Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal SOciety of Chemistry 2002 data_global #=================================================================== # 0. AUDIT DETAILS _audit_creation_date 2-Oct-00 _audit_creation_method 'PLATON option' _audit_update_record ; 2-Oct-00 Updated by the Author E.H. 18-Oct-00 Updated by the Author E.H. Textwriting by E.H. Checkcif OK 12-Feb-02 Updated by the Author E.H. ; #=================================================================== # 1. SUBMISSION DETAILS #=================================================================== _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Estler, F.' ; Anorganisch-chemisches Institut der Technischen Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching bei Munchen ; 'Herdtweck, E.' ; Anorganisch-chemisches Institut der Technischen Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching bei Munchen ; 'Anwander, R.' ; Anorganisch-chemisches Institut der Technischen Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching bei Munchen ; _publ_contact_author_name 'Dr Reiner Anwander' _publ_contact_author_address ; Anorganisch-chemisches Institut Technische Universitat Muenchen Lichtenbergstr. 4 Garching D-85747 GERMANY ; _publ_contact_author_email 'REINER.ANWANDER@CH.TUM.DE' _publ_contact_author_fax ' +49(0)89 289 13473' _publ_contact_author_phone '+49(0)89 289 13143' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; O-Benzylated-calix[4]arenes as Ancillary Ligands in Organolanthanide Chemistry ; _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; _publ_section_abstract ; 25,27-O-Benzylated-calix[4]arenes H2L react with Ln[SiHMe2)2]3(thf)x (Ln=Sc(x=1), Lu (x=2)) via an exteended silylamide route to yield monomeric, hetroleptic ... ; # Insert blank lines between paragraphs _publ_section_comment ; none ; _publ_section_experimental ; none ; # Insert blank lines between references _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436. Nonius (2000a). Data Collection Software for Nonius Kappa-CCD devices. Nonius BV, Delft, The Netherlands. Nonius (2000b). DENZO Processing Software for Nonius Kappa-CCD devices, Nonius BV, Delft, The Netherlands. Sheldrick, G. M. (1998). SHELXL97, University of Gottingen, Gottingen, Germany. Spek, A. L. (2001). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_figure_captions ; View of the title compound with the appropriate atom numbering scheme Displacement ellipsoids for non-H atoms are drawn at the 50% probability level ; _publ_section_acknowledgements ; none ; _publ_section_table_legends ; none ; data_ESTB-4090-123 _database_code_CSD 182440 #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C62 H80 N O4 Sc Si2, 3(C7 H8)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C83 H104 N O4 Sc Si2' _chemical_formula_weight 1280.81 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz x,y,z x,-y,1/2+z 1/2+x,1/2+y,z 1/2+x,1/2-y,1/2+z _cell_length_a 17.5600(4) _cell_length_b 24.5441(7) _cell_length_c 17.2735(4) _cell_angle_alpha 90 _cell_angle_beta 92.577(2) _cell_angle_gamma 90 _cell_volume 7437.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 37074 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 25.34 _exptl_crystal_description 'fragment' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method none _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 0.180 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min 0.8934 _exptl_absorpt_correction_T_max 0.9233 _exptl_absorpt_process_details ; Neither decay correction nor absorption correction necessary Denzo-SNM; Scale-Pack ; _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 30 s per film repetition 1 258 films measured in 3 data sets set 1: phis-scan with delta_phi = 1.0 set 2 to 3 omega-scan with delta_omega = 1.0 ; _publ_section_exptl_prep ; the crystal was fixed in a capillary with perfluorinated ether and transfered to the diffractometer ; _publ_section_exptl_refinement ; straight forward after integration with the program NPROCESS; source: 'Denzo-SMN (Nonius, 2000b)' Hydrogen atoms could be located in the difference Fourier maps and refined freely only for the Si-H spezies. All other hydrogen atoms are calculated in ideal positions riding on the parent carbon atom with U(iso) 1.2 times U(iso) parent carbon atom. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Kappa CCD (Nonius)' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean '18 # 9 for binned mode' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 12313 _diffrn_reflns_av_R_equivalents 0.0066 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.34 _reflns_number_total 12306 _reflns_number_gt 11125 # number of observed reflections (> n sig(I)) _reflns_threshold_expression >2sigma(i) _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2000a)' _computing_cell_refinement 'DENZO (Nonius, 2000b)' _computing_data_reduction 'DENZO (Nonius, 2000b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+13.9657P] 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 # see text _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.48(3) _refine_ls_number_reflns 12306 _refine_ls_number_parameters 829 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1276 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.710 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.049 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Sc Sc Uani 0.05488(4) 0.07095(2) 0.34846(4) 1.000 0.0198(2) Si1 Si Uani 0.06100(6) -0.04094(4) 0.44104(6) 1.000 0.0326(3) Si2 Si Uani 0.06238(7) -0.05285(4) 0.26792(6) 1.000 0.0368(3) O1 O Uani 0.02931(13) 0.10246(10) 0.44515(13) 1.000 0.0262(8) O2 O Uani -0.07035(13) 0.08427(9) 0.31332(13) 1.000 0.0217(7) O3 O Uani 0.07700(13) 0.10977(10) 0.25618(13) 1.000 0.0242(7) O4 O Uani 0.17818(13) 0.08543(9) 0.38300(13) 1.000 0.0213(7) N N Uani 0.0584(2) -0.01296(9) 0.3494(2) 1.000 0.0262(7) C1 C Uani 0.01624(19) 0.13928(13) 0.49977(18) 1.000 0.0200(10) C2 C Uani 0.07627(19) 0.15874(14) 0.54849(19) 1.000 0.0212(10) C3 C Uani 0.06235(19) 0.19824(14) 0.60312(19) 1.000 0.0230(10) C4 C Uani -0.0108(2) 0.22021(13) 0.61108(19) 1.000 0.0227(10) C5 C Uani -0.0694(2) 0.19954(14) 0.56241(19) 1.000 0.0248(10) C6 C Uani -0.0573(2) 0.15980(14) 0.50744(19) 1.000 0.0237(10) C7 C Uani -0.12078(19) 0.13849(14) 0.45265(19) 1.000 0.0229(10) C8 C Uani -0.11902(19) 0.16549(14) 0.37351(19) 1.000 0.0217(10) C9 C Uani -0.14664(19) 0.21840(14) 0.3648(2) 1.000 0.0227(10) C10 C Uani -0.14755(18) 0.24610(14) 0.2942(2) 1.000 0.0247(10) C11 C Uani -0.1163(2) 0.21993(14) 0.2327(2) 1.000 0.0246(10) C12 C Uani -0.08691(19) 0.16684(14) 0.23703(19) 1.000 0.0212(10) C13 C Uani -0.09205(19) 0.13993(14) 0.30796(19) 1.000 0.0199(10) C14 C Uani -0.0508(2) 0.14300(14) 0.1668(2) 1.000 0.0238(10) C15 C Uani 0.0274(2) 0.16707(14) 0.15600(19) 1.000 0.0233(10) C16 C Uani 0.0406(2) 0.20844(14) 0.10257(19) 1.000 0.0239(10) C17 C Uani 0.1120(2) 0.23143(14) 0.09439(19) 1.000 0.0250(10) C18 C Uani 0.17291(19) 0.21144(14) 0.14227(19) 1.000 0.0223(10) C19 C Uani 0.16221(19) 0.17005(14) 0.19689(18) 1.000 0.0212(10) C20 C Uani 0.08882(19) 0.14900(13) 0.20383(18) 1.000 0.0194(9) C21 C Uani 0.22565(19) 0.14858(14) 0.24998(19) 1.000 0.0236(10) C22 C Uani 0.22307(19) 0.17115(14) 0.33246(19) 1.000 0.0214(10) C23 C Uani 0.24733(19) 0.22395(14) 0.3473(2) 1.000 0.0239(10) C24 C Uani 0.24852(19) 0.24725(14) 0.4208(2) 1.000 0.0254(10) C25 C Uani 0.21888(19) 0.21670(14) 0.4799(2) 1.000 0.0237(10) C26 C Uani 0.19200(19) 0.16396(14) 0.4691(2) 1.000 0.0222(10) C27 C Uani 0.19717(19) 0.14084(14) 0.3950(2) 1.000 0.0218(10) C28 C Uani 0.15556(19) 0.13563(14) 0.53688(18) 1.000 0.0217(10) C29 