# CIF-file generated for C22H55N4Si2Y (1) CP576 #============================================================================== data_global #============================================================================== # 0. AUDIT DETAILS _audit_creation_date '2001-01-16 14:21:39' _audit_creation_method 'PLATON option' _audit_update_record ; ? ; #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondence ; Drs. A. Meetsma ; _publ_contact_author_address # Address of author for correspondence ; Crystal Structure Center, Inorganic Solid State Chemistry Laboratory Chemical Physics, Materials Science Center, Groningen University, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; _publ_contact_author_email A.Meetsma@fwn.rug.nl _publ_contact_author_fax '+31 50 3634441' _publ_contact_author_phone '+31 50 3634368' _publ_requested_journal 'Organometallics' # Publication choise FI FM FO CI CM CO _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission : 2003-12-08 Consider this CIF submission for deposition of the second X-ray structure of a manuscript to be submitted to : Organometallics (Our Compound_Identification_Code : CP576) ; #=============================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Meetsma, Auke' ; ? # author related footnote ; ; Crystal Structure Center, Inorganic Solid State Chemistry Laboratory Chemical Physics, Materials Science Center, Groningen University, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; #=============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; # Insert blank lines between paragraphs _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; # Insert blank lines between references _publ_section_references ; Beurskens, P.T., Beurskens, G., Gelder, R. de Garc\'ia-Granda, S. Gould, R.O. Isra\"el, & 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, SAINT, SADABS, XPREP and SHELXTL/NT. Software Reference Manual Bruker AXS Inc. Madison, Wisconsin, USA. International Tables for Crystallography (1983). Vol. A. Space-group symmetry, edited by T. Hahn. Dordrecht: Reidel. (Present distributor Kluwer Academic Publishers, Dordrecht). International Tables for Crystallography (1992). Vol. C. Edited by A.J.C Wilson, Kluwer Academic Publishers, Dordrecht, The Netherlands. Le Page, Y. (1987). J. Appl. Cryst. 20, 264-269. Le Page, Y. (1988). J. Appl. Cryst. 21, 983-984. Meetsma, A. (2000). Extended version of the program PLUTO. Groningen University, The Netherlands. (unpublished). Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany, 1997. Sheldrick, G.M. SHELXS97. Program for Crystal Structure solution. University of G\"ottingen, Germany, 1997. Sheldrick, G.M. SADABS. Version 2. Empirical Absorption Correction Program. University of G\"ottingen, Germany, 2000 Spek, A.L. (1988). J. Appl. Cryst. 21, 578-579. Spek, A.L. (1990). Acta Cryst. A46, C-34. Spek, A.L. (1997). HELENA, Program for Datareduction, Utrecht University, The Netherlands. Spek, A.L. (1994). Am. Crystallogr. Assoc.-Abstracts, 22, 66. ; _publ_section_figure_captions ; Fig. 1. Chemical structural diagram (scheme 1) of the title compound Fig. 2. Perspective PLUTO drawing of the molecule illustrating the configuration and the adopted numbering scheme. Fig. 3. Molecular packing viewed down unit cell axes. Fig. 4. Perspective ORTEP drawing of the title compound. All non-hydrogen atoms are represented by thermal vibrational ellipsoids drawn to encompass 50% of the electron density. The hydrogen atoms are drawn with an arbitrary radius. ; #=============================================================================== data_c22h55n4 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H55 N4 Si2 Y' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C22 H55 N4 Si2 Y' _chemical_formula_weight 520.79 _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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.5799(4) _cell_length_b 9.8987(5) _cell_length_c 17.4468(8) _cell_angle_alpha 99.185(1) _cell_angle_beta 98.943(1) _cell_angle_gamma 111.086(1) _cell_volume 1482.62(12) _cell_formula_units_Z 2 _cell_measurement_temperature 90 _cell_measurement_reflns_used 7010 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.48 _cell_special_details ; The final unit cell was obtained from the xyz centroids of 7010 reflections after integration using the SAINT software package (Bruker, 2000). The intensity data were corrected for decay and absorption using SADABS (Sheldrick, 2000). ; _exptl_crystal_description ' block' _exptl_crystal_colour ' colorless' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.320 _exptl_crystal_size_min 0.220 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 2.062 _exptl_absorpt_correction_type 'Semi-empirical' _exptl_absorpt_process_detais '(SADABS (Sheldrick, Bruker, 2000))' _exptl_absorpt_correction_T_min 0.7043 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine focus sealed Siemens Mo tube ' _diffrn_radiation_monochromator 'parallel mounted graphite' _diffrn_radiation_detector ; CCD area-detector ; _diffrn_measurement_device_type ; Bruker Smart Apex ; _diffrn_measurement_method '\w/2\q' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temparature unit (KROFLEX, (Bruker, 2000)). ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'negligible' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 12916 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.978 _diffrn_reflns_reduction_process ; Intensity data were corrected for Lorentz and polarization effects, decay and absorption and reduced to F~o~^2^ using SAINT (Bruker, 2000) and SABABS (Sheldrick, 2000) ; # number of unique reflections _reflns_number_total 6650 _reflns_number_gt 5549 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker Version 5.168, 2000' _computing_cell_refinement 'SAINT, Bruker Version 6.02A, 2000' _computing_data_reduction 'XPREP, Bruker Version 5.1/NT, 2000' _computing_structure_solution ; DIRDIF-99 (Beurskens et al., 1999) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTO (Meetsma, 2000) PLATON (Spek, 1994, 1996) ; _computing_publication_material ; PLATON (Spek, 1990) SHELXL (Sheldrick, 1997) ; #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_details calc _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6650 _refine_ls_number_parameters 482 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0569 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.618 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.058 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Y1 Y Uani 0.02229(2) 0.18448(2) 0.24513(1) 1.000 0.0142(1) Si1 Si Uani 0.29086(6) 0.20740(5) 0.45428(3) 1.000 0.0182(2) Si2 Si Uani 0.33577(6) 0.46544(5) 0.16585(3) 1.000 0.0181(2) N1 N Uani -0.02597(17) -0.05762(15) 0.22290(8) 1.000 0.0159(4) N2 N Uani -0.23447(16) 0.05542(15) 0.27746(8) 1.000 0.0159(4) N3 N Uani -0.23865(17) 0.11632(16) 0.11750(8) 1.000 0.0181(4) N4 N Uani -0.05065(17) 0.37560(15) 0.33123(8) 1.000 0.0173(4) C1 C Uani 0.1495(3) -0.0347(2) 0.13647(13) 1.000 0.0270(7) C2 C Uani -0.0580(3) -0.2837(2) 0.12074(13) 1.000 0.0283(7) C3 C Uani 0.1637(3) -0.1766(2) 0.23897(12) 1.000 0.0246(6) C4 C Uani 0.0528(2) -0.13908(19) 0.18111(10) 1.000 0.0203(6) C5 C Uani -0.1286(2) -0.1442(2) 0.26622(11) 1.000 0.0186(5) C6 C Uani -0.1841(2) -0.0458(2) 0.31947(11) 1.000 0.0182(5) C7 C Uani -0.3647(2) -0.0312(2) 0.20806(11) 1.000 0.0198(6) C8 C Uani -0.3787(2) 0.0599(2) 0.14807(11) 1.000 0.0198(6) C9 C Uani -0.2322(3) -0.0062(2) 0.05952(11) 1.000 0.0241(6) C10 C Uani -0.2479(3) 0.2296(2) 0.07371(12) 1.000 0.0235(6) C11 C Uani -0.2780(2) 0.1533(2) 0.33384(11) 1.000 0.0191(6) C12 C Uani -0.1401(2) 0.2911(2) 0.38223(11) 1.000 0.0195(6) C13 C Uani -0.1414(3) 0.4393(2) 0.28404(12) 1.000 0.0226(6) C14 C Uani 0.0873(3) 0.5015(2) 0.38247(12) 1.000 0.0242(6) C15 C Uani 0.2446(2) 0.2484(2) 0.35659(11) 1.000 0.0197(6) C16 C Uani 0.2024(3) 0.0040(2) 0.45301(13) 1.000 0.0298(7) C17 C Uani 0.5024(3) 0.2659(3) 0.49607(13) 1.000 0.0317(7) C18 C Uani 0.2265(3) 0.3076(3) 0.53372(12) 1.000 0.0255(7) C19 C Uani 0.1357(2) 0.3445(2) 0.15851(11) 1.000 0.0188(6) C20 C Uani 0.4563(3) 0.3544(3) 0.15503(17) 1.000 0.0364(8) C21 C Uani 0.3633(3) 0.5785(3) 0.08795(13) 1.000 0.0304(7) C22 C Uani 0.4278(3) 0.6004(2) 0.26548(12) 1.000 0.0244(6) H1 H Uiso 0.089(2) -0.010(2) 0.0985(12) 1.000 0.033(6) H1' H Uiso 0.224(2) 0.050(2) 0.1732(12) 1.000 0.033(6) H1" H Uiso 0.208(2) -0.078(2) 0.1098(12) 1.000 0.034(6) H2 H Uiso -0.121(2) -0.263(2) 0.0806(12) 1.000 0.035(6) H2' H Uiso -0.124(2) -0.356(2) 0.1452(11) 1.000 0.025(5) H2" H Uiso 0.000(2) -0.332(2) 0.0942(12) 1.000 0.031(6) H3 H Uiso 0.244(2) -0.087(2) 0.2739(12) 1.000 0.032(6) H3' H Uiso 0.112(2) -0.239(2) 0.2712(12) 1.000 0.034(6) H3" H Uiso 0.215(2) -0.225(2) 0.2109(12) 1.000 0.033(6) H5 H Uiso -0.218(2) -0.2273(19) 0.2300(10) 1.000 0.014(4) H5' H Uiso -0.081(2) -0.1882(19) 0.3028(10) 1.000 0.015(5) H6 H Uiso -0.272(2) -0.1070(18) 0.3377(9) 1.000 0.009(4) H6' H Uiso -0.102(2) 0.0201(19) 0.3663(10) 1.000 0.015(4) H7 H Uiso -0.3481(19) -0.1138(19) 0.1834(10) 1.000 0.010(4) H7' H Uiso -0.460(2) -0.0667(19) 0.2273(10) 1.000 0.015(5) H8 H Uiso -0.3974(19) 0.1440(19) 0.1712(10) 1.000 0.015(5) H8' H Uiso -0.469(2) 0.0016(19) 0.1051(10) 1.000 0.015(5) H9 H Uiso -0.227(2) -0.081(2) 0.0843(11) 1.000 0.025(5) H9' H Uiso -0.135(2) 0.0331(19) 0.0398(10) 1.000 0.017(5) H9" H Uiso -0.323(2) -0.053(2) 0.0147(11) 1.000 0.026(5) H10 H Uiso -0.339(2) 0.193(2) 0.0314(12) 1.000 0.027(5) H10' H Uiso -0.165(2) 0.267(2) 0.0521(11) 1.000 0.026(6) H10" H Uiso -0.244(2) 0.313(2) 0.1089(12) 1.000 0.028(5) H11 H Uiso -0.357(2) 0.1773(19) 0.3047(10) 1.000 0.016(5) H11' H Uiso -0.331(2) 0.099(2) 0.3686(11) 1.000 0.021(5) H12 H Uiso -0.071(2) 0.2663(19) 0.4167(10) 1.000 0.016(5) H12' H Uiso -0.172(2) 0.355(2) 0.4168(11) 1.000 0.024(5) H13 H Uiso -0.082(2) 0.4913(19) 0.2547(10) 1.000 0.017(5) H13' H Uiso -0.231(2) 0.365(2) 0.2481(11) 1.000 0.023(5) H13" H Uiso -0.176(2) 0.504(2) 0.3187(11) 1.000 0.026(5) H14 H Uiso 0.145(2) 0.465(2) 0.4159(12) 1.000 0.028(6) H14' H Uiso 0.150(2) 0.554(2) 0.3501(11) 1.000 0.023(5) H14" H Uiso 0.060(2) 0.572(2) 0.4156(11) 1.000 0.026(5) H15 H Uiso 0.300(2) 0.354(2) 0.3622(12) 1.000 0.037(6) H15' H Uiso 0.287(2) 0.199(2) 0.3229(12) 1.000 0.040(6) H16 H Uiso 0.227(3) -0.013(2) 0.5016(14) 1.000 0.045(7) H16' H Uiso 0.237(3) -0.052(3) 0.4183(14) 1.000 0.050(7) H16" H Uiso 0.098(3) -0.034(3) 0.4384(15) 1.000 0.062(9) H17 H Uiso 0.526(2) 0.238(2) 0.5438(13) 1.000 0.040(6) H17' H Uiso 0.560(3) 0.367(3) 0.5026(15) 1.000 0.065(9) H17" H Uiso 0.542(3) 0.224(3) 0.4621(16) 1.000 0.069(9) H18 H Uiso 0.264(2) 0.295(2) 0.5851(12) 1.000 0.032(6) H18' H Uiso 0.115(3) 0.266(2) 0.5242(12) 1.000 0.040(6) H18" H Uiso 0.261(2) 0.406(2) 0.5333(12) 1.000 0.041(7) H19 H Uiso 0.099(2) 0.284(2) 0.1063(11) 1.000 0.024(5) H19' H Uiso 0.079(2) 0.403(2) 0.1567(12) 1.000 0.034(6) H20 H Uiso 0.417(3) 0.284(3) 0.1083(14) 1.000 0.047(7) H20' H Uiso 0.551(3) 0.415(3) 0.1566(14) 1.000 0.056(8) H20" H Uiso 0.464(2) 0.304(2) 0.2023(14) 1.000 0.044(7) H21 H Uiso 0.465(3) 0.633(2) 0.0896(12) 1.000 0.035(6) H21' H Uiso 0.322(2) 0.520(2) 0.0393(13) 1.000 0.033(6) H21" H Uiso 0.309(2) 0.643(2) 0.0932(12) 1.000 0.037(6) H22 H Uiso 0.532(3) 0.662(2) 0.2674(12) 1.000 0.036(6) H22' H Uiso 0.426(2) 0.552(2) 0.3066(12) 1.000 0.033(6) H22" H Uiso 0.375(2) 0.666(2) 0.2788(12) 1.000 0.041(6) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0162(1) 0.0133(1) 0.0137(1) 0.0043(1) 0.0052(1) 0.0054(1) Si1 0.0193(3) 0.0198(3) 0.0155(2) 0.0052(2) 0.0040(2) 0.0073(2) Si2 0.0170(3) 0.0173(3) 0.0206(3) 0.0064(2) 0.0062(2) 0.0057(2) N1 0.0194(8) 0.0136(7) 0.0166(7) 0.0048(6) 0.0080(6) 0.0065(6) N2 0.0191(8) 0.0155(7) 0.0146(7) 0.0047(6) 0.0046(6) 0.0076(6) N3 0.0184(8) 0.0198(8) 0.0164(7) 0.0054(6) 0.0044(6) 0.0071(7) N4 0.0193(8) 0.0154(7) 0.0166(7) 0.0039(6) 0.0045(6) 0.0058(7) C1 0.0347(13) 0.0298(12) 0.0272(11) 0.0096(9) 0.0173(10) 0.0195(11) C2 0.0378(14) 0.0224(11) 0.0253(11) 0.0004(9) 0.0055(10) 0.0154(10) C3 0.0288(12) 0.0251(11) 0.0259(10) 0.0074(9) 0.0106(9) 0.0150(10) C4 0.0280(11) 0.0175(9) 0.0185(9) 0.0034(7) 0.0079(8) 0.0117(8) C5 0.0201(10) 0.0159(9) 0.0198(9) 0.0056(8) 0.0054(8) 0.0061(8) C6 0.0190(10) 0.0194(9) 0.0174(9) 0.0072(8) 0.0066(8) 0.0069(8) C7 0.0162(10) 0.0187(10) 0.0210(10) 0.0039(8) 0.0034(8) 0.0035(8) C8 0.0161(10) 0.0210(10) 0.0200(9) 0.0038(8) 0.0020(8) 0.0059(8) C9 0.0299(12) 0.0269(11) 0.0157(9) 0.0037(8) 0.0037(9) 0.0125(10) C10 0.0219(12) 0.0274(11) 0.0216(10) 0.0100(9) 0.0033(9) 0.0091(9) C11 0.0204(11) 0.0220(10) 0.0191(9) 0.0075(8) 0.0103(8) 0.0098(8) C12 0.0249(11) 0.0221(10) 0.0158(9) 0.0044(8) 0.0072(8) 0.0131(9) C13 0.0268(12) 0.0188(10) 0.0230(10) 0.0068(9) 0.0047(9) 0.0095(9) C14 0.0264(12) 0.0186(10) 0.0245(10) 0.0017(8) 0.0022(9) 0.0082(9) C15 0.0210(11) 0.0182(10) 0.0188(9) 0.0053(8) 0.0058(8) 0.0055(8) C16 0.0411(15) 0.0242(11) 0.0205(11) 0.0069(9) 0.0013(10) 0.0105(11) C17 0.0251(12) 0.0491(15) 0.0227(11) 0.0091(10) 0.0045(9) 0.0167(12) C18 0.0314(13) 0.0314(12) 0.0190(10) 0.0104(9) 0.0080(9) 0.0158(10) C19 0.0191(10) 0.0190(9) 0.0200(10) 0.0071(8) 0.0058(8) 0.0080(8) C20 0.0244(13) 0.0285(12) 0.0560(16) 0.0051(12) 0.0132(12) 0.0106(11) C21 0.0328(14) 0.0282(12) 0.0218(11) 0.0075(9) 0.0079(10) 0.0011(11) C22 0.0240(12) 0.0232(10) 0.0218(10) 0.0091(9) 0.0042(9) 0.0032(9) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N1 2.2266(15) . . yes Y1 N2 2.5300(16) . . yes Y1 N4 2.5873(15) . . yes Y1 C15 2.463(2) . . yes Y1 C19 2.4515(19) . . yes Si1 C15 1.8389(19) . . yes Si1 C16 1.877(2) . . yes Si1 C17 1.880(3) . . yes Si1 C18 1.885(3) . . yes Si2 C19 1.829(2) . . yes Si2 C20 1.869(3) . . yes Si2 C21 1.885(3) . . yes Si2 C22 1.876(2) . . yes N1 C4 1.474(3) . . yes N1 C5 1.450(2) . . yes N2 C6 1.499(2) . . yes N2 C7 1.479(2) . . yes N2 C11 1.481(2) . . yes N3 C8 1.475(3) . . yes N3 C9 1.476(3) . . yes N3 C10 1.474(3) . . yes N4 C12 1.478(2) . . yes N4 C13 1.473(3) . . yes N4 C14 1.480(3) . . yes C1 C4 1.525(3) . . no C2 C4 1.537(3) . . no C3 C4 1.535(3) . . no C5 C6 1.527(3) . . no C7 C8 1.507(3) . . no C11 C12 1.519(3) . . no C1 H1 0.93(2) . . no C1 H1' 0.94(2) . . no C1 H1" 0.95(2) . . no C2 H2 0.95(2) . . no C2 H2' 0.975(19) . . no C2 H2" 0.98(2) . . no C3 H3 0.97(2) . . no C3 H3' 0.96(2) . . no C3 H3" 0.94(2) . . no C5 H5 0.984(18) . . no C5 H5' 0.973(18) . . no C6 H6 0.977(19) . . no C6 H6' 0.986(18) . . no C7 H7 0.939(18) . . no C7 H7' 0.99(2) . . no C8 H8 0.954(18) . . no C8 H8' 0.972(18) . . no C9 H9 0.927(19) . . no C9 H9' 1.01(2) . . no C9 H9" 0.983(19) . . no C10 H10 0.96(2) . . no C10 H10' 0.91(2) . . no C10 H10" 0.93(2) . . no C11 H11 0.967(19) . . no C11 H11' 0.958(19) . . no C12 H12 0.949(19) . . no C12 H12' 0.97(2) . . no C13 H13 0.903(18) . . no C13 H13' 0.950(19) . . no C13 H13" 0.99(2) . . no C14 H14 0.94(2) . . no C14 H14' 0.961(19) . . no C14 H14" 0.97(2) . . no C15 H15 0.967(19) . . no C15 H15' 0.94(2) . . no C16 H16 0.90(2) . . no C16 H16' 0.93(3) . . no C16 H16" 0.91(3) . . no C17 H17 0.94(2) . . no C17 H17' 0.93(3) . . no C17 H17" 0.88(3) . . no C18 H18 0.96(2) . . no C18 H18' 0.97(3) . . no C18 H18" 0.911(19) . . no C19 H19 0.942(19) . . no C19 H19' 0.93(2) . . no C20 H20 0.91(2) . . no C20 H20' 0.88(3) . . no C20 H20" 1.04(2) . . no C21 H21 0.92(3) . . no C21 H21' 0.89(2) . . no C21 H21" 0.96(2) . . no C22 H22 0.96(3) . . no C22 H22' 0.92(2) . . no C22 H22" 0.98(2) . . 