# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Bambirra, Sergio' ; Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; 'Leusen, Daan van' ; Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; 'Meetsma, Auke' ; Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; 'Hessen, Bart' ; Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; 'Teuben, Jan H.' ; Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; _publ_contact_author_name ; Dr. B. Hessen ; _publ_contact_author_address ; Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; _publ_contact_author_email hessen@chem.rug.nl _publ_contact_author_fax '+31 50 3634441' _publ_contact_author_phone '+31 50 3634315' _publ_requested_journal 'Chemical Communication.' _publ_section_title ; Yttrium alkyl complexes with a sterically demanding benzamidinate ligand: synthesis, structure and catalytic ethene polymerisation ; _publ_contact_letter # Include date of submission ; Date of submission : 2002-08-30 Consider this CIF submission for depostion of the X-ray structure of a manuscript entitled: Yttrium alkyl complexes with a sterically demanding benzamidinate ligand: synthesis, structure and catalytic ethene polymerisation. to be submitted to : Chemical Communications (Our Code : CP500) ; _publ_section_exptl_refinement ; The electron density of the carbon C19 and C39 atoms appeared to be spread out, indicating conformational disorder. A disorder model, with two positions for each, was used in the refinement. The s.o.f. of the major component of the disorder model refined to a value of 0.63(5) and 0.54(5), respectively. A subsequent difference Fourier synthesis resulted in the location of most of the hydrogen atoms, which coordinates and isotropic displacement parameters were refined. Positional and isotropic displacement parameters of all H atoms were refined freely, except those belonging to C19 and C39. These hydrogen atoms were included in the final refinement riding on their carrier atoms with their positions calculated by using sp^3^ hybridization at the C-atom as appropriate with U~iso~ = 1.5 x U~equiv~ of their parent atom and at a multiplicity of the s.o.f due to a disorder in the carbon atom positions. The methyl-groups were refined as rigid groups, which were allowed to rotate free. ; # Insert blank lines between references _publ_section_references ; Beurskens, P.T., Beurskens, G., Bosman, W.P., Gelder, R. de Garcia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M. & (1997) The DIRDIF97 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Boer, J.L. de & Duisenberg, A.J.M. (1984). Acta Cryst. A40, C-410. Boeyens, J.C.A. (1978). J.Cryst.Mol.Struct. 8, 317-320. Bolhuis, F. van (1971). J. Appl. Cryst. 4, 263-264. Bondi, A. (1964). J. Phys. Chem. 68, 441-451. Duisenberg, A.J.M. (1992). J. Appl. Cryst. 25, 92-96. Enraf-Nonius (1994). CAD4-UNIX Software. Version 5.1 Utrecht modified version October 1994. Enraf-Nonius, Delft, The Netherlands. Furrugia, L.J. (1998). ORTEP-3 for Windows. Version 1.04. Department of Chemistry, Univ. of Glasgow, Scotland, UK. International Tables for Crystallography (1983). Vol. A. Space-group symmetry, edited by T. Hahn. Dordrecht: Reidel. (Present distributor Kluwer Academic Publishers, Dordrecht). International Tables for Crystallography (1992). Vol. C. Edited by A.J.C Wilson, Kluwer Academic Publishers, Dordrecht, The Netherlands. Le Page, Y. (1987). J. Appl. Cryst. 20, 264-269. Le Page, Y. (1988). J. Appl. Cryst. 21, 983-984. Meetsma, A. (1996). Extended version of the program PLUTO. Groningen University, The Netherlands. (unpublished). Sheldrick, G.M. (1997). SHELXL-97. Program for the Refinement of Crystal Structures, University of Gottingen, Germany. Snow, M.R. & Tiekink, E.R.T. (1988). Acta Cryst. B44, 676-677. Spek, A.L. (1987). Acta Cryst. C43, 1233-1235. Spek, A.L. (1988). J. Appl. Cryst. 21, 578-579. Spek, A.L. (1990). Acta Cryst. A46, C-34. Spek, A.L. (1993). HELENA, Program for Data Reduction, Utrecht University, The Netherlands. Spek, A.L. (1994). Am. Crystallogr. Assoc.-Abstracts, 22, 66. ; _publ_section_figure_captions ; Fig. 1. Chemical structural diagram (scheme 1) of the title compound Fig. 2. PLUTO drawing of the molecule illustrating the puckering and the adopted numbering scheme. Fig. 3. Molecular packing viewed down unit cell axes. Fig. 4. Perspective ORTEP drawing of the title compound. All non-hydrogen atoms are represented by thermal vibrational ellipsoids drawn to encompass 50% of the electron density. The hydrogen atoms are drawn with an arbitrary radius. ; _publ_section_acknowledgements ; ? ; #=============================================================================== data_c43h69n2 _database_code_CSD 192682 _audit_creation_date 1999-10-29 _audit_creation_method 'PLATON option' _audit_update_record ; ? ; #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H69 N2 O Si2 Y' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C43 H69 N2 O Si2 Y' _chemical_formula_weight 775.11 _chemical_compound_source 'by syntheses' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si .0817 .0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C .0033 .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 12.537(1) _cell_length_b 13.340(1) _cell_length_c 13.925(1) _cell_angle_alpha 101.964(9) _cell_angle_beta 98.18(1) _cell_angle_gamma 93.65(1) _cell_volume 2244.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 130 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 15.05 _cell_measurement_theta_max 20.14 _cell_special_details ; Unit cell parameters (Duisenberg, 1992) and orientation matrix were determined from a least-squares treatment of SET4 (de Boer & Duisenberg, 1984) setting. Reduced cell calculations did not indicate any higher metric lattice symmetry and examination of the final atomic coordinates of the structure did not yield extra symmetry elements (Spek, 1988; Le Page 1987, 1988) ; _exptl_crystal_description parallelepiped _exptl_crystal_colour 'colorless transparent' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.12 _exptl_crystal_size_rad ? _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method ? _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 1.38 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type ' none' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 130 _diffrn_radiation_wavelength .71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine focus sealed Philips Mo tube ' _diffrn_radiation_monochromator 'perpendicular mounted graphite' _diffrn_radiation_detector ; scintillation NaI crystal with photomultiplier ; _diffrn_measurement_device_type ; Enraf Nonius CAD-4F diffractometer ; _diffrn_measurement_method '\w/2\q' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temperature unit (Bolhuis, 1971), on an Enraf-Nonius CAD-4F diffractometer. Graphite-monochromated Mo K\a radiation, \w/2\q scan, \D\w = (1.00 + 0.34 tg \q)\%. ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 180 _diffrn_standards_decay_% 1.0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 10187 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 26.97 _diffrn_reflns_reduction_process ; Intensity data were corrected for Lorentz and polarization effects, scale variation, but not for absorption and reduced to F~o~^2^ ; # number of unique reflections _reflns_number_total 9732 _reflns_number_gt 7479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-UNIX Software Version 5.1, 1994' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1993)' _computing_structure_solution ; DIRDIF-97 (Beurskens et al., 1997) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTO (Meetsma, 1997) ORTEP (Furrugia, 1998) PLATON (Spek, 1994, 1996) ; _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0886P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9732 _refine_ls_number_parameters 702 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1390 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.137 _refine_diff_density_min -1.225 _refine_diff_density_rms .088 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _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 Y Uani .20416(2) .31365(2) .20063(2) 1.000 .0226(1) Si1 Uani .22079(10) .60581(7) .24972(8) 1.000 .0415(3) Si2 Uani .31992(10) .29252(8) -.04823(7) 1.000 .0422(3) O Uani .01413(18) .31343(19) .16761(17) 1.000 .0350(7) N1 Uani .3425(2) .23250(19) .27590(18) 1.000 .0219(7) N2 Uani .1738(2) .20350(18) .30937(18) 1.000 .0219(7) C1 Uani .2789(2) .1915(2) .3307(2) 1.000 .0199(8) C2 Uani .3252(2) .1424(2) .4131(2) 1.000 .0229(9) C3 Uani .4077(3) .1970(3) .4858(2) 1.000 .0296(10) C4 Uani .4502(3) .1550(3) .5647(3) 1.000 .0375(11) C5 Uani .4105(3) .0583(3) .5705(3) 1.000 .0374(11) C6 Uani .3304(3) .0024(3) .4985(3) 1.000 .0349(11) C7 Uani .2861(3) .0447(3) .4201(2) 1.000 .0276(9) C8 Uani .4479(2) .2005(2) .2698(2) 1.000 .0236(9) C9 Uani .5396(3) .2709(3) .3113(2) 1.000 .0305(10) C10 Uani .6419(3) .2368(3) .3034(3) 1.000 .0428(11) C11 Uani .6539(3) .1385(3) .2544(3) 1.000 .0481(16) C12 Uani .5640(3) .0713(3) .2108(3) 1.000 .0387(12) C13 Uani .4592(3) .0997(2) .2182(2) 1.000 .0280(9) C14 Uani .5281(3) .3806(3) .3606(3) 1.000 .0333(11) C15 Uani .6117(5) .4226(5) .4544(4) 1.000 .0604(17) C16 Uani .5315(5) .4515(3) .2881(4) 1.000 .0512(16) C17 Uani .3631(3) .0235(3) .1670(3) 1.000 .0353(11) C18 Uani .3707(5) -.0837(3) .1862(5) 1.000 .0560(18) C19A Uani .357(2) .0066(12) .0516(9) .63(5) .063(4) C20 Uani .0948(2) .1675(2) .3618(2) 1.000 .0261(9) C21 Uani .0231(3) .0822(3) .3106(3) 1.000 .0357(11) C22 Uani -.0580(3) .0476(3) .3595(4) 1.000 .0532(14) C23 Uani -.0669(4) .0959(4) .4544(4) 1.000 .063(2) C24 Uani .0026(3) .1799(4) .5024(4) 1.000 .0514(16) C25 Uani .0842(3) .2188(3) .4582(3) 1.000 .0310(10) C26 Uani .0306(3) .0255(3) .2061(4) 1.000 .0502(14) C27 Uani -.0692(5) .0352(4) .1323(4) 1.000 .0640(19) C28 Uani .0441(7) -.0885(5) .1998(7) 1.000 .093(3) C29 Uani .1557(3) .3136(3) .5159(3) 1.000 .0359(11) C30 Uani .0922(5) .4081(4) .5292(4) 1.000 .0540(17) C31 Uani .2099(4) .2985(5) .6171(3) 1.000 .0582(18) C32 Uani .2318(3) .4863(3) .2936(3) 1.000 .0355(11) C33 Uani .3302(8) .6239(5) .1742(5) 1.000 .078(3) C34 Uani .2335(4) .7244(3) .3511(4) 1.000 .0480(16) C35 Uani .0852(7) .6025(5) .1713(7) 1.000 .092(3) C36 Uani .2149(4) .2788(5) .0275(3) 1.000 .075(2) C37 Uani .3016(4) .1879(4) -.1632(3) 1.000 .0486(14) C38 Uani .4606(5) .2911(8) .0187(4) 1.000 .078(2) C39C Uani .3413(18) .4143(13) -.0939(14) .54(5) .066(5) C40 Uani -.0516(4) .3442(5) .2455(3) 1.000 .0501(14) C41 Uani -.1497(4) .3824(5) .1975(5) 1.000 .071(2) C42 Uani -.1662(4) .3190(6) .0960(5) 1.000 .086(2) C43 Uani -.0521(4) .3094(5) .0720(3) 1.000 .0523(14) C39D Uani .282(5) .4131(14) -.0890(13) .46(5) .088(14) C19B Uani .317(2) .037(3) .0651(17) .37(5) .051(6) H4 Uiso .508(3) .199(3) .615(3) 1.000 .053(12) H5 Uiso .437(3) .035(3) .617(3) 1.000 .046(12) H7 Uiso .229(2) .005(2) .370(2) 1.000 .017(8) H10 Uiso .705(3) .282(3) .335(3) 1.000 .047(11) H6 Uiso .302(3) -.060(3) .509(3) 1.000 .040(10) H3 Uiso .439(3) .259(3) .483(3) 1.000 .031(9) H14 Uiso .462(3) .375(3) .378(3) 1.000 .037(10) H15 Uiso .612(5) .377(4) .502(4) 1.000 .09(2) H15' Uiso .594(4) .486(5) .484(4) 1.000 .083(18) H15" Uiso .677(5) .425(5) .435(5) 1.000 .10(2) H16 Uiso .593(4) .452(3) .264(3) 1.000 .056(13) H16' Uiso .526(3) .521(4) .321(3) 1.000 .055(13) H16" Uiso .470(3) .429(3) .229(3) 1.000 .044(11) H17 Uiso .309(3) .046(3) .195(3) 1.000 .037(10) H18 Uiso .423(5) -.102(4) .155(4) 1.000 .078(19) H18' Uiso .307(3) -.129(3) .153(3) 1.000 .046(11) H18" Uiso .382(5) -.087(4) .255(5) 1.000 .09(2) H19A Uiso .35109 .07277 .03201 .63(5) .0940 H19B Uiso .29267 -.04058 .01865 .63(5) .0940 H19C Uiso .42186 -.02293 .03199 .63(5) .0940 H22 Uiso -.106(3) -.005(3) .327(3) 1.000 .039(11) H23 Uiso -.113(4) .070(4) .484(3) 1.000 .063(14) H24 Uiso .001(4) .214(3) .564(3) 1.000 .057(14) H26 Uiso .088(3) .054(3) .186(3) 1.000 .043(11) H27 Uiso -.137(4) -.001(3) .151(3) 1.000 .056(13) H27' Uiso -.071(4) .003(4) .065(4) 1.000 .065(15) H27" Uiso -.067(4) .096(4) .125(4) 1.000 .077(17) H28 Uiso .106(6) -.096(5) .240(5) 1.000 .11(2) H28' Uiso .058(5) -.108(5) .150(5) 1.000 .09(2) H28" Uiso -.030(6) -.129(6) .197(6) 1.000 .13(3) H29 Uiso .215(3) .332(3) .479(3) 1.000 .031(9) H30 Uiso .060(4) .418(4) .468(4) 1.000 .079(17) H30' Uiso .135(4) .464(4) .567(4) 1.000 .058(14) H30" Uiso .030(4) .397(3) .562(3) 1.000 .057(13) H31 Uiso .162(5) .300(4) .667(4) 1.000 .083(16) H31' Uiso .258(4) .358(4) .645(3) 1.000 .052(13) H31" Uiso .236(4) .235(4) .613(4) 1.000 .070(16) H32 Uiso .184(3) .481(3) .338(3) 1.000 .039(11) H32' Uiso .302(4) .484(4) .330(4) 1.000 .081(17) H33 Uiso .391(6) .632(6) .213(5) 1.000 .11(3) H33' Uiso .323(5) .685(5) .147(5) 1.000 .11(2) H33" Uiso .315(5) .570(5) .118(5) 1.000 .11(2) H34 Uiso .192(5) .712(4) .392(4) 1.000 .079(18) H34' Uiso .224(4) .783(4) .324(4) 1.000 .075(15) H34" Uiso .311(4) .738(4) .393(4) 1.000 .076(16) H35 Uiso .078(4) .543(4) .114(4) 1.000 .068(15) H35' Uiso .076(4) .664(5) .157(4) 1.000 .088(18) H35" Uiso .036(5) .589(5) .204(5) 1.000 .08(3) H36 Uiso .18741 .20515 .00490 1.000 .0909 H36' Uiso .15677 .31667 .00009 1.000 .0909 H37 Uiso .296(4) .121(4) -.143(4) 1.000 .086(17) H37' Uiso .356(4) .206(4) -.198(4) 1.000 .069(15) H37" Uiso .232(4) .193(4) -.202(4) 1.000 .070(15) H38 Uiso .476(6) .345(6) .064(6) 1.000 .12(3) H38' Uiso .522(4) .293(4) -.022(4) 1.000 .082(16) H38" Uiso .461(5) .236(4) .047(4) 1.000 .08(2) H39A Uiso .39915 .40814 -.13460 .54(5) .0986 H39B Uiso .36168 .47256 -.03683 .54(5) .0986 H39C Uiso .27417 .42578 -.13389 .54(5) .0986 H40 Uiso -.011(5) .398(5) .286(4) 1.000 .09(2) H40' Uiso -.069(3) .290(3) .272(3) 1.000 .051(13) H41 Uiso -.206(4) .386(4) .231(4) 1.000 .069(15) H41' Uiso -.135(6) .448(6) .188(6) 1.000 .14(3) H42 Uiso -.20942 .35294 .04905 1.000 .1032 H42' Uiso -.20356 .25049 .09310 1.000 .1032 H43 Uiso -.050(3) .248(3) .041(3) 1.000 .038(12) H43' Uiso -.021(3) .364(3) .047(3) 1.000 .050(12) H11 Uiso .721(3) .118(3) .252(3) 1.000 .042(11) H12 Uiso .578(3) .003(3) .179(3) 1.000 .051(12) H19D Uiso .28262 .10137 .07097 .37(5) .0770 H19E Uiso .26292 -.02101 .03258 .37(5) .0770 H19F Uiso .37520 .03886 .02525 .37(5) .0770 H39D Uiso .22794 .39509 -.14930 .46(5) .1326 H39E Uiso .34689 .44945 -.10289 .46(5) .1326 H39F Uiso .25262 .45772 -.03609 .46(5) .1326 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y .0282(2) .0243(2) .0181(2) .0084(1) .0050(1) .0088(1) Si1 .0641(7) .0237(5) .0364(6) .0096(4) .0012(5) .0076(5) Si2 .0665(7) .0434(6) .0239(5) .0123(4) .0175(5) .0197(5) O .0298(12) .0482(14) .0299(12) .0110(11) .0056(10) .0152(11) N1 .0244(13) .0230(12) .0208(12) .0081(10) .0059(10) .0050(10) N2 .0224(13) .0229(12) .0217(12) .0059(10) .0056(10) .0037(10) C1 .0271(15) .0173(13) .0163(13) .0038(11) .0053(11) .0047(11) C2 .0219(15) .0283(15) .0223(15) .0096(12) .0081(12) .0067(12) C3 .0313(18) .0348(18) .0256(16) .0135(14) .0043(13) .0034(14) C4 .0312(18) .055(2) .0281(18) .0153(17) .0005(15) .0074(17) C5 .0344(19) .053(2) .0346(19) .0274(18) .0076(16) .0144(17) C6 .0313(18) .0391(19) .046(2) .0282(17) .0138(16) .0114(15) C7 .0251(16) .0329(17) .0285(16) .0130(14) .0057(13) .0063(13) C8 .0266(16) .0295(16) .0204(14) .0126(12) .0095(12) .0090(13) C9 .0320(18) .0377(18) .0275(16) .0149(14) .0106(14) .0067(14) C10 .0256(19) .053(2) .056(2) .021(2) .0132(17) .0062(17) C11 .033(2) .056(3) .069(3) .028(2) .025(2) .0220(19) C12 .044(2) .037(2) .046(2) .0179(17) .0221(17) .0220(17) C13 .0381(18) .0288(16) .0239(15) .0140(13) .0114(14) .0125(14) C14 .0286(18) .0358(19) .0353(19) .0084(15) .0055(15) -.0020(15) C15 .049(3) .061(3) .058(3) -.003(3) -.009(2) -.002(2) C16 .067(3) .037(2) .058(3) .017(2) .027(3) .008(2) C17 .041(2) .0286(17) .0369(19) .0061(15) .0048(16) .0152(15) C18 .057(3) .033(2) .076(4) .015(2) -.002(3) .007(2) C19A .082(11) .059(6) .043(5) .015(4) -.014(6) .011(6) C20 .0217(15) .0289(16) .0339(17) .0171(14) .0070(13) .0102(13) C21 .0258(17) .0331(18) .051(2) .0141(16) .0068(16) .0065(14) C22 .029(2) .049(2) .083(3) .022(2) .006(2) -.0052(18) C23 .044(3) .082(4) .079(4) .037(3) .032(3) .001(2) C24 .041(2) .076(3) .050(3) .028(2) .025(2) .014(2) C25 .0300(17) .0392(18) .0311(17) .0160(15) .0121(14) .0152(14) C26 .033(2) .038(2) .070(3) -.009(2) .010(2) -.0047(17) C27 .085(4) .046(3) .058(3) .012(2) .001(3) .006(3) C28 .083(5) .057(3) .106(6) -.027(4) -.041(4) .037(3) C29 .0372(19) .050(2) .0230(16) .0061(15) .0127(15) .0110(16) C30 .065(3) .052(3) .046(3) .002(2) .020(2) .017(2) C31 .054(3) .093(4) .027(2) .011(2) .005(2) .013(3) C32 .046(2) .0296(18) .0319(18) .0114(15) .0014(17) .0061(16) C33 .140(7) .045(3) .063(4) .020(3) .050(4) .017(4) C34 .061(3) .031(2) .055(3) .0089(19) .016(2) .0127(19) C35 .116(6) .047(3) .098(5) .028(3) -.050(5) .006(4) C36 .055(3) .152(5) .024(2) .016(3) .0138(19) .040(3) C37 .063(3) .046(2) .040(2) .0093(19) .014(2) .017(2) C38 .058(3) .131(6) .045(3) .020(4) .014(3) -.011(4) C39C .088(11) .043(6) .076(9) .015(5) .035(7) .023(6) C40 .042(2) .071(3) .047(2) .021(2) .021(2) .020(2) C41 .052(3) .104(5) .084(4) .053(4) .033(3) .043(3) C42 .047(3) .130(5) .083(4) .031(4) -.004(3) .036(3) C43 .043(2) .072(3) .040(2) .013(2) -.0072(18) .019(2) C39D .19(4) .041(7) .040(7) .015(5) .019(12) .049(13) C19B .036(9) .077(15) .044(8) .026(9) -.002(7) .010(7) #=============================================================================== # 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 Y O 2.361(2) . . yes Y N1 2.339(3) . . yes Y N2 2.369(2) . . yes Y C1 2.784(3) . . yes Y C32 2.374(4) . . yes Y C36 2.384(4) . . yes Si1 C32 1.828(4) . . yes Si1 C33 1.876(9) . . yes Si1 C34 1.871(5) . . yes Si1 C35 1.878(9) . . yes Si2 C36 1.823(5) . . yes Si2 C37 1.869(5) . . yes Si2 C38 1.877(6) . . yes Si2 C39C 1.881(18) . . yes Si2 C39D 1.88(2) . . yes O C40 1.462(5) . . yes O C43 1.454(5) . . yes N1 C1 1.345(4) . . yes N1 C8 1.423(4) . . yes N2 C1 1.336(4) . . yes N2 C20 1.427(4) . . yes C1 C2 1.501(4) . . no C2 C3 1.388(4) . . no C2 C7 1.390(5) . . no C3 C4 1.390(5) . . no C4 C5 1.375(6) . . no C5 C6 1.370(6) . . no C6 C7 1.393(5) . . no C8 C9 1.409(5) . . no C8 C13 1.413(4) . . no C9 C10 1.399(5) . . no C9 C14 1.507(6) . . no C10 C11 1.375(6) . . no C11 C12 1.376(6) . . no C12 C13 1.402(5) . . no C13 C17 1.514(5) . . no C14 C15 1.533(7) . . no C14 C16 1.523(6) . . no C17 C18 1.515(6) . . no C17 C19A 1.566(13) . . no C17 C19B 1.51(3) . . no C20 C21 1.401(5) . . no C20 C25 1.403(5) . . no C21 C22 1.406(6) . . no C21 C26 1.513(7) . . no C22 C23 1.368(7) . . no C23 C24 1.364(7) . . no C24 C25 1.392(6) . . no C25 C29 1.509(6) . . no C26 C27 1.532(7) . . no C26 C28 1.527(8) . . no C29 C30 1.527(7) . . no C29 C31 1.533(6) . . no C40 C41 1.485(8) . . no C41 C42 1.468(10) . . no C42 C43 1.522(7) . . no C3 H3 .90(4) . . no C4 H4 1.00(4) . . no C5 H5 .81(4) . . no C6 H6 .93(4) . . no C7 H7 .97(3) . . no C10 H10 .96(4) . . no C11 H11 .90(4) . . no C12 H12 .97(4) . . no C14 H14 .90(4) . . no C15 H15 .99(5) . . no C15 H15' .92(6) . . no C15 H15" .90(6) . . no C16 H16 .88(5) . . no C16 H16' .96(5) . . no C16 H16" 1.02(4) . . no C17 H17 .87(4) . . no C18 H18 .86(6) . . no C18 H18' .97(4) . . no C18 H18" .96(7) . . no C19A H19A .9806 . . no C19A H19B .9836 . . no C19A H19C .9749 . . no C19B H19F .9796 . . no C19B H19D .9787 . . no C19B H19E .9819 . . no C22 H22 .89(4) . . no C23 H23 .85(5) . . no C24 H24 .89(4) . . no C26 H26 .90(4) . . no C27 H27' .94(5) . . no C27 H27 1.04(5) . . no C27 H27" .84(5) . . no C28 H28 .91(7) . . no C28 H28' .74(7) . . no C28 H28" 1.04(8) . . no C29 H29 1.01(4) . . no C30 H30' .91(5) . . no C30 H30 .93(5) . . no C30 H30" .98(5) . . no C31 H31 .98(6) . . no C31 H31' .94(5) . . no C31 H31" .92(5) . . no C32 H32 .93(4) . . no C32 H32' .96(5) . . no C33 H33" .93(7) . . no C33 H33' .97(7) . . no C33 H33 .86(7) . . no C34 H34 .86(6) . . no C34 H34' .94(5) . . no C34 H34" 1.04(5) . . no C35 H35" .85(7) . . no C35 H35 .99(5) . . no C35 H35' .89(7) . . no C36 H36 .9904 . . no C36 H36' .9898 . . no C37 H37 .99(5) . . no C37 H37' .94(5) . . no C37 H37" .97(5) . . no C38 H38" .90(6) . . no C38 H38' 1.02(5) . . no C38 H38 .84(8) . . no C39C H39A .9794 . . no C39C H39B .9807 . . no C39C H39C .9799 . . no C39D H39F .9778 . . no C39D H39D .9777 . . no C39D H39E .9838 . . no C40 H40 .89(6) . . no C40 H40' .91(4) . . no C41 H41' .92(8) . . no C41 H41 .90(5) . . no C42 H42 .9895 . . no C42 H42' .9905 . . no C43 H43' .95(4) . . no C43 H43 .85(4) . . 