C Uani -0.0269(2) 0.26602(15) 0.6687(2) 1.000 0.0290(11) C30 C Uani -0.0913(2) 0.24969(17) 0.7195(2) 1.000 0.0408(11) C31 C Uani 0.0411(3) 0.2788(3) 0.7229(4) 1.000 0.087(2) C32 C Uani -0.0521(3) 0.31803(17) 0.6227(2) 1.000 0.0585(16) C33 C Uani -0.1877(2) 0.30169(15) 0.2855(2) 1.000 0.0323(11) C34 C Uani -0.2730(2) 0.2909(2) 0.2739(3) 1.000 0.0517(16) C35 C Uani -0.1615(3) 0.3335(2) 0.2163(3) 1.000 0.066(2) C36 C Uani -0.1736(3) 0.33747(18) 0.3577(3) 1.000 0.0528(16) C37 C Uani 0.1234(2) 0.27808(16) 0.0365(2) 1.000 0.0316(11) C38 C Uani 0.0850(4) 0.2657(3) -0.0407(4) 1.000 0.124(3) C39 C Uani 0.2012(3) 0.2898(4) 0.0235(6) 1.000 0.204(6) C40 C Uani 0.0745(4) 0.3273(2) 0.0601(4) 1.000 0.098(3) C41 C Uani 0.2861(2) 0.30299(15) 0.4357(2) 1.000 0.0306(11) C42 C Uani 0.2623(3) 0.32858(17) 0.5120(3) 1.000 0.0487(16) C43 C Uani 0.3727(2) 0.29356(17) 0.4424(3) 1.000 0.0412(14) C44 C Uani 0.2674(3) 0.34243(16) 0.3702(3) 1.000 0.0497(16) C45 C Uani 0.23893(19) 0.04739(14) 0.4118(2) 1.000 0.0250(11) C46 C Uani 0.31332(19) 0.05732(15) 0.3741(2) 1.000 0.0250(10) C47 C Uani 0.3330(2) 0.02747(16) 0.3104(2) 1.000 0.0334(11) C48 C Uani 0.4013(2) 0.0373(2) 0.2744(2) 1.000 0.0425(14) C49 C Uani 0.4498(2) 0.0775(2) 0.3031(3) 1.000 0.0458(14) C50 C Uani 0.4313(2) 0.10758(17) 0.3663(3) 1.000 0.0394(14) C51 C Uani 0.3637(2) 0.09729(16) 0.4022(2) 1.000 0.0335(12) C52 C Uani -0.1296(2) 0.04673(15) 0.2817(2) 1.000 0.0305(11) C53 C Uani -0.2051(2) 0.05377(15) 0.3173(2) 1.000 0.0275(11) C54 C Uani -0.2265(2) 0.0195(2) 0.3767(3) 1.000 0.0483(16) C55 C Uani -0.2957(3) 0.0262(3) 0.4088(3) 1.000 0.069(2) C56 C Uani -0.3443(3) 0.0661(3) 0.3852(3) 1.000 0.0603(18) C57 C Uani -0.3238(2) 0.1007(2) 0.3269(3) 1.000 0.0560(18) C58 C Uani -0.2554(2) 0.09460(17) 0.2935(3) 1.000 0.0383(14) C59 C Uani -0.0364(2) -0.05030(18) 0.4775(2) 1.000 0.0457(12) C60 C Uani 0.1154(3) -0.10635(19) 0.4495(3) 1.000 0.0591(19) C61 C Uani -0.0091(4) -0.10848(19) 0.2668(3) 1.000 0.0627(19) C62 C Uani 0.0459(3) -0.01339(17) 0.1772(2) 1.000 0.0460(14) C70 C Uani 0.0343(4) 0.4351(2) 0.3587(5) 1.000 0.097(3) C71 C Uani 0.0422(3) 0.37590(19) 0.3579(3) 1.000 0.0589(17) C72 C Uani 0.0406(3) 0.34476(19) 0.4241(3) 1.000 0.0455(16) C73 C Uani 0.0452(3) 0.2891(2) 0.4236(3) 1.000 0.0542(17) C74 C Uani 0.0537(3) 0.26055(17) 0.3568(3) 1.000 0.0448(11) C75 C Uani 0.0585(3) 0.2926(2) 0.2876(3) 1.000 0.0557(17) C76 C Uani 0.0510(3) 0.3466(2) 0.2878(3) 1.000 0.0493(16) C80 C Uani 0.1548(4) 0.5628(3) 0.1112(3) 1.000 0.088(3) C81 C Uani 0.2040(4) 0.5129(2) 0.1284(3) 1.000 0.070(2) C82 C Uani 0.1781(4) 0.4731(3) 0.1774(3) 1.000 0.080(2) C83 C Uani 0.2217(4) 0.4286(3) 0.1925(4) 1.000 0.094(3) C84 C Uani 0.2920(5) 0.4216(3) 0.1615(4) 1.000 0.085(3) C85 C Uani 0.3188(4) 0.4609(3) 0.1122(3) 1.000 0.080(3) C86 C Uani 0.2754(4) 0.5066(2) 0.0961(3) 1.000 0.071(2) C90 C Uani 0.4720(4) -0.0248(3) 0.0450(4) 1.000 0.102(3) C91 C Uani 0.3942(3) -0.0032(3) 0.0636(3) 1.000 0.0631(19) C92 C Uani 0.3732(4) 0.0498(3) 0.0437(3) 1.000 0.075(2) C93 C Uani 0.3036(4) 0.0706(3) 0.0617(4) 1.000 0.077(3) C94 C Uani 0.2534(3) 0.0389(3) 0.0993(3) 1.000 0.068(2) C95 C Uani 0.2729(4) -0.0140(3) 0.1186(3) 1.000 0.071(2) C96 C Uani 0.3420(4) -0.0344(2) 0.1002(3) 1.000 0.0644(18) H1 H Uiso 0.093(2) -0.0004(16) 0.489(2) 1.000 0.045(11) H2 H Uiso 0.137(2) -0.0770(15) 0.265(2) 1.000 0.039(10) H3 H Uiso 0.10330 0.21090 0.63620 1.000 0.0280 H5 H Uiso -0.11960 0.21330 0.56720 1.000 0.0300 H7A H Uiso -0.11520 0.09860 0.44670 1.000 0.0270 H7B H Uiso -0.17070 0.14560 0.47520 1.000 0.0270 H9 H Uiso -0.16560 0.23640 0.40870 1.000 0.0270 H11 H Uiso -0.11460 0.23880 0.18480 1.000 0.0290 H14A H Uiso -0.08390 0.15030 0.12010 1.000 0.0290 H14B H Uiso -0.04630 0.10300 0.17300 1.000 0.0290 H16 H Uiso -0.00100 0.22130 0.07060 1.000 0.0290 H18 H Uiso 0.22240 0.22630 0.13750 1.000 0.0270 H21A H Uiso 0.27520 0.15820 0.22850 1.000 0.0280 H21B H Uiso 0.22230 0.10830 0.25190 1.000 0.0280 H23 H Uiso 0.26390 0.24530 0.30530 1.000 0.0290 H25 H Uiso 0.21690 0.23250 0.53000 1.000 0.0280 H28A H Uiso 0.15180 0.09600 0.52650 1.000 0.0260 H28B H Uiso 0.18800 0.14090 0.58470 1.000 0.0260 H30A H Uiso -0.10160 0.27940 0.75550 1.000 0.0490 H30B H Uiso -0.07670 0.21690 0.74900 1.000 0.0490 H30C H Uiso -0.13730 0.24220 0.68690 1.000 0.0490 H31A H Uiso 0.08440 0.28970 0.69240 1.000 0.1050 H31B H Uiso 0.05490 0.24640 0.75360 1.000 0.1050 H31C H Uiso 0.02810 0.30870 0.75760 1.000 0.1050 H32A H Uiso -0.01130 0.32940 0.58940 1.000 0.0700 H32B H Uiso -0.06280 0.34740 0.65910 1.000 0.0700 H32C H Uiso -0.09820 0.31000 0.59060 1.000 0.0700 H34A H Uiso -0.29080 0.27020 0.31800 1.000 0.0620 H34B H Uiso -0.28260 0.26990 0.22620 1.000 0.0620 H34C H Uiso -0.30040 0.32560 0.26990 1.000 0.0620 H35A H Uiso -0.18850 0.36840 0.21290 1.000 0.0790 H35B H Uiso -0.17250 0.31250 0.16880 1.000 0.0790 H35C H Uiso -0.10650 0.34010 0.22230 1.000 0.0790 H36A H Uiso -0.19000 0.31790 0.40350 1.000 0.0630 H36B H Uiso -0.20260 0.37140 0.35150 1.000 0.0630 H36C H Uiso -0.11910 0.34590 0.36410 1.000 0.0630 H38A H Uiso 0.03160 0.25590 -0.03360 1.000 0.1490 H38B H Uiso 0.11100 0.23520 -0.06480 1.000 0.1490 H38C H Uiso 0.08720 0.29780 -0.07420 1.000 0.1490 H39A H Uiso 0.22820 0.29830 0.07290 1.000 0.2440 H39B H Uiso 0.20420 0.32120 -0.01140 1.000 0.2440 H39C H Uiso 0.22500 0.25810 -0.00010 1.000 0.2440 H40A H Uiso 0.02220 0.31520 0.06770 1.000 0.1180 H40B H Uiso 0.07440 0.35490 0.01920 1.000 0.1180 H40C H Uiso 0.09600 0.34290 0.10850 1.000 0.1180 H42A H Uiso 0.28800 0.36380 0.51950 1.000 0.0580 H42B H Uiso 0.27690 0.30430 0.55520 1.000 0.0580 H42C H Uiso 0.20700 0.33400 0.51010 1.000 0.0580 H43A H Uiso 0.39860 0.32830 0.45300 1.000 0.0500 H43B H Uiso 0.38980 0.27840 0.39360 1.000 0.0500 H43C H Uiso 0.38480 0.26800 0.48470 1.000 0.0500 H44A H Uiso 0.29180 0.37760 0.38170 1.000 0.0590 H44B H Uiso 0.21200 0.34740 0.36460 1.000 0.0590 H44C H Uiso 0.28630 0.32780 0.32190 1.000 0.0590 H45A H Uiso 0.22230 0.00940 0.40150 1.000 0.0300 H45B H Uiso 0.24660 0.05170 0.46860 1.000 0.0300 H47 H Uiso 0.29960 -0.00020 0.29080 1.000 0.0400 H48 H Uiso 0.41430 0.01650 0.23060 1.000 0.0510 H49 H Uiso 0.49640 0.08430 0.27890 1.000 0.0550 H50 H Uiso 0.46470 0.13540 0.38560 1.000 0.0470 H51 H Uiso 0.35150 0.11780 0.44660 1.000 0.0400 H52A H Uiso -0.11210 0.00880 0.29020 1.000 0.0360 H52B H Uiso -0.13620 0.05260 0.22510 1.000 0.0360 H54 H Uiso -0.19310 -0.00860 0.39490 1.000 0.0580 H55 H Uiso -0.30990 0.00220 0.44880 1.000 0.0830 H56 H Uiso -0.39190 0.07020 0.40850 1.000 0.0720 H57 H Uiso -0.35760 0.12890 0.30980 1.000 0.0670 H58 H Uiso -0.24200 0.11870 0.25330 1.000 0.0460 H59A H Uiso -0.06450 -0.01590 0.47300 1.000 0.0550 H59B H Uiso -0.03250 -0.06160 0.53190 1.000 0.0550 H59C H Uiso -0.06350 -0.07840 0.44670 1.000 0.0550 H60A H Uiso 0.16650 -0.10110 0.43010 1.000 0.0710 H60B H Uiso 0.08860 -0.13460 0.41890 1.000 0.0710 H60C H Uiso 0.11980 -0.11760 0.50400 1.000 0.0710 H61A H Uiso -0.00160 -0.13060 0.31380 1.000 0.0750 H61B H Uiso -0.00300 -0.13150 0.22110 1.000 0.0750 H61C H Uiso -0.06050 -0.09280 0.26500 1.000 0.0750 H62A H Uiso 0.08400 0.01560 0.17490 1.000 0.0550 H62B H Uiso -0.00520 0.00270 0.17630 1.000 0.0550 H62C H Uiso 0.05000 -0.03770 0.13260 1.000 0.0550 H70A H Uiso 0.03710 0.44910 0.30580 1.000 0.1170 H70B H Uiso 0.07550 0.45100 0.39160 1.000 0.1170 H70C H Uiso -0.01500 0.44490 0.37930 1.000 0.1170 H72 H Uiso 0.03610 0.36280 0.47240 1.000 0.0550 H73 H Uiso 0.04240 0.26980 0.47110 1.000 0.0650 H74 H Uiso 0.05630 0.22190 0.35610 1.000 0.0540 H75 H Uiso 0.06730 0.27470 0.24000 1.000 0.0670 H76 H Uiso 0.05160 0.36600 0.24020 1.000 0.0590 H80A H Uiso 0.18070 0.58700 0.07570 1.000 0.1050 H80B H