# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Philip Mountford' 'Eric Clot' 'Ainara Nova' 'A. Daniel Schofield' 'Jonathan D. Selby' 'Pei-Jen Tiong.' _publ_contact_author_name 'Philip Mountford' _publ_contact_author_email PHILIP.MOUNTFORD@CHEM.OX.AC.UK _publ_section_title ; Single and double substrate insertion into the Ti=N bonds of terminal titanium hydrazides ; # Attachment 'B920090H_Xray_ESI.cif' data_Compound_2a _database_code_depnum_ccdc_archive 'CCDC 752046' # Local code DS9 _audit_creation_method CRYSTALS_ver_12.86 _chemical_name_systematic ; Cp*Ti{MeC(NiPr)2}{OC(O)N(NPh2)C(O)O} ; _chemical_melting_point ? _publ_section_exptl_refinement ; No special comments. H atoms were placed in calculated positions with reference to a Fourier difference map ; _cell_length_a 14.2642(3) _cell_length_b 13.3667(2) _cell_length_c 17.0300(4) _cell_angle_alpha 90 _cell_angle_beta 109.1092(8) _cell_angle_gamma 90 _cell_volume 3068.11(11) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C32 H42 N4 O4 Ti1' _chemical_formula_moiety 'C32 H42 N4 O4 Ti1' _chemical_compound_source ? _chemical_formula_weight 594.61 _cell_measurement_reflns_used 6986 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.321 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.97 _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 13753 _reflns_number_total 6980 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_theta_min 5.106 _diffrn_reflns_theta_max 27.493 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.393 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -18 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 1.79 _oxford_diffrn_Wilson_scale 14.32 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.52 _refine_diff_density_max 1.05 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 4534 _refine_ls_number_restraints 0 _refine_ls_number_parameters 370 _oxford_refine_ls_R_factor_ref 0.0511 _refine_ls_wR_factor_ref 0.0531 _refine_ls_goodness_of_fit_ref 1.1004 _refine_ls_shift/su_max 0.001126 # The values computed from all data _oxford_reflns_number_all 6980 _refine_ls_R_factor_all 0.0875 _refine_ls_wR_factor_all 0.0748 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4992 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_gt 0.0562 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.716 0.341 0.536 0.973E-01 0.136 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ti1 Ti 0.77151(3) 0.39235(3) 0.62951(3) 0.0175 1.0000 Uani . . . . . . . N1 N 0.72690(16) 0.61412(16) 0.69509(13) 0.0210 1.0000 Uani . . . . . . . N2 N 0.72139(17) 0.69707(16) 0.74299(13) 0.0244 1.0000 Uani . . . . . . . N3 N 0.90430(16) 0.35708(16) 0.71885(13) 0.0218 1.0000 Uani . . . . . . . N4 N 0.76448(16) 0.28548(17) 0.71703(14) 0.0240 1.0000 Uani . . . . . . . C1 C 0.66862(19) 0.78146(19) 0.70060(16) 0.0215 1.0000 Uani . . . . . . . C2 C 0.6781(2) 0.8115(2) 0.62518(17) 0.0266 1.0000 Uani . . . . . . . C3 C 0.6258(2) 0.8934(2) 0.58303(19) 0.0324 1.0000 Uani . . . . . . . C4 C 0.5645(2) 0.9467(2) 0.6159(2) 0.0348 1.0000 Uani . . . . . . . C5 C 0.5545(2) 0.9182(2) 0.6907(2) 0.0341 1.0000 Uani . . . . . . . C6 C 0.6055(2) 0.8346(2) 0.73291(18) 0.0284 1.0000 Uani . . . . . . . C7 C 0.76272(19) 0.68635(19) 0.82919(16) 0.0221 1.0000 Uani . . . . . . . C8 C 0.7824(2) 0.7702(2) 0.88150(17) 0.0259 1.0000 Uani . . . . . . . C9 C 0.8227(2) 0.7584(2) 0.96712(18) 0.0301 1.0000 Uani . . . . . . . C10 C 0.8457(2) 0.6648(2) 1.00218(18) 0.0327 1.0000 Uani . . . . . . . C11 C 0.8296(2) 0.5823(2) 0.95125(19) 0.0354 1.0000 Uani . . . . . . . C12 C 0.7890(2) 0.5919(2) 0.86542(18) 0.0309 1.0000 Uani . . . . . . . C13 C 0.64746(19) 0.54338(19) 0.68029(15) 0.0208 1.0000 Uani . . . . . . . C14 C 0.81374(19) 0.6074(2) 0.67169(15) 0.0215 1.0000 Uani . . . . . . . C15 C 0.8601(2) 0.2979(2) 0.75964(16) 0.0223 1.0000 Uani . . . . . . . C16 C 0.9145(2) 0.2504(3) 0.84189(19) 0.0354 1.0000 Uani . . . . . . . C17 C 1.00678(19) 0.3936(2) 0.75844(16) 0.0247 1.0000 Uani . . . . . . . C18 C 1.0517(2) 0.4269(3) 0.6935(2) 0.0381 1.0000 Uani . . . . . . . C19 C 1.0110(2) 0.4797(2) 0.81834(19) 0.0338 1.0000 Uani . . . . . . . C20 C 0.6918(2) 0.2446(2) 0.7546(2) 0.0350 1.0000 Uani . . . . . . . C21 C 0.5928(4) 0.2278(4) 0.6965(3) 0.0729 1.0000 Uani . . . . . . . C22 C 0.6836(3) 0.3130(3) 0.8243(2) 0.0437 1.0000 Uani . . . . . . . C23 C 0.6567(2) 0.3254(2) 0.50548(16) 0.0231 1.0000 Uani . . . . . . . C24 C 0.7049(2) 0.4087(2) 0.48412(15) 0.0234 1.0000 Uani . . . . . . . C25 C 0.80742(19) 0.3841(2) 0.50302(15) 0.0215 1.0000 Uani . . . . . . . C26 C 0.8224(2) 0.28666(19) 0.53767(16) 0.0226 1.0000 Uani . . . . . . . C27 C 0.7288(2) 0.25035(19) 0.53832(16) 0.0232 1.0000 Uani . . . . . . . C28 C 0.5474(2) 0.3185(3) 0.4903(2) 0.0358 1.0000 Uani . . . . . . . C29 C 