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 N1 Y1 N2 72.69(5) . . . yes N1 Y1 N4 138.63(5) . . . yes N1 Y1 C15 92.74(6) . . . yes N1 Y1 C19 123.78(6) . . . yes N2 Y1 N4 69.67(5) . . . yes N2 Y1 C15 113.80(6) . . . yes N2 Y1 C19 140.29(6) . . . yes N4 Y1 C15 87.17(6) . . . yes N4 Y1 C19 96.47(6) . . . yes C15 Y1 C19 101.96(6) . . . yes C15 Si1 C16 113.44(9) . . . yes C15 Si1 C17 114.10(10) . . . yes C15 Si1 C18 112.50(10) . . . yes C16 Si1 C17 105.03(13) . . . yes C16 Si1 C18 106.76(12) . . . yes C17 Si1 C18 104.21(12) . . . yes C19 Si2 C20 111.01(11) . . . yes C19 Si2 C21 114.36(11) . . . yes C19 Si2 C22 112.55(11) . . . yes C20 Si2 C21 106.20(13) . . . yes C20 Si2 C22 105.32(13) . . . yes C21 Si2 C22 106.80(10) . . . yes Y1 N1 C4 128.59(11) . . . yes Y1 N1 C5 116.80(12) . . . yes C4 N1 C5 113.63(14) . . . yes Y1 N2 C6 94.83(11) . . . yes Y1 N2 C7 115.75(11) . . . yes Y1 N2 C11 114.17(11) . . . yes C6 N2 C7 110.93(14) . . . yes C6 N2 C11 109.80(13) . . . yes C7 N2 C11 110.33(15) . . . yes C8 N3 C9 109.34(16) . . . yes C8 N3 C10 108.98(17) . . . yes C9 N3 C10 106.82(14) . . . yes Y1 N4 C12 104.45(10) . . . yes Y1 N4 C13 113.59(11) . . . yes Y1 N4 C14 111.62(14) . . . yes C12 N4 C13 110.75(17) . . . yes C12 N4 C14 109.18(14) . . . yes C13 N4 C14 107.22(15) . . . yes N1 C4 C1 106.50(16) . . . yes N1 C4 C2 113.49(18) . . . yes N1 C4 C3 112.42(15) . . . yes C1 C4 C2 108.70(15) . . . no C1 C4 C3 107.05(18) . . . no C2 C4 C3 108.41(16) . . . no N1 C5 C6 110.75(15) . . . yes N2 C6 C5 112.80(15) . . . yes N2 C7 C8 111.80(15) . . . yes N3 C8 C7 112.51(16) . . . yes N2 C11 C12 112.28(16) . . . yes N4 C12 C11 112.38(15) . . . yes Y1 C15 Si1 139.95(10) . . . yes Y1 C19 Si2 130.45(10) . . . yes C4 C1 H1 111.9(13) . . . no C4 C1 H1' 109.5(12) . . . no C4 C1 H1" 111.5(12) . . . no H1 C1 H1' 111.9(17) . . . no H1 C1 H1" 107.8(18) . . . no H1' C1 H1" 103.9(18) . . . no C4 C2 H2 110.6(12) . . . no C4 C2 H2' 113.2(11) . . . no C4 C2 H2" 110.1(12) . . . no H2 C2 H2' 108.6(17) . . . no H2 C2 H2" 107.3(17) . . . no H2' C2 H2" 106.8(16) . . . no C4 C3 H3 111.2(12) . . . no C4 C3 H3' 112.3(13) . . . no C4 C3 H3" 110.6(12) . . . no H3 C3 H3' 108.6(17) . . . no H3 C3 H3" 105.4(17) . . . no H3' C3 H3" 108.5(17) . . . no N1 C5 H5 111.8(10) . . . no N1 C5 H5' 114.2(12) . . . no C6 C5 H5 109.4(12) . . . no C6 C5 H5' 104.2(11) . . . no H5 C5 H5' 106.1(15) . . . no N2 C6 H6 107.0(11) . . . no N2 C6 H6' 105.6(11) . . . no C5 C6 H6 110.4(10) . . . no C5 C6 H6' 111.7(12) . . . no H6 C6 H6' 109.1(14) . . . no N2 C7 H7 108.3(11) . . . no N2 C7 H7' 108.6(10) . . . no C8 C7 H7 108.9(11) . . . no C8 C7 H7' 110.3(11) . . . no H7 C7 H7' 108.9(16) . . . no N3 C8 H8 107.4(11) . . . no N3 C8 H8' 111.6(11) . . . no C7 C8 H8 110.8(10) . . . no C7 C8 H8' 109.5(11) . . . no H8 C8 H8' 104.7(16) . . . no N3 C9 H9 110.1(12) . . . no N3 C9 H9' 108.7(10) . . . no N3 C9 H9" 113.3(12) . . . no H9 C9 H9' 107.2(17) . . . no H9 C9 H9" 106.4(16) . . . no H9' C9 H9" 110.9(15) . . . no N3 C10 H10 112.8(12) . . . no N3 C10 H10' 113.0(12) . . . no N3 C10 H10" 109.9(12) . . . no H10 C10 H10' 107.7(17) . . . no H10 C10 H10" 109.6(18) . . . no H10' C10 H10" 103.4(17) . . . no N2 C11 H11 109.1(11) . . . no N2 C11 H11' 110.3(12) . . . no C12 C11 H11 112.6(11) . . . no C12 C11 H11' 110.3(11) . . . no H11 C11 H11' 101.8(17) . . . no N4 C12 H12 106.6(12) . . . no N4 C12 H12' 109.9(11) . . . no C11 C12 H12 111.6(11) . . . no C11 C12 H12' 110.7(12) . . . no H12 C12 H12' 105.4(16) . . . no N4 C13 H13 107.8(13) . . . no N4 C13 H13' 112.5(12) . . . no N4 C13 H13" 111.4(11) . . . no H13 C13 H13' 107.5(16) . . . no H13 C13 H13" 110.7(16) . . . no H13' C13 H13" 106.9(17) . . . no N4 C14 H14 109.5(12) . . . no N4 C14 H14' 110.2(11) . . . no N4 C14 H14" 111.7(12) . . . no H14 C14 H14' 109.2(17) . . . no H14 C14 H14" 108.5(17) . . . no H14' C14 H14" 107.8(16) . . . no Y1 C15 H15 102.9(12) . . . no Y1 C15 H15' 89.4(13) . . . no Si1 C15 H15 107.6(12) . . . no Si1 C15 H15' 105.5(12) . . . no H15 C15 H15' 107.0(17) . . . no Si1 C16 H16 111.6(13) . . . no Si1 C16 H16' 111.6(17) . . . no Si1 C16 H16" 112.4(18) . . . no H16 C16 H16' 106(2) . . . no H16 C16 H16" 106(2) . . . no H16' C16 H16" 108(2) . . . no Si1 C17 H17 114.3(13) . . . no Si1 C17 H17' 114.0(19) . . . no Si1 C17 H17" 110.1(19) . . . no H17 C17 H17' 109(2) . . . no H17 C17 H17" 106(2) . . . no H17' C17 H17" 103(3) . . . no Si1 C18 H18 110.6(12) . . . no Si1 C18 H18' 110.5(13) . . . no Si1 C18 H18" 109.2(13) . . . no H18 C18 H18' 106.4(17) . . . no H18 C18 H18" 110.5(17) . . . no H18' C18 H18" 109.6(18) . . . no Y1 C19 H19 106.0(12) . . . no Y1 C19 H19' 102.3(12) . . . no Si2 C19 H19 106.1(12) . . . no Si2 C19 H19' 107.3(12) . . . no H19 C19 H19' 101.1(18) . . . no Si2 C20 H20 110.6(19) . . . no Si2 C20 H20' 109.0(19) . . . no Si2 C20 H20" 111.1(12) . . . no H20 C20 H20' 110(2) . . . no H20 C20 H20" 110(2) . . . no H20' C20 H20" 106(2) . . . no Si2 C21 H21 113.6(13) . . . no Si2 C21 H21' 110.8(13) . . . no Si2 C21 H21" 109.7(12) . . . no H21 C21 H21' 106.8(19) . . . no H21 C21 H21" 110.2(19) . . . no H21' C21 H21" 105.5(18) . . . no Si2 C22 H22 110.5(13) . . . no Si2 C22 H22' 111.6(12) . . . no Si2 C22 H22" 113.7(12) . . . no H22 C22 H22' 109.0(18) . . . no H22 C22 H22" 107.6(18) . . . no H22' C22 H22" 104.0(17) . . . 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 N2 Y1 N1 C4 167.52(15) . . . . no N2 Y1 N1 C5 -24.59(12) . . . . no N4 Y1 N1 C4 -167.22(12) . . . . no N4 Y1 N1 C5 0.67(17) . . . . no C15 Y1 N1 C4 -78.38(14) . . . . no C15 Y1 N1 C5 89.50(13) . . . . no C19 Y1 N1 C4 27.97(17) . . . . no C19 Y1 N1 C5 -164.15(12) . . . . no N1 Y1 N2 C6 41.99(9) . . . . no N1 Y1 N2 C7 -74.03(12) . . . . no N1 Y1 N2 C11 156.22(12) . . . . no N4 Y1 N2 C6 -120.51(10) . . . . no N4 Y1 N2 C7 123.47(13) . . . . no N4 Y1 N2 C11 -6.28(11) . . . . no C15 Y1 N2 C6 -43.27(11) . . . . no C15 Y1 N2 C7 -159.29(12) . . . . no C15 Y1 N2 C11 70.96(13) . . . . no C19 Y1 N2 C6 164.43(10) . . . . no C19 Y1 N2 C7 48.41(15) . . . . no C19 Y1 N2 C11 -81.34(14) . . . . no N1 Y1 N4 C12 5.85(15) . . . . no N1 Y1 N4 C13 -114.93(14) . . . . no N1 Y1 N4 C14 123.70(12) . . . . no N2 Y1 N4 C12 31.60(11) . . . . no N2 Y1 N4 C13 -89.18(14) . . . . no N2 Y1 N4 C14 149.45(12) . . . . no C15 Y1 N4 C12 -85.09(11) . . . . no C15 Y1 N4 C13 154.13(14) . . . . no C15 Y1 N4 C14 32.76(12) . . . . no C19 Y1 N4 C12 173.19(11) . . . . no C19 Y1 N4 C13 52.41(14) . . . . no C19 