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 O Y N1 142.97(9) . . . yes O Y N2 86.50(9) . . . yes O Y C1 115.08(8) . . . yes O Y C32 94.06(11) . . . yes O Y C36 91.38(13) . . . yes N1 Y N2 57.27(9) . . . yes N1 Y C1 28.79(8) . . . yes N1 Y C32 104.04(11) . . . yes N1 Y C36 106.62(15) . . . yes N2 Y C1 28.64(8) . . . yes N2 Y C32 108.68(11) . . . yes N2 Y C36 131.82(17) . . . yes C1 Y C32 106.48(11) . . . yes C1 Y C36 124.88(16) . . . yes C32 Y C36 119.48(19) . . . yes C32 Si1 C33 110.1(3) . . . yes C32 Si1 C34 114.4(2) . . . yes C32 Si1 C35 110.3(3) . . . yes C33 Si1 C34 106.6(3) . . . yes C33 Si1 C35 109.2(4) . . . yes C34 Si1 C35 106.1(3) . . . yes C36 Si2 C37 111.9(2) . . . yes C36 Si2 C38 113.6(2) . . . yes C36 Si2 C39C 120.1(7) . . . yes C36 Si2 C39D 99.2(17) . . . yes C37 Si2 C38 106.9(3) . . . yes C37 Si2 C39C 104.3(6) . . . yes C37 Si2 C39D 106.6(6) . . . yes C38 Si2 C39C 98.6(7) . . . yes C38 Si2 C39D 118.6(17) . . . yes Y O C40 123.0(2) . . . yes Y O C43 127.1(2) . . . yes C40 O C43 108.2(3) . . . yes Y N1 C1 94.29(17) . . . yes Y N1 C8 144.25(19) . . . yes C1 N1 C8 120.0(2) . . . yes Y N2 C1 93.18(17) . . . yes Y N2 C20 143.31(19) . . . yes C1 N2 C20 122.4(2) . . . yes Y C1 N1 56.92(15) . . . yes Y C1 N2 58.18(14) . . . yes Y C1 C2 170.39(19) . . . yes N1 C1 N2 114.6(2) . . . yes N1 C1 C2 121.6(2) . . . yes N2 C1 C2 123.6(2) . . . yes C1 C2 C3 119.1(3) . . . no C1 C2 C7 121.9(2) . . . no C3 C2 C7 119.0(3) . . . no C2 C3 C4 120.6(4) . . . no C3 C4 C5 119.7(4) . . . no C4 C5 C6 120.6(4) . . . no C5 C6 C7 120.0(4) . . . no C2 C7 C6 120.1(3) . . . no N1 C8 C9 119.7(3) . . . yes N1 C8 C13 119.5(3) . . . yes C9 C8 C13 120.8(3) . . . no C8 C9 C10 118.1(3) . . . no C8 C9 C14 121.1(3) . . . no C10 C9 C14 120.8(3) . . . no C9 C10 C11 121.6(4) . . . no C10 C11 C12 120.0(4) . . . no C11 C12 C13 121.2(4) . . . no C8 C13 C12 118.2(3) . . . no C8 C13 C17 122.7(3) . . . no C12 C13 C17 119.0(3) . . . no C9 C14 C15 113.5(4) . . . no C9 C14 C16 111.4(3) . . . no C15 C14 C16 110.2(4) . . . no C13 C17 C18 114.3(4) . . . no C13 C17 C19A 109.5(8) . . . no C13 C17 C19B 114.0(14) . . . no C18 C17 C19A 103.6(7) . . . no C18 C17 C19B 119.9(15) . . . no N2 C20 C21 117.1(3) . . . yes N2 C20 C25 121.8(3) . . . yes C21 C20 C25 120.9(3) . . . no C20 C21 C22 118.2(4) . . . no C20 C21 C26 122.7(3) . . . no C22 C21 C26 119.1(4) . . . no C21 C22 C23 121.0(4) . . . no C22 C23 C24 119.9(5) . . . no C23 C24 C25 122.1(5) . . . no C20 C25 C24 117.8(4) . . . no C20 C25 C29 123.7(3) . . . no C24 C25 C29 118.5(4) . . . no C21 C26 C27 111.5(4) . . . no C21 C26 C28 112.3(5) . . . no C27 C26 C28 108.8(5) . . . no C25 C29 C30 111.1(4) . . . no C25 C29 C31 111.6(4) . . . no C30 C29 C31 110.4(4) . . . no Y C32 Si1 129.1(2) . . . yes Y C36 Si2 136.1(3) . . . yes O C40 C41 106.3(4) . . . yes C40 C41 C42 102.5(5) . . . no C41 C42 C43 104.0(4) . . . no O C43 C42 104.3(4) . . . yes C2 C3 H3 123(3) . . . no C4 C3 H3 117(3) . . . no C3 C4 H4 116(2) . . . no C5 C4 H4 124(2) . . . no C4 C5 H5 118(3) . . . no C6 C5 H5 121(3) . . . no C5 C6 H6 117(2) . . . no C7 C6 H6 122(2) . . . no C2 C7 H7 120.4(16) . . . no C6 C7 H7 119.4(17) . . . no C9 C10 H10 119(2) . . . no C11 C10 H10 119(2) . . . no C10 C11 H11 120(3) . . . no C12 C11 H11 120(3) . . . no C11 C12 H12 116(2) . . . no C13 C12 H12 123(2) . . . no C9 C14 H14 102(3) . . . no C15 C14 H14 109(3) . . . no C16 C14 H14 111(3) . . . no C14 C15 H15 112(3) . . . no C14 C15 H15' 108(3) . . . no C14 C15 H15" 107(4) . . . no H15 C15 H15' 109(5) . . . no H15 C15 H15" 108(6) . . . no H15' C15 H15" 113(6) . . . no C14 C16 H16 112(3) . . . no C14 C16 H16' 110(3) . . . no C14 C16 H16" 111(2) . . . no H16 C16 H16' 106(4) . . . no H16 C16 H16" 107(4) . . . no H16' C16 H16" 110(3) . . . no C13 C17 H17 105(3) . . . no C18 C17 H17 105(3) . . . no C19A C17 H17 120(3) . . . no C19B C17 H17 95(3) . . . no C17 C18 H18 100(4) . . . no C17 C18 H18' 111(2) . . . no C17 C18 H18" 115(3) . . . no H18 C18 H18' 107(4) . . . no H18 C18 H18" 115(5) . . . no H18' C18 H18" 108(4) . . . no C17 C19A H19A 109.39 . . . no C17 C19A H19B 109.17 . . . no C17 C19A H19C 109.68 . . . no H19A C19A H19B 109.13 . . . no H19A C19A H19C 109.86 . . . no H19B C19A H19C 109.60 . . . no C17 C19B H19F 109.51 . . . no C17 C19B H19D 109.57 . . . no C17 C19B H19E 109.34 . . . no H19E C19B H19F 109.36 . . . no H19D C19B H19E 109.43 . . . no H19D C19B H19F 109.62 . . . no C21 C22 H22 119(3) . . . no C23 C22 H22 120(3) . . . no C24 C23 H23 121(3) . . . no C22 C23 H23 119(3) . . . no C23 C24 H24 124(3) . . . no C25 C24 H24 114(3) . . . no C27 C26 H26 107(3) . . . no C21 C26 H26 109(3) . . . no C28 C26 H26 108(3) . . . no H27 C27 H27" 122(4) . . . no C26 C27 H27' 117(3) . . . no H27' C27 H27" 97(5) . . . no C26 C27 H27 109(2) . . . no C26 C27 H27" 108(4) . . . no H27 C27 H27' 103(4) . . . no C26 C28 H28' 106(5) . . . no C26 C28 H28 110(4) . . . no H28 C28 H28" 124(6) . . . no C26 C28 H28" 110(4) . . . no H28 C28 H28' 102(7) . . . no H28' C28 H28" 103(7) . . . no C31 C29 H29 107(2) . . . no C25 C29 H29 112(2) . . . no C30 C29 H29 104(2) . . . no H30' C30 H30" 108(4) . . . no C29 C30 H30" 111(3) . . . no C29 C30 H30 111(3) . . . no C29 C30 H30' 110(3) . . . no H30 C30 H30' 114(5) . . . no H30 C30 H30" 103(4) . . . no C29 C31 H31' 106(3) . . . no C29 C31 H31 115(3) . . . no H31 C31 H31" 103(5) . . . no C29 C31 H31" 112(3) . . . no H31 C31 H31' 102(4) . . . no H31' C31 H31" 119(5) . . . no Si1 C32 H32 111(3) . . . no Y C32 H32 98(3) . . . no Y C32 H32' 99(3) . . . no Si1 C32 H32' 112(3) . . . no H32 C32 H32' 105(4) . . . no H33 C33 H33" 121(7) . . . no Si1 C33 H33 108(5) . . . no H33' C33 H33" 103(6) . . . no H33 C33 H33' 108(7) . . . no Si1 C33 H33' 111(4) . . . no Si1 C33 H33" 105(4) . . . no Si1 C34 H34' 110(3) . . . no Si1 C34 H34 107(4) . . . no H34 C34 H34" 104(5) . . . no Si1 C34 H34" 111(3) . . . no H34 C34 H34' 118(5) . . . no H34' C34 H34" 105(4) . . . no Si1 C35 H35" 109(5) . . . no Si1 C35 H35 108(3) . . . no Si1 C35 H35' 110(3) . . . no H35 C35 H35" 105(6) . . . no H35' C35 H35" 108(6) . . . no H35 C35 H35' 117(5) . . . no Si2 C36 H36' 103.18 . . . no H36 C36 H36' 105.12 . . . no Y C36 H36 103.07 . . . no Y C36 H36' 103.09 . . . no Si2 C36 H36 103.16 . . . no Si2 C37 H37" 107(3) . . . no Si2 C37 H37 108(3) . . . no Si2 C37 H37' 104(3) . . . no H37' C37 H37" 108(5) . . . no H37 C37 H37' 122(4) . . . no H37 C37 H37" 107(4) . . . no Si2 C38 H38 109(5) . . . no H38' C38 H38" 111(5) . . . no Si2 C38 H38" 108(4) . . . no H38 C38 H38' 103(6) . . . no Si2 C38 H38' 117(3) . . . no H38 C38 H38" 109(7) . . . no Si2 C39C H39C 109.48 . . . no H39A C39C H39B 109.46 . . . no Si2 C39C H39B 109.43 . . . no Si2 C39C H39A 109.51 . . . no H39A C39C H39C 109.52 . . . no H39B C39C H39C 109.42 . . . no Si2 C39D H39D 109.54 . . . no H39E C39D H39F 109.34 . . . no H39D C39D H39F 109.85 . . . no Si2 C39D H39E 109.21 . . . no Si2 C39D H39F 109.53 . . . no H39D C39D H39E 109.36 . . . no C41 C40 H40 108(4) . . . no C41 C40 H40' 111(2) . . . no H40 C40 H40' 117(5) . . . no O C40 H40' 110(3) . . . no O C40 H40 103(4) . . . no H41 C41 H41' 105(6) . . . no C40 C41 H41' 111(5) . . . no C42 C41 H41 118(3) . . . no C40 C41 H41 116(3) . . . no C42 C41 H41' 103(5) . . . no C41 C42 H42 110.97 . . . no C41 C42 H42' 110.93 . . . no C43 C42 H42 110.97 . . . no C43 C42 H42' 110.93 . . . no H42 C42 H42' 108.96 . . . no C42 C43 H43 107(3) . . . no C42 C43 H43' 117(2) . . . no H43 C43 H43' 118(4) . . . no O C43 H43 103(3) . . . no O C43 H43' 105(2) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Y O C40 67.7(4) . . . . no N1 Y O C43 -128.9(4) . . . . no N2 Y O C40 56.3(4) . . . . no N2 Y O C43 -140.2(4) . . . . no C1 Y O C40 58.1(4) . . . . no C1 Y O C43 -138.4(4) . . . . no C32 Y O C40 -52.2(4) . . . . no C32 Y O C43 111.3(4) . . . . no C36 Y O C40 -171.9(4) . . . . no C36 Y O C43 -8.4(4) . . . . no O Y N1 C1 -18.2(2) . . . . no O Y N1 C8 145.9(3) . . . . no N2 Y N1 C1 -4.65(15) . . . . no N2 Y N1 C8 159.4(4) . . . . no C1 Y N1 C8 164.1(4) . . . . no C32 Y N1 C1 98.75(19) . . . . no C32 Y N1 C8 -97.2(3) . . . . no C36 Y N1 C1 -134.1(2) . . . . no C36 Y N1 C8 30.0(4) . . . . no O Y N2 C1 176.57(17) . . . . no O Y N2 C20 -16.6(3) . . . . no N1 Y N2 C1 4.67(15) . . . . no N1 Y N2 C20 171.5(3) . . . . no C1 Y N2 C20 166.8(4) . . . . no C32 Y N2 C1 -90.33(19) . . . . no C32 Y N2 C20 76.5(3) . . . . no C36 Y N2 C1 87.8(2) . . . . no C36 Y N2 C20 -105.3(3) . . . . no O Y C1 N1 168.04(16) . . . . no O Y C1 N2 -3.78(19) . . . . no N1 Y C1 N2 -171.8(3) . . . . no N2 Y C1 N1 171.8(3) . . . . no C32 Y C1 N1 -89.26(19) . . . . no C32 Y C1 N2 98.92(19) . . . . no C36 Y C1 N1 57.0(2) . . . . no C36 Y C1 N2 -114.8(2) . . . . no O Y C32 Si1 -73.0(2) . . . . no N1 Y C32 Si1 139.5(2) . . . . no N2 Y C32 Si1 -160.7(2) . . . . no C1 Y C32 Si1 169.3(2) . . . . no C36 Y C32 Si1 20.9(3) . . . . no O Y C36 Si2 160.2(5) . . . . no N1 Y C36 Si2 -52.6(5) . . . . no N2 Y C36 Si2 -113.3(4) . . . . no C1 Y C36 Si2 -77.6(5) . . . . no C32 Y C36 Si2 64.7(5) . . . . no C1 Y C32 H32' 42(3) . . . . no C36 Y C32 H32 146(2) . . . . no C36 Y C32 H32' -107(3) . . . . no O Y C36 H36 -74.48 . . . . no O Y C36 H36' 34.72 . . . . no N1 Y C36 H36 72.72 . . . . no N1 Y C36 H36' -178.08 . . . . no N2 Y C36 H36 12.06 . . . . no N2 Y C36 H36' 121.26 . . . . no C1 Y C36 H36 47.78 . . . . no C1 Y C36 H36' 156.98 . . . . no C32 Y C36 H36 -169.93 . . . . no C32 Y C36 H36' -60.73 . . . . no N2 Y C32 H32 -35(2) . . . . no N2 Y C32 H32' 72(3) . . . . no C1 Y C32 H32 -65(2) . . . . no N1 Y C32 H32 -95(2) . . . . no O Y C32 H32 52(2) . . . . no O Y C32 H32' 159(3) . . . . no N1 Y C32 H32' 12(3) . . . . no C33 Si1 C32 Y -67.1(3) . . . . no C34 Si1 C32 Y 173.0(2) . . . . no C35 Si1 C32 Y 53.5(4) . . . . no C37 Si2 C36 Y 146.4(4) . . . . no C39C Si2 C36 Y -90.9(8) . . . . no C38 Si2 C36 Y 25.3(6) . . . . no Y O C40 C41 153.1(3) . . . . no Y O C43 C42 -176.1(4) . . . . no C40 O C43 C42 -10.7(6) . . . . no C43 O C40 C41 -13.1(6) . . . . no Y O C40 H40 40(4) . . . . no Y O C40 H40' -86(3) . . . . no Y O C43 H43' -53(3) . . . . no C40 O C43 H43 -123(3) . . . . no C40 O C43 H43' 113(3) . . . . no Y O C43 H43 72(3) . . . . no C43 O C40 H40 -127(4) . . . . no C43 O C40 H40' 108(3) . . . . no C8 N1 C1 N2 -161.7(2) . . . . no Y N1 C1 N2 7.6(3) . . . . no Y N1 C1 C2 -168.7(2) . . . . no C8 N1 C1 Y -169.3(3) . . . . no Y N1 C8 C13 -92.5(4) . . . . no C8 N1 C1 C2 21.9(4) . . . . no Y N1 C8 C9 84.6(4) . . . . no C1 N1 C8 C9 -113.8(3) . . . . no C1 N1 C8 C13 69.1(3) . . . . no C20 N2 C1 N1 -178.2(2) . . . . no Y N2 C1 N1 -7.5(2) . . . . no Y N2 C1 C2 168.8(2) . . . . no C20 N2 C1 Y -170.7(3) . . . . no Y N2 C20 C21 86.9(4) . . . . no Y N2 C20 C25 -89.1(4) . . . . no C20 N2 C1 C2 -1.9(4) . . . . no C1 N2 C20 C25 75.3(4) . . . . no C1 N2 C20 C21 -108.8(3) . . . . no N1 C1 C2 C7 -129.4(3) . . . . no N1 C1 C2 C3 52.2(4) . . . . no N2 C1 C2 C7 54.5(4) . . . . no N2 C1 C2 C3 -123.9(3) . . . . no C1 C2 C3 C4 178.1(3) . . . . no C3 C2 C7 C6 -.7(5) . . . . no C7 C2 C3 C4 -.4(5) . . . . no C1 C2 C7 C6 -179.2(3) . . . . no C2 C3 C4 C5 .3(5) . . . . no C3 C4 C5 C6 .9(6) . . . . no C4 C5 C6 C7 -2.0(6) . . . . no C5 C6 C7 C2 1.9(5) . . . . no N1 C8 C13 C12 178.1(3) . . . . no C13 C8 C9 C14 176.0(3) . . . . no N1 C8 C9 C10 -179.7(3) . . . . no N1 C8 C9 C14 -1.2(4) . . . . no C13 C8 C9 C10 -2.5(4) . . . . no C9 C8 C13 C12 1.0(4) . . . . no C9 C8 C13 C17 -176.2(3) . . . . no N1 C8 C13 C17 1.0(4) . . . . no C10 C9 C14 C16 84.3(5) . . . . no C10 C9 C14 C15 -40.7(5) . . . . no C8 C9 C10 C11 1.8(5) . . . . no C14 C9 C10 C11 -176.7(4) . . . . no C8 C9 C14 C15 140.9(4) . . . . no C8 C9 C14 C16 -94.1(4) . . . . no C9 C10 C11 C12 .6(6) . . . . no C10 C11 C12 C13 -2.3(6) . . . . no C11 C12 C13 C8 1.5(5) . . . . no C11 C12 C13 C17 178.7(4) . . . . no C8 C13 C17 C18 -134.7(4) . . . . no C8 C13 C17 C19A 109.5(8) . . . . no C12 C13 C17 C18 48.2(5) . . . . no C12 C13 C17 C19A -67.6(9) . . . . no N2 C20 C21 C22 -177.7(3) . . . . no N2 C20 C21 C26 3.1(5) . . . . no C25 C20 C21 C22 -1.7(5) . . . . no C25 C20 C21 C26 179.1(4) . . . . no N2 C20 C25 C24 178.0(3) . . . . no N2 C20 C25 C29 -1.6(5) . . . . no C21 C20 C25 C24 2.2(5) . . . . no C21 C20 C25 C29 -177.4(3) . . . . no C20 C21 C22 C23 .1(6) . . . . no C26 C21 C22 C23 179.3(4) . . . . no C20 C21 C26 C27 -115.4(4) . . . . no C20 C21 C26 C28 122.3(5) . . . . no C22 C21 C26 C27 65.5(5) . . . . no C22 C21 C26 C28 -56.8(6) . . . . no C21 C22 C23 C24 1.0(7) . . . . no C22 C23 C24 C25 -.5(8) . . . . no C23 C24 C25 C20 -1.1(7) . . . . no C23 C24 C25 C29 178.5(4) . . . . no C20 C25 C29 C30 111.6(4) . . . . no C20 C25 C29 C31 -124.7(4) . . . . no C24 C25 C29 C30 -68.0(5) . . . . no C24 C25 C29 C31 55.7(5) . . . . no O C40 C41 C42 32.1(6) . . . . no C40 C41 C42 C43 -38.2(7) . . . . no C41 C42 C43 O 30.7(7) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Y C14 4.289(4) . . no Y C16 4.289(6) . . no Y C17 4.435(4) . . no Y C26 4.315(4) . . no Y C19B 4.21(3) . . no Y H16" 3.51(4) . . no Y H17 3.87(4) . . no Y H14 3.71(4) . . no Y H29 3.82(4) . . no Y H35 3.86(5) . . no Y H26 3.62(4) . . no Y H19D 3.3147 . . no Si2 H19A 3.3726 . . no Si2 H19D 3.3615 . . no N1 H3 2.90(4) . . no N1 H14 2.41(4) . . no N1 H17 2.49(4) . . no N2 H26 2.42(4) . . no N2 H29 2.58(4) . . no C1 C17 3.194(5) . . no C1 C29 3.377(5) . . no C2 C17 3.576(5) . . no C2 C25 3.351(5) . . no C2 C13 3.360(4) . . no C2 C29 3.451(5) . . no C3 C9 3.397(5) . . no C3 C8 3.129(4) . . no C3 C31 3.467(6) . . no C5 C5 3.427(6) . 2_656 no C7 C21 3.542(5) . . no C7 C20 3.097(5) . . no C7 C25 3.564(6) . . no C8 C3 3.129(4) . . no C9 C3 3.397(5) . . no C13 C2 3.360(4) . . no C14 Y 4.289(4) . . no C16 Y 4.289(6) . . no C17 C1 3.194(5) . . no C17 Y 4.435(4) . . no C17 C2 3.576(5) . . no C19B Y 4.21(3) . . no C20 C7 3.097(5) . . no C20 C40 3.583(6) . . no C21 C7 3.542(5) . . no C23 C23 3.502(8) . 2_556 no C25 C2 3.351(5) . . no C25 C7 3.564(6) . . no C26 Y 4.315(4) . . no C29 C1 3.377(5) . . no C29 C2 3.451(5) . . no C31 C3 3.467(6) . . no C40 C20 3.583(6) . . no C1 H29 2.73(4) . . no C1 H17 2.50(4) . . no C2 H29 3.00(4) . . no C2 H17 3.02(4) . . no C3 H31" 2.98(5) . . no C4 H31" 3.06(5) . . no C6 H23 2.89(5) . 2_556 no C7 H18" 3.03(6) . . no C8 H3 2.93(4) . . no C9 H3 2.88(4) . . no C10 H15 3.09(5) . . no C10 H15" 2.75(7) . . no C10 H41 3.08(5) . 1_655 no C12 H5 3.03(4) . 2_656 no C12 H18 2.72(6) . . no C12 H19C 2.8478 . . no C14 H3 2.87(4) . . no C15 H32' 3.01(5) . 2_666 no C15 H15' 3.08(5) . 2_666 no C15 H10 2.68(4) . . no C16 H32' 3.06(5) . . no C18 H12 2.80(4) . . no C18 H33' 3.02(7) . 1_545 no C19A H12 3.08(4) . . no C19B H36 3.0381 . . no C20 H40' 3.00(4) . . no C20 H7 2.84(3) . . no C21 H7 2.91(3) . . no C22 H28" 2.99(8) . . no C22 H27 2.85(4) . . no C23 H6 3.09(4) . 2_556 no C24 H31" 3.07(5) . . no C24 H31 2.93(6) . . no C24 H30" 2.83(4) . . no C27 H19E 3.0627 . 2_555 no C27 H22 2.96(4) . . no C28 H7 3.06(3) . . no C28 H22 2.88(4) . . no C30 H30 3.09(5) . 2_566 no C30 H24 2.92(4) . . no C31 H24 2.72(5) . . no C36 H19D 2.7190 . . no C37 H12 3.03(4) . 2_655 no C39D H41' 3.08(9) . 2_565 no C43 H27" 3.09(5) . . no C43 H36' 2.9365 . . no H3 C8 2.93(4) . . no H3 H14 2.37(6) . . no H3 C9 2.88(4) . . no H3 C14 2.87(4) . . no H3 N1 2.90(4) . . no H3 H15 2.55(7) . . no H4 H34" 2.39(6) . 2_666 no H5 C12 3.03(4) . 2_656 no H6 H23 2.38(6) . 2_556 no H6 C23 3.09(4) . 2_556 no H7 C28 3.06(3) . . no H7 C21 2.91(3) . . no H7 C20 2.84(3) . . no H7 H28 2.32(7) . . no H10 C15 2.68(4) . . no H10 H15" 2.20(8) . . no H10 H41 2.52(7) . 1_655 no H12 H18 2.26(7) . . no H12 C37 3.03(4) . 2_655 no H12 H37 2.39(7) . 2_655 no H12 H19C 2.5733 . . no H12 C18 2.80(4) . . no H12 C19A 3.08(4) . . no H14 H15' 2.59(7) . 2_666 no H14 H3 2.37(6) . . no H14 Y 3.71(4) . . no H14 N1 2.41(4) . . no H15 C10 3.09(5) . . no H15 H3 2.55(7) . . no H15 H34" 2.48(8) . 2_666 no H15' H16' 2.46(7) . . no H15' H15' 2.50(7) . 2_666 no H15' C15 3.08(5) . 2_666 no H15' H14 2.59(7) . 2_666 no H15" C10 2.75(7) . . no H15" H10 2.20(8) . . no H15" H16 2.57(8) . . no H16 H15" 2.57(8) . . no H16' H15' 2.46(7) . . no H16" Y 3.51(4) . . no H16" H38 2.35(9) . . no H17 C1 2.50(4) . . no H17 N1 2.49(4) . . no H17 Y 3.87(4) . . no H17 C2 3.02(4) . . no H18 C12 2.72(6) . . no H18 H12 2.26(7) . . no H18 H19C 2.1888 . . no H18' H19E 2.4559 . . no H18' H19B 2.4020 . . no H18' H33' 2.49(8) . 1_545 no H18" C7 3.03(6) . . no H19A Si2 3.3726 . . no H19A H38" 2.4559 . . no H19B H18' 2.4020 . . no H19C H18 2.1888 . . no H19C H19C 2.3615 . 2_655 no H19C C12 2.8478 . . no H19C H12 2.5733 . . no H19D C36 2.7190 . . no H19D H36 2.1480 . . no H19D Y 3.3147 . . no H19D Si2 3.3615 . . no H19E H18' 2.4559 . . no H19E C27 3.0627 . 2_555 no H22 C27 2.96(4) . . no H22 C28 2.88(4) . . no H22 H28" 2.52(9) . . no H22 H27 2.44(6) . . no H23 H6 2.38(6) . 2_556 no H23 C6 2.89(5) . 2_556 no H24 C30 2.92(4) . . no H24 H31 2.38(8) . . no H24 C31 2.72(5) . . no H24 H30" 2.45(6) . . no H26 Y 3.62(4) . . no H26 N2 2.42(4) . . no H27 C22 2.85(4) . . no H27 H37 2.45(7) . 2_555 no H27 H22 2.44(6) . . no H27 H28" 2.37(9) . . no H27' H28' 2.59(9) . . no H27" H43 2.55(7) . . no H27" C43 3.09(5) . . no H28 H7 2.32(7) . . no H28 H34' 2.60(9) . 1_545 no H28' H27' 2.59(9) . . no H28" H22 2.52(9) . . no H28" C22 2.99(8) . . no H28" H27 2.37(9) . . no H29 N2 2.58(4) . . no H29 Y 3.82(4) . . no H29 C2 3.00(4) . . no H29 C1 2.73(4) . . no H30 H40 2.52(8) . . no H30 C30 3.09(5) . 2_566 no H30' H31' 2.45(7) . . no H30" C24 2.83(4) . . no H30" H24 2.45(6) . . no H31 H39D 2.5991 . 1_556 no H31 H24 2.38(8) . . no H31 C24 2.93(6) . . no H31' H30' 2.45(7) . . no H31" C3 2.98(5) . . no H31" C4 3.06(5) . . no H31" C24 3.07(5) . . no H32 H40 2.56(7) . . no H32' C16 3.06(5) . . no H32' C15 3.01(5) . 2_666 no H33' C18 3.02(7) . 1_565 no H33' H18' 2.49(8) . 1_565 no H33" H39B 2.4443 . . no H33" H39F 2.3452 . . no H34' H28 2.60(9) . 1_565 no H34" H15 2.48(8) . 2_666 no H34" H4 2.39(6) . 2_666 no H35 Y 3.86(5) . . no H35 H43' 2.55(7) . . no H36 H19D 2.1480 . . no H36 C19B 3.0381 . . no H36' H39F 2.3486 . . no H36' C43 2.9365 . . no H36' H43' 2.4930 . . no H37 H27 2.45(7) . 2_555 no H37 H12 2.39(7) . 2_655 no H38 H16" 2.35(9) . . no H38" H19A 2.4559 . . no H39B H33" 2.4443 . . no H39D H31 2.5991 . 1_554 no H39D H41' 2.5747 . 2_565 no H39F H36' 2.3486 . . no H39F H33" 2.3452 . . no H40 H32 2.56(7) . . no H40 H30 2.52(8) . . no H40' C20 3.00(4) . . no H41 C10 3.08(5) . 1_455 no H41 H10 2.52(7) . 1_455 no H41' H39D 2.5747 . 2_565 no H41' C39D 3.08(9) . 2_565 no H43 H27" 2.55(7) . . no H43' H36' 2.4930 . . no H43' H35 2.55(7) . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C14 H14 N1 .90(4) 2.41(4) 2.894(5) 114(3) . yes C17 H17 N1 .87(4) 2.49(4) 2.931(5) 112(3) . yes C26 H26 N2 .90(4) 2.42(4) 2.870(5) 111(3) . yes C29 H29 N2 1.01(4) 2.58(4) 2.993(5) 104(3) . yes #===END of Crystallographic Information File data_c47h77n2 _database_code_CSD 192683 _audit_creation_date '2001-02-20 14:27:13' _audit_creation_method 'PLATON