Uiso 0.14620 0.58220 0.15960 1.000 0.1050 H80C H Uiso 0.10570 0.55140 0.08720 1.000 0.1050 H82 H Uiso 0.13020 0.47700 0.20030 1.000 0.0960 H83 H Uiso 0.20320 0.40120 0.22560 1.000 0.1130 H84 H Uiso 0.32170 0.39010 0.17370 1.000 0.1030 H85 H Uiso 0.36680 0.45650 0.08970 1.000 0.0960 H86 H Uiso 0.29380 0.53390 0.06290 1.000 0.0850 H90A H Uiso 0.50070 0.00370 0.01940 1.000 0.1230 H90B H Uiso 0.46620 -0.05640 0.01060 1.000 0.1230 H90C H Uiso 0.49970 -0.03570 0.09310 1.000 0.1230 H92 H Uiso 0.40780 0.07210 0.01720 1.000 0.0900 H93 H Uiso 0.29050 0.10700 0.04790 1.000 0.0920 H94 H Uiso 0.20530 0.05320 0.11220 1.000 0.0810 H95 H Uiso 0.23800 -0.03630 0.14470 1.000 0.0850 H96 H Uiso 0.35430 -0.07110 0.11320 1.000 0.0770 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 Sc 0.0228(3) 0.0169(3) 0.0198(2) -0.0007(3) 0.0025(2) 0.0000(3) Si1 0.0408(6) 0.0250(5) 0.0323(5) 0.0067(4) 0.0048(4) 0.0020(4) Si2 0.0543(7) 0.0239(5) 0.0332(5) -0.0075(4) 0.0147(5) -0.0010(5) O1 0.0251(13) 0.0278(13) 0.0258(13) -0.0068(10) 0.0014(10) -0.0002(11) O2 0.0225(12) 0.0195(12) 0.0232(12) -0.0036(10) 0.0012(10) -0.0035(10) O3 0.0219(12) 0.0260(13) 0.0247(13) 0.0072(10) 0.0013(10) -0.0017(10) O4 0.0197(12) 0.0203(12) 0.0238(12) -0.0003(10) 0.0011(10) 0.0032(10) N 0.0314(14) 0.0200(12) 0.0277(12) 0.0015(15) 0.0060(10) 0.0009(15) C1 0.0240(18) 0.0175(16) 0.0189(16) 0.0005(13) 0.0051(14) -0.0012(13) C2 0.0217(18) 0.0238(17) 0.0186(16) 0.0011(13) 0.0050(13) 0.0023(14) C3 0.0220(17) 0.0296(19) 0.0173(16) -0.0013(13) 0.0003(13) -0.0022(14) C4 0.0264(18) 0.0221(17) 0.0198(16) -0.0021(13) 0.0049(13) 0.0007(14) C5 0.0233(18) 0.0289(18) 0.0224(17) 0.0022(14) 0.0034(14) 0.0005(15) C6 0.0260(18) 0.0238(17) 0.0213(16) 0.0031(13) 0.0015(14) -0.0017(14) C7 0.0200(17) 0.0275(18) 0.0215(17) -0.0020(14) 0.0035(13) -0.0015(14) C8 0.0147(16) 0.0261(18) 0.0244(17) -0.0029(14) 0.0015(13) -0.0027(14) C9 0.0170(16) 0.0282(18) 0.0228(16) -0.0058(14) 0.0012(13) 0.0016(14) C10 0.0136(16) 0.0272(19) 0.0330(18) -0.0036(15) -0.0021(14) -0.0008(14) C11 0.0215(17) 0.0269(18) 0.0254(17) 0.0047(14) 0.0022(14) -0.0022(14) C12 0.0170(17) 0.0264(18) 0.0201(17) 0.0009(14) 0.0005(13) -0.0052(14) C13 0.0164(16) 0.0205(17) 0.0225(17) -0.0022(14) -0.0014(13) -0.0035(13) C14 0.0240(18) 0.0257(18) 0.0217(17) -0.0017(14) 0.0009(14) -0.0043(14) C15 0.0234(18) 0.0302(19) 0.0164(16) -0.0040(14) 0.0034(14) 0.0022(14) C16 0.0236(18) 0.0282(19) 0.0196(17) 0.0002(13) -0.0010(14) 0.0002(14) C17 0.0250(18) 0.0293(19) 0.0209(16) 0.0006(14) 0.0041(14) 0.0012(15) C18 0.0181(16) 0.0284(18) 0.0207(16) -0.0006(14) 0.0031(13) -0.0052(14) C19 0.0217(18) 0.0259(18) 0.0163(15) -0.0031(13) 0.0029(13) 0.0005(14) C20 0.0246(18) 0.0174(16) 0.0164(15) -0.0016(12) 0.0018(13) -0.0021(13) C21 0.0208(17) 0.0267(18) 0.0235(17) -0.0008(14) 0.0048(14) -0.0005(14) C22 0.0161(17) 0.0257(18) 0.0221(17) 0.0019(14) -0.0017(13) 0.0050(14) C23 0.0193(17) 0.0237(18) 0.0287(18) 0.0019(14) 0.0011(14) -0.0002(14) C24 0.0212(17) 0.0215(18) 0.0330(19) -0.0023(14) -0.0034(14) -0.0002(14) C25 0.0211(17) 0.0279(18) 0.0219(17) -0.0056(14) -0.0020(14) 0.0028(14) C26 0.0178(17) 0.0246(18) 0.0240(17) 0.0019(14) -0.0016(14) 0.0032(14) C27 0.0173(17) 0.0215(18) 0.0263(18) -0.0020(14) -0.0027(14) 0.0008(13) C28 0.0210(17) 0.0280(18) 0.0159(16) -0.0005(13) -0.0009(13) 0.0011(14) C29 0.033(2) 0.0301(19) 0.0242(17) -0.0071(15) 0.0035(15) 0.0036(16) C30 0.050(2) 0.041(2) 0.0327(19) -0.0076(17) 0.0157(18) 0.0068(19) C31 0.046(3) 0.121(5) 0.094(4) -0.089(4) -0.013(3) 0.024(3) C32 0.110(4) 0.032(2) 0.035(2) -0.0049(18) 0.019(2) 0.015(2) C33 0.0274(19) 0.0296(19) 0.040(2) 0.0043(16) 0.0030(16) 0.0059(16) C34 0.029(2) 0.049(3) 0.076(3) -0.002(2) -0.009(2) 0.0118(19) C35 0.081(4) 0.040(3) 0.079(4) 0.018(3) 0.024(3) 0.024(3) C36 0.063(3) 0.031(2) 0.063(3) -0.009(2) -0.012(2) 0.012(2) C37 0.034(2) 0.032(2) 0.0293(18) 0.0091(15) 0.0075(16) -0.0046(16) C38 0.125(6) 0.151(7) 0.089(5) 0.090(5) -0.065(4) -0.086(5) C39 0.038(3) 0.305(13) 0.267(11) 0.266(11) 0.000(5) -0.008(5) C40 0.136(6) 0.066(4) 0.095(4) 0.035(4) 0.043(4) 0.020(4) C41 0.0274(19) 0.0229(18) 0.041(2) -0.0026(16) -0.0040(16) -0.0047(15) C42 0.052(3) 0.031(2) 0.063(3) -0.019(2) 0.003(2) -0.0122(19) C43 0.031(2) 0.034(2) 0.058(3) -0.0012(19) -0.0055(19) -0.0086(17) C44 0.054(3) 0.025(2) 0.068(3) 0.006(2) -0.020(2) -0.0084(19) C45 0.0241(18) 0.0235(19) 0.0271(18) 0.0055(14) -0.0022(15) 0.0072(14) C46 0.0220(18) 0.0276(18) 0.0251(18) 0.0069(14) -0.0031(14) 0.0073(15) C47 0.0273(19) 0.041(2) 0.0317(19) -0.0038(17) -0.0022(16) 0.0061(17) C48 0.035(2) 0.063(3) 0.030(2) -0.0012(19) 0.0073(17) 0.010(2) C49 0.027(2) 0.063(3) 0.048(2) 0.020(2) 0.0069(18) 0.004(2) C50 0.029(2) 0.037(2) 0.052(3) 0.009(2) -0.0004(19) -0.0046(18) C51 0.034(2) 0.032(2) 0.034(2) -0.0014(17) -0.0050(17) 0.0072(18) C52 0.0274(19) 0.025(2) 0.039(2) -0.0097(16) 0.0016(16) -0.0087(16) C53 0.0271(19) 0.0257(18) 0.0295(18) -0.0025(15) -0.0004(15) -0.0096(16) C54 0.029(2) 0.063(3) 0.052(3) 0.021(2) -0.0073(19) -0.010(2) C55 0.039(3) 0.126(5) 0.042(3) 0.023(3) 0.002(2) -0.026(3) C56 0.027(2) 0.101(4) 0.053(3) -0.021(3) 0.003(2) -0.002(3) C57 0.025(2) 0.050(3) 0.092(4) -0.017(3) -0.010(2) 0.002(2) C58 0.0214(19) 0.035(2) 0.058(3) 0.002(2) -0.0045(18) -0.0038(17) C59 0.052(2) 0.051(2) 0.035(2) 0.0122(18) 0.0104(18) -0.010(2) C60 0.084(4) 0.038(3) 0.055(3) 0.012(2) 0.000(3) 0.016(2) C61 0.105(4) 0.036(3) 0.048(3) -0.016(2) 0.014(3) -0.027(3) C62 0.064(3) 0.040(2) 0.035(2) -0.0080(17) 0.0134(19) 0.000(2) C70 0.131(7) 0.058(3) 0.104(5) 0.005(4) 0.018(5) -0.013(4) C71 0.052(3) 0.052(3) 0.073(3) 0.011(3) 0.007(2) 0.006(2) C72 0.049(3) 0.047(3) 0.041(2) -0.003(2) 0.0080(19) -0.003(2) C73 0.050(3) 0.062(3) 0.051(3) 0.015(2) 0.008(2) 0.001(2) C74 0.0313(17) 0.055(2) 0.048(2) -0.010(2) 0.0018(16) 0.002(2) C75 0.044(3) 0.071(3) 0.052(3) -0.012(3) 0.000(2) -0.008(3) C76 0.047(3) 0.066(3) 0.035(2) 0.008(2) 0.0021(19) 0.005(2) C80 0.111(5) 0.084(4) 0.067(4) 0.010(3) -0.007(3) -0.020(4) C81 0.101(5) 0.060(3) 0.046(3) -0.002(3) -0.026(3) -0.004(3) C82 0.093(4) 0.080(4) 0.065(3) 0.012(3) -0.023(3) -0.023(4) C83 0.104(5) 0.085(5) 0.090(5) 0.031(4) -0.025(4) -0.025(4) C84 0.108(6) 0.062(4) 0.082(4) -0.002(3) -0.035(4) -0.012(4) C85 0.100(5) 0.087(5) 0.052(3) -0.019(3) -0.019(3) -0.008(4) C86 0.104(5) 0.063(4) 0.044(3) -0.002(3) -0.011(3) -0.026(3) C90 0.077(4) 0.121(6) 0.108(5) -0.035(5) -0.011(4) -0.014(4) C91 0.066(3) 0.083(4) 0.040(3) -0.017(3) -0.001(2) -0.027(3) C92 0.100(5) 0.068(4) 0.057(3) 0.001(3) 0.004(3) -0.040(4) C93 0.105(5) 0.059(4) 0.064(4) -0.004(3) -0.013(3) -0.013(3) C94 0.080(4) 0.076(4) 0.046(3) -0.025(3) -0.003(3) -0.019(3) C95 0.096(4) 0.083(4) 0.034(2) -0.015(2) 0.008(3) -0.049(4) C96 0.095(4) 0.061(3) 0.036(2) -0.006(2) -0.009(3) -0.027(3) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc O1 1.912(2) . . yes Sc O2 2.278(2) . . yes Sc O3 1.912(2) . . yes Sc O4 2.248(2) . . yes Sc N 2.060(2) . . yes Si1 N 1.724(3) . . yes Si1 C59 1.863(4) . . yes Si1 C60 1.870(5) . . yes Si2 N 1.718(3) . . yes Si2 C61 1.854(6) . . yes Si2 C62 1.854(4) . . yes Si1 H1 1.40(4) . . no Si2 H2 1.44(4) . . no O1 C1 1.334(4) . . yes O2 C13 1.420(4) . . yes O2 C52 1.476(4) . . yes O3 C20 1.343(4) . . yes O4 C27 1.413(4) . . yes O4 C45 1.486(4) . . yes C1 C2 1.403(5) . . no C1 C6 1.398(5) . . no C2 C3 1.382(5) . . no C2 C28 1.525(5) . . no C3 C4 1.406(5) . . no C4 C5 1.395(5) . . no C4 C29 1.536(5) . . no C5 C6 1.384(5) . . no C6 C7 1.522(5) . . no C7 C8 1.521(5) . . no C8 C13 1.396(5) . . no C8 C9 1.392(5) . . no C9 C10 1.396(5) . . no C10 C11 1.376(5) . . no C10 C33 1.540(5) . . no C11 C12 1.402(5) . . no C12 C14 1.512(5) . . no