# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1548 # CIF-file generated for C33H41ClF10N5Si4V CP482 #============================================================================== data_global #============================================================================== # 0. AUDIT DETAILS _audit_creation_date 1999-05-20 _audit_creation_method 'PLATON option' _audit_update_record ; ? ; #=============================================================================== # 1. SUBMISSION DETAILS # Name and address of author for correspondence _publ_contact_author_name ; Drs. A. Meetsma ; _publ_contact_author_address ; Crystal Structure Center, 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 ? # Publication choise FI FM FO CI CM CO AD _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission : 1999--12-09 Consider this CIF submission for depostion of the first Xray-structure of the manuscript (Our Code : CP482) ; #=============================================================================== # 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 ; The N,N'-bis(trimethylsilyl)-pentafluorobenzamidinate ligand; enhanced ethene oligomerisation with a neutral V(III) bis(benzamidinated) alkyl catalyst. ; _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_address 'Brussee, Edward A.C.' ; Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen , Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; 'Meetsma, Auke' ; Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen , Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; 'Hessen, Bart' ; Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen , Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; 'Teuben, Jan H.' ; Centre for Catalytic Olefin Polymerisation, Stratingh Institute of Chemistry and Chemical Engineering, University of Groningen , Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; #=============================================================================== # 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., Bosman, W.P., Gelder, R. de, Garc\'ia-Granda, S., Gould, R.O., Isra\"el, R. & Smits, J.M.M. & (1997) The DIRDIF97 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Boer, J.L. de & Duisenberg, A.J.M. (1984). Acta Cryst. A40, C-410. Bolhuis, F. van (1971). J. Appl. Cryst. 4, 263-264. Bondi, A. (1964). J. Phys. Chem. 68, 441-451. Duisenberg, A.J.M. (1992). J. Appl. Cryst. 25, 92-96. Enraf-Nonius (1994). CAD4-UNIX Software. Version 5.1 Utrecht modified version October 1994. Enraf-Nonius, Delft, The Netherlands. Furrugia, L.J. (1998). ORTEP-3 for Windows. Version 1.04. Department of Chemistry, Univ. of Glasgow, Scotland, UK. International Tables for Crystallography (1983). Vol. A. Space-group symmetry, edited by T. Hahn. Dordrecht: Reidel. (Present distributor Kluwer Academic Publishers, Dordrecht). International Tables for Crystallography (1992). Vol. C. Edited by A.J.C Wilson, Kluwer Academic Publishers, Dordrecht, The Netherlands. Le Page, Y. (1987). J. Appl. Cryst. 20, 264-269. Le Page, Y. (1988). J. Appl. Cryst. 21, 983-984. Meetsma, A. (1996). Extended version of the program PLUTO. Groningen University, The Netherlands. (unpublished). Sheldrick, G.M. (1997). SHELXL-97. Program for the Refinement of Crystal Structures, University of G\\"ottingen, 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. (1997). HELENA, Program for Data Reduction, Utrecht University, The Netherlands. Spek, A.L. (1994). Am. Crystallogr. Assoc.-Abstracts, 22, 66. ; _publ_section_figure_captions ; Fig. 1. Chemical structural diagram (scheme 1) of the title compound Fig. 2. PLUTO drawing of the molecule illustrating the puckering and the adopted numbering scheme. Fig. 3. Molecular packing viewed down unit cell axes. Fig. 4. Perspective ORTEP drawing of the title compound. All non-hydrogen atoms are represented by thermal vibrational ellipsoids drawn to encompass 50% of the electron density. The hydrogen atoms are omit for sake of clarity. ; _publ_section_acknowledgements ; ? ; data_c33h51cl #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H51 Cl N5 Si4 V' _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 'C33 H51 Cl N5 Si4 V' _chemical_formula_weight 716.54 _chemical_compound_source 'by syntheses' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source V V 0.3005 0.5294 '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' Cl Cl 0.1484 0.1585 '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 Orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,y,1/2-z 1/2-x,1/2+y,z x,1/2-y,1/2+z _cell_length_a 20.778(1) _cell_length_b 17.918(1) _cell_length_c 21.623(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8050.2(7) _cell_formula_units_Z 8 _cell_measurement_temperature 130 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 16.06 _cell_measurement_theta_max 16.68 _cell_special_details ; Unit cell parameters (Duisenberg, 1992) and orientation matrix were determined from a least-squares treatment of SET4 (de Boer & Duisenberg, 1984) setting. Reduced cell calculations did not indicate any higher metric lattice symmetry and examination of the final atomic coordinates of the structure did not yield extra symmetry elements (Spek, 1988; Le Page 1987, 1988) ; _exptl_crystal_description paralleplepiped _exptl_crystal_colour 'colorless transparent' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 0.46 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type 'none' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 130 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine focus sealed Philips Mo tube ' _diffrn_radiation_monochromator 'perpendicular mounted graphite' _diffrn_radiation_detector ; scintillation NaI crystal with photomultiplier ; _diffrn_measurement_device_type ; Enraf Nonius CAD-4F diffractometer ; _diffrn_measurement_method '\w/2\q' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temperature unit (Bolhuis, 1971), on an Enraf-Nonius CAD-4F diffractometer. Graphite-monochromated Mo K\a radiation, \w/2\q scan, \D\w = (0.70 + 0.34 tg \q)\%. ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 180 _diffrn_standards_decay_% 1.7 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -4 5 -5 -3 -1 2 -4 5 # number of measured reflections (redundant set) _diffrn_reflns_number 8007 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.5 _diffrn_reflns_reduction_process ; Intensity data were corrected for Lorentz and polarization effects, scale variation, but not for absorption and reduced to F~o~^2^ ; # number of unique reflections _reflns_number_total 8007 # number of observed reflections (> n sig(I)) _reflns_number_gt >2sigma(I) _reflns_threshold_expression 5016 _computing_data_collection 'CAD4-UNIX software Version 5.1, 1994' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1993)' _computing_structure_solution ; DIRDIF (Beurskens et al., 1994) ; _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ; PLUTO (Meetsma, 1995) ORTEP (Johnson, 1976) PLATON (Spek, 1994, 1996) ; _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2, conventional R-factors R are based on F, with F set to zero for negative F^2. The observed criterion of F^2 > 2sigma(F^2) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+2.0] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment isotropic _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6875 _refine_ls_number_parameters 601 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1086 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1093 _refine_ls_wR_factor_gt ? _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max .36 _refine_diff_density_min -.29 _refine_diff_density_rms .07 #=============================================================================== # 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 