option' _audit_update_record ; ? ; #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H77 N2 O2 Si2 Y' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C47 H77 N2 O2 Si2 Y' _chemical_formula_weight 847.22 _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 Y Y -2.7962 3.5667 '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' 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 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 10.8885(6) _cell_length_b 11.7658(6) _cell_length_c 20.830(1) _cell_angle_alpha 80.246(1) _cell_angle_beta 85.581(1) _cell_angle_gamma 69.055(1) _cell_volume 2455.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 90 _cell_measurement_reflns_used 5821 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.47 _cell_special_details ; The final unit cell was obtained from the xyz centroids of 5821 reflections after integration using the SAINT software package (Bruker, 2000). The intensity data were corrected for decay and absorption using SADABS (Sheldrick, 2000). ; _exptl_crystal_description ' block' _exptl_crystal_colour ' colorless' _exptl_crystal_size_max 0.380 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.260 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 1.271 _exptl_absorpt_correction_type 'Semi-empirical' _exptl_absorpt_process_detais 'SADABS (Sheldrick, Bruker, 2000)' _exptl_absorpt_correction_T_min 0.6437 _exptl_absorpt_correction_T_max 0.7334 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine focus sealed Siemens Mo tube ' _diffrn_radiation_monochromator 'parallel mounted graphite' _diffrn_radiation_detector ; CCD area-detector ; _diffrn_measurement_device_type ; Bruker Smart Apex ; _diffrn_measurement_method 'phi and omega scans' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temparature unit (KROFLEX, (Bruker, 2000)). ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'negligible' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 21485 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _diffrn_reflns_reduction_process ; Intensity data were corrected for Lorentz and polarization effects, decay and absorption and reduced to F~o~^2^ using SAINT (Bruker, 2000) and SABABS (Sheldrick, 2000) ; # number of unique reflections _reflns_number_total 11035 _reflns_number_gt 9712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker Version 5.168, 2000' _computing_cell_refinement 'SAINT, Bruker Version 6.02A, 2000' _computing_data_reduction 'XPREP, Bruker Version 5.1/NT, 2000' _computing_structure_solution ; DIRDIF-99 (Beurskens et al., 1999) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTO (Meetsma, 2000) PLATON (Spek, 1994, 1996) ; _computing_publication_material ; PLATON (Spek, 1990) SHELXL (Sheldrick, 1997) ; #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_details calc _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.4948P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens difmapm _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 11035 _refine_ls_number_parameters 795 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0782 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.711 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.055 #=============================================================================== # 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 Y1 Y Uani 0.19275(1) 0.30469(1) 0.29423(1) 1.000 0.0141(1) Si1 Si Uani -0.16992(4) 0.32210(4) 0.35187(2) 1.000 0.0210(1) Si2 Si Uani 0.34220(4) 0.37330(4) 0.44513(2) 1.000 0.0205(1) O1 O Uani 0.10450(11) 0.52503(10) 0.29591(5) 1.000 0.0200(3) O2 O Uani 0.21243(11) 0.11317(10) 0.36775(5) 1.000 0.0222(3) N1 N Uani 0.30725(12) 0.16733(12) 0.21904(6) 1.000 0.0165(3) N2 N Uani 0.24461(12) 0.36984(12) 0.18340(6) 1.000 0.0160(3) C1 C Uani 0.34217(16) 0.04020(14) 0.21322(8) 1.000 0.0196(4) C2 C Uani 0.25817(17) -0.00042(15) 0.18217(8) 1.000 0.0237(5) C3 C Uani 0.2901(2) -0.12755(17) 0.18412(10) 1.000 0.0311(6) C4 C Uani 0.3995(2) -0.21142(18) 0.21628(11) 1.000 0.0383(7) C5 C Uani 0.4826(2) -0.17125(16) 0.24607(10) 1.000 0.0341(6) C6 C Uani 0.45732(17) -0.04559(15) 0.24479(9) 1.000 0.0257(5) C7 C Uani 0.13367(18) 0.08659(17) 0.14725(9) 1.000 0.0265(5) C8 C Uani 0.0104(2) 0.0610(2) 0.17663(11) 1.000 0.0342(6) C9 C Uani 0.1444(3) 0.0792(2) 0.07377(10) 1.000 0.0393(7) C10 C Uani 0.55443(18) -0.00549(17) 0.27580(9) 1.000 0.0300(5) C11 C Uani 0.5634(2) -0.0473(2) 0.34910(11) 1.000 0.0398(7) C12 C Uani 0.6947(2) -0.0528(2) 0.24537(11) 1.000 0.0419(7) C13 C Uani 0.30352(14) 0.25617(14) 0.16875(7) 1.000 0.0159(4) C14 C Uani 0.36245(15) 0.22947(14) 0.10270(7) 1.000 0.0172(4) C15 C Uani 0.48126(17) 0.13171(15) 0.09842(8) 1.000 0.0223(5) C16 C Uani 0.53902(18) 0.10555(16) 0.03804(9) 1.000 0.0260(5) C17 C Uani 0.47850(19) 0.17626(17) -0.01876(9) 1.000 0.0260(5) C18 C Uani 0.36142(17) 0.27412(16) -0.01519(8) 1.000 0.0228(5) C19 C Uani 0.30344(16) 0.30105(15) 0.04511(8) 1.000 0.0194(5) C20 C Uani 0.24825(15) 0.47723(14) 0.14106(7) 1.000 0.0155(4) C21 C Uani 0.36810(15) 0.49633(14) 0.12326(7) 1.000 0.0174(4) C22 C Uani 0.36418(18) 0.60546(15) 0.08310(8) 1.000 0.0220(5) C23 C Uani 0.24641(18) 0.69390(16) 0.06054(8) 1.000 0.0250(5) C24 C Uani 0.12930(18) 0.67619(15) 0.07995(8) 1.000 0.0234(5) C25 C Uani 0.12664(16) 0.56947(15) 0.12050(7) 1.000 0.0189(4) C26 C Uani 0.50203(16) 0.40531(15) 0.14745(8) 1.000 0.0191(5) C27 C Uani 0.59958(18) 0.36876(17) 0.09063(9) 1.000 0.0254(5) C28 C Uani 0.56092(18) 0.45681(17) 0.19497(9) 1.000 0.0266(5) C29 C Uani -0.00315(16) 0.55296(16) 0.14290(8) 1.000 0.0227(5) C30 C Uani -0.04397(19) 0.47964(19) 0.10015(10) 1.000 0.0294(6) C31 C Uani -0.11534(19) 0.67521(19) 0.14818(10) 1.000 0.0314(6) C32 C Uani 0.17646(18) 0.61032(16) 0.27979(9) 1.000 0.0226(5) C33 C Uani 0.0832(2) 0.73312(16) 0.29634(10) 1.000 0.0285(5) C34 C Uani -0.00393(19) 0.69583(17) 0.35059(9) 1.000 0.0270(5) C35 C Uani -0.01809(17) 0.58414(16) 0.32949(9) 1.000 0.0234(5) C36 C Uani 0.1616(2) 0.01997(17) 0.35533(9) 1.000 0.0269(5) C37 C Uani 0.2083(2) -0.08368(18) 0.41095(10) 1.000 0.0329(6) C38 C Uani 0.19842(19) -0.01484(17) 0.46813(9) 1.000 0.0267(5) C39 C Uani 0.23621(19) 0.09550(17) 0.43724(8) 1.000 0.0246(5) C40 C Uani -0.03509(16) 0.31962(17) 0.29238(8) 1.000 0.0219(5) C41 C Uani -0.25052(19) 0.20846(19) 0.34208(11) 1.000 0.0305(6) C42 C Uani -0.11513(19) 0.28157(18) 0.43912(9) 1.000 0.0281(5) C43 C Uani -0.30036(19) 0.48035(19) 0.34597(12) 1.000 0.0337(6) C44 C Uani 0.35110(16) 0.31421(16) 0.36757(8) 1.000 0.0197(5) C45 C Uani 0.4799(2) 0.2722(2) 0.50088(10) 1.000 0.0330(6) C46 C Uani 0.1867(2) 0.3870(2) 0.49497(10) 1.000 0.0338(6) C47 C Uani 0.3499(2) 0.53306(18) 0.43337(10) 1.000 0.0300(6) H3 H Uiso 0.2359(19) -0.1508(18) 0.1631(9) 1.000 0.025(5) H4 H Uiso 0.415(2) -0.291(2) 0.2177(11) 1.000 0.039(6) H5 H Uiso 0.5599(19) -0.2334(19) 0.2690(10) 1.000 0.029(5) H7 H Uiso 0.1202(17) 0.1716(17) 0.1528(9) 1.000 0.020(5) H8 H Uiso 0.013(2) -0.017(2) 0.1687(10) 1.000 0.034(6) H8' H Uiso -0.063(2) 0.119(2) 0.1563(11) 1.000 0.038(6) H8" H Uiso -0.002(2) 0.067(2) 0.2250(12) 1.000 0.042(6) H9 H Uiso 0.222(2) 0.095(2) 0.0538(11) 1.000 0.041(6) H9' H Uiso 0.067(2) 0.137(2) 0.0544(12) 1.000 0.047(7) H9" H Uiso 0.146(2) -0.002(2) 0.0666(11) 1.000 0.046(6) H10 H Uiso 0.5277(19) 0.076(2) 0.2684(10) 1.000 0.030(5) H11 H Uiso 0.471(2) -0.017(2) 0.3711(12) 1.000 0.050(7) H11' H Uiso 0.630(3) -0.021(2) 0.3713(12) 1.000 0.057(7) H11" H Uiso 0.5969(19) -0.1322(19) 0.3541(9) 1.000 0.022(5) H12 H Uiso 0.753(2) -0.020(2) 0.2653(12) 1.000 0.053(7) H12' H Uiso 0.694(2) -0.028(2) 0.1968(13) 1.000 0.057(7) H12" H Uiso 0.736(3) -0.144(3) 0.2541(13) 1.000 0.061(8) H15 H Uiso 0.5193(18) 0.0871(18) 0.1354(10) 1.000 0.025(5) H16 H Uiso 0.620(2) 0.037(2) 0.0369(10) 1.000 0.034(5) H17 H Uiso 0.5142(19) 0.1598(18) -0.0586(10) 1.000 0.030(5) H18 H Uiso 0.3214(18) 0.3198(17) -0.0525(10) 1.000 0.021(5) H19 H Uiso 0.2245(18) 0.3670(17) 0.0476(9) 1.000 0.018(4) H22 H Uiso 0.4427(17) 0.6188(16) 0.0715(9) 1.000 0.016(4) H23 H Uiso 0.2469(19) 0.7637(19) 0.0333(10) 1.000 0.030(5) H24 H Uiso 0.050(2) 0.7357(19) 0.0652(10) 1.000 0.029(5) H26 H Uiso 0.4886(16) 0.3370(16) 0.1707(8) 1.000 0.014(4) H27 H Uiso 0.6186(18) 0.4393(18) 0.0684(9) 1.000 0.025(5) H27' H Uiso 0.5633(19) 0.3377(18) 0.0589(10) 1.000 0.029(5) H27" H Uiso 0.6840(19) 0.3049(18) 0.1085(9) 1.000 0.027(5) H28 H Uiso 0.5774(19) 0.5335(19) 0.1718(10) 1.000 0.031(5) H28' H Uiso 0.648(2) 0.394(2) 0.2113(10) 1.000 0.035(6) H28" H Uiso 0.502(2) 0.4744(19) 0.2344(10) 1.000 0.034(5) H29 H Uiso 0.0130(17) 0.5070(17) 0.1846(9) 1.000 0.019(4) H30 H Uiso -0.123(2) 0.470(2) 0.1156(11) 1.000 0.039(6) H30' H Uiso 0.022(2) 0.398(2) 0.0989(10) 1.000 0.032(5) H30" H Uiso -0.054(2) 0.519(2) 0.0559(12) 1.000 0.040(6) H31 H Uiso -0.089(2) 0.721(2) 0.1744(11) 1.000 0.036(6) H31' H Uiso -0.189(2) 0.6550(18) 0.1689(10) 1.000 0.031(5) H31" H Uiso -0.143(2) 0.7253(19) 0.1030(11) 1.000 0.035(6) H32 H Uiso 0.2011(19) 0.6118(18) 0.2342(10) 1.000 0.025(5) H32' H Uiso 0.2529(19) 0.5796(17) 0.3059(9) 1.000 0.022(5) H33 H Uiso 0.034(2) 0.782(2) 0.2613(11) 1.000 0.041(6) H33' H Uiso 0.130(2) 0.7732(19) 0.3098(10) 1.000 0.031(5) H34 H Uiso 0.0362(19) 0.6724(18) 0.3925(10) 1.000 0.028(5) H34' H Uiso -0.086(2) 0.757(2) 0.3539(11) 1.000 0.041(6) H35 H Uiso -0.0323(18) 0.5241(18) 0.3644(9) 1.000 0.024(5) H35' H Uiso -0.0899(19) 0.6071(18) 0.2968(10) 1.000 0.027(5) H36 H Uiso 0.1949(18) -0.0015(17) 0.3152(10) 1.000 0.023(5) H36' H Uiso 0.061(2) 0.057(2) 0.3556(10) 1.000 0.040(6) H37 H Uiso 0.308(2) -0.140(2) 0.4015(11) 1.000 0.042(6) H37' H Uiso 0.141(2) -0.128(2) 0.4173(12) 1.000 0.054(7) H38 H Uiso 0.110(2) 0.0127(19) 0.4879(10) 1.000 0.034(6) H38' H Uiso 0.257(2) -0.0657(19) 0.5034(10) 1.000 0.034(5) H39 H Uiso 0.186(2) 0.170(2) 0.4553(10) 1.000 0.030(5) H39' H Uiso 0.325(2) 0.0809(19) 0.4419(10) 1.000 0.030(5) H40 H Uiso -0.074(2) 0.384(2) 0.2565(12) 1.000 0.056(7) H40' H Uiso -0.013(2) 0.250(2) 0.2727(11) 1.000 0.038(6) H41 H Uiso -0.278(2) 0.217(2) 0.3011(12) 1.000 0.044(6) H41' H Uiso -0.325(2) 0.213(2) 0.3708(12) 1.000 0.052(7) H41" H Uiso -0.189(2) 0.123(2) 0.3520(11) 1.000 0.041(6) H42 H Uiso -0.054(2) 0.196(2) 0.4493(11) 1.000 0.047(6) H42' H Uiso -0.193(2) 0.289(2) 0.4685(11) 1.000 0.040(6) H42" H Uiso -0.066(2) 0.335(2) 0.4480(11) 1.000 0.049(7) H43 H Uiso -0.273(2) 0.539(2) 0.3624(11) 1.000 0.041(6) H43' H Uiso -0.383(3) 0.475(3) 0.3731(16) 1.000 0.095(10) H43" H Uiso -0.325(2) 0.510(2) 0.3043(13) 1.000 0.053(7) H44 H Uiso 0.404(2) 0.232(2) 0.3726(11) 1.000 0.043(6) H44' H Uiso 0.395(2) 0.356(2) 0.3355(11) 1.000 0.037(6) H45 H Uiso 0.477(2) 0.191(2) 0.5079(11) 1.000 0.045(6) H45' H Uiso 0.469(2) 0.298(2) 0.5426(12) 1.000 0.043(6) H45" H Uiso 0.568(2) 0.272(2) 0.4814(11) 1.000 0.046(6) H46 H Uiso 0.108(2) 0.423(2) 0.4668(12) 1.000 0.055(7) H46' H Uiso 0.185(2) 0.432(2) 0.5302(12) 1.000 0.045(6) H46" H Uiso 0.182(2) 0.304(2) 0.5163(12) 1.000 0.051(7) H47 H Uiso 0.415(3) 0.545(2) 0.4039(12) 1.000 0.055(7) H47' H Uiso 0.375(2) 0.546(2) 0.4751(12) 1.000 0.050(7) H47" H Uiso 0.266(3) 0.596(2) 0.4184(12) 1.000 0.057(7) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0162(1) 0.0133(1) 0.0126(1) -0.0028(1) 0.0037(1) -0.0052(1) Si1 0.0165(2) 0.0204(2) 0.0252(2) -0.0030(2) 0.0035(2) -0.0064(2) Si2 0.0171(2) 0.0252(2) 0.0206(2) -0.0080(2) 0.0013(2) -0.0074(2) O1 0.0211(5) 0.0149(5) 0.0238(6) -0.0052(4) 0.0064(5) -0.0065(5) O2 0.0294(6) 0.0214(6) 0.0171(6) 0.0012(5) 0.0001(5) -0.0126(5) N1 0.0203(6) 0.0123(6) 0.0159(6) -0.0035(5) 0.0040(5) -0.0046(5) N2 0.0184(6) 0.0136(6) 0.0152(6) -0.0028(5) 0.0041(5) -0.0051(5) C1 0.0270(8) 0.0129(7) 0.0171(8) -0.0034(6) 0.0104(6) -0.0066(6) C2 0.0333(9) 0.0195(8) 0.0198(8) -0.0056(7) 0.0108(7) -0.0122(7) C3 0.0442(11) 0.0235(9) 0.0331(10) -0.0132(8) 0.0136(9) -0.0198(9) C4 0.0485(12) 0.0149(9) 0.0494(13) -0.0095(9) 0.0194(10) -0.0107(9) C5 0.0363(10) 0.0151(8) 0.0417(11) -0.0017(8) 0.0103(9) -0.0012(8) C6 0.0288(9) 0.0167(8) 0.0270(9) -0.0028(7) 0.0093(7) -0.0046(7) C7 0.0366(10) 0.0243(9) 0.0247(9) -0.0059(7) 0.0013(7) -0.0173(8) C8 0.0360(11) 0.0369(11) 0.0366(11) -0.0072(9) -0.0006(9) -0.0204(9) C9 0.0620(15) 0.0439(13) 0.0245(10) -0.0049(9) -0.0003(10) -0.0339(12) C10 0.0295(9) 0.0180(9) 0.0350(10) -0.0011(8) -0.0003(8) -0.0006(7) C11 0.0352(11) 0.0428(13) 0.0353(11) -0.0062(10) 0.0059(9) -0.0074(10) C12 0.0297(10) 0.0525(14) 0.0360(12) 0.0015(10) 0.0033(9) -0.0098(10) C13 0.0156(7) 0.0171(7) 0.0157(7) -0.0041(6) 0.0029(6) -0.0065(6) C14 0.0222(8) 0.0168(7) 0.0161(7) -0.0060(6) 0.0069(6) -0.0110(6) C15 0.0266(8) 0.0180(8) 0.0217(8) -0.0042(7) 0.0068(7) -0.0080(7) C16 0.0308(9) 0.0195(8) 0.0290(9) -0.0098(7) 0.0142(7) -0.0105(7) C17 0.0402(10) 0.0272(9) 0.0196(8) -0.0130(7) 0.0156(7) -0.0217(8) C18 0.0314(9) 0.0276(9) 0.0158(8) -0.0048(7) 0.0037(7) -0.0182(8) C19 0.0234(8) 0.0193(8) 0.0187(8) -0.0058(6) 0.0043(6) -0.0111(7) C20 0.0239(8) 0.0128(7) 0.0098(7) -0.0034(5) 0.0036(6) -0.0065(6) C21 0.0240(8) 0.0157(7) 0.0140(7) -0.0049(6) 0.0029(6) -0.0082(6) C22 0.0299(9) 0.0204(8) 0.0191(8) -0.0039(7) 0.0053(7) -0.0136(7) C23 0.0392(10) 0.0153(8) 0.0189(8) 0.0015(7) 0.0029(7) -0.0100(7) C24 0.0287(9) 0.0169(8) 0.0182(8) -0.0010(6) -0.0005(7) -0.0011(7) C25 0.0232(8) 0.0182(8) 0.0129(7) -0.0038(6) 0.0023(6) -0.0044(6) C26 0.0218(8) 0.0184(8) 0.0180(8) -0.0025(6) 0.0033(6) -0.0090(6) C27 0.0249(9) 0.0268(9) 0.0261(9) -0.0075(8) 0.0075(7) -0.0109(8) C28 0.0279(9) 0.0267(9) 0.0260(9) -0.0072(8) -0.0005(7) -0.0092(8) C29 0.0207(8) 0.0248(9) 0.0164(8) 0.0005(7) 0.0018(6) -0.0026(7) C30 0.0238(9) 0.0286(10) 0.0352(11) -0.0083(8) 0.0063(8) -0.0082(8) C31 0.0238(9) 0.0336(10) 0.0324(10) -0.0142(9) 0.0010(8) -0.0008(8) C32 0.0294(9) 0.0213(8) 0.0205(8) -0.0057(7) 0.0064(7) -0.0133(7) C33 0.0385(10) 0.0185(8) 0.0300(10) -0.0043(8) -0.0003(8) -0.0117(8) C34 0.0287(9) 0.0218(9) 0.0270(9) -0.0088(7) 0.0040(7) -0.0033(7) C35 0.0226(8) 0.0221(8) 0.0233(9) -0.0065(7) 0.0071(7) -0.0054(7) C36 0.0371(10) 0.0259(9) 0.0231(9) -0.0019(7) 0.0013(8) -0.0189(8) C37 0.0435(11) 0.0256(9) 0.0300(10) -0.0005(8) 0.0005(8) -0.0144(9) C38 0.0342(10) 0.0244(9) 0.0202(9) 0.0017(7) 0.0024(7) -0.0114(8) C39 0.0309(9) 0.0265(9) 0.0172(8) 0.0002(7) -0.0003(7) -0.0127(8) C40 0.0210(8) 0.0231(9) 0.0221(8) -0.0036(7) 0.0043(6) -0.0091(7) C41 0.0259(9) 0.0322(10) 0.0365(11) -0.0049(9) 0.0037(8) -0.0149(8) C42 0.0281(9) 0.0288(10) 0.0247(9) -0.0032(8) 0.0055(7) -0.0083(8) C43 0.0215(9) 0.0278(10) 0.0490(13) -0.0085(9) -0.0038(9) -0.0035(8) C44 0.0199(8) 0.0192(8) 0.0192(8) -0.0038(7) 0.0027(6) -0.0061(7) C45 0.0345(11) 0.0358(11) 0.0274(10) -0.0044(9) -0.0064(8) -0.0097(9) C46 0.0303(10) 0.0483(13) 0.0321(10) -0.0226(10) 0.0129(8) -0.0203(9) C47 0.0280(9) 0.0296(10) 0.0358(11) -0.0133(8) 0.0024(8) -0.0111(8) #=============================================================================== # 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 Y1 O1 2.4269(11) . . yes Y1 O2 2.4505(11) . . yes Y1 N1 2.3949(13) . . yes Y1 N2 2.3969(13) . . yes Y1 C13 2.8530(15) . . yes Y1 C40 2.4265(19) . . yes Y1 C44 2.4333(18) . . yes Si1 C40 1.8420(18) . . yes Si1 C41 1.886(2) . . yes Si1 C42 1.8858(19) . . yes Si1 C43 1.886(2) . . yes Si2 C44 1.8469(17) . . yes Si2 C45 1.881(2) . . yes Si2 C46 1.887(2) . . yes Si2 C47 1.885(2) . . yes O1 C32 1.463(2) . . yes O1 C35 1.453(2) . . yes O2 C36 1.459(2) . . yes O2 C39 1.457(2) . . yes N1 C1 1.430(2) . . yes N1 C13 1.340(2) . . yes N2 C13 1.337(2) . . yes N2 C20 1.424(2) . . yes C1 C2 1.411(3) . . no C1 C6 1.422(3) . . no C2 C3 1.403(3) . . no C2 C7 1.524(3) . . no C3 C4 1.378(3) . . no C4 C5 1.385(3) . . no C5 C6 1.400(2) . . no C6 C10 1.524(3) . . no C7 C8 1.538(3) . . no C7 C9 1.541(3) . . no C10 C11 1.522(3) . . no C10 C12 1.551(3) . . no C13 C14 1.507(2) . . no C14 C15 1.399(2) . . no C14 C19 1.397(2) . . no C15 C16 1.394(3) . . no C16 C17 1.386(3) . . no C17 C18 1.386(3) . . no C18 C19 1.395(2) . . no C20 C21 1.413(2) . . no C20 C25 1.420(2) . . no C21 C22 1.397(2) . . no C21 C26 1.530(2) . . no C22 C23 1.386(3) . . no C23 C24 1.384(3) . . no C24 C25 1.398(2) . . no C25 C29 1.522(3) . . no C26 C27 1.538(3) . . no C26 C28 1.529(3) . . no C29 C30 1.526(3) . . no C29 C31 1.533(3) . . no C32 C33 1.518(3) . . no C33 C34 1.528(3) . . no C34 C35 1.515(3) . . no C36 C37 1.502(3) . . no C37 C38 1.527(3) . . no C38 C39 1.525(3) . . no C3 H3 0.90(2) . . no C4 H4 0.89(2) . . no C5 H5 0.99(2) . . no C7 H7 0.983(19) . . no C8 H8 0.95(2) . . no C8 H8' 0.92(2) . . no C8 H8" 1.02(2) . . no C9 H9 0.98(2) . . no C9 H9' 0.94(2) . . no C9 H9" 0.99(2) . . no C10 H10 0.89(2) . . no C11 H11 1.04(2) . . no C11 H11' 1.05(3) . . no C11 H11" 0.92(2) . . no C12 H12 1.00(2) . . no C12 H12' 1.00(3) . . no C12 H12" 0.99(3) . . no C15 H15 0.89(2) . . no C16 H16 0.96(2) . . no C17 H17 0.91(2) . . no C18 H18 0.91(2) . . no C19 H19 0.93(2) . . no C22 H22 0.93(2) . . no C23 H23 0.92(2) . . no C24 H24 0.93(2) . . no C26 H26 0.918(18) . . no C27 H27 0.96(2) . . no C27 H27' 0.98(2) . . no C27 H27" 1.01(2) . . no C28 H28 1.02(2) . . no C28 H28' 1.01(2) . . no C28 H28" 1.01(2) . . no C29 H29 0.935(19) . . no C30 H30 0.93(2) . . no C30 H30' 0.98(2) . . no C30 H30" 0.95(2) . . no C31 H31 0.95(2) . . no C31 H31' 0.97(2) . . no C31 H31" 1.03(2) . . no C32 H32 0.97(2) . . no C32 H32' 0.95(2) . . no C33 H33 0.92(2) . . no C33 H33' 0.89(2) . . no C34 H34 0.96(2) . . no C34 H34' 0.93(2) . . no C35 H35 0.969(19) . . no C35 H35' 1.01(2) . . no C36 H36 0.92(2) . . no C36 H36' 1.02(2) . . no C37 H37 1.07(2) . . no C37 H37' 1.03(2) . . no C38 H38 0.98(2) . . no C38 H38' 0.98(2) . . no C39 H39 0.97(2) . . no C39 H39' 0.93(2) . . no C40 H40 0.97(2) . . no C40 H40' 0.92(2) . . no C41 H41 0.90(2) . . no C41 H41' 0.96(2) . . no C41 H41" 0.99(2) . . no C42 H42 0.99(2) . . no C42 H42' 0.99(2) . . no C42 H42" 1.01(2) . . no C43 H43 0.96(2) . . no C43 H43' 1.04(3) . . no C43 H43" 0.90(3) . . no C44 H44 0.92(2) . . no C44 H44' 0.96(2) . . no C45 H45 0.95(2) . . no C45 H45' 0.95(2) . . no C45 H45" 1.01(2) . . no C46 H46 1.00(2) . . no C46 H46' 0.97(2) . . no C46 H46" 1.02(2) . . no C47 H47 0.93(3) . . no C47 H47' 0.98(2) . . no C47 H47" 0.98(3) . . 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 Y1 O2 138.80(4) . . . yes O1 Y1 N1 137.87(4) . . . yes O1 Y1 N2 82.23(4) . . . yes O1 Y1 C13 110.03(4) . . . yes O1 Y1 C40 85.53(5) . . . yes O1 Y1 C44 82.12(5) . . . yes O2 Y1 N1 83.32(4) . . . yes O2 Y1 N2 138.95(4) . . . yes O2 Y1 C13 111.17(4) . . . yes O2 Y1 C40 82.34(5) . . . yes O2 Y1 C44 82.77(5) . . . yes N1 Y1 N2 55.70(4) . . . yes N1 Y1 C13 27.89(4) . . . yes N1 Y1 C40 105.42(5) . . . yes N1 Y1 C44 108.82(5) . . . yes N2 Y1 C13 27.81(4) . . . yes N2 Y1 C40 104.49(5) . . . yes N2 Y1 C44 110.66(5) . . . yes C13 Y1 C40 106.69(5) . . . yes C13 Y1 C44 112.74(5) . . . yes C40 Y1 C44 140.56(6) . . . yes C40 Si1 C41 112.81(9) . . . yes C40 Si1 C42 113.39(9) . . . yes C40 Si1 C43 111.33(9) . . . yes C41 Si1 C42 104.98(10) . . . yes C41 Si1 C43 108.50(10) . . . yes C42 Si1 C43 105.33(10) . . . yes C44 Si2 C45 112.10(9) . . . yes C44 Si2 C46 115.03(9) . . . yes C44 Si2 C47 112.93(9) . . . yes C45 Si2 C46 105.15(10) . . . yes C45 Si2 C47 106.80(10) . . . yes C46 Si2 C47 104.05(10) . . . yes Y1 O1 C32 126.33(10) . . . yes Y1 O1 C35 122.41(10) . . . yes C32 O1 C35 109.53(13) . . . yes Y1 O2 C36 125.24(10) . . . yes Y1 O2 C39 123.37(10) . . . yes C36 O2 C39 108.57(13) . . . yes Y1 N1 C1 138.58(10) . . . yes Y1 N1 C13 95.43(9) . . . yes C1 N1 C13 124.10(13) . . . yes Y1 N2 C13 95.43(9) . . . yes Y1 N2 C20 140.62(10) . . . yes C13 N2 C20 122.90(13) . . . yes N1 C1 C2 120.79(15) . . . yes N1 C1 C6 118.21(15) . . . yes C2 C1 C6 120.74(15) . . . no C1 C2 C3 118.36(17) . . . no C1 C2 C7 123.39(15) . . . no C3 C2 C7 118.25(17) . . . no C2 C3 C4 121.2(2) . . . no C3 C4 C5 120.28(18) . . . no C4 C5 C6 121.16(19) . . . no C1 C6 C5 118.20(17) . . . no C1 C6 C10 122.44(15) . . . no C5 C6 C10 119.34(17) . . . no C2 C7 C8 111.93(16) . . . no C2 C7 C9 111.21(17) . . . no C8 C7 C9 109.86(19) . . . no C6 C10 C11 112.44(17) . . . no C6 C10 C12 112.45(16) . . . no C11 C10 C12 108.49(17) . . . no Y1 C13 N1 56.68(8) . . . yes Y1 C13 N2 56.76(8) . . . yes