C12 C13 1.398(5) . . no C14 C15 1.514(5) . . no C15 C20 1.401(5) . . no C15 C16 1.398(5) . . no C16 C17 1.388(5) . . no C17 C37 1.539(5) . . no C17 C18 1.410(5) . . no C18 C19 1.405(5) . . no C19 C21 1.506(5) . . no C19 C20 1.399(5) . . no C21 C22 1.531(5) . . no C22 C23 1.384(5) . . no C22 C27 1.404(5) . . no C23 C24 1.392(5) . . no C24 C41 1.536(5) . . no C24 C25 1.387(5) . . no C25 C26 1.388(5) . . no C26 C28 1.527(5) . . no C26 C27 1.407(5) . . no C29 C30 1.516(5) . . no C29 C31 1.517(7) . . no C29 C32 1.557(5) . . no C33 C34 1.525(5) . . no C33 C36 1.536(6) . . no C33 C35 1.516(6) . . no C37 C39 1.424(7) . . no C37 C38 1.498(8) . . no C37 C40 1.547(7) . . no C41 C43 1.537(5) . . no C41 C42 1.535(6) . . no C41 C44 1.514(6) . . no C45 C46 1.505(5) . . no C46 C51 1.394(5) . . no C46 C47 1.379(5) . . no C47 C48 1.397(5) . . no C48 C49 1.381(6) . . no C49 C50 1.369(7) . . no C50 C51 1.387(5) . . no C52 C53 1.496(5) . . no C53 C58 1.386(5) . . no C53 C54 1.391(6) . . no C54 C55 1.368(7) . . no C55 C56 1.350(9) . . no C56 C57 1.378(8) . . no C57 C58 1.364(5) . . no C3 H3 0.9504 . . no C5 H5 0.9511 . . no C7 H7A 0.9898 . . no C7 H7B 0.9906 . . no C9 H9 0.9507 . . no C11 H11 0.9498 . . no C14 H14A 0.9892 . . no C14 H14B 0.9904 . . no C16 H16 0.9497 . . no C18 H18 0.9495 . . no C21 H21A 0.9897 . . no C21 H21B 0.9910 . . no C23 H23 0.9511 . . no C25 H25 0.9504 . . no C28 H28A 0.9907 . . no C28 H28B 0.9906 . . no C30 H30A 0.9804 . . no C30 H30B 0.9805 . . no C30 H30C 0.9811 . . no C31 H31A 0.9815 . . no C31 H31B 0.9802 . . no C31 H31C 0.9809 . . no C32 H32A 0.9793 . . no C32 H32B 0.9803 . . no C32 H32C 0.9804 . . no C34 H34A 0.9785 . . no C34 H34B 0.9800 . . no C34 H34C 0.9791 . . no C35 H35A 0.9795 . . no C35 H35B 0.9808 . . no C35 H35C 0.9802 . . no C36 H36A 0.9798 . . no C36 H36B 0.9795 . . no C36 H36C 0.9805 . . no C38 H38A 0.9811 . . no C38 H38B 0.9794 . . no C38 H38C 0.9793 . . no C39 H39A 0.9798 . . no C39 H39B 0.9813 . . no C39 H39C 0.9806 . . no C40 H40A 0.9796 . . no C40 H40B 0.9787 . . no C40 H40C 0.9797 . . no C42 H42A 0.9810 . . no C42 H42B 0.9800 . . no C42 H42C 0.9792 . . no C43 H43A 0.9798 . . no C43 H43B 0.9808 . . no C43 H43C 0.9791 . . no C44 H44A 0.9801 . . no C44 H44B 0.9809 . . no C44 H44C 0.9798 . . no C45 H45A 0.9908 . . no C45 H45B 0.9900 . . no C47 H47 0.9497 . . no C48 H48 0.9490 . . no C49 H49 0.9502 . . no C50 H50 0.9507 . . no C51 H51 0.9499 . . no C52 H52A 0.9893 . . no C52 H52B 0.9899 . . no C54 H54 0.9497 . . no C55 H55 0.9498 . . no C56 H56 0.9492 . . no C57 H57 0.9502 . . no C58 H58 0.9498 . . no C59 H59A 0.9793 . . no C59 H59B 0.9792 . . no C59 H59C 0.9810 . . no C60 H60A 0.9804 . . no C60 H60B 0.9794 . . no C60 H60C 0.9808 . . no C61 H61A 0.9806 . . no C61 H61B 0.9805 . . no C61 H61C 0.9804 . . no C62 H62A 0.9787 . . no C62 H62B 0.9799 . . no C62 H62C 0.9796 . . no C70 C71 1.460(7) . . no C71 C72 1.377(7) . . no C71 C76 1.423(7) . . no C72 C73 1.369(7) . . no C73 C74 1.364(7) . . no C74 C75 1.437(7) . . no C75 C76 1.332(7) . . no C70 H70A 0.9795 . . no C70 H70B 0.9807 . . no C70 H70C 0.9806 . . no C72 H72 0.9509 . . no C73 H73 0.9506 . . no C74 H74 0.9498 . . no C75 H75 0.9510 . . no C76 H76 0.9506 . . no C80 C81 1.520(9) . . no C81 C82 1.383(8) . . no C81 C86 1.404(10) . . no C82 C83 1.352(10) . . no C83 C84 1.378(11) . . no C84 C85 1.383(10) . . no C85 C86 1.377(9) . . no C80 H80A 0.9802 . . no C80 H80B 0.9797 . . no C80 H80C 0.9805 . . no C82 H82 0.9503 . . no C83 H83 0.9494 . . no C84 H84 0.9509 . . no C85 H85 0.9501 . . no C86 H86 0.9481 . . no C90 C91 1.513(9) . . no C91 C92 1.391(10) . . no C91 C96 1.371(9) . . no C92 C93 1.373(10) . . no C93 C94 1.362(9) . . no C94 C95 1.380(10) . . no C95 C96 1.363(10) . . no C90 H90A 0.9792 . . no C90 H90B 0.9796 . . no C90 H90C 0.9809 . . no C92 H92 0.9504 . . no C93 H93 0.9503 . . no C94 H94 0.9504 . . no C95 H95 0.9504 . . no C96 H96 0.9508 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sc O2 85.01(9) . . . yes O1 Sc O3 126.24(11) . . . yes O1 Sc O4 88.02(9) . . . yes O1 Sc N 113.92(12) . . . yes O2 Sc O3 86.34(9) . . . yes O2 Sc O4 162.65(8) . . . yes O2 Sc N 100.01(12) . . . yes O3 Sc O4 85.02(9) . . . yes O3 Sc N 119.84(12) . . . yes O4 Sc N 97.34(12) . . . yes N Si1 C59 111.88(17) . . . yes N Si1 C60 113.95(19) . . . yes C59 Si1 C60 109.9(2) . . . yes N Si2 C61 112.1(2) . . . yes N Si2 C62 112.59(16) . . . yes C61 Si2 C62 107.2(2) . . . yes C60 Si1 H1 112.0(15) . . . no N Si1 H1 104.7(15) . . . no C59 Si1 H1 103.8(14) . . . no N Si2 H2 109.5(14) . . . no C61 Si2 H2 108.2(15) . . . no C62 Si2 H2 107.0(14) . . . no Sc O1 C1 161.2(2) . . . yes C13 O2 C52 113.2(2) . . . yes Sc O2 C13 114.10(18) . . . yes Sc O2 C52 131.67(19) . . . yes Sc O3 C20 164.1(2) . . . yes Sc O4 C27 114.15(19) . . . yes Sc O4 C45 131.12(18) . . . yes C27 O4 C45 113.2(2) . . . yes Si1 N Si2 121.64(14) . . . yes Sc N Si2 124.42(18) . . . yes Sc N Si1 113.88(16) . . . yes O1 C1 C2 120.4(3) . . . yes O1 C1 C6 120.0(3) . . . yes C2 C1 C6 119.5(3) . . . no C1 C2 C3 119.8(3) . . . no C1 C2 C28 117.4(3) . . . no C3 C2 C28 122.8(3) . . . no C2 C3 C4 121.8(3) . . . no C3 C4 C5 117.0(3) . . . no C3 C4 C29 122.7(3) . . . no C5 C4 C29 120.3(3) . . . no C4 C5 C6 122.5(3) . . . no C5 C6 C7 122.5(3) . . . no C1 C6 C7 118.1(3) . . . no C1 C6 C5 119.3(3) . . . no C6 C7 C8 111.4(3) . . . no C7 C8 C13 123.7(3) . . . no C7 C8 C9 118.9(3) . . . no C9 C8 C13 117.4(3) . . . no C8 C9 C10 122.6(3) . . . no C9 C10 C11 117.2(3) . . . no C9 C10 C33 120.3(3) . . . no C11 C10 C33 122.3(3) . . . no C10 C11 C12 123.4(3) . . . no C11 C12 C13 116.6(3) . . . no C13 C12 C14 124.5(3) . . . no C11 C12 C14 118.9(3) . . . no O2 C13 C8 118.6(3) . . . yes C8 C13 C12 122.4(3) . . . no O2 C13 C12 118.9(3) . . . yes C12 C14 C15 111.3(3) . . . no C14 C15 C20 118.8(3) . . . no C14 C15 C16 122.9(3) . . . no C16 C15 C20 118.2(3) . . . no C15 C16 C17 122.7(3) . . . no C16 C17 C18 117.6(3) . . . no C16 C17 C37 120.9(3) . . . no C18 C17 C37 121.5(3) . . . no C17 C18 C19 121.6(3) . . . no C18 C19 C20 118.4(3) . . . no C18 C19 C21 123.0(3) . . . no C20 C19 C21 118.5(3) . . . no C15 C20 C19 121.4(3) . . . no O3 C20 C15 119.1(3) . . . yes O3 C20 C19 119.6(3) . . . yes C19 C21 C22 112.8(3) . . . no C23 C22 C27 117.5(3) . . . no C21 C22 C23 119.3(3) . . . no C21 C22 C27 123.3(3) . . . no C22 C23 C24 123.1(3) . . . no C25 C24 C41 122.1(3) . . . no C23 C24 C25 117.3(3) . . . no C23 C24 C41 120.5(3) . . . no C24 C25 C26 122.8(3) . . . no C27 C26 C28 124.1(3) . . . no C25 C26 C27 117.6(3) . . . no C25 C26 C28 118.3(3) . . . no O4 C27 C26 119.8(3) . . . yes C22 C27 C26 121.5(3) . . . no O4 C27 C22 118.6(3) . . . yes C2 C28 C26 110.4(3) . . . no C4 C29 C32 109.0(3) . . . no C30 C29 C31 106.5(3) . . . no C4 C29 C30 110.2(3) . . . no C4 C29 C31 112.9(4) . . . no C30 C29 C32 108.0(3) . . . no C31 C29 C32 110.1(4) . . . no C34 C33 C36 109.1(3) . . . no C10 C33 C34 107.5(3) . . . no C10 C33 C35 112.3(3) . . . no C10 C33 C36 111.8(3) . . . no C34 C33 C35 108.5(3) . . . no C35 C33 C36 107.6(3) . . . no C38 C37 C40 99.2(4) . . . no C17 C37 C39 114.0(5) . . . no C39 C37 C40 115.6(5) . . . no C17 C37 C38 111.2(4) . . . no C17 C37 C40 108.6(3) . . . no C38 C37 C39 107.3(5) . . . no C24 C41 C43 107.1(3) . . . no C24 C41 C42 112.1(3) . . . no C42 C41 C44 108.8(3) . . . no C24 C41 C44 111.5(3) . . . no C42 C41 C43 107.7(3) . . . no C43 C41 C44 109.5(3) . . . no O4 C45 C46 112.2(3) . . . yes C45 C46 C51 120.9(3) . . . no C45 C46 C47 120.8(3) . . . no C47 C46 C51 118.3(3) . . . no C46 C47 C48 121.0(4) . . . no C47 C48 C49 119.5(4) . . . no C48 C49 C50 120.5(4) . . . no C49 C50 C51 119.8(4) . . . no C46 C51 C50 