# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_address ; Stratingh Institute University of Groningen Nijenborgh 4 Groningen 9747 AG NETHERLANDS ; _publ_contact_author_email B.HESSEN@RUG.NL _publ_contact_author_name 'Bart Hessen' _publ_contact_letter # Include date of submission ; Date of submission : 2006-05-01 11:34:17 Consider this CIF submission for deposition of the first X-ray structure of a manuscript to be submitted to : Chem. Comm (Our Compound_Identification_Code : Q1079) ; _publ_section_title ; The 6-amino-6-methyl-1,4-diazepine group as ancillary ligand framework for neutral and cationic scandium and yttrium alkyls ; loop_ _publ_author_name 'Bart Hessen' 'Sergio Bambirra' 'Shaozhong Ge' 'Auke Meetsma' data_Q1079 _database_code_depnum_ccdc_archive 'CCDC 606108' #============================================================================== # 0. AUDIT DETAILS _audit_creation_date '2006-01-31 16:44:17' _audit_creation_method ; PLATON option (version :: 300106) SHELXL97-2 & Manual Editing ; _audit_update_record ; ? ; # Insert blank lines between references _publ_section_references ; Allen, F.H. (2000). Acta Cryst. B58, 380-388. Beurskens, P.T., Beurskens, G., Gelder, R. de, Garc\'ia-Granda, S. Gould, R.O., Israel, & Smits, J.M.M. (1999). The DIRDIF99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Bondi, A. (1964). J. Phys. Chem. 68, 441-451. Bruker, (2000). SMART, SAINTPLUS and XPREP. Software Reference Manual Bruker AXS Inc. Madison, Wisconsin, USA. Hahn, T. (1983) Ed. International Tables for Crystallography, Volume A, Space-group symmetry, 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. (2005). Extended version of the program PLUTO. Groningen University, The Netherlands. (unpublished). Sheldrick, G.M. SHELXL97. Program for Crystal Structure Refinement. University of Gottingen, Germany, 1997. Sheldrick, G.M. SADABS. Version 2.03 Multi-Scan Absorption Correction Program. University of Gottingen, Germany, 2001 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. (2003). J. Appl. Cryst. 36, 7-13. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; Fig. 1. Perspective PLUTO drawing of the moolecule illustrating the configuration and the adopted numbering scheme. Fig. 2. Molecular packing viewed down unit cell axes. Fig. 3. Perspective ORTEP drawing of the title compound. Displacement ellipsoids for non-H are represented at the 50% probability level. The H-atoms have been omitted to improve clarity. ; #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H56 N3 Sc Si3' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C22 H56 N3 Sc Si3' _chemical_formula_iupac ? _chemical_formula_weight 491.92 _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' 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 '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 18.418(1) _cell_length_b 17.990(1) _cell_length_c 18.694(1) _cell_angle_alpha 90 _cell_angle_beta 95.799(1) _cell_angle_gamma 90 _cell_volume 6162.4(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 7628 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.85 _cell_special_details ; The final unit cell was obtained from the xyz centroids of 7628 reflections after integration using the SAINT software package (Bruker, 2000). ; _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.368 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details '(SADABS, Sheldrick, Bruker, 2001))' _exptl_absorpt_correction_T_min 0.8804 _exptl_absorpt_correction_T_max 0.9534 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 100(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; CCD area detector ; _diffrn_measurement_method '\f and \w scans' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temparature unit (KRYOFLEX, (Bruker, 2000)). ; _diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 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 41674 _diffrn_reflns_av_R_equivalents 0.1157 _diffrn_reflns_av_sigmaI/netI 0.1319 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 26.02 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _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 SADABS (Sheldrick, 2001) ; # number of unique reflections _reflns_number_total 12024 _reflns_number_gt 7135 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART, Version 5.624, (Bruker, 2001)' _computing_cell_refinement 'SAINTPLUS, Version 6.02A, (Bruker, 2000)' _computing_data_reduction 'XPREP, Version 5.1/NT, (Bruker, 2000)' _computing_structure_solution ; DIRDIF-99 (Beurskens et al., 1999) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTO (Meetsma, 2005) PLATON (Spek, 2003) ; _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _chemical_absolute_configuration ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 12024 _refine_ls_number_parameters 971 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.1162 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.393 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.076 _vrn_publ_code_squeezed_elec 0.0 _vrn_publ_code_void_volume 0.0 _vrn_publ_code_frame_time_sec 10.0 _vrn_publ_code_meas_time_hour 7.0 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT 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 Sc1 Sc Uani 0.56844(3) 0.12363(3) 0.31174(3) 1.000 0.0121(2) . . Si11 Si Uani 0.68628(5) 0.29695(5) 0.29317(5) 1.000 0.0166(3) . . Si12 Si Uani 0.70520(5) 0.08852(5) 0.46532(5) 1.000 0.0173(3) . . Si13 Si Uani 0.44720(5) 0.22201(5) 0.43613(5) 1.000 0.0173(3) . . N11 N Uani 0.61089(14) 0.07532(13) 0.19743(13) 1.000 0.0151(9) . . N12 N Uani 0.50884(15) 0.00192(14) 0.28995(13) 1.000 0.0165(9) . . N13 N Uani 0.46533(14) 0.12556(14) 0.21224(14) 1.000 0.0152(9) . . C11 C Uani 0.6809(2) 0.0334(2) 0.2027(2) 1.000 0.0203(12) . . C12 C Uani 0.6237(2) 0.14139(19) 0.15199(19) 1.000 0.0177(11) . . C13 C Uani 0.54763(18) 0.02821(17) 0.16595(16) 1.000 0.0152(11) . . C14 C Uani 0.5335(2) -0.03038(18) 0.22274(19) 1.000 0.0194(11) . . C15 C Uani 0.5250(3) -0.0526(2) 0.3496(2) 1.000 0.0239(14) . . C16 C Uani 0.4283(2) 0.0142(2) 0.2795(2) 1.000 0.0237(12) . . C17 C Uani 0.4072(2) 0.0905(2) 0.2492(2) 1.000 0.0214(12) . . C18 C Uani 0.4377(2) 0.1995(2) 0.1856(2) 1.000 0.0235(12) . . C19 C Uani 0.4811(2) 0.0785(2) 0.15028(19) 1.000 0.0182(12) . . C110 C Uani 0.5612(2) -0.0120(2) 0.0968(2) 1.000 0.0231(14) . . C111 C Uani 0.6020(2) 0.24420(18) 0.3022(2) 1.000 0.0183(11) . . C112 C Uani 0.6850(3) 0.3365(2) 0.1999(2) 1.000 0.0269(14) . . C113 C Uani 0.7735(2) 0.2416(2) 0.3078(2) 1.000 0.0257(12) . . C114 C Uani 0.6976(3) 0.3764(2) 0.3594(2) 1.000 0.0268(14) . . C115 C Uani 0.6706(2) 0.0750(2) 0.37035(18) 1.000 0.0167(12) . . C116 C Uani 0.8056(2) 0.0664(2) 0.4832(2) 1.000 0.0272(14) . . C117 C Uani 0.6942(2) 0.1870(2) 0.4956(2) 1.000 0.0210(14) . . C118 C Uani 0.6559(3) 0.0265(2) 0.5256(2) 1.000 0.0310(14) . . C119 C Uani 0.4950(2) 0.14065(19) 0.40346(18) 1.000 0.0182(12) . . C120 C Uani 0.5120(2) 0.2918(2) 0.4821(2) 1.000 0.0249(14) . . C121 C Uani 0.3821(2) 0.1980(2) 0.5037(2) 1.000 0.0272(14) . . C122 C Uani 0.3920(2) 0.2759(2) 0.3641(2) 1.000 0.0243(14) . . H11 H Uiso 0.6958(16) 0.0217(15) 0.1522(16) 1.000 0.014(8) . . H11' H Uiso 0.6767(17) -0.0108(18) 0.2292(16) 1.000 0.023(10) . . H11" H Uiso 0.7191(17) 0.0656(16) 0.2291(16) 1.000 0.018(9) . . H12 H Uiso 0.6694(16) 0.1646(15) 0.1741(14) 1.000 0.008(8) . . H12' H Uiso 0.5837(18) 0.1806(18) 0.1532(16) 1.000 0.029(10) . . H12" H Uiso 0.6289(16) 0.1282(16) 0.1004(17) 1.000 0.021(9) . . H14 H Uiso 0.4957(17) -0.0647(16) 0.2017(15) 1.000 0.016(8) . . H14' H Uiso 0.5823(16) -0.0586(15) 0.2399(15) 1.000 0.012(8) . . H15 H Uiso 0.4974(17) -0.1026(17) 0.3393(16) 1.000 0.023(9) . . H15' H Uiso 0.5074(16) -0.0324(15) 0.3918(16) 1.000 0.009(8) . . H15" H Uiso 0.580(2) -0.0607(18) 0.3530(18) 1.000 0.035(11) . . H16 H Uiso 0.4100(16) 0.0080(15) 0.3243(16) 1.000 0.009(9) . . H16' H Uiso 0.4069(16) -0.0236(16) 0.2499(16) 1.000 0.017(9) . . H17 H Uiso 0.3631(16) 0.0904(14) 0.2168(15) 1.000 0.009(8) . . H17' H Uiso 0.3975(15) 0.1228(15) 0.2890(16) 1.000 0.008(8) . . H18 H Uiso 0.3931(18) 0.1935(16) 0.1552(17) 1.000 0.022(9) . . H18' H Uiso 0.4739(19) 0.2218(17) 0.1578(17) 1.000 0.025(10) . . H18" H Uiso 0.4291(16) 0.2298(16) 0.2272(17) 1.000 0.016(9) . . H19 H Uiso 0.4906(16) 0.1106(16) 0.1131(16) 1.000 0.012(9) . . H19' H Uiso 0.4378(16) 0.0477(15) 0.1336(15) 1.000 0.013(8) . . H110 H Uiso 0.5738(18) 0.0212(18) 0.0595(18) 1.000 0.029(10) . . H110' H Uiso 0.518(2) -0.0335(18) 0.0776(18) 1.000 0.034(11) . . H110" H Uiso 0.5978(18) -0.0528(18) 0.1049(16) 1.000 0.028(10) . . H111 H Uiso 0.566(2) 0.268(2) 0.271(2) 1.000 0.048(12) . . H111' H Uiso 0.5906(19) 0.2522(18) 0.3468(19) 1.000 0.032(11) . . H112 H Uiso 0.6896(19) 0.299(2) 0.1680(19) 1.000 0.038(12) . . H112' H Uiso 0.723(2) 0.370(2) 0.196(2) 1.000 0.058(14) . . H112" H Uiso 0.644(2) 0.364(2) 0.186(2) 1.000 0.051(13) . . H113 H Uiso 0.784(2) 0.218(2) 0.356(2) 1.000 0.047(12) . . H113' H Uiso 0.815(2) 0.272(2) 0.3012(18) 1.000 0.039(12) . . H113" H Uiso 0.7733(18) 0.2084(18) 0.2723(18) 1.000 0.023(10) . . H114 H Uiso 0.656(2) 0.408(2) 0.3580(19) 1.000 0.042(12) . . H114' H Uiso 0.740(2) 0.405(2) 0.355(2) 1.000 0.049(13) . . H114" H Uiso 0.7055(17) 0.3570(17) 0.4070(18) 1.000 0.025(10) . . H115 H Uiso 0.6746(17) 0.0227(18) 0.3604(16) 1.000 0.025(9) . . H115' H Uiso 0.7029(19) 0.0960(18) 0.3465(18) 1.000 0.027(11) . . H116 H Uiso 0.816(2) 0.017(2) 0.4734(18) 1.000 0.045(12) . . H116' H Uiso 0.8219(19) 0.0749(18) 0.531(2) 1.000 0.037(11) . . H116" H Uiso 0.833(2) 0.097(2) 0.456(2) 1.000 0.063(16) . . H117 H Uiso 0.7125(19) 0.2215(19) 0.4648(19) 1.000 0.036(11) . . H117' H Uiso 0.7192(18) 0.1935(17) 0.5448(19) 1.000 0.032(10) . . H117" H Uiso 0.642(2) 0.1962(18) 0.4970(18) 1.000 0.036(11) . . H118 H Uiso 0.603(2) 0.036(2) 0.521(2) 1.000 0.056(14) . . H118' H Uiso 0.672(2) 0.0355(19) 0.578(2) 1.000 0.050(12) . . H118" H Uiso 0.666(2) -0.024(2) 0.5203(18) 1.000 0.043(12) . . H119 H Uiso 0.4608(18) 0.1009(17) 0.4045(16) 1.000 0.027(10) . . H119' H Uiso 0.5315(18) 0.1290(16) 0.4395(17) 1.000 0.019(9) . . H120 H Uiso 0.5370(16) 0.2717(16) 0.5280(17) 1.000 0.018(9) . . H120' H Uiso 0.485(2) 0.335(2) 0.4939(19) 1.000 0.045(12) . . H120" H Uiso 0.549(2) 0.3091(18) 0.4549(18) 1.000 0.032(11) . . H121 H Uiso 0.3439(19) 0.1682(18) 0.4859(17) 1.000 0.026(10) . . H121' H Uiso 0.3585(19) 0.2375(19) 0.5215(18) 1.000 0.032(11) . . H121" H Uiso 0.4083(19) 0.1731(18) 0.5410(19) 1.000 0.033(11) . . H122 H Uiso 0.4209(19) 0.3017(18) 0.3331(18) 1.000 0.027(10) . . H122' H Uiso 0.3633(17) 0.3089(17) 0.3836(16) 1.000 0.016(9) . . H122" H Uiso 0.3570(18) 0.2425(18) 0.3348(17) 1.000 0.028(10) . . Sc2 Sc Uani 0.09137(3) 0.14360(3) 0.20218(3) 1.000 0.0128(2) . . Si21 Si Uani -0.08889(5) 0.20152(5) 0.09287(5) 1.000 0.0204(3) . . Si22 Si Uani 0.16272(5) 0.33840(5) 0.18764(5) 1.000 0.0208(3) . . Si23 Si Uani 0.18384(6) 0.10156(5) 0.03536(5) 1.000 0.0237(3) . . N21 N Uani 0.01502(15) 0.13335(14) 0.30466(14) 1.000 0.0174(9) . . N22 N Uani 0.17295(15) 0.09715(14) 0.30485(14) 1.000 0.0167(9) . . N23 N Uani 0.07188(14) 0.00865(14) 0.23165(14) 1.000 0.0164(9) . . C21 C Uani 0.0075(3) 0.2019(2) 0.3478(2) 1.000 0.0303(14) . . C22 C Uani -0.0604(2) 0.1146(2) 0.2745(2) 1.000 0.0237(12) . . C23 C Uani 0.05044(18) 0.07037(18) 0.34878(17) 1.000 0.0182(11) . . C24 C Uani 0.13079(19) 0.0917(2) 0.36854(19) 1.000 0.0222(12) . . C25 C Uani 0.2376(2) 0.1454(2) 0.3235(2) 1.000 0.0253(12) . . C26 C Uani 0.2006(2) 0.0219(2) 0.2868(2) 1.000 0.0243(12) . . C27 C Uani 0.1472(2) -0.0213(2) 0.2345(2) 1.000 0.0237(14) . . C28 C Uani 0.0262(3) -0.0349(2) 0.1765(2) 1.000 0.0265(14) . . C29 C Uani 0.0442(2) -0.00031(19) 0.30307(18) 1.000 0.0197(11) . . C210 C Uani 0.0171(2) 0.0552(2) 0.4193(2) 1.000 0.0273(16) . . C211 C Uani -0.0021(2) 0.1524(2) 0.11478(19) 1.000 0.0215(12) . . C212 C Uani -0.1715(2) 0.1457(3) 0.1099(3) 1.000 0.0274(16) . . C213 C Uani -0.0937(3) 0.2912(2) 0.1442(3) 1.000 0.0349(16) . . C214 C Uani -0.1015(3) 0.2280(4) -0.0046(3) 1.000 0.054(2) . . C215 C Uani 0.1137(2) 0.26498(19) 0.2315(2) 1.000 0.0229(12) . . C216 C Uani 0.1656(3) 0.4280(2) 0.2401(3) 1.000 0.0395(18) . . C217 C Uani 0.1141(3) 0.3585(3) 0.0969(3) 1.000 0.0444(19) . . C218 C Uani 0.2611(2) 0.3186(3) 0.1774(3) 1.000 0.0363(17) . . C219 C Uani 0.1848(2) 0.1204(2) 0.1323(2) 1.000 0.0204(12) . . C220 C Uani 0.1579(3) 0.1864(3) -0.0206(3) 1.000 0.050(2) . . C221 C Uani 0.2752(3) 0.0719(3) 0.0092(3) 1.000 0.0385(17) . . C222 C Uani 0.1194(3) 0.0252(3) 0.0040(3) 1.000 0.044(2) . . H21 H Uiso -0.0071(19) 0.2417(19) 0.3167(18) 1.000 0.035(11) . . H21' H Uiso 0.0576(18) 0.2133(16) 0.3727(16) 1.000 0.017(9) . . H21" H Uiso -0.026(2) 0.1936(18) 0.3844(19) 1.000 0.036(12) . . H22 H Uiso -0.088(2) 0.0994(18) 0.3142(19) 1.000 0.038(11) . . H22' H Uiso -0.0600(15) 0.0727(16) 0.2370(16) 1.000 0.012(8) . . H22" H Uiso -0.0843(18) 0.1591(19) 0.2561(17) 1.000 0.033(10) . . H24 H Uiso 0.1349(16) 0.1420(17) 0.3909(16) 1.000 0.019(9) . . H24' H Uiso 0.1523(17) 0.0575(16) 0.4036(16) 1.000 0.020(9) . . H25 H Uiso 0.2234(16) 0.1913(16) 0.3387(15) 1.000 0.008(8) . . H25' H Uiso 0.2633(18) 0.1540(17) 0.2795(18) 1.000 0.024(10) . . H25" H Uiso 0.2742(18) 0.1204(16) 0.3620(17) 1.000 0.026(9) . . H26 H Uiso 0.2121(16) -0.0060(16) 0.3313(16) 1.000 0.014(8) . . H26' H Uiso 0.2449(19) 0.0302(18) 0.2648(17) 1.000 0.029(11) . . H27 H Uiso 0.1610(17) -0.0174(16) 0.1838(17) 1.000 0.018(9) . . H27' H Uiso 0.1471(19) -0.073(2) 0.2467(18) 1.000 0.044(11) . . H28 H Uiso 0.0254(18) -0.086(2) 0.1934(18) 1.000 0.037(11) . . H28' H Uiso 0.0498(17) -0.0296(16) 0.1283(18) 1.000 0.022(9) . . H28" H Uiso -0.0230(19) -0.0168(17) 0.1718(17) 1.000 0.025(10) . . H29 H Uiso 0.0715(16) -0.0407(16) 0.3305(15) 1.000 0.014(8) . . H29' H Uiso -0.0094(16) -0.0161(14) 0.2944(14) 1.000 0.008(8) . . H210 H Uiso 0.0244(18) 0.0980(18) 0.4539(18) 1.000 0.032(10) . . H210' H Uiso 0.038(2) 0.009(2) 0.4417(19) 1.000 0.052(12) . . H210" H Uiso -0.0344(19) 0.0480(16) 0.4101(16) 1.000 0.022(10) . . H211 H Uiso 0.031(2) 0.175(2) 0.086(2) 1.000 0.051(13) . . H211' H Uiso -0.0084(19) 0.104(2) 0.0952(18) 1.000 0.040(11) . . H212 H Uiso -0.176(2) 0.104(2) 0.087(2) 1.000 0.070(16) . . H212' H Uiso -0.216(2) 0.169(2) 0.093(2) 1.000 0.052(13) . . H212" H Uiso -0.172(2) 0.132(2) 0.158(2) 1.000 0.061(14) . . H213 H Uiso -0.089(2) 0.288(2) 0.198(2) 1.000 0.059(14) . . H213' H Uiso -0.135(2) 0.3155(19) 0.1325(19) 1.000 0.036(12) . . H213" H Uiso -0.050(2) 0.324(2) 0.1325(19) 1.000 0.048(12) . . H214 H Uiso -0.063(3) 0.260(2) -0.013(2) 1.000 0.075(19) . . H214' H Uiso -0.143(2) 0.255(2) -0.015(2) 1.000 0.064(15) . . H214" H Uiso -0.097(2) 0.182(2) -0.036(2) 1.000 0.054(14) . . H215 H Uiso 0.067(2) 0.2790(19) 0.2259(19) 1.000 0.042(12) . . H215' H Uiso 0.1294(19) 0.2672(18) 0.2813(19) 1.000 0.037(11) . . H216 H Uiso 0.121(2) 0.442(2) 0.253(2) 1.000 0.060(15) . . H216' H Uiso 0.184(2) 0.471(2) 0.211(2) 1.000 0.071(15) . . H216" H Uiso 0.198(2) 0.418(2) 0.290(2) 1.000 0.071(15) . . H217 H Uiso 0.114(2) 0.316(2) 0.066(2) 1.000 0.054(14) . . H217' H Uiso 0.145(2) 0.398(2) 0.076(2) 1.000 0.065(14) . . H217" H Uiso 0.060(3) 0.381(3) 0.096(3) 1.000 0.098(19) . . H218 H Uiso 0.286(2) 0.308(2) 0.222(2) 1.000 0.051(14) . . H218' H Uiso 0.284(2) 0.361(2) 0.159(2) 1.000 0.050(12) . . H218" H Uiso 0.269(2) 0.276(2) 0.149(2) 1.000 0.054(14) . . H219 H Uiso 0.2051(19) 0.1604(19) 0.1411(18) 1.000 0.031(11) . . H219' H Uiso 0.217(2) 0.086(2) 0.1552(19) 1.000 0.044(12) . . H220 H Uiso 0.107(2) 0.2014(18) -0.0146(17) 1.000 0.029(10) . . H220' H Uiso 0.154(3) 0.174(2) -0.069(3) 1.000 0.077(18) . . H220" H Uiso 0.196(3) 0.225(3) -0.011(2) 1.000 0.085(19) . . H221 H Uiso 0.311(2) 0.110(2) 0.023(2) 1.000 0.049(13) . . H221' H Uiso 0.280(2) 0.066(2) -0.036(2) 1.000 0.055(15) . . H221" H Uiso 0.289(2) 0.026(2) 0.033(2) 1.000 0.061(14) . . H222 H Uiso 0.125(2) -0.020(3) 0.031(2) 1.000 0.077(18) . . H222' H Uiso 0.119(2) 0.0181(19) -0.047(2) 1.000 0.046(12) . . H222" H Uiso 0.073(2) 0.039(2) 0.006(2) 1.000 0.060(16) . . 