Y1 C13 C14 179.54(11) . . . yes N1 C13 N2 113.43(13) . . . yes N1 C13 C14 122.86(14) . . . yes N2 C13 C14 123.70(13) . . . yes C13 C14 C15 119.45(14) . . . no C13 C14 C19 122.01(15) . . . no C15 C14 C19 118.53(14) . . . no C14 C15 C16 120.81(15) . . . no C15 C16 C17 120.07(17) . . . no C16 C17 C18 119.70(17) . . . no C17 C18 C19 120.48(16) . . . no C14 C19 C18 120.40(16) . . . no N2 C20 C21 121.52(14) . . . yes N2 C20 C25 117.97(15) . . . yes C21 C20 C25 120.38(14) . . . no C20 C21 C22 118.52(15) . . . no C20 C21 C26 123.34(14) . . . no C22 C21 C26 118.11(16) . . . no C21 C22 C23 121.57(18) . . . no C22 C23 C24 119.47(16) . . . no C23 C24 C25 121.65(17) . . . no C20 C25 C24 118.32(17) . . . no C20 C25 C29 120.69(14) . . . no C24 C25 C29 120.98(16) . . . no C21 C26 C27 111.66(14) . . . no C21 C26 C28 111.67(14) . . . no C27 C26 C28 109.65(16) . . . no C25 C29 C30 112.50(15) . . . no C25 C29 C31 112.97(15) . . . no C30 C29 C31 110.01(16) . . . no O1 C32 C33 105.74(16) . . . yes C32 C33 C34 103.10(15) . . . no C33 C34 C35 102.37(15) . . . no O1 C35 C34 105.75(15) . . . yes O2 C36 C37 105.26(16) . . . yes C36 C37 C38 102.12(16) . . . no C37 C38 C39 103.07(15) . . . no O2 C39 C38 106.50(15) . . . yes Y1 C40 Si1 137.32(9) . . . yes Y1 C44 Si2 135.72(9) . . . yes C2 C3 H3 116.5(13) . . . no C4 C3 H3 122.3(13) . . . no C3 C4 H4 118.7(15) . . . no C5 C4 H4 121.0(15) . . . no C4 C5 H5 118.5(13) . . . no C6 C5 H5 120.3(13) . . . no C2 C7 H7 109.2(11) . . . no C8 C7 H7 106.1(12) . . . no C9 C7 H7 108.4(11) . . . no C7 C8 H8 110.3(14) . . . no C7 C8 H8' 109.2(14) . . . no C7 C8 H8" 112.6(13) . . . no H8 C8 H8' 107(2) . . . no H8 C8 H8" 110.9(18) . . . no H8' C8 H8" 106.7(19) . . . no C7 C9 H9 111.7(14) . . . no C7 C9 H9' 107.7(15) . . . no C7 C9 H9" 110.0(13) . . . no H9 C9 H9' 111(2) . . . no H9 C9 H9" 110.4(19) . . . no H9' C9 H9" 106(2) . . . no C6 C10 H10 108.3(14) . . . no C11 C10 H10 108.4(13) . . . no C12 C10 H10 106.5(14) . . . no C10 C11 H11 110.5(14) . . . no C10 C11 H11' 113.6(14) . . . no C10 C11 H11" 105.0(12) . . . no H11 C11 H11' 111(2) . . . no H11 C11 H11" 110.5(18) . . . no H11' C11 H11" 106.2(19) . . . no C10 C12 H12 109.4(14) . . . no C10 C12 H12' 111.6(13) . . . no C10 C12 H12" 112.5(19) . . . no H12 C12 H12' 110.0(19) . . . no H12 C12 H12" 106(2) . . . no H12' C12 H12" 107(2) . . . no C14 C15 H15 118.2(13) . . . no C16 C15 H15 121.0(13) . . . no C15 C16 H16 118.6(12) . . . no C17 C16 H16 121.3(12) . . . no C16 C17 H17 121.3(13) . . . no C18 C17 H17 119.1(13) . . . no C17 C18 H18 119.5(13) . . . no C19 C18 H18 120.0(13) . . . no C14 C19 H19 119.0(11) . . . no C18 C19 H19 120.6(11) . . . no C21 C22 H22 118.9(11) . . . no C23 C22 H22 119.5(11) . . . no C22 C23 H23 119.7(14) . . . no C24 C23 H23 120.8(14) . . . no C23 C24 H24 119.7(14) . . . no C25 C24 H24 118.6(14) . . . no C21 C26 H26 107.4(12) . . . no C27 C26 H26 110.2(11) . . . no C28 C26 H26 106.1(11) . . . no C26 C27 H27 110.0(12) . . . no C26 C27 H27' 111.3(13) . . . no C26 C27 H27" 108.9(11) . . . no H27 C27 H27' 107.6(17) . . . no H27 C27 H27" 108.3(17) . . . no H27' C27 H27" 110.6(17) . . . no C26 C28 H28 109.6(12) . . . no C26 C28 H28' 110.1(13) . . . no C26 C28 H28" 110.8(13) . . . no H28 C28 H28' 108.1(18) . . . no H28 C28 H28" 111.5(17) . . . no H28' C28 H28" 106.6(17) . . . no C25 C29 H29 104.8(12) . . . no C30 C29 H29 108.0(12) . . . no C31 C29 H29 108.3(12) . . . no C29 C30 H30 110.3(14) . . . no C29 C30 H30' 112.3(13) . . . no C29 C30 H30" 111.5(14) . . . no H30 C30 H30' 108.1(19) . . . no H30 C30 H30" 109(2) . . . no H30' C30 H30" 105.3(18) . . . no C29 C31 H31 109.7(14) . . . no C29 C31 H31' 106.9(12) . . . no C29 C31 H31" 111.2(12) . . . no H31 C31 H31' 109.6(19) . . . no H31 C31 H31" 110.7(18) . . . no H31' C31 H31" 108.8(18) . . . no O1 C32 H32 107.3(13) . . . no O1 C32 H32' 107.9(12) . . . no C33 C32 H32 113.8(12) . . . no C33 C32 H32' 111.4(11) . . . no H32 C32 H32' 110.3(18) . . . no C32 C33 H33 112.5(14) . . . no C32 C33 H33' 108.9(14) . . . no C34 C33 H33 111.2(15) . . . no C34 C33 H33' 112.4(14) . . . no H33 C33 H33' 109(2) . . . no C33 C34 H34 113.1(13) . . . no C33 C34 H34' 113.0(14) . . . no C35 C34 H34 109.2(12) . . . no C35 C34 H34' 110.6(14) . . . no H34 C34 H34' 108.4(19) . . . no O1 C35 H35 108.3(12) . . . no O1 C35 H35' 106.3(12) . . . no C34 C35 H35 115.5(12) . . . no C34 C35 H35' 112.4(12) . . . no H35 C35 H35' 108.1(17) . . . no O2 C36 H36 107.1(13) . . . no O2 C36 H36' 108.4(13) . . . no C37 C36 H36 113.7(12) . . . no C37 C36 H36' 110.5(12) . . . no H36 C36 H36' 111.6(17) . . . no C36 C37 H37 109.5(12) . . . no C36 C37 H37' 107.0(13) . . . no C38 C37 H37 111.8(12) . . . no C38 C37 H37' 109.8(14) . . . no H37 C37 H37' 115.7(18) . . . no C37 C38 H38 113.4(13) . . . no C37 C38 H38' 112.1(12) . . . no C39 C38 H38 110.5(13) . . . no C39 C38 H38' 112.1(13) . . . no H38 C38 H38' 105.8(18) . . . no O2 C39 H39 110.3(12) . . . no O2 C39 H39' 107.3(13) . . . no C38 C39 H39 112.7(13) . . . no C38 C39 H39' 112.0(13) . . . no H39 C39 H39' 108.0(19) . . . no Y1 C40 H40 105.6(14) . . . no Y1 C40 H40' 92.2(15) . . . no Si1 C40 H40 105.7(14) . . . no Si1 C40 H40' 109.1(14) . . . no H40 C40 H40' 101(2) . . . no Si1 C41 H41 113.0(15) . . . no Si1 C41 H41' 113.5(14) . . . no Si1 C41 H41" 111.2(14) . . . no H41 C41 H41' 107(2) . . . no H41 C41 H41" 106.0(19) . . . no H41' C41 H41" 105.4(19) . . . no Si1 C42 H42 112.5(13) . . . no Si1 C42 H42' 109.2(13) . . . no Si1 C42 H42" 110.4(13) . . . no H42 C42 H42' 106.6(19) . . . no H42 C42 H42" 105.9(19) . . . no H42' C42 H42" 112.3(19) . . . no Si1 C43 H43 113.4(14) . . . no Si1 C43 H43' 109.4(18) . . . no Si1 C43 H43" 110.6(15) . . . no H43 C43 H43' 107(2) . . . no H43 C43 H43" 108(2) . . . no H43' C43 H43" 108(2) . . . no Y1 C44 H44 97.8(14) . . . no Y1 C44 H44' 96.5(14) . . . no Si2 C44 H44 109.3(14) . . . no Si2 C44 H44' 108.4(14) . . . no H44 C44 H44' 106(2) . . . no Si2 C45 H45 108.1(14) . . . no Si2 C45 H45' 111.5(14) . . . no Si2 C45 H45" 111.0(13) . . . no H45 C45 H45' 106.5(19) . . . no H45 C45 H45" 110.5(19) . . . no H45' C45 H45" 109.1(19) . . . no Si2 C46 H46 110.9(14) . . . no Si2 C46 H46' 108.2(14) . . . no Si2 C46 H46" 113.2(13) . . . no H46 C46 H46' 114.6(19) . . . no H46 C46 H46" 103.5(19) . . . no H46' C46 H46" 106(2) . . . no Si2 C47 H47 114.7(14) . . . no Si2 C47 H47' 107.5(13) . . . no Si2 C47 H47" 111.8(17) . . . no H47 C47 H47' 104(2) . . . no H47 C47 H47" 107(2) . . . no H47' C47 H47" 111(2) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Y1 O1 C32 124.88(12) . . . . no O2 Y1 O1 C35 -38.49(14) . . . . no N1 Y1 O1 C32 -53.98(14) . . . . no N1 Y1 O1 C35 142.66(11) . . . . no N2 Y1 O1 C32 -56.80(12) . . . . no N2 Y1 O1 C35 139.83(12) . . . . no C13 Y1 O1 C32 -55.97(12) . . . . no C13 Y1 O1 C35 140.67(11) . . . . no C40 Y1 O1 C32 -162.11(12) . . . . no C40 Y1 O1 C35 34.52(12) . . . . no C44 Y1 O1 C32 55.44(12) . . . . no C44 Y1 O1 C35 -107.93(12) . . . . no O1 Y1 O2 C36 122.44(13) . . . . no O1 Y1 O2 C39 -36.37(15) . . . . no N1 Y1 O2 C36 -58.33(13) . . . . no N1 Y1 O2 C39 142.86(13) . . . . no N2 Y1 O2 C36 -55.02(15) . . . . no N2 Y1 O2 C39 146.16(12) . . . . no C13 Y1 O2 C36 -56.71(14) . . . . no C13 Y1 O2 C39 144.48(13) . . . . no C40 Y1 O2 C36 48.28(13) . . . . no C40 Y1 O2 C39 -110.53(13) . . . . no C44 Y1 O2 C36 -168.34(14) . . . . no C44 Y1 O2 C39 32.85(13) . . . . no O1 Y1 N1 C1 -167.51(14) . . . . no O1 Y1 N1 C13 -4.00(13) . . . . no O2 Y1 N1 C1 13.25(16) . . . . no O2 Y1 N1 C13 176.76(10) . . . . no N2 Y1 N1 C1 -164.12(18) . . . . no N2 Y1 N1 C13 -0.61(9) . . . . no C13 Y1 N1 C1 -163.5(2) . . . . no C40 Y1 N1 C1 -66.88(17) . . . . no C40 Y1 N1 C13 96.63(10) . . . . no C44 Y1 N1 C1 93.24(17) . . . . no C44 Y1 N1 C13 -103.25(10) . . . . no O1 Y1 N2 C13 178.32(10) . . . . no O1 Y1 N2 C20 10.95(17) . . . . no O2 Y1 N2 C13 -3.36(13) . . . . no O2 Y1 N2 C20 -170.73(15) . . . . no N1 Y1 N2 C13 0.61(9) . . . . no N1 Y1 N2 C20 -166.75(19) . . . . no C13 Y1 N2 C20 -167.4(2) . . . . no C40 Y1 N2 C13 -98.37(10) . . . . no C40 Y1 N2 C20 94.26(17) . . . . no C44 Y1 N2 C13 99.82(10) . . . . no C44 Y1 N2 C20 -67.55(18) . . . . no O1 Y1 C13 N1 177.15(9) . . . . no O1 Y1 C13 N2 -1.77(11) . . . . no O2 Y1 C13 N1 -3.45(11) . . . . no O2 Y1 C13 N2 177.63(9) . . . . no N1 Y1 C13 N2 -178.92(16) . . . . no N2 Y1 C13 N1 178.92(16) . . . . no C40 Y1 C13 N1 -91.55(10) . . . . no C40 Y1 C13 N2 89.53(11) . . . . no C44 Y1 C13 N1 87.46(11) . . . . no C44 Y1 C13 N2 -91.46(11) . . . . no O1 Y1 C40 Si1 -83.31(14) . . . . no O2 Y1 C40 Si1 57.23(14) . . . . no N1 Y1 C40 Si1 138.09(13) . . . . no N2 Y1 C40 Si1 -164.09(13) . . . . no C13 Y1 C40 Si1 167.10(13) . . . . no C44 Y1 C40 Si1 -11.5(2) . . . . no O1 Y1 C44 Si2 55.02(12) . . . . no O2 Y1 C44 Si2 -86.54(12) . . . . no N1 Y1 C44 Si2 -166.93(11) . . . . no N2 Y1 C44 Si2 133.59(12) . . . . no C13 Y1 C44 Si2 163.49(11) . . . . no C40 Y1 C44 Si2 -18.00(18) . . . . no C41 Si1 C40 Y1 -129.53(14) . . . . no C42 Si1 C40 Y1 -10.36(17) . . . . no C43 Si1 C40 Y1 108.21(15) . . . . no C45 Si2 C44 Y1 143.03(12) . . . . no C46 Si2 C44 Y1 22.97(16) . . . . no C47 Si2 C44 Y1 -96.28(14) . . . . no C32 O1 C35 C34 -15.36(18) . . . . no Y1 O1 C35 C34 150.47(11) . . . . no Y1 O1 C32 C33 -173.18(10) . . . . no C35 O1 C32 C33 -8.03(18) . . . . no Y1 O2 C36 C37 175.02(11) . . . . no C39 O2 C36 C37 -23.5(2) . . . . no Y1 O2 C39 C38 162.24(11) . . . . no C36 O2 C39 C38 0.4(2) . . . . no Y1 N1 C1 C2 90.5(2) . . . . no Y1 N1 C13 N2 0.99(15) . . . . no Y1 N1 C13 C14 179.95(16) . . . . no C1 N1 C13 Y1 166.89(18) . . . . no C1 N1 C13 N2 167.88(15) . . . . no Y1 N1 C1 C6 -83.7(2) . . . . no C13 N1 C1 C2 -69.6(2) . . . . no C13 N1 C1 C6 116.22(19) . . . . no C1 N1 C13 C14 -13.2(2) . . . . no C20 N2 C13 N1 169.50(14) . . . . no Y1 N2 C20 C21 103.08(18) . . . . no Y1 N2 C20 C25 -72.7(2) . . . . no C20 N2 C13 C14 -9.5(2) . . . . no Y1 N2 C13 N1 -0.99(14) . . . . no Y1 N2 C13 C14 -179.94(14) . . . . no