0.6565(2) 0.5045(2) 0.44568(19) 0.0325 1.0000 Uani . . . . . . . C30 C 0.8827(2) 0.4499(2) 0.48474(18) 0.0285 1.0000 Uani . . . . . . . C31 C 0.9153(2) 0.2250(2) 0.56139(18) 0.0301 1.0000 Uani . . . . . . . C32 C 0.7108(3) 0.1446(2) 0.5586(2) 0.0348 1.0000 Uani . . . . . . . O1 O 0.65892(13) 0.46032(14) 0.64497(12) 0.0252 1.0000 Uani . . . . . . . O2 O 0.57697(14) 0.56385(15) 0.70151(12) 0.0296 1.0000 Uani . . . . . . . O3 O 0.82130(13) 0.52842(13) 0.63025(12) 0.0234 1.0000 Uani . . . . . . . O4 O 0.87389(14) 0.67536(14) 0.68955(13) 0.0309 1.0000 Uani . . . . . . . H21 H 0.7208 0.7754 0.6026 0.0334 1.0000 Uiso R . . . . . . H31 H 0.6324 0.9131 0.5315 0.0384 1.0000 Uiso R . . . . . . H41 H 0.5289 1.0029 0.5868 0.0401 1.0000 Uiso R . . . . . . H51 H 0.5128 0.9555 0.7134 0.0419 1.0000 Uiso R . . . . . . H61 H 0.5974 0.8137 0.7836 0.0375 1.0000 Uiso R . . . . . . H81 H 0.7681 0.8352 0.8582 0.0332 1.0000 Uiso R . . . . . . H91 H 0.8345 0.8155 1.0022 0.0354 1.0000 Uiso R . . . . . . H101 H 0.8727 0.6573 1.0608 0.0388 1.0000 Uiso R . . . . . . H111 H 0.8465 0.5177 0.9749 0.0420 1.0000 Uiso R . . . . . . H121 H 0.7783 0.5342 0.8310 0.0370 1.0000 Uiso R . . . . . . H161 H 0.9655 0.2083 0.8361 0.0449 1.0000 Uiso R . . . . . . H162 H 0.9429 0.3010 0.8817 0.0449 1.0000 Uiso R . . . . . . H163 H 0.8695 0.2116 0.8598 0.0449 1.0000 Uiso R . . . . . . H171 H 1.0456 0.3400 0.7890 0.0304 1.0000 Uiso R . . . . . . H181 H 1.0524 0.3724 0.6579 0.0482 1.0000 Uiso R . . . . . . H182 H 1.0129 0.4798 0.6618 0.0482 1.0000 Uiso R . . . . . . H183 H 1.1177 0.4497 0.7199 0.0482 1.0000 Uiso R . . . . . . H191 H 1.0776 0.5014 0.8431 0.0404 1.0000 Uiso R . . . . . . H192 H 0.9855 0.4577 0.8605 0.0404 1.0000 Uiso R . . . . . . H193 H 0.9717 0.5335 0.7886 0.0404 1.0000 Uiso R . . . . . . H201 H 0.7166 0.1819 0.7788 0.0460 1.0000 Uiso R . . . . . . H211 H 0.5510 0.2014 0.7249 0.1036 1.0000 Uiso R . . . . . . H212 H 0.5666 0.2897 0.6714 0.1036 1.0000 Uiso R . . . . . . H213 H 0.5963 0.1821 0.6549 0.1036 1.0000 Uiso R . . . . . . H221 H 0.6377 0.2851 0.8480 0.0589 1.0000 Uiso R . . . . . . H222 H 0.7466 0.3196 0.8660 0.0589 1.0000 Uiso R . . . . . . H223 H 0.6608 0.3770 0.8017 0.0589 1.0000 Uiso R . . . . . . H281 H 0.5325 0.2558 0.5098 0.0440 1.0000 Uiso R . . . . . . H282 H 0.5279 0.3709 0.5194 0.0440 1.0000 Uiso R . . . . . . H283 H 0.5124 0.3245 0.4326 0.0440 1.0000 Uiso R . . . . . . H291 H 0.6150 0.4923 0.3902 0.0402 1.0000 Uiso R . . . . . . H292 H 0.7065 0.5515 0.4458 0.0402 1.0000 Uiso R . . . . . . H293 H 0.6181 0.5299 0.4775 0.0402 1.0000 Uiso R . . . . . . H301 H 0.8867 0.5117 0.5132 0.0389 1.0000 Uiso R . . . . . . H302 H 0.9456 0.4179 0.5029 0.0389 1.0000 Uiso R . . . . . . H303 H 0.8636 0.4619 0.4266 0.0389 1.0000 Uiso R . . . . . . H311 H 0.9045 0.1671 0.5272 0.0389 1.0000 Uiso R . . . . . . H312 H 0.9679 0.2634 0.5540 0.0389 1.0000 Uiso R . . . . . . H313 H 0.9322 0.2056 0.6180 0.0389 1.0000 Uiso R . . . . . . H321 H 0.7436 0.1000 0.5327 0.0456 1.0000 Uiso R . . . . . . H322 H 0.7356 0.1354 0.6171 0.0456 1.0000 Uiso R . . . . . . H323 H 0.6415 0.1316 0.5390 0.0456 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0210(2) 0.0157(2) 0.0167(2) -0.00123(19) 0.00726(16) -0.00121(18) N1 0.0265(11) 0.0153(10) 0.0220(10) -0.0046(9) 0.0093(8) -0.0016(9) N2 0.0346(12) 0.0180(11) 0.0200(11) -0.0026(9) 0.0080(9) 0.0056(9) N3 0.0228(11) 0.0220(11) 0.0199(10) 0.0024(9) 0.0060(9) -0.0001(8) N4 0.0257(11) 0.0249(11) 0.0234(11) 0.0022(9) 0.0108(9) -0.0027(9) C1 0.0217(12) 0.0166(12) 0.0248(13) -0.0017(10) 0.0055(10) -0.0016(10) C2 0.0311(14) 0.0239(14) 0.0273(14) 0.0010(11) 0.0128(11) 0.0012(11) C3 0.0352(15) 0.0270(14) 0.0323(14) 0.0058(13) 0.0073(12) -0.0017(13) C4 0.0290(15) 0.0245(15) 0.0443(17) 0.0048(13) 0.0029(13) 0.0035(12) C5 0.0282(15) 0.0273(15) 0.0471(18) -0.0030(13) 0.0125(13) 0.0060(11) C6 0.0278(14) 0.0276(14) 0.0325(15) -0.0027(12) 0.0133(12) 0.0014(11) C7 0.0245(13) 0.0219(13) 0.0203(12) -0.0005(10) 0.0080(10) 0.0020(10) C8 0.0312(15) 0.0198(13) 0.0262(13) -0.0011(11) 0.0090(11) 0.0007(11) C9 0.0303(15) 0.0339(15) 0.0250(14) -0.0078(12) 0.0076(11) -0.0004(12) C10 0.0331(15) 0.0410(17) 0.0225(14) 0.0017(13) 0.0072(12) 0.0034(13) C11 0.0443(18) 0.0289(15) 0.0289(15) 0.0062(12) 0.0066(13) 0.0051(13) C12 0.0405(16) 0.0226(14) 0.0262(13) -0.0009(11) 0.0062(12) 0.0028(12) C13 0.0242(13) 0.0210(12) 0.0181(11) 0.0036(10) 0.0079(10) 0.0020(10) C14 0.0269(13) 0.0160(12) 0.0209(12) -0.0002(10) 0.0070(10) 0.0008(11) C15 0.0273(13) 0.0225(13) 0.0188(12) 0.0005(10) 0.0096(10) 0.0021(10) C16 0.0318(16) 0.0436(18) 0.0306(15) 0.0152(14) 0.0102(12) 0.0040(13) C17 0.0228(12) 0.0238(13) 0.0258(13) -0.0010(11) 0.0055(10) 0.0004(11) C18 0.0306(16) 0.0487(19) 0.0355(16) -0.0050(14) 0.0114(13) -0.0113(14) C19 0.0316(15) 0.0297(15) 