121.0(4) . . . no O2 C52 C53 113.5(3) . . . yes C52 C53 C54 120.5(3) . . . no C52 C53 C58 121.8(3) . . . no C54 C53 C58 117.8(3) . . . no C53 C54 C55 120.0(4) . . . no C54 C55 C56 121.7(5) . . . no C55 C56 C57 119.0(5) . . . no C56 C57 C58 120.4(4) . . . no C53 C58 C57 121.0(4) . . . no C2 C3 H3 119.18 . . . no C4 C3 H3 119.07 . . . no C4 C5 H5 118.69 . . . no C6 C5 H5 118.77 . . . no C6 C7 H7A 109.35 . . . no C6 C7 H7B 109.34 . . . no C8 C7 H7A 109.37 . . . no C8 C7 H7B 109.32 . . . no H7A C7 H7B 107.97 . . . no C8 C9 H9 118.69 . . . no C10 C9 H9 118.68 . . . no C10 C11 H11 118.29 . . . no C12 C11 H11 118.27 . . . no C12 C14 H14A 109.39 . . . no C12 C14 H14B 109.34 . . . no C15 C14 H14A 109.38 . . . no C15 C14 H14B 109.37 . . . no H14A C14 H14B 107.99 . . . no C15 C16 H16 118.62 . . . no C17 C16 H16 118.71 . . . no C17 C18 H18 119.24 . . . no C19 C18 H18 119.12 . . . no C19 C21 H21A 109.08 . . . no C19 C21 H21B 109.03 . . . no C22 C21 H21A 109.01 . . . no C22 C21 H21B 109.00 . . . no H21A C21 H21B 107.76 . . . no C22 C23 H23 118.47 . . . no C24 C23 H23 118.48 . . . no C24 C25 H25 118.69 . . . no C26 C25 H25 118.49 . . . no C2 C28 H28A 109.58 . . . no C2 C28 H28B 109.63 . . . no C26 C28 H28A 109.58 . . . no C26 C28 H28B 109.56 . . . no H28A C28 H28B 108.07 . . . no C29 C30 H30A 109.52 . . . no C29 C30 H30B 109.47 . . . no C29 C30 H30C 109.49 . . . no H30A C30 H30B 109.40 . . . no H30A C30 H30C 109.44 . . . no H30B C30 H30C 109.50 . . . no C29 C31 H31A 109.42 . . . no C29 C31 H31B 109.56 . . . no C29 C31 H31C 109.48 . . . no H31A C31 H31B 109.45 . . . no H31A C31 H31C 109.35 . . . no H31B C31 H31C 109.57 . . . no C29 C32 H32A 109.55 . . . no C29 C32 H32B 109.50 . . . no C29 C32 H32C 109.40 . . . no H32A C32 H32B 109.49 . . . no H32A C32 H32C 109.41 . . . no H32B C32 H32C 109.47 . . . no C33 C34 H34A 109.51 . . . no C33 C34 H34B 109.42 . . . no C33 C34 H34C 109.56 . . . no H34A C34 H34B 109.42 . . . no H34A C34 H34C 109.48 . . . no H34B C34 H34C 109.44 . . . no C33 C35 H35A 109.53 . . . no C33 C35 H35B 109.48 . . . no C33 C35 H35C 109.52 . . . no H35A C35 H35B 109.44 . . . no H35A C35 H35C 109.50 . . . no H35B C35 H35C 109.35 . . . no C33 C36 H36A 109.44 . . . no C33 C36 H36B 109.46 . . . no C33 C36 H36C 109.45 . . . no H36A C36 H36B 109.56 . . . no H36A C36 H36C 109.47 . . . no H36B C36 H36C 109.45 . . . no C37 C38 H38A 109.45 . . . no C37 C38 H38B 109.49 . . . no C37 C38 H38C 109.55 . . . no H38A C38 H38B 109.40 . . . no H38A C38 H38C 109.54 . . . no H38B C38 H38C 109.40 . . . no C37 C39 H39A 109.62 . . . no C37 C39 H39B 109.51 . . . no C37 C39 H39C 109.58 . . . no H39A C39 H39B 109.30 . . . no H39A C39 H39C 109.41 . . . no H39B C39 H39C 109.40 . . . no C37 C40 H40A 109.47 . . . no C37 C40 H40B 109.46 . . . no C37 C40 H40C 109.44 . . . no H40A C40 H40B 109.59 . . . no H40A C40 H40C 109.38 . . . no H40B C40 H40C 109.49 . . . no C41 C42 H42A 109.43 . . . no C41 C42 H42B 109.45 . . . no C41 C42 H42C 109.56 . . . no H42A C42 H42B 109.40 . . . no H42A C42 H42C 109.53 . . . no H42B C42 H42C 109.46 . . . no C41 C43 H43A 109.41 . . . no C41 C43 H43B 109.42 . . . no C41 C43 H43C 109.47 . . . no H43A C43 H43B 109.47 . . . no H43A C43 H43C 109.56 . . . no H43B C43 H43C 109.50 . . . no C41 C44 H44A 109.49 . . . no C41 C44 H44B 109.52 . . . no C41 C44 H44C 109.37 . . . no H44A C44 H44B 109.45 . . . no H44A C44 H44C 109.49 . . . no H44B C44 H44C 109.51 . . . no O4 C45 H45A 109.25 . . . no O4 C45 H45B 109.16 . . . no C46 C45 H45A 109.22 . . . no C46 C45 H45B 109.23 . . . no H45A C45 H45B 107.72 . . . no C46 C47 H47 119.44 . . . no C48 C47 H47 119.59 . . . no C47 C48 H48 120.28 . . . no C49 C48 H48 120.27 . . . no C48 C49 H49 119.80 . . . no C50 C49 H49 119.73 . . . no C49 C50 H50 120.15 . . . no C51 C50 H50 120.06 . . . no C46 C51 H51 119.45 . . . no C50 C51 H51 119.55 . . . no O2 C52 H52A 108.87 . . . no O2 C52 H52B 108.90 . . . no C53 C52 H52A 108.83 . . . no C53 C52 H52B 108.82 . . . no H52A C52 H52B 107.78 . . . no C53 C54 H54 119.99 . . . no C55 C54 H54 119.98 . . . no C54 C55 H55 119.16 . . . no C56 C55 H55 119.11 . . . no C55 C56 H56 120.38 . . . no C57 C56 H56 120.57 . . . no C56 C57 H57 119.75 . . . no C58 C57 H57 119.88 . . . no C53 C58 H58 119.45 . . . no C57 C58 H58 119.52 . . . no Si1 C59 H59A 109.50 . . . no Si1 C59 H59B 109.49 . . . no Si1 C59 H59C 109.49 . . . no H59A C59 H59B 109.49 . . . no H59A C59 H59C 109.43 . . . no H59B C59 H59C 109.43 . . . no Si1 C60 H60A 109.42 . . . no Si1 C60 H60B 109.52 . . . no Si1 C60 H60C 109.54 . . . no H60A C60 H60B 109.48 . . . no H60A C60 H60C 109.35 . . . no H60B C60 H60C 109.51 . . . no Si2 C61 H61A 109.48 . . . no Si2 C61 H61B 109.53 . . . no Si2 C61 H61C 109.46 . . . no H61A C61 H61B 109.39 . . . no H61A C61 H61C 109.44 . . . no H61B C61 H61C 109.54 . . . no Si2 C62 H62A 109.46 . . . no Si2 C62 H62B 109.39 . . . no Si2 C62 H62C 109.41 . . . no H62A C62 H62B 109.48 . . . no H62A C62 H62C 109.65 . . . no H62B C62 H62C 109.43 . . . no C70 C71 C72 122.6(5) . . . no C70 C71 C76 121.7(5) . . . no C72 C71 C76 115.7(4) . . . no C71 C72 C73 123.1(5) . . . no C72 C73 C74 121.8(5) . . . no C73 C74 C75 115.8(4) . . . no C74 C75 C76 122.2(5) . . . no C71 C76 C75 121.3(5) . . . no C71 C70 H70A 109.36 . . . no C71 C70 H70B 109.49 . . . no C71 C70 H70C 109.48 . . . no H70A C70 H70B 109.53 . . . no H70A C70 H70C 109.55 . . . no H70B C70 H70C 109.42 . . . no C71 C72 H72 118.41 . . . no C73 C72 H72 118.53 . . . no C72 C73 H73 119.12 . . . no C74 C73 H73 119.08 . . . no C73 C74 H74 122.08 . . . no C75 C74 H74 122.12 . . . no C74 C75 H75 118.97 . . . no C76 C75 H75 118.81 . . . no C71 C76 H76 119.26 . . . no C75 C76 H76 119.42 . . . no C80 C81 C82 119.3(6) . . . no C80 C81 C86 121.4(5) . . . no C82 C81 C86 119.3(5) . . . no C81 C82 C83 119.3(6) . . . no C82 C83 C84 122.3(7) . . . no C83 C84 C85 119.2(7) . . . no C84 C85 C86 119.5(6) . . . no C81 C86 C85 120.4(5) . . . no C81 C80 H80A 109.56 . . . no C81 C80 H80B 109.44 . . . no C81 C80 H80C 109.51 . . . no H80A C80 H80B 109.45 . . . no H80A C80 H80C 109.41 . . . no H80B C80 H80C 109.46 . . . no C81 C82 H82 120.35 . . . no C83 C82 H82 120.33 . . . no C82 C83 H83 118.82 . . . no C84 C83 H83 118.84 . . . no C83 C84 H84 120.47 . . . no C85 C84 H84 120.33 . . . no C84 C85 H85 120.35 . . . no C86 C85 H85 120.20 . . . no C81 C86 H86 119.83 . . . no C85 C86 H86 119.81 . . . no C90 C91 C92 120.5(6) . . . no C90 C91 C96 122.1(6) . . . no C92 C91 C96 117.5(5) . . . no C91 C92 C93 121.4(6) . . . no C92 C93 C94 119.8(7) . . . no C93 C94 C95 119.6(6) . . . no C94 C95 C96 120.2(6) . . . no C91 C96 C95 121.5(5) . . . no C91 C90 H90A 109.48 . . . no C91 C90 H90B 109.63 . . . no C91 C90 H90C 109.50 . . . no H90A C90 H90B 109.47 . . . no H90A C90 H90C 109.37 . . . no H90B C90 H90C 109.39 . . . no C91 C92 H92 119.31 . . . no C93 C92 H92 119.33 . . . no C92 C93 H93 120.04 . . . no C94 C93 H93 120.14 . . . no C93 C94 H94 120.12 . . . no C95 C94 H94 120.29 . . . no C94 C95 H95 119.88 . . . no C96 C95 H95 119.92 . . . no C91 C96 H96 119.26 . . . no C95 C96 H96 119.21 . . . no # End of Crystallographic Information File data_ESTC-4144-173 _database_code_CSD 182441 #=================================================================== # 0. AUDIT DETAILS _audit_creation_date 22-Jun-01 _audit_creation_method 'PLATON