Y1 N4 C14 -68.96(12) . . . . no N1 Y1 C15 Si1 -59.21(16) . . . . no N2 Y1 C15 Si1 13.07(17) . . . . no N4 Y1 C15 Si1 79.38(15) . . . . no C19 Y1 C15 Si1 175.40(15) . . . . no N1 Y1 C19 Si2 -95.25(13) . . . . no N2 Y1 C19 Si2 160.55(9) . . . . no N4 Y1 C19 Si2 94.79(13) . . . . no C15 Y1 C19 Si2 6.32(14) . . . . no C16 Si1 C15 Y1 45.8(2) . . . . no C17 Si1 C15 Y1 166.03(15) . . . . no C18 Si1 C15 Y1 -75.52(18) . . . . no C20 Si2 C19 Y1 64.33(16) . . . . no C21 Si2 C19 Y1 -175.54(12) . . . . no C22 Si2 C19 Y1 -53.43(15) . . . . no Y1 N1 C4 C1 -14.1(2) . . . . no Y1 N1 C4 C2 -133.68(14) . . . . no C5 N1 C4 C3 -65.4(2) . . . . no Y1 N1 C5 C6 0.38(18) . . . . no C4 N1 C5 C6 170.07(15) . . . . no C5 N1 C4 C2 58.1(2) . . . . no Y1 N1 C4 C3 102.83(16) . . . . no C5 N1 C4 C1 177.68(16) . . . . no Y1 N2 C6 C5 -58.87(15) . . . . no C11 N2 C7 C8 79.83(19) . . . . no Y1 N2 C11 C12 -20.34(18) . . . . no C6 N2 C11 C12 84.70(18) . . . . no C7 N2 C11 C12 -152.74(15) . . . . no Y1 N2 C7 C8 -51.74(18) . . . . no C7 N2 C6 C5 61.1(2) . . . . no C11 N2 C6 C5 -176.72(15) . . . . no C6 N2 C7 C8 -158.27(16) . . . . no C9 N3 C8 C7 75.92(19) . . . . no C10 N3 C8 C7 -167.66(15) . . . . no Y1 N4 C12 C11 -56.46(17) . . . . no C13 N4 C12 C11 66.2(2) . . . . no C14 N4 C12 C11 -175.97(17) . . . . no N1 C5 C6 N2 45.8(2) . . . . no N2 C7 C8 N3 58.8(2) . . . . no N2 C11 C12 N4 54.3(2) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Y1 N3 2.8703(15) . . no Y1 C9 3.504(2) . . no Y1 C10 3.833(2) . . no Y1 H1 3.24(2) . . no Y1 H1' 3.03(2) . . no Y1 H8 3.880(19) . . no Y1 H9 3.396(19) . . no Y1 H9' 3.512(17) . . no Y1 H10' 3.909(19) . . no Y1 H10" 3.90(2) . . no Si1 H6' 3.50(2) . . no Si1 H14 3.42(2) . . no N1 C9 3.424(3) . . no N3 C19 3.366(3) . . no N3 Y1 2.8703(15) . . no N1 H9 2.768(19) . . no N1 H7 2.879(19) . . no C9 Y1 3.504(2) . . no C9 N1 3.424(3) . . no C10 C19 3.428(3) . . no C10 Y1 3.833(2) . . no C19 C10 3.428(3) . . no C19 N3 3.366(3) . . no C1 H9' 3.060(17) . 2_555 no C2 H9 3.08(2) . . no C2 H5 2.735(19) . . no C3 H16' 3.04(2) . . no C3 H22" 3.03(2) . 1_545 no C3 H5' 2.72(2) . . no C5 H7 2.500(19) . . no C5 H3' 2.78(2) . . no C5 H2' 2.745(19) . . no C6 H22 3.05(2) . 1_445 no C6 H12 2.990(18) . . no C6 H16" 3.09(3) . . no C7 H5 2.815(19) . . no C7 H9 2.77(2) . . no C8 H13' 2.940(19) . . no C8 H11 2.738(17) . . no C9 H1 3.06(2) . . no C9 H7 2.769(18) . . no C10 H13' 3.077(19) . . no C10 H19' 2.96(2) . . no C11 H13' 2.713(19) . . no C11 H8 2.864(17) . . no C12 H6' 2.812(19) . . no C13 H11 2.792(19) . . no C13 H10" 2.97(2) . . no C14 H15 2.93(2) . . no C15 H14 2.77(2) . . no C18 H14 2.94(2) . . no C18 H12 3.089(19) . . no C19 H10' 2.94(2) . . no C20 H8 2.923(19) . 1_655 no H1 Y1 3.24(2) . . no H1 C9 3.06(2) . . no H1 H2 2.52(3) . . no H1 H9' 2.44(3) . . no H1 H9' 2.51(3) . 2_555 no H1' Y1 3.03(2) . . no H1' H3 2.41(3) . . no H1" H2" 2.52(3) . . no H1" H3" 2.47(3) . . no H2 H1 2.52(3) . . no H2 H9 2.36(3) . . no H2' C5 2.745(19) . . no H2' H5 2.29(3) . . no H2" H1" 2.52(3) . . no H2" H3" 2.44(3) . . no H3 H1' 2.41(3) . . no H3 H16' 2.50(3) . . no H3' C5 2.78(2) . . no H3' H5' 2.21(3) . . no H3' H13 2.59(3) . 1_545 no H3" H1" 2.47(3) . . no H3" H2" 2.44(3) . . no H3" H22" 2.44(3) . 1_545 no H5 C2 2.735(19) . . no H5 C7 2.815(19) . . no H5 H2' 2.29(3) . . no H5 H7 2.11(3) . . no H5 H22 2.49(3) . 1_445 no H5' C3 2.72(2) . . no H5' H3' 2.21(3) . . no H5' H16" 2.56(3) . . no H6 H11' 2.31(3) . . no H6 H22 2.36(3) . 1_445 no H6 H18 2.48(3) . 2_556 no H6' Si1 3.50(2) . . no H6' C12 2.812(19) . . no H6' H11' 2.58(3) . . no H6' H12 2.35(3) . . no H6' H16" 2.40(4) . . no H7 N1 2.879(19) . . no H7 C5 2.500(19) . . no H7 C9 2.769(18) . . no H7 H5 2.11(3) . . no H7 H9 2.23(3) . . no H7 H21 2.59(3) . 1_445 no H7' H11 2.34(2) . . no H7' H11' 2.57(3) . . no H8 Y1 3.880(19) . . no H8 C11 2.864(17) . . no H8 C20 2.923(19) . 1_455 no H8 H10" 2.33(3) . . no H8 H11 2.25(2) . . no H8 H13' 2.24(3) . . no H8 H20" 2.46(3) . 1_455 no H8' H9" 2.39(3) . . no H8' H10 2.52(3) . . no H9 Y1 3.396(19) . . no H9 N1 2.768(19) . . no H9 C2 3.08(2) . . no H9 C7 2.77(2) . . no H9 H2 2.36(3) . . no H9 H7 2.23(3) . . no H9' Y1 3.512(17) . . no H9' H1 2.44(3) . . no H9' H10' 2.41(3) . . no H9' C1 3.060(17) . 2_555 no H9' H1 2.51(3) . 2_555 no H9" H8' 2.39(3) . . no H9" H10 2.47(3) . . no H10 H8' 2.52(3) . . no H10 H9" 2.47(3) . . no H10' Y1 3.909(19) . . no H10' C19 2.94(2) . . no H10' H9' 2.41(3) . . no H10' H19 2.49(3) . . no H10' H19' 2.50(3) . . no H10" Y1 3.90(2) . . no H10" C13 2.97(2) . . no H10" H8 2.33(3) . . no H10" H13' 2.37(3) . . no H11 C8 2.738(17) . . no H11 C13 2.792(19) . . no H11 H7' 2.34(2) . . no H11 H8 2.25(2) . . no H11 H13' 2.29(3) . . no H11' H6 2.31(3) . . no H11' H6' 2.58(3) . . no H11' H7' 2.57(3) . . no H11' H17" 2.59(4) . 1_455 no H12 C6 2.990(18) . . no H12 C18 3.089(19) . . no H12 H6' 2.35(3) . . no H12 H14 2.29(3) . . no H12 H18' 2.38(3) . . no H12' H13" 2.44(3) . . no H12' H14" 2.48(3) . . no H13 H3' 2.59(3) . 1_565 no H13 H14' 2.37(3) . . no H13' C8 2.940(19) . . no H13' C10 3.077(19) . . no H13' C11 2.713(19) . . no H13' H8 2.24(3) . . no H13' H10" 2.37(3) . . no H13' H11 2.29(3) . . no H13" H12' 2.44(3) . . no H13" H14" 2.40(3) . . no H14 Si1 3.42(2) . . no H14 C15 2.77(2) . . no H14 C18 2.94(2) . . no H14 H12 2.29(3) . . no H14 H15 2.36(3) . . no H14 H18" 2.43(3) . . no H14' H13 2.37(3) . . no H14" H12' 2.48(3) . . no H14" H13" 2.40(3) . . no H15 C14 2.93(2) . . no H15 H14 2.36(3) . . no H15 H22' 2.35(3) . . no H16' C3 3.04(2) . . no H16' H3 2.50(3) . . no H16" C6 3.09(3) . . no H16" H5' 2.56(3) . . no H16" H6' 2.40(4) . . no H17' H18" 2.53(3) . 2_666 no H17" H11' 2.59(4) . 1_655 no H18 H6 2.48(3) . 2_556 no H18' H12 2.38(3) . . no H18" H14 2.43(3) . . no H18" H17' 2.53(3) . 2_666 no H19 H10' 2.49(3) . . no H19' C10 2.96(2) . . no H19' H10' 2.50(3) . . no H20" H8 2.46(3) . 1_655 no H21 H7 2.59(3) . 1_665 no H22 C6 3.05(2) . 1_665 no H22 H5 2.49(3) . 1_665 no H22 H6 2.36(3) . 1_665 no H22' H15 2.35(3) . . no H22" C3 3.03(2) . 1_565 no H22" H3" 2.44(3) . 1_565 no #===End of Crystallographic Information File # CIF-file generated for C23H48N5SiY (6) CP594 #============================================================================== data_global #============================================================================== # 0. AUDIT DETAILS _audit_creation_date '2001-03-15 13:48:20' _audit_creation_method 'PLATON
option' _audit_update_record ; ? ; #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondence ; Drs. A. Meetsma ; _publ_contact_author_address # Address of author for correspondence ; Crystal Structure Center, Inorganic Solid State Chemistry Laboratory Chemical Physics, Materials Science Center, Groningen University, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; _publ_contact_author_email A.Meetsma@fwn.rug.nl _publ_contact_author_fax '+31 50 3634441' _publ_contact_author_phone '+31 50 3634368' _publ_requested_journal 'Organometallics' # Publication choise FI FM FO CI CM CO _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission : 2003-12-08 Consider this CIF submission for deposition of the first X-ray structure of a manuscript to be submitted to : Organometallics (Our Compound_Identification_Code : CP594) ; #=============================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Meetsma, Auke' ; ? # author related footnote ; ; Crystal Structure Center, Inorganic Solid State Chemistry Laboratory Chemical Physics, Materials Science Center, Groningen University, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; #=============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; # Insert blank lines between paragraphs _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; # Insert blank lines between references _publ_section_references ; Beurskens, P.T., Beurskens, G., Gelder, R. de Garc\'ia-Granda, S. Gould, R.O. Isra\"el, & 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, SAINT, SADABS, XPREP and SHELXTL/NT. Software Reference Manual Bruker AXS Inc. Madison, Wisconsin, USA. International Tables for Crystallography (1983). Vol. A. Space-group symmetry, edited by T. Hahn. Dordrecht: Reidel. (Present distributor Kluwer Academic Publishers, Dordrecht). International Tables for Crystallography (1992). Vol. C. Edited by A.J.C Wilson, Kluwer Academic Publishers, Dordrecht, The Netherlands. Le Page, Y. (1987). J. Appl. Cryst. 20, 264-269. Le Page, Y. (1988). J. Appl. Cryst. 21, 983-984. Meetsma, A. (2000). Extended version of the program PLUTO. Groningen University, The Netherlands. (unpublished). Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany, 1997. Sheldrick, G.M. SADABS. Version 2. Empirical Absorption Correction Program. University of G\"ottingen, Germany, 2001 Spek, A.L. (1988). J. Appl. Cryst. 21, 578-579. Spek, A.L. (1990). Acta Cryst. A46, C-34. Spek, A.L. (1997). HELENA, Program for Datareduction, Utrecht University, The Netherlands. Spek, A.L. (1994). Am. Crystallogr. Assoc.-Abstracts, 22, 66. ; _publ_section_figure_captions ; Fig. 1. Chemical structural diagram (scheme 1) of the title compound Fig. 2. Perspective PLUTO drawing of the molecule illustrating the configuration and the adopted numbering scheme. Fig. 3. Molecular packing viewed down unit cell axes. Fig. 4. Perspective ORTEP drawing of the title compound. All non-hydrogen atoms are represented by thermal vibrational ellipsoids drawn to encompass 50% of the electron density. The hydrogen atoms are drawn with an arbitrary radius. ; #=============================================================================== data_c23h48n5 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H48 N5 Si Y' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C23 H48 N5 Si Y' _chemical_formula_weight 511.66 _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' 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' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 14.7891(6) _cell_length_b 9.4573(4) _cell_length_c 19.2445(8) _cell_angle_alpha 90 _cell_angle_beta 91.167(1) _cell_angle_gamma 90 _cell_volume 2691.07(19) _cell_formula_units_Z 4 _cell_measurement_temperature 95 _cell_measurement_reflns_used 7104 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 29.03 _cell_special_details ; The final unit cell was obtained from the xyz centroids of 1108 reflections after integration using the SAINT software package (Bruker, 2000). Reduced cell calculations did not indicate any higher metric lattice symmetry and examination of the final atomic coordinates of the structure did not yield extra symmetry elements (Spek, 1988; Le Page 1987, 1988) ; _exptl_crystal_description 'thick needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 2.230 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_process_details 'SADABS (Sheldrick, Bruker, 2000)' _exptl_absorpt_correction_T_min 0.5543 _exptl_absorpt_correction_T_max 0.7454 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 95(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine focus sealed Siemens Mo tube ' _diffrn_radiation_monochromator 'parallel mounted graphite' _diffrn_radiation_detector ; CCD area-detector ; _diffrn_measurement_device_type ; Bruker Smart Apex ; _diffrn_measurement_method 'phi and omega scans' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temparature unit (KRYOFLEX, (Bruker, 2000)). ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? 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 25856 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 29.81 _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 29.81 _diffrn_measured_fraction_theta_full 0.884 _diffrn_reflns_reduction_process ; Intensity data were corrected for Lorentz and polarization effects, decay and absorption and reduced to F~o~^2^ using SAINT (Bruker, 2000) and SABABS (Sheldrick, 2000) Intensity data were corrected for Lorentz and polarization effects, scale variation, for absorption and reduced to F~o~^2^ ; # number of unique reflections _reflns_number_total 7205 _reflns_number_gt 5715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker Version 5.168, 2000' _computing_cell_refinement 'SAINT, Bruker Version 6.02A, 2000' _computing_data_reduction 'XPREP, Bruker Version 5.1/NT, 2000' _computing_structure_solution ; DIRDIF-99 (Beurskens et al., 1999) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTO (Meetsma, 2000) PLATON (Spek, 1994, 1996) ; _computing_publication_material ; PLATON (Spek, 1990) SHELXL (Sheldrick, 1997) ; #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_details calc _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.0787P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 7205 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.528 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.073 #=============================================================================== # 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 Y Y Uani 0.25130(1) 0.10076(2) 0.42060(1) 1.000 0.0132(1) . . Si Si Uani 0.09070(3) -0.09790(5) 0.29494(3) 1.000 0.0164(2) . . N1 N Uani 0.28964(10) 0.00575(16) 0.52330(8) 1.000 0.0177(4) . . N2 N Uani 0.34752(10) 0.28043(16) 0.48460(8) 1.000 0.0197(5) . . N3 N Uani 0.32805(10) 0.26396(16) 0.33383(8) 1.000 0.0184(4) . . N4 N Uani 0.14961(10) 0.31058(16) 0.47328(8) 1.000 0.0187(4) . . N5 N Uani 0.35723(9) -0.01973(17) 0.35826(8) 1.000 0.0174(5) . . C1 C Uani 0.16563(16) -0.1596(3) 0.51767(13) 1.000 0.0298(7) . . C2 C Uani 0.31346(16) -0.2435(2) 0.56412(12) 1.000 0.0260(7) . . C3 C Uani 0.22046(19) -0.0797(3) 0.63358(12) 1.000 0.0321(7) . . C4 C Uani 0.24944(13) -0.1154(2) 0.55946(10) 1.000 0.0202(5) . . C5 C Uani 0.36503(14) 0.0681(2) 0.56181(11) 1.000 0.0245(6) . . C6 C Uani 0.41214(13) 0.1807(2) 0.51971(12) 1.000 0.0247(6) . . C7 C Uani 0.39720(13) 0.3770(2) 0.43872(11) 1.000 0.0237(6) . . C8 C Uani 0.41380(12) 0.3101(2) 0.36856(11) 1.000 0.0232(6) . . C9 C Uani 0.29478(14) 0.3602(2) 0.53599(11) 1.000 0.0243(6) . . C10 C Uani 0.20919(14) 0.4211(2) 0.50335(12) 1.000 0.0229(6) . . C11 C Uani 0.09983(15) 0.2405(2) 0.52917(11) 1.000 0.0243(6) . . C12 C Uani 0.08182(14) 0.3789(2) 0.42665(11) 1.000 0.0231(6) . . C13 C Uani 0.27779(14) 0.3887(2) 0.30765(12) 1.000 0.0250(6) . . C14 C Uani 0.34729(13) 0.1717(2) 0.27325(10) 1.000 0.0209(6) . . C15 C Uani 0.39461(12) 0.0343(2) 0.29311(10) 1.000 0.0193(5) . . C16 C Uani 0.38670(13) -0.0750(2) 0.23643(11) 1.000 0.0229(6) . . C17 C Uani 0.40795(12) -0.2078(2) 0.25361(11) 1.000 0.0247(6) . . C18 C Uani 0.42257(13) -0.2435(2) 0.32570(11) 1.000 0.0232(6) . . C19 C