0.0331(15) -0.0071(13) 0.0012(12) 0.0016(12) C20 0.0336(16) 0.0342(16) 0.0434(17) 0.0078(14) 0.0212(14) -0.0023(13) C21 0.073(3) 0.072(3) 0.084(3) -0.010(3) 0.040(3) -0.013(2) C22 0.0461(19) 0.054(2) 0.0419(18) 0.0112(16) 0.0292(16) 0.0080(16) C23 0.0273(13) 0.0224(12) 0.0177(12) -0.0021(10) 0.0047(10) -0.0072(10) C24 0.0289(13) 0.0237(13) 0.0170(11) -0.0005(10) 0.0066(10) -0.0036(10) C25 0.0270(13) 0.0208(12) 0.0189(11) -0.0019(10) 0.0104(10) -0.0031(10) C26 0.0318(14) 0.0194(12) 0.0185(12) -0.0032(10) 0.0108(10) -0.0014(10) C27 0.0317(14) 0.0194(13) 0.0201(12) -0.0042(10) 0.0105(11) -0.0046(11) C28 0.0264(15) 0.0401(17) 0.0365(16) 0.0028(14) 0.0045(12) -0.0080(13) C29 0.0356(16) 0.0278(15) 0.0316(15) 0.0084(12) 0.0075(12) 0.0020(12) C30 0.0356(15) 0.0265(14) 0.0288(14) -0.0006(11) 0.0178(12) -0.0058(12) C31 0.0374(16) 0.0244(14) 0.0328(15) -0.0036(12) 0.0171(13) 0.0024(12) C32 0.0481(18) 0.0215(14) 0.0389(17) -0.0029(13) 0.0200(15) -0.0068(13) O1 0.0247(9) 0.0194(9) 0.0340(10) -0.0032(8) 0.0132(8) -0.0027(7) O2 0.0283(10) 0.0311(11) 0.0342(11) -0.0021(9) 0.0169(8) 0.0017(8) O3 0.0276(10) 0.0170(9) 0.0297(10) -0.0033(8) 0.0148(8) -0.0021(7) O4 0.0291(10) 0.0188(9) 0.0439(12) -0.0063(9) 0.0110(9) -0.0060(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2639(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . N3 . 2.059(2) yes Ti1 . N4 . 2.090(2) yes Ti1 . C23 . 2.383(3) yes Ti1 . C24 . 2.354(3) yes Ti1 . C25 . 2.374(2) yes Ti1 . C26 . 2.390(3) yes Ti1 . C27 . 2.401(3) yes Ti1 . O1 . 1.9367(19) yes Ti1 . O3 . 1.9512(18) yes N1 . N2 . 1.394(3) yes N1 . C13 . 1.433(3) yes N1 . C14 . 1.423(3) yes N2 . C1 . 1.416(3) yes N2 . C7 . 1.399(3) yes N3 . C15 . 1.339(3) yes N3 . C17 . 1.478(3) yes N4 . C15 . 1.329(4) yes N4 . C20 . 1.489(3) yes C1 . C2 . 1.394(4) yes C1 . C6 . 1.394(4) yes C2 . C3 . 1.386(4) yes C2 . H21 . 0.950 no C3 . C4 . 1.381(4) yes C3 . H31 . 0.950 no C4 . C5 . 1.381(5) yes C4 . H41 . 0.950 no C5 . C6 . 1.396(4) yes C5 . H51 . 0.950 no C6 . H61 . 0.950 no C7 . C8 . 1.401(4) yes C7 . C12 . 1.401(4) yes C8 . C9 . 1.390(4) yes C8 . H81 . 0.950 no C9 . C10 . 1.378(4) yes C9 . H91 . 0.950 no C10 . C11 . 1.376(4) yes C10 . H101 . 0.950 no C11 . C12 . 1.391(4) yes C11 . H111 . 0.950 no C12 . H121 . 0.950 no C13 . O1 . 1.298(3) yes C13 . O2 . 1.206(3) yes C14 . O3 . 1.294(3) yes C14 . O4 . 1.218(3) yes C15 . C16 . 1.502(4) yes C16 . H161 . 0.950 no C16 . H162 . 0.950 no C16 . H163 . 0.950 no C17 . C18 . 1.515(4) yes C17 . C19 . 1.526(4) yes C17 . H171 . 0.950 no C18 . H181 . 0.950 no C18 . H182 . 0.950 no C18 . H183 . 0.950 no C19 . H191 . 0.950 no C19 . H192 . 0.950 no C19 . H193 . 0.950 no C20 . C21 . 1.452(6) yes C20 . C22 . 1.533(5) yes C20 . H201 . 0.950 no C21 . H211 . 0.950 no C21 . H212 . 0.950 no C21 . H213 . 0.950 no C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 no C23 . C24 . 1.417(4) yes C23 . C27 . 1.414(4) yes C23 . C28 . 1.498(4) yes C24 . C25 . 1.429(4) yes C24 . C29 . 1.499(4) yes C25 . C26 . 1.417(4) yes C25 . C30 . 1.498(4) yes C26 . C27 . 1.424(4) yes C26 . C31 . 1.499(4) yes C27 . C32 . 1.498(4) yes C28 . H281 . 0.950 no C28 . H282 . 0.950 no C28 . H283 . 0.950 no C29 . H291 . 0.950 no C29 . H292 . 0.950 no C29 . H293 . 0.950 no C30 . H301 . 0.950 no C30 . H302 . 0.950 no C30 . H303 . 0.950 no C31 . H311 . 0.950 no C31 . H312 . 0.950 no C31 . H313 . 0.950 no C32 . H321 . 0.950 no C32 . H322 . 0.950 no C32 . H323 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N3 . Ti1 . N4 . 64.14(9) yes N3 . Ti1 . C23 . 140.18(9) yes N4 . Ti1 . C23 . 101.30(9) yes N3 . Ti1 . C24 . 139.08(9) yes N4 . Ti1 . C24 . 135.76(9) yes C23 . Ti1 . C24 . 34.80(9) yes N3 . Ti1 . C25 . 103.91(9) yes N4 . Ti1 . C25 . 133.65(9) yes C23 . Ti1 . C25 . 57.87(9) yes C24 . Ti1 . C25 . 35.18(9) yes N3 . Ti1 . C26 . 86.86(9) yes N4 . Ti1 . C26 . 99.12(9) yes C23 . Ti1 . C26 . 57.70(9) yes C24 . Ti1 . C26 . 58.07(9) yes C25 . Ti1 . C26 . 34.61(9) yes N3 . Ti1 . C27 . 105.91(9) yes N4 . Ti1 . C27 . 81.94(9) yes C23 . Ti1 . C27 . 34.39(9) yes C24 . Ti1 . C27 . 57.56(9) yes C25 . Ti1 . C27 . 57.38(9) yes N3 . Ti1 . O1 . 127.61(9) yes N4 . Ti1 . O1 . 89.33(9) yes C23 . Ti1 . O1 . 86.38(9) yes C24 . Ti1 . O1 . 91.84(9) yes C25 . Ti1 . O1 . 125.44(9) yes N3 . Ti1 . O3 . 87.92(8) yes N4 . Ti1 . O3 . 137.28(9) yes C23 . Ti1 . O3 . 119.92(9) yes C24 . Ti1 . O3 . 86.61(9) yes C25 . Ti1 . O3 . 82.12(8) yes C26 . Ti1 . C27 . 34.57(9) yes C26 . Ti1 . O1 . 144.02(9) yes C27 . Ti1 . O1 . 114.38(9) yes C26 . Ti1 . O3 . 111.55(8) yes C27 . Ti1 . O3 . 139.09(8) yes O1 . Ti1 . O3 . 82.99(8) yes N2 . N1 . C13 . 115.8(2) yes N2 . N1 . C14 . 115.8(2) yes C13 . N1 . C14 . 128.3(2) yes N1 . N2 . C1 . 117.2(2) yes N1 . N2 . C7 . 116.6(2) yes C1 . N2 . C7 . 126.0(2) yes Ti1 . N3 . C15 . 92.47(16) yes Ti1 . N3 . C17 . 