# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global #=================================================================== _journal_coden_Cambridge 182 _publ_contact_author_name 'ProfD Matthias Tamm' _publ_contact_author_address ; Department Chemie Technische Universitat Munchen Lehrstuhl fur Anorganische Chemie Lichtenbergstr 4 Garching D-85747 GERMANY ; _publ_contact_author_email MATTHIAS.TAMM@CH.TUM.DE _publ_section_title ; Regioselective Si-C Bond Activation in Silicon-Bridged Ansa-Cycloheptatrienyl-Cyclopentadienyl Complexes ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Tamm, M.' ; Department Chemie, Lehrstuhl fur Anorganische Chemie, Technische Universitat Munchen, Lichtenbergstrasse 4, D-85747 Garching bei Munchen, Germany. ; 'Kunst, A.' ; Department Chemie, Lehrstuhl fur Anorganische Chemie, Technische Universitat Munchen, Lichtenbergstrasse 4, D-85747 Garching bei Munchen, Germany. ; 'Herdtweck, E.' ; Department Chemie, Lehrstuhl fur Anorganische Chemie, Technische Universitat Munchen, Lichtenbergstrasse 4, D-85747 Garching bei Munchen, Germany. ; # Insert blank lines between references _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436. Nonius (2001a). Data Collection Software for Nonius Kappa-CCD devices. Nonius BV, Delft, The Netherlands. Nonius (2001b). DENZO Processing Software for Nonius Kappa-CCD devices, Nonius BV, Delft, The Netherlands. Sheldrick, G. M. (1998). SHELXL97, University of Gottingen, Gottingen, Germany. Spek, A. L. (2001). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; #=================================================================== # CIF-file generated for KUNC 4357-123 # Compound 3a data_KUNC-4357-123 _database_code_depnum_ccdc_archive 'CCDC 257302' _audit_creation_date 9-Nov-04 _audit_creation_method 'PLATON option' _audit_update_record ; 10-Nov-04 Updated by the Author E.H. Text writing by E.H. Checkcif OK 11-Nov-04 Updated by the Author E.H. 24-Nov-04 Updated by the Author E.H. ; #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C26 H46 P2 Pt Si Ti' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H46 P2 Pt Si Ti' _chemical_formula_weight 691.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 21 21 21' 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 _cell_length_a 7.8446(1) _cell_length_b 17.6912(1) _cell_length_c 20.2936(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2816.35(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 2980 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 25.36 _exptl_crystal_description fragment _exptl_crystal_colour green _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method none _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 5.414 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.154 _exptl_absorpt_correction_T_max 0.338 _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 5 s per film repetition 1 dx 40 1147 films measured in 9 data sets set 1: phi-scan with delta_phi = 1.0 set 2 to 9: omega-scans with delta_omega = 1.0 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Straight forward after integration with the program NPROCESS, source: Nonius (2001b). Hydrogen atoms could be located in the difference Fourier maps and refined freely. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 68763 _diffrn_reflns_av_R_equivalents 0.065 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.36 _reflns_number_total 5155 _reflns_number_gt 5071 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or 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 sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0191P)^2^+1.5843P] 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 refall _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(4) _chemical_absolute_configuration ad _refine_ls_number_reflns 5155 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0167 _refine_ls_R_factor_gt 0.0160 _refine_ls_wR_factor_ref 0.0366 _refine_ls_wR_factor_gt 0.0364 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.671 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.073 #=================================================================== # 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 _atom_site_calc_flag _atom_site_refinement_flags Pt Pt Uani 0.95143(1) 0.47009(1) 0.13474(1) 1.000 0.0141(1) . . Ti Ti Uani 1.19036(7) 0.65413(3) 0.07199(3) 1.000 0.0147(2) . . P1 P Uani 0.82105(11) 0.35542(5) 0.11832(4) 1.000 0.0190(3) . . P2 P Uani 0.95899(10) 0.47124(5) 0.25234(3) 1.000 0.0163(2) . . Si Si Uani 0.94637(13) 0.49932(5) 0.01987(4) 1.000 0.0158(2) . . C1 C Uani 1.0786(4) 0.57392(16) 0.14237(15) 1.000 0.0144(8) . . C2 C Uani 0.9776(4) 0.64094(17) 0.14159(16) 1.000 0.0170(9) . . C3 C Uani 1.0291(4) 0.71840(17) 0.14164(15) 1.000 0.0188(9) . . C4 C Uani 1.1971(4) 0.74944(19) 0.14275(17) 1.000 0.0208(10) . . C5 C Uani 1.3548(4) 0.71045(19) 0.14594(16) 1.000 0.0203(10) . . C6 C Uani 1.3822(4) 0.6313(2) 0.14824(16) 1.000 0.0222(10) . . C7 C Uani 1.2599(4) 0.57140(19) 0.14723(16) 1.000 0.0191(10) . . C8 C Uani 1.0924(4) 0.57719(18) -0.00979(15) 1.000 0.0170(9) . . C9 C Uani 1.2742(4) 0.5764(2) -0.01243(16) 1.000 0.0194(10) . . C10 C Uani 1.3352(4) 0.64961(19) -0.02836(15) 1.000 0.0200(10) . . C11 C Uani 1.1932(5) 0.6970(2) -0.03670(15) 1.000 0.0206(10) . . C12 C Uani 1.0441(5) 0.65294(18) -0.02631(14) 1.000 0.0184(9) . . C13 C Uani 1.0000(5) 0.4228(2) -0.04289(19) 1.000 0.0277(12) . . C14 C Uani 0.7304(4) 0.5388(2) -0.00340(18) 1.000 0.0235(11) . . C15 C Uani 0.9686(5) 0.2830(2) 0.0883(2) 1.000 0.0310(11) . . C16 C Uani 1.1041(5) 0.2610(2) 0.1395(3) 1.000 0.0450(16) . . C17 C Uani 0.6482(5) 0.3505(2) 0.05766(19) 1.000 0.0257(11) . . C18 C Uani 0.4907(5) 0.3941(3) 0.0781(2) 1.000 0.0387(16) . . C19 C Uani 0.7151(5) 0.3085(2) 0.18825(18) 1.000 0.0257(11) . . C20 C Uani 0.6317(6) 0.2318(2) 0.1761(2) 1.000 0.0320(12) . . C21 C Uani 1.0707(5) 0.39421(19) 0.29439(18) 1.000 0.0246(11) . . C22 C Uani 1.2628(6) 0.3958(3) 0.2848(3) 1.000 0.0413(16) . . C23 C Uani 0.7475(4) 0.4712(2) 0.29113(16) 1.000 0.0215(10) . . C24 C Uani 0.6355(6) 0.5333(3) 0.2637(2) 1.000 0.0393(14) . . C25 C Uani 1.0558(6) 0.55540(19) 0.28988(16) 1.000 0.0232(10) . . C26 C Uani 1.0468(6) 0.5597(2) 0.36509(18) 1.000 0.0318(11) . . H21 H Uiso 0.859(4) 0.6356(18) 0.1289(18) 1.000 0.017(8) . . H31 H Uiso 0.941(4) 0.7537(18) 0.1305(17) 1.000 0.015(8) . . H41 H Uiso 1.202(5) 0.800(2) 0.135(2) 1.000 0.031(10) . . H51 H Uiso 1.447(5) 0.7377(18) 0.1409(15) 1.000 0.015(8) . . H61 H Uiso 1.501(4) 0.6154(17) 0.1448(16) 