V V Uani 0.15443(2) 0.25369(3) 0.14438(2) 1.000 0.0180(2) Cl1 Cl Uani 0.20914(5) 0.17385(6) 0.21274(5) 1.000 0.0368(3) Si1 Si Uani 0.05702(5) 0.28872(6) 0.27975(5) 1.000 0.0254(3) Si2 Si Uani 0.06442(5) 0.11812(5) 0.06479(5) 1.000 0.0256(3) Si3 Si Uani 0.07642(5) 0.39286(5) 0.05831(5) 1.000 0.0227(3) Si4 Si Uani 0.29806(5) 0.21617(6) 0.05764(5) 1.000 0.0312(3) N1 N Uani 0.07375(12) 0.26120(14) 0.20368(12) 1.000 0.0202(8) N2 N Uani 0.08113(13) 0.18277(14) 0.12299(12) 1.000 0.0199(8) N3 N Uani 0.13520(12) 0.32653(14) 0.07307(12) 1.000 0.0183(8) N4 N Uani 0.22136(12) 0.25204(16) 0.07168(12) 1.000 0.0206(8) N5 N Uani 0.21253(14) 0.34205(16) 0.18338(14) 1.000 0.0291(10) C1 C Uani 0.1299(2) 0.3363(3) 0.3095(2) 1.000 0.0407(16) C2 C Uani 0.0413(2) 0.2078(3) 0.33129(19) 1.000 0.0333(14) C3 C Uani -0.0115(2) 0.3559(2) 0.2845(2) 1.000 0.0367(14) C4 C Uani 0.1033(3) 0.0280(3) 0.0849(2) 1.000 0.0420(16) C5 C Uani -0.0231(2) 0.1063(3) 0.0493(3) 1.000 0.0483(19) C6 C Uani 0.1025(3) 0.1523(3) -0.00776(19) 1.000 0.0360(16) C7 C Uani 0.04749(16) 0.20531(18) 0.17206(15) 1.000 0.0213(10) C8 C Uani -0.01383(16) 0.16827(19) 0.19172(15) 1.000 0.0226(10) C9 C Uani -0.01487(19) 0.0930(2) 0.20721(17) 1.000 0.0283(12) C10 C Uani -0.07047(19) 0.0605(2) 0.22887(18) 1.000 0.0343(12) C11 C Uani -0.12574(19) 0.1017(2) 0.23560(19) 1.000 0.0367(14) C12 C Uani -0.12586(19) 0.1760(2) 0.21885(19) 1.000 0.0367(12) C13 C Uani -0.06987(18) 0.2097(2) 0.19702(17) 1.000 0.0290(12) C14 C Uani 0.0727(3) 0.4546(3) 0.1265(2) 1.000 0.0450(17) C15 C Uani -0.0005(2) 0.3427(3) 0.0503(3) 1.000 0.0433(18) C16 C Uani 0.0885(2) 0.4490(3) -0.0129(2) 1.000 0.0393(17) C17 C Uani 0.3253(3) 0.2274(4) -0.0243(3) 1.000 0.060(2) C18 C Uani 0.3562(3) 0.2634(4) 0.1099(3) 1.000 0.059(2) C19 C Uani 0.2954(3) 0.1157(3) 0.0749(4) 1.000 0.061(2) C20 C Uani 0.19069(15) 0.30847(18) 0.04542(14) 1.000 0.0191(10) C21 C Uani 0.21651(15) 0.3512(2) -0.00817(15) 1.000 0.0219(10) C22 C Uani 0.20267(18) 0.3311(2) -0.06852(17) 1.000 0.0300(12) C23 C Uani 0.2280(2) 0.3717(3) -0.11740(18) 1.000 0.0380(14) C24 C Uani 0.2656(2) 0.4332(3) -0.1064(2) 1.000 0.0433(16) C25 C Uani 0.2792(2) 0.4539(3) -0.0466(2) 1.000 0.0463(17) C26 C Uani 0.25513(19) 0.4131(2) 0.00224(17) 1.000 0.0311(11) C27 C Uani 0.24834(18) 0.3750(2) 0.21211(16) 1.000 0.0275(11) C28 C Uani 0.29354(16) 0.41251(19) 0.25175(16) 1.000 0.0229(10) C29 C Uani 0.31656(19) 0.4827(2) 0.23651(19) 1.000 0.0313(12) C30 C Uani 0.36066(19) 0.5168(2) 0.2749(2) 1.000 0.0363(14) C31 C Uani 0.3820(2) 0.4810(3) 0.3270(2) 1.000 0.0393(14) C32 C Uani 0.3588(2) 0.4121(3) 0.3424(2) 1.000 0.0447(17) C33 C Uani 0.3143(2) 0.3771(2) 0.30493(19) 1.000 0.0353(12) H1 H Uiso 0.127(2) 0.346(3) 0.350(2) 1.000 0.070(15) H1' H Uiso 0.138(2) 0.381(2) 0.291(2) 1.000 0.049(14) H1" H Uiso 0.168(2) 0.305(2) 0.3089(19) 1.000 0.048(13) H2 H Uiso 0.0360(18) 0.227(2) 0.3705(18) 1.000 0.039(11) H2' H Uiso 0.077(2) 0.178(2) 0.3302(19) 1.000 0.047(13) H2" H Uiso 0.0045(17) 0.1861(18) 0.3189(16) 1.000 0.021(10) H3 H Uiso -0.0096(19) 0.376(2) 0.321(2) 1.000 0.045(13) H3' H Uiso -0.051(2) 0.328(2) 0.2809(19) 1.000 0.052(13) H3" H Uiso -0.010(2) 0.394(2) 0.252(2) 1.000 0.057(14) H4 H Uiso 0.102(2) -0.005(2) 0.050(2) 1.000 0.052(13) H4' H Uiso 0.0855(19) 0.004(2) 0.115(2) 1.000 0.039(13) H4" H Uiso 0.149(2) 0.033(2) 0.092(2) 1.000 0.051(14) H5 H Uiso -0.0284(19) 0.077(2) 0.014(2) 1.000 0.049(13) H5' H Uiso -0.039(2) 0.152(3) 0.045(2) 1.000 0.059(17) H5" H Uiso -0.048(2) 0.078(2) 0.081(2) 1.000 0.059(15) H6 H Uiso 0.092(2) 0.117(2) -0.040(2) 1.000 0.059(14) H6' H Uiso 0.145(2) 0.156(2) -0.0068(19) 1.000 0.048(14) H6" H Uiso 0.0859(17) 0.197(2) -0.0184(16) 1.000 0.027(10) H9 H Uiso 0.0220(16) 0.0673(18) 0.2017(15) 1.000 0.023(10) H10 H Uiso -0.0705(17) 0.009(2) 0.2395(18) 1.000 0.036(11) H11 H Uiso -0.1661(17) 0.0776(19) 0.2487(16) 1.000 0.030(10) H12 H Uiso -0.1655(16) 0.2067(18) 0.2217(15) 1.000 0.023(9) H13 H Uiso -0.0686(16) 0.2592(18) 0.1880(16) 1.000 0.024(10) H14 H Uiso 0.040(2) 0.490(3) 0.122(2) 1.000 0.078(17) H14' H Uiso 0.110(2) 0.477(2) 0.1302(18) 1.000 0.037(13) H14" H Uiso 0.0663(19) 0.425(2) 0.162(2) 1.000 0.050(13) H15 H Uiso -0.034(2) 0.379(3) 0.042(2) 1.000 0.064(15) H15' H Uiso -0.011(3) 0.319(3) 0.089(3) 1.000 0.10(2) H15" H Uiso -0.001(2) 0.316(2) 0.016(2) 1.000 0.044(14) H16 H Uiso 0.0504(18) 0.482(2) -0.0199(18) 1.000 0.039(11) H16' H Uiso 0.090(2) 0.418(3) -0.048(2) 1.000 0.077(18) H16" H Uiso 0.128(2) 0.475(2) -0.0093(19) 1.000 0.043(12) H17 H Uiso 0.364(2) 0.201(2) -0.0270(19) 1.000 0.048(12) H17' H Uiso 0.332(3) 0.284(4) -0.035(3) 1.000 0.12(2) H17" H Uiso 0.299(2) 0.198(2) -0.048(2) 1.000 0.051(15) H18 H Uiso 0.397(3) 0.243(3) 0.098(3) 1.000 0.090(18) H18' H Uiso 0.345(3) 0.251(3) 0.152(3) 1.000 0.11(2) H18" H Uiso 0.363(3) 0.309(3) 0.096(3) 1.000 0.08(2) H19 H Uiso 0.338(3) 0.100(3) 0.071(2) 1.000 0.079(17) H19' H Uiso 0.265(3) 0.094(3) 0.056(2) 1.000 0.07(2) H19" H Uiso 0.279(2) 0.103(2) 0.113(2) 1.000 0.055(16) H22 H Uiso 0.1771(15) 0.2892(18) -0.0795(14) 1.000 0.016(9) H23 H Uiso 0.2146(18) 0.355(2) -0.1562(19) 1.000 0.044(12) H24 H Uiso 0.283(2) 0.464(2) -0.141(2) 1.000 0.062(14) H25 H Uiso 0.3053(16) 0.4922(19) -0.0385(16) 1.000 0.020(10) H26 H Uiso 0.2646(17) 0.426(2) 0.0437(17) 1.000 0.033(10) H29 H Uiso 0.300(2) 0.506(2) 0.207(2) 1.000 0.048(14) H30 H Uiso 0.376(2) 0.562(2) 0.264(2) 1.000 0.053(14) H31 H Uiso 0.4104(17) 0.5065(19) 0.3497(18) 1.000 0.032(11) H32 H Uiso 0.3701(18) 0.388(2) 0.3796(18) 1.000 0.043(12) H33 H Uiso 0.2952(16) 0.3331(19) 0.3153(16) 1.000 0.026(10) 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 V 0.0187(3) 0.0210(3) 0.0143(3) -0.0009(3) -0.0011(2) -0.0010(3) Cl1 0.0340(5) 0.0438(6) 0.0326(5) 0.0140(5) -0.0069(4) 0.0052(4) Si1 0.0282(5) 0.0290(5) 0.0190(5) -0.0038(4) 0.0038(4) -0.0019(4) Si2 0.0296(5) 0.0270(5) 0.0203(5) -0.0054(4) -0.0029(4) -0.0062(4) Si3 0.0219(5) 0.0231(5) 0.0232(5) 0.0035(4) 0.0049(4) 0.0036(4) Si4 0.0216(5) 0.0415(6) 0.0306(6) -0.0023(5) -0.0010(5) 0.0110(5) N1 0.0220(14) 0.0219(15) 0.0166(14) 0.0000(12) 0.0002(12) -0.0009(12) N2 0.0197(15) 0.0217(14) 0.0183(15) -0.0034(12) -0.0005(12) -0.0029(12) N3 0.0178(14) 0.0223(14) 0.0148(14) 0.0010(12) 0.0004(11) 0.0008(12) N4 0.0182(13) 0.0253(14) 0.0182(14) -0.0011(13) 0.0017(11) 0.0035(13) N5 0.0301(18) 0.0317(17) 0.0254(17) -0.0034(14) -0.0002(14) -0.0081(15) C1 0.044(3) 0.059(3) 0.019(2) -0.013(2) 0.0012(19) -0.014(2) C2 0.042(3) 0.041(2) 0.017(2) -0.0005(18) 0.0050(19) 0.001(2) C3 0.039(2) 0.034(2) 0.037(3) -0.005(2) 0.007(2) 0.000(2) C4 0.057(3) 0.032(2) 0.037(3) -0.007(2) 0.001(2) -0.003(2) C5 0.043(3) 0.063(4) 0.039(3) -0.017(3) -0.012(2) -0.015(3) C6 0.045(3) 0.040(3) 0.023(2) -0.0066(19) 0.001(2) -0.003(2) C7 0.0229(18) 0.0217(17) 0.0193(17) 0.0015(14) -0.0009(15) 0.0043(15) C8 0.0236(18) 0.0283(19) 0.0159(17) 0.0017(15) 0.0006(14) -0.0021(16) C9 0.031(2) 0.028(2) 0.026(2) 0.0061(16) 0.0027(17) 0.0008(18) C10 0.040(2) 0.032(2) 0.031(2) 0.0072(18) 0.0016(19) -0.0081(19) C11 0.027(2) 0.049(3) 0.034(2) 0.003(2) 0.0048(18) -0.014(2) C12 0.026(2) 0.041(2) 0.043(2) 0.003(2) 0.0038(19) -0.0007(19) C13 0.030(2) 0.026(2) 0.031(2) 0.0021(17) 0.0011(17) -0.0045(18) C14 0.061(3) 0.035(3) 0.039(3) -0.001(2) 0.012(2) 0.011(3) C15 0.022(2) 0.043(3) 0.065(4) 0.010(3) -0.002(2) 0.0044(19) C16 0.033(3) 0.045(3) 0.040(3) 0.020(2) 0.011(2) 0.018(2) C17 0.038(3) 0.099(5) 0.044(3) -0.002(3) 0.015(2) 0.035(3) C18 0.036(3) 0.075(4) 0.065(4) -0.006(3) -0.010(3) 0.002(3) C19 0.049(3) 0.048(3) 0.087(5) 0.001(3) 0.012(4) 0.022(3) C20 0.0196(18) 0.0225(17) 0.0152(16) -0.0023(14) -0.0037(14) -0.0030(14) C21 0.0119(17) 0.036(2) 0.0179(17) -0.0002(15) 0.0010(14) 0.0007(15) C22 0.027(2) 0.040(2) 0.023(2) 0.0001(18) 0.0000(16) 0.0007(18) C23 0.041(2) 0.056(3) 0.017(2) -0.0007(19) 0.0036(18) 