142.63(18) yes C15 . N3 . C17 . 121.5(2) yes Ti1 . N4 . C15 . 91.34(16) yes Ti1 . N4 . C20 . 139.48(19) yes C15 . N4 . C20 . 123.1(2) yes N2 . C1 . C2 . 120.2(2) yes N2 . C1 . C6 . 120.6(2) yes C2 . C1 . C6 . 119.2(2) yes C1 . C2 . C3 . 120.4(3) yes C1 . C2 . H21 . 119.6 no C3 . C2 . H21 . 120.0 no C2 . C3 . C4 . 120.2(3) yes C2 . C3 . H31 . 119.9 no C4 . C3 . H31 . 119.9 no C3 . C4 . C5 . 120.1(3) yes C3 . C4 . H41 . 119.9 no C5 . C4 . H41 . 120.0 no C4 . C5 . C6 . 120.1(3) yes C4 . C5 . H51 . 119.9 no C6 . C5 . H51 . 120.0 no C5 . C6 . C1 . 120.0(3) yes C5 . C6 . H61 . 120.4 no C1 . C6 . H61 . 119.7 no N2 . C7 . C8 . 120.9(2) yes N2 . C7 . C12 . 121.0(2) yes C8 . C7 . C12 . 118.1(2) yes C7 . C8 . C9 . 120.3(3) yes C7 . C8 . H81 . 119.7 no C9 . C8 . H81 . 120.1 no C8 . C9 . C10 . 121.0(3) yes C8 . C9 . H91 . 119.7 no C10 . C9 . H91 . 119.3 no C9 . C10 . C11 . 119.2(3) yes C9 . C10 . H101 . 120.5 no C11 . C10 . H101 . 120.3 no C10 . C11 . C12 . 121.0(3) yes C10 . C11 . H111 . 119.6 no C12 . C11 . H111 . 119.4 no C7 . C12 . C11 . 120.4(3) yes C7 . C12 . H121 . 119.5 no C11 . C12 . H121 . 120.1 no N1 . C13 . O1 . 115.7(2) yes N1 . C13 . O2 . 119.1(2) yes O1 . C13 . O2 . 125.2(2) yes N1 . C14 . O3 . 116.1(2) yes N1 . C14 . O4 . 119.3(2) yes O3 . C14 . O4 . 124.5(2) yes N3 . C15 . N4 . 111.4(2) yes N3 . C15 . C16 . 123.1(2) yes N4 . C15 . C16 . 125.5(2) yes C15 . C16 . H161 . 109.4 no C15 . C16 . H162 . 109.5 no H161 . C16 . H162 . 109.5 no C15 . C16 . H163 . 109.5 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no N3 . C17 . C18 . 110.8(2) yes N3 . C17 . C19 . 111.7(2) yes C18 . C17 . C19 . 109.5(3) yes N3 . C17 . H171 . 108.2 no C18 . C17 . H171 . 108.2 no C19 . C17 . H171 . 108.3 no C17 . C18 . H181 . 109.6 no C17 . C18 . H182 . 109.0 no H181 . C18 . H182 . 109.5 no C17 . C18 . H183 . 109.8 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no C17 . C19 . H191 . 110.0 no C17 . C19 . H192 . 109.3 no H191 . C19 . H192 . 109.5 no C17 . C19 . H193 . 109.1 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no N4 . C20 . C21 . 115.0(3) yes N4 . C20 . C22 . 110.7(3) yes C21 . C20 . C22 . 108.4(3) yes N4 . C20 . H201 . 107.3 no C21 . C20 . H201 . 107.5 no C22 . C20 . H201 . 107.7 no C20 . C21 . H211 . 110.1 no C20 . C21 . H212 . 108.9 no H211 . C21 . H212 . 109.5 no C20 . C21 . H213 . 109.4 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C20 . C22 . H221 . 109.4 no C20 . C22 . H222 . 109.9 no H221 . C22 . H222 . 109.5 no C20 . C22 . H223 . 109.1 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no Ti1 . C23 . C24 . 71.48(14) yes Ti1 . C23 . C27 . 73.51(15) yes C24 . C23 . C27 . 107.9(2) yes Ti1 . C23 . C28 . 123.38(19) yes C24 . C23 . C28 . 124.7(3) yes C27 . C23 . C28 . 127.2(2) yes Ti1 . C24 . C23 . 73.72(14) yes Ti1 . C24 . C25 . 73.18(14) yes C23 . C24 . C25 . 107.9(2) yes Ti1 . C24 . C29 . 120.55(19) yes C23 . C24 . C29 . 126.2(2) yes C25 . C24 . C29 . 125.9(2) yes Ti1 . C25 . C24 . 71.63(14) yes Ti1 . C25 . C26 . 73.30(14) yes C24 . C25 . C26 . 108.0(2) yes Ti1 . C25 . C30 . 122.94(18) yes C24 . C25 . C30 . 124.7(2) yes C26 . C25 . C30 . 127.3(2) yes Ti1 . C26 . C25 . 72.09(14) yes Ti1 . C26 . C27 . 73.15(15) yes C25 . C26 . C27 . 107.6(2) yes Ti1 . C26 . C31 . 125.41(18) yes C25 . C26 . C31 . 128.1(2) yes C27 . C26 . C31 . 124.0(2) yes Ti1 . C27 . C26 . 72.28(14) yes Ti1 . C27 . C23 . 72.10(15) yes C26 . C27 . C23 . 108.5(2) yes Ti1 . C27 . C32 . 128.56(19) yes C26 . C27 . C32 . 123.8(3) yes C23 . C27 . C32 . 127.1(3) yes C23 . C28 . H281 . 109.5 no C23 . C28 . H282 . 109.2 no H281 . C28 . H282 . 109.5 no C23 . C28 . H283 . 109.7 no H281 . C28 . H283 . 109.5 no H282 . C28 . H283 . 109.5 no C24 . C29 . H291 . 109.6 no C24 . C29 . H292 . 109.0 no H291 . C29 . H292 . 109.8 no C24 . C29 . H293 . 109.0 no H291 . C29 . H293 . 109.8 no H292 . C29 . H293 . 109.5 no C25 . C30 . H301 . 109.4 no C25 . C30 . H302 . 109.4 no H301 . C30 . H302 . 109.5 no C25 . C30 . H303 . 109.6 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no C26 . C31 . H311 . 109.3 no C26 . C31 . H312 . 109.5 no H311 . C31 . H312 . 109.6 no C26 . C31 . H313 . 109.4 no H311 . C31 . H313 . 109.6 no H312 . C31 . H313 . 109.5 no C27 . C32 . H321 . 109.7 no C27 . C32 . H322 . 109.3 no H321 . C32 . H322 . 109.6 no C27 . C32 . H323 . 109.2 no H321 . C32 . H323 . 109.6 no H322 . C32 . H323 . 109.5 no C13 . O1 . Ti1 . 134.43(17) yes C14 . O3 . Ti1 . 