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 Sc1 0.0119(4) 0.0139(3) 0.0104(3) -0.0004(3) 0.0005(3) -0.0007(3) Si11 0.0170(6) 0.0162(5) 0.0167(5) 0.0007(4) 0.0030(4) -0.0017(4) Si12 0.0187(6) 0.0177(5) 0.0147(5) 0.0016(4) -0.0025(4) -0.0003(4) Si13 0.0189(6) 0.0191(5) 0.0143(5) -0.0031(4) 0.0038(4) -0.0015(4) N11 0.0122(17) 0.0177(15) 0.0149(15) 0.0017(12) -0.0016(13) 0.0030(12) N12 0.0189(18) 0.0193(15) 0.0120(15) -0.0010(12) 0.0047(13) -0.0027(13) N13 0.0124(17) 0.0178(14) 0.0153(15) 0.0011(12) 0.0014(13) 0.0033(12) C11 0.017(2) 0.026(2) 0.018(2) -0.0015(18) 0.0019(18) 0.0061(17) C12 0.019(2) 0.0190(19) 0.015(2) 0.0012(16) 0.0016(17) -0.0005(17) C13 0.014(2) 0.0206(18) 0.0107(18) -0.0043(14) -0.0008(15) 0.0008(15) C14 0.017(2) 0.0202(19) 0.021(2) -0.0045(16) 0.0014(17) -0.0048(16) C15 0.034(3) 0.0158(19) 0.023(2) 0.0044(17) 0.009(2) -0.0043(18) C16 0.017(2) 0.030(2) 0.024(2) -0.0040(18) 0.0020(19) -0.0079(17) C17 0.010(2) 0.031(2) 0.022(2) -0.0053(18) -0.0047(17) -0.0002(16) C18 0.020(2) 0.028(2) 0.023(2) 0.0008(19) 0.004(2) 0.0102(19) C19 0.014(2) 0.025(2) 0.015(2) -0.0004(16) -0.0011(16) -0.0025(16) C110 0.024(3) 0.029(2) 0.016(2) -0.0085(18) 0.0009(19) -0.0009(19) C111 0.020(2) 0.0197(19) 0.016(2) -0.0007(16) 0.0058(18) 0.0019(16) C112 0.032(3) 0.023(2) 0.026(2) 0.0002(19) 0.004(2) -0.001(2) C113 0.021(2) 0.035(2) 0.021(2) -0.001(2) 0.0018(19) -0.0007(19) C114 0.030(3) 0.025(2) 0.026(2) -0.0054(18) 0.006(2) -0.011(2) C115 0.016(2) 0.019(2) 0.015(2) 0.0013(15) 0.0006(17) -0.0014(16) C116 0.024(3) 0.030(2) 0.025(2) -0.006(2) -0.010(2) 0.0070(19) C117 0.024(3) 0.023(2) 0.016(2) -0.0010(17) 0.0024(19) -0.0016(18) C118 0.040(3) 0.028(2) 0.024(2) 0.0068(18) -0.002(2) -0.007(2) C119 0.015(2) 0.023(2) 0.016(2) -0.0024(16) -0.0006(17) -0.0035(16) C120 0.027(3) 0.027(2) 0.021(2) -0.0093(18) 0.004(2) -0.0020(19) C121 0.027(3) 0.027(2) 0.028(2) -0.0010(19) 0.005(2) 0.004(2) C122 0.032(3) 0.016(2) 0.026(2) -0.0047(18) 0.008(2) -0.0007(19) Sc2 0.0114(4) 0.0136(3) 0.0133(3) 0.0006(3) 0.0015(3) 0.0016(3) Si21 0.0130(6) 0.0269(5) 0.0211(6) 0.0071(4) 0.0008(4) 0.0031(4) Si22 0.0163(6) 0.0148(5) 0.0307(6) 0.0025(4) 0.0002(5) -0.0002(4) Si23 0.0218(6) 0.0302(6) 0.0200(6) 0.0000(4) 0.0069(5) 0.0042(5) N21 0.0167(17) 0.0197(15) 0.0159(16) -0.0012(12) 0.0023(13) 0.0021(12) N22 0.0157(17) 0.0205(15) 0.0135(15) 0.0000(12) -0.0005(13) 0.0005(12) N23 0.0113(16) 0.0196(15) 0.0187(16) -0.0005(12) 0.0036(13) -0.0002(12) C21 0.038(3) 0.032(2) 0.022(2) -0.0032(19) 0.009(2) 0.007(2) C22 0.018(2) 0.030(2) 0.024(2) 0.0058(19) 0.0069(19) 0.0032(18) C23 0.020(2) 0.0255(19) 0.0090(18) 0.0042(14) 0.0006(16) 0.0016(16) C24 0.018(2) 0.034(2) 0.014(2) 0.0032(18) -0.0010(17) 0.0016(18) C25 0.016(2) 0.037(2) 0.022(2) -0.001(2) -0.0027(19) -0.0031(19) C26 0.017(2) 0.031(2) 0.025(2) 0.0087(18) 0.0027(19) 0.0089(18) C27 0.021(2) 0.016(2) 0.035(3) 0.0039(17) 0.008(2) 0.0032(16) C28 0.034(3) 0.019(2) 0.027(2) -0.0017(17) 0.005(2) -0.0066(19) C29 0.018(2) 0.0218(19) 0.019(2) 0.0063(16) 0.0002(17) 0.0030(16) C210 0.023(3) 0.040(3) 0.019(2) 0.0051(19) 0.0024(19) 0.002(2) C211 0.018(2) 0.026(2) 0.020(2) 0.0000(17) -0.0002(18) 0.0027(17) C212 0.020(3) 0.035(2) 0.028(3) 0.000(2) 0.006(2) -0.002(2) C213 0.018(3) 0.027(2) 0.059(3) 0.004(2) 0.001(2) 0.006(2) C214 0.038(4) 0.088(4) 0.036(3) 0.025(3) 0.003(3) 0.026(3) C215 0.017(2) 0.025(2) 0.027(2) 0.0000(17) 0.0034(19) 0.0042(17) C216 0.017(3) 0.021(2) 0.080(4) -0.007(2) 0.003(3) -0.0006(19) C217 0.052(4) 0.035(3) 0.043(3) 0.016(2) -0.011(3) -0.018(3) C218 0.025(3) 0.029(3) 0.056(3) 0.006(2) 0.010(2) -0.004(2) C219 0.019(2) 0.020(2) 0.023(2) 0.0000(17) 0.0063(17) -0.0002(17) C220 0.041(4) 0.068(4) 0.042(3) 0.024(3) 0.010(3) 0.016(3) C221 0.040(3) 0.048(3) 0.031(3) 0.000(2) 0.021(2) 0.011(2) C222 0.041(4) 0.060(4) 0.031(3) -0.023(3) 0.003(3) -0.003(3) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's 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 Sc1 N11 2.504(3) . . yes Sc1 N12 2.465(3) . . yes Sc1 N13 2.521(3) . . yes Sc1 C111 2.267(3) . . yes Sc1 C115 2.256(4) . . yes Sc1 C119 2.309(4) . . yes Sc2 C215 2.279(3) . . yes Sc2 C219 2.301(4) . . yes Sc2 N23 2.523(3) . . yes Sc2 N21 2.495(3) . . yes Sc2 N22 2.461(3) . . yes Sc2 C211 2.256(4) . . yes Si11 C113 1.886(4) . . yes Si11 C111 1.842(4) . . yes Si11 C112 1.881(4) . . yes Si11 C114 1.889(4) . . yes Si12 C115 1.841(4) . . yes Si12 C116 1.888(4) . . yes Si12 C118 1.883(4) . . yes Si12 C117 1.877(4) . . yes Si13 C121 1.878(4) . . yes Si13 C120 1.879(4) . . yes Si13 C119 1.844(4) . . yes Si13 C122 1.874(4) . . yes Si21 C211 1.836(4) . . yes Si21 C214 1.875(6) . . yes Si21 C213 1.884(4) . . yes Si21 C212 1.877(4) . . yes Si22 C216 1.885(4) . . yes Si22 C215 1.839(4) . . yes Si22 C217 1.872(6) . . yes Si22 C218 1.875(4) . . yes Si23 C219 1.842(4) . . yes Si23 C221 1.877(6) . . yes Si23 C222 1.871(6) . . yes Si23 C220 1.884(6) . . yes N11 C13 1.511(4) . . yes N11 C11 1.488(4) . . yes N11 C12 1.494(4) . . yes N12 C14 1.496(4) . . yes N12 C15 1.492(4) . . yes N12 C16 1.493(5) . . yes N13 C18 1.492(4) . . yes N13 C19 1.487(4) . . yes N13 C17 1.473(5) . . yes N21 C23 1.510(4) . . yes N21 C22 1.484(5) . . yes N21 C21 1.488(4) . . yes N22 C24 1.489(4) . . yes N22 C25 1.486(5) . . yes N22 C26 1.497(4) . . yes N23 C27 1.484(5) . . yes N23 C28 1.486(5) . . yes N23 C29 1.485(4) . . yes C13 C14 1.537(5) . . no C13 C110 1.524(5) . . no C13 C19 1.528(5) . . no C16 C17 1.520(5) . . no C11 H11" 1.00(3) . . no C11 H11 1.03(3) . . no C11 H11' 0.94(3) . . no C12 H12' 1.02(3) . . no C12 H12 0.99(3) . . no C12 H12" 1.01(3) . . no C14 H14 0.98(3) . . no C14 H14' 1.05(3) . . no C15 H15" 1.02(4) . . no C15 H15 1.04(3) . . no C15 H15' 0.96(3) . . no C16 H16 0.94(3) . . no C16 H16' 0.94(3) . . no C17 H17' 0.98(3) . . no C17 H17 0.96(3) . . no C18 H18" 0.98(3) . . no C18 H18 0.96(3) . . no C18 H18' 0.97(3) . . no C19 H19 0.93(3) . . no C19 H19' 1.00(3) . . no C110 H110 0.96(3) . . no C110 H110' 0.92(4) . . no C110 H110" 1.00(3) . . no C111 H111 0.94(4) . . no C111 H111' 0.89(4) . . no C112 H112 0.91(4) . . no C112 H112' 0.93(4) . . no C112 H112" 0.92(4) . . no C113 H113' 0.96(4) . . no C113 H113" 0.89(3) . . no C113 H113 1.00(4) . . no C114 H114' 0.95(4) . . no C114 H114" 0.95(3) . . no C114 H114 0.95(4) . . no C115 H115 0.96(3) . . no C115 H115' 0.87(3) . . no C116 H116" 0.93(4) . . no C116 H116 0.93(4) . . no C116 H116' 0.93(4) . . no C117 H117' 0.99(4) . . no C117 H117" 0.98(4) . . no C117 H117 0.93(4) . . no C118 H118" 0.94(4) . . no C118 H118' 1.01(4) . . no C118 H118 0.98(4) . . no C119 H119' 0.93(3) . . no C119 H119 0.95(3) . . no C120 H120 1.00(3) . . no C120 H120' 0.96(4) . . no C120 H120" 0.94(4) . . no C121 H121 0.92(3) . . no C121 H121" 0.92(4) . . no C121 H121' 0.91(3) . . no C122 H122" 1.00(3) . . no C122 H122 0.95(3) . . no C122 H122' 0.90(3) . . no C23 C24 1.537(5) . . no C23 C29 1.530(5) . . no C23 C210 1.534(5) . . no C26 C27 1.527(5) . . no C21 H21 0.94(3) . . no C21 H21' 1.01(3) . . no C21 H21" 0.98(4) . . no C22 H22 0.98(4) . . no C22 H22' 1.03(3) . . no C22 H22" 0.96(3) . . no C24 H24 1.00(3) . . no C24 H24' 0.96(3) . . no C25 H25 0.92(3) . . no C25 H25' 1.00(3) . . no C25 H25" 1.04(3) . . no C26 H26 0.98(3) . . no C26 H26' 0.96(3) . . no C27 H27 1.01(3) . . no C27 H27' 0.96(4) . . no C28 H28 0.97(4) . . no C28 H28' 1.04(3) . . no C28 H28" 0.96(4) . . no C29 H29 1.00(3) . . no C29 H29' 1.02(3) . . no C210 H210' 0.99(4) . . no C210 H210" 0.96(3) . . no C210 H210 1.01(3) . . no C211 H211' 0.95(4) . . no C211 H211 0.95(4) . . no C212 H212' 0.95(4) . . no C212 H212" 0.93(4) . . no C212 H212 0.86(4) . . no C213 H213' 0.89(4) . . no C213 H213" 1.04(4) . . no C213 H213 1.00(4) . . no C214 H214' 0.91(4) . . no C214 H214" 1.02(4) . . no C214 H214 0.94(5) . . no C215 H215' 0.95(4) . . no C215 H215 0.89(4) . . no C216 H216' 1.02(4) . . no C216 H216" 1.07(4) . . no C216 H216 0.92(4) . . no C217 H217' 1.01(4) . . no C217 H217" 1.07(6) . . no C217 H217 0.96(4) . . no C218 H218' 0.95(4) . . no C218 H218" 0.95(4) . . no C218 H218 0.93(4) . . no C219 H219' 0.93(4) . . no C219 H219 0.82(4) . . no C220 H220' 0.93(5) . . no C220 H220" 0.99(6) . . no C220 H220 0.99(4) . . no C221 H221' 0.87(4) . . no C221 H221" 0.96(4) . . no C221 H221 0.97(4) . . no C222 H222' 0.96(4) . . no C222 H222" 0.89(4) . . no C222 H222 0.96(5) . . 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 N11 Sc1 N12 73.91(8) . . . yes N11 Sc1 N13 69.63(8) . . . yes N11 Sc1 C111 98.85(11) . . . yes N11 Sc1 C115 87.87(11) . . . yes N11 Sc1 C119 159.47(11) . . . yes N12 Sc1 N13 66.45(8) . . . yes N12 Sc1 C111 163.19(11) . . . yes N12 Sc1 C115 94.10(11) . . . yes N12 Sc1 C119 87.48(11) . . . yes N13 Sc1 C111 96.88(11) . . . yes N13 Sc1 C115 153.24(11) . . . yes N13 Sc1 C119 95.28(11) . . . yes C111 Sc1 C115 100.87(13) . . . yes C111 Sc1 C119 96.68(13) . . . yes C115 Sc1 C119 102.31(13) . . . yes N22 Sc2 N23 65.93(9) . . . yes N22 Sc2 C211 161.75(11) . . . yes N22 Sc2 C215 93.25(11) . . . yes N22 Sc2 C219 87.05(11) . . . yes N23 Sc2 C211 96.35(11) . . . yes N23 Sc2 C215 153.61(11) . . . yes N23 Sc2 C219 94.62(11) . . . yes C211 Sc2 C215 102.29(13) . . . yes C211 Sc2 C219 99.28(13) . . . yes C215 Sc2 C219 100.56(13) . . . yes N21 Sc2 N22 73.93(9) . . . yes N21 Sc2 N23 69.98(8) . . . yes N21 Sc2 C211 96.50(11) . . . yes N21 Sc2 C215 89.32(11) . . . yes N21 Sc2 C219 159.09(11) . . . yes C111 Si11 C112 110.4(2) . . . yes C111 Si11 C113 115.34(16) . . . yes C111 Si11 C114 111.6(2) . . . yes C112 Si11 C113 105.4(2) . . . yes C112 Si11 C114 108.16(16) . . . yes C113 Si11 C114 105.6(2) . . . yes C115 Si12 C116 112.35(17) . . . yes C115 Si12 C117 112.22(17) . . . yes C115 Si12 C118 110.98(18) . . . yes C116 Si12 C117 106.21(16) . . . yes C116 Si12 C118 107.0(2) . . . yes C117 Si12 C118 107.79(17) . . . yes C120 Si13 C122 104.86(16) . . . yes C119 Si13 C120 112.30(17) . . . yes C119 Si13 C121 113.51(16) . . . yes C119 Si13 C122 114.54(16) . . . yes C120 Si13 C121 105.38(17) . . . yes C121 Si13 C122 105.40(17) . . . yes C211 Si21 C212 114.02(19) . . . yes C211 Si21 C213 112.5(2) . . . yes C211 Si21 C214 111.0(2) . . . yes C212 Si21 C213 106.9(2) . . . yes C212 Si21 C214 106.1(3) . . . yes C213 Si21 C214 105.7(3) . . . yes C215 Si22 C216 111.8(2) . . . yes C215 Si22 C217 109.4(2) . . . yes C216 Si22 C217 107.0(2) . . . yes C216 Si22 C218 103.8(2) . . . yes C217 Si22 C218 108.8(2) . . . yes C215 Si22 C218 115.6(2) . . . yes C219 Si23 C220 112.0(2) . . . yes C219 Si23 C222 112.7(2) . . . yes C220 Si23 C221 105.6(2) . . . yes C219 Si23 C221 112.9(2) . . . yes C220 Si23 C222 107.7(2) . . . yes C221 Si23 C222 105.5(2) . . . yes Sc1 N11 C11 117.55(19) . . . yes C11 N11 C12 104.8(3) . . . yes C11 N11 C13 111.7(2) . . . yes C12 N11 C13 112.6(2) . . . yes Sc1 N11 C13 103.42(17) . . . yes Sc1 N11 C12 106.86(18) . . . yes Sc1 N12 C15 114.1(2) . . . yes Sc1 N12 C14 108.42(19) . . . yes C14 N12 C16 109.2(3) . . . yes C15 N12 C16 108.4(3) . . . yes Sc1 N12 C16 108.07(19) . . . yes C14 N12 C15 108.5(3) . . . yes Sc1 N13 C17 100.20(19) . . . yes C17 N13 C18 107.4(3) . . . yes Sc1 N13 C18 117.7(2) . . . yes Sc1 N13 C19 112.03(19) . . . yes C18 N13 C19 109.6(3) . . . yes C17 N13 C19 109.3(3) . . . yes Sc2 N21 C22 107.7(2) . . . yes Sc2 N21 C21 116.5(2) . . . yes C21 N21 C23 112.6(3) . . . yes Sc2 N21 C23 103.23(18) . . . yes C21 N21 C22 105.0(3) . . . yes C22 N21 C23 111.9(2) . . . yes Sc2 N22 C26 109.03(19) . . . yes C24 N22 C25 108.7(3) . . . yes C25 N22 C26 107.4(3) . . . yes Sc2 N22 C25 113.3(2) . . . yes C24 N22 C26 109.7(3) . . . yes Sc2 N22 C24 108.6(2) . . . yes Sc2 N23 C27 101.78(19) . . . yes C27 N23 C28 107.2(3) . . . yes C27 N23 C29 109.4(3) . . . yes C28 N23 C29 110.2(3) . . . yes Sc2 N23 C29 111.72(19) . . . yes Sc2 N23 C28 116.0(2) . . . yes C14 C13 C110 108.3(3) . . . no C14 C13 C19 110.5(3) . . . no N11 C13 C14 107.1(2) . . . yes N11 C13 C19 108.3(2) . . . yes N11 C13 C110 114.2(3) . . . yes C19 C13 C110 108.4(3) . . . no N12 C14 C13 113.6(3) . . . yes N12 C16 C17 113.3(3) . . . yes N13 C17 C16 113.0(3) . . . yes N13 C19 C13 113.8(3) . . . yes N11 C11 H11" 107.5(17) . . . no Sc1 C111 Si11 137.66(19) . . . yes H11' C11 H11" 109(3) . . . no N11 C11 H11' 110.2(19) . . . no H11 C11 H11' 111(2) . . . no H11 C11 H11" 109(2) . . . no N11 C11 H11 110.6(16) . . . no N11 C12 H12 105.9(15) . . . no H12 C12 H12" 110(2) . . . no H12 C12 H12' 107(2) . . . no N11 C12 H12' 112.4(18) . . . no H12' C12 H12" 109(2) . . . no N11 C12 H12" 113.1(17) . . . no C13 C14 H14 108.5(17) . . . no C13 C14 H14' 110.0(15) . . . no N12 C14 H14 108.5(18) . . . no N12 C14 H14' 104.7(15) . . . no H14 C14 H14' 112(2) . . . no H15' C15 H15" 115(3) . . . no N12 C15 H15" 105.2(19) . . . no Sc1 C115 Si12 127.42(18) . . . yes H15 C15 H15" 111(3) . . . no N12 C15 H15' 108.0(17) . . . no H15 C15 H15' 106(2) . . . no N12 C15 H15 111.9(17) . . . no H16 C16 H16' 106(3) . . . no C17 C16 H16 109.7(17) . . . no C17 C16 H16' 111.0(18) . . . no N12 C16 H16 107.9(18) . . . no N12 C16 H16' 108.8(19) . . . no C16 C17 H17 113.6(15) . . . no H17 C17 H17' 106(2) . . . no N13 C17 H17 108.2(17) . . . no N13 C17 H17' 107.5(16) . . . no C16 C17 H17' 108.3(17) . . . no H18 C18 H18" 110(3) . . . no N13 C18 H18' 108.5(19) . . . no N13 C18 H18 110.0(18) . . . no H18' C18 H18" 112(3) . . . no N13 C18 H18" 108.0(18) . . . no H18 C18 H18' 109(3) . . . no Sc1 C119 Si13 133.35(18) . . . yes C13 C19 H19' 109.4(17) . . . no C13 C19 H19 107.6(18) . . . no H19 C19 H19' 108(2) . . . no N13 C19 H19 107.1(18) . . . no N13 C19 H19' 110.4(17) . . . no C13 C110 H110 113(2) . . . no H110' C110 H110" 107(3) . . . no H110' C110 