0.006(2) C24 0.045(3) 0.055(3) 0.030(2) 0.017(2) 0.013(2) -0.002(2) C25 0.040(3) 0.052(3) 0.047(3) 0.011(2) 0.007(2) -0.018(2) C26 0.033(2) 0.040(2) 0.0202(19) -0.0021(18) 0.0016(18) -0.0070(18) C27 0.0276(19) 0.030(2) 0.0248(19) -0.0013(17) 0.0060(17) -0.0014(17) C28 0.0224(18) 0.0262(17) 0.0200(17) -0.0025(15) -0.0021(15) -0.0039(15) C29 0.033(2) 0.032(2) 0.029(2) -0.0021(18) 0.0020(18) -0.0045(18) C30 0.029(2) 0.035(2) 0.045(3) -0.010(2) 0.0059(19) -0.0116(19) C31 0.028(2) 0.054(3) 0.036(2) -0.021(2) -0.0059(19) -0.003(2) C32 0.044(3) 0.058(3) 0.032(3) -0.001(2) -0.012(2) 0.011(2) C33 0.040(2) 0.029(2) 0.037(2) 0.0019(19) -0.0048(19) -0.0016(19) #=============================================================================== # 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 V Cl1 2.3503(12) . . yes V N1 2.115(3) . . yes V N2 2.037(3) . . yes V N3 2.059(3) . . yes V N4 2.099(3) . . yes V N5 2.162(3) . . yes Si1 N1 1.752(3) . . yes Si1 C1 1.853(5) . . yes Si1 C2 1.858(5) . . yes Si1 C3 1.867(4) . . yes Si2 N2 1.745(3) . . yes Si2 C4 1.857(6) . . yes Si2 C5 1.861(4) . . yes Si2 C6 1.861(5) . . yes Si3 N3 1.734(3) . . yes Si3 C14 1.845(5) . . yes Si3 C15 1.842(5) . . yes Si3 C16 1.856(5) . . yes Si4 N4 1.745(3) . . yes Si4 C17 1.871(7) . . yes Si4 C18 1.858(7) . . yes Si4 C19 1.839(6) . . yes N1 C7 1.330(4) . . yes N2 C7 1.333(4) . . yes N3 C20 1.338(4) . . yes N4 C20 1.323(4) . . yes N5 C27 1.135(5) . . yes C7 C8 1.498(5) . . no C8 C9 1.390(5) . . no C8 C13 1.386(5) . . no C9 C10 1.376(5) . . no C10 C11 1.373(5) . . no C11 C12 1.380(5) . . no C12 C13 1.393(5) . . no C20 C21 1.489(5) . . no C21 C22 1.384(5) . . no C21 C26 1.387(5) . . no C22 C23 1.387(6) . . no C23 C24 1.372(7) . . no C24 C25 1.375(6) . . no C25 C26 1.378(6) . . no C27 C28 1.438(5) . . no C28 C29 1.385(5) . . no C28 C33 1.382(5) . . no C29 C30 1.379(6) . . no C30 C31 1.370(6) . . no C31 C32 1.367(7) . . no C32 C33 1.380(6) . . no C1 H1 0.89(4) . . no C1 H1' 0.91(4) . . no C1 H1" 0.97(4) . . no C2 H2 0.92(4) . . no C2 H2' 0.91(4) . . no C2 H2" 0.90(3) . . no C3 H3 0.87(4) . . no C3 H3' 0.96(4) . . no C3 H3" 0.98(4) . . no C4 H4 0.96(4) . . no C4 H4' 0.86(4) . . no C4 H4" 0.97(4) . . no C5 H5 0.93(4) . . no C5 H5' 0.89(5) . . no C5 H5" 1.00(4) . . no C6 H6 0.97(4) . . no C6 H6' 0.89(4) . . no C6 H6" 0.90(4) . . no C9 H9 0.90(3) . . no C10 H10 0.95(4) . . no C11 H11 0.98(4) . . no C12 H12 0.99(3) . . no C13 H13 0.91(3) . . no C14 H14 0.93(5) . . no C14 H14' 0.88(4) . . no C14 H14" 0.94(4) . . no C15 H15 0.97(5) . . no C15 H15' 0.96(6) . . no C15 H15" 0.88(4) . . no C16 H16 1.00(4) . . no C16 H16' 0.94(5) . . no C16 H16" 0.95(4) . . no C17 H17 0.93(4) . . no C17 H17' 1.05(7) . . no C17 H17" 0.92(4) . . no C18 H18 0.96(6) . . no C18 H18' 0.97(6) . . no C18 H18" 0.88(6) . . no C19 H19 0.93(6) . . no C19 H19' 0.85(6) . . no C19 H19" 0.92(4) . . no C22 H22 0.95(3) . . no C23 H23 0.93(4) . . no C24 H24 1.00(4) . . no C25 H25 0.89(3) . . no C26 H26 0.95(4) . . no C29 H29 0.84(4) . . no C30 H30 0.90(4) . . no C31 H31 0.89(4) . . no C32 H32 0.94(4) . . no C33 H33 0.91(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 Cl1 V N1 92.34(8) . . . yes Cl1 V N2 97.17(8) . . . yes Cl1 V N3 161.91(8) . . . yes Cl1 V N4 98.16(8) . . . yes Cl1 V N5 86.01(8) . . . yes N1 V N2 65.46(10) . . . yes N1 V N3 105.06(10) . . . yes N1 V N4 168.56(10) . . . yes N1 V N5 99.18(11) . . . yes N2 V N3 94.61(10) . . . yes N2 V N4 108.46(11) . . . yes N2 V N5 164.35(11) . . . yes N3 V N4 64.96(10) . . . yes N3 V N5 86.35(11) . . . yes N4 V N5 86.13(11) . . . yes N1 Si1 C1 107.05(17) . . . yes N1 Si1 C2 112.24(17) . . . yes N1 Si1 C3 112.60(17) . . . yes C1 Si1 C2 107.1(2) . . . yes C1 Si1 C3 107.9(2) . . . yes C2 Si1 C3 109.64(19) . . . yes N2 Si2 C4 108.77(18) . . . yes N2 Si2 C5 113.6(2) . . . yes N2 Si2 C6 107.75(19) . . . yes C4 Si2 C5 111.6(3) . . . yes C4 Si2 C6 107.4(2) . . . yes C5 Si2 C6 107.5(3) . . . yes N3 Si3 C14 107.1(2) . . . yes N3 Si3 C15 107.10(19) . . . yes N3 Si3 C16 115.40(17) . . . yes C14 Si3 C15 109.4(3) . . . yes C14 Si3 C16 110.1(2) . . . yes C15 Si3 C16 107.7(2) . . . yes N4 Si4 C17 113.7(2) . . . yes N4 Si4 C18 108.7(2) . . . yes N4 Si4 C19 107.3(2) . . . yes C17 Si4 C18 109.3(3) . . . yes C17 Si4 C19 107.8(3) . . . yes C18 Si4 C19 110.0(3) . . . yes V N1 Si1 138.11(15) . . . yes V N1 C7 88.03(19) . . . yes Si1 N1 C7 127.8(2) . . . yes V N2 Si2 136.60(15) . . . yes V N2 C7 91.28(19) . . . yes Si2 N2 C7 132.1(2) . . . yes V N3 Si3 135.15(15) . . . yes V N3 C20 90.81(19) . . . yes Si3 N3 C20 133.7(2) . . . yes V N4 Si4 137.78(15) . . . yes V N4 C20 89.52(19) . . . yes Si4 N4 C20 130.3(2) . . . yes V N5 C27 163.8(3) . . . yes N1 C7 N2 115.0(3) . . . yes N1 C7 C8 122.5(3) . . . yes N2 C7 C8 122.5(3) . . . yes C7 C8 C9 120.8(3) . . . no C7 C8 C13 120.1(3) . . . no C9 C8 C13 119.1(3) . . . no C8 C9 C10 120.4(3) . . . no C9 C10 C11 120.7(3) . . . no C10 C11 C12 119.5(4) . . . no C11 C12 C13 120.4(4) . . . no C8 C13 C12 119.8(3) . . . no N3 C20 N4 114.1(3) . . . yes N3 C20 C21 122.3(3) . . . yes N4 C20 C21 123.6(3) . . . yes C20 C21 C22 121.7(3) . . . no C20 C21 C26 119.6(3) . . . no C22 C21 C26 118.8(3) . . . no C21 C22 C23 120.2(4) . . . no C22 C23 C24 120.4(4) . . . no C23 C24 C25 119.8(4) . . . no C24 C25 C26 120.2(4) . . . no C21 C26 C25 120.6(4) . . . no N5 C27 C28 175.9(4) . . . yes C27 C28 C29 120.5(3) . . . no C27 C28 C33 119.0(3) . . . no C29 C28 C33 120.5(3) . . . no C28 C29 C30 119.2(4) . . . no C29 C30 C31 120.2(4) . . . no C30 C31 C32 120.6(4) . . . no C31 C32 C33 120.3(4) . . . no C28 C33 C32 119.3(4) . . . no Si1 C1 H1 112(3) . . . no Si1 C1 H1' 114(3) . . . no Si1 C1 H1" 113(2) . . . no H1 C1 H1' 106(4) . . . no H1 C1 H1" 100(4) . . . no H1' C1 H1" 111(3) . . . no Si1 C2 H2 106(2) . . . no Si1 C2 H2' 107(2) . . . no Si1 C2 H2" 108(2) . . . no H2 C2 H2' 110(3) . . . no H2 C2 H2" 110(3) . . . no H2' C2 H2" 115(3) . . . no Si1 C3 H3 106(3) . . . no Si1 C3 H3' 108(2) . . . no Si1 C3 H3" 113(2) . . . no H3 C3 H3' 109(4) . . . no H3 C3 H3" 111(3) . . . no H3' C3 H3" 109(3) . . . no Si2 C4 H4 110(2) . . . no Si2 C4 H4' 115(3) . . . no Si2 C4 H4" 113(2) . . . no H4 C4 H4' 106(4) . . . no H4 C4 H4" 102(3) . . . no H4' C4 H4" 110(4) . . . no Si2 C5 H5 109(2) . . . no Si2 C5 H5' 106(3) . . . no Si2 C5 H5" 116(2) . . . no H5 C5 H5' 113(4) . . . no H5 C5 H5" 102(3) . . . no H5' C5 H5" 110(4) . . . no Si2 C6 H6 107(2) . . . no Si2 C6 H6' 115(3) . . . no Si2 C6 H6" 110(2) . . . no H6 C6 H6' 107(4) . . . no H6 C6 H6" 108(3) . . . no H6' C6 H6" 109(3) . . . no C8 C9 H9 117(2) . . . no C10 C9 H9 123(2) . . . no C9 C10 H10 120(2) . . . no C11 C10 H10 120(2) . . . no C10 C11 H11 120(2) . . . no C12 C11 H11 120(2) . . . no C11 C12 H12 121.3(19) . . . no C13 C12 H12 118.3(19) . . . no C8 C13 H13 119(2) . . . no C12 C13 H13 121(2) . . . no Si3 C14 H14 111(3) . . . no Si3 C14 H14' 108(3) . . . no Si3 C14 H14" 109(2) . . . no H14 C14 H14' 110(4) . . . no H14 C14 H14" 111(4) . . . no H14' C14 H14" 108(4) . . . no Si3 C15 H15 108(3) . . . no Si3 C15 H15' 109(4) . . . no Si3 C15 H15" 111(3) . . . no H15 C15 H15' 107(4) . . . no H15 C15 H15" 102(4) . . . no H15' C15 H15" 119(4) . . . no Si3 C16 H16 110(2) . . . no Si3 C16 H16' 111(3) . . . no Si3 C16 H16" 108(2) . . . no H16 C16 H16' 105(4) . . . no H16 C16 H16" 114(3) . . . no H16' C16 H16" 109(4) . . . no Si4 C17 H17 105(3) . . . no Si4 C17 H17' 111(4) . . . no Si4 C17 H17" 107(3) . . . no H17 C17 H17' 111(4) . . . no H17 C17 H17" 101(3) . . . no H17' C17 H17" 121(4) . . . no Si4 C18 H18 104(4) . . . no Si4 C18 H18' 108(4) . . . no Si4 C18 H18" 109(4) . . . no H18 C18 H18' 112(5) . . . no H18 C18 H18" 97(5) . . . no H18' C18 H18" 125(5) . . . no Si4 C19 H19 104(3) . . . no Si4 C19 H19' 112(4) . . . no Si4 C19 H19" 116(2) . . . no H19 