Uani 0.38783(12) -0.1522(2) 0.37312(11) 1.000 0.0204(6) . . C20 C Uani 0.10887(12) 0.0403(2) 0.36075(10) 1.000 0.0181(6) . . C21 C Uani 0.13197(15) -0.0418(3) 0.20747(11) 1.000 0.0246(7) . . C22 C Uani -0.03191(13) -0.1427(3) 0.27976(12) 1.000 0.0248(6) . . C23 C Uani 0.14818(15) -0.2686(2) 0.31904(12) 1.000 0.0263(7) . . H1 H Uiso 0.1408(15) -0.248(3) 0.5360(12) 1.000 0.037(6) . . H1' H Uiso 0.1174(16) -0.085(2) 0.5216(12) 1.000 0.033(6) . . H1" H Uiso 0.1812(15) -0.179(2) 0.4722(13) 1.000 0.034(7) . . H2 H Uiso 0.2848(14) -0.320(2) 0.5892(11) 1.000 0.023(5) . . H2' H Uiso 0.3288(16) -0.280(3) 0.5199(13) 1.000 0.040(7) . . H2" H Uiso 0.3671(16) -0.225(2) 0.5864(12) 1.000 0.037(7) . . H3 H Uiso 0.1878(15) -0.156(2) 0.6544(12) 1.000 0.033(6) . . H3' H Uiso 0.2702(16) -0.063(2) 0.6629(13) 1.000 0.032(6) . . H3" H Uiso 0.1799(17) -0.001(3) 0.6325(13) 1.000 0.049(7) . . H5 H Uiso 0.3459(15) 0.105(2) 0.6056(13) 1.000 0.029(6) . . H5' H Uiso 0.4120(13) 0.005(2) 0.5731(10) 1.000 0.018(5) . . H6 H Uiso 0.4487(13) 0.133(2) 0.4815(11) 1.000 0.017(5) . . H6' H Uiso 0.4535(14) 0.230(2) 0.5481(11) 1.000 0.028(6) . . H7 H Uiso 0.3629(14) 0.462(2) 0.4337(11) 1.000 0.030(6) . . H7' H Uiso 0.4559(14) 0.4026(19) 0.4602(11) 1.000 0.018(5) . . H8 H Uiso 0.4523(12) 0.229(2) 0.3747(10) 1.000 0.016(5) . . H8' H Uiso 0.4439(14) 0.375(2) 0.3399(12) 1.000 0.022(5) . . H9 H Uiso 0.2787(13) 0.295(2) 0.5737(10) 1.000 0.015(5) . . H9' H Uiso 0.3310(14) 0.437(2) 0.5561(11) 1.000 0.026(6) . . H10 H Uiso 0.2250(13) 0.483(2) 0.4691(10) 1.000 0.018(5) . . H10' H Uiso 0.1755(14) 0.478(2) 0.5384(12) 1.000 0.032(6) . . H11 H Uiso 0.1400(14) 0.197(2) 0.5591(12) 1.000 0.027(6) . . H11' H Uiso 0.0650(13) 0.308(2) 0.5562(10) 1.000 0.022(5) . . H11" H Uiso 0.0605(14) 0.171(2) 0.5091(12) 1.000 0.029(6) . . H12 H Uiso 0.1116(16) 0.419(2) 0.3898(13) 1.000 0.033(7) . . H12' H Uiso 0.0485(14) 0.457(2) 0.4510(11) 1.000 0.027(6) . . H12" H Uiso 0.0410(14) 0.310(2) 0.4092(11) 1.000 0.026(6) . . H13 H Uiso 0.2234(14) 0.361(2) 0.2840(11) 1.000 0.024(6) . . H13' H Uiso 0.2642(13) 0.453(2) 0.3452(11) 1.000 0.018(5) . . H13" H Uiso 0.3117(15) 0.441(2) 0.2733(12) 1.000 0.036(7) . . H14 H Uiso 0.2866(12) 0.1475(19) 0.2514(10) 1.000 0.011(5) . . H14' H Uiso 0.3824(14) 0.224(2) 0.2405(11) 1.000 0.027(6) . . H15 H Uiso 0.4612(14) 0.054(2) 0.3009(10) 1.000 0.024(5) . . H16 H Uiso 0.3682(14) -0.050(2) 0.1912(12) 1.000 0.032(6) . . H17 H Uiso 0.4061(12) -0.281(2) 0.2199(10) 1.000 0.020(5) . . H18 H Uiso 0.4388(14) -0.337(3) 0.3411(12) 1.000 0.030(6) . . H19 H Uiso 0.3800(13) -0.183(2) 0.4207(11) 1.000 0.022(5) . . H20 H Uiso 0.0909(15) 0.125(2) 0.3410(12) 1.000 0.030(6) . . H20' H Uiso 0.0692(16) 0.022(3) 0.3946(13) 1.000 0.042(7) . . H21 H Uiso 0.1093(15) -0.101(2) 0.1729(12) 1.000 0.026(6) . . H21' H Uiso 0.1132(19) 0.051(3) 0.1955(14) 1.000 0.059(8) . . H21" H Uiso 0.1940(18) -0.040(3) 0.2063(12) 1.000 0.044(7) . . H22 H Uiso -0.0651(16) -0.061(3) 0.2656(13) 1.000 0.040(7) . . H22' H Uiso -0.0405(16) -0.214(3) 0.2450(14) 1.000 0.050(8) . . H22" H Uiso -0.0594(16) -0.170(3) 0.3215(14) 1.000 0.040(7) . . H23 H Uiso 0.2150(17) -0.256(2) 0.3237(12) 1.000 0.038(6) . . H23' H Uiso 0.1353(16) -0.339(3) 0.2837(13) 1.000 0.040(7) . . H23" H Uiso 0.1227(16) -0.308(3) 0.3613(14) 1.000 0.043(7) . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.0145(1) 0.0129(1) 0.0122(1) -0.0012(1) -0.0007(1) 0.0008(1) Si 0.0179(2) 0.0156(3) 0.0156(3) -0.0015(2) -0.0015(2) 0.0003(2) N1 0.0225(7) 0.0163(8) 0.0143(8) -0.0010(7) -0.0017(6) 0.0021(6) N2 0.0207(7) 0.0166(8) 0.0215(9) -0.0025(7) -0.0037(6) 0.0002(6) N3 0.0177(7) 0.0177(8) 0.0197(8) 0.0000(7) 0.0002(6) -0.0013(6) N4 0.0214(7) 0.0159(8) 0.0187(8) -0.0012(7) -0.0008(6) 0.0028(6) N5 0.0174(7) 0.0197(9) 0.0152(8) -0.0008(7) 0.0001(6) 0.0020(6) C1 0.0348(12) 0.0243(12) 0.0301(13) 0.0096(10) -0.0032(10) -0.0060(10) C2 0.0366(12) 0.0181(11) 0.0232(12) 0.0010(9) 0.0002(10) 0.0059(9) C3 0.0513(14) 0.0257(13) 0.0196(11) 0.0027(10) 0.0085(10) 0.0080(11) C4 0.0293(9) 0.0180(10) 0.0134(9) 0.0005(8) -0.0004(7) 0.0031(8) C5 0.0299(10) 0.0235(11) 0.0198(11) -0.0023(8) -0.0092(8) 0.0059(8) C6 0.0219(9) 0.0230(11) 0.0287(12) -0.0028(9) -0.0101(9) -0.0003(8) C7 0.0217(9) 0.0192(11) 0.0299(12) -0.0043(9) -0.0034(8) -0.0040(8) C8 0.0176(9) 0.0210(10) 0.0312(12) 0.0014(9) 0.0021(8) -0.0048(8) C9 0.0312(10) 0.0190(10) 0.0225(11) -0.0071(9) -0.0037(9) 0.0014(8) C10 0.0291(10) 0.0168(11) 0.0228(11) -0.0036(9) 0.0015(8) 0.0032(8) C11 0.0284(10) 0.0227(11) 0.0220(11) 0.0005(9) 0.0055(9) 0.0057(9) C12 0.0245(9) 0.0215(11) 0.0234(11) -0.0002(9) -0.0001(8) 0.0073(8) C13 0.0284(10) 0.0228(11) 0.0237(11) 0.0044(10) 0.0001(9) 0.0028(9) C14 0.0231(9) 0.0233(11) 0.0163(10) 0.0008(8) 0.0038(8) -0.0014(8) C15 0.0158(8) 0.0238(10) 0.0184(10) -0.0018(8) 0.0032(7) -0.0008(7) C16 0.0214(9) 0.0315(12) 0.0159(10) -0.0050(9) 0.0026(8) 0.0032(8) C17 0.0196(9) 0.0291(12) 0.0256(11) -0.0110(10) 0.0019(8) 0.0035(8) C18 0.0225(9) 0.0211(11) 0.0259(11) -0.0030(9) -0.0003(8) 0.0057(8) C19 0.0189(9) 0.0230(10) 0.0192(10) -0.0001(8) -0.0017(7) 0.0045(7) C20 0.0197(9) 0.0172(10) 0.0172(10) -0.0011(8) -0.0014(7) 0.0019(7) C21 0.0300(11) 0.0233(12) 0.0206(11) -0.0034(9) 0.0021(9) -0.0022(9) C22 0.0214(9) 0.0286(12) 0.0244(12) -0.0063(10) -0.0007(9) -0.0038(8) C23 0.0350(12) 0.0181(11) 0.0255(12) -0.0029(9) -0.0044(9) 0.0043(9) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y N1 2.2337(15) . . yes Y N2 2.5215(15) . . yes Y N3 2.5566(15) . . yes Y N4 2.6998(15) . . yes Y N5 2.2953(15) . . yes Y C20 2.4478(18) . . yes Si C20 1.836(2) . . yes Si C21 1.879(2) . . yes Si C22 1.879(2) . . yes Si C23 1.878(2) . . yes N1 C4 1.472(2) . . yes N1 C5 1.451(3) . . yes N2 C6 1.494(3) . . yes N2 C7 1.476(2) . . yes N2 C9 1.479(3) . . yes N3 C8 1.487(2) . . yes N3 C13 1.477(2) . . yes N3 C14 1.488(2) . . yes N4 C10 1.477(3) . . yes N4 C11 1.473(3) . . yes N4 C12 1.480(3) . . yes N5 C15 1.472(2) . . yes N5 C19 1.360(2) . . yes C1 C4 1.522(3) . . no C2 C4 1.539(3) . . no C3 C4 1.535(3) . . no C5 C6 1.516(3) . . no C7 C8 1.516(3) . . no C9 C10 1.515(3) . . no C14 C15 1.521(3) . . no C15 C16 1.506(3) . . no C16 C17 1.335(3) . . no C17 C18 1.440(3) . . no C18 C19 1.364(3) . . no C1 H1 0.98(3) . . no C1 H1' 1.01(2) . . no C1 H1" 0.93(2) . . no C2 H2 0.97(2) . . no C2 H2' 0.95(3) . . no C2 H2" 0.91(2) . . no C3 H3 0.96(2) . . no C3 H3' 0.93(2) . . no C3 H3" 0.96(3) . . no C5 H5 0.96(2) . . no C5 H5' 0.938(19) . . no C6 H6 1.03(2) . . no C6 H6' 0.94(2) . . no C7 H7 0.954(19) . . no C7 H7' 0.98(2) . . no C8 H8 0.961(19) . . no C8 H8' 0.94(2) . . no C9 H9 0.985(19) . . no C9 H9' 0.98(2) . . no C10 H10 0.915(19) . . no C10 H10' 1.00(2) . . no C11 H11 0.92(2) . . no C11 H11' 0.977(19) . . no C11 H11" 0.95(2) . . no C12 H12 0.92(2) . . no C12 H12' 1.01(2) . . no C12 H12" 0.95(2) . . no C13 H13 0.95(2) . . no C13 H13' 0.97(2) . . no C13 H13" 0.97(2) . . no C14 H14 1.010(18) . . no C14 H14' 0.96(2) . . no C15 H15 1.01(2) . . no C16 H16 0.94(2) . . no C17 H17 0.949(19) . . no C18 H18 0.96(3) . . no C19 H19 0.97(2) . . no C20 H20 0.92(2) . . no C20 H20' 0.90(2) . . no C21 H21 0.93(2) . . no C21 H21' 0.95(3) . . no C21 H21" 0.92(3) . . no C22 H22 0.95(3) . . no C22 H22' 0.96(3) . . no C22 H22" 0.94(3) . . no C23 H23 1.00(3) . . no C23 H23' 