131.98(16) yes #===end data_Compound_7 _database_code_depnum_ccdc_archive 'CCDC 752047' # Local code DS7 _audit_creation_method CRYSTALS_ver_12.86 _chemical_name_systematic ; Ti(N2NMe){NC(ArF)NNPh2}(py) ; _publ_section_exptl_refinement ; No special comments. H atoms were placed in calculated positions with reference to a Fourier difference map ; _chemical_melting_point . _cell_length_a 13.7067(2) _cell_length_b 18.2074(2) _cell_length_c 15.3084(2) _cell_angle_alpha 90 _cell_angle_beta 93.8645(6) _cell_angle_gamma 90 _cell_volume 3811.73(9) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C35 H44 F5 N7 Si2 Ti1' _chemical_formula_moiety 'C35 H44 F5 N7 Si2 Ti1' _chemical_compound_source ? _chemical_formula_weight 761.84 _cell_measurement_reflns_used 8820 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 0.347 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.93 _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 62187 _reflns_number_total 8662 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_min 5.099 _diffrn_reflns_theta_max 27.472 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.922 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 2.44 _oxford_diffrn_Wilson_scale 1.69 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.30 _refine_diff_density_max 0.30 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 7207 _refine_ls_number_restraints 0 _refine_ls_number_parameters 451 _oxford_refine_ls_R_factor_ref 0.0329 _refine_ls_wR_factor_ref 0.0335 _refine_ls_goodness_of_fit_ref 1.1133 _refine_ls_shift/su_max 0.000784 # The values computed from all data _oxford_reflns_number_all 8662 _refine_ls_R_factor_all 0.0426 _refine_ls_wR_factor_all 0.0397 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7532 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_gt 0.0343 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.32 0.130 1.10 0.135E-01 0.277 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ti1 Ti 0.139217(16) 0.582445(12) 0.231009(15) 0.0255 1.0000 Uani . . . . . . . N1 N 0.08346(8) 0.65995(6) 0.27817(7) 0.0282 1.0000 Uani . . . . . . . N2 N 0.05087(8) 0.77732(6) 0.32733(8) 0.0301 1.0000 Uani . . . . . . . N3 N -0.01665(8) 0.81625(6) 0.37874(7) 0.0299 1.0000 Uani . . . . . . . N4 N 0.14401(9) 0.61122(6) 0.10770(8) 0.0315 1.0000 Uani . . . . . . . N5 N 0.25605(8) 0.56367(6) 0.30929(8) 0.0339 1.0000 Uani . . . . . . . N6 N 0.20019(8) 0.47606(6) 0.17060(8) 0.0336 1.0000 Uani . . . . . . . N7 N 0.01120(8) 0.51327(6) 0.24970(7) 0.0301 1.0000 Uani . . . . . . . C1 C 0.02718(9) 0.70811(7) 0.31750(8) 0.0267 1.0000 Uani . . . . . . . C2 C -0.06654(9) 0.67738(7) 0.34978(9) 0.0281 1.0000 Uani . . . . . . . C3 C -0.15811(10) 0.69933(7) 0.31417(9) 0.0296 1.0000 Uani . . . . . . . C4 C -0.24356(10) 0.66964(8) 0.34120(9) 0.0334 1.0000 Uani . . . . . . . C5 C -0.24066(10) 0.61711(9) 0.40563(10) 0.0371 1.0000 Uani . . . . . . . C6 C -0.15129(11) 0.59417(8) 0.44252(10) 0.0380 1.0000 Uani . . . . . . . C7 C -0.06659(10) 0.62421(8) 0.41389(9) 0.0330 1.0000 Uani . . . . . . . C8 C -0.00406(10) 0.80389(7) 0.47086(9) 0.0306 1.0000 Uani . . . . . . . C9 C -0.08604(11) 0.80513(10) 0.51922(10) 0.0436 1.0000 Uani . . . . . . . C10 C -0.07711(14) 0.79357(11) 0.60898(11) 0.0530 1.0000 Uani . . . . . . . C11 C 0.01335(14) 0.77813(10) 0.65034(11) 0.0492 1.0000 Uani . . . . . . . C12 C 0.09451(13) 0.77548(9) 0.60223(11) 0.0467 1.0000 Uani . . . . . . . C13 C 0.08691(11) 0.78896(8) 0.51232(10) 0.0373 1.0000 Uani . . . . . . . C14 C -0.03967(9) 0.88700(7) 0.34665(9) 0.0298 1.0000 Uani . . . . . . . C15 C -0.05483(11) 0.94638(8) 0.40223(11) 0.0368 1.0000 Uani . . . . . . . C16 C -0.07890(11) 1.01501(8) 0.36712(12) 0.0438 1.0000 Uani . . . . . . . C17 C -0.08865(11) 1.02573(8) 0.27767(12) 0.0443 1.0000 Uani . . . . . . . C18 C -0.07380(11) 0.96702(9) 0.22237(11) 0.0406 1.0000 Uani . . . . . . . C19 C -0.04904(10) 0.89818(8) 0.25588(10) 0.0347 1.0000 Uani . . . . . . . C20 C 0.19896(13) 0.56381(9) 0.05057(11) 0.0435 1.0000 Uani . . . . . . . C21 C 0.26084(12) 0.51018(9) 0.10588(12) 0.0439 1.0000 Uani . . . . . . . C22 C 0.31665(12) 0.49754(9) 0.29642(13) 0.0478 1.0000 Uani . . . . . . . C23 C 0.25976(12) 0.44009(8) 0.24237(12) 0.0429 1.0000 Uani . . . . . . . C24 C 0.13336(12) 0.42226(8) 0.12660(11) 0.0413 1.0000 Uani . . . . . . . C25 C 0.15258(13) 0.77642(8) 0.10674(12) 0.0452 1.0000 Uani . . . . . . . C26 C 0.10207(13) 0.68947(10) -0.05947(11) 0.0480 1.0000 Uani . . . . . . . C27 C -0.04137(11) 0.69814(9) 0.07885(10) 0.0413 1.0000 Uani . . . . . . . C28 C 0.44084(12) 0.60387(11) 0.41077(15) 0.0601 1.0000 Uani . . . . . . . C29 C 0.25080(13) 0.62314(10) 0.49246(11) 0.0476 1.0000 Uani . . . . . . . C30 C 0.30458(13) 0.72258(9) 0.34554(11) 0.0428 1.0000 Uani . . . . . . . C31 C -0.07006(10) 0.51982(9) 0.19617(10) 0.0372 1.0000 Uani . . . . . . . C32 C -0.15415(12) 0.48040(11) 0.20815(12) 0.0496 1.0000 Uani . . . . . . . C33 C -0.15543(14) 0.43226(11) 0.27750(13) 0.0542 1.0000 Uani . . . . . . . C34 C -0.07302(15) 0.42517(10) 0.33259(12) 0.0524 1.0000 Uani . . . . . . . C35 C 0.00896(12) 0.46651(9) 0.31711(11) 0.0420 1.0000 Uani . . . . . . . F1 F -0.16597(6) 0.75063(5) 0.25122(6) 0.0376 1.0000 Uani . . . . . . . F2 F -0.33011(6) 0.69187(5) 0.30379(6) 0.0437 1.0000 Uani . . . . . . . F3 F -0.32316(7) 0.58787(6) 0.43250(7) 0.0517 1.0000 Uani . . . . . . . F4 F -0.14733(8) 0.54316(6) 0.50583(7) 0.0570 1.0000 Uani . . . . . . . F5 F 0.01851(6) 0.59999(5) 0.45270(6) 0.0439 1.0000 Uani . . . . . . . Si1 Si 0.09221(3) 0.69122(2) 0.06222(3) 0.0334 1.0000 Uani . . . . . . . Si2 Si 0.30840(3) 0.62587(2) 0.38591(3) 0.0307 1.0000 Uani . . . . . . . H91 H -0.1487 0.8139 0.4907 0.0523 1.0000 Uiso R . . . . . . H101 H -0.1332 0.7963 0.6421 0.0639 1.0000 Uiso R . . . . . . H111 H 0.0194 0.7694 0.7116 0.0589 1.0000 Uiso R . . . . . . H121 H 0.1565 0.7643 0.6306 0.0554 1.0000 Uiso R . . . . . . H131 H 0.1435 0.7879 0.4798 0.0446 1.0000 Uiso R . . . . . . H151 H -0.0487 0.9398 0.4639 0.0440 1.0000 Uiso R . . . . . . H161 H -0.0888 1.0551 0.4052 0.0523 1.0000 Uiso R . . . . . . H171 H -0.1053 1.0728 0.2543 0.0527 1.0000 Uiso R . . . . . . H181 H -0.0807 0.9740 0.1608 0.0485 1.0000 Uiso R . . . . . . H191 H -0.0384 0.8586 0.2173 0.0417 1.0000 Uiso R . . . . . . H201 H 0.2400 0.5933 0.0173 0.0531 1.0000 Uiso R . . . . . . H202 H 0.1544 0.5374 0.0121 0.0531 1.0000 Uiso R . . . . . . H211 H 0.3139 0.5356 0.1354 0.0533 1.0000 Uiso R . . . . . . H212 H 0.2854 0.4732 0.0694 0.0533 1.0000 Uiso R . . . . . . H221 H 0.3727 0.5113 0.2670 0.0564 1.0000 Uiso R . . . . . . H222 H 0.3367 0.4773 0.3520 0.0564 1.0000 Uiso R . . . . . . H231 H 0.2181 0.4141 0.2787 0.0509 1.0000 Uiso R . . . . . . H232 H 0.3041 0.4067 0.2184 0.0509 1.0000 Uiso R . . . . . . H241 H 0.0943 0.4003 0.1684 0.0494 1.0000 Uiso R . . . . . . H242 H 0.0924 0.4464 0.0831 0.0494 1.0000 Uiso R . . . . . . H243 H 0.1703 0.3854 0.0999 0.0494 1.0000 Uiso R . . . . . . H251 H 0.1217 0.8182 0.0799 0.0542 1.0000 Uiso R . . . . . . H252 H 0.1471 0.7785 0.1682 0.0542 1.0000 Uiso R . . . . . . H253 H 0.2197 0.7759 0.0948 0.0542 1.0000 Uiso R . . . . . . H261 H 0.0740 0.7329 -0.0846 0.0580 1.0000 Uiso R . . . . . . H262 H 0.1690 0.6868 -0.0718 0.0580 1.0000 Uiso R . . . . . . H263 H 0.0683 0.6478 -0.0836 0.0580 1.0000 Uiso R . . . . . . H271 H -0.0666 0.7423 0.0532 0.0496 1.0000 Uiso R . . . . . . H272 H -0.0508 0.6983 0.1398 0.0496 1.0000 Uiso R . . . . . . H273 H -0.0745 0.6573 0.0520 0.0496 1.0000 Uiso R . . . . . . H281 H 0.4685 0.6380 0.4524 0.0715 1.0000 Uiso R . . . . . . H282 H 0.4743 0.6069 0.3585 0.0715 1.0000 Uiso R . . . . . . H283 H 0.4469 0.5556 0.4339 0.0715 1.0000 Uiso R . . . . . . H291 H 0.2819 0.6578 0.5314 0.0574 1.0000 Uiso R . . . . . . H292 H 0.1833 0.6349 0.4834 0.0574 1.0000 Uiso R . . . . . . H293 H 0.2577 0.5753 0.5169 0.0574 1.0000 Uiso R . . . . . . H301 H 0.3338 0.7540 0.3894 0.0513 1.0000 Uiso R . . . . . . H302 H 0.2385 0.7369 0.3325 0.0513 1.0000 Uiso R . . . . . . H303 H 0.3394 0.7261 0.2941 0.0513 1.0000 Uiso R . . . . . . H311 H -0.0697 0.5529 0.1482 0.0447 1.0000 Uiso R . . . . . . H321 H -0.2104 0.4864 0.1691 0.0596 1.0000 Uiso R . . . . . . H331 H -0.2124 0.4045 0.2869 0.0660 1.0000 Uiso R . . . . . . H341 H -0.0721 0.3923 0.3808 0.0634 1.0000 Uiso R . . . . . . H351 H 0.0657 0.4615 0.3558 0.0504 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.02440(11) 0.02049(10) 0.03116(12) -0.00249(9) -0.00187(8) 0.00134(8) N1 0.0265(5) 0.0255(5) 0.0321(5) -0.0018(4) -0.0018(4) 0.0020(4) N2 0.0297(5) 0.0263(5) 0.0344(6) -0.0038(4) 0.0016(4) 0.0037(4) N3 0.0325(6) 0.0247(5) 0.0324(6) -0.0036(4) 0.0009(4) 0.0056(4) N4 0.0355(6) 0.0257(5) 0.0337(6) -0.0026(4) 0.0045(5) 0.0006(4) N5 0.0277(5) 0.0268(5) 0.0459(7) -0.0076(5) -0.0068(5) 0.0051(4) N6 0.0332(6) 0.0226(5) 0.0441(7) -0.0058(5) -0.0033(5) 0.0015(4) N7 0.0309(5) 0.0271(5) 0.0320(6) -0.0014(4) 0.0004(4) -0.0011(4) C1 0.0260(6) 0.0257(6) 0.0277(6) -0.0006(5) -0.0034(5) 0.0034(5) C2 0.0269(6) 0.0253(6) 0.0315(6) -0.0056(5) -0.0024(5) 0.0017(5) C3 0.0297(6) 0.0261(6) 0.0323(6) -0.0048(5) -0.0030(5) 0.0038(5) C4 0.0249(6) 0.0353(7) 0.0390(7) -0.0116(6) -0.0051(5) 0.0037(5) C5 0.0303(7) 0.0427(8) 0.0384(7) -0.0084(6) 0.0036(6) -0.0083(6) C6 0.0405(8) 0.0383(8) 0.0345(7) 0.0045(6) -0.0017(6) -0.0081(6) C7 0.0294(6) 0.0332(7) 0.0354(7) -0.0004(6) -0.0058(5) 0.0010(5) C8 0.0357(7) 0.0224(6) 0.0330(7) -0.0033(5) -0.0017(5) -0.0001(5) C9 0.0347(7) 0.0561(10) 0.0398(8) -0.0057(7) 0.0004(6) -0.0038(7) C10 0.0491(9) 0.0701(12) 0.0405(9) -0.0062(8) 0.0084(7) -0.0138(8) C11 0.0626(11) 0.0493(9) 0.0351(8) 0.0019(7) -0.0017(7) -0.0093(8) C12 0.0521(9) 0.0433(8) 0.0428(8) -0.0015(7) -0.0121(7) 0.0070(7) C13 0.0363(7) 0.0355(7) 0.0394(8) -0.0031(6) -0.0020(6) 0.0052(6) C14 0.0255(6) 0.0237(6) 0.0398(7) -0.0015(5) -0.0015(5) 0.0009(5) C15 0.0369(7) 0.0284(6) 0.0442(8) -0.0058(6) -0.0032(6) 0.0042(6) C16 0.0405(8) 0.0271(7) 0.0629(10) -0.0072(7) -0.0029(7) 