C19 H19' 122(5) . . . no H19 C19 H19" 111(4) . . . no H19' C19 H19" 92(4) . . . no C21 C22 H22 123.9(19) . . . no C23 C22 H22 115.9(19) . . . no C22 C23 H23 114(2) . . . no C24 C23 H23 126(2) . . . no C23 C24 H24 121(2) . . . no C25 C24 H24 119(2) . . . no C24 C25 H25 121(2) . . . no C26 C25 H25 119(2) . . . no C21 C26 H26 118(2) . . . no C25 C26 H26 121(2) . . . no C28 C29 H29 120(3) . . . no C30 C29 H29 121(3) . . . no C29 C30 H30 118(3) . . . no C31 C30 H30 121(3) . . . no C30 C31 H31 115(2) . . . no C32 C31 H31 124(2) . . . no C31 C32 H32 122(2) . . . no C33 C32 H32 117(2) . . . no C28 C33 H33 118(2) . . . no C32 C33 H33 123(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 Cl1 V N1 Si1 58.0(2) . . . . no Cl1 V N1 C7 -93.72(18) . . . . no N2 V N1 Si1 154.8(2) . . . . no N2 V N1 C7 3.09(18) . . . . no N3 V N1 Si1 -117.0(2) . . . . no N3 V N1 C7 91.28(19) . . . . no N5 V N1 Si1 -28.3(2) . . . . no N5 V N1 C7 179.9(4) . . . . no Cl1 V N2 Si2 -94.6(2) . . . . no Cl1 V N2 C7 86.22(18) . . . . no N1 V N2 Si2 176.1(2) . . . . no N1 V N2 C7 -3.08(18) . . . . no N3 V N2 Si2 71.6(2) . . . . no N3 V N2 C7 -107.54(19) . . . . no N4 V N2 Si2 6.5(2) . . . . no N4 V N2 C7 -172.66(18) . . . . no N1 V N3 Si3 7.9(2) . . . . no N1 V N3 C20 -178.89(18) . . . . no N2 V N3 Si3 73.7(2) . . . . no N2 V N3 C20 -113.08(19) . . . . no N4 V N3 Si3 -178.1(2) . . . . no N4 V N3 C20 -4.85(18) . . . . no N5 V N3 Si3 -90.7(2) . . . . no N5 V N3 C20 82.58(19) . . . . no Cl1 V N4 Si4 -5.9(2) . . . . no Cl1 V N4 C20 -168.27(17) . . . . no N2 V N4 Si4 -106.3(2) . . . . no N2 V N4 C20 91.3(2) . . . . no N3 V N4 Si4 167.3(3) . . . . no N3 V N4 C20 4.90(18) . . . . no N5 V N4 Si4 79.5(2) . . . . no N5 V N4 C20 -82.87(19) . . . . no C1 Si1 N1 V 11.1(3) . . . . no C1 Si1 N1 C7 154.3(3) . . . . no C2 Si1 N1 V -106.1(2) . . . . no C2 Si1 N1 C7 37.0(3) . . . . no C3 Si1 N1 V 129.6(2) . . . . no C3 Si1 N1 C7 -87.3(3) . . . . no C4 Si2 N2 V 83.8(3) . . . . no C4 Si2 N2 C7 -97.3(4) . . . . no C5 Si2 N2 V -151.2(3) . . . . no C5 Si2 N2 C7 27.6(4) . . . . no C6 Si2 N2 V -32.3(3) . . . . no C6 Si2 N2 C7 146.6(3) . . . . no C14 Si3 N3 V 51.7(3) . . . . no C14 Si3 N3 C20 -119.0(3) . . . . no C15 Si3 N3 V -65.6(3) . . . . no C15 Si3 N3 C20 123.8(4) . . . . no C16 Si3 N3 V 174.6(2) . . . . no C16 Si3 N3 C20 3.9(4) . . . . no C17 Si4 N4 V 173.0(3) . . . . no C17 Si4 N4 C20 -30.4(4) . . . . no C18 Si4 N4 V -65.1(3) . . . . no C18 Si4 N4 C20 91.5(4) . . . . no C19 Si4 N4 V 53.8(4) . . . . no C19 Si4 N4 C20 -149.6(4) . . . . no V N1 C7 N2 -4.7(3) . . . . no V N1 C7 C8 172.7(3) . . . . no Si1 N1 C7 N2 -161.1(2) . . . . no Si1 N1 C7 C8 16.3(5) . . . . no V N2 C7 C8 -172.5(3) . . . . no Si2 N2 C7 N1 -174.3(2) . . . . no V N2 C7 N1 4.9(3) . . . . no Si2 N2 C7 C8 8.3(5) . . . . no V N3 C20 N4 7.6(3) . . . . no V N3 C20 C21 -169.4(3) . . . . no Si3 N3 C20 C21 4.0(5) . . . . no Si3 N3 C20 N4 -178.9(2) . . . . no V N4 C20 C21 169.5(3) . . . . no Si4 N4 C20 N3 -172.0(2) . . . . no V N4 C20 N3 -7.5(3) . . . . no Si4 N4 C20 C21 5.0(5) . . . . no N2 C7 C8 C9 59.4(5) . . . . no N1 C7 C8 C9 -117.9(4) . . . . no N1 C7 C8 C13 59.6(5) . . . . no N2 C7 C8 C13 -123.2(4) . . . . no C7 C8 C9 C10 176.0(3) . . . . no C13 C8 C9 C10 -1.5(5) . . . . no C7 C8 C13 C12 -176.2(3) . . . . no C9 C8 C13 C12 1.3(5) . . . . no C8 C9 C10 C11 -0.1(6) . . . . no C9 C10 C11 C12 1.8(6) . . . . no C10 C11 C12 C13 -1.9(6) . . . . no C11 C12 C13 C8 0.4(6) . . . . no N4 C20 C21 C26 -89.2(4) . . . . no N3 C20 C21 C22 -92.0(4) . . . . no N4 C20 C21 C22 91.2(4) . . . . no N3 C20 C21 C26 87.6(4) . . . . no C20 C21 C22 C23 -179.4(3) . . . . no C22 C21 C26 C25 0.1(6) . . . . no C26 C21 C22 C23 1.0(5) . . . . no C20 C21 C26 C25 -179.5(4) . . . . no C21 C22 C23 C24 -1.7(6) . . . . no C22 C23 C24 C25 1.2(7) . . . . no C23 C24 C25 C26 -0.1(7) . . . . no C24 C25 C26 C21 -0.6(6) . . . . no C27 C28 C33 C32 178.5(4) . . . . no C27 C28 C29 C30 -179.0(4) . . . . no C33 C28 C29 C30 0.2(6) . . . . no C29 C28 C33 C32 -0.7(6) . . . . no C28 C29 C30 C31 0.9(6) . . . . no C29 C30 C31 C32 -1.6(6) . . . . no C30 C31 C32 C33 1.2(7) . . . . no C31 C32 C33 C28 0.0(6) . . . . 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 Cl1 C19 3.631(8) . . no Cl1 C30 3.439(4) . 7_545 no Cl1 C29 3.504(4) . 7_545 no Cl1 H12 3.02(3) . 6_555 no Cl1 H19" 2.89(4) . . no Cl1 H29 3.02(4) . 7_545 no Cl1 H30 2.89(4) . 7_545 no Cl1 H23 2.88(4) . 8_555 no Si1 C13 3.487(4) . . no Si2 C9 3.521(4) . . no Si3 C22 3.953(4) . . no Si3 C26 3.923(4) . . no Si4 C22 3.951(4) . . no Si4 C26 3.832(4) . . no Si1 H13 3.32(3) . . no Si2 H9 3.22(3) . . no N5 C1 3.224(5) . . no N2 H9 2.95(3) . . no N4 H6' 2.89(4) . . no N5 H1' 2.88(4) . . no N5 H1" 2.94(4) . . no C1 N5 3.224(5) . . no C1 C27 3.312(6) . . no C2 C8 3.305(5) . . no C2 C9 3.577(6) . . no C3 C13 3.451(5) . . no C5 C8 3.279(7) . . no C5 C9 3.427(7) . . no C6 C20 3.537(6) . . no C8 C5 3.279(7) . . no C8 C2 3.305(5) . . no C9 C5 3.427(7) . . no C9 Si2 3.521(4) . . no C9 C2 3.577(6) . . no C13 Si1 3.487(4) . . no C13 C3 3.451(5) . . no C16 C26 3.537(6) . . no C16 C21 3.187(6) . . no C16 C22 3.397(6) . . no C17 C22 3.295(8) . . no C17 C21 3.186(8) . . no C19 Cl1 3.631(8) . . no C20 C6 3.537(6) . . no C21 C16 3.187(6) . . no C21 C17 3.186(8) . . no C22 C17 3.295(8) . . no C22 Si4 3.951(4) . . no C22 Si3 3.953(4) . . no C22 C16 3.397(6) . . no C23 C30 3.579(6) . 2_564 no C26 Si4 3.832(4) . . no C26 C16 3.537(6) . . no C26 Si3 3.923(4) . . no C27 C1 3.312(6) . . no C29 Cl1 3.504(4) . 7_555 no C30 C23 3.579(6) . 2_565 no C30 Cl1 3.439(4) . 7_555 no C3 H13 2.96(3) . . no C7 H15' 2.98(6) . . no C8 H5" 2.98(4) . . no C8 H2" 2.79(3) . . no C9 H5" 2.83(4) . . no C9 H2" 2.96(3) . . no C11 H24 3.03(4) . 3_455 no C13 H3' 2.82(4) . . no C13 H2" 3.08(3) . . no C14 H10 3.06(4) . 4_555 no C15 H17 2.97(4) . 3_455 no C16 H31 3.08(4) . 2_564 no C17 H32 3.08(4) . 8_554 no C21 H16' 3.01(4) . . no C21 H16" 2.88(4) . . no C21 H17' 2.75(6) . . no C22 H16' 2.85(5) . . no C22 H17' 2.91(6) . . no C26 H17' 2.92(7) . . no C26 H16" 2.88(4) . . no C27 H1' 2.86(4) . . no C27 H1" 2.96(4) . . no C30 H9 3.04(3) . 7_555 no H1 H6 2.57(6) . 8_555 no H1' N5 2.88(4) . . no H1' C27 2.86(4) . . no H1" N5 2.94(4) . . no H1" C27 2.96(4) . . no H2" C8 2.79(3) . . no H2" C9 2.96(3) . . no H2" C13 3.08(3) . . no H3' C13 2.82(4) . . no H3' H13 2.39(5) . . no H3" H14" 2.57(6) . . no H4 H5 2.43(6) . 5_555 no H4' H9 2.56(5) . . no H5 H4 2.43(6) . 5_555 no H5" C8 2.98(4) . . no H5" C9 2.83(4) . . no H6 H1 2.57(6) . 8_554 no H6' N4 2.89(4) . . no H9 Si2 3.22(3) . . no H9 N2 2.95(3) . . no H9 H4' 2.56(5) . . no H9 C30 3.04(3) . 7_545 no H9 H30 2.51(5) . 7_545 no H10 C14 3.06(4) . 4_545 no H12 Cl1 3.02(3) . 6_455 no H12 H33 2.54(5) . 6_455 no H13 Si1 3.32(3) . . no H13 C3 2.96(3) . . no H13 H3' 2.39(5) . . no H14" H3" 2.57(6) . . no H15 H17 2.58(6) . 3_455 no H15 H16 2.56(6) . 5_565 no H15' C7 2.98(6) . . no H16 H15 2.56(6) . 5_565 no H16 H16 2.35(5) . 5_565 no H16' C21 3.01(4) . . no H16' C22 2.85(5) . . no H16' H31 2.59(6) . 2_564 no H16" C21 2.88(4) . . no H16" C26 2.88(4) . . no H17 C15 2.97(4) . 3_555 no H17 H15 2.58(6) . 3_555 no H17 H32 2.58(5) . 8_554 no H17' C21 2.75(6) . . no H17' C22 2.91(6) . . no H17' C26 2.92(7) . . no H19" Cl1 2.89(4) . . no H23 Cl1 2.88(4) . 8_554 no H24 C11 3.03(4) . 3_555 no H29 Cl1 3.02(4) . 7_555 no H30 Cl1 2.89(4) . 7_555 no H30 H9 2.51(5) . 7_555 no H31 C16 3.08(4) . 2_565 no H31 H16' 2.59(6) . 2_565 no H32 C17 3.08(4) . 8_555 no H32 H17 2.58(5) . 8_555 no H33 H12 2.54(5) . 