0.97(3) . . no C23 H23" 0.98(3) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y N2 73.04(5) . . . yes N1 Y N3 135.45(5) . . . yes N1 Y N4 95.55(5) . . . yes N1 Y N5 95.69(5) . . . yes N1 Y C20 121.53(6) . . . yes N2 Y N3 70.04(5) . . . yes N2 Y N4 68.56(5) . . . yes N2 Y N5 101.86(5) . . . yes N2 Y C20 149.20(6) . . . yes N3 Y N4 93.42(5) . . . yes N3 Y N5 68.99(5) . . . yes N3 Y C20 102.88(6) . . . yes N4 Y N5 162.26(5) . . . yes N4 Y C20 82.40(5) . . . yes N5 Y C20 103.18(6) . . . yes C20 Si C21 111.80(10) . . . yes C20 Si C22 113.26(10) . . . yes C20 Si C23 112.48(9) . . . yes C21 Si C22 104.74(10) . . . yes C21 Si C23 108.08(11) . . . yes C22 Si C23 105.96(11) . . . yes Y N1 C4 129.32(12) . . . yes Y N1 C5 117.83(12) . . . yes C4 N1 C5 112.85(15) . . . yes Y N2 C6 98.33(10) . . . yes Y N2 C7 114.05(11) . . . yes Y N2 C9 111.74(11) . . . yes C6 N2 C7 109.84(14) . . . yes C6 N2 C9 111.15(15) . . . yes C7 N2 C9 111.10(14) . . . yes Y N3 C8 105.64(11) . . . yes Y N3 C13 118.54(11) . . . yes Y N3 C14 104.61(10) . . . yes C8 N3 C13 109.73(14) . . . yes C8 N3 C14 110.44(14) . . . yes C13 N3 C14 107.69(15) . . . yes Y N4 C10 109.55(11) . . . yes Y N4 C11 103.53(11) . . . yes Y N4 C12 117.95(11) . . . yes C10 N4 C11 109.59(15) . . . yes C10 N4 C12 108.65(14) . . . yes C11 N4 C12 107.25(15) . . . yes Y N5 C15 123.02(11) . . . yes Y N5 C19 125.10(12) . . . yes C15 N5 C19 111.69(15) . . . yes N1 C4 C1 107.24(17) . . . yes N1 C4 C2 112.72(16) . . . yes N1 C4 C3 113.02(17) . . . yes C1 C4 C2 107.94(18) . . . no C1 C4 C3 108.15(18) . . . no C2 C4 C3 107.58(18) . . . no N1 C5 C6 111.66(17) . . . yes N2 C6 C5 112.85(16) . . . yes N2 C7 C8 111.48(15) . . . yes N3 C8 C7 111.77(15) . . . yes N2 C9 C10 111.36(17) . . . yes N4 C10 C9 112.33(15) . . . yes N3 C14 C15 113.48(15) . . . yes N5 C15 C14 109.37(15) . . . yes N5 C15 C16 110.72(15) . . . yes C14 C15 C16 112.08(16) . . . no C15 C16 C17 116.88(18) . . . no C16 C17 C18 119.30(19) . . . no C17 C18 C19 116.42(17) . . . no N5 C19 C18 124.78(19) . . . yes Y C20 Si 127.11(9) . . . yes C4 C1 H1 110.5(13) . . . no C4 C1 H1' 109.8(13) . . . no C4 C1 H1" 109.7(14) . . . no H1 C1 H1' 107.4(19) . . . no H1 C1 H1" 105.8(19) . . . no H1' C1 H1" 113.5(19) . . . no C4 C2 H2 109.9(12) . . . no C4 C2 H2' 113.1(16) . . . no C4 C2 H2" 113.9(12) . . . no H2 C2 H2' 107(2) . . . no H2 C2 H2" 107.1(18) . . . no H2' C2 H2" 106(2) . . . no C4 C3 H3 112.0(13) . . . no C4 C3 H3' 111.6(15) . . . no C4 C3 H3" 109.8(15) . . . no H3 C3 H3' 105.8(19) . . . no H3 C3 H3" 106(2) . . . no H3' C3 H3" 112(2) . . . no N1 C5 H5 111.0(13) . . . no N1 C5 H5' 114.7(12) . . . no C6 C5 H5 111.1(12) . . . no C6 C5 H5' 103.0(12) . . . no H5 C5 H5' 105.0(18) . . . no N2 C6 H6 107.2(11) . . . no N2 C6 H6' 110.7(12) . . . no C5 C6 H6 109.2(11) . . . no C5 C6 H6' 109.9(13) . . . no H6 C6 H6' 106.8(17) . . . no N2 C7 H7 108.2(13) . . . no N2 C7 H7' 110.3(12) . . . no C8 C7 H7 110.9(13) . . . no C8 C7 H7' 108.6(12) . . . no H7 C7 H7' 107.3(16) . . . no N3 C8 H8 108.6(11) . . . no N3 C8 H8' 109.7(13) . . . no C7 C8 H8 109.3(12) . . . no C7 C8 H8' 109.7(13) . . . no H8 C8 H8' 107.8(16) . . . no N2 C9 H9 108.2(11) . . . no N2 C9 H9' 110.6(12) . . . no C10 C9 H9 109.3(11) . . . no C10 C9 H9' 109.2(12) . . . no H9 C9 H9' 108.2(17) . . . no N4 C10 H10 109.2(12) . . . no N4 C10 H10' 110.0(12) . . . no C9 C10 H10 108.5(12) . . . no C9 C10 H10' 110.3(13) . . . no H10 C10 H10' 106.2(17) . . . no N4 C11 H11 109.5(13) . . . no N4 C11 H11' 111.8(11) . . . no N4 C11 H11" 108.9(14) . . . no H11 C11 H11' 107.5(18) . . . no H11 C11 H11" 109.1(18) . . . no H11' C11 H11" 110.0(17) . . . no N4 C12 H12 108.5(15) . . . no N4 C12 H12' 111.7(12) . . . no N4 C12 H12" 109.5(12) . . . no H12 C12 H12' 107.5(17) . . . no H12 C12 H12" 108.7(19) . . . no H12' C12 H12" 110.8(17) . . . no N3 C13 H13 110.9(12) . . . no N3 C13 H13' 110.9(12) . . . no N3 C13 H13" 112.0(12) . . . no H13 C13 H13' 110.1(17) . . . no H13 C13 H13" 104.9(18) . . . no H13' C13 H13" 107.8(17) . . . no N3 C14 H14 106.1(11) . . . no N3 C14 H14' 109.0(12) . . . no C15 C14 H14 108.2(10) . . . no C15 C14 H14' 110.6(12) . . . no H14 C14 H14' 109.3(17) . . . no N5 C15 H15 108.6(11) . . . no C14 C15 H15 108.8(11) . . . no C16 C15 H15 107.2(11) . . . no C15 C16 H16 121.1(12) . . . no C17 C16 H16 122.0(12) . . . no C16 C17 H17 120.9(12) . . . no C18 C17 H17 119.3(12) . . . no C17 C18 H18 123.0(14) . . . no C19 C18 H18 118.1(14) . . . no N5 C19 H19 115.4(11) . . . no C18 C19 H19 119.7(11) . . . no Y C20 H20 103.2(14) . . . no Y C20 H20' 105.7(16) . . . no Si C20 H20 107.3(14) . . . no Si C20 H20' 105.9(17) . . . no H20 C20 H20' 106(2) . . . no Si C21 H21 110.7(14) . . . no Si C21 H21' 112.4(17) . . . no Si C21 H21" 111.7(15) . . . no H21 C21 H21' 107(2) . . . no H21 C21 H21" 110(2) . . . no H21' C21 H21" 105(2) . . . no Si C22 H22 110.6(15) . . . no Si C22 H22' 112.4(14) . . . no Si C22 H22" 111.1(15) . . . no H22 C22 H22' 108(2) . . . no H22 C22 H22" 104(2) . . . no H22' C22 H22" 110(2) . . . no Si C23 H23 111.2(11) . . . no Si C23 H23' 109.6(16) . . . no Si C23 H23" 110.7(16) . . . no H23 C23 H23' 109.0(19) . . . no H23 C23 H23" 111.6(19) . . . no H23' C23 H23" 104(2) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Y N1 C4 163.02(16) . . . . no N2 Y N1 C5 -17.42(12) . . . . no N3 Y N1 C4 -161.94(13) . . . . no N3 Y N1 C5 17.63(16) . . . . no N4 Y N1 C4 97.45(15) . . . . no N4 Y N1 C5 -82.98(13) . . . . no N5 Y N1 C4 -96.29(15) . . . . no N5 Y N1 C5 83.27(13) . . . . no C20 Y N1 C4 12.97(17) . . . . no C20 Y N1 C5 -167.46(12) . . . . no N1 Y N2 C6 36.56(11) . . . . no N1 Y N2 C7 152.72(13) . . . . no N1 Y N2 C9 -80.24(12) . . . . no N3 Y N2 C6 -118.06(12) . . . . no N3 Y N2 C7 -1.90(11) . . . . no N3 Y N2 C9 125.14(12) . . . . no N4 Y N2 C6 139.76(12) . . . . no N4 Y N2 C7 -104.07(12) . . . . no N4 Y N2 C9 22.96(11) . . . . no N5 Y N2 C6 -55.84(12) . . . . no N5 Y N2 C7 60.33(12) . . . . no N5 Y N2 C9 -172.64(12) . . . . no C20 Y N2 C6 160.34(12) . . . . no C20 Y N2 C7 -83.49(16) . . . . no C20 Y N2 C9 43.54(18) . . . . no N1 Y N3 C8 -6.94(14) . . . . no N1 Y N3 C13 -130.39(13) . . . . no N1 Y N3 C14 109.66(12) . . . . no N2 Y N3 C8 28.82(10) . . . . no N2 Y N3 C13 -94.63(13) . . . . no N2 Y N3 C14 145.42(12) . . . . no N4 Y N3 C8 94.53(11) . . . . no N4 Y N3 C13 -28.92(13) . . . . no N4 Y N3 C14 -148.87(11) . . . . no N5 Y N3 C8 -83.12(11) . . . . no N5 Y N3 C13 153.43(14) . . . . no N5 Y N3 C14 33.48(10) . . . . no C20 Y N3 C8 177.51(11) . . . . no C20 Y N3 C13 54.06(14) . . . . no C20 Y N3 C14 -65.89(11) . . . . no N1 Y N4 C10 75.62(12) . . . . no N1 Y N4 C11 -41.21(12) . . . . no N1 Y N4 C12 -159.45(12) . . . . no N2 Y N4 C10 6.29(12) . . . . no N2 Y N4 C11 -110.54(12) . . . . no N2 Y N4 C12 131.23(13) . . . . no N3 Y N4 C10 -60.70(12) . . . . no N3 Y N4 C11 -177.53(11) . . . . no N3 Y N4 C12 64.24(13) . . . . no C20 Y N4 C10 -163.25(13) . . . . no C20 Y N4 C11 79.92(12) . . . . no C20 Y N4 C12 -38.31(13) . . . . no N1 Y N5 C15 -153.44(13) . . . . no N1 Y N5 C19 31.96(15) . . . . no N2 Y N5 C15 -79.62(13) . . . . no N2 Y N5 C19 105.78(14) . . . . no N3 Y N5 C15 -16.64(12) . . . . no N3 Y N5 C19 168.76(15) . . . . no C20 Y N5 C15 82.29(13) . . . . no C20 Y N5 C19 -92.31(15) . . . . no N1 Y C20 Si -93.33(12) . . . . no