H110 104(3) . . . no C13 C110 H110" 112.8(17) . . . no C13 C110 H110' 109(2) . . . no H110" C110 H110 111(3) . . . no H111' C111 H111 107(3) . . . no Sc1 C111 H111 108(2) . . . no Sc1 C111 H111' 89(2) . . . no Si11 C111 H111' 106(2) . . . no Si11 C111 H111 105(2) . . . no Si11 C112 H112' 112(2) . . . no H112' C112 H112 108(3) . . . no H112" C112 H112 110(3) . . . no Si11 C112 H112" 114(2) . . . no Si11 C112 H112 110(2) . . . no H112' C112 H112" 103(3) . . . no Si11 C113 H113' 111(2) . . . no Si11 C113 H113" 108(2) . . . no Si11 C113 H113 116(2) . . . no H113" C113 H113 112(3) . . . no H113' C113 H113" 103(3) . . . no H113' C113 H113 106(3) . . . no Si11 C114 H114' 113(2) . . . no Si11 C114 H114" 109.3(19) . . . no Si11 C114 H114 114(2) . . . no H114' C114 H114" 103(3) . . . no H114" C114 H114 107(3) . . . no H114' C114 H114 110(3) . . . no Si12 C115 H115 106.8(18) . . . no Si12 C115 H115' 105(2) . . . no Sc1 C115 H115' 99(2) . . . no H115' C115 H115 105(3) . . . no Sc1 C115 H115 111.2(18) . . . no Si12 C116 H116' 111(2) . . . no Si12 C116 H116" 111(2) . . . no Si12 C116 H116 113(2) . . . no H116' C116 H116" 107(3) . . . no H116' C116 H116 107(3) . . . no H116" C116 H116 109(3) . . . no Si12 C117 H117" 107.7(19) . . . no Si12 C117 H117 113(2) . . . no Si12 C117 H117' 109.7(18) . . . no H117" C117 H117 109(3) . . . no H117' C117 H117" 109(3) . . . no H117' C117 H117 109(3) . . . no Si12 C118 H118" 114(2) . . . no H118' C118 H118 104(3) . . . no Si12 C118 H118 112(2) . . . no H118' C118 H118" 103(3) . . . no Si12 C118 H118' 112(2) . . . no H118" C118 H118 111(3) . . . no Si13 C119 H119' 105.9(19) . . . no H119' C119 H119 104(3) . . . no Sc1 C119 H119 110.7(19) . . . no Si13 C119 H119 105(2) . . . no Sc1 C119 H119' 94(2) . . . no Si13 C120 H120' 109(2) . . . no H120" C120 H120 107(3) . . . no H120' C120 H120 108(3) . . . no Si13 C120 H120" 116(2) . . . no Si13 C120 H120 111.5(17) . . . no H120' C120 H120" 106(3) . . . no Si13 C121 H121 114(2) . . . no H121' C121 H121" 110(3) . . . no H121' C121 H121 102(3) . . . no Si13 C121 H121" 107(2) . . . no Si13 C121 H121' 115(2) . . . no H121" C121 H121 108(3) . . . no H122' C122 H122 108(3) . . . no H122" C122 H122 109(3) . . . no Si13 C122 H122' 110.5(19) . . . no Si13 C122 H122" 110.8(19) . . . no Si13 C122 H122 113(2) . . . no H122' C122 H122" 104(3) . . . no N21 C23 C24 107.2(3) . . . yes N21 C23 C29 108.3(3) . . . yes N21 C23 C210 114.5(3) . . . yes C24 C23 C29 111.0(3) . . . no C24 C23 C210 107.3(3) . . . no C29 C23 C210 108.6(3) . . . no N22 C24 C23 113.0(3) . . . yes N22 C26 C27 113.1(3) . . . yes N23 C27 C26 112.2(3) . . . yes N23 C29 C23 113.5(3) . . . yes H21 C21 H21" 113(3) . . . no H21' C21 H21" 109(3) . . . no N21 C21 H21" 110.7(19) . . . no N21 C21 H21 109(2) . . . no N21 C21 H21' 106.7(17) . . . no H21 C21 H21' 109(3) . . . no N21 C22 H22 108(2) . . . no H22' C22 H22" 114(3) . . . no N21 C22 H22" 109(2) . . . no H22 C22 H22' 111(3) . . . no N21 C22 H22' 110.7(16) . . . no H22 C22 H22" 105(3) . . . no N22 C24 H24' 112.2(18) . . . no C23 C24 H24 111.0(17) . . . no N22 C24 H24 104.6(17) . . . no C23 C24 H24' 109.1(19) . . . no H24 C24 H24' 107(2) . . . no H25 C25 H25" 111(2) . . . no N22 C25 H25" 111.0(17) . . . no H25 C25 H25' 107(3) . . . no N22 C25 H25 110.5(19) . . . no N22 C25 H25' 109.4(19) . . . no H25' C25 H25" 108(3) . . . no N22 C26 H26 108.8(17) . . . no N22 C26 H26' 106.2(19) . . . no H26 C26 H26' 109(3) . . . no C27 C26 H26' 108.9(19) . . . no C27 C26 H26 110.7(17) . . . no C26 C27 H27 111.1(18) . . . no N23 C27 H27' 110(2) . . . no N23 C27 H27 105.3(18) . . . no C26 C27 H27' 111(2) . . . no H27 C27 H27' 107(3) . . . no H28 C28 H28" 108(3) . . . no N23 C28 H28" 110.4(19) . . . no H28 C28 H28' 113(3) . . . no N23 C28 H28 107(2) . . . no N23 C28 H28' 107.1(18) . . . no H28' C28 H28" 111(3) . . . no N23 C29 H29 109.9(17) . . . no N23 C29 H29' 107.5(15) . . . no H29 C29 H29' 108(2) . . . no C23 C29 H29' 109.6(15) . . . no C23 C29 H29 108.3(17) . . . no Sc2 C211 Si21 141.14(19) . . . yes Sc2 C215 Si22 131.75(19) . . . yes Sc2 C219 Si23 131.18(19) . . . yes C23 C210 H210' 110(2) . . . no C23 C210 H210" 110.2(18) . . . no C23 C210 H210 112.2(19) . . . no H210' C210 H210" 107(3) . . . no H210' C210 H210 111(3) . . . no H210" C210 H210 107(3) . . . no Sc2 C211 H211' 106(2) . . . no Sc2 C211 H211 87(2) . . . no Si21 C211 H211' 107(2) . . . no Si21 C211 H211 105(2) . . . no H211' C211 H211 104(3) . . . no Si21 C212 H212' 113(2) . . . no Si21 C212 H212" 113(2) . . . no Si21 C212 H212 115(2) . . . no H212' C212 H212" 110(3) . . . no H212' C212 H212 101(3) . . . no H212" C212 H212 104(3) . . . no Si21 C213 H213' 112(2) . . . no Si21 C213 H213" 108(2) . . . no Si21 C213 H213 117(2) . . . no H213' C213 H213" 109(3) . . . no H213' C213 H213 105(3) . . . no H213" C213 H213 105(3) . . . no Si21 C214 H214' 111(2) . . . no Si21 C214 H214" 110(2) . . . no Si21 C214 H214 107(2) . . . no H214' C214 H214" 115(3) . . . no H214' C214 H214 106(4) . . . no H214" C214 H214 107(3) . . . no Sc2 C215 H215' 108(2) . . . no Sc2 C215 H215 95(2) . . . no Si22 C215 H215' 107(2) . . . no Si22 C215 H215 105(2) . . . no H215' C215 H215 107(3) . . . no Si22 C216 H216' 111(2) . . . no Si22 C216 H216" 107(2) . . . no Si22 C216 H216 113(2) . . . no H216' C216 H216" 114(3) . . . no H216' C216 H216 107(3) . . . no H216" C216 H216 105(3) . . . no Si22 C217 H217' 104(2) . . . no Si22 C217 H217" 116(3) . . . no Si22 C217 H217 111(2) . . . no H217' C217 H217" 107(4) . . . no H217' C217 H217 107(3) . . . no H217" C217 H217 110(4) . . . no Si22 C218 H218' 111(2) . . . no Si22 C218 H218" 114(2) . . . no Si22 C218 H218 110(2) . . . no H218' C218 H218" 110(3) . . . no H218' C218 H218 107(3) . . . no H218" C218 H218 104(3) . . . no Sc2 C219 H219' 110(2) . . . no Sc2 C219 H219 95(2) . . . no Si23 C219 H219' 106(2) . . . no Si23 C219 H219 109(2) . . . no H219' C219 H219 104(3) . . . no Si23 C220 H220' 110(2) . . . no Si23 C220 H220" 109(3) . . . no Si23 C220 H220 110.3(19) . . . no H220' C220 H220" 109(4) . . . no H220' C220 H220 101(4) . . . no H220" C220 H220 117(4) . . . no Si23 C221 H221' 118(2) . . . no Si23 C221 H221" 109(2) . . . no Si23 C221 H221 110(2) . . . no H221' C221 H221" 107(3) . . . no H221' C221 H221 102(3) . . . no H221" C221 H221 110(3) . . . no Si23 C222 H222' 111(2) . . . no Si23 C222 H222" 111(2) . . . no Si23 C222 H222 115(2) . . . no H222' C222 H222" 100(3) . . . no H222' C222 H222 114(3) . . . no H222" C222 H222 105(3) . . . 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 N12 Sc1 N11 C11 -93.9(2) . . . . no N12 Sc1 N11 C12 148.8(2) . . . . no N12 Sc1 N11 C13 29.77(16) . . . . no N13 Sc1 N11 C11 -164.2(2) . . . . no N13 Sc1 N11 C12 78.5(2) . . . . no N13 Sc1 N11 C13 -40.57(16) . . . . no C111 Sc1 N11 C11 101.7(2) . . . . no C111 Sc1 N11 C12 -15.6(2) . . . . no C111 Sc1 N11 C13 -134.68(18) . . . . no C115 Sc1 N11 C11 1.0(2) . . . . no C115 Sc1 N11 C12 -116.3(2) . . . . no C115 Sc1 N11 C13 124.65(19) . . . . no C119 Sc1 N11 C11 -119.6(3) . . . . no C119 Sc1 N11 C12 123.1(3) . . . . no C119 Sc1 N11 C13 4.0(4) . . . . no N11 Sc1 N12 C14 1.10(19) . . . . no N11 Sc1 N12 C15 122.2(3) . . . . no N11 Sc1 N12 C16 -117.2(2) . . . . no N13 Sc1 N12 C14 75.5(2) . . . . no N13 Sc1 N12 C15 -163.5(3) . . . . no N13 Sc1 N12 C16 -42.82(19) . . . . no C115 Sc1 N12 C14 -85.5(2) . . . . no C115 Sc1 N12 C15 35.6(3) . . . . no C115 Sc1 N12 C16 156.2(2) . . . . no C119 Sc1 N12 C14 172.3(2) . . . . no C119 Sc1 N12 C15 -66.6(3) . . . . no C119 Sc1 N12 C16 54.0(2) . . . . no N11 Sc1 N13 C17 132.0(2) . . . . no N11 Sc1 N13 C18 -112.1(2) . . . . no N11 Sc1 N13 C19 16.26(19) . . . . no N12 Sc1 N13 C17 51.26(19) . . . . no N12 Sc1 N13 C18 167.2(2) . . . . no N12 Sc1 N13 C19 -64.5(2) . . . . no C111 Sc1 N13 C17 -131.1(2) . . . . no C111 Sc1 N13 C18 -15.1(2) . . . . no C111 Sc1 N13 C19 113.2(2) . . . . no C115 Sc1 N13 C17 97.5(3) . . . . no C115 Sc1 N13 C18 -146.5(3) . . . . no C115 Sc1 N13 C19 -18.2(4) . . . . no C119 Sc1 N13 C17 -33.7(2) . . . . no C119 Sc1 N13 C18 82.3(2) . . . . no C119 Sc1 N13 C19 -149.4(2) . . . . no N11 Sc1 C111 Si11 -58.1(3) . . . . no N13 Sc1 C111 Si11 -128.5(3) . . . . no C115 Sc1 C111 Si11 31.4(3) . . . . no C119 Sc1 C111 Si11 135.4(3) . . . . no N11 Sc1 C115 Si12 171.0(2) . . . . no N12 Sc1 C115 Si12 -115.3(2) . . . . no N13 Sc1 C115 Si12 -156.91(16) . . . . no C111 Sc1 C115 Si12 72.4(2) . . . . no C119 Sc1 C115 Si12 -27.0(3) . . . . no N11 Sc1 C119 Si13 -117.1(3) . . . . no N12 Sc1 C119 Si13 -141.8(2) . . . . no N13 Sc1 C119 Si13 -75.7(2) . . . . no C111 Sc1 C119 Si13 21.9(3) . . . . no C115 Sc1 C119 Si13 124.6(2) . . . . no C219 Sc2 N22 C26 -53.2(2) . . . . no N21 Sc2 N23 C27 -131.8(2) . . . . no N21 Sc2 N23 C28 112.3(3) . . . . no N21 Sc2 N23 C29 -15.1(2) . . . . no N22 Sc2 N23 C27 -50.97(19) . . . . no N22 Sc2 N23 C28 -166.9(3) . . . . no N22 Sc2 N23 C29 65.7(2) . . . . no C211 Sc2 N23 C27 133.6(2) . . . . no C211 Sc2 N23 C28 17.7(3) . . . . no C211 Sc2 N23 C29 -109.7(2) . . . . no C215 Sc2 N23 C27 -91.5(3) . . . . no C215 Sc2 N23 C28 152.6(3) . . . . no C215 Sc2 N23 C29 25.2(4) . . . . no C219 Sc2 N23 C27 33.7(2) . . . . no C219 Sc2 N23 C28 -82.2(3) . . . . no C219 Sc2 N23 C29 150.4(2) . . . . no N21 Sc2 C211 Si21 46.8(3) . . . . no N23 Sc2 C211 Si21 117.3(3) . . . . no C215 Sc2 C211 Si21 -43.9(3) . . . . no C219 Sc2 C211 Si21 -147.0(3) . . . . no N21 Sc2 C215 Si22 -175.3(2) . . . . no N22 Sc2 C215 Si22 110.9(2) . . . . no N23 Sc2 C215 Si22 147.30(19) . . . . no C211 Sc2 C215 Si22 -78.8(3) . . . . no C219 Sc2 C215 Si22 23.3(3) . . . . no N21 Sc2 C219 Si23 131.1(3) . . . . no N22 Sc2 C219 Si23 155.4(2) . . . . no N23 Sc2 C219 Si23 89.8(2) . . . . no C211 Sc2 C219 Si23 -7.4(3) . . . . no C215 Sc2 C219 Si23 -111.9(2) . . . . no C219 Sc2 N22 C24 -172.7(2) . . . . no C219 Sc2 N22 C25 66.4(2) . . . . no C215 Sc2 N21 C22 118.3(2) . . . . no C215 Sc2 N21 C23 -123.2(2) . . . . no C219 Sc2 N21 C21 119.6(4) . . . . no C219 Sc2 N21 C22 -122.8(3) . . . . no C219 Sc2 N21 C23 -4.3(4) . . . . no N22 Sc2 N21 C21 94.3(3) . . . . no N22 Sc2 N21 C22 -148.1(2) . . . . no N22 Sc2 N21 C23 -29.61(17) . . . . no N23 Sc2 N21 C21 164.0(3) . . . . no N23 Sc2 N21 C22 -78.4(2) . . . . no N23 Sc2 N21 C23 40.10(17) . . . . no C211 Sc2 N21 C21 -101.5(3) . . . . no C211 Sc2 N21 C22 16.0(2) . . . . no C211 Sc2 N21 C23 134.52(19) . . . . no C215 Sc2 N21 C21 0.8(3) . . . . no N21 Sc2 N22 C26 118.1(2) . . . . no N23 Sc2 N22 C24 -76.3(2) . . . . no N23 Sc2 N22 C25 162.7(2) . . . . no N23 Sc2 N22 C26 43.2(2) . . . . no C215 Sc2 N22 C24 86.9(2) . . . . no N21 Sc2 N22 C24 -1.46(19) . . . . no N21 Sc2 N22 C25 -122.4(2) . . . . no C215 Sc2 N22 C26 -153.6(2) . . . . no C215 Sc2 N22 C25 -34.1(2) . . . . no C113 Si11 C111 Sc1 -10.8(4) . . . . no C112 Si11 C111 Sc1 108.4(3) . . . . no C114 Si11 C111 Sc1 -131.3(3) . . . . no C117 Si12 C115 Sc1 -40.5(3) . . . . no C116 Si12 C115 Sc1 -160.1(2) . . . . no C118 Si12 C115 Sc1 80.2(3) . . . . no C120 Si13 C119 Sc1 -70.5(3) . . . . no C121 Si13 C119 Sc1 170.1(2) . . . . no C122 Si13 C119 Sc1 49.0(3) . . . . no C212 Si21 C211 Sc2 -99.5(3) . . . . no C213 Si21 C211 Sc2 22.5(4) . . . . no C214 Si21 C211 Sc2 140.7(3) . . . . no C217 Si22 C215 Sc2 63.7(3) . . . . no C218 Si22 C215 Sc2 -59.5(3) . . . . no C216 Si22 C215 Sc2 -178.0(3) . . . . no C220 Si23 C219 Sc2 69.9(3) . . . . no C222 Si23 C219 Sc2 -51.7(3) . . . . no C221 Si23 C219 Sc2 -171.1(2) . . . . no Sc1 N11 C13 C19 62.4(2) . . . . no Sc1 N11 C13 C110 -176.7(2) . . . . no C11 N11 C13 C19 -170.3(3) . . . . no C11 N11 C13 C110 -49.4(3) . . . . no C11 N11 C13 C14 70.5(3) . . . . no Sc1 N11 C13 C14 -56.8(2) . . . . no C12 N11 C13 C110 68.3(3) . . . . no C12 N11 C13 C14 -171.8(3) . . . . no C12 N11 C13 C19 -52.6(3) . . . . no Sc1 N12 C14 C13 -33.4(3) . . . . no Sc1 N12 C16 C17 28.1(3) . . . . no C15 N12 C14 C13 -157.9(3) . . . . no C16 N12 C14 C13 84.1(3) . . . . no C15 N12 C16 C17 152.2(3) . . . . no C14 N12 C16 C17 -89.7(3) . . . . no C18 N13 C17 C16 -179.8(3) . . . . no C19 N13 C17 C16 61.4(4) . . . . no C17 N13 C19 C13 -98.7(3) . . . . no C18 N13 C19 C13 144.0(3) . . . . no Sc1 N13 C19 C13 11.4(3) . . . . no Sc1 N13 C17 C16 -56.4(3) . . . . no C22 N21 C23 C210 -68.5(3) . . . . no Sc2 N21 C23 C29 -62.8(3) . . . . no Sc2 N21 C23 C210 176.0(2) . . . . no C21 N21 C23 C24 -69.3(4) . . . . no C21 N21 C23 C29 170.8(3) . . . . no C22 N21 C23 C24 172.6(3) . . . . no C22 N21 C23 C29 52.8(3) . . . . no Sc2 N21 C23 C24 57.1(2) . . . . no C21 N21 C23 C210 49.5(4) . . . . no Sc2 N22 C24 C23 33.8(3) . . . . no C26 N22 C24 C23 -85.3(3) . . . . no Sc2 N22 C26 C27 -29.4(3) . . . . no C25 N22 C24 C23 157.6(3) . . . . no C24 N22 C26 C27 89.5(3) . . . . no C25 N22 C26 C27 -152.6(3) . . . . no Sc2 N23 C27 C26 54.7(3) . . . . no C28 N23 C27 C26 177.0(3) . . . . no C29 N23 C27 C26 -63.6(3) . . . . no Sc2 N23 C29 C23 -13.2(3) . . . . no C27 N23 C29 C23 98.8(3) . . . . no C28 N23 C29 C23 -143.7(3) . . . . no C19 C13 C14 N12 -53.1(4) . . . . no C110 C13 C14 N12 -171.7(3) . . . . no N11 C13 C19 N13 -51.0(3) . . . . no C14 C13 C19 N13 66.0(4) . . . . no C110 C13 C19 N13 -175.5(3) . . . . no N11 C13 C14 N12 64.7(3) . . . . no N12 C16 C17 N13 21.0(4) . . . . no N21 C23 C24 N22 -65.1(3) . . . . no C29 C23 C24 N22 53.1(4) . . . . no C210 C23 C24 N22 171.5(3) . . . . no N21 C23 C29 N23 52.6(4) . . . . no C24 C23 C29 N23 -64.9(4) . . . . no C210 C23 C29 N23 177.4(3) . . . . no N22 C26 C27 N23 -18.7(4) . . . . 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 Si11 C12 3.938(4) . . no Si21 C22 3.727(4) . . no Si11 H117 3.47(4) . . no Si11 H12 3.25(3) . . no Si12 H119' 3.27(3) . . no Si13 H17' 3.33(3) . . no Si13 H111' 3.31(4) . . no Si21 H22" 3.14(3) . . no Si22 H219 3.43(3) . . no Si23 H211 3.33(4) . . no N11 N12 2.987(4) . . no N11 N13 2.869(4) . . no N11 C14 2.451(4) . . no N11 C19 2.464(4) . . no N11 C115 3.308(4) . . no N12 N13 2.732(4) . . no N12 C13 2.538(4) . . no N12 N11 2.987(4) . . no N12 C119 3.302(4) . . no N12 C19 2.951(4) . . no N12 C17 2.517(5) . . no N13 C13 2.526(4) . . no N13 C12 3.244(5) . . no N13 N12 2.732(4) . . no N13 C14 3.072(4) . . no N13 C16 2.497(4) . . no N13 N11 2.869(4) . . no N21 C215 3.359(4) . . no N21 N22 2.980(4) . . no N21 N23 2.878(4) . . no N21 C24 2.454(4) . . no N21 C29 2.465(4) . . no N22 C23 2.524(4) . . no N22 C27 2.524(4) . . no N22 C29 2.947(4) . . no N22 C215 3.447(4) . . no N22 C219 3.282(5) . . no N22 N23 2.713(4) . . no N22 N21 2.980(4) . . no N23 N21 2.878(4) . . no N23 C22 3.257(4) . . no N23 C23 2.522(4) . . no N23 C24 3.066(4) . . no N23 C26 2.499(5) . . no N23 N22 2.713(4) . . no N13 H12' 2.73(3) . . no N23 H22' 2.70(3) . . no C11 C216 3.482(6) . 2_645 no C12 Si11 3.938(4) . . no C22 Si21 3.727(4) . . no C22 C212 3.563(6) . . no C11 H115 2.97(3) . . no C111 C115 3.487(5) . . no C11 H14' 2.60(3) . . no C11 H216' 3.04(4) . 