6_555 no #===END of Crystallographic Information File #=============================================================================== data_c33h41cl #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H41 Cl F10 N5 Si4 V' _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 'C33 H41 Cl F10 N5 Si4 V' _chemical_formula_weight 896.44 _chemical_compound_source 'by syntheses' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source V V .3005 .5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si .0817 .0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 10.206(2) _cell_length_b 13.176(2) _cell_length_c 17.922(3) _cell_angle_alpha 86.41(1) _cell_angle_beta 74.73(1) _cell_angle_gamma 67.63(1) _cell_volume 2148.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 130 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 18.08 _cell_measurement_theta_max 20.48 _cell_special_details ; Unit cell parameters (Duisenberg, 1992) and orientation matrix were determined from a least-squares treatment of SET4 (de Boer & Duisenberg, 1984) setting. Reduced cell calculations did not indicate any higher metric lattice symmetry and examination of the final atomic coordinates of the structure did not yield extra symmetry elements (Spek, 1988; Le Page 1987, 1988) ; _exptl_crystal_description parallelepiped _exptl_crystal_colour 'colorless transparent' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.33 _exptl_crystal_size_rad ? _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method ? _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu .48 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type ' none' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 130 _diffrn_radiation_wavelength .71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine focus sealed Philips Mo tube ' _diffrn_radiation_monochromator 'perpendicular mounted graphite' _diffrn_radiation_detector ; scintillation NaI crystal with photomultiplier ; _diffrn_measurement_device_type ; Enraf Nonius CAD-4F diffractometer ; _diffrn_measurement_method '\w/2\q' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temperature unit (Bolhuis, 1971), on an Enraf-Nonius CAD-4F diffractometer. Graphite-monochromated Mo K\a radiation, \w/2\q scan, \D\w = (0.95 + 0.34 tg \q)\%. ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 180 _diffrn_standards_decay_% 1.0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -1 4 -1 -4 -1 -3 -1 -2 # number of measured reflections (redundant set) _diffrn_reflns_number 8473 _diffrn_reflns_av_R_equivalents 0.1167 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_reduction_process ; Intensity data were corrected for Lorentz and polarization effects, scale variation, but not for absorption and reduced to F~o~^2^ ; # number of unique reflections _reflns_number_total 8160 _reflns_number_gt 7274 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-UNIX Software Version 5.1, 1994' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1993)' _computing_structure_solution ; DIRDIF-97 (Beurskens et al., 1997) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTO (Meetsma, 1997) ORTEP (Burnett et al., 1996) PLATON (Spek, 1994, 1996) ; _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+1.0579P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8144 _refine_ls_number_parameters 650 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0986 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max .408 _refine_diff_density_min -.355 _refine_diff_density_rms .056 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv V1 Uani .11395(3) .06864(2) .29807(2) 1.000 .0207(1) Cl Uani .20139(6) .01440(4) .40624(4) 1.000 .0441(2) Si1 Uani -.01484(6) -.15285(4) .33650(4) 1.000 .0329(2) Si2 Uani .47068(5) -.06554(4) .17305(4) 1.000 .0286(2) Si3 Uani -.03983(5) .14824(4) .13432(3) 1.000 .0252(2) Si4 Uani .21676(6) .29445(4) .32372(4) 1.000 .0281(2) F1 Uani .17591(14) -.18328(10) .10414(8) 1.000 .0418(4) F2 Uani .30589(17) -.38955(12) .04248(9) 1.000 .0540(5) F3 Uani .49431(16) -.54791(10) .10902(9) 1.000 .0511(5) F4 Uani .55101(14) -.49947(9) .23945(9) 1.000 .0454(5) F5 Uani .42173(13) -.29348(9) .30150(8) 1.000 .0374(4) F6 Uani .24471(14) .28251(10) .07723(7) 1.000 .0405(4) F7 Uani .16730(17) .47766(11) .01185(8) 1.000 .0496(5) F8 Uani -.07418(18) .64989(10) .08626(10) 1.000 .0586(6) F9 Uani -.24223(14) .62160(9) .22538(10) 1.000 .0531(5) F10 Uani -.16570(12) .42517(9) .29043(8) 1.000 .0400(4) N1 Uani .08751(15) -.07780(12) .28505(10) 1.000 .0239(5) N2 Uani .28992(15) -.04694(11) .22251(9) 1.000 .0225(4) N3 Uani .04079(15) .16042(11) .20641(10) 1.000 .0233(5) N4 Uani .15092(16) .21713(11) .27870(10) 1.000 .0239(5) N5 Uani -.10079(17) .16518(13) .36848(10) 1.000 .0305(5) C1 Uani .22202(18) -.11608(13) .23851(11) 1.000 .0220(5) C2 Uani .29383(18) -.23247(14) .20482(12) 1.000 .0242(6) C3 Uani .2683(2) -.26016(15) .13877(13) 1.000 .0299(6) C4 Uani .3343(2) -.36517(17) .10624(13) 1.000 .0346(7) C5 Uani .4306(2) -.44600(15) .14024(14) 1.000 .0349(7) C6 Uani .4583(2) -.42122(14) .20561(13) 1.000 .0309(6) C7 Uani .3904(2) -.31500(14) .23787(12) 1.000 .0271(6) C8 Uani -.2014(2) -.0541(2) .38370(16) 1.000 .0411(8) C9 Uani -.0295(3) -.2522(2) .2724(2) 1.000 .0484(9) C10 Uani .0743(4) -.2296(3) .4119(3) 1.000 .0708(14) C11 Uani .4670(2) .06498(18) .12749(18) 1.000 .0421(8) C12 Uani .5804(3) -.0987(2) .24522(18) 1.000 .0430(8) C13 Uani .5539(3) -.1755(2) .09503(17) 1.000 .0456(8) C14 Uani .08159(18) .23788(13) .22409(11) 1.000 .0236(5) C15 Uani .04267(19) .34774(13) .18594(12) 1.000 .0259(6) C16 Uani .1241(2) .36487(15) .11555(13) 1.000 .0298(6) C17 Uani .0867(2) .46538(16) .08118(14) 1.000 .0360(7) C18 Uani -.0367(3) .55210(15) .11896(15) 1.000 .0390(8) C19 Uani -.1209(2) .53795(15) .18902(15) 1.000 .0374(7) C20 Uani -.0811(2) .43662(15) .22162(13) 1.000 .0304(6) C21 Uani -.1703(3) .2820(2) .1114(2) 1.000 .0563(12) C22 Uani -.1443(3) .0592(2) .17086(16) 1.000 .0383(8) C23 Uani .1070(3) .0840(3) .04560(17) 1.000 .0495(10) C24B Uani .0642(8) .3836(11) .4043(6) .60(3) .053(2) C25 Uani .2673(6) .3974(4) .2601(3) 1.000 .0830(19) C26D Uani .4001(15) .2019(10) .3340(11) .60(3) .065(4) C27 Uani -.2163(2) .21676(15) .40341(12) 1.000 .0279(6) C28 Uani -.36372(19) .28074(16) .44614(12) 1.000 .0287(6) C29 Uani -.4246(2) .2451(2) .51625(15) 1.000 .0429(8) C30 Uani -.5676(3) .3076(3) .55522(17) 1.000 .0550(10) C31 Uani -.6470(2) .4030(2) .52526(17) 1.000 .0507(9) C32 Uani -.5863(2) .43776(19) .45619(17) 1.000 .0449(8) C33 Uani -.4434(2) .37738(16) .41563(15) 1.000 .0353(7) C24A Uani .0977(19) .3350(19) .4191(9) .40(3) .061(4) C26C Uani .362(2) .2025(11) .3678(13) .40(3) .050(5) H8" Uiso -.248(3) -.005(3) .3452(18) 1.000 .060(8) H8 Uiso -.198(3) -.008(3) .4243(19) 1.000 .067(9) H8' Uiso -.255(4) -.092(3) .403(2) 1.000 .077(10) H9" Uiso .057(3) -.317(2) .2542(16) 1.000 .056(8) H10 Uiso .172(5) -.274(4) .397(2) 1.000 .111(15) H10' Uiso .023(4) -.258(3) .437(2) 1.000 .086(12) H10" Uiso .085(5) -.181(3) .442(2) 1.000 .097(15) H11 Uiso .414(4) .074(3) .090(2) 1.000 .080(11) H9 Uiso -.051(3) -.226(2) .2239(19) 1.000 .054(9) H9' Uiso -.108(4) -.280(3) .2980(19) 1.000 .075(9) H12 Uiso .534(4) -.049(3) .288(2) 1.000 .087(11) H12' Uiso .676(4) -.101(3) .223(2) 1.000 .092(11) H12" Uiso .590(3) -.167(3) .2638(17) 1.000 .060(8) H13 Uiso .570(4) -.249(3) .113(2) 1.000 .080(10) H13' Uiso .648(4) -.175(3) .067(2) 1.000 .085(11) H13" Uiso .493(3) -.165(2) .0601(18) 1.000 .061(9) H21 Uiso -.248(3) .318(3) .1652(19) 1.000 .065(9) H21' Uiso -.220(4) .264(3) .081(2) 1.000 .076(10) H21" Uiso -.131(4) .333(3) .0897(19) 1.000 .075(10) H22 Uiso -.079(3) -.013(3) .1825(18) 1.000 .064(9) H22' Uiso -.187(3) .048(2) .1336(17) 1.000 .054(8) H22" Uiso -.223(3) .093(2) .2154(16) 1.000 .041(7) H23 Uiso .152(4) .128(3) .0268(19) 1.000 .069(9) H23' Uiso .062(4) .075(3) .006(2) 1.000 .073(10) H23" Uiso .181(4) .010(3) .058(2) 1.000 .082(11) H24D Uiso -.00581 .44302 .38242 .60(3) .0791 H24E Uiso .10484 .41505 .43640 .60(3) .0791 H24F Uiso .01399 .33936 .43615 .60(3) .0791 H25 Uiso .311(8) .379(6) .213(5) 