C20 N2 C13 Y1 170.49(17) . . . . no C13 N2 C20 C25 122.35(17) . . . . no C13 N2 C20 C21 -61.9(2) . . . . no N1 C1 C2 C3 -173.08(16) . . . . no N1 C1 C2 C7 6.2(3) . . . . no C6 C1 C2 C7 -179.74(17) . . . . no N1 C1 C6 C5 172.11(16) . . . . no C6 C1 C2 C3 1.0(3) . . . . no C2 C1 C6 C10 176.72(17) . . . . no C2 C1 C6 C5 -2.1(3) . . . . no N1 C1 C6 C10 -9.1(3) . . . . no C1 C2 C7 C8 -120.94(19) . . . . no C7 C2 C3 C4 -178.37(19) . . . . no C3 C2 C7 C9 -64.9(2) . . . . no C1 C2 C7 C9 115.8(2) . . . . no C3 C2 C7 C8 58.4(2) . . . . no C1 C2 C3 C4 1.0(3) . . . . no C2 C3 C4 C5 -1.7(3) . . . . no C3 C4 C5 C6 0.5(3) . . . . no C4 C5 C6 C10 -177.50(19) . . . . no C4 C5 C6 C1 1.3(3) . . . . no C5 C6 C10 C11 -64.4(2) . . . . no C1 C6 C10 C11 116.8(2) . . . . no C1 C6 C10 C12 -120.39(19) . . . . no C5 C6 C10 C12 58.4(2) . . . . no N2 C13 C14 C15 140.61(17) . . . . no N2 C13 C14 C19 -38.1(2) . . . . no N1 C13 C14 C15 -38.2(2) . . . . no N1 C13 C14 C19 143.07(17) . . . . no C13 C14 C15 C16 -179.27(16) . . . . no C19 C14 C15 C16 -0.5(3) . . . . no C13 C14 C19 C18 179.50(16) . . . . no C15 C14 C19 C18 0.8(3) . . . . no C14 C15 C16 C17 -0.3(3) . . . . no C15 C16 C17 C18 1.0(3) . . . . no C16 C17 C18 C19 -0.7(3) . . . . no C17 C18 C19 C14 -0.2(3) . . . . no N2 C20 C21 C22 -178.11(14) . . . . no N2 C20 C21 C26 -0.1(2) . . . . no C21 C20 C25 C29 -176.20(14) . . . . no C21 C20 C25 C24 3.0(2) . . . . no N2 C20 C25 C29 -0.4(2) . . . . no C25 C20 C21 C22 -2.4(2) . . . . no C25 C20 C21 C26 175.57(14) . . . . no N2 C20 C25 C24 178.80(14) . . . . no C20 C21 C26 C27 126.52(16) . . . . no C20 C21 C26 C28 -110.32(18) . . . . no C22 C21 C26 C27 -55.5(2) . . . . no C26 C21 C22 C23 -178.36(15) . . . . no C20 C21 C22 C23 -0.2(2) . . . . no C22 C21 C26 C28 67.71(19) . . . . no C21 C22 C23 C24 2.3(3) . . . . no C22 C23 C24 C25 -1.8(3) . . . . no C23 C24 C25 C29 178.32(15) . . . . no C23 C24 C25 C20 -0.9(2) . . . . no C20 C25 C29 C30 -85.02(19) . . . . no C20 C25 C29 C31 149.68(15) . . . . no C24 C25 C29 C30 95.81(19) . . . . no C24 C25 C29 C31 -29.5(2) . . . . no O1 C32 C33 C34 27.79(19) . . . . no C32 C33 C34 C35 -36.34(19) . . . . no C33 C34 C35 O1 32.11(18) . . . . no O2 C36 C37 C38 36.7(2) . . . . no C36 C37 C38 C39 -35.7(2) . . . . no C37 C38 C39 O2 22.3(2) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Y1 C10 4.352(2) . . no Y1 C29 4.0596(17) . . no Y1 H7 3.816(19) . . no Y1 H10 3.74(2) . . no Y1 H29 3.198(19) . . no Si1 C35 3.9363(19) . . no Si2 C39 3.867(2) . . no Si1 H35 3.28(2) . . no Si1 H36' 3.22(2) . . no Si1 H28' 3.48(2) . 1_455 no Si2 H32' 3.407(19) . . no Si2 H39 3.37(2) . . no O1 C29 3.404(2) . . no O1 H29 2.662(19) . . no O2 H11 2.68(2) . . no N2 C30 3.425(3) . . no N1 H10 2.48(2) . . no N1 H15 2.76(2) . . no N1 H7 2.53(2) . . no N2 H19 2.861(19) . . no N2 H26 2.544(19) . . no N2 H29 2.46(2) . . no C1 C15 2.984(2) . . no C1 C36 3.447(3) . . no C2 C15 3.534(3) . . no C2 C14 3.426(2) . . no C6 C15 3.439(2) . . no C7 C13 3.267(3) . . no C7 C14 3.464(3) . . no C9 C19 3.566(3) . . no C9 C14 3.565(4) . . no C10 Y1 4.352(2) . . no C13 C26 3.201(2) . . no C13 C7 3.267(3) . . no C14 C9 3.565(4) . . no C14 C7 3.464(3) . . no C14 C26 3.253(2) . . no C14 C2 3.426(2) . . no C14 C21 3.262(2) . . no C14 C27 3.493(3) . . no C15 C2 3.534(3) . . no C15 C27 3.442(3) . . no C15 C6 3.439(2) . . no C15 C1 2.984(2) . . no C16 C16 3.529(3) . 2_655 no C16 C17 3.479(3) . 2_655 no C17 C16 3.479(3) . 2_655 no C17 C22 3.599(3) . 2_665 no C19 C21 3.320(2) . . no C19 C9 3.566(3) . . no C19 C20 2.997(2) . . no C20 C19 2.997(2) . . no C20 C32 3.424(2) . . no C21 C19 3.320(2) . . no C21 C14 3.262(2) . . no C22 C27 3.583(2) . 2_665 no C22 C17 3.599(3) . 2_665 no C23 C27 3.516(3) . 2_665 no C25 C32 3.541(2) . . no C26 C14 3.253(2) . . no C26 C13 3.201(2) . . no C27 C22 3.583(2) . 2_665 no C27 C14 3.493(3) . . no C27 C15 3.442(3) . . no C27 C23 3.516(3) . 2_665 no C29 O1 3.404(2) . . no C29 Y1 4.0596(17) . . no C30 N2 3.425(3) . . no C32 C20 3.424(2) . . no C32 C25 3.541(2) . . no C35 Si1 3.9363(19) . . no C36 C1 3.447(3) . . no C39 Si2 3.867(2) . . no C1 H15 2.57(2) . . no C1 H36 2.65(2) . . no C2 H36 2.80(2) . . no C3 H9" 2.89(2) . . no C3 H8 2.85(2) . . no C5 H12" 2.91(4) . . no C5 H11" 2.83(2) . . no C6 H15 2.72(2) . . no C6 H36 3.02(2) . . no C8 H3 2.84(2) . . no C9 H3 2.903(19) . . no C10 H15 2.95(2) . . no C11 H5 2.98(2) . . no C12 H5 2.95(2) . . no C12 H15 2.96(2) . . no C13 H7 2.59(2) . . no C13 H26 2.523(19) . . no C14 H9 2.90(2) . . no C14 H26 2.765(18) . . no C14 H7 3.02(2) . . no C14 H27' 2.92(2) . . no C15 H27' 2.85(2) . . no C15 H26 3.082(18) . . no C15 H12' 3.07(2) . . no C16 H27' 2.94(2) . . no C17 H27' 3.10(2) . . no C17 H22 2.862(19) . 2_665 no C18 H22 2.924(19) . 2_665 no C19 H27' 3.05(2) . . no C19 H30' 3.06(2) . . no C19 H9 2.84(2) . . no C20 H32 2.62(2) . . no C20 H19 2.591(19) . . no C21 H32 3.02(2) . . no C22 H28 2.87(2) . . no C22 H27' 3.03(2) . 2_665 no C22 H27 2.79(2) . . no C23 H27' 3.10(2) . 2_665 no C23 H3 3.009(19) . 1_565 no C24 H31 2.92(2) . . no C24 H31" 2.83(2) . . no C25 H32 2.74(2) . . no C25 H19 2.877(19) . . no C27 H22 2.801(18) . . no C28 H4 2.92(2) . 1_565 no C28 H43" 2.93(3) . 1_655 no C28 H22 3.000(19) . . no C29 H40 3.06(2) . . no C30 H19 2.95(2) . . no C31 H18 3.09(2) . 2_565 no C31 H24 2.60(2) . . no C31 H35' 3.07(2) . . no C32 H47" 3.08(3) . . no C35 H43 3.02(2) . . no C36 H40' 3.02(2) . . no C38 H42 2.97(2) . . no C39 H11 2.80(2) . . no C39 H42 2.96(2) . . no C39 H44 2.95(2) . . no C39 H46" 3.04(2) . . no C40 H29 3.024(19) . . no C40 H35 3.05(2) . . no C40 H36' 2.98(2) . . no C42 H39 3.09(2) . . no C44 H32' 3.002(19) . . no C44 H39' 3.01(2) . . no C45 H37 3.00(2) . 2_656 no C45 H38' 3.03(2) . 2_656 no C46 H39 2.82(2) . . no C47 H32' 2.827(19) . . no C47 H43' 2.97(3) . 1_655 no H3 C8 2.84(2) . . no H3 C9 2.903(19) . . no H3 C23 3.009(19) . 1_545 no H3 H8 2.38(3) . . no H3 H9" 2.44(3) . . no H4 C28 2.92(2) . 1_545 no H4 H28 2.47(3) . 1_545 no H4 H28" 2.55(3) . 1_545 no H5 C11 2.98(2) . . no H5 C12 2.95(2) . . no H5 H11" 2.43(3) . . no H5 H12" 2.47(4) . . no H7 Y1 3.816(19) . . no H7 N1 2.53(2) . . no H7 C13 2.59(2) . . no H7 C14 3.02(2) . . no H7 H30' 2.58(3) . . no H8 C3 2.85(2) . . no H8 H3 2.38(3) . . no H8 H9" 2.50(3) . . no H8' H9' 2.48(3) . . no H8" H40' 2.48(3) . . no H9 C14 2.90(2) . . no H9 C19 2.84(2) . . no H9' H8' 2.48(3) . . no H9" C3 2.89(2) . . no H9" H3 2.44(3) . . no H9" H8 2.50(3) . . no H10 Y1 3.74(2) . . no H10 N1 2.48(2) . . no H11 O2 2.68(2) . . no H11 C39 2.80(2) . . no H11 H39' 2.22(3) . . no H11' H12 2.49(4) . . no H11" C5 2.83(2) . . no H11" H5 2.43(3) . . no H11" H12" 2.47(4) . . no H12 H11' 2.49(4) . . no H12' C15 3.07(2) . . no H12' H15 2.24(3) . . no H12" C5 2.91(4) . . no H12" H5 2.47(4) . . no H12" H11" 2.47(4) . . no H15 N1 2.76(2) . . no H15 C1 2.57(2) . . no H15 C6 2.72(2) . . no H15 C10 2.95(2) . . no H15 C12 2.96(2) . . no H15 H12' 2.24(3) . . no H18 C31 3.09(2) . 2_565 no H18 H31" 2.53(3) . 2_565 no H19 N2 2.861(19) . . no H19 C20 2.591(19) . . no H19 C25 2.877(19) . . no H19 C30 2.95(2) . . no H19 H30' 2.31(3) . . no H22 C27 2.801(18) . . no H22 C28 3.000(19) . . no H22 H27 2.30(3) . . no H22 H28 2.50(3) . . no H22 C17 2.862(19) . 2_665 no H22 C18 2.92(2) . 2_665 no H24 C31 2.60(2) . . no H24 H31" 2.22(3) . . no H26 N2 2.544(19) . . no H26 C13 2.523(19) . . no H26 C14 2.765(18) . . no H26 C15 3.082(18) . . no H27 C22 2.79(2) . . no H27 H22 2.30(3) . . no H27 H28 2.52(3) . . no H27' C14 2.92(2) . . no H27' C15 2.85(2) . . no H27' C16 2.94(2) . . no H27' C17 3.10(2) . . no H27' C19 3.05(2) . . no H27' C22 3.03(2) . 2_665 no H27' C23 3.10(2) . 2_665 no H27" H28' 2.49(3) . . no H28 C22 2.87(2) . . no H28 H4 2.47(3) . 1_565 no H28 H22 2.50(3) . . no H28 H27 2.52(3) . . no H28' Si1 3.48(2) . 1_655 no H28' H27" 2.49(3) . . no H28' H41 2.49(3) . 1_655 no H28" H4 2.55(3) . 1_565 no H29 Y1 3.198(19) . . no H29 O1 2.662(19) . . no H29 N2 2.46(2) . . no H29 C40 3.024(19) . . no H29 H40 2.29(3) . . no H30 H31' 2.46(3) . . no H30' C19 3.06(2) . . no H30' H7 2.58(3) . . no H30' H19 2.31(3) . . no H30" H30" 2.56(3) . 2_565 no H31 C24 2.92(2) . . no H31' H30 2.46(3) . . no H31" C24 2.83(2) . . no H31" H24 2.22(3) . . no H31" H18 2.53(3) . 2_565 no H32 C20 2.62(2) . . no H32 C21 3.02(2) . . no H32 C25 2.74(2) . . no H32' Si2 3.407(19) . . no H32' C44 3.002(19) . . no H32' C47 2.827(19) . . no H32' H44' 2.53(3) . . no H32' H47" 2.40(3) . . no H34 H47" 2.41(4) . . no H35 Si1 3.28(2) . . no H35 C40 3.05(2) . . no H35 H43 2.57(3) . . no H35 H46 2.58(3) . . no H35' C31 3.07(2) . . no H36 C1 2.65(2) . . no H36 C2 2.80(2) . . no H36 C6 3.02(2) . . no H36' Si1 3.22(2) . . no H36' C40 2.98(2) . . no H36' H40' 2.52(3) . . no H36' H41" 2.55(3) . . no H37 C45 3.00(2) . 2_656 no H38 H42 2.32(3) . . no H38 H38 2.52(3) . 2_556 no H38' C45 3.03(2) . 2_656 no H38' H45" 2.48(3) . 2_656 no H39 Si2 3.37(2) . . no H39 C42 3.09(2) . . no H39 C46 2.82(2) . . no H39 H42 2.53(3) . . no H39 H46" 2.17(3) . . no H39' C44 3.01(2) . . no H39' H11 2.22(3) . . no H39' H44 2.45(3) . . no H40 C29 3.06(2) . . no H40 H29 2.29(3) . . no H40' C36 3.02(2) . . no H40' H8" 2.48(3) . . no H40' H36' 2.52(3) . . no H41 H28' 2.49(3) . 1_455 no H41' H45" 2.59(3) . 1_455 no H41" H36' 2.55(3) . . no H42 C38 2.97(2) . . no H42 C39 2.96(2) . . no H42 H38 2.32(3) . . no H42 H39 2.53(3) . . no H42' H47' 2.60(3) . 2_566 no H42" H46 2.54(3) . . no H43 C35 3.02(2) . . no H43 H35 2.57(3) . . no H43' C47 2.97(3) . 1_455 no H43' H47 2.14(5) . 1_455 no H43" C28 2.93(3) . 1_455 no H44 C39 2.95(2) . . no H44 H39' 2.45(3) . . no H44' H32' 2.53(3) . . no H45" H41' 2.59(3) . 1_655 no H45" H38' 2.48(3) . 2_656 no H46 H35 2.58(3) . . no H46 H42" 2.54(3) . . no H46" C39 3.04(2) . . no H46" H39 2.17(3) . . no H47 H43' 2.14(5) . 1_655 no H47' H42' 2.60(3) . 2_566 no H47" C32 3.08(3) . . no H47" H32' 2.40(3) . . no H47" H34 2.41(4) . . no #===END of Crystallographic Information File