2_645 no C11 H216" 3.04(4) . 2_645 no C111 C119 3.419(5) . . no C11 H115' 2.91(3) . . no C111 Si13 4.000(4) . . no C111 C12 3.419(5) . . no C11 H110" 2.74(3) . . no C12 H19 2.55(3) . . no C12 H112 3.09(4) . . no C12 H110 2.86(3) . . no C14 H11' 2.65(3) . . no C115 C119 3.556(5) . . no C115 C11 3.246(5) . . no C15 H115 3.06(3) . . no C115 C111 3.487(5) . . no C115 N11 3.308(4) . . no C115 C15 3.522(6) . . no C16 H119 2.82(3) . . no C16 H19' 2.82(3) . . no C17 H119 2.98(3) . . no C17 H25' 2.99(3) . . no C18 H111 2.98(4) . . no C18 H12' 2.84(3) . . no C119 C111 3.419(5) . . no C119 C115 3.556(5) . . no C19 H16' 3.04(3) . . no C19 H12' 2.63(3) . . no C119 C17 3.287(5) . . no C19 H12" 3.10(3) . . no C119 N12 3.302(4) . . no C119 C16 3.388(5) . . no C21 H210 2.72(3) . . no C21 H24 2.63(3) . . no C21 H215' 2.92(4) . . no C21 H215 2.97(4) . . no C22 H29' 2.55(3) . . no C22 H210" 2.80(3) . . no C22 H212" 2.86(4) . . no C24 H21' 2.58(3) . . no C25 H215' 3.01(3) . . no C25 H122" 2.80(3) . . no C26 H112' 3.08(4) . 2_645 no C26 H29 2.83(3) . . no C26 H219' 2.76(4) . . no C27 H114' 3.09(4) . 2_645 no C27 H219' 2.82(4) . . no C28 H211' 2.96(4) . . no C28 H22' 2.81(3) . . no C29 H26 3.09(3) . . no C29 H22' 2.54(3) . . no C29 H22 3.05(4) . . no C110 H12" 2.81(3) . . no C110 H11 2.66(3) . . no C110 H11' 3.10(3) . . no C111 H12' 3.00(3) . . no C211 C22 3.343(5) . . no C211 C28 3.583(5) . . no C211 Si23 3.975(4) . . no C211 C219 3.473(5) . . no C211 C215 3.532(5) . . no C212 C22 3.563(6) . . no C112 H117' 3.08(4) . 4_554 no C113 H115' 3.04(3) . . no C115 H11' 3.07(3) . . no C215 N21 3.359(4) . . no C215 N22 3.447(4) . . no C115 H15" 2.96(3) . . no C215 C211 3.532(5) . . no C115 H11" 2.88(3) . . no C215 C21 3.271(6) . . no C215 C25 3.464(5) . . no C215 C219 3.523(5) . . no C216 C11 3.482(6) . 2_655 no C119 H111' 2.94(3) . . no C119 H17' 2.67(3) . . no C219 C215 3.523(5) . . no C219 C211 3.473(5) . . no C219 C26 3.376(5) . . no C219 C27 3.301(5) . . no C219 N22 3.282(5) . . no C120 H117" 2.94(4) . . no C120 H19 3.07(3) . 4_555 no C122 H18" 2.84(3) . . no C122 H17' 3.10(3) . . no C210 H21' 3.09(3) . . no C210 H21" 2.67(3) . . no C210 H22 2.73(4) . . no C211 H22' 2.98(3) . . no C212 H22" 3.04(3) . . no C213 H29 3.08(3) . 2_555 no C214 H21" 2.97(4) . 4_554 no C215 H21 2.90(3) . . no C215 H21' 3.07(3) . . no C215 H25 3.01(3) . . no C216 H29' 3.05(3) . 2_555 no C217 H210 3.10(3) . 4_554 no C218 H219 3.08(3) . . no C219 H26' 3.07(3) . . no C219 H25' 3.04(3) . . no C219 H211 3.04(4) . . no C219 H27 2.71(3) . . no C220 H217 3.00(4) . . no C222 H28' 2.94(3) . . no H110' H14 2.46(4) . . no H110' H19' 2.39(4) . . no H110" H11 2.35(4) . . no H110" H14' 2.57(4) . . no H110" H122' 2.59(4) . 2_645 no H110" C11 2.74(3) . . no H111' Si13 3.31(4) . . no H111' H120" 2.46(5) . . no H112' C26 3.08(4) . 2_655 no H112" H16' 2.58(5) . 2_655 no H114' H27 2.46(5) . 2_655 no H114' C27 3.09(4) . 2_655 no H115' C11 2.91(3) . . no H115' C113 3.04(3) . . no H115' H11" 2.31(4) . . no H11 C110 2.66(3) . . no H11 H110" 2.35(4) . . no H11 H12" 2.43(4) . . no H11' H14' 1.97(4) . . no H11' H115 2.53(4) . . no H11' C110 3.10(3) . . no H11' C115 3.07(3) . . no H11' C14 2.65(3) . . no H11" C115 2.88(3) . . no H11" H115' 2.31(4) . . no H11" H12 2.21(4) . . no H12 Si11 3.25(3) . . no H12 H11" 2.21(4) . . no H12 H112 2.45(5) . . no H12' C18 2.84(3) . . no H12' H18' 2.16(5) . . no H12' C19 2.63(3) . . no H12' C111 3.00(3) . . no H12' N13 2.73(3) . . no H12' H120 2.56(4) . 4_554 no H12' H19 2.20(4) . . no H12" C110 2.81(3) . . no H12" H11 2.43(4) . . no H12" C19 3.10(3) . . no H12" H110 2.27(4) . . no H117' H112 2.42(5) . 4_555 no H117' C112 3.08(4) . 4_555 no H14 H19' 2.56(4) . . no H14 H110' 2.46(4) . . no H14 H16' 2.08(4) . . no H14' C11 2.60(3) . . no H14' H15" 2.12(4) . . no H14' H110" 2.57(4) . . no H14' H11' 1.97(4) . . no H117" H120 2.48(5) . . no H117" H119' 2.51(5) . . no H117" C120 2.94(4) . . no H15 H16 2.56(4) . . no H15' H119 2.57(4) . . no H15' H16 2.21(4) . . no H15" C115 2.96(3) . . no H15" H14' 2.12(4) . . no H15" H115 2.29(5) . . no H16 H119 2.37(4) . . no H16 H15 2.56(4) . . no H16 H15' 2.21(4) . . no H16' C19 3.04(3) . . no H16' H14 2.08(4) . . no H16' H112" 2.58(5) . 2_645 no H16' H114 2.54(5) . 2_645 no H17 H19' 2.31(4) . . no H17 H25' 2.55(4) . . no H17 H18 2.28(4) . . no H17' Si13 3.33(3) . . no H17' C119 2.67(3) . . no H17' H18" 2.35(4) . . no H17' H122" 2.46(4) . . no H17' C122 3.10(3) . . no H17' H119 2.38(4) . . no H17' H25' 2.52(4) . . no H119' Si12 3.27(3) . . no H119' H117" 2.51(5) . . no H119' H118 2.54(5) . . no H18 H17 2.28(4) . . no H18 H19 2.52(4) . . no H18' H19 2.20(4) . . no H18' H12' 2.16(5) . . no H18" H17' 2.35(4) . . no H18" C122 2.84(3) . . no H18" H122 2.38(5) . . no H18" H122" 2.53(4) . . no H120' H19 2.43(5) . 4_555 no H19 H12' 2.20(4) . . no H19 H18 2.52(4) . . no H19 H18' 2.20(4) . . no H19 C12 2.55(3) . . no H19 H110 2.50(4) . . no H19 C120 3.07(3) . 4_554 no H19 H120' 2.43(5) . 4_554 no H19' H110' 2.39(4) . . no H19' H14 2.56(4) . . no H19' H17 2.31(4) . . no H19' C16 2.82(3) . . no H120" H111' 2.46(5) . . no H21 C215 2.90(3) . . no H21 H22" 2.28(5) . . no H21 H215 2.38(5) . . no H21' C24 2.58(3) . . no H21' C210 3.09(3) . . no H21' H24 1.92(4) . . no H21' H215' 2.46(5) . . no H21' C215 3.07(3) . . no H21" C210 2.67(3) . . no H21" H210 2.29(5) . . no H21" C214 2.97(4) . 4_555 no H21" H22 2.37(5) . . no H21" H214 2.26(5) . 4_555 no H22 H210" 2.17(5) . . no H22 H29' 2.58(4) . . no H22 C210 2.73(4) . . no H22 H21" 2.37(5) . . no H22 C29 3.05(4) . . no H22' C28 2.81(3) . . no H22' H28" 2.17(4) . . no H22' C29 2.54(3) . . no H22' C211 2.98(3) . . no H22' N23 2.70(3) . . no H22' H29' 2.09(4) . . no H22" H21 2.28(5) . . no H22" H213 2.56(5) . . no H22" C212 3.04(3) . . no H22" H212" 2.37(5) . . no H22" Si21 3.14(3) . . no H122' H110" 2.59(4) . 2_655 no H122" H18" 2.53(4) . . no H122" C25 2.80(3) . . no H122" H17' 2.46(4) . . no H122" H25' 2.49(5) . . no H24 C21 2.63(3) . . no H24 H21' 1.92(4) . . no H24 H25 2.17(4) . . no H24 H210 2.58(4) . . no H24' H210' 2.45(5) . . no H24' H26 2.16(4) . . no H210' H24' 2.45(5) . . no H210' H29 2.40(5) . . no H25 H24 2.17(4) . . no H25 H215' 2.37(4) . . no H25 C215 3.01(3) . . no H25' C17 2.99(3) . . no H25' C219 3.04(3) . . no H25' H17' 2.52(4) . . no H25' H122" 2.49(5) . . no H25' H17 2.55(4) . . no H25' H26' 2.27(4) . . no H25" H26 2.58(4) . . no H25" H26' 2.46(4) . . no H210" H29' 2.53(4) . . no H210" H22 2.17(5) . . no H210" C22 2.80(3) . . no H26 H25" 2.58(4) . . no H26 H24' 2.16(4) . . no H26 C29 3.09(3) . . no H26' H25" 2.46(4) . . no H26' C219 3.07(3) . . no H26' H25' 2.27(4) . . no H26' H219' 2.29(5) . . no H211' C28 2.96(4) . . no H27 H28' 2.21(4) . . no H27 C219 2.71(3) . . no H27 H114' 2.46(5) . 2_645 no H27 H219' 2.22(5) . . no H27' H28 2.37(5) . . no H27' H29 2.27(4) . . no H28 H29' 2.41(4) . . no H28 H27' 2.37(5) . . no H28' H27 2.21(4) . . no H28' C222 2.94(3) . . no H28' H222 2.40(5) . . no H28" H29' 2.28(4) . . no H28" H22' 2.17(4) . . no H28" H216 2.51(5) . 2_545 no H212" H22" 2.37(5) . . no H212" C22 2.86(4) . . no H29 C26 2.83(3) . . no H29 H210' 2.40(5) . . no H29 H27' 2.27(4) . . no H29 C213 3.08(3) . 2_545 no H29 H213" 2.57(5) . 2_545 no H29' H28 2.41(4) . . no H29' H28" 2.28(4) . . no H29' H210" 2.53(4) . . no H29' C22 2.55(3) . . no H29' H22 2.58(4) . . no H29' H22' 2.09(4) . . no H29' C216 3.05(3) . 2_545 no H29' H216 2.28(5) . 2_545 no H213" H217" 2.43(7) . . no H213" H29 2.57(5) . 2_555 no H215' C21 2.92(4) . . no H215' C25 3.01(3) . . no H215' H21' 2.46(5) . . no H215' H25 2.37(4) . . no H216' C11 3.04(4) . 2_655 no H216" C11 3.04(4) . 2_655 no H217' H116 2.47(5) . 2_655 no H217" H213" 2.43(7) . . no H218" H219 2.39(5) . . no H219' C27 2.82(4) . . no H219' C26 2.76(4) . . no H219' H26' 2.29(5) . . no H219' H27 2.22(5) . . no H222' H212 2.58(5) . 3_555 no H110 H19 2.50(4) . . no H110 C12 2.86(3) . . no H110 H12" 2.27(4) . . no H111 C18 2.98(4) . . no H112 H12 2.45(5) . . no H112 H117' 2.42(5) . 4_554 no H112 C12 3.09(4) . . no H113 H117 2.53(5) . . no H114 H16' 2.54(5) . 2_655 no H115 H11' 2.53(4) . . no H115 C11 2.97(3) . . no H115 C15 3.06(3) . . no H115 H15" 2.29(5) . . no H116 H217' 2.47(5) . 2_645 no H117 Si11 3.47(4) . . no H117 H113 2.53(5) . . no H118 H119' 2.54(5) . . no H119 H17' 2.38(4) . . no H119 C16 2.82(3) . . no H119 H16 2.37(4) . . no H119 H15' 2.57(4) . . no H119 C17 2.98(3) . . no H120 H117" 2.48(5) . . no H120 H12' 2.56(4) . 4_555 no H122 H18" 2.38(5) . . no H210 C21 2.72(3) . . no H210 H21" 2.29(5) . . no H210 H24 2.58(4) . . no H210 C217 3.10(3) . 4_555 no H211 Si23 3.33(4) . . no H211 H220 2.50(5) . . no H212 H222' 2.58(5) . 3_555 no H213 H22" 2.56(5) . . no H214 H21" 2.26(5) . 4_554 no H215 C21 2.97(4) . . no H215 H21 2.38(5) . . no H216 H28" 2.51(5) . 2_555 no H216 H29' 2.28(5) . 2_555 no H217 C220 3.00(4) . . no H217 H220 2.55(5) . . no H219 Si22 3.43(3) . . no H219 C218 3.08(3) . . no H219 H218" 2.39(5) . . no H220 H211 2.50(5) . . no H220 H217 2.55(5) . . no H222 H28' 2.40(5) . . no # Loop Mechanism for Extra Tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tableA_col_1' #'_geom_extra_tableA_col_2' #'_geom_extra_tableA_col_3' #'_geom_extra_table_head_A' #'_geom_table_footnote_A' #'_geom_extra_tableB_col_1' #'_geom_extra_tableB_col_2' #'_geom_extra_tableB_col_3' #'_geom_extra_table_head_B' #'_geom_table_footnote_B' # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 # ? ? ? # #loop_ #_geom_extra_tableB_col_1 #_geom_extra_tableB_col_2 #_geom_extra_tableB_col_3 # ? ? ? # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; #===END of Crystallographic Information File # Attachment '3rev.cif' # CIF-file generated for C131H264N12O4Si12Y4 P-1 Q1104 #============================================================================== data_Q1104 _database_code_depnum_ccdc_archive 'CCDC 606109' #============================================================================== # 0. AUDIT DETAILS _audit_creation_date '2006-04-11 10:53:50' _audit_creation_method ; PLATON
option (version :: 280206) SHELXL97-2 & Manual Editing ; _audit_update_record ; ? ; # 4. TEXT _publ_section_synopsis ; The asymmetric unit consists of two molecules of the title compound and an half toluene solvate molecule, which is highly disordered over an inversion center ; _publ_section_abstract ; ? ; # Insert blank lines between paragraphs _publ_section_comment ; ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; Refinement was frustrated by a disorder problem: from the solution, it was clear that the atom positions of the toluene solvate molecule were highly disordered: the molecule was located over an inversion center, implying disorder (the electron density of the atoms appeared to be smeared out). To improve the parameters chemical more reasonable a disorder model with a regular hexagon constrain and a DFIX constrain for C36-C37 was used in the refinement with an s.o.f. of 0.5, and ultimately all the parameters were fixed. The disorder is compensated by large displacement parameters. The hydrogen atoms were generated by geometrical considerations, constrained to idealized geometries, and allowed to ride on their carrier atoms with an isotropic displacement parameter related to the equivalent displacement parameter of their carrier atoms. The methyl-groups were refined as rigid groups, which were allowed to rotate free, except the hydrogen atoms connected to the methyl (C37) of the highly disordered toluene (these H-positions did not converge; probably due to rotational disorder). ; # Insert blank lines between references _publ_section_references ; Allen, F.H. (2000). Acta Cryst. B58, 380-388. Beurskens, P.T., Beurskens, G., Gelder, R. de, Garc\'ia-Granda, S. Gould, R.O., Israel, & Smits, J.M.M. (1999). The DIRDIF99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Bondi, A. (1964). J. Phys. Chem. 68, 441-451. Bruker, (2000). SMART, SAINTPLUS and XPREP. Software Reference Manual Bruker AXS Inc. Madison, Wisconsin, USA. Hahn, T. (1983). Ed. International Tables for Crystallography, Volume A, Space-group symmetry, 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. (2005). Extended version of the program PLUTO. University of Groningen, The Netherlands. (unpublished). Sheldrick, G.M. (1997). SHELXL-97. Program for Crystal Structure Refinement. University of Gottingen, Germany. Sheldrick, G.M. (2001). SADABS. Version 2.03. Multi-Scan Absorption Correction Program. University of Gottingen, Germany. 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. (2003). J. Appl. Cryst. 36, 7-13. Wilson, A.J.C. (1992). Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; Fig. 1. Perspective PLUTO drawing of the moolecule illustrating the configuration and the adopted numbering scheme. Fig. 2. Molecular packing viewed down unit cell axes. Fig. 3. Perspective ORTEP drawing of the title compound. Displacement ellipsoids for non-H are represented at the 50% probability level. The H-atoms have been omitted to improve clarity. ; #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C31 H64 N3 O Si3 Y), 0.5(C7 H8)' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C131 H264 N12 O4 Si12 Y4' _chemical_formula_iupac ? _chemical_formula_weight 1382.13 _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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 10.653(1) _cell_length_b 17.454(2) _cell_length_c 21.730(2) _cell_angle_alpha 80.864(2) _cell_angle_beta 87.771(2) _cell_angle_gamma 85.449(2) _cell_volume 3975.