1.000 .22(4) H25' Uiso .307(4) .436(3) .288(2) 1.000 .089(11) H25" Uiso .173(5) .455(4) .267(3) 1.000 .115(18) H26D Uiso .39110 .13971 .36487 .60(3) .0972 H26E Uiso .43986 .24241 .35989 .60(3) .0972 H26F Uiso .46609 .17476 .28263 .60(3) .0972 H29 Uiso -.375(3) .180(3) .5331(17) 1.000 .059(8) H30 Uiso -.608(3) .286(3) .601(2) 1.000 .069(10) H31 Uiso -.741(4) .441(3) .5545(19) 1.000 .077(10) H32 Uiso -.643(3) .503(2) .4394(17) 1.000 .057(8) H33 Uiso -.396(3) .400(2) .3652(16) 1.000 .048(7) H11' Uiso .560(4) .059(2) .1062(18) 1.000 .065(9) H11" Uiso .431(3) .126(2) .1640(16) 1.000 .048(7) H24A Uiso -.00275 .37721 .41559 .40(3) .0925 H24B Uiso .13050 .38046 .44523 .40(3) .0925 H24C Uiso .10030 .26942 .44869 .40(3) .0925 H26A Uiso .32225 .15842 .40626 .40(3) .0743 H26B Uiso .39811 .24665 .39315 .40(3) .0743 H26C Uiso .44349 .15371 .32747 .40(3) .0743 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 V1 .0185(1) .0193(1) .0233(2) .0027(1) -.0086(1) -.0041(1) Cl .0534(3) .0419(3) .0340(4) .0038(2) -.0271(3) -.0045(2) Si1 .0288(3) .0328(3) .0404(4) .0116(2) -.0102(2) -.0161(2) Si2 .0186(2) .0244(2) .0380(4) .0036(2) -.0039(2) -.0055(2) Si3 .0269(2) .0248(2) .0263(4) .0043(2) -.0130(2) -.0089(2) Si4 .0311(3) .0252(2) .0329(4) .0012(2) -.0127(2) -.0129(2) F1 .0502(7) .0369(6) .0395(9) .0053(5) -.0289(6) -.0070(5) F2 .0727(10) .0495(8) .0430(10) -.0108(7) -.0267(7) -.0168(7) F3 .0594(8) .0268(6) .0559(10) -.0124(6) -.0096(7) -.0055(6) F4 .0455(7) .0245(6) .0600(10) .0088(5) -.0242(6) -.0005(5) F5 .0432(7) .0327(6) .0389(9) .0042(5) -.0249(6) -.0080(5) F6 .0427(7) .0327(6) .0350(8) .0022(5) -.0003(5) -.0088(5) F7 .0714(9) .0509(8) .0380(9) .0201(6) -.0186(7) -.0355(7) F8 .0754(10) .0275(6) .0829(12) .0276(7) -.0414(9) -.0204(6) F9 .0415(7) .0217(6) .0866(12) -.0016(6) -.0208(7) .0017(5) F10 .0312(6) .0329(6) .0446(9) .0001(5) -.0025(5) -.0045(5) N1 .0216(7) .0240(7) .0271(10) .0053(6) -.0096(6) -.0083(5) N2 .0198(6) .0204(6) .0254(10) .0020(6) -.0067(6) -.0052(5) N3 .0216(7) .0203(6) .0272(10) .0041(6) -.0090(6) -.0057(5) N4 .0251(7) .0218(7) .0263(11) .0021(6) -.0112(6) -.0076(6) N5 .0275(8) .0284(8) .0317(11) .0028(7) -.0075(7) -.0067(6) C1 .0235(8) .0202(7) .0230(12) .0042(7) -.0127(7) -.0050(6) C2 .0244(8) .0218(8) .0264(13) .0016(7) -.0075(7) -.0083(6) C3 .0311(9) .0267(9) .0320(14) .0050(8) -.0133(8) -.0083(7) C4 .0431(11) .0369(10) .0267(14) -.0035(9) -.0113(9) -.0159(9) C5 .0385(10) .0232(9) .0374(15) -.0040(8) -.0046(9) -.0083(8) C6 .0303(9) .0224(8) .0371(15) .0082(8) -.0118(8) -.0058(7) C7 .0295(9) .0253(8) .0287(14) .0037(7) -.0121(8) -.0100(7) C8 .0348(11) .0497(13) .0393(17) .0010(11) .0011(10) -.0236(10) C9 .0364(12) .0367(11) .073(2) -.0056(12) -.0047(12) -.0200(10) C10 .065(2) .085(2) .075(3) .056(2) -.0321(18) -.0408(18) C11 .0286(10) .0353(11) .0578(19) .0133(11) -.0046(10) -.0131(8) C12 .0281(10) .0388(11) .064(2) .0076(11) -.0205(11) -.0099(9) C13 .0354(11) .0411(12) .0463(18) -.0049(10) .0094(11) -.0116(9) C14 .0209(8) .0191(7) .0264(12) .0028(7) -.0048(7) -.0040(6) C15 .0295(9) .0190(8) .0316(13) .0036(7) -.0135(8) -.0084(7) C16 .0343(9) .0253(8) .0318(14) .0033(8) -.0123(8) -.0113(7) C17 .0499(12) .0335(10) .0354(15) .0123(9) -.0193(10) -.0236(9) C18 .0522(12) .0224(9) .0535(17) .0155(9) -.0322(11) -.0160(8) C19 .0360(10) .0202(8) .0563(17) .0018(9) -.0206(10) -.0051(7) C20 .0289(9) .0243(8) .0380(14) .0025(8) -.0121(8) -.0079(7) C21 .0683(18) .0367(12) .080(3) .0156(13) -.0575(18) -.0139(12) C22 .0360(11) .0486(13) .0422(17) .0102(11) -.0192(11) -.0243(10) C23 .0540(15) .0680(17) .0330(18) -.0089(12) -.0016(12) -.0349(14) C24B .046(3) .056(4) .052(4) -.024(3) -.002(2) -.018(3) C25 .133(4) .104(3) .079(3) .040(2) -.059(3) -.102(3) C26D .057(5) .055(3) .096(10) -.020(6) -.054(5) -.010(3) C27 .0289(9) .0290(9) .0248(13) .0024(8) -.0097(8) -.0083(7) C28 .0223(8) .0335(9) .0279(13) -.0042(8) -.0073(7) -.0065(7) C29 .0293(10) .0570(14) .0344(16) .0077(11) -.0096(9) -.0076(10) C30 .0301(11) .089(2) .0348(18) .0011(14) -.0022(10) -.0143(12) C31 .0229(10) .0653(16) .0505(19) -.0226(13) -.0058(10) -.0008(10) C32 .0306(10) .0351(11) .0629(19) -.0085(11) -.0180(11) -.0003(9) C33 .0309(10) .0315(10) .0427(16) -.0010(9) -.0135(9) -.0079(8) C24A .056(7) .068(8) .066(7) -.026(6) .000(5) -.036(7) C26C .063(8) .028(3) .073(12) -.001(5) -.050(7) -.012(4) #=============================================================================== # 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 V1 Cl 2.3060(9) . . yes V1 N1 2.0823(16) . . yes V1 N2 2.0673(16) . . yes V1 N3 2.1044(17) . . yes V1 N4 2.1210(15) . . yes V1 N5 2.1531(18) . . yes Si1 N1 1.7561(18) . . yes Si1 C8 1.854(3) . . yes Si1 C9 1.866(3) . . yes Si1 C10 1.858(5) . . yes Si2 N2 1.7524(18) . . yes Si2 C11 1.848(2) . . yes Si2 C12 1.854(3) . . yes Si2 C13 1.862(3) . . yes Si3 N3 1.7488(18) . . yes Si3 C21 1.860(3) . . yes Si3 C22 1.852(3) . . yes Si3 C23 1.854(3) . . yes Si4 N4 1.7464(18) . . yes Si4 C24B 1.878(11) . . yes Si4 C25 1.853(5) . . yes Si4 C26D 1.854(15) . . yes Si4 C24A 1.792(17) . . yes Si4 C26C 1.849(19) . . yes F1 C3 1.343(2) . . yes F2 C4 1.336(3) . . yes F3 C5 1.333(2) . . yes F4 C6 1.344(2) . . yes F5 C7 1.336(3) . . yes F6 C16 1.340(2) . . yes F7 C17 1.336(3) . . yes F8 C18 1.341(2) . . yes F9 C19 1.341(3) . . yes F10 C20 1.343(3) . . yes N1 C1 1.326(3) . . yes N2 C1 1.317(2) . . yes N3 C14 1.322(2) . . yes N4 C14 1.310(3) . . yes N5 C27 1.139(3) . . yes C1 C2 1.510(2) . . no C2 C3 1.375(3) . . no C2 C7 1.384(3) . . no C3 C4 1.376(3) . . no C4 C5 1.382(3) . . no C5 C6 1.361(3) . . no C6 C7 1.388(3) . . no C14 C15 1.517(2) . . no C15 C16 1.374(3) . . no C15 C20 1.385(3) . . no C16 C17 1.384(3) . . no C17 C18 1.379(3) . . no C18 C19 1.369(4) . . no C19 C20 1.380(3) . . no C27 C28 1.439(3) . . no C28 C29 1.386(3) . . no C28 C33 1.393(3) . . no C29 C30 1.384(4) . . no C30 C31 1.376(4) . . no C31 C32 1.366(4) . . no C32 C33 1.385(3) . . no C8 H8 .99(3) . . no C8 H8' .87(4) . . no C8 H8" 1.00(3) . . no C9 H9 .96(3) . . no C9 H9' 1.00(4) . . no C9 H9" .96(3) . . no C10 H10 .92(5) . . no C10 H10' .79(4) . . no C10 H10" .92(4) . . no C11 H11 .94(4) . . no C11 H11' .90(4) . . no C11 H11" .96(3) . . no C12 H12 .94(4) . . no C12 H12' .94(4) . . no C12 H12" .92(4) . . no C13 H13 .97(4) . . no C13 H13' .96(4) . . no C13 H13" .96(3) . . no C21 H21 1.07(3) . . no C21 H21' .93(4) . . no C21 H21" .92(4) . . no C22 H22 .98(4) . . no C22 H22' .93(3) . . no C22 H22" .96(3) . . no C23 H23 .87(4) . . no C23 H23' .98(4) . . no C23 H23" 1.03(4) . . no C24A H24B .9800 . . no C24A H24C .9804 . . no C24A H24A .9797 . . no C24B H24F .9797 . . no C24B H24E .9803 . . no C24B H24D .9801 . . no C25 H25 .85(9) . . no C25 H25' .98(4) . . no C25 H25" .95(5) . . no C26C H26C .9808 . . no C26C H26A .9793 . . no C26C H26B .9824 . . no C26D H26D .9797 . . no C26D H26E .9798 . . no C26D H26F .9800 . . no C29 H29 .89(4) . . no C30 H30 .90(4) . . no C31 H31 .92(4) . . no C32 H32 .92(3) . . no C33 H33 .99(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 Cl V1 N1 93.73(5) . . . yes Cl V1 N2 95.60(5) . . . yes Cl V1 N3 163.31(5) . . . yes Cl V1 N4 99.52(5) . . . yes Cl V1 N5 91.33(5) . . . yes N1 V1 N2 65.59(6) . . . yes N1 V1 N3 102.94(6) . . . yes N1 V1 N4 164.65(7) . . . yes N1 V1 N5 100.34(7) . . . yes N2 V1 N3 92.05(6) . . . yes N2 V1 N4 105.13(6) . . . yes N2 V1 N5 164.63(7) . . . yes N3 V1 N4 64.10(6) . . . yes N3 V1 N5 84.98(7) . . . yes N4 V1 N5 87.15(7) . . . yes N1 Si1 C8 108.06(10) . . . yes N1 Si1 C9 112.29(12) . . . yes N1 Si1 C10 109.00(15) . . . yes C8 Si1 C9 109.16(13) . . . yes C8 Si1 C10 109.32(17) . . . yes C9 Si1 C10 108.96(16) . . . yes N2 Si2 C11 107.48(9) . . . yes N2 Si2 C12 107.68(12) . . . yes N2 Si2 C13 113.27(12) . . . yes C11 Si2 C12 110.54(12) . . . yes C11 Si2 C13 