option' _audit_update_record ; 7-Feb-02 Updated by the Author E.H. Textwriting by E.H. Checkcif OK 12-Feb-02 Updated by the Author E.H. ; #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C46 H48 Lu N O4 Si2, C7 H8' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C53 H56 Lu N O4 Si2' _chemical_formula_weight 1002.14 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.3794(1) _cell_length_b 14.0015(2) _cell_length_c 16.9067(3) _cell_angle_alpha 69.3972(6) _cell_angle_beta 75.8968(6) _cell_angle_gamma 69.8248(8) _cell_volume 2343.69(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 6876 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 25.38 _exptl_crystal_description 'fragment' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method none _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 2.203 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8629 _exptl_absorpt_correction_T_max 0.9077 _exptl_absorpt_process_details ; not applied ; _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 15 s per film repetition 1 443 films measured in 2 data sets set 1: phi-scan with delta_phi = 1.0 set 2 to set 2 omega-scan with delta_omega = 1.0 ; _publ_section_exptl_prep ; the crystal was fixed in a capillary with perfluorinated ether and transfered to the diffractometer ; _publ_section_exptl_refinement ; straight forward after integration with the program NPROCESS; source: 'Denzo-SMN (Nonius, 2000b)' Hydrogen atoms could be located in the difference Fourier maps and refined freely only for the Si-H spezies. All other hydrogen atoms are calculated in ideal positions riding on the parent carbon atom with U(iso) 1.2 times U(iso) parent carbon atom. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Kappa CCD (Nonius)' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 21461 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.38 _reflns_number_total 8139 _reflns_number_gt 7126 # number of observed reflections (> n sig(I)) _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2000a)' _computing_cell_refinement 'DENZO (Nonius, 2000b)' _computing_data_reduction 'DENZO (Nonius, 2000b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+12.9760P] 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 8139 _refine_ls_number_parameters 563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 1.254 _refine_diff_density_min -1.026 _refine_diff_density_rms 0.091 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Lu Lu Uani 0.15489(1) 0.12960(1) 0.22621(1) 1.000 0.0254(1) . . Si1 Si Uani 0.12378(12) -0.08029(10) 0.37838(8) 1.000 0.0397(4) . . Si2 Si Uani 0.33319(13) -0.13215(10) 0.24062(9) 1.000 0.0500(5) . . O1 O Uani -0.0167(2) 0.2201(2) 0.26205(18) 1.000 0.0348(9) . . O2 O Uani 0.0600(2) 0.14607(19) 0.11134(16) 1.000 0.0254(8) . . O3 O Uani 0.2802(3) 0.1928(2) 0.13458(17) 1.000 0.0326(9) . . O4 O Uani 0.2291(2) 0.1874(2) 0.31479(16) 1.000 0.0309(9) . . N N Uani 0.2089(3) -0.0436(3) 0.2802(2) 1.000 0.0325(11) . . C1 C Uani -0.1190(4) 0.3000(3) 0.2714(2) 1.000 0.0286(12) . . C2 C Uani -0.1270(4) 0.3518(3) 0.3305(2) 1.000 0.0305(12) . . C3 C Uani -0.2362(4) 0.4320(3) 0.3428(3) 1.000 0.0368(16) . . C4 C Uani -0.3331(4) 0.4626(3) 0.2955(3) 1.000 0.0386(14) . . C5 C Uani -0.3227(4) 0.4130(3) 0.2357(3) 1.000 0.0333(12) . . C6 C Uani -0.2158(4) 0.3322(3) 0.2218(2) 1.000 0.0276(12) . . C7 C Uani -0.1957(4) 0.2763(3) 0.1550(3) 1.000 0.0303(12) . . C8 C Uani -0.1039(3) 0.3135(3) 0.0770(2) 1.000 0.0255(12) . . C9 C Uani -0.1426(4) 0.4149(3) 0.0214(3) 1.000 0.0336(14) . . C10 C Uani -0.0643(4) 0.4531(3) -0.0499(3) 1.000 0.0368(16) . . C11 C Uani 0.0579(4) 0.3913(3) -0.0666(3) 1.000 0.0336(12) . . C12 C Uani 0.1028(4) 0.2888(3) -0.0121(2) 1.000 0.0283(12) . . C13 C Uani 0.0194(3) 0.2516(3) 0.0577(2) 1.000 0.0232(12) . . C14 C Uani 0.2411(4) 0.2274(3) -0.0308(2) 1.000 0.0281(12) . . C15 C Uani 0.3297(3) 0.2744(3) -0.0127(3) 1.000 0.0284(12) . . C16 C Uani 0.3974(4) 0.3367(3) -0.0758(3) 1.000 0.0334(12) . . C17 C Uani 0.4739(4) 0.3805(3) -0.0556(3) 1.000 0.0362(14) . . C18 C Uani 0.4830(4) 0.3629(3) 0.0290(3) 1.000 0.0339(14) . . C19 C Uani 0.4170(4) 0.3008(3) 0.0944(3) 1.000 0.0302(12) . . C20 C Uani 0.3407(4) 0.2552(3) 0.0727(3) 1.000 0.0296(12) . . C21 C Uani 0.4206(4) 0.2793(3) 0.1875(3) 1.000 0.0333(14) . . C22 C Uani 0.2989(4) 0.3431(3) 0.2286(3) 1.000 0.0321(14) . . C23 C Uani 0.2732(4) 0.4532(4) 0.2043(3) 1.000 0.0422(17) . . C24 C Uani 0.1623(5) 0.5169(4) 0.2353(3) 1.000 0.0444(17) . . C25 C Uani 0.0715(4) 0.4720(4) 0.2906(3) 1.000 0.0392(17) . . C26 C Uani 0.0921(4) 0.3618(3) 0.3182(2) 1.000 0.0315(14) . . C27 C Uani 0.2070(4) 0.2996(3) 0.2877(2) 1.000 0.0292(12) . . C28 C Uani -0.0149(4) 0.3198(3) 0.3764(3) 1.000 0.0344(14) . . C45 C Uani 0.2738(4) 0.1332(4) 0.3992(3) 1.000 0.0369(14) . . C46 C Uani 0.4129(4) 0.1159(3) 0.3925(2) 1.000 0.0328(14) . . C47 C Uani 0.4987(4) 0.0233(4) 0.3794(3) 1.000 0.0420(17) . . C48 C Uani 0.6273(5) 0.0114(4) 0.3709(3) 1.000 0.0580(19) . . C49 C Uani 0.6700(5) 0.0895(5) 0.3746(3) 1.000 0.0566(19) . . C50 C Uani 0.5851(5) 0.1815(4) 0.3887(3) 1.000 0.0501(17) . . C51 C Uani 0.4571(4) 0.1943(4) 0.3985(3) 1.000 0.0401(16) . . C52 C Uani 0.0562(4) 0.0638(3) 0.0769(3) 1.000 0.0298(12) . . C53 C Uani -0.0759(4) 0.0679(3) 0.0750(3) 1.000 0.0294(12) . . C54 C Uani -0.1369(5) 0.0024(4) 0.1401(3) 1.000 0.0461(17) . . C55 C Uani -0.2615(5) 0.0081(5) 0.1384(4) 1.000 0.060(2) . . C56 C Uani -0.3227(5) 0.0810(5) 0.0721(4) 1.000 0.061(2) . . C57 C Uani -0.2634(5) 0.1459(4) 0.0069(4) 1.000 0.0524(19) . . C58 C Uani -0.1406(4) 0.1387(3) 0.0078(3) 1.000 0.0377(16) . . C59 C Uani -0.0004(5) -0.1391(5) 0.3797(3) 1.000 0.0634(19) . . C60 C Uani 0.2227(5) -0.1707(5) 0.4635(3) 1.000 0.065(2) . . C61 C Uani 0.2887(8) -0.2473(5) 0.2383(5) 1.000 0.111(3) . . C62 C Uani 0.4048(5) -0.0675(4) 0.1326(3) 1.000 0.0543(17) . . C70 C Uani 0.2441(10) 0.2667(6) 0.6904(6) 1.000 0.150(5) . . C71 C Uani 0.2727(7) 0.3300(5) 0.6034(4) 1.000 0.075(3) . . C72 C Uani 0.1755(7) 0.3800(6) 0.5513(6) 1.000 0.092(3) . . C73 C Uani 0.1983(9) 0.4430(7) 0.4734(6) 1.000 0.108(4) . . C74 C Uani 0.3185(10) 0.4606(6) 0.4401(5) 1.000 0.108(4) . . C75 C Uani 0.4098(7) 0.4101(6) 0.4888(5) 1.000 0.082(3) . . C76 C Uani 0.3879(6) 0.3457(5) 0.5694(4) 1.000 0.065(2) . . H1 H Uiso 0.064(3) 0.019(3) 0.399(2) 1.000 0.027(10) . . H2 H Uiso 0.431(5) -0.172(4) 0.290(3) 1.000 0.072(16) . . H31 H Uiso -0.24430 0.46620 0.38420 1.000 0.0440 calc R H41 H Uiso -0.40720 0.51800 0.30420 1.000 0.0470 calc R H51 H Uiso -0.39010 0.43470 0.20340 1.000 0.0400 calc R H71 H Uiso -0.27800 0.29010 0.13700 1.000 0.0360 calc R H72 H Uiso -0.16250 0.19850 0.18070 1.000 0.0360 calc R H91 H Uiso -0.22550 0.45910 0.03290 1.000 0.0400 calc R H101 H Uiso -0.09410 0.52200 -0.08790 1.000 0.0440 calc R H111 H Uiso 0.11190 0.41860 -0.11570 1.000 0.0400 calc R H141 H Uiso 0.25500 0.15230 0.00460 1.000 0.0340 calc R H142 H Uiso 0.26050 0.22880 -0.09150 1.000 0.0340 calc R H161 H Uiso 0.39130 0.34970 -0.13390 1.000 0.0400 calc R H171 H Uiso 0.52040 0.42280 -0.09990 1.000 0.0440 calc R H181 H Uiso 0.53520 0.39390 0.04220 1.000 0.0410 calc R H211 H Uiso 0.49320 0.29830 0.19380 1.000 0.0400 calc R H212 H Uiso 0.43260 0.20240 0.21700 1.000 0.0400 calc R H231 H Uiso 0.33410 0.48540 0.16510 1.000 0.0500 calc R H241 H Uiso 0.14830 0.59170 0.21870 1.000 0.0530 calc R H251 H Uiso -0.00620 0.51660 0.31010 1.000 0.0470 calc R H281 H Uiso 0.01530 0.24120 0.39780 1.000 0.0410 calc R H282 H Uiso -0.04110 0.34790 0.42610 1.000 0.0410 calc R H451 H Uiso 0.25520 0.06360 0.42370 1.000 0.0440 calc R H452 H Uiso 0.22750 0.17680 0.43830 1.000 0.0440 calc R H471 H Uiso 0.47030 -0.03140 0.37620 1.000 0.0510 calc R H481 H Uiso 0.68670 -0.05250 0.36230 1.000 0.0700 calc R H491 H Uiso 0.75830 0.08040 0.36740 1.000 0.0680 calc R H501 H Uiso 0.61440 0.23580 0.39170 1.000 0.0600 calc R H511 H Uiso 0.39840 0.25710 0.40960 1.000 0.0480 calc R H521 H Uiso 0.09920 -0.00740 0.11240 1.000 0.0350 calc R H522 H Uiso 0.10280 0.07420 