0.0061(6) C17 0.0384(8) 0.0283(7) 0.0652(10) 0.0076(7) -0.0030(7) 0.0033(6) C18 0.0368(8) 0.0361(7) 0.0482(9) 0.0089(6) -0.0015(6) -0.0004(6) C19 0.0339(7) 0.0299(7) 0.0401(7) 0.0011(6) 0.0005(6) -0.0007(5) C20 0.0543(9) 0.0340(7) 0.0442(8) -0.0032(6) 0.0181(7) 0.0011(7) C21 0.0416(8) 0.0335(7) 0.0580(10) -0.0087(7) 0.0144(7) 0.0049(6) C22 0.0387(8) 0.0353(8) 0.0665(11) -0.0161(7) -0.0176(7) 0.0130(6) C23 0.0437(8) 0.0265(7) 0.0564(9) -0.0077(6) -0.0124(7) 0.0100(6) C24 0.0443(8) 0.0284(7) 0.0499(9) -0.0108(6) -0.0057(7) -0.0001(6) C25 0.0516(9) 0.0278(7) 0.0548(10) 0.0041(7) -0.0056(7) -0.0009(6) C26 0.0526(9) 0.0532(10) 0.0384(8) 0.0091(7) 0.0042(7) -0.0019(8) C27 0.0414(8) 0.0454(8) 0.0366(7) 0.0042(6) -0.0023(6) 0.0060(7) C28 0.0349(8) 0.0626(11) 0.0800(13) -0.0346(10) -0.0172(8) 0.0095(8) C29 0.0508(9) 0.0499(9) 0.0421(8) -0.0017(7) 0.0025(7) -0.0169(8) C30 0.0485(9) 0.0358(8) 0.0434(8) -0.0020(6) -0.0018(7) -0.0112(6) C31 0.0313(7) 0.0405(8) 0.0395(7) 0.0019(6) -0.0004(6) -0.0006(6) C32 0.0315(7) 0.0618(11) 0.0553(10) -0.0065(8) 0.0012(7) -0.0063(7) C33 0.0476(10) 0.0559(10) 0.0614(11) -0.0068(9) 0.0197(8) -0.0190(8) C34 0.0683(12) 0.0434(9) 0.0467(9) 0.0060(7) 0.0138(8) -0.0133(8) C35 0.0495(9) 0.0374(8) 0.0385(8) 0.0048(6) -0.0007(6) -0.0041(7) F1 0.0347(4) 0.0346(4) 0.0422(5) 0.0043(3) -0.0071(3) 0.0058(3) F2 0.0253(4) 0.0482(5) 0.0560(5) -0.0107(4) -0.0081(4) 0.0055(4) F3 0.0352(5) 0.0668(6) 0.0536(6) -0.0045(5) 0.0072(4) -0.0170(4) F4 0.0547(6) 0.0631(6) 0.0517(6) 0.0244(5) -0.0069(5) -0.0172(5) F5 0.0335(4) 0.0469(5) 0.0495(5) 0.0142(4) -0.0110(4) 0.0018(4) Si1 0.0384(2) 0.02831(18) 0.03331(19) 0.00255(15) 0.00062(15) -0.00087(15) Si2 0.02541(17) 0.02875(18) 0.0372(2) -0.00542(15) -0.00329(14) 0.00000(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.7899(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . N1 . 1.7808(11) yes Ti1 . N4 . 1.9644(12) yes Ti1 . N5 . 1.9644(11) yes Ti1 . N6 . 2.3259(11) yes Ti1 . N7 . 2.1944(11) yes N1 . C1 . 1.3375(17) yes N2 . N3 . 1.4410(15) yes N2 . C1 . 1.3075(17) yes N3 . C8 . 1.4271(18) yes N3 . C14 . 1.4069(17) yes N4 . C20 . 1.4717(18) yes N4 . Si1 . 1.7446(12) yes N5 . C22 . 1.4834(18) yes N5 . Si2 . 1.7493(12) yes N6 . C21 . 1.473(2) yes N6 . C23 . 1.4770(19) yes N6 . C24 . 1.4727(18) yes N7 . C31 . 1.3429(18) yes N7 . C35 . 1.3397(19) yes C1 . C2 . 1.5143(18) yes C2 . C3 . 1.3929(18) yes C2 . C7 . 1.379(2) yes C3 . C4 . 1.379(2) yes C3 . F1 . 1.3411(16) yes C4 . C5 . 1.373(2) yes C4 . F2 . 1.3445(15) yes C5 . C6 . 1.379(2) yes C5 . F3 . 1.3395(17) yes C6 . C7 . 1.381(2) yes C6 . F4 . 1.3408(17) yes C7 . F5 . 1.3471(16) yes C8 . C9 . 1.387(2) yes C8 . C13 . 1.387(2) yes C9 . C10 . 1.387(2) yes C9 . H91 . 0.950 no C10 . C11 . 1.383(3) yes C10 . H101 . 0.950 no C11 . C12 . 1.376(3) yes C11 . H111 . 0.950 no C12 . C13 . 1.395(2) yes C12 . H121 . 0.950 no C13 . H131 . 0.950 no C14 . C15 . 1.3999(19) yes C14 . C19 . 1.402(2) yes C15 . C16 . 1.391(2) yes C15 . H151 . 0.950 no C16 . C17 . 1.381(3) yes C16 . H161 . 0.950 no C17 . C18 . 1.387(2) yes C17 . H171 . 0.950 no C18 . C19 . 1.388(2) yes C18 . H181 . 0.950 no C19 . H191 . 0.950 no C20 . C21 . 1.514(2) yes C20 . H201 . 0.950 no C20 . H202 . 0.950 no C21 . H211 . 0.950 no C21 . H212 . 0.950 no C22 . C23 . 1.516(2) yes C22 . H221 . 0.950 no C22 . H222 . 0.950 no C23 . H231 . 0.950 no C23 . H232 . 0.950 no C24 . H241 . 0.950 no C24 . H242 . 0.950 no C24 . H243 . 0.950 no C25 . Si1 . 1.8654(16) yes C25 . H251 . 0.950 no C25 . H252 . 0.950 no C25 . H253 . 0.950 no C26 . Si1 . 1.8771(17) yes C26 . H261 . 0.950 no C26 . H262 . 0.950 no C26 . H263 . 0.950 no C27 . Si1 . 1.8698(16) yes C27 . H271 . 0.950 no C27 . H272 . 0.950 no C27 . H273 . 0.950 no C28 . Si2 . 1.8728(17) yes C28 . H281 . 0.950 no C28 . H282 . 0.950 no C28 . H283 . 0.950 no C29 . Si2 . 1.8601(17) yes C29 . H291 . 0.950 no C29 . H292 . 0.950 no C29 . H293 . 0.950 no C30 . Si2 . 1.8657(16) yes C30 . H301 . 0.950 no C30 . H302 . 0.950 no C30 . H303 . 0.950 no C31 . C32 . 1.380(2) yes C31 . H311 . 0.950 no C32 . C33 . 1.378(3) yes C32 . H321 . 0.950 no C33 . C34 . 1.369(3) yes C33 . H331 . 0.950 no C34 . C35 . 1.386(2) yes C34 . H341 . 0.950 no C35 . H351 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ti1 . N4 . 102.78(5) yes N1 . Ti1 . N5 . 104.19(5) yes N4 . Ti1 . N5 . 123.64(5) yes N1 . Ti1 . N6 . 175.33(5) yes N4 . Ti1 . N6 . 78.69(5) yes N5 . Ti1 . N6 . 78.32(4) yes N1 . Ti1 . N7 . 91.90(5) yes N4 . Ti1 . N7 . 110.93(5) yes N5 . Ti1 . N7 . 116.53(5) yes N6 . Ti1 . N7 . 83.44(4) yes Ti1 . N1 . C1 . 168.03(10) yes N3 . N2 . C1 . 111.92(11) yes N2 . N3 . C8 . 115.01(10) yes N2 . N3 . C14 . 113.39(11) yes C8 . N3 . C14 . 119.91(11) yes Ti1 . N4 . C20 . 117.78(9) yes Ti1 . N4 . Si1 . 124.55(6) yes C20 . N4 . Si1 . 