107.77(13) . . . yes C12 Si2 C13 110.08(13) . . . yes N3 Si3 C21 113.11(11) . . . yes N3 Si3 C22 107.26(11) . . . yes N3 Si3 C23 108.89(12) . . . yes C21 Si3 C22 107.74(14) . . . yes C21 Si3 C23 109.62(15) . . . yes C22 Si3 C23 110.18(14) . . . yes N4 Si4 C24B 109.4(3) . . . yes N4 Si4 C25 112.89(19) . . . yes N4 Si4 C26D 107.2(5) . . . yes N4 Si4 C24A 107.7(7) . . . yes N4 Si4 C26C 110.1(5) . . . yes C24B Si4 C25 102.1(4) . . . yes C24B Si4 C26D 124.7(7) . . . yes C25 Si4 C26D 100.2(5) . . . yes C24A Si4 C25 120.2(8) . . . yes C25 Si4 C26C 114.8(7) . . . yes C24A Si4 C26C 88.7(10) . . . yes V1 N1 Si1 138.65(10) . . . yes V1 N1 C1 88.42(11) . . . yes Si1 N1 C1 128.06(12) . . . yes V1 N2 Si2 137.67(9) . . . yes V1 N2 C1 89.29(11) . . . yes Si2 N2 C1 131.74(13) . . . yes V1 N3 Si3 138.08(8) . . . yes V1 N3 C14 89.61(12) . . . yes Si3 N3 C14 132.31(13) . . . yes V1 N4 Si4 136.99(9) . . . yes V1 N4 C14 89.21(11) . . . yes Si4 N4 C14 133.08(12) . . . yes V1 N5 C27 177.51(17) . . . yes N1 C1 N2 116.51(15) . . . yes N1 C1 C2 122.01(17) . . . yes N2 C1 C2 121.48(17) . . . yes C1 C2 C3 121.14(17) . . . no C1 C2 C7 121.61(18) . . . no C3 C2 C7 117.24(17) . . . no F1 C3 C2 119.77(17) . . . yes F1 C3 C4 118.0(2) . . . yes C2 C3 C4 122.23(19) . . . no F2 C4 C3 120.7(2) . . . yes F2 C4 C5 119.90(19) . . . yes C3 C4 C5 119.4(2) . . . no F3 C5 C4 119.5(2) . . . yes F3 C5 C6 120.65(18) . . . yes C4 C5 C6 119.80(18) . . . no F4 C6 C5 120.26(17) . . . yes F4 C6 C7 119.65(19) . . . yes C5 C6 C7 120.09(18) . . . no F5 C7 C2 120.38(16) . . . yes F5 C7 C6 118.37(17) . . . yes C2 C7 C6 121.24(19) . . . no N3 C14 N4 116.78(15) . . . yes N3 C14 C15 121.46(17) . . . yes N4 C14 C15 121.68(16) . . . yes C14 C15 C16 123.19(17) . . . no C14 C15 C20 120.14(18) . . . no C16 C15 C20 116.67(17) . . . no F6 C16 C15 120.11(16) . . . yes F6 C16 C17 117.3(2) . . . yes C15 C16 C17 122.56(19) . . . no F7 C17 C16 120.52(19) . . . yes F7 C17 C18 120.51(19) . . . yes C16 C17 C18 119.0(2) . . . no F8 C18 C17 119.5(2) . . . yes F8 C18 C19 120.3(2) . . . yes C17 C18 C19 120.11(19) . . . no F9 C19 C18 120.30(18) . . . yes F9 C19 C20 120.1(2) . . . yes C18 C19 C20 119.6(2) . . . no F10 C20 C15 119.60(17) . . . yes F10 C20 C19 118.25(18) . . . yes C15 C20 C19 122.1(2) . . . no N5 C27 C28 178.4(2) . . . yes C27 C28 C29 119.81(19) . . . no C27 C28 C33 119.05(19) . . . no C29 C28 C33 121.1(2) . . . no C28 C29 C30 118.3(2) . . . no C29 C30 C31 120.8(3) . . . no C30 C31 C32 120.6(2) . . . no C31 C32 C33 120.2(2) . . . no C28 C33 C32 118.9(2) . . . no Si1 C8 H8 111(2) . . . no Si1 C8 H8' 107(3) . . . no Si1 C8 H8" 111.4(19) . . . no H8 C8 H8' 111(3) . . . no H8 C8 H8" 109(3) . . . no H8' C8 H8" 107(3) . . . no Si1 C9 H9 117.0(16) . . . no Si1 C9 H9' 112(2) . . . no Si1 C9 H9" 116.6(19) . . . no H9 C9 H9' 104(3) . . . no H9 C9 H9" 100(2) . . . no H9' C9 H9" 105(3) . . . no Si1 C10 H10 118(2) . . . no Si1 C10 H10' 108(3) . . . no Si1 C10 H10" 109(2) . . . no H10 C10 H10' 115(4) . . . no H10 C10 H10" 96(4) . . . no H10' C10 H10" 111(4) . . . no Si2 C11 H11 105(2) . . . no Si2 C11 H11' 108.4(16) . . . no Si2 C11 H11" 113.6(16) . . . no H11 C11 H11' 112(3) . . . no H11 C11 H11" 115(3) . . . no H11' C11 H11" 102(3) . . . no Si2 C12 H12 111(3) . . . no Si2 C12 H12' 111(2) . . . no Si2 C12 H12" 110(2) . . . no H12 C12 H12' 111(4) . . . no H12 C12 H12" 107(3) . . . no H12' C12 H12" 107(3) . . . no Si2 C13 H13 115(2) . . . no Si2 C13 H13' 108(2) . . . no Si2 C13 H13" 111.9(16) . . . no H13 C13 H13' 107(3) . . . no H13 C13 H13" 105(3) . . . no H13' C13 H13" 110(3) . . . no Si3 C21 H21 106.5(19) . . . no Si3 C21 H21' 105(2) . . . no Si3 C21 H21" 117(3) . . . no H21 C21 H21' 108(3) . . . no H21 C21 H21" 107(3) . . . no H21' C21 H21" 113(3) . . . no Si3 C22 H22 110(2) . . . no Si3 C22 H22' 110.7(18) . . . no Si3 C22 H22" 110.9(17) . . . no H22 C22 H22' 107(3) . . . no H22 C22 H22" 111(2) . . . no H22' C22 H22" 107(3) . . . no Si3 C23 H23 110(2) . . . no Si3 C23 H23' 109(2) . . . no Si3 C23 H23" 110(2) . . . no H23 C23 H23' 106(3) . . . no H23 C23 H23" 110(4) . . . no H23' C23 H23" 112(3) . . . no H24A C24A H24B 109.49 . . . no H24A C24A H24C 109.47 . . . no H24B C24A H24C 109.44 . . . no Si4 C24A H24A 109.49 . . . no Si4 C24A H24B 109.48 . . . no Si4 C24A H24C 109.46 . . . no H24D C24B H24E 109.43 . . . no H24D C24B H24F 109.49 . . . no H24E C24B H24F 109.46 . . . no Si4 C24B H24D 109.47 . . . no Si4 C24B H24E 109.46 . . . no Si4 C24B H24F 109.50 . . . no Si4 C25 H25" 100(3) . . . no Si4 C25 H25 118(5) . . . no Si4 C25 H25' 109(2) . . . no H25' C25 H25" 96(4) . . . no H25 C25 H25' 117(6) . . . no H25 C25 H25" 113(6) . . . no Si4 C26C H26A 109.68 . . . no H26A C26C H26B 109.34 . . . no Si4 C26C H26B 109.52 . . . no Si4 C26C H26C 109.60 . . . no H26A C26C H26C 109.47 . . . no H26B C26C H26C 109.22 . . . no Si4 C26D H26D 109.45 . . . no H26E C26D H26F 109.49 . . . no Si4 C26D H26F 109.43 . . . no H26D C26D H26E 109.51 . . . no Si4 C26D H26E 109.44 . . . no H26D C26D H26F 109.50 . . . no C28 C29 H29 120(2) . . . no C30 C29 H29 121(2) . . . no C29 C30 H30 119(2) . . . no C31 C30 H30 120(2) . . . no C30 C31 H31 116(2) . . . no C32 C31 H31 123(2) . . . no C31 C32 H32 117.2(19) . . . no C33 C32 H32 122.6(19) . . . no C32 C33 H33 122.4(16) . . . no C28 C33 H33 118.7(16) . . . 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 Cl V1 N1 Si1 62.56(14) . . . . no Cl V1 N1 C1 -91.89(11) . . . . no N2 V1 N1 Si1 157.02(16) . . . . no N2 V1 N1 C1 2.57(11) . . . . no N3 V1 N1 Si1 -116.65(14) . . . . no N3 V1 N1 C1 88.90(12) . . . . no N5 V1 N1 Si1 -29.47(15) . . . . no N5 V1 N1 C1 176.08(11) . . . . no Cl V1 N2 Si2 -78.21(13) . . . . no Cl V1 N2 C1 88.98(11) . . . . no N1 V1 N2 Si2 -169.78(15) . . . . no N1 V1 N2 C1 -2.59(11) . . . . no N3 V1 N2 Si2 86.94(13) . . . . no N3 V1 N2 C1 -105.87(12) . . . . no N4 V1 N2 Si2 23.24(15) . . . . no N4 V1 N2 C1 -169.57(11) . . . . no N1 V1 N3 Si3 5.27(15) . . . . no N1 V1 N3 C14 -174.54(11) . . . . no N2 V1 N3 Si3 70.68(14) . . . . no N2 V1 N3 C14 -109.13(12) . . . . no N4 V1 N3 Si3 176.53(16) . . . . no N4 V1 N3 C14 -3.28(11) . . . . no N5 V1 N3 Si3 -94.21(14) . . . . no N5 V1 N3 C14 85.98(12) . . . . no Cl V1 N4 Si4 -2.71(14) . . . . no Cl V1 N4 C14 -173.36(11) . . . . no N2 V1 N4 Si4 -101.22(14) . . . . no N2 V1 N4 C14 88.14(12) . . . . no N3 V1 N4 Si4 173.96(16) . . . . no N3 V1 N4 C14 3.31(11) . . . . no N5 V1 N4 Si4 88.15(14) . . . . no N5 V1 N4 C14 -82.49(12) . . . . no C8 Si1 N1 V1 38.72(18) . . . . no C8 Si1 N1 C1 -174.48(18) . . . . no C9 Si1 N1 V1 159.17(15) . . . . no C9 Si1 N1 C1 -54.0(2) . . . . no C10 Si1 N1 V1 -80.0(2) . . . . no C10 Si1 N1 C1 66.8(2) . . . . no C11 Si2 N2 V1 -47.04(17) . . . . no C11 Si2 N2 C1 150.25(19) . . . . no C12 Si2 N2 V1 72.07(15) . . . . no C12 Si2 N2 C1 -90.6(2) . . . . no C13 Si2 N2 V1 -165.97(14) . . . . no C13 Si2 N2 C1 31.3(2) . . . . no C21 Si3 N3 V1 145.76(16) . . . . no C21 Si3 N3 C14 -34.5(2) . . . . no C22 Si3 N3 V1 27.11(17) . . . . no C22 Si3 N3 C14 -153.15(19) . . . . no C23 Si3 N3 V1 -92.11(18) . . . . no C23 Si3 N3 C14 87.6(2) . . . . no C24B Si4 N4 V1 -83.0(4) . . . . no C24B Si4 N4 C14 84.1(4) . . . . no C25 Si4 N4 V1 164.1(2) . . . . no C25 Si4 N4 C14 -28.8(3) . . . . no C26D Si4 N4 V1 54.7(6) . . . . no C26D Si4 N4 C14 -138.1(6) . . . . no V1 N1 C1 N2 -4.11(17) . . . . no Si1 N1 C1 N2 -162.90(14) . . . . no Si1 N1 C1 C2 17.6(3) . . . . no V1 N1 C1 C2 176.41(17) . . . . no Si2 N2 C1 N1 172.60(14) . . . . no Si2 N2 C1 C2 -7.9(3) . . . . no V1 N2 C1 N1 4.14(17) . . . . no V1 N2 C1 C2 -176.38(16) . . . . no V1 N3 C14 C15 -171.45(16) . . . . no Si3 N3 C14 N4 -174.47(15) . . . . no V1 N3 C14 N4 5.36(18) . . . . no Si3 N3 C14 C15 8.7(3) . . . . no Si4 N4 C14 N3 -176.59(15) . . . . no Si4 N4 C14 C15 .2(3) . . . . no V1 N4 C14 