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 8235 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.45 _cell_special_details ; The final unit cell was obtained from the xyz centroids of 8235 reflections after integration using the SAINTPLUS software package (Bruker, 2000). Reduced cell calculations did not indicate any higher metric lattice symmetry and examination of the finalatomic coordinates of the structure did not yield extra symmetry elements (Spek, 1988; Le Page 1987, 1988) ; _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1490 _exptl_absorpt_coefficient_mu 1.584 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details '(SADABS, Sheldrick, Bruker, 2001))' _exptl_absorpt_correction_T_min 0.6121 _exptl_absorpt_correction_T_max 0.8451 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 100(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; CCD area detector ; _diffrn_measurement_method '\f and \w scans' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temparature unit (KRYOFLEX, (Bruker, 2000)). ; _diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 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 30900 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.1077 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 26.02 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _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 SADABS (Sheldrick, 2001) ; # number of unique reflections _reflns_number_total 15266 _reflns_number_gt 10248 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART, Version 5.624, (Bruker, 2001)' _computing_cell_refinement 'SAINTPLUS, Version 6.02A, (Bruker, 2000)' _computing_data_reduction 'XPREP, Version 5.1/NT, (Bruker, 2000)' _computing_structure_solution ; DIRDIF-99 (Beurskens et al., 1999) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTO (Meetsma, 2006) PLATON (Spek, 2003) ; _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _chemical_absolute_configuration ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 15266 _refine_ls_number_parameters 729 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0956 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1013 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.800 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.088 _vrn_publ_code_squeezed_elec 0.0 _vrn_publ_code_void_volume 0.0 _vrn_publ_code_frame_time_sec 10.0 _vrn_publ_code_meas_time_hour 11.0 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT 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 Y1 Y Uani 0.23658(3) 0.66144(2) 0.31101(2) 1.000 0.0155(1) . . Si11 Si Uani 0.01449(11) 0.80966(7) 0.48150(5) 1.000 0.0261(4) . . Si12 Si Uani 0.34088(10) 0.86661(6) 0.26559(5) 1.000 0.0221(4) . . Si13 Si Uani -0.12657(10) 0.71890(6) 0.28312(5) 1.000 0.0226(4) . . O1 O Uani 0.3192(3) 0.64296(15) 0.20535(12) 1.000 0.0265(9) . . N11 N Uani 0.1697(3) 0.51470(18) 0.31687(15) 1.000 0.0231(11) . . N12 N Uani 0.4054(3) 0.55000(17) 0.34705(15) 1.000 0.0227(11) . . N13 N Uani 0.2034(3) 0.61933(17) 0.41153(14) 1.000 0.0192(10) . . C11 C Uani 0.2779(4) 0.4614(2) 0.3003(2) 1.000 0.0302(16) . . C12 C Uani 0.4065(4) 0.4927(2) 0.30358(19) 1.000 0.0263(14) . . C13 C Uani 0.3671(4) 0.5147(2) 0.41124(17) 1.000 0.0236(14) . . C14 C Uani 0.2272(4) 0.5335(2) 0.42587(18) 1.000 0.0235(14) . . C15 C Uani 0.1404(4) 0.4970(2) 0.38523(18) 1.000 0.0252(14) . . C16 C Uani 0.0573(4) 0.5003(2) 0.2836(2) 1.000 0.0335(16) . . C17 C Uani 0.5354(3) 0.5758(2) 0.3475(2) 1.000 0.0284(14) . . C18 C Uani 0.2024(4) 0.4944(2) 0.49344(19) 1.000 0.0346(16) . . C19 C Uani 0.1469(4) 0.6604(2) 0.46080(18) 1.000 0.0226(12) . . C110 C Uani 0.2341(4) 0.6628(2) 0.51420(19) 1.000 0.0290(16) . . C111 C Uani 0.3559(4) 0.6862(2) 0.5035(2) 1.000 0.0364(16) . . C112 C Uani 0.4316(6) 0.6932(3) 0.5525(3) 1.000 0.059(2) . . C113 C Uani 0.3875(8) 0.6756(3) 0.6138(3) 1.000 0.070(3) . . C114 C Uani 0.2700(7) 0.6503(3) 0.6247(3) 1.000 0.069(3) . . C115 C Uani 0.1932(5) 0.6433(3) 0.5762(2) 1.000 0.0423(19) . . C116 C Uani 0.1077(4) 0.7454(2) 0.43130(18) 1.000 0.0215(12) . . C117 C Uani 0.1142(4) 0.8441(3) 0.5389(2) 1.000 0.0383(17) . . C118 C Uani -0.1196(4) 0.7551(3) 0.5208(2) 1.000 0.0355(17) . . C119 C Uani -0.0549(5) 0.9005(3) 0.4334(2) 1.000 0.0464(17) . . C120 C Uani 0.3792(3) 0.7672(2) 0.30587(18) 1.000 0.0196(12) . . C121 C Uani 0.4638(4) 0.9380(3) 0.2697(2) 1.000 0.0417(17) . . C122 C Uani 0.1927(4) 0.9088(2) 0.3004(2) 1.000 0.0328(16) . . C123 C Uani 0.3165(4) 0.8702(3) 0.17991(18) 1.000 0.0341(17) . . C124 C Uani 0.0397(4) 0.7108(3) 0.2595(2) 1.000 0.0315(16) . . C125 C Uani -0.1654(4) 0.6564(2) 0.35900(19) 1.000 0.0303(16) . . C126 C Uani -0.1775(5) 0.8214(3) 0.2942(3) 1.000 0.066(2) . . C127 C Uani -0.2358(5) 0.6951(4) 0.2256(2) 1.000 0.072(2) . . C128 C Uani 0.2493(5) 0.6181(3) 0.1577(2) 1.000 0.059(2) . . C129 C Uani 0.3197(8) 0.6340(4) 0.0997(3) 1.000 0.113(4) . . C130 C Uani 0.4189(6) 0.6821(4) 0.1079(2) 1.000 0.071(3) . . C131 C Uani 0.4375(4) 0.6683(3) 0.1774(2) 1.000 0.0366(17) . . H11 H Uiso 0.26709 0.45079 0.25748 1.000 0.0362 . . H11' H Uiso 0.27588 0.41127 0.32888 1.000 0.0362 . . H12 H Uiso 0.46897 0.44886 0.31729 1.000 0.0312 . . H12' H Uiso 0.43287 0.51762 0.26143 1.000 0.0312 . . H13 H Uiso 0.41828 0.53419 0.44169 1.000 0.0281 . . H13' H Uiso 0.38451 0.45754 0.41597 1.000 0.0281 . . H15 H Uiso 0.14711 0.43988 0.39810 1.000 0.0301 . . H15' H Uiso 0.05216 0.51610 0.39316 1.000 0.0301 . . H16 H Uiso 0.0757(9) 0.5085(14) 0.2384(10) 1.000 0.0502 . . H16' H Uiso -0.0138(17) 0.5364(12) 0.2930(10) 1.000 0.0502 . . H16" H Uiso 0.0353(15) 0.4465(12) 0.2971(9) 1.000 0.0502 . . H17 H Uiso 0.59312 0.53137 0.36391 1.000 0.0431 . . H17' H Uiso 0.53616 0.61622 0.37405 1.000 0.0431 . . H17" H Uiso 0.56224 0.59677 0.30496 1.000 0.0431 . . H18 H Uiso 0.25770 0.51414 0.52136 1.000 0.0524 . . H18' H Uiso 0.21943 0.43795 0.49641 1.000 0.0524 . . H18" H Uiso 0.11427 0.50624 0.50554 1.000 0.0524 . . H19 H Uiso 0.06967 0.63455 0.47800 1.000 0.0268 . . H111 H Uiso 0.38777 0.69750 0.46189 1.000 0.0439 . . H112 H Uiso 0.51390 0.71026 0.54412 1.000 0.0711 . . H113 H Uiso 0.43861 0.68103 0.64751 1.000 0.0844 . . H114 H Uiso 0.23988 0.63714 0.66650 1.000 0.0835 . . H115 H Uiso 0.11175 0.62513 0.58524 1.000 0.0508 . . H116 H Uiso 0.05758 0.74355 0.39420 1.000 0.0259 . . H116' H Uiso 0.18533 0.77091 0.41632 1.000 0.0259 . . H117 H Uiso 0.18147 0.87330 0.51656 1.000 0.0571 . . H117' H Uiso 0.15141 0.79922 0.56691 1.000 0.0571 . . H117" H Uiso 0.06209 0.87789 0.56322 1.000 0.0571 . . H118 H Uiso -0.08595 0.70759 0.54705 1.000 0.0531 . . H118' H Uiso -0.17303 0.74141 0.48913 1.000 0.0531 . . H118" H Uiso -0.16951 0.78800 0.54674 1.000 0.0531 . . H119 H Uiso -0.09659 0.93466 0.46088 1.000 0.0697 . . H119' H Uiso -0.11667 0.88698 0.40536 1.000 0.0697 . . H119" H Uiso 0.01210 0.92733 0.40874 1.000 0.0697 . . H120 H Uiso 0.39678 0.77173 0.34950 1.000 0.0240 . . H120' H Uiso 0.45971 0.74858 0.28700 1.000 0.0240 . . H121 H Uiso 0.47918 0.94074 0.31339 1.000 0.0625 . . H121' H Uiso 0.43355 0.98956 0.24842 1.000 0.0625 . . H121" H Uiso 0.54223 0.92065 0.24927 1.000 0.0625 . . H122 H Uiso 0.12417 0.87531 0.29751 1.000 0.0493 . . H122' H Uiso 0.17073 0.96090 0.27753 1.000 0.0493 . . H122" H Uiso 0.20558 0.91219 0.34421 1.000 0.0493 . . H123 H Uiso 0.39541 0.85317 0.15978 1.000 0.0507 . . H123' H Uiso 0.29020 0.92366 0.16116 1.000 0.0507 . . H123" H Uiso 0.25105 0.83578 0.17413 1.000 0.0507 . . H124 H Uiso 0.05612 0.76475 0.24099 1.000 0.0378 . . H124' H Uiso 0.04027 0.68193 0.22378 1.000 0.0378 . . H125 H Uiso -0.16880 0.60241 0.35224 1.000 0.0449 . . H125' H Uiso -0.24731 0.67514 0.37524 1.000 0.0449 . . H125" H Uiso -0.10035 0.65901 0.38912 1.000 0.0449 . . H126 H Uiso -0.11616 0.84040 0.31959 1.000 0.0989 . . H126' H Uiso -0.26038 0.82259 0.31541 1.000 0.0989 . . H126" H Uiso -0.18249 0.85479 0.25350 1.000 0.0989 . . H127 H Uiso -0.23000 0.73246 0.18697 1.000 0.1072 . . H127' H Uiso -0.32220 0.69795 0.24264 1.000 0.1072 . . H127" H Uiso -0.21269 0.64243 0.21668 1.000 0.1072 . . H128 H Uiso 0.16514 0.64662 0.15428 1.000 0.0708 . . H128' H Uiso 0.23781 0.56170 0.16812 1.000 0.0708 . . H129 H Uiso 0.35567 0.58457 0.08703 1.000 0.1355 . . H129' H Uiso 0.26343 0.66090 0.06655 1.000 0.1355 . . H130 H Uiso 0.39414 0.73753 0.09281 1.000 0.0858 . . H130' H Uiso 0.49689 0.66650 0.08530 1.000 0.0858 . . H131 H Uiso 0.50675 0.62777 0.18862 1.000 0.0437 . . H131' H Uiso 0.45808 0.71678 0.19173 1.000 0.0437 . . Y2 Y Uani 0.87175(3) 0.16978(2) 0.16691(2) 1.000 0.0142(1) . . Si21 Si Uani 1.16011(10) 0.36436(6) 0.04250(5) 1.000 0.0221(3) . . Si22 Si Uani 1.14929(10) 0.18476(6) 0.27499(5) 1.000 0.0202(3) . . Si23 Si Uani 0.69879(10) 0.38547(6) 0.15759(5) 1.000 0.0193(3) . . O2 O Uani 0.7531(2) 0.11269(14) 0.25942(11) 1.000 0.0216(9) . . N21 N Uani 0.6727(3) 0.13912(16) 0.10761(14) 1.000 0.0167(10) . . N22 N Uani 0.8724(3) 0.03065(16) 0.13517(14) 1.000 0.0161(10) . . N23 N Uani 0.9340(3) 0.17563(16) 0.06783(14) 1.000 0.0169(10) . . C21 C Uani 0.6393(4) 0.0569(2) 0.12484(19) 1.000 0.0227(14) . . C22 C Uani 0.7465(3) 0.0030(2) 0.15411(18) 1.000 0.0202(12) . . C23 C Uani 0.8912(4) 0.04121(19) 0.06601(16) 1.000 0.0167(11) . . C24 C Uani 0.8622(3) 0.1262(2) 0.03499(17) 1.000 0.0169(12) . . C25 C Uani 0.7227(3) 0.1518(2) 0.04185(17) 1.000 0.0199(12) . . C26 C Uani 0.5574(4) 0.1908(2) 0.11082(19) 1.000 0.0254(14) . . C27 C Uani 0.9694(3) -0.0268(2) 0.16522(17) 1.000 0.0201(12) . . C28 C Uani 0.8907(4) 0.1302(2) -0.03509(17) 1.000 0.0236(14) . . C29 C Uani 1.0268(3) 0.2230(2) 0.03278(17) 1.000 0.0172(11) . . C210 C Uani 1.1481(4) 0.1781(2) 0.01227(18) 1.000 0.0193(12) . . C211 C Uani 1.2021(4) 0.1970(2) -0.04653(18) 1.000 0.0246(14) . . C212 C Uani 1.3162(4) 0.1598(2) -0.0636(2) 1.000 0.0296(16) . . C213 C Uani 1.3755(4) 0.1011(2) -0.0223(2) 1.000 0.0303(16) . . C214 C Uani 1.3207(4) 0.0802(2) 0.0364(2) 1.000 0.0262(14) . . C215 C Uani 1.2079(4) 0.1183(2) 0.05339(19) 1.000 0.0218(12) . . C216 C Uani 1.0645(3) 0.2810(2) 0.07473(17) 1.000 0.0181(12) . . C217 C Uani 1.3313(4) 0.3369(3) 0.0308(2) 1.000 0.0386(17) . . C218 C Uani 1.0899(4) 0.4130(2) -0.03222(19) 1.000 0.0301(16) . . C219 C Uani 1.1479(4) 0.4327(2) 0.1012(2) 1.000 0.0329(16) . . C220 C Uani 1.0632(3) 0.1313(2) 0.22697(17) 1.000 0.0168(12) . . C221 C Uani 1.2242(4) 0.1202(2) 0.34379(19) 1.000 0.0361(17) . . C222 C Uani 1.2806(5) 0.2340(3) 0.2293(2) 1.000 0.067(3) . . C223 C Uani 1.0492(4) 0.2625(2) 0.3083(2) 1.000 0.0412(17) . . C224 C Uani 0.7981(3) 0.2990(2) 0.19038(17) 1.000 0.0170(12) . . C225 C Uani 0.5282(3) 0.3775(2) 0.1822(2) 1.000 0.0296(14) . . C226 C Uani 0.7421(4) 0.4783(2) 0.1825(2) 1.000 0.0311(16) . . C227 C Uani 0.7066(4) 0.4021(2) 0.07012(18) 1.000 0.0304(16) . . C228 C Uani 0.8052(4) 0.0629(2) 0.31450(18) 1.000 0.0273(14) . . C229 C Uani 0.6965(4) 0.0498(2) 0.36026(19) 1.000 0.0315(16) . . C230 C Uani 0.6137(4) 0.1247(3) 0.34483(19) 1.000 0.0360(17) . . C231 C Uani 0.6243(4) 0.1404(2) 0.27461(19) 1.000 0.0281(14) . . H21 H Uiso 0.61368 0.03796 0.08697 1.000 0.0272 . . H21' H Uiso 0.56625 0.05531 0.15448 1.000 0.0272 . . H22 H Uiso 0.73659 -0.00245 0.20005 1.000 0.0242 . . H22' H Uiso 0.74148 -0.04909 0.14222 1.000 0.0242 . . H23 H Uiso 0.83588 0.00743 0.04866 1.000 0.0199 . . H23' H Uiso 0.97953 0.02450 0.05581 1.000 0.0199 . . H25 H Uiso 0.70956 0.20775 0.02474 1.000 0.0242 . . H25' H Uiso 0.67376 0.12275 0.01664 1.000 0.0242 . . H26 H Uiso 0.4971(15) 0.1791(10) 0.0825(10) 1.000 0.0381 . . H26' H Uiso 0.5774(6) 0.2441(11) 0.0995(11) 1.000 0.0381 . . H26" H Uiso 0.5222(14) 0.1831(10) 0.1526(9) 1.000 0.0381 . . H27 H Uiso 0.95777 -0.03216 0.21062 1.000 0.0297 . . H27' H Uiso 1.05322 -0.00904 0.15318 1.000 0.0297 . . H27" H Uiso 0.96174 -0.07715 0.15181 1.000 0.0297 . . H28 H Uiso 0.86948 0.18324 -0.05636 1.000 0.0354 . . H28' H Uiso 0.84038 0.09392 -0.05170 1.000 0.0354 . . H28" H Uiso 0.98042 0.11607 -0.04202 1.000 0.0354 . . H29 H Uiso 0.98635 0.25327 -0.00522 1.000 0.0203 . . H211 H Uiso 1.16071 0.23604 -0.07593 1.000 0.0297 . . H212 H Uiso 1.35308 0.17505 -0.10374 1.000 0.0355 . . H213 H Uiso 1.45271 0.07539 -0.03390 1.000 0.0359 . . H214 H Uiso 1.36039 0.03967 0.06513 1.000 0.0315 . . H215 H Uiso 1.17124 0.10318 0.09362 1.000 0.0258 . . H216 H Uiso 1.11124 0.25017 0.10996 1.000 0.0217 . . H216' H Uiso 0.98553 0.30328 0.09262 1.000 0.0217 . . H217 H Uiso 1.34206 0.30192 -0.00043 1.000 0.0577 . . H217' H Uiso 1.36617 0.31054 0.07030 1.000 0.0577 . . H217" H Uiso 1.37540 0.38390 0.01628 1.000 0.0577 . . H218 H Uiso 1.12978 0.46155 -0.04659 1.000 0.0450 . . H218' H Uiso 0.99925 0.42440 -0.02567 1.000 0.0450 . . H218" H Uiso 1.10373 0.37846 -0.06368 1.000 0.0450 . . H219 H Uiso 1.18466 0.48132 0.08321 1.000 0.0494 . . H219' H Uiso 1.19362 0.40879 0.13848 1.000 0.0494 . . H219" H Uiso 1.05913 0.44381 0.11243 1.000 0.0494 . . H220 H Uiso 1.04369 0.08298 0.25502 1.000 0.0202 . . H220' H Uiso 1.12672 0.11498 0.19624 1.000 0.0202 . . H221 H Uiso 1.15844 0.09537 0.37091 1.000 0.0538 . . H221' H Uiso 1.27093 0.15163 0.36724 1.000 0.0538 . . H221" H Uiso 1.28197 0.08014 0.32897 1.000 0.0538 . . H222 H Uiso 1.33545 0.19547 0.21080 1.000 0.1008 . . H222' H Uiso 1.32951 0.25860 0.25699 1.000 0.1008 . . H222" H Uiso 1.24566 0.27374 0.19611 1.000 0.1008 . . H223 H Uiso 1.02054 0.30344 0.27442 1.000 0.0616 . . H223' H Uiso 1.09871 0.28493 0.33714 1.000 0.0616 . . H223" H Uiso 0.97595 0.23985 0.33071 1.000 0.0616 . . H224 H Uiso 0.76059 0.28633 0.23283 1.000 0.0206 . . H224' H Uiso 0.87823 0.32147 0.19656 1.000 0.0206 . . H225 H Uiso 0.49655 0.33302 0.16677 1.000 0.0444 . . H225' H Uiso 0.47891 0.42530 0.16469 1.000 0.0444 . . H225" H Uiso 0.52022 0.37006 0.22775 1.000 0.0444 . . H226 H Uiso 0.72579 0.47576 0.22744 1.000 0.0466 . . H226' H Uiso 0.69133 0.52246 0.16001 1.000 0.0466 . . H226" H Uiso 0.83160 0.48489 0.17298 1.000 0.0466 . . H227 H Uiso 0.79468 0.40454 0.05563 1.000 0.0454 . . H227' H Uiso 0.65910 0.45126 0.05438 1.000 0.0454 . . H227" H Uiso 0.67010 0.35923 0.05466 1.000 0.0454 . . H228 H Uiso 0.87152 0.08867 0.33233 1.000 0.0331 . . H228' H Uiso 0.84205 0.01276 0.30357 1.000 0.0331 . . H229 H Uiso 0.72485 0.04244 0.40379 1.000 0.0380 . . H229' H Uiso 0.65194 0.00418 0.35386 1.000 0.0380 . . H230 H Uiso 0.52551 0.11768 0.35937 1.000 0.0431 . . H230' H Uiso 0.64557 0.16737 0.36348 1.000 0.0431 . . H231 H Uiso 0.56263 0.11189 0.25597 1.000 0.0334 . . H231' H Uiso 0.60923 0.19671 0.25900 1.000 0.0334 . . C31 C Uani 0.40502 0.01859 0.47582 0.500 0.0675 . . C32 C Uani 0.41955 0.08653 0.50107 0.500 0.0697 . . C33 C Uani 0.52630 0.09191 0.53568 0.500 0.0825 . . C34 C Uani 0.61852 0.02935 0.54503 0.500 0.0568 . . C35 C Uani 0.60399 -0.03859 0.51978 0.500 0.0420 . . C36 C Uani 0.49724 -0.04398 0.48518 0.500 0.0539 . . C37 C Uani 0.47704 -0.11274 0.45327 0.500 0.0771 . . H31 H Uiso 0.33283 0.01495 0.45241 0.500 0.0810 . . H32 H Uiso 0.35719 0.12883 0.49474 0.500 0.0836 . . H33 H Uiso 0.53613 0.13785 0.55275 0.500 0.0991 . . H34 H Uiso 0.69071 0.03298 0.56844 0.500 0.0682 . . H35 H Uiso 0.66635 -0.08090 0.52611 0.500 0.0504 . . H37 H Uiso 0.48647 -0.09765 0.40802 0.500 0.1156 . . H37' H Uiso 0.39213 -0.12956 0.46363 0.500 0.1156 . . H37" H Uiso 0.53944 -0.15561 0.46746 0.500 0.1156 . . 