117.61(10) yes Ti1 . N5 . C22 . 120.06(9) yes Ti1 . N5 . Si2 . 125.24(6) yes C22 . N5 . Si2 . 113.99(9) yes Ti1 . N6 . C21 . 98.64(8) yes Ti1 . N6 . C23 . 105.60(9) yes C21 . N6 . C23 . 112.24(12) yes Ti1 . N6 . C24 . 120.44(9) yes C21 . N6 . C24 . 109.56(13) yes C23 . N6 . C24 . 109.93(11) yes Ti1 . N7 . C31 . 120.47(10) yes Ti1 . N7 . C35 . 121.68(10) yes C31 . N7 . C35 . 117.74(13) yes N1 . C1 . N2 . 122.50(12) yes N1 . C1 . C2 . 115.62(11) yes N2 . C1 . C2 . 121.88(11) yes C1 . C2 . C3 . 121.88(12) yes C1 . C2 . C7 . 122.20(11) yes C3 . C2 . C7 . 115.88(12) yes C2 . C3 . C4 . 122.10(13) yes C2 . C3 . F1 . 120.51(12) yes C4 . C3 . F1 . 117.39(12) yes C3 . C4 . C5 . 120.33(12) yes C3 . C4 . F2 . 119.82(13) yes C5 . C4 . F2 . 119.86(13) yes C4 . C5 . C6 . 119.17(13) yes C4 . C5 . F3 . 120.90(13) yes C6 . C5 . F3 . 119.93(14) yes C5 . C6 . C7 . 119.52(14) yes C5 . C6 . F4 . 119.84(13) yes C7 . C6 . F4 . 120.64(13) yes C6 . C7 . C2 . 123.00(13) yes C6 . C7 . F5 . 116.86(13) yes C2 . C7 . F5 . 120.14(12) yes N3 . C8 . C9 . 118.46(13) yes N3 . C8 . C13 . 121.88(13) yes C9 . C8 . C13 . 119.64(14) yes C8 . C9 . C10 . 120.38(15) yes C8 . C9 . H91 . 119.8 no C10 . C9 . H91 . 119.8 no C9 . C10 . C11 . 120.06(16) yes C9 . C10 . H101 . 120.0 no C11 . C10 . H101 . 120.0 no C10 . C11 . C12 . 119.64(16) yes C10 . C11 . H111 . 120.2 no C12 . C11 . H111 . 120.2 no C11 . C12 . C13 . 120.84(15) yes C11 . C12 . H121 . 119.6 no C13 . C12 . H121 . 119.6 no C12 . C13 . C8 . 119.40(15) yes C12 . C13 . H131 . 120.3 no C8 . C13 . H131 . 120.3 no N3 . C14 . C15 . 122.27(13) yes N3 . C14 . C19 . 118.85(12) yes C15 . C14 . C19 . 118.87(13) yes C14 . C15 . C16 . 120.00(15) yes C14 . C15 . H151 . 120.0 no C16 . C15 . H151 . 120.0 no C15 . C16 . C17 . 120.98(15) yes C15 . C16 . H161 . 119.5 no C17 . C16 . H161 . 119.5 no C16 . C17 . C18 . 119.20(14) yes C16 . C17 . H171 . 120.4 no C18 . C17 . H171 . 120.4 no C17 . C18 . C19 . 120.85(15) yes C17 . C18 . H181 . 119.6 no C19 . C18 . H181 . 119.6 no C14 . C19 . C18 . 120.10(14) yes C14 . C19 . H191 . 119.9 no C18 . C19 . H191 . 120.0 no N4 . C20 . C21 . 109.62(13) yes N4 . C20 . H201 . 109.5 no C21 . C20 . H201 . 109.5 no N4 . C20 . H202 . 109.4 no C21 . C20 . H202 . 109.4 no H201 . C20 . H202 . 109.5 no C20 . C21 . N6 . 109.14(12) yes C20 . C21 . H211 . 109.5 no N6 . C21 . H211 . 109.6 no C20 . C21 . H212 . 109.6 no N6 . C21 . H212 . 109.6 no H211 . C21 . H212 . 109.5 no N5 . C22 . C23 . 111.13(12) yes N5 . C22 . H221 . 109.0 no C23 . C22 . H221 . 109.0 no N5 . C22 . H222 . 109.1 no C23 . C22 . H222 . 109.1 no H221 . C22 . H222 . 109.5 no C22 . C23 . N6 . 109.77(12) yes C22 . C23 . H231 . 109.4 no N6 . C23 . H231 . 109.4 no C22 . C23 . H232 . 109.4 no N6 . C23 . H232 . 109.4 no H231 . C23 . H232 . 109.5 no N6 . C24 . H241 . 109.5 no N6 . C24 . H242 . 109.4 no H241 . C24 . H242 . 109.5 no N6 . C24 . H243 . 109.5 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no Si1 . C25 . H251 . 109.5 no Si1 . C25 . H252 . 109.5 no H251 . C25 . H252 . 109.5 no Si1 . C25 . H253 . 109.4 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no Si1 . C26 . H261 . 109.5 no Si1 . C26 . H262 . 109.5 no H261 . C26 . H262 . 109.5 no Si1 . C26 . H263 . 109.5 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no Si1 . C27 . H271 . 109.5 no Si1 . C27 . H272 . 109.5 no H271 . C27 . H272 . 109.5 no Si1 . C27 . H273 . 109.4 no H271 . C27 . H273 . 109.5 no H272 . C27 . H273 . 109.5 no Si2 . C28 . H281 . 109.5 no Si2 . C28 . H282 . 109.4 no H281 . C28 . H282 . 109.5 no Si2 . C28 . H283 . 109.5 no H281 . C28 . H283 . 109.5 no H282 . C28 . H283 . 109.5 no Si2 . C29 . H291 . 109.5 no Si2 . C29 . H292 . 109.4 no H291 . C29 . H292 . 109.5 no Si2 . C29 . H293 . 109.5 no H291 . C29 . H293 . 109.5 no H292 . C29 . H293 . 109.5 no Si2 . C30 . H301 . 109.5 no Si2 . C30 . H302 . 109.4 no H301 . C30 . H302 . 109.5 no Si2 . C30 . H303 . 109.5 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no N7 . C31 . C32 . 122.56(15) yes N7 . C31 . H311 . 118.7 no C32 . C31 . H311 . 118.7 no C31 . C32 . C33 . 119.16(16) yes C31 . C32 . H321 . 120.4 no C33 . C32 . H321 . 120.4 no C32 . C33 . C34 . 118.79(15) yes C32 . C33 . H331 . 120.6 no C34 . C33 . H331 . 120.6 no C33 . C34 . C35 . 119.22(16) yes C33 . C34 . H341 . 120.4 no C35 . C34 . H341 . 120.4 no C34 . C35 . N7 . 122.52(16) yes C34 . C35 . H351 . 118.7 no N7 . C35 . H351 . 118.7 no C26 . Si1 . C27 . 105.84(8) yes C26 . Si1 . C25 . 108.48(8) yes C27 . Si1 . C25 . 107.97(8) yes C26 . Si1 . N4 . 109.10(7) yes C27 . Si1 . N4 . 112.19(7) yes C25 . Si1 . N4 . 112.96(7) yes C28 . Si2 . C30 . 105.92(9) yes C28 . Si2 . C29 . 106.20(9) yes C30 . Si2 . C29 . 108.15(8) yes C28 . Si2 . N5 . 110.24(7) yes C30 . Si2 . N5 . 112.82(7) yes C29 . Si2 . N5 . 113.05(7) yes #===end