) . . ? C43 C44 C45 130.4(7) . . ? N6 C45 C44 126.0(6) . . ? N6 C45 C52 121.4(6) . . ? C44 C45 C52 112.7(6) . . ? C51 C46 C47 119.1(6) . . ? C51 C46 C43 121.8(6) . . ? C47 C46 C43 119.0(6) . . ? C46 C47 C48 121.2(7) . . ? C47 C48 C49 119.7(8) . . ? C50 C49 C48 119.4(8) . . ? C49 C50 C51 120.5(9) . . ? C46 C51 C50 120.0(8) . . ? C53 C52 C57 117.9(7) . . ? C53 C52 C45 119.3(6) . . ? C57 C52 C45 122.8(6) . . ? C52 C53 C54 121.5(8) . . ? C53 C54 C55 120.4(8) . . ? C56 C55 C54 118.0(8) . . ? C55 C56 C57 121.6(8) . . ? C52 C57 C56 120.5(7) . . ? O C64 C65 104.1(8) . . ? C64 C65 C66 103.5(8) . . ? C67 C66 C65 106.2(8) . . ? O C67 C66 105.3(8) . . ?