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 0.0171(2) 0.0138(2) 0.0157(2) -0.0027(2) 0.0027(2) -0.0016(2) Si11 0.0273(7) 0.0249(6) 0.0259(7) -0.0079(5) 0.0019(5) 0.0060(5) Si12 0.0226(6) 0.0176(6) 0.0253(7) 0.0003(5) 0.0005(5) -0.0047(5) Si13 0.0191(6) 0.0232(6) 0.0240(7) 0.0027(5) -0.0016(5) -0.0043(5) O1 0.0244(16) 0.0365(17) 0.0200(16) -0.0095(13) 0.0024(13) -0.0027(13) N11 0.023(2) 0.0202(18) 0.028(2) -0.0108(15) 0.0015(16) -0.0006(15) N12 0.027(2) 0.0198(18) 0.0206(19) -0.0032(14) 0.0021(16) 0.0018(15) N13 0.029(2) 0.0139(16) 0.0144(18) -0.0032(13) 0.0027(15) 0.0011(14) C11 0.038(3) 0.018(2) 0.037(3) -0.0131(19) 0.005(2) -0.0024(19) C12 0.030(3) 0.021(2) 0.028(2) -0.0084(18) 0.003(2) 0.0042(19) C13 0.034(3) 0.020(2) 0.016(2) -0.0018(17) -0.0052(19) 0.0022(19) C14 0.032(3) 0.016(2) 0.021(2) -0.0013(17) 0.0066(19) -0.0003(18) C15 0.032(3) 0.017(2) 0.025(2) 0.0010(18) 0.009(2) -0.0049(18) C16 0.031(3) 0.024(2) 0.047(3) -0.006(2) -0.001(2) -0.011(2) C17 0.019(2) 0.025(2) 0.039(3) -0.001(2) 0.000(2) 0.0033(18) C18 0.057(3) 0.017(2) 0.027(3) 0.0016(19) 0.010(2) -0.001(2) C19 0.025(2) 0.022(2) 0.020(2) -0.0046(17) 0.0071(19) 0.0013(18) C110 0.044(3) 0.019(2) 0.023(3) -0.0074(18) -0.005(2) 0.015(2) C111 0.044(3) 0.023(2) 0.043(3) -0.012(2) -0.014(2) 0.012(2) C112 0.073(4) 0.029(3) 0.080(5) -0.021(3) -0.047(4) 0.017(3) C113 0.124(6) 0.037(3) 0.052(4) -0.022(3) -0.065(4) 0.044(4) C114 0.125(6) 0.048(4) 0.031(3) -0.015(3) -0.024(4) 0.049(4) C115 0.070(4) 0.037(3) 0.016(3) -0.003(2) -0.004(2) 0.020(3) C116 0.020(2) 0.023(2) 0.020(2) -0.0010(17) -0.0030(18) 0.0042(17) C117 0.040(3) 0.037(3) 0.041(3) -0.017(2) 0.004(2) -0.003(2) C118 0.028(3) 0.043(3) 0.037(3) -0.017(2) 0.010(2) 0.004(2) C119 0.051(3) 0.037(3) 0.047(3) -0.007(2) 0.004(3) 0.020(2) C120 0.019(2) 0.022(2) 0.018(2) -0.0042(17) 0.0000(18) -0.0010(17) C121 0.044(3) 0.031(3) 0.051(3) -0.002(2) -0.001(3) -0.017(2) C122 0.034(3) 0.020(2) 0.041(3) 0.001(2) 0.007(2) 0.004(2) C123 0.037(3) 0.036(3) 0.026(3) 0.004(2) 0.001(2) -0.002(2) C124 0.024(2) 0.037(3) 0.029(3) 0.007(2) -0.001(2) 0.001(2) C125 0.023(2) 0.036(3) 0.030(3) 0.000(2) 0.001(2) -0.002(2) C126 0.063(4) 0.040(3) 0.082(4) 0.011(3) 0.032(3) 0.013(3) C127 0.070(4) 0.116(5) 0.031(3) 0.006(3) -0.008(3) -0.052(4) C128 0.050(4) 0.103(5) 0.038(3) -0.045(3) 0.002(3) -0.021(3) C129 0.225(9) 0.101(5) 0.026(4) -0.004(3) 0.010(5) -0.107(6) C130 0.095(5) 0.096(5) 0.027(3) -0.017(3) 0.026(3) -0.029(4) C131 0.030(3) 0.044(3) 0.034(3) -0.007(2) 0.017(2) 0.001(2) Y2 0.0167(2) 0.0125(2) 0.0135(2) -0.0033(2) 0.0001(2) 0.0005(2) Si21 0.0195(6) 0.0145(5) 0.0315(7) -0.0022(5) 0.0003(5) 0.0000(5) Si22 0.0177(6) 0.0250(6) 0.0176(6) -0.0027(5) 0.0002(5) -0.0022(5) Si23 0.0215(6) 0.0154(5) 0.0207(6) -0.0039(5) 0.0025(5) 0.0013(5) O2 0.0241(16) 0.0219(15) 0.0174(15) -0.0012(12) 0.0025(12) 0.0023(12) N21 0.0156(17) 0.0123(16) 0.0233(19) -0.0079(14) 0.0005(15) 0.0020(13) N22 0.0175(18) 0.0146(16) 0.0154(18) -0.0011(13) -0.0047(14) 0.0031(13) N23 0.0193(18) 0.0147(16) 0.0166(18) -0.0027(13) 0.0022(14) -0.0016(14) C21 0.022(2) 0.018(2) 0.030(3) -0.0082(18) -0.0008(19) -0.0050(17) C22 0.024(2) 0.016(2) 0.021(2) -0.0029(17) 0.0037(18) -0.0054(17) C23 0.021(2) 0.0140(19) 0.016(2) -0.0060(16) -0.0010(17) 0.0013(16) C24 0.020(2) 0.016(2) 0.015(2) -0.0041(16) -0.0001(17) 0.0004(16) C25 0.024(2) 0.019(2) 0.018(2) -0.0064(17) -0.0037(18) -0.0002(17) C26 0.023(2) 0.024(2) 0.030(3) -0.0086(19) 0.000(2) 0.0017(18) C27 0.024(2) 0.019(2) 0.017(2) -0.0028(17) -0.0028(18) 0.0004(17) C28 0.033(3) 0.021(2) 0.018(2) -0.0063(17) 0.0016(19) -0.0042(19) C29 0.024(2) 0.0151(19) 0.011(2) 0.0018(15) 0.0000(17) -0.0003(16) C210 0.024(2) 0.016(2) 0.020(2) -0.0091(17) 0.0068(18) -0.0046(17) C211 0.034(3) 0.020(2) 0.020(2) -0.0039(18) 0.005(2) -0.0044(19) C212 0.034(3) 0.030(2) 0.030(3) -0.020(2) 0.018(2) -0.013(2) C213 0.017(2) 0.031(3) 0.048(3) -0.022(2) 0.002(2) -0.0031(19) C214 0.022(2) 0.024(2) 0.034(3) -0.0098(19) -0.004(2) 0.0019(18) C215 0.022(2) 0.020(2) 0.024(2) -0.0053(18) 0.0043(19) -0.0049(17) C216 0.019(2) 0.017(2) 0.018(2) -0.0045(16) 0.0017(17) 0.0034(16) C217 0.029(3) 0.032(3) 0.057(3) -0.014(2) 0.004(2) -0.005(2) C218 0.033(3) 0.018(2) 0.037(3) 0.0033(19) 0.000(2) -0.0032(19) C219 0.032(3) 0.022(2) 0.047(3) -0.012(2) -0.006(2) -0.001(2) C220 0.014(2) 0.019(2) 0.017(2) -0.0038(16) -0.0014(17) 0.0045(16) C221 0.044(3) 0.036(3) 0.028(3) -0.009(2) -0.015(2) 0.014(2) C222 0.050(4) 0.112(5) 0.044(4) -0.005(3) 0.002(3) -0.049(4) C223 0.054(3) 0.031(3) 0.041(3) -0.015(2) -0.025(3) 0.012(2) C224 0.015(2) 0.018(2) 0.019(2) -0.0057(16) 0.0003(17) -0.0024(16) C225 0.023(2) 0.027(2) 0.040(3) -0.012(2) 0.005(2) 0.0020(19) C226 0.033(3) 0.022(2) 0.038(3) -0.004(2) -0.001(2) -0.002(2) C227 0.035(3) 0.023(2) 0.031(3) 0.0008(19) 0.003(2) -0.001(2) C228 0.039(3) 0.025(2) 0.016(2) -0.0005(18) -0.001(2) 0.004(2) C229 0.040(3) 0.035(3) 0.019(2) 0.0011(19) 0.007(2) -0.014(2) C230 0.032(3) 0.049(3) 0.027(3) -0.006(2) 0.010(2) -0.008(2) C231 0.017(2) 0.031(2) 0.035(3) -0.002(2) 0.002(2) -0.0015(19) C31 0.0731 0.0635 0.0461 0.0400 0.0249 0.0065 C32 0.0662 0.0692 0.0511 0.0497 0.0147 0.0073 C33 0.1825 0.0483 0.0164 -0.0074 0.0323 -0.0184 C34 0.0832 0.0440 0.0419 0.0033 0.0235 -0.0291 C35 0.0417 0.0431 0.0388 0.0039 0.0083 -0.0135 C36 0.0522 0.0905 0.0113 0.0183 0.0046 -0.0134 C37 0.1119 0.0866 0.0397 -0.0136 0.0013 -0.0446 #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's 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 2.487(3) . . yes Y1 N11 2.695(3) . . yes Y1 N12 2.589(3) . . yes Y1 N13 2.215(3) . . yes Y1 C120 2.469(3) . . yes Y1 C124 2.446(4) . . yes Y2 O2 2.449(2) . . yes Y2 N21 2.656(3) . . yes Y2 N22 2.627(3) . . yes Y2 N23 2.217(3) . . yes Y2 C220 2.455(3) . . yes Y2 C224 2.453(4) . . yes Si11 C118 1.881(5) . . yes Si11 C116 1.887(4) . . yes Si11 C117 1.868(5) . . yes Si11 C119 1.871(5) . . yes Si12 C122 1.872(4) . . yes Si12 C120 1.838(4) . . yes Si12 C121 1.892(5) . . yes Si12 C123 1.880(4) . . yes Si13 C124 1.826(4) . . yes Si13 C125 1.878(4) . . yes Si13 C127 1.856(5) . . yes Si13 C126 1.878(5) . . yes Si21 C217 1.867(4) . . yes Si21 C218 1.863(4) . . yes Si21 C216 1.871(4) . . yes Si21 C219 1.874(4) . . yes Si22 C220 1.822(4) . . yes Si22 C221 1.886(4) . . yes Si22 C223 1.877(4) . . yes Si22 C222 1.869(5) . . yes Si23 C225 1.884(3) . . yes Si23 C224 1.835(4) . . yes Si23 C226 1.884(4) . . yes Si23 C227 1.876(4) . . yes O1 C128 1.438(6) . . yes O1 C131 1.448(5) . . yes O2 C228 1.463(5) . . yes O2 C231 1.461(5) . . yes N11 C11 1.493(5) . . yes N11 C15 1.494(5) . . yes N11 C16 1.481(5) . . yes N12 C12 1.480(5) . . yes N12 C17 1.491(5) . . yes N12 C13 1.488(5) . . yes N13 C14 1.484(5) . . yes N13 C19 1.465(5) . . yes N21 C21 1.492(5) . . yes N21 C25 1.495(5) . . yes N21 C26 1.471(5) . . yes N22 C22 1.483(5) . . yes N22 C23 1.492(5) . . yes N22 C27 1.476(5) . . yes N23 C24 1.477(5) . . yes N23 C29 1.453(5) . . yes C11 C12 1.523(6) . . no C13 C14 1.533(6) . . no C14 C15 1.542(6) . . no C14 C18 1.540(6) . . no C19 C116 1.551(5) . . no C19 C110 1.522(6) . . no C110 C115 1.398(6) . . no C110 C111 1.391(6) . . no C11 H11 0.9900 . . no C111 C112 1.387(8) . . no C11 H11' 0.9900 . . no C12 H12' 0.9900 . . no C112 C113 1.391(9) . . no C12 H12 0.9900 . . no C113 C114 1.360(11) . . no C13 H13 0.9900 . . no C13 H13' 0.9900 . . no C114 C115 1.385(8) . . no C15 H15 0.9900 . . no C15 H15' 0.9900 . . no C16 H16" 0.98(2) . . no C16 H16' 0.98(2) . . no C16 H16 0.98(2) . . no C17 H17' 0.9800 . . no C17 H17 0.9800 . . no C17 H17" 0.9800 . . no C18 H18' 0.9800 . . no C18 H18" 0.9800 . . no C18 H18 0.9800 . . no C19 H19 1.0000 . . no C128 C129 1.441(8) . . no C129 C130 1.434(10) . . no C130 C131 1.509(6) . . no C111 H111 0.9500 . . no C112 H112 0.9500 . . no C113 H113 0.9500 . . no C114 H114 0.9500 . . no C115 H115 0.9500 . . no C116 H116' 0.9900 . . no C116 H116 0.9900 . . no C117 H117 0.9800 . . no C117 H117' 0.9800 . . no C117 H117" 0.9800 . . no C118 H118' 0.9800 . . no C118 H118 0.9800 . . no C118 H118" 0.9800 . . no C119 H119" 0.9800 . . no C119 H119' 0.9800 . . no C119 H119 0.9800 . . no C120 H120' 0.9900 . . no C120 H120 0.9900 . . no C21 C22 1.513(5) . . no C121 H121 0.9800 . . no C121 H121' 0.9800 . . no C121 H121" 0.9800 . . no C122 H122' 0.9800 . . no C122 H122 0.9800 . . no C122 H122" 0.9800 . . no C123 H123' 0.9800 . . no C23 C24 1.542(5) . . no C123 H123" 0.9800 . . no C123 H123 0.9800 . . no C24 C25 1.526(5) . . no C124 H124' 0.9900 . . no C124 H124 0.9900 . . no C24 C28 1.533(5) . . no C125 H125' 0.9800 . . no C125 H125" 0.9800 . . no C125 H125 0.9800 . . no C126 H126" 0.9800 . . no C126 H126 0.9800 . . no C126 H126' 0.9800 . . no C127 H127' 0.9800 . . no C127 H127 0.9800 . . no C127 H127" 0.9800 . . no C128 H128' 0.9900 . . no C128 H128 0.9900 . . no C129 H129 0.9900 . . no C29 C216 1.550(5) . . no C129 H129' 0.9900 . . no C29 C210 1.545(5) . . no C130 H130' 0.9900 . . no C130 H130 0.9900 . . no C131 H131' 0.9900 . . no C131 H131 0.9900 . . no C21 H21' 0.9900 . . no C21 H21 0.9900 . . no C22 H22 0.9900 . . no C22 H22' 0.9900 . . no C23 H23' 0.9900 . . no C23 H23 0.9900 . . no C25 H25' 0.9900 . . no C25 H25 0.9900 . . no C26 H26' 0.962(19) . . no C26 H26" 0.962(19) . . no C26 H26 0.962(19) . . no C27 H27" 0.9800 . . no C27 H27 0.9800 . . no C27 H27' 0.9800 . . no C28 H28 0.9800 . . no C28 H28" 0.9800 . . no C28 H28' 0.9800 . . no C29 H29 1.0000 . . no C210 C215 1.392(5) . . no C210 C211 1.383(6) . . no C211 C212 1.397(6) . . no C212 C213 1.380(6) . . no C213 C214 1.389(6) . . no C214 C215 1.393(6) . . no C228 C229 1.504(6) . . no C229 C230 1.517(6) . . no C230 C231 1.508(6) . . no C31 C32 1.4048 . . no C31 C36 1.4050 . . no C32 C33 1.4048 . . no C33 C34 1.4048 . . no C34 C35 1.4048 . . no C35 C36 1.4048 . . no C36 C37 1.5114 . . no C211 H211 0.9500 . . no C212 H212 0.9500 . . no C213 H213 0.9500 . . no C214 H214 0.9500 . . no C215 H215 0.9500 . . no C216 H216 0.9900 . . no C216 H216' 0.9900 . . no C217 H217' 0.9800 . . no C217 H217" 0.9800 . . no C217 H217 0.9800 . . no C218 H218' 0.9800 . . no C218 H218" 0.9800 . . no C218 H218 0.9800 . . no C219 H219' 0.9800 . . no C219 H219" 0.9800 . . no C219 H219 0.9800 . . no C220 H220' 0.9900 . . no C220 H220 0.9900 . . no C221 H221 0.9800 . . no C221 H221' 0.9800 . . no C221 H221" 0.9800 . . no C222 H222 0.9800 . . no C222 H222" 0.9800 . . no C222 H222' 0.9800 . . no C223 H223' 0.9800 . . no C223 H223" 0.9800 . . no C223 H223 0.9800 . . no C224 H224' 0.9900 . . no C224 H224 0.9900 . . no C225 H225' 0.9800 . . no C225 H225" 0.9800 . . no C225 H225 0.9800 . . no C226 H226" 0.9800 . . no C226 H226' 0.9800 . . no C226 H226 0.9800 . . no C227 H227 0.9800 . . no C227 H227' 0.9800 . . no C227 H227" 0.9800 . . no C228 H228' 0.9900 . . no C228 H228 0.9900 . . no C229 H229' 0.9900 . . no C229 H229 0.9900 . . no C230 H230' 0.9900 . . no C230 H230 0.9900 . . no C231 H231' 0.9900 . . no C231 H231 0.9900 . . no C31 H31 0.9500 . . no C32 H32 0.9500 . . no C33 H33 0.9500 . . no C34 H34 0.9500 . . no C35 H35 0.9500 . . no C37 H37 0.9800 . . no C37 H37' 0.9800 . . no C37 H37" 0.9800 . . 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 N11 83.65(9) . . . yes O1 Y1 N12 83.17(10) . . . yes O1 Y1 N13 152.12(10) . . . yes O1 Y1 C120 87.37(11) . . . yes O1 Y1 C124 85.74(13) . . . yes N11 Y1 N12 62.94(10) . . . yes N11 Y1 N13 74.85(10) . . . yes N11 Y1 C120 157.45(10) . . . yes N11 Y1 C124 89.86(14) . . . yes N12 Y1 N13 71.39(11) . . . yes N12 Y1 C120 95.51(11) . . . yes N12 Y1 C124 151.54(14) . . . yes N13 Y1 C120 105.86(12) . . . yes N13 Y1 C124 111.34(13) . . . yes C120 Y1 C124 110.10(14) . . . yes O2 Y2 N22 84.33(9) . . . yes O2 Y2 N23 152.13(10) . . . yes O2 Y2 C220 87.18(10) . . . yes O2 Y2 C224 88.49(10) . . . yes N21 Y2 N22 62.76(9) . . . yes N21 Y2 N23 74.49(11) . . . yes N21 Y2 C220 152.90(10) . . . yes N21 Y2 C224 99.31(10) . . . yes N22 Y2 N23 70.81(10) . . . yes N22 Y2 C220 91.18(11) . . . yes N22 Y2 C224 161.32(10) . . . yes N23 Y2 C220 105.25(12) . . . yes N23 Y2 C224 111.12(11) . . . yes C220 Y2 C224 105.70(12) . . . yes O2 Y2 N21 83.16(8) . . . yes C116 Si11 C117 112.5(2) . . . yes C116 Si11 C118 108.5(2) . . . yes C116 Si11 C119 111.24(19) . . . yes C117 Si11 C118 112.0(2) . . . yes C117 Si11 C119 105.0(2) . . . yes C118 Si11 C119 107.6(2) . . . yes C120 Si12 C121 115.47(18) . . . yes C120 Si12 C122 109.82(17) . . . yes C120 Si12 C123 112.5(2) . . . yes C121 Si12 C122 105.87(19) . . . yes C121 Si12 C123 104.8(2) . . . yes C122 Si12 C123 107.8(2) . . . yes C124 Si13 C125 114.1(2) . . . yes C124 Si13 C126 110.6(2) . . . yes C125 Si13 C126 105.7(2) . . . yes C125 Si13 C127 106.0(2) . . . yes C124 Si13 C127 114.5(2) . . . yes C126 Si13 C127 105.2(3) . . . yes C216 Si21 C217 114.4(2) . . . yes C216 Si21 C218 108.03(17) . . . yes C218 Si21 C219 110.19(17) . . . yes C216 Si21 C219 106.69(17) . . . yes C217 Si21 C218 110.63(19) . . . yes C217 Si21 C219 106.8(2) . . . yes C220 Si22 C222 111.20(19) . . . yes C220 Si22 C223 113.76(18) . . . yes C221 Si22 C222 106.1(2) . . . yes C220 Si22 C221 112.92(17) . . . yes C221 Si22 C223 105.79(18) . . . yes C222 Si22 C223 106.6(2) . . . yes C225 Si23 C227 107.25(19) . . . yes C224 Si23 C227 111.78(17) . . . yes C225 Si23 C226 104.96(18) . . . yes C224 Si23 C225 112.05(16) . . . yes C224 Si23 C226 113.93(17) . . . yes C226 Si23 C227 106.36(18) . . . yes Y1 O1 C128 125.8(3) . . . yes Y1 O1 C131 125.6(2) . . . yes C128 O1 C131 107.8(3) . . . yes Y2 O2 C228 126.5(2) . . . yes Y2 O2 C231 123.1(2) . . . yes C228 O2 C231 108.6(3) . . . yes Y1 N11 C11 111.6(2) . . . yes Y1 N11 C15 99.0(2) . . . yes Y1 N11 C16 119.5(2) . . . yes C11 N11 C15 109.5(3) . . . yes C11 N11 C16 108.9(3) . . . yes C15 N11 C16 107.7(3) . . . yes Y1 N12 C13 106.7(2) . . . yes Y1 N12 C17 114.0(2) . . . yes Y1 N12 C12 108.0(2) . . . yes C13 N12 C17 109.4(3) . . . yes C12 N12 C13 111.0(3) . . . yes C12 N12 C17 107.8(3) . . . yes Y1 N13 C19 130.2(2) . . . yes C14 N13 C19 118.1(3) . . . yes Y1 N13 C14 111.0(2) . . . yes Y2 N21 C26 117.4(2) . . . yes C21 N21 C25 109.5(3) . . . yes Y2 N21 C21 113.0(2) . . . yes Y2 N21 C25 100.2(2) . . . yes C21 N21 C26 108.5(3) . . . yes C25 N21 C26 107.8(3) . . . yes C22 N22 C27 108.6(3) . . . yes Y2 N22 C22 105.9(2) . . . yes Y2 N22 C23 106.38(19) . . . yes Y2 N22 C27 114.7(2) . . . yes C22 N22 C23 111.1(3) . . . yes C23 N22 C27 110.1(3) . . . yes Y2 N23 C24 111.9(2) . . . yes Y2 N23 C29 129.1(2) . . . yes C24 N23 C29 118.9(3) . . . yes N11 C11 C12 114.3(3) . . . yes N12 C12 C11 112.1(3) . . . yes N12 C13 C14 112.4(3) . . . yes C13 C14 C18 106.3(3) . . . no C15 C14 C18 105.9(3) . . . no C13 C14 C15 112.4(3) . . . no N13 C14 C13 106.9(3) . . . yes N13 C14 C15 107.8(3) . . . yes N13 C14 C18 117.6(3) . . . yes N11 C15 C14 114.0(3) . . . yes C110 C19 C116 108.1(3) . . . no N13 C19 C116 108.2(3) . . . yes N13 C19 C110 114.2(3) . . . yes C19 C110 C111 121.7(4) . . . no C19 C110 C115 120.9(4) . . . no C111 C110 C115 117.4(4) . . . no C110 C111 C112 121.2(4) . . . no N11 C11 H11' 109.00 . . . no C12 C11 H11 109.00 . . . no C12 C11 H11' 109.00 . . . no H11 C11 H11' 108.00 . . . no N11 C11 H11 109.00 . . . no N12 C12 H12' 109.00 . . . no C11 C12 H12 109.00 . . . no H12 C12 H12' 108.00 . . . no N12 C12 H12 109.00 . . . no C11 C12 H12' 109.00 . . . no C111 C112 C113 120.3(6) . . . no C14 C13 H13 109.00 . . . no N12 C13 H13 109.00 . . . no C112 C113 C114 118.8(6) . . . no H13 C13 H13' 108.00 . . . no C14 C13 H13' 109.00 . . . no N12 C13 H13' 109.00 . . . no C113 C114 C115 121.4(6) . . . no N11 C15 H15' 109.00 . . . no C14 C15 H15 109.00 . . . no C14 C15 H15' 109.00 . . . no H15 C15 H15' 108.00 . . . no C110 C115 C114 120.8(5) . . . no N11 C15 H15 109.00 . . . no Si11 C116 C19 118.0(3) . . . yes H16' C16 H16" 