N2 Y C20 Si 155.53(9) . . . . no N3 Y C20 Si 83.01(12) . . . . no N4 Y C20 Si 174.80(12) . . . . no N5 Y C20 Si 11.92(13) . . . . no N1 Y C20 H20' 31.4(19) . . . . no N2 Y C20 H20 31.5(15) . . . . no N2 Y C20 H20' -79.8(19) . . . . no N3 Y C20 H20 -41.0(15) . . . . no N3 Y C20 H20' -152.3(19) . . . . no N4 Y C20 H20 50.7(15) . . . . no N4 Y C20 H20' -60.5(19) . . . . no N5 Y C20 H20 -112.1(15) . . . . no N5 Y C20 H20' 136.6(19) . . . . no N1 Y C20 H20 142.6(15) . . . . no C22 Si C20 Y 164.47(12) . . . . no C23 Si C20 Y 44.35(14) . . . . no C21 Si C20 Y -77.47(14) . . . . no C23 Si C22 H22 -177.9(16) . . . . no C21 Si C22 H22' 57.2(18) . . . . no C21 Si C22 H22" -178.4(18) . . . . no C20 Si C22 H22" -56.3(19) . . . . no C21 Si C22 H22 -63.8(16) . . . . no C22 Si C21 H21" -164.9(19) . . . . no C23 Si C21 H21 70.5(14) . . . . no C23 Si C21 H21' -170.5(18) . . . . no C23 Si C21 H21" -52.3(19) . . . . no C20 Si C22 H22 58.3(16) . . . . no C20 Si C22 H22' 179.3(18) . . . . no C22 Si C23 H23" -60.6(16) . . . . no C21 Si C20 H20' 157.9(17) . . . . no C22 Si C20 H20 -73.1(15) . . . . no C22 Si C20 H20' 39.8(17) . . . . no C23 Si C20 H20 166.7(15) . . . . no C23 Si C20 H20' -80.3(17) . . . . no C20 Si C21 H21 -165.1(14) . . . . no C20 Si C21 H21' -46.1(18) . . . . no C20 Si C21 H21" 72.0(19) . . . . no C22 Si C21 H21 -42.1(14) . . . . no C22 Si C21 H21' 76.9(18) . . . . no C21 Si C23 H23 62.8(14) . . . . no C21 Si C23 H23' -57.8(16) . . . . no C21 Si C23 H23" -172.5(16) . . . . no C22 Si C23 H23 174.6(14) . . . . no C22 Si C23 H23' 54.0(16) . . . . no C21 Si C20 H20 44.9(15) . . . . no C20 Si C23 H23' 178.3(16) . . . . no C20 Si C23 H23" 63.6(16) . . . . no C23 Si C22 H22" 67.5(19) . . . . no C20 Si C23 H23 -61.1(14) . . . . no C23 Si C22 H22' -56.9(18) . . . . no Y N1 C4 C1 -6.6(2) . . . . no Y N1 C4 C2 112.08(17) . . . . no Y N1 C5 C6 -6.5(2) . . . . no C4 N1 C5 C6 173.11(15) . . . . no C5 N1 C4 C1 173.84(17) . . . . no C5 N1 C4 C2 -67.5(2) . . . . no Y N1 C4 C3 -125.67(17) . . . . no C5 N1 C4 C3 54.7(2) . . . . no Y N2 C6 C5 -54.50(17) . . . . no C7 N2 C6 C5 -173.89(16) . . . . no C6 N2 C7 C8 83.53(19) . . . . no C9 N2 C7 C8 -153.08(16) . . . . no Y N2 C9 C10 -51.41(17) . . . . no C6 N2 C9 C10 -160.16(15) . . . . no C7 N2 C9 C10 77.20(19) . . . . no C9 N2 C6 C5 62.8(2) . . . . no Y N2 C7 C8 -25.72(18) . . . . no C13 N3 C14 C15 -176.83(15) . . . . no C8 N3 C14 C15 63.37(19) . . . . no Y N3 C8 C7 -55.08(16) . . . . no C13 N3 C8 C7 73.8(2) . . . . no C14 N3 C8 C7 -167.65(15) . . . . no Y N3 C14 C15 -49.86(16) . . . . no C12 N4 C10 C9 -164.71(17) . . . . no C11 N4 C10 C9 78.4(2) . . . . no Y N4 C10 C9 -34.56(19) . . . . no Y N5 C15 C14 -4.02(19) . . . . no C15 N5 C19 C18 -20.7(2) . . . . no C19 N5 C15 C14 171.23(15) . . . . no C19 N5 C15 C16 47.2(2) . . . . no Y N5 C15 C16 -128.01(13) . . . . no Y N5 C19 C18 154.42(15) . . . . no N1 C5 C6 N2 46.0(2) . . . . no N2 C7 C8 N3 56.4(2) . . . . no N2 C9 C10 N4 59.1(2) . . . . no N3 C14 C15 C16 161.71(15) . . . . no N3 C14 C15 N5 38.5(2) . . . . no N5 C15 C16 C17 -43.3(2) . . . . no C14 C15 C16 C17 -165.74(17) . . . . no C15 C16 C17 C18 9.9(3) . . . . no C16 C17 C18 C19 19.2(3) . . . . no C17 C18 C19 N5 -13.6(3) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Y H1' 3.31(2) . . no Y H1" 3.02(2) . . no Y H23 3.89(2) . . no N1 H9 2.908(19) . . no N5 H8 2.755(19) . . no C6 C19 3.582(3) . 3_656 no C8 C17 3.572(3) . 3_556 no C17 C8 3.572(3) . 3_556 no C19 C6 3.582(3) . 3_656 no C2 H5' 2.769(19) . . no C2 H19 3.00(2) . . no C2 H9' 3.037(19) . . no C3 H5 2.61(2) . . no C5 H3' 2.72(2) . . no C5 H9 2.510(19) . . no C5 H2" 2.812(19) . . no C6 H8 2.901(19) . . no C7 H10 2.809(19) . . no C7 H13' 2.74(2) . . no C8 H15 2.844(19) . . no C8 H6 2.78(2) . . no C9 H11 2.80(2) . . no C9 H5 2.85(2) . . no C10 H7 2.69(2) . . no C11 H9 2.812(19) . . no C11 H22" 3.02(3) . 3_556 no C11 H1' 3.093(19) . . no C12 H20 2.92(2) . . no C13 H7 2.80(2) . . no C13 H12 2.96(2) . . no C15 H8 2.555(19) . . no C16 H21" 2.92(3) . . no C16 H8' 2.97(2) . 3_556 no C17 H8' 2.97(2) . 3_556 no C18 H15 2.912(19) . . no C18 H6' 3.02(2) . 3_656 no C18 H23 3.07(3) . . no C19 H23 2.88(2) . . no C19 H6' 2.86(2) . 3_656 no C20 H12" 2.90(2) . . no C21 H14 3.012(18) . . no C22 H13 3.06(2) . 2_545 no C23 H1" 3.10(2) . . no H1 H2 2.44(3) . . no H1 H3 2.52(3) . . no H1' Y 3.31(2) . . no H1' C11 3.093(19) . . no H1' H3" 2.44(3) . . no H1' H11" 2.57(3) . . no H1" Y 3.02(2) . . no H1" C23 3.10(2) . . no H1" H2' 2.54(3) . . no H1" H23" 2.59(4) . . no H2 H1 2.44(3) . . no H2 H3 2.47(3) . . no H2 H9' 2.48(3) . . no H2' H1" 2.54(3) . . no H2' H19 2.26(3) . . no H2" C5 2.812(19) . . no H2" H3' 2.58(3) . . no H2" H5' 2.29(3) . . no H3 H1 2.52(3) . . no H3 H2 2.47(3) . . no H3' C5 2.72(2) . . no H3' H2" 2.58(3) . . no H3' H5 2.25(3) . . no H3' H13" 2.48(3) . 1_565 no H3" H1' 2.44(3) . . no H3" H11 2.41(3) . . no H3" H22" 2.58(4) . 3_556 no H5 C3 2.61(2) . . no H5 C9 2.85(2) . . no H5 H3' 2.25(3) . . no H5 H9 2.14(3) . . no H5' C2 2.769(19) . . no H5' H2" 2.29(3) . . no H6 C8 2.78(2) . . no H6 H7' 2.58(3) . . no H6 H8 2.25(3) . . no H6' H7' 2.35(3) . . no H6' C18 3.02(2) . 3_656 no H6' C19 2.86(2) . 3_656 no H6' H19 2.56(3) . 3_656 no H7 C10 2.69(2) . . no H7 C13 2.80(2) . . no H7 H9' 2.42(3) . . no H7 H10 2.17(3) . . no H7 H13' 2.22(3) . . no H7' H6 2.58(3) . . no H7' H6' 2.35(3) . . no H8 N5 2.755(19) . . no H8 C6 2.901(19) . . no H8 C15 2.555(19) . . no H8 H6 2.25(3) . . no H8 H15 2.19(3) . . no H8' H13" 2.40(3) . . no H8' H14' 2.54(3) . . no H8' C16 2.97(2) . 3_556 no H8' C17 2.97(2) . 3_556 no H9 N1 2.908(19) . . no H9 C5 2.510(19) . . no H9 C11 2.812(19) . . no H9 H5 2.14(3) . . no H9 H11 2.26(3) . . no H9' C2 3.037(19) . 1_565 no H9' H2 2.48(3) . 1_565 no H9' H7 2.42(3) . . no H10 C7 2.809(19) . . no H10 H7 2.17(3) . . no H10 H12 2.32(3) . . no H10 H13' 2.48(3) . . no H10' H11' 2.32(3) . . no H10' H12' 2.50(3) . . no H11 C9 2.80(2) . . no H11 H3" 2.41(3) . . no H11 H9 2.26(3) . . no H11' H10' 2.32(3) . . no H11' H12' 2.47(3) . . no H11" H1' 2.57(3) . . no H11" H12" 2.34(3) . . no H12 C13 2.96(2) . . no H12 H10 2.32(3) . . no H12 H13' 2.45(3) . . no H12' H10' 2.50(3) . . no H12' H11' 2.47(3) . . no H12' H12' 2.53(3) . 1_565 no H12" C20 2.90(2) . . no H12" H11" 2.34(3) . . no H12" H20 2.32(3) . . no H13 H14 2.32(3) . . no H13 C22 3.06(2) . 2_555 no H13' C7 2.74(2) . . no H13' H7 2.22(3) . . no H13' H10 2.48(3) . . no H13' H12 2.45(3) . . no H13" H8' 2.40(3) . . no H13" H14' 2.39(3) . . no H13" H3' 2.48(3) . 2_545 no H14 C21 3.012(18) . . no H14 H13 2.32(3) . . no H14 H16 2.52(3) . . no H14 H21" 2.39(3) . . no H14' H8' 2.54(3) . . no H14' H13" 2.39(3) . . no H15 C8 2.844(19) . . no H15 C18 2.912(19) . . no H15 H8 2.19(3) . . no H15 H17 2.55(3) . 3_556 no H16 H14 2.52(3) . . no H17 H15 2.55(3) . 3_556 no H19 C2 3.00(2) . . no H19 H2' 2.26(3) . . no H19 H6' 2.56(3) . 3_656 no H20 C12 2.92(2) . . no H20 H12" 2.32(3) . . no H20 H22' 2.36(3) . 2_555 no H21" C16 2.92(3) . . no H21" H14 2.39(3) . . no H22 H23' 2.52(4) . 2_555 no H22' H20 2.36(3) . 2_545 no H22" C11 3.02(3) . 3_556 no H22" H3" 2.58(4) . 3_556 no H23 Y 3.89(2) . . no H23 C18 3.07(3) . . no H23 C19 2.88(2) . . no H23' H22 2.52(4) . 2_545 no H23" H1" 2.59(4) . . no # End of Crystallographic Information File