N3 -5.32(18) . . . . no V1 N4 C14 C15 171.49(17) . . . . no N2 C1 C2 C7 82.9(3) . . . . no N1 C1 C2 C3 83.9(3) . . . . no N1 C1 C2 C7 -97.6(2) . . . . no N2 C1 C2 C3 -95.6(2) . . . . no C1 C2 C3 F1 -1.3(3) . . . . no C1 C2 C3 C4 178.9(2) . . . . no C7 C2 C3 F1 -179.82(19) . . . . no C3 C2 C7 C6 -.1(3) . . . . no C7 C2 C3 C4 .3(3) . . . . no C1 C2 C7 F5 .6(3) . . . . no C1 C2 C7 C6 -178.6(2) . . . . no C3 C2 C7 F5 179.09(19) . . . . no C2 C3 C4 F2 179.3(2) . . . . no C2 C3 C4 C5 -.5(3) . . . . no F1 C3 C4 C5 179.6(2) . . . . no F1 C3 C4 F2 -.5(3) . . . . no F2 C4 C5 F3 -.1(3) . . . . no F2 C4 C5 C6 -179.4(2) . . . . no C3 C4 C5 F3 179.8(2) . . . . no C3 C4 C5 C6 .5(4) . . . . no F3 C5 C6 C7 -179.5(2) . . . . no C4 C5 C6 F4 179.5(2) . . . . no F3 C5 C6 F4 .2(4) . . . . no C4 C5 C6 C7 -.2(3) . . . . no F4 C6 C7 F5 1.1(3) . . . . no F4 C6 C7 C2 -179.7(2) . . . . no C5 C6 C7 C2 .0(3) . . . . no C5 C6 C7 F5 -179.2(2) . . . . no N3 C14 C15 C20 94.9(2) . . . . no N4 C14 C15 C16 99.1(3) . . . . no N3 C14 C15 C16 -84.3(3) . . . . no N4 C14 C15 C20 -81.7(3) . . . . no C20 C15 C16 F6 -179.47(19) . . . . no C14 C15 C20 F10 .5(3) . . . . no C14 C15 C20 C19 -179.9(2) . . . . no C20 C15 C16 C17 .3(3) . . . . no C14 C15 C16 F6 -.2(3) . . . . no C14 C15 C16 C17 179.5(2) . . . . no C16 C15 C20 F10 179.8(2) . . . . no C16 C15 C20 C19 -.6(3) . . . . no C15 C16 C17 C18 .3(4) . . . . no F6 C16 C17 F7 1.3(3) . . . . no C15 C16 C17 F7 -178.5(2) . . . . no F6 C16 C17 C18 -180.0(2) . . . . no C16 C17 C18 C19 -.6(4) . . . . no F7 C17 C18 F8 -1.2(4) . . . . no C16 C17 C18 F8 -180.0(2) . . . . no F7 C17 C18 C19 178.2(2) . . . . no F8 C18 C19 F9 .4(4) . . . . no C17 C18 C19 C20 .3(4) . . . . no F8 C18 C19 C20 179.7(2) . . . . no C17 C18 C19 F9 -179.0(2) . . . . no C18 C19 C20 C15 .3(4) . . . . no F9 C19 C20 F10 -.8(3) . . . . no F9 C19 C20 C15 179.6(2) . . . . no C18 C19 C20 F10 179.9(7) . . . . no C27 C28 C33 C32 178.8(2) . . . . no C27 C28 C29 C30 -178.9(2) . . . . no C33 C28 C29 C30 .5(4) . . . . no C29 C28 C33 C32 -.6(3) . . . . no C28 C29 C30 C31 -.3(4) . . . . no C29 C30 C31 C32 .2(5) . . . . no C30 C31 C32 C33 -.3(4) . . . . no C31 C32 C33 C28 .5(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 Cl C26C 3.404(19) . . no Cl H26D 2.9238 . . no Cl H26A 2.6276 . . no Cl H8 3.02(3) . 2_556 no Cl H29 2.84(4) . 2_556 no Si1 C3 3.877(2) . . no Si1 C7 3.833(2) . . no Si2 C7 3.728(2) . . no Si3 C16 3.779(2) . . no Si4 C20 3.777(2) . . no Si1 H22 3.29(3) . . no Si4 H11" 3.42(3) . . no F1 F2 2.688(2) . . no F2 F3 2.705(2) . . no F2 F7 2.789(2) . 1_545 no F2 F1 2.688(2) . . no F2 F3 2.880(2) . 2_645 no F3 F2 2.705(2) . . no F3 F4 2.718(2) . . no F3 C21 3.312(3) . 1_645 no F3 C25 3.308(6) . 1_545 no F3 F2 2.880(2) . 2_645 no F4 F10 3.045(2) . 1_645 no F4 F9 3.048(2) . 1_645 no F4 F5 2.6876(17) . . no F4 F3 2.718(2) . . no F5 F9 3.111(2) . 1_645 no F5 C30 3.254(4) . 2_556 no F5 F4 2.6876(17) . . no F6 C13 3.277(3) . 2_655 no F6 F7 2.6782(19) . . no F6 C11 3.159(3) . . no F7 F6 2.6782(19) . . no F7 F8 3.047(2) . 2_565 no F7 C18 3.096(3) . 2_565 no F7 F2 2.789(2) . 1_565 no F7 F8 2.719(2) . . no F7 C17 3.271(3) . 2_565 no F8 F9 2.723(2) . . no F8 F7 2.719(2) . . no F8 F7 3.047(2) . 2_565 no F9 F5 3.111(2) . 1_465 no F9 F4 3.048(2) . 1_465 no F9 F8 2.723(2) . . no F9 F10 2.6890(18) . . no F10 C33 3.361(3) . . no F10 F4 3.045(2) . 1_465 no F10 F9 2.6890(18) . . no F1 H23" 2.64(4) . . no F1 H22 2.79(4) . . no F2 H21' 2.80(4) . 2_555 no F3 H25 2.69(9) . 1_545 no F4 H33 2.62(3) . 1_645 no F4 H21 2.64(4) . 1_645 no F4 H25' 2.84(4) . 1_545 no F5 H10 2.60(5) . . no F5 H12" 2.76(4) . . no F6 H13' 2.77(4) . 2_655 no F6 H11 2.66(4) . . no F6 H23 2.83(4) . . no F9 H9' 2.78(4) . 1_565 no F9 H12" 2.67(4) . 1_465 no F10 H24D 2.6822 . . no F10 H33 2.51(3) . . no N1 C22 3.447(3) . . no N5 C8 3.389(3) . . no N1 H22 2.71(3) . . no N4 H11" 2.91(3) . . no N5 H8 2.85(4) . . no C2 C9 3.306(4) . . no C2 C13 3.172(4) . . no C3 C9 3.307(4) . . no C3 C13 3.394(4) . . no C3 Si1 3.877(2) . . no C5 C25 3.439(6) . 1_545 no C6 C25 3.566(6) . 1_545 no C7 Si2 3.728(2) . . no C7 C13 3.495(4) . . no C7 Si1 3.833(2) . . no C8 C27 3.550(3) . . no C8 N5 3.389(3) . . no C9 C3 3.307(4) . . no C9 C2 3.306(4) . . no C10 C24A 3.565(19) . 2_556 no C11 F6 3.159(3) . . no C13 F6 3.277(3) . 2_655 no C13 C7 3.495(4) . . no C13 C3 3.394(4) . . no C13 C2 3.172(4) . . no C15 C25 3.210(7) . . no C15 C21 3.220(4) . . no C16 C21 3.585(4) . . no C16 C25 3.412(6) . . no C16 Si3 3.779(2) . . no C17 F7 3.271(3) . 2_565 no C18 F7 3.096(3) . 2_565 no C20 Si4 3.777(2) . . no C20 C21 3.427(4) . . no C21 C15 3.220(4) . . no C21 F3 3.312(3) . 1_465 no C21 C20 3.427(4) . . no C21 C16 3.585(4) . . no C22 N1 3.447(3) . . no C24A C10 3.565(19) . 2_556 no C25 F3 3.308(6) . 1_565 no C25 C5 3.439(6) . 1_565 no C25 C6 3.566(6) . 1_565 no C25 C15 3.210(7) . . no C25 C16 3.412(6) . . no C26C Cl 3.404(19) . . no C27 C8 3.550(3) . . no C30 F5 3.254(4) . 2_556 no C32 C32 3.498(4) . 2_466 no C32 C33 3.596(4) . 2_466 no C33 F10 3.361(3) . . no C33 C32 3.596(4) . 2_466 no C2 H9" 2.94(3) . . no C2 H13 2.80(4) . . no C3 H9" 2.86(3) . . no C3 H13 3.05(4) . . no C3 H9 3.08(3) . . no C3 H13" 3.01(3) . . no C5 H25 3.07(8) . 1_545 no C6 H25' 2.96(4) . 1_545 no C7 H10 3.05(4) . . no C7 H13 2.82(4) . . no C10 H24C 2.8099 . 2_556 no C10 H24F 3.0864 . 2_556 no C15 H21" 2.84(4) . . no C15 H25" 2.93(5) . . no C15 H25 3.08(9) . . no C16 H25 2.96(9) . . no C16 H21" 2.94(4) . . no C20 H21" 3.05(4) . . no C20 H21 3.08(4) . . no C20 H25" 3.01(6) . . no C24A H10' 2.85(4) . 2_556 no C27 H8 2.90(4) . . no C28 H26B 3.0187 . 1_455 no C28 H26E 3.0272 . 1_455 no C31 H26B 3.0621 . 1_455 no C31 H24B 3.0959 . 1_455 no C32 H26B 2.8980 . 1_455 no C32 H26E 3.0766 . 1_455 no C33 H26E 2.8359 . 1_455 no C33 H26B 2.8804 . 1_455 no H8 C27 2.90(4) . . no H8 N5 2.85(4) . . no H8 Cl 3.02(3) . 2_556 no H8" H22" 2.59(4) . . no H9 C3 3.08(3) . . no H9' F9 2.78(4) . 1_545 no H9" C2 2.94(3) . . no H9" C3 2.86(3) . . no H10 F5 2.60(5) . . no H10 C7 3.05(4) . . no H10' H24C 2.1333 . 2_556 no H10' H24F 2.4517 . 2_556 no H10' C24A 2.85(4) . 2_556 no H11 F6 2.66(4) . . no H11" Si4 3.42(3) . . no H11" N4 2.91(3) . . no H11" H26F 2.4101 . . no H12 H26C 2.5499 . . no H12" F5 2.76(4) . . no H12" F9 2.67(4) . 1_645 no H13 C2 2.80(4) . . no H13 C3 3.05(4) . . no H13 C7 2.82(4) . . no H13' F6 2.77(3) . 2_655 no H13' H23 2.53(6) . 2_655 no H13" C3 3.01(3) . . no H21 C20 3.08(4) . . no H21 F4 2.64(4) . 1_465 no H21' F2 2.80(4) . 2_555 no H21" C15 2.84(4) . . no H21" C16 2.94(4) . . no H21" C20 3.05(4) . . no H22 F1 2.79(4) . . no H22 N1 2.71(3) . . no H22 Si1 3.29(3) . . no H22" H8" 2.59(4) . . no H23 F6 2.83(4) . . no H23 H13' 2.53(6) . 2_655 no H23" F1 2.64(4) . . no H24B C31 3.0959 . 1_655 no H24B H26B 2.5763 . . no H24C H10' 2.1333 . 2_556 no H24C H26A 2.1351 . . no H24C C10 2.8099 . 2_556 no H24D H25" 2.4133 . . no H24D H31 2.4418 . 2_466 no H24D F10 2.6822 . . no H24F C10 3.0864 . 2_556 no H24F H10' 2.4517 . 2_556 no H25 C5 3.07(8) . 1_565 no H25 C15 3.08(9) . . no H25 F3 2.69(9) . 1_565 no H25 C16 2.96(9) . . no H25' F4 2.84(4) . 1_565 no H25' C6 2.96(4) . 1_565 no H25" C15 2.93(5) . . no H25" C20 3.01(6) . . no H25" H24D 2.4133 . . no H26A Cl 2.6276 . . no H26A H24C 2.1351 . . no H26B H24B 2.5763 . . no H26B C28 3.0187 . 1_655 no H26B C31 3.0621 . 1_655 no H26B C32 2.8980 . 1_655 no H26B C33 2.8804 . 1_655 no H26C H12 2.5499 . . no H26D Cl 2.9238 . . no H26E C28 3.0272 . 1_655 no H26E C33 2.8359 . 1_655 no H26E C32 3.0766 . 1_655 no H26F H11" 2.4101 . . no H29 Cl 2.84(4) . 2_556 no H31 H24D 2.4418 . 2_466 no H33 F4 2.62(3) . 1_465 no H33 F10 2.51(3) . . 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) # C33 H33 F10 .99(3) 2.51(3) 3.361(3) 143(2) . yes #===END of Crystallographic Information File