0.01820 1.000 0.0350 calc R H541 H Uiso -0.09410 -0.04700 0.18640 1.000 0.0560 calc R H551 H Uiso -0.30310 -0.03810 0.18290 1.000 0.0730 calc R H561 H Uiso -0.40810 0.08650 0.07150 1.000 0.0740 calc R H571 H Uiso -0.30690 0.19590 -0.03900 1.000 0.0630 calc R H581 H Uiso -0.09880 0.18300 -0.03850 1.000 0.0450 calc R H591 H Uiso -0.05150 -0.09260 0.33420 1.000 0.0950 calc R H592 H Uiso -0.05460 -0.14650 0.43500 1.000 0.0950 calc R H593 H Uiso 0.03950 -0.20940 0.37070 1.000 0.0950 calc R H601 H Uiso 0.29660 -0.14650 0.45700 1.000 0.0960 calc R H602 H Uiso 0.25070 -0.24320 0.45880 1.000 0.0960 calc R H603 H Uiso 0.17280 -0.17010 0.51950 1.000 0.0960 calc R H611 H Uiso 0.25500 -0.28340 0.29610 1.000 0.1660 calc R H612 H Uiso 0.36350 -0.29720 0.21700 1.000 0.1660 calc R H613 H Uiso 0.22410 -0.22170 0.20060 1.000 0.1660 calc R H621 H Uiso 0.42790 -0.00700 0.13420 1.000 0.0820 calc R H622 H Uiso 0.34370 -0.04230 0.09250 1.000 0.0820 calc R H623 H Uiso 0.48060 -0.11900 0.11410 1.000 0.0820 calc R H701 H Uiso 0.17090 0.24250 0.69490 1.000 0.2250 calc R H702 H Uiso 0.22500 0.30990 0.72910 1.000 0.2250 calc R H703 H Uiso 0.31720 0.20480 0.70590 1.000 0.2250 calc R H721 H Uiso 0.09450 0.36840 0.57190 1.000 0.1110 calc R H731 H Uiso 0.13220 0.47740 0.43900 1.000 0.1300 calc R H741 H Uiso 0.33320 0.50710 0.38450 1.000 0.1290 calc R H751 H Uiso 0.49190 0.41900 0.46720 1.000 0.0980 calc R H761 H Uiso 0.45530 0.31080 0.60280 1.000 0.0780 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu 0.0256(1) 0.0224(1) 0.0284(1) -0.0035(1) -0.0077(1) -0.0084(1) Si1 0.0402(7) 0.0399(7) 0.0357(7) 0.0017(6) -0.0102(6) -0.0172(6) Si2 0.0422(8) 0.0342(8) 0.0541(8) -0.0049(6) -0.0072(6) 0.0049(6) O1 0.0291(15) 0.0392(17) 0.0405(17) -0.0221(14) -0.0108(13) -0.0004(13) O2 0.0269(14) 0.0200(14) 0.0328(15) -0.0073(12) -0.0109(12) -0.0069(11) O3 0.0365(16) 0.0380(17) 0.0292(15) -0.0030(13) -0.0026(13) -0.0261(14) O4 0.0342(16) 0.0335(17) 0.0278(15) -0.0045(13) -0.0119(12) -0.0124(13) N 0.0339(19) 0.0245(19) 0.035(2) -0.0024(15) -0.0090(15) -0.0070(15) C1 0.027(2) 0.027(2) 0.030(2) -0.0074(18) -0.0026(17) -0.0076(18) C2 0.032(2) 0.033(2) 0.026(2) -0.0059(18) -0.0033(17) -0.0122(19) C3 0.043(3) 0.035(3) 0.033(2) -0.015(2) -0.002(2) -0.009(2) C4 0.036(2) 0.028(2) 0.042(3) -0.011(2) 0.001(2) -0.001(2) C5 0.028(2) 0.032(2) 0.035(2) -0.006(2) -0.0069(18) -0.0050(19) C6 0.026(2) 0.026(2) 0.031(2) -0.0075(18) -0.0024(17) -0.0098(18) C7 0.024(2) 0.030(2) 0.038(2) -0.0086(19) -0.0116(18) -0.0056(18) C8 0.026(2) 0.027(2) 0.029(2) -0.0100(18) -0.0119(17) -0.0068(17) C9 0.033(2) 0.027(2) 0.043(3) -0.013(2) -0.017(2) -0.0006(19) C10 0.041(3) 0.030(2) 0.039(3) -0.007(2) -0.017(2) -0.005(2) C11 0.036(2) 0.035(2) 0.031(2) -0.008(2) -0.0082(19) -0.011(2) C12 0.029(2) 0.029(2) 0.032(2) -0.0132(19) -0.0137(18) -0.0036(18) C13 0.027(2) 0.021(2) 0.024(2) -0.0063(17) -0.0107(16) -0.0051(17) C14 0.031(2) 0.027(2) 0.027(2) -0.0071(18) -0.0041(17) -0.0100(18) C15 0.024(2) 0.024(2) 0.035(2) -0.0088(18) -0.0029(17) -0.0049(18) C16 0.030(2) 0.029(2) 0.035(2) -0.0060(19) -0.0034(19) -0.0052(19) C17 0.029(2) 0.030(2) 0.040(3) -0.002(2) 0.0048(19) -0.0120(19) C18 0.025(2) 0.028(2) 0.047(3) -0.007(2) -0.0067(19) -0.0085(19) C19 0.027(2) 0.027(2) 0.033(2) -0.0052(19) -0.0054(18) -0.0061(18) C20 0.026(2) 0.028(2) 0.035(2) -0.0107(19) -0.0058(18) -0.0055(18) C21 0.027(2) 0.040(3) 0.038(2) -0.008(2) -0.0077(18) -0.017(2) C22 0.034(2) 0.038(3) 0.032(2) -0.011(2) -0.0104(19) -0.015(2) C23 0.048(3) 0.044(3) 0.043(3) -0.010(2) -0.008(2) -0.025(2) C24 0.058(3) 0.036(3) 0.050(3) -0.017(2) -0.012(2) -0.019(2) C25 0.043(3) 0.041(3) 0.039(3) -0.018(2) -0.006(2) -0.012(2) C26 0.038(2) 0.037(3) 0.027(2) -0.0119(19) -0.0095(18) -0.014(2) C27 0.036(2) 0.030(2) 0.028(2) -0.0067(18) -0.0133(18) -0.0130(19) C28 0.036(2) 0.040(3) 0.030(2) -0.013(2) -0.0069(19) -0.010(2) C45 0.039(2) 0.044(3) 0.027(2) 0.000(2) -0.0128(19) -0.016(2) C46 0.041(2) 0.035(3) 0.024(2) -0.0024(19) -0.0152(18) -0.012(2) C47 0.050(3) 0.040(3) 0.040(3) -0.008(2) -0.020(2) -0.012(2) C48 0.047(3) 0.066(4) 0.059(3) -0.030(3) -0.013(3) 0.002(3) C49 0.038(3) 0.087(4) 0.051(3) -0.018(3) -0.016(2) -0.021(3) C50 0.055(3) 0.061(3) 0.041(3) 0.000(3) -0.024(2) -0.028(3) C51 0.045(3) 0.044(3) 0.034(2) -0.006(2) -0.018(2) -0.013(2) C52 0.033(2) 0.020(2) 0.041(2) -0.0119(19) -0.0114(18) -0.0060(18) C53 0.031(2) 0.029(2) 0.036(2) -0.016(2) -0.0063(19) -0.0102(19) C54 0.056(3) 0.047(3) 0.046(3) -0.017(2) -0.009(2) -0.023(3) C55 0.055(3) 0.075(4) 0.071(4) -0.036(3) 0.017(3) -0.045(3) C56 0.032(3) 0.076(4) 0.094(5) -0.051(4) -0.011(3) -0.010(3) C57 0.045(3) 0.045(3) 0.078(4) -0.033(3) -0.030(3) 0.004(3) C58 0.038(3) 0.032(2) 0.049(3) -0.017(2) -0.016(2) -0.005(2) C59 0.052(3) 0.084(4) 0.048(3) 0.007(3) -0.010(3) -0.037(3) C60 0.067(4) 0.083(4) 0.043(3) 0.013(3) -0.025(3) -0.041(3) C61 0.153(7) 0.040(4) 0.112(6) -0.035(4) 0.061(5) -0.036(4) C62 0.042(3) 0.056(3) 0.065(3) -0.023(3) 0.003(3) -0.016(3) C70 0.212(11) 0.060(5) 0.135(8) -0.010(5) 0.012(7) -0.031(6) C71 0.101(5) 0.048(4) 0.077(5) -0.026(3) -0.006(4) -0.019(4) C72 0.073(5) 0.103(6) 0.132(7) -0.083(6) -0.042(5) 0.006(4) C73 0.100(6) 0.120(7) 0.118(7) -0.080(6) -0.070(6) 0.037(5) C74 0.143(8) 0.083(5) 0.075(5) -0.036(4) -0.041(6) 0.025(5) C75 0.083(5) 0.080(5) 0.088(5) -0.049(4) 0.000(4) -0.012(4) C76 0.057(4) 0.059(4) 0.080(4) -0.031(3) -0.026(3) 0.004(3) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu Si1 3.2146(13) . . yes Lu O1 2.011(3) . . yes Lu O2 2.351(3) . . yes Lu O3 2.011(3) . . yes Lu O4 2.356(3) . . yes Lu N 2.186(4) . . yes Si1 N 1.708(4) . . yes Si1 C59 1.857(7) . . yes Si1 C60 1.861(6) . . yes Si2 N 1.702(4) . . yes Si2 C61 1.864(8) . . yes Si2 C62 1.854(5) . . yes Si1 H1 1.45(4) . . no Si2 H2 1.39(6) . . no O1 C1 1.330(5) . . yes O2 C52 1.479(5) . . yes O2 C13 1.418(5) . . yes O3 C20 1.324(6) . . yes O4 C45 1.482(5) . . yes O4 C27 1.421(5) . . yes C1 C6 1.400(6) . . no C1 C2 1.397(5) . . no C2 C28 1.508(7) . . no C2 C3 1.387(6) . . no C3 C4 1.379(7) . . no C4 C5 1.378(6) . . no C5 C6 1.383(6) . . no C6 C7 1.521(6) . . no C7 C8 1.524(6) . . no C8 C13 1.401(5) . . no C8 C9 1.387(6) . . no C9 C10 1.373(7) . . no C10 C11 1.383(7) . . no C11 C12 1.401(6) . . no C12 C13 1.388(5) . . no C12 C14 1.527(6) . . no C14 C15 1.514(6) . . no C15 C16 1.379(6) . . no C15 C20 1.402(7) . . no C16 C17 1.382(7) . . no C17 C18 1.387(7) . . no C18 C19 1.383(7) . . no C19 C21 1.503(7) . . no C19 C20 1.414(7) . . no C21 C22 1.521(6) . . no C22 C27 1.402(6) . . no C22 C23 1.390(7) . . no C23 C24 1.376(8) . . no C24 C25 1.379(7) . . no C25 C26 1.397(7) . . no C26 C27 1.391(6) . . no C26 C28 1.516(6) . . no C45 C46 1.498(7) . . no C46 C51 1.397(7) . . no C46 C47 1.381(7) . . no C47 C48 1.391(8) . . no C48 C49 1.366(9) . . no C49 C50 1.377(9) . . no C50 C51 1.380(8) . . no C52 C53 1.492(7) . . no C53 C58 1.388(7) . . no C53 C54 1.375(7) . . no C54 C55 1.399(9) . . no C55 C56 1.367(9) . . no C56 C57 1.361(9) . . no C57 C58 1.369(8) . . no C3 H31 0.9496 . . no C4 H41 0.9503 . . no C5 H51 0.9515 . . no C7 H71 0.9898 . . no C7 H72 0.9905 . . no C9 H91 0.9504 . . no C10 H101 0.9501 . . no C11 H111 0.9502 . . no C14 H141 0.9886 . . no C14 H142 0.9903 . . no C16 H161 0.9495 . . no C17 H171 0.9500 . . no C18 H181 0.9496 . . no C21 H211 0.9895 . . no C21 H212 0.9902 . . no C23 H231 0.9509 . . no C24 H241 0.9491 . . no C25 H251 0.9499 . . no C28 H281 0.9898 . . no C28 H282 0.9896 . . no C45 H451 0.9907 . . no C45 H452 0.9898 . . no C47 H471 0.9499 . . no C48 H481 0.9513 . . no C49 H491 0.9506 . . no C50 H501 0.9497 . . no C51 H511 0.9510 . . no C52 H521 0.9895 . . no C52 H522 0.9912 . . no C54 H541 0.9491 . . no C55 H551 0.9506 . . no C56 H561 0.9503 . . no C57 H571 0.9503 . . no C58 H581 0.9508 . . no C59 H591 0.9788 . . no C59 H592 0.9799 . . no C59 H593 0.9806 . . no C60 H601 0.9795 . . no C60 H602 0.9796 . . no C60 H603 0.9794 . . no C61 H611 0.9803 . . no C61 H612 0.9797 . . no C61 H613 0.9803 . . no C62 H621 0.9801 . . no C62 H622 0.9796 . . no C62 H623 0.9798 . . no C70 C71 1.450(11) . . no C71 C72 1.413(12) . . no C71 C76 1.356(11) . . no C72 C73 1.324(13) . . no C73 C74 1.417(16) . . no C74 C75 1.326(13) . . no C75 C76 1.363(10) . . no C70 H701 0.9798 . . no C70 H702 0.9797 . . no C70 H703 0.9802 . . no C72 H721 0.9509 . . no C73 H731 0.9498 . . no C74 H741 0.9504 . . no C75 H751 0.9506 . . no C76 H761 0.9509 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si1 Lu O1 93.59(8) . . . yes Si1 Lu O2 109.46(7) . . . yes Si1 Lu O3 143.74(9) . . . yes Si1 Lu O4 91.48(7) . . . yes Si1 Lu N 29.81(9) . . . yes O1 Lu O2 83.39(10) . . . yes O1 Lu O3 121.77(11) . . . yes O1 Lu O4 85.64(10) . . . yes O1 Lu N 121.12(12) . . . yes O2 Lu O3 84.43(11) . . . yes O2 Lu O4 156.86(9) . . . yes O2 Lu N 99.44(11) . . . yes O3 Lu O4 84.15(11) . . . yes O3 Lu N 117.01(12) . . . yes O4 Lu N 103.67(11) . . . yes Lu Si1 N 39.51(14) . . . yes Lu Si1 C59 118.56(17) . . . yes Lu Si1 C60 131.8(2) . . . yes N Si1 C59 114.0(2) . . . yes N Si1 C60 113.9(2) . . . yes C59 Si1 C60 109.2(3) . . . yes N Si2 C61 112.3(3) . . . yes N Si2 C62 111.7(2) . . . yes C61 Si2 C62 109.8(3) . . . yes Lu Si1 H1 64.7(13) . . . no N Si1 H1 103.4(13) . . . no C59 Si1 H1 109.0(15) . . . no C60 Si1 H1 106.9(14) . . . no C61 Si2 H2 108(2) . . . no C62 Si2 H2 104(2) . . . no N Si2 H2 111(2) . . . no Lu O1 C1 165.3(3) . . . yes Lu O2 C13 114.6(2) . . . yes Lu O2 C52 130.4(2) . . . yes C13 O2 C52 114.0(3) . . . yes Lu O3 C20 166.6(3) . . . yes Lu O4 C27 112.3(2) . . . yes Lu O4 C45 132.5(3) . . . yes C27 O4 C45 114.3(3) . . . yes Si1 N Si2 122.3(2) . . . yes Lu N Si1 110.7(2) . . . yes Lu N Si2 126.36(19) . . . yes O1 C1 C2 118.8(4) . . . yes O1 C1 C6 120.3(3) . . . yes C2 C1 C6 120.9(4) . . . no C1 C2 C3 118.7(4) . . . no C1 C2 C28 118.4(4) . . . no C3 C2 C28 122.9(4) . . . no C2 C3 C4 120.7(4) . . . no C3 C4 C5 120.1(4) . . . no C4 C5 C6 121.1(4) . . . no C1 C6 C5 118.5(4) . . . no C5 C6 C7 124.1(4) . . . no C1 C6 C7 117.5(4) . . . no C6 C7 C8 112.2(4) . . . no C7 C8 C9 118.9(4) . . . no C9 C8 C13 117.1(3) . . . no C7 C8 C13 124.0(3) . . . no C8 C9 C10 121.7(4) . . . no C9 C10 C11 120.1(4) . . . no C10 C11 C12 120.7(4) . . . no C11 C12 C13 117.5(4) . . . no C11 C12 C14 118.2(4) . . . no C13 C12 C14 124.3(3) . . . no O2 C13 C8 118.4(3) . . . yes O2 C13 C12 118.7(3) . . . yes C8 C13 C12 122.8(4) . . . no C12 C14 C15 111.7(3) . . . no C14 C15 C16 123.3(4) . . . no C14 C15 C20 118.0(4) . . . no C16 C15 C20 118.8(4) . . . no C15 C16 C17 120.9(4) . . . no C16 C17 C18 120.3(4) . . . no C17 C18 C19 120.8(4) . . . no C18 C19 C20 118.2(4) . . . no C18 C19 C21 124.0(4) . . . no C20 C19 C21 117.8(4) . . . no O3 C20 C15 120.2(4) . . . yes O3 C20 C19 118.8(4) . . . yes C15 C20 C19 121.0(4) . . . no C19 C21 C22 111.1(4) . . . no C21 C22 C27 124.8(4) . . . no C23 C22 C27 116.7(4) . . . no C21 C22 C23 118.4(4) . . . no C22 C23 C24 121.9(5) . . . no C23 C24 C25 120.0(5) . . . no C24 C25 C26 120.9(5) . . . no C27 C26 C28 125.2(4) . . . no C25 C26 C28 117.2(4) . . . no C25 C26 C27 117.6(4) . . . no O4 C27 C22 118.8(4) . . . yes O4 C27 C26 118.3(4) . . . yes C22 C27 C26 122.9(4) . . . no C2 C28 C26 111.5(4) . . . no O4 C45 C46 111.5(3) . . . yes C45 C46 C47 120.6(4) . . . no C45 C46 C51 120.1(4) . . . no C47 C46 C51 119.3(5) . . . no C46 C47 C48 119.0(5) . . . no C47 C48 C49 121.4(5) . . . no C48 C49 C50 120.0(6) . . . no C49 C50 C51 119.6(5) . . . no C46 C51 C50 120.7(5) . . . no O2 C52 C53 112.1(3) . . . yes C52 C53 C54 120.8(4) . . . no C52 C53 C58 120.8(4) . . . no C54 C53 C58 118.4(5) . . . no C53 C54 C55 120.4(5) . . . no C54 C55 C56 119.2(6) . . . no C55 C56 C57 121.1(6) . . . no C56 C57 C58 119.6(6) . . . no C53 C58 C57 121.3(5) . . . no C2 C3 H31 119.66 . . . no C4 C3 H31 119.66 . . . no C3 C4 H41 119.92 . . . no C5 C4 H41 119.95 . . . no C4 C5 H51 119.48 . . . no C6 C5 H51 119.46 . . . no C6 C7 H71 109.16 . . . no C6 C7 H72 109.14 . . . no C8 C7 H71 109.24 . . . no C8 C7 H72 109.18 . . . no H71 C7 H72 107.85 . . . no C8 C9 H91 119.19 . . . no C10 C9 H91 119.09 . . . no C9 C10 H101 120.00 . . . no C11 C10 H101 119.93 . . . no C10 C11 H111 119.61 . . . no C12 C11 H111 119.65 . . . no C12 C14 H141 109.32 . . . no C12 C14 H142 109.23 . . . no C15 C14 H141 109.30 . . . no C15 C14 H142 109.19 . . . no H141 C14 H142 107.99 . . . no C15 C16 H161 119.50 . . . no C17 C16 H161 119.61 . . . no C16 C17 H171 119.79 . . . no C18 C17 H171 119.94 . . . no C17 C18 H181 119.60 . . . no C19 C18 H181 119.55 . . . no C19 C21 H211 109.37 . . . no C19 C21 H212 109.36 . . . no C22 C21 H211 109.51 . . . no C22 C21 H212 109.38 . . . no H211 C21 H212 108.11 . . . no C22 C23 H231 119.00 . . . no C24 C23 H231 119.06 . . . no C23 C24 H241 120.07 . . . no C25 C24 H241 119.98 . . . no C24 C25 H251 119.58 . . . no C26 C25 H251 119.54 . . . no C2 C28 H281 109.36 . . . no C2 C28 H282 109.35 . . . no C26 C28 H281 109.31 . . . no C26 C28 H282 109.27 . . . no H281 C28 H282 108.01 . . . no O4 C45 H451 109.30 . . . no O4 C45 H452 109.34 . . . no C46 C45 H451 109.32 . . . no C46 C45 H452 109.32 . . . no H451 C45 H452 107.94 . . . no C46 C47 H471 120.46 . . . no C48 C47 H471 120.54 . . . no C47 C48 H481 119.26 . . . no C49 C48 H481 119.34 . . . no C48 C49 H491 120.05 . . . no C50 C49 H491 119.98 . . . no C49 C50 H501 120.23 . . . no C51 C50 H501 120.20 . . . no C46 C51 H511 119.70 . . . no C50 C51 H511 119.59 . . . no O2 C52 H521 109.29 . . . no O2 C52 H522 109.20 . . . no C53 C52 H521 109.21 . . . no C53 C52 H522 109.11 . . . no H521 C52 H522 107.87 . . . no C53 C54 H541 119.72 . . . no C55 C54 H541 119.88 . . . no C54 C55 H551 120.36 . . . no C56 C55 H551 120.43 . . . no C55 C56 H561 119.48 . . . no C57 C56 H561 119.41 . . . no C56 C57 H571 120.23 . . . no C58 C57 H571 120.18 . . . no C53 C58 H581 119.34 . . . no C57 C58 H581 119.39 . . . no Si1 C59 H591 109.47 . . . no Si1 C59 H592 109.46 . . . no Si1 C59 H593 109.48 . . . no H591 C59 H592 109.51 . . . no H591 C59 H593 109.50 . . . no H592 C59 H593 109.40 . . . no Si1 C60 H601 109.52 . . . no Si1 C60 H602 109.46 . . . no Si1 C60 H603 109.45 . . . no H601 C60 H602 109.45 . . . no H601 C60 H603 109.54 . . . no H602 C60 H603 109.41 . . . no Si2 C61 H611 109.43 . . . no Si2 C61 H612 109.47 . . . no Si2 C61 H613 109.43 . . . no H611 C61 H612 109.53 . . . no H611 C61 H613 109.47 . . . no H612 C61 H613 109.51 . . . no Si2 C62 H621 109.42 . . . no Si2 C62 H622 109.46 . . . no Si2 C62 H623 109.48 . . . no H621 C62 H622 109.47 . . . no H621 C62 H623 109.49 . . . no H622 C62 H623 109.51 . . . no C70 C71 C72 118.8(8) . . . no C70 C71 C76 123.4(8) . . . no C72 C71 C76 117.8(6) . . . no C71 C72 C73 119.4(9) . . . no C72 C73 C74 121.8(9) . . . no C73 C74 C75 118.0(8) . . . no C74 C75 C76 121.1(8) . . . no C71 C76 C75 121.9(7) . . . no C71 C70 H701 109.41 . . . no C71 C70 H702 109.52 . . . no C71 C70 H703 109.43 . . . no H701 C70 H702 109.55 . . . no H701 C70 H703 109.44 . . . no H702 C70 H703 109.47 . . . no C71 C72 H721 120.33 . . . no C73 C72 H721 120.27 . . . no C72 C73 H731 119.05 . . . no C74 C73 H731 119.16 . . . no C73 C74 H741 120.97 . . . no C75 C74 H741 121.05 . . . no C74 C75 H751 119.50 . . . no C76 C75 H751 119.41 . . . no C71 C76 H761 119.04 . . . no C75 C76 H761 119.06 . . . no # End of Crystallographic Information File