109.4(16) . . . no N11 C16 H16 109.4(8) . . . no N11 C16 H16' 109.6(12) . . . no H16 C16 H16" 109.4(18) . . . no H16 C16 H16' 109.4(17) . . . no N11 C16 H16" 109.6(11) . . . no N12 C17 H17' 109.00 . . . no N12 C17 H17" 109.00 . . . no H17 C17 H17" 110.00 . . . no H17 C17 H17' 109.00 . . . no N12 C17 H17 109.00 . . . no H17' C17 H17" 109.00 . . . no C14 C18 H18' 109.00 . . . no C14 C18 H18" 109.00 . . . no H18 C18 H18' 109.00 . . . no C14 C18 H18 109.00 . . . no H18 C18 H18" 109.00 . . . no H18' C18 H18" 109.00 . . . no N13 C19 H19 109.00 . . . no C116 C19 H19 109.00 . . . no C110 C19 H19 109.00 . . . no Y1 C120 Si12 123.33(16) . . . yes Y1 C124 Si13 135.7(2) . . . yes O1 C128 C129 107.7(5) . . . yes C128 C129 C130 108.9(5) . . . no C129 C130 C131 104.1(5) . . . no O1 C131 C130 105.7(4) . . . yes C110 C111 H111 119.00 . . . no C112 C111 H111 119.00 . . . no C111 C112 H112 120.00 . . . no C113 C112 H112 120.00 . . . no C112 C113 H113 121.00 . . . no C114 C113 H113 121.00 . . . no C115 C114 H114 119.00 . . . no C113 C114 H114 119.00 . . . no C110 C115 H115 120.00 . . . no C114 C115 H115 120.00 . . . no Si11 C116 H116' 108.00 . . . no C19 C116 H116 108.00 . . . no H116' C116 H116 107.00 . . . no Si11 C116 H116 108.00 . . . no C19 C116 H116' 108.00 . . . no Si11 C117 H117 109.00 . . . no Si11 C117 H117' 109.00 . . . no Si11 C117 H117" 109.00 . . . no H117" C117 H117 109.00 . . . no H117' C117 H117 109.00 . . . no H117' C117 H117" 110.00 . . . no H118' C118 H118 110.00 . . . no H118' C118 H118" 110.00 . . . no Si11 C118 H118 109.00 . . . no H118" C118 H118 109.00 . . . no Si11 C118 H118" 109.00 . . . no Si11 C118 H118' 109.00 . . . no Si11 C119 H119" 109.00 . . . no Si11 C119 H119' 109.00 . . . no H119' C119 H119" 109.00 . . . no H119' C119 H119 109.00 . . . no Si11 C119 H119 109.00 . . . no H119" C119 H119 110.00 . . . no Y1 C120 H120 106.00 . . . no Si12 C120 H120' 107.00 . . . no Y1 C120 H120' 106.00 . . . no H120' C120 H120 107.00 . . . no Si12 C120 H120 107.00 . . . no Si12 C121 H121 109.00 . . . no N21 C21 C22 113.1(3) . . . yes H121" C121 H121 110.00 . . . no H121' C121 H121" 109.00 . . . no H121' C121 H121 110.00 . . . no Si12 C121 H121' 109.00 . . . no Si12 C121 H121" 109.00 . . . no H122' C122 H122 109.00 . . . no H122" C122 H122 110.00 . . . no Si12 C122 H122 109.00 . . . no Si12 C122 H122' 109.00 . . . no Si12 C122 H122" 109.00 . . . no H122' C122 H122" 110.00 . . . no N22 C22 C21 113.2(3) . . . yes Si12 C123 H123' 109.00 . . . no N22 C23 C24 112.6(3) . . . yes Si12 C123 H123 110.00 . . . no H123' C123 H123" 109.00 . . . no Si12 C123 H123" 109.00 . . . no H123" C123 H123 110.00 . . . no H123' C123 H123 109.00 . . . no N23 C24 C25 107.7(3) . . . yes N23 C24 C23 107.3(3) . . . yes Y1 C124 H124' 103.00 . . . no Y1 C124 H124 103.00 . . . no N23 C24 C28 116.4(3) . . . yes C23 C24 C25 111.4(3) . . . no C23 C24 C28 107.6(3) . . . no C25 C24 C28 106.4(3) . . . no Si13 C124 H124' 103.00 . . . no Si13 C124 H124 103.00 . . . no H124' C124 H124 105.00 . . . no N21 C25 C24 113.9(3) . . . yes H125' C125 H125 109.00 . . . no H125" C125 H125 109.00 . . . no Si13 C125 H125' 109.00 . . . no Si13 C125 H125" 109.00 . . . no Si13 C125 H125 109.00 . . . no H125' C125 H125" 109.00 . . . no H126" C126 H126 109.00 . . . no Si13 C126 H126 109.00 . . . no Si13 C126 H126' 110.00 . . . no Si13 C126 H126" 110.00 . . . no H126' C126 H126" 109.00 . . . no H126' C126 H126 109.00 . . . no Si13 C127 H127' 110.00 . . . no Si13 C127 H127 109.00 . . . no H127' C127 H127" 110.00 . . . no Si13 C127 H127" 109.00 . . . no H127" C127 H127 109.00 . . . no H127' C127 H127 109.00 . . . no C129 C128 H128' 110.00 . . . no O1 C128 H128 110.00 . . . no O1 C128 H128' 110.00 . . . no H128' C128 H128 108.00 . . . no C129 C128 H128 110.00 . . . no N23 C29 C216 107.2(3) . . . yes N23 C29 C210 115.7(3) . . . yes C128 C129 H129' 110.00 . . . no C128 C129 H129 110.00 . . . no C130 C129 H129' 110.00 . . . no C130 C129 H129 110.00 . . . no H129' C129 H129 108.00 . . . no C210 C29 C216 108.2(3) . . . no C129 C130 H130 111.00 . . . no C131 C130 H130' 111.00 . . . no C129 C130 H130' 111.00 . . . no H130' C130 H130 109.00 . . . no C131 C130 H130 111.00 . . . no O1 C131 H131' 111.00 . . . no O1 C131 H131 111.00 . . . no C130 C131 H131 111.00 . . . no H131' C131 H131 109.00 . . . no C130 C131 H131' 111.00 . . . no N21 C21 H21 109.00 . . . no N21 C21 H21' 109.00 . . . no C22 C21 H21 109.00 . . . no C22 C21 H21' 109.00 . . . no H21 C21 H21' 108.00 . . . no N22 C22 H22 109.00 . . . no N22 C22 H22' 109.00 . . . no C21 C22 H22 109.00 . . . no C21 C22 H22' 109.00 . . . no H22 C22 H22' 108.00 . . . no N22 C23 H23 109.00 . . . no N22 C23 H23' 109.00 . . . no C24 C23 H23 109.00 . . . no C24 C23 H23' 109.00 . . . no H23 C23 H23' 108.00 . . . no N21 C25 H25' 109.00 . . . no C24 C25 H25 109.00 . . . no C24 C25 H25' 109.00 . . . no H25 C25 H25' 108.00 . . . no N21 C25 H25 109.00 . . . no N21 C26 H26 109.5(11) . . . no N21 C26 H26" 109.5(10) . . . no H26 C26 H26' 109.5(16) . . . no N21 C26 H26' 109.5(7) . . . no H26' C26 H26" 109.4(17) . . . no H26 C26 H26" 109.4(16) . . . no N22 C27 H27 109.00 . . . no N22 C27 H27' 109.00 . . . no H27 C27 H27' 109.00 . . . no H27 C27 H27" 110.00 . . . no N22 C27 H27" 110.00 . . . no H27' C27 H27" 109.00 . . . no C24 C28 H28 109.00 . . . no C24 C28 H28' 109.00 . . . no C24 C28 H28" 109.00 . . . no H28 C28 H28' 109.00 . . . no H28 C28 H28" 109.00 . . . no H28' C28 H28" 109.00 . . . no N23 C29 H29 109.00 . . . no C210 C29 H29 109.00 . . . no C216 C29 H29 109.00 . . . no C211 C210 C215 118.0(4) . . . no C29 C210 C211 121.4(3) . . . no C29 C210 C215 120.6(3) . . . no C210 C211 C212 121.3(4) . . . no C211 C212 C213 120.2(4) . . . no C212 C213 C214 119.1(4) . . . no C213 C214 C215 120.4(4) . . . no C210 C215 C214 120.9(4) . . . no Si21 C216 C29 121.0(3) . . . yes Y2 C220 Si22 130.74(18) . . . yes Y2 C224 Si23 140.13(19) . . . yes O2 C228 C229 105.9(3) . . . yes C228 C229 C230 102.3(3) . . . no C229 C230 C231 102.2(3) . . . no O2 C231 C230 105.0(3) . . . yes C32 C31 C36 120.00 . . . no C31 C32 C33 120.00 . . . no C32 C33 C34 120.00 . . . no C33 C34 C35 120.01 . . . no C34 C35 C36 120.00 . . . no C31 C36 C37 116.17 . . . no C31 C36 C35 119.99 . . . no C35 C36 C37 123.75 . . . no C210 C211 H211 119.00 . . . no C212 C211 H211 119.00 . . . no C213 C212 H212 120.00 . . . no C211 C212 H212 120.00 . . . no C212 C213 H213 120.00 . . . no C214 C213 H213 121.00 . . . no C215 C214 H214 120.00 . . . no C213 C214 H214 120.00 . . . no C210 C215 H215 120.00 . . . no C214 C215 H215 119.00 . . . no C29 C216 H216 107.00 . . . no Si21 C216 H216' 107.00 . . . no Si21 C216 H216 107.00 . . . no H216' C216 H216 107.00 . . . no C29 C216 H216' 107.00 . . . no Si21 C217 H217" 109.00 . . . no Si21 C217 H217 109.00 . . . no Si21 C217 H217' 109.00 . . . no H217' C217 H217 110.00 . . . no H217" C217 H217 109.00 . . . no H217' C217 H217" 110.00 . . . no Si21 C218 H218' 109.00 . . . no Si21 C218 H218" 109.00 . . . no Si21 C218 H218 109.00 . . . no H218' C218 H218" 109.00 . . . no H218' C218 H218 110.00 . . . no H218" C218 H218 109.00 . . . no Si21 C219 H219' 109.00 . . . no Si21 C219 H219 109.00 . . . no H219' C219 H219" 110.00 . . . no H219' C219 H219 109.00 . . . no H219" C219 H219 109.00 . . . no Si21 C219 H219" 109.00 . . . no Y2 C220 H220 105.00 . . . no Si22 C220 H220' 105.00 . . . no Y2 C220 H220' 105.00 . . . no H220' C220 H220 106.00 . . . no Si22 C220 H220 105.00 . . . no H221' C221 H221 109.00 . . . no H221" C221 H221 110.00 . . . no Si22 C221 H221' 109.00 . . . no Si22 C221 H221" 109.00 . . . no Si22 C221 H221 109.00 . . . no H221' C221 H221" 110.00 . . . no Si22 C222 H222" 109.00 . . . no Si22 C222 H222 109.00 . . . no H222' C222 H222" 109.00 . . . no H222' C222 H222 109.00 . . . no H222" C222 H222 109.00 . . . no Si22 C222 H222' 109.00 . . . no Si22 C223 H223" 110.00 . . . no Si22 C223 H223 109.00 . . . no Si22 C223 H223' 110.00 . . . no H223' C223 H223" 109.00 . . . no H223' C223 H223 109.00 . . . no H223" C223 H223 109.00 . . . no Y2 C224 H224' 102.00 . . . no Y2 C224 H224 102.00 . . . no Si23 C224 H224' 102.00 . . . no Si23 C224 H224 102.00 . . . no H224' C224 H224 105.00 . . . no Si23 C225 H225" 110.00 . . . no Si23 C225 H225 109.00 . . . no H225' C225 H225" 110.00 . . . no H225' C225 H225 109.00 . . . no H225" C225 H225 110.00 . . . no Si23 C225 H225' 109.00 . . . no Si23 C226 H226' 109.00 . . . no H226' C226 H226" 110.00 . . . no Si23 C226 H226" 109.00 . . . no Si23 C226 H226 109.00 . . . no H226' C226 H226 109.00 . . . no H226" C226 H226 110.00 . . . no H227' C227 H227" 109.00 . . . no Si23 C227 H227' 109.00 . . . no Si23 C227 H227" 109.00 . . . no H227' C227 H227 109.00 . . . no H227" C227 H227 109.00 . . . no Si23 C227 H227 109.00 . . . no O2 C228 H228' 111.00 . . . no O2 C228 H228 111.00 . . . no C229 C228 H228 111.00 . . . no H228' C228 H228 109.00 . . . no C229 C228 H228' 110.00 . . . no C228 C229 H229' 111.00 . . . no C228 C229 H229 111.00 . . . no C230 C229 H229' 111.00 . . . no C230 C229 H229 111.00 . . . no H229' C229 H229 109.00 . . . no C229 C230 H230' 111.00 . . . no C229 C230 H230 111.00 . . . no C231 C230 H230 111.00 . . . no H230' C230 H230 109.00 . . . no C231 C230 H230' 111.00 . . . no O2 C231 H231' 111.00 . . . no O2 C231 H231 111.00 . . . no C230 C231 H231 111.00 . . . no H231' C231 H231 109.00 . . . no C230 C231 H231' 111.00 . . . no C32 C31 H31 120.00 . . . no C36 C31 H31 120.00 . . . no C31 C32 H32 120.00 . . . no C33 C32 H32 120.00 . . . no C32 C33 H33 120.00 . . . no C34 C33 H33 120.00 . . . no C33 C34 H34 120.00 . . . no C35 C34 H34 120.00 . . . no C34 C35 H35 120.00 . . . no C36 C35 H35 120.00 . . . no C36 C37 H37 109.00 . . . no C36 C37 H37' 109.00 . . . no C36 C37 H37" 109.00 . . . no H37 C37 H37' 109.00 . . . no H37 C37 H37" 109.00 . . . no H37' C37 H37" 109.00 . . . 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 N11 Y1 O1 C128 53.2(3) . . . . no N11 Y1 O1 C131 -138.5(3) . . . . no N12 Y1 O1 C128 116.6(3) . . . . no N12 Y1 O1 C131 -75.1(3) . . . . no N13 Y1 O1 C128 92.6(4) . . . . no N13 Y1 O1 C131 -99.1(4) . . . . no C120 Y1 O1 C128 -147.5(3) . . . . no C120 Y1 O1 C131 20.8(3) . . . . no C124 Y1 O1 C128 -37.2(3) . . . . no C124 Y1 O1 C131 131.2(3) . . . . no O1 Y1 N11 C11 51.4(2) . . . . no O1 Y1 N11 C15 166.6(2) . . . . no O1 Y1 N11 C16 -77.1(3) . . . . no N12 Y1 N11 C11 -34.1(2) . . . . no N12 Y1 N11 C15 81.1(2) . . . . no N12 Y1 N11 C16 -162.7(3) . . . . no N13 Y1 N11 C11 -110.6(3) . . . . no N13 Y1 N11 C15 4.5(2) . . . . no N13 Y1 N11 C16 120.8(3) . . . . no C120 Y1 N11 C11 -15.7(4) . . . . no C120 Y1 N11 C15 99.5(3) . . . . no C120 Y1 N11 C16 -144.3(3) . . . . no C124 Y1 N11 C11 137.2(3) . . . . no C124 Y1 N11 C15 -107.7(2) . . . . no C124 Y1 N11 C16 8.6(3) . . . . no O1 Y1 N12 C12 -39.6(2) . . . . no O1 Y1 N12 C13 -159.0(2) . . . . no O1 Y1 N12 C17 80.1(3) . . . . no N11 Y1 N12 C12 46.7(2) . . . . no N11 Y1 N12 C13 -72.7(2) . . . . no N11 Y1 N12 C17 166.4(3) . . . . no N13 Y1 N12 C12 128.8(3) . . . . no N13 Y1 N12 C13 9.4(2) . . . . no N13 Y1 N12 C17 -111.5(3) . . . . no C120 Y1 N12 C12 -126.3(2) . . . . no C120 Y1 N12 C13 114.3(2) . . . . no C120 Y1 N12 C17 -6.6(3) . . . . no C124 Y1 N12 C12 28.2(4) . . . . no C124 Y1 N12 C13 -91.2(3) . . . . no C124 Y1 N12 C17 147.9(3) . . . . no O1 Y1 N13 C14 -13.1(4) . . . . no O1 Y1 N13 C19 176.7(3) . . . . no N11 Y1 N13 C14 27.8(2) . . . . no N11 Y1 N13 C19 -142.5(3) . . . . no N12 Y1 N13 C14 -38.3(2) . . . . no N12 Y1 N13 C19 151.4(3) . . . . no C120 Y1 N13 C14 -128.9(2) . . . . no C120 Y1 N13 C19 60.9(3) . . . . no C124 Y1 N13 C14 111.5(3) . . . . no C124 Y1 N13 C19 -58.8(4) . . . . no O1 Y1 C120 Si12 82.1(2) . . . . no N11 Y1 C120 Si12 148.5(2) . . . . no N12 Y1 C120 Si12 165.0(2) . . . . no N13 Y1 C120 Si12 -122.9(2) . . . . no C124 Y1 C120 Si12 -2.4(3) . . . . no O1 Y1 C124 Si13 155.3(4) . . . . no N11 Y1 C124 Si13 71.7(4) . . . . no N12 Y1 C124 Si13 88.1(4) . . . . no N13 Y1 C124 Si13 -2.0(4) . . . . no C120 Y1 C124 Si13 -119.1(4) . . . . no N23 Y2 O2 C228 105.8(3) . . . . no N23 Y2 O2 C231 -91.3(3) . . . . no C220 Y2 O2 C228 -12.2(3) . . . . no C220 Y2 O2 C231 150.6(2) . . . . no C224 Y2 O2 C228 -118.0(3) . . . . no C224 Y2 O2 C231 44.8(2) . . . . no O2 Y2 N21 C21 -51.7(2) . . . . no O2 Y2 N21 C25 -168.0(2) . . . . no O2 Y2 N21 C26 75.8(2) . . . . no N22 Y2 N21 C21 35.4(2) . . . . no N22 Y2 N21 C25 -80.9(2) . . . . no N22 Y2 N21 C26 162.9(3) . . . . no N23 Y2 N21 C21 111.5(2) . . . . no N23 Y2 N21 C25 -4.82(19) . . . . no N23 Y2 N21 C26 -121.0(3) . . . . no C220 Y2 N21 C21 18.2(4) . . . . no C220 Y2 N21 C25 -98.1(3) . . . . no C220 Y2 N21 C26 145.7(3) . . . . no C224 Y2 N21 C21 -139.0(2) . . . . no C224 Y2 N21 C25 104.7(2) . . . . no C224 Y2 N21 C26 -11.6(3) . . . . no O2 Y2 N22 C22 38.6(2) . . . . no O2 Y2 N22 C23 156.8(2) . . . . no O2 Y2 N22 C27 -81.2(2) . . . . no N21 Y2 N22 C22 -46.6(2) . . . . no N21 Y2 N22 C23 71.6(2) . . . . no N21 Y2 N22 C27 -166.4(3) . . . . no N23 Y2 N22 C22 -128.6(2) . . . . no N23 Y2 N22 C23 -10.4(2) . . . . no N23 Y2 N22 C27 111.6(2) . . . . no C220 Y2 N22 C22 125.7(2) . . . . no C220 Y2 N22 C23 -116.1(2) . . . . no C220 Y2 N22 C27 5.9(2) . . . . no O2 Y2 N23 C24 10.9(4) . . . . no O2 Y2 N23 C29 -172.8(2) . . . . no N21 Y2 N23 C24 -27.1(2) . . . . no N21 Y2 N23 C29 149.3(3) . . . . no N22 Y2 N23 C24 39.0(2) . . . . no N22 Y2 N23 C29 -144.7(3) . . . . no C220 Y2 N23 C24 124.8(2) . . . . no C220 Y2 N23 C29 -58.8(3) . . . . no C224 Y2 N23 C24 -121.2(2) . . . . no C224 Y2 N23 C29 55.1(3) . . . . no O2 Y2 C220 Si22 -92.5(2) . . . . no N21 Y2 C220 Si22 -161.52(17) . . . . no N22 Y2 C220 Si22 -176.8(2) . . . . no N23 Y2 C220 Si22 112.8(2) . . . . no C224 Y2 C220 Si22 -4.9(3) . . . . no O2 Y2 C224 Si23 -114.9(3) . . . . no N21 Y2 C224 Si23 -32.1(3) . . . . no N23 Y2 C224 Si23 44.8(3) . . . . no C220 Y2 C224 Si23 158.5(3) . . . . no N21 Y2 O2 C228 142.4(3) . . . . no N21 Y2 O2 C231 -54.7(2) . . . . no N22 Y2 O2 C228 79.2(2) . . . . no N22 Y2 O2 C231 -117.9(2) . . . . no C117 Si11 C116 C19 75.8(4) . . . . no C118 Si11 C116 C19 -48.7(4) . . . . no C119 Si11 C116 C19 -166.8(3) . . . . no C122 Si12 C120 Y1 59.1(3) . . . . no C123 Si12 C120 Y1 -61.1(3) . . . . no C121 Si12 C120 Y1 178.7(2) . . . . no C125 Si13 C124 Y1 -16.7(4) . . . . no C126 Si13 C124 Y1 102.3(4) . . . . no C127 Si13 C124 Y1 -139.0(4) . . . . no C217 Si21 C216 C29 -76.7(3) . . . . no C218 Si21 C216 C29 47.0(3) . . . . no C219 Si21 C216 C29 165.5(3) . . . . no C223 Si22 C220 Y2 26.1(3) . . . . no C222 Si22 C220 Y2 -94.2(3) . . . . no C221 Si22 C220 Y2 146.7(2) . . . . no C225 Si23 C224 Y2 87.2(3) . . . . no C226 Si23 C224 Y2 -153.8(3) . . . . no C227 Si23 C224 Y2 -33.2(3) . . . . no Y1 O1 C128 C129 165.5(4) . . . . no C128 O1 C131 C130 17.8(5) . . . . no C131 O1 C128 C129 -4.6(5) . . . . no Y1 O1 C131 C130 -152.3(3) . . . . no Y2 O2 C228 C229 174.6(2) . . . . no C231 O2 C228 C229 9.7(4) . . . . no Y2 O2 C231 C230 -149.8(3) . . . . no C228 O2 C231 C230 15.7(4) . . . . no C16 N11 C15 C14 -161.0(3) . . . . no C16 N11 C11 C12 151.9(3) . . . . no Y1 N11 C11 C12 17.9(4) . . . . no C15 N11 C11 C12 -90.6(4) . . . . no Y1 N11 C15 C14 -36.0(3) . . . . no C11 N11 C15 C14 80.8(4) . . . . no C13 N12 C12 C11 59.4(4) . . . . no Y1 N12 C12 C11 -57.3(3) . . . . no C12 N12 C13 C14 -97.7(4) . . . . no C17 N12 C12 C11 179.1(3) . . . . no Y1 N12 C13 C14 19.7(3) . . . . no C17 N12 C13 C14 143.5(3) . . . . no Y1 N13 C14 C18 -177.2(3) . . . . no Y1 N13 C14 C13 63.4(3) . . . . no Y1 N13 C14 C15 -57.7(3) . . . . no C14 N13 C19 C116 -169.1(3) . . . . no C14 N13 C19 C110 70.4(4) . . . . no C19 N13 C14 C18 -5.6(5) . . . . no C19 N13 C14 C13 -125.0(3) . . . . no C19 N13 C14 C15 113.9(4) . . . . no Y1 N13 C19 C110 -119.9(3) . . . . no Y1 N13 C19 C116 0.6(5) . . . . no C26 N21 C21 C22 -151.3(3) . . . . no C25 N21 C21 C22 91.4(4) . . . . no Y2 N21 C21 C22 -19.3(4) . . . . no Y2 N21 C25 C24 35.9(3) . . . . no C21 N21 C25 C24 -83.0(4) . . . . no C26 N21 C25 C24 159.1(3) . . . . no Y2 N22 C22 C21 57.5(3) . . . . no C23 N22 C22 C21 -57.6(4) . . . . no C27 N22 C22 C21 -178.8(3) . . . . no Y2 N22 C23 C24 -18.0(4) . . . . no C22 N22 C23 C24 96.7(3) . . . . no C27 N22 C23 C24 -142.9(3) . . . . no C29 N23 C24 C28 -1.0(4) . . . . no C24 N23 C29 C210 -71.5(4) . . . . no C24 N23 C29 C216 167.7(3) . . . . no Y2 N23 C24 C28 175.8(2) . . . . no C29 N23 C24 C23 119.6(3) . . . . no C29 N23 C24 C25 -120.4(3) . . . . no Y2 N23 C29 C210 112.3(3) . . . . no Y2 N23 C29 C216 -8.4(4) . . . . no Y2 N23 C24 C23 -63.7(3) . . . . no Y2 N23 C24 C25 56.4(3) . . . . no N11 C11 C12 N12 25.1(5) . . . . no N12 C13 C14 N13 -52.8(4) . . . . no N12 C13 C14 C15 65.3(4) . . . . no N12 C13 C14 C18 -179.2(3) . . . . no C18 C14 C15 N11 -167.7(3) . . . . no C13 C14 C15 N11 -52.0(4) . . . . no N13 C14 C15 N11 65.6(4) . . . . no N13 C19 C110 C111 49.9(5) . . . . no C110 C19 C116 Si11 -62.9(4) . . . . no N13 C19 C110 C115 -131.7(4) . . . . no C116 C19 C110 C115 107.8(4) . . . . no C116 C19 C110 C111 -70.6(4) . . . . no N13 C19 C116 Si11 172.9(3) . . . . no N21 C21 C22 N22 -25.7(4) . . . . no N22 C23 C24 N23 51.4(4) . . . . no N22 C23 C24 C25 -66.3(4) . . . . no N22 C23 C24 C28 177.4(3) . . . . no N23 C24 C25 N21 -64.1(4) . . . . no C23 C24 C25 N21 53.4(4) . . . . no C28 C24 C25 N21 170.5(3) . . . . no N23 C29 C210 C211 138.1(4) . . . . no C216 C29 C210 C211 -101.7(4) . . . . no N23 C29 C210 C215 -43.4(5) . . . . no C216 C29 C210 C215 76.8(4) . . . . no N23 C29 C216 Si21 -169.0(2) . . . . no C210 C29 C216 Si21 65.7(3) . . . . no C29 C210 C211 C212 175.7(3) . . . . no C211 C210 C215 C214 1.8(6) . . . . no C215 C210 C211 C212 -2.8(6) . . . . no C29 C210 C215 C214 -176.7(3) . . . . no C210 C211 C212 C213 2.2(6) . . . . no C211 C212 C213 C214 -0.6(6) . . . . no C212 C213 C214 C215 -0.4(6) . . . . no C213 C214 C215 C210 -0.3(6) . . . . no O2 C228 C229 C230 -30.8(4) . . . . no C228 C229 C230 C231 39.7(4) . . . . no C229 C230 C231 O2 -34.4(4) . . . . no C36 C31 C32 C33 0.00 . . . . no C32 C31 C36 C35 0.00 . . . . no C32 C31 C36 C37 -176.72 . . . . no C31 C32 C33 C34 0.00 . . . . no C32 C33 C34 C35 -0.02 . . . . no C33 C34 C35 C36 0.00 . . . . no C34 C35 C36 C31 0.00 . . . . no C34 C35 C36 C37 176.45 . . . . 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 Y2 C215 4.384(4) . . no Y1 H116' 3.2100 . . no Y1 H125" 3.9100 . . no Y1 H111 3.8700 . . no Y1 H123" 3.9100 . . no Y1 H122 3.8000 . . no Y1 H116 3.0100 . . no Y2 H215 3.7000 . . no Y2 H216 3.1300 . . no Y2 H216' 2.9300 . . no Si11 C115 3.718(5) . . no Si21 C211 3.741(4) . . no Si12 H131' 3.4100 . . no Si13 H116 3.2700 . . no Si13 H16' 3.29(2) . . no Si23 H26' 3.313(18) . . no O1 C12 3.208(5) . . no O1 C124 3.356(5) . . no O2 C22 3.214(4) . . no O2 C220 3.381(4) . . no O1 H12' 2.5700 . . no O2 H22 2.5800 . . no N11 C14 2.547(5) . . no N11 N12 2.760(5) . . no N11 N13 3.008(4) . . no N11 C12 2.534(5) . . no N11 C13 2.994(5) . . no N12 C11 2.492(5) . . no N12 C14 2.510(5) . . no N12 C15 3.083(5) . . no N12 N13 2.819(4) . . no N12 N11 2.760(5) . . no N13 N12 2.819(4) . . no N13 N11 3.008(4) . . no N13 C13 2.424(5) . . no N13 C15 2.446(5) . . no N21 C24 2.532(5) . . no N21 N22 2.751(4) . . no N21 N23 2.970(5) . . no N21 C22 2.507(5) . . no N21 C23 2.975(5) . . no N22 C21 2.501(5) . . no N22 N21 2.751(4) . . no N22 C24 2.524(5) . . no N22 C25 3.079(5) . . no N22 N23 2.826(4) . . no N23 N22 2.826(4) . . no N23 C23 2.432(4) . . no N23 N21 2.970(5) . . no N23 C25 2.425(5) . . no N13 H111 2.8300 . . no N23 H215 2.7700 . . no C18 C115 3.381(6) . . no C18 C110 3.090(5) . . no C28 C211 3.589(6) . . no C28 C210 3.183(6) . . no C35 C221 3.5826 . 2_756 no C110 C117 3.432(6) . . no C110 C18 3.090(5) . . no C11 H13' 2.7900 . . no C12 H225" 3.0500 . . no C13 H11' 2.9700 . . no C115 C18 3.381(6) . . no C115 Si11 3.718(5) . . no C115 C117 3.512(7) . . no C117 C115 3.512(7) . . no C117 C110 3.432(6) . . no C18 H19 2.7100 . . no C19 H18 2.8700 . . no C19 H18" 2.7600 . . no C120 C131 3.519(6) . . no C21 H23 2.7900 . . no C23 H21 2.9800 . . no C23 H28" 3.0800 . 2_755 no C124 C128 3.560(7) . . no C124 O1 3.356(5) . . no C26 H217' 2.8600 . 1_455 no C26 H225 2.9500 . . no C27 H126" 3.1000 . 1_645 no C28 H23' 3.0200 . 2_755 no C28 H29 2.6300 . . no C29 H28 2.8100 . . no C29 H28" 2.7500 . . no C31 H229 2.9900 . 2_656 no C34 H117 2.9700 . 2_666 no C35 H230 3.0900 . 2_656 no C35 H229 2.9900 . . no C37 H121 3.0300 . 1_545 no C210 C28 3.183(6) . . no C210 C217 3.595(6) . . no C110 H18 2.5700 . . no C110 H117' 2.8700 . . no C211 C217 3.563(6) . . no C111 H116' 2.8300 . . no C211 C28 3.589(6) . . no C211 Si21 3.741(4) . . no C113 H12 2.8100 . 2_666 no C113 H230' 2.8500 . 2_666 no C114 H117' 2.9100 . . no C115 H117' 2.7000 . . no C215 Y2 4.384(4) . . no C115 H18 2.7400 . . no C116 H125" 3.0300 . . no C217 C211 3.563(6) . . no C217 C210 3.595(6) . . no C118 H223' 3.0700 . 2_666 no C118 H19 3.0300 . . no C119 H126 2.9500 . . no C220 O2 3.381(4) . . no C220 C27 3.483(5) . . no C220 C228 3.463(5) . . no C120 H131' 2.8400 . . no C121 H37 2.9900 . 1_565 no C221 C35 3.5826 . 2_756 no C122 H119" 3.0200 . . no C123 H131' 2.9500 . . no C124 H128 2.9300 . . no C124 H116 3.0900 . . no C125 H16' 3.05(2) . . no C126 H119' 2.9500 . . no C128 H124' 2.8500 . . no C128 H16 3.07(2) . . no C131 H127' 3.0900 . 1_655 no C131 H12' 2.9600 . . no C131 H120' 2.9700 . . no C210 H217 3.0800 . . no C210 H28" 2.5800 . . no C211 H28" 2.8400 . . no C211 H217 2.7800 . . no C212 H217 3.0500 . . no C212 H22' 2.8900 . 2_755 no C213 H21 2.9800 . 2_755 no C214 H26 2.954(18) . 1_655 no C215 H23' 3.0300 . . no C215 H216 2.8800 . . no C217 H130' 3.0600 . 2_765 no C218 H29 3.0400 . . no C219 H128' 3.1000 . 1_655 no C220 H228 3.0500 . . no C220 H216 3.0700 . . no C221 H31 2.9600 . 1_655 no C221 H35 3.0600 . 2_756 no C221 H118" 3.0900 . 2_666 no C223 H224' 3.0900 . . no C224 H216' 2.8500 . . no C224 H231' 2.9900 . . no C224 H223 3.0600 . . no C227 H218 3.0300 . 2_765 no C228 H220 2.8300 . . no C228 H22 3.0300 . . no C231 H224 3.0300 . . no C231 H26" 2.870(19) . . no H116' C111 2.8300 . . no H116' H111 2.5700 . . no H116' Y1 3.2100 . . no H117' C110 2.8700 . . no H117' H223" 2.5900 . 2_666 no H117' C114 2.9100 . . no H117' C115 2.7000 . . no H117" H228 2.5700 . 2_666 no H118" H221' 2.4600 . 2_666 no H118" C221 3.0900 . 2_666 no H118" H32 2.4900 . 2_566 no H119' H126 2.1500 . . no H119' C126 2.9500 . . no H119" C122 3.0200 . . no H119" H122" 2.4700 . . no H120' H131' 2.2300 . . no H120' C131 2.9700 . . no H11 H16" 2.5900 . . no H11 H128' 2.5200 . . no H11 H16 2.2300 . . no H11' C13 2.9700 . . no H11' H13' 2.5300 . . no H11' H15 2.0900 . . no H122' H220 2.4200 . 1_465 no H12 H225" 2.5700 . . no H12 C113 2.8100 . 2_666 no H12 H113 2.4200 . 2_666 no H12 H17 2.3900 . . no H12 H13' 2.3200 . . no H12' C131 2.9600 . . no H12' H17" 2.3500 . . no H12' O1 2.5700 . . no H12' H131 2.4500 . . no H122" H119" 2.4700 . . no H122" H34 2.5800 . 2_666 no H13 H17' 2.2900 . . no H13 H18 2.3900 . . no H13 H17 2.4700 . . no H13' H11' 2.5300 . . no H13' H18' 2.4400 . . no H13' H12 2.3200 . . no H13' C11 2.7900 . . no H123" Y1 3.9100 . . no H15 H16" 2.5200 . . no H15 H18' 2.2900 . . no H15 H11' 2.0900 . . no H15' H16" 2.6000 . . no H15' H18" 2.5300 . . no H15' H16' 2.2800 . . no H124' H128 2.1100 . . no H124' C128 2.8500 . . no H16 H11 2.2300 . . no H16 H128' 2.4000 . . no H16 C128 3.07(2) . . no H16' C125 3.05(2) . . no H16' Si13 3.29(2) . . no H16' H125 2.3900 . . no H16' H15' 2.2800 . . no H16" H15' 2.6000 . . no H16" H15 2.5200 . . no H16" H11 2.5900 . . no H17 H13 2.4700 . . no H17 H12 2.3900 . . no H17' H13 2.2900 . . no H17" H12' 2.3500 . . no H17" H127' 2.4300 . 1_655 no H17" H131 2.5800 . . no H125" H116 2.3400 . . no H125" Y1 3.9100 . . no H125" C116 3.0300 . . no H18 H13 2.3900 . . no H18 C19 2.8700 . . no H18 C110 2.5700 . . no H18 C115 2.7400 . . no H18' H15 2.2900 . . no H18' H13' 2.4400 . . no H18" H18" 2.4900 . 2_566 no H18" H15' 2.5300 . . no H18" H19 2.2400 . . no H18" C19 2.7600 . . no H19 H18" 2.2400 . . no H19 H118 2.5900 . . no H19 H115 2.3700 . . no H19 C118 3.0300 . . no H19 C18 2.7100 . . no H126" C27 3.1000 . 1_465 no H127' H17" 2.4300 . 1_455 no H127' C131 3.0900 . 1_455 no H21 C23 2.9800 . . no H21 H23 2.5200 . . no H21 H213 2.6000 . 2_755 no H21 H25' 2.0700 . . no H21 C213 2.9800 . 2_755 no H21' H231 2.5500 . . no H21' H26 2.5300 . . no H21' H26" 2.2400 . . no H22 C228 3.0300 . . no H22 O2 2.5800 . . no H22 H27 2.3800 . . no H22' C212 2.8900 . 2_755 no H22' H27" 2.3700 . . no H22' H23 2.3400 . . no H128' C219 3.1000 . 1_455 no H128' H219 2.5900 . 1_455 no H128' H16 2.4000 . . no H128' H11 2.5200 . . no H23 H21 2.5200 . . no H23 C21 2.7900 . . no H23 H22' 2.3400 . . no H23 H28' 2.4500 . . no H23 H25' 2.5700 . . no H23' H27' 2.2600 . . no H23' C215 3.0300 . . no H23' H27" 2.5300 . . no H23' H28" 2.4500 . . no H23' C28 3.0200 . 2_755 no H23' H28" 2.5200 . 2_755 no H130' C217 3.0600 . 2_765 no H130' H217 2.5000 . 2_765 no H25 H28 2.4700 . . no H25 H26 2.5900 . . no H25 H26' 2.2400 . . no H25' H21 2.0700 . . no H25' H26 2.5500 . . no H25' H28' 2.3500 . . no H25' H23 2.5700 . . no H131' C120 2.8400 . . no H131' C123 2.9500 . . no H131' H120' 2.2300 . . no H131' Si12 3.4100 . . no H131' H123 2.4200 . . no H26 H25 2.5900 . . no H26 C214 2.954(18) . 1_455 no H26 H25' 2.5500 . . no H26 H217' 2.5700 . 1_455 no H26 H21' 2.5300 . . no H26' H225 2.3900 . . no H26' H217' 2.5000 . 1_455 no H26' H227" 2.3600 . . no H26' Si23 3.313(18) . . no H26' H25 2.2400 . . no H26" C231 2.870(19) . . no H26" H222 2.3300 . 1_455 no H26" H231 2.4200 . . no H26" H21' 2.2400 . . no H26" H231' 2.5800 . . no H216' H224' 2.5500 . . no H216' C224 2.8500 . . no H216' Y2 2.9300 . . no H27 H228' 2.5200 . . no H27 H22 2.3800 . . no H27' H23' 2.2600 . . no H27' H215 2.5600 . . no H27" H23' 2.5300 . . no H27" H22' 2.3700 . . no H217' C26 2.8600 . 1_655 no H217' H26' 2.5000 . 1_655 no H217' H26 2.5700 . 1_655 no H28 C29 2.8100 . . no H28 H29 2.2500 . . no H28 H25 2.4700 . . no H28' H23 2.4500 . . no H28' H25' 2.3500 . . no H28" C29 2.7500 . . no H28" H23' 2.4500 . . no H28" C210 2.5800 . . no H28" C211 2.8400 . . no H28" C23 3.0800 . 2_755 no H28" H23' 2.5200 . 2_755 no H29 C218 3.0400 . . no H29 C28 2.6300 . . no H29 H28 2.2500 . . no H29 H211 2.4000 . . no H218" H211 2.5600 . . no H31 C221 2.9600 . 1_455 no H31 H37' 2.5300 . . no H219' H222" 2.5200 . . no H32 H118" 2.4900 . 2_566 no H220' H215 2.3000 . . no H34 H122" 2.5800 . 2_666 no H221' H118" 2.4600 . 2_666 no H221' H35 2.5300 . 2_756 no H35 H37" 2.4700 . . no H35 H221' 2.5300 . 2_756 no H35 C221 3.0600 . 2_756 no H37 H121 2.0600 . 1_545 no H37 C121 2.9900 . 1_545 no H37' H117 2.4800 . 1_545 no H37' H31 2.5300 . . no H37" H35 2.4700 . . no H222" H219' 2.5200 . . no H222" H216 2.5000 . . no H223' C118 3.0700 . 2_666 no H223' H118 2.5400 . 2_666 no H223" H117' 2.5900 . 2_666 no H224' H216' 2.5500 . . no H224' C223 3.0900 . . no H224' H223 2.2800 . . no H225" H12 2.5700 . . no H225" C12 3.0500 . . no H227" H26' 2.3600 . . no H228' H27 2.5200 . . no H229' H121 2.4800 . 1_545 no H230' C113 2.8500 . 2_666 no H231' C224 2.9900 . . no H231' H26" 2.5800 . . no H231' H224 2.3300 . . no H111 N13 2.8300 . . no H111 H120 2.5800 . . no H111 H116' 2.5700 . . no H111 Y1 3.8700 . . no H113 H12 2.4200 . 2_666 no H115 H19 2.3700 . . no H115 H118 2.5400 . . no H116 C124 3.0900 . . no H116 H125" 2.3400 . . no H116 Y1 3.0100 . . no H116 Si13 3.2700 . . no H117 C34 2.9700 . 2_666 no H117 H37' 2.4800 . 1_565 no H118 H115 2.5400 . . no H118 H19 2.5900 . . no H118 H223' 2.5400 . 2_666 no H120 H111 2.5800 . . no H121 H37 2.0600 . 1_565 no H121 H229' 2.4800 . 1_565 no H121 C37 3.0300 . 1_565 no H122 Y1 3.8000 . . no H123 H131' 2.4200 . . no H125 H16' 2.3900 . . no H126 H119' 2.1500 . . no H126 C119 2.9500 . . no H127 H212 2.5500 . 2_665 no H127 H211 2.4800 . 2_665 no H128 H124' 2.1100 . . no H128 C124 2.9300 . . no H131 H17" 2.5800 . . no H131 H12' 2.4500 . . no H211 H29 2.4000 . . no H211 H218" 2.5600 . . no H211 H127 2.4800 . 2_665 no H212 H127 2.5500 . 2_665 no H213 H21 2.6000 . 2_755 no H215 Y2 3.7000 . . no H215 N23 2.7700 . . no H215 H27' 2.5600 . . no H215 H220' 2.3000 . . no H216 C220 3.0700 . . no H216 H222" 2.5000 . . no H216 C215 2.8800 . . no H216 Y2 3.1300 . . no H217 C212 3.0500 . . no H217 C210 3.0800 . . no H217 C211 2.7800 . . no H217 H130' 2.5000 . 2_765 no H218 H227 2.5100 . 2_765 no H218 C227 3.0300 . 2_765 no H219 H128' 2.5900 . 1_655 no H220 H228 2.4500 . . no H220 C228 2.8300 . . no H220 H122' 2.4200 . 1_645 no H222 H26" 2.3300 . 1_655 no H223 C224 3.0600 . . no H223 H224' 2.2800 . . no H224 C231 3.0300 . . no H224 H231' 2.3300 . . no H225 C26 2.9500 . . no H225 H26' 2.3900 . . no H227 H218 2.5100 . 2_765 no H228 C220 3.0500 . . no H228 H220 2.4500 . . no H228 H117" 2.5700 . 2_666 no H229 C31 2.9900 . 2_656 no H229 C35 2.9900 . . no H230 C35 3.0900 . 2_656 no H231 H21' 2.5500 . . no H231 H26" 2.4200 . . 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) # C12 H12' O1 0.9900 2.5700 3.208(5) 122.00 . yes C22 H22 O2 0.9900 2.5800 3.214(4) 122.00 . yes # Loop Mechanism for Extra Tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tableA_col_1' #'_geom_extra_tableA_col_2' #'_geom_extra_tableA_col_3' #'_geom_extra_table_head_A' #'_geom_table_footnote_A' #'_geom_extra_tableB_col_1' #'_geom_extra_tableB_col_2' #'_geom_extra_tableB_col_3' #'_geom_extra_table_head_B' #'_geom_table_footnote_B' # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 # ? ? ? # #loop_ #_geom_extra_tableB_col_1 #_geom_extra_tableB_col_2 #_geom_extra_tableB_col_3 # ? ? ? # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; #===END of Crystallographic Information File