1.000 0.009(8) . . H71 H Uiso 1.308(4) 0.526(2) 0.1432(16) 1.000 0.022(9) . . H91 H Uiso 1.342(4) 0.537(2) -0.0031(15) 1.000 0.011(8) . . H101 H Uiso 1.452(6) 0.665(2) -0.0313(19) 1.000 0.037(10) . . H111 H Uiso 1.192(5) 0.751(2) -0.0451(17) 1.000 0.024(10) . . H121 H Uiso 0.934(5) 0.6704(19) -0.0275(17) 1.000 0.019(9) . . H131 H Uiso 0.921(5) 0.375(2) -0.0421(19) 1.000 0.035(11) . . H132 H Uiso 0.992(6) 0.445(3) -0.085(2) 1.000 0.054(14) . . H133 H Uiso 1.109(6) 0.406(2) -0.038(2) 1.000 0.034(12) . . H141 H Uiso 0.689(6) 0.582(3) 0.026(2) 1.000 0.046(12) . . H142 H Uiso 0.640(6) 0.506(3) -0.002(2) 1.000 0.045(13) . . H143 H Uiso 0.727(6) 0.562(2) -0.048(2) 1.000 0.044(12) . . H151 H Uiso 1.025(6) 0.304(2) 0.051(2) 1.000 0.048(13) . . H152 H Uiso 0.908(5) 0.237(2) 0.0760(18) 1.000 0.030(11) . . H161 H Uiso 1.165(6) 0.304(3) 0.157(2) 1.000 0.049(14) . . H162 H Uiso 1.186(6) 0.228(3) 0.118(2) 1.000 0.046(13) . . H163 H Uiso 1.046(7) 0.238(3) 0.183(2) 1.000 0.064(15) . . H171 H Uiso 0.696(5) 0.371(2) 0.020(2) 1.000 0.035(11) . . H172 H Uiso 0.619(5) 0.298(2) 0.0478(18) 1.000 0.028(10) . . H181 H Uiso 0.445(5) 0.3717(19) 0.1087(17) 1.000 0.015(9) . . H182 H Uiso 0.503(5) 0.443(3) 0.088(2) 1.000 0.041(13) . . H183 H Uiso 0.394(5) 0.398(2) 0.042(2) 1.000 0.033(11) . . H191 H Uiso 0.635(5) 0.346(2) 0.210(2) 1.000 0.037(11) . . H192 H Uiso 0.794(5) 0.305(2) 0.223(2) 1.000 0.030(10) . . H201 H Uiso 0.547(7) 0.231(2) 0.148(2) 1.000 0.049(13) . . H202 H Uiso 0.583(6) 0.206(2) 0.219(2) 1.000 0.054(13) . . H203 H Uiso 0.718(7) 0.197(3) 0.158(2) 1.000 0.057(15) . . H211 H Uiso 1.029(5) 0.351(2) 0.2759(19) 1.000 0.031(11) . . H212 H Uiso 1.041(5) 0.399(2) 0.3434(18) 1.000 0.029(10) . . H221 H Uiso 1.313(6) 0.350(3) 0.298(2) 1.000 0.054(14) . . H222 H Uiso 1.283(6) 0.405(3) 0.240(2) 1.000 0.051(14) . . H223 H Uiso 1.315(6) 0.435(3) 0.311(2) 1.000 0.048(13) . . H231 H Uiso 0.758(4) 0.477(2) 0.3361(18) 1.000 0.017(8) . . H232 H Uiso 0.702(5) 0.424(2) 0.2836(17) 1.000 0.022(10) . . H241 H Uiso 0.624(6) 0.529(3) 0.213(3) 1.000 0.060(14) . . H242 H Uiso 0.513(6) 0.536(3) 0.289(2) 1.000 0.053(13) . . H243 H Uiso 0.685(6) 0.578(3) 0.273(2) 1.000 0.042(14) . . H251 H Uiso 1.003(4) 0.601(2) 0.2685(17) 1.000 0.019(9) . . H252 H Uiso 1.166(6) 0.558(2) 0.275(2) 1.000 0.041(13) . . H261 H Uiso 1.107(6) 0.518(3) 0.384(2) 1.000 0.055(14) . . H262 H Uiso 1.116(5) 0.603(2) 0.3812(19) 1.000 0.037(11) . . H263 H Uiso 0.930(6) 0.566(3) 0.380(2) 1.000 0.059(15) . . 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 Pt 0.0166(1) 0.0130(1) 0.0127(1) 0.0010(1) 0.0001(1) 0.0000(1) Ti 0.0180(3) 0.0152(3) 0.0110(3) 0.0017(2) 0.0004(2) -0.0002(2) P1 0.0216(4) 0.0154(4) 0.0200(5) -0.0007(3) 0.0003(3) -0.0017(3) P2 0.0203(4) 0.0159(3) 0.0126(4) 0.0035(3) -0.0014(3) -0.0027(5) Si 0.0173(4) 0.0176(4) 0.0125(4) -0.0009(3) 0.0005(4) 0.0001(4) C1 0.0150(14) 0.0155(15) 0.0128(15) 0.0019(12) -0.0019(12) 0.0029(11) C2 0.0200(16) 0.0182(15) 0.0128(15) -0.0002(13) 0.0039(13) -0.0023(13) C3 0.0245(16) 0.0178(15) 0.0142(16) 0.0007(13) 0.0008(15) 0.0054(14) C4 0.0329(18) 0.0149(16) 0.0146(17) -0.0003(14) 0.0012(15) -0.0036(13) C5 0.0221(16) 0.0236(17) 0.0151(18) 0.0035(13) -0.0033(14) -0.0096(14) C6 0.0174(15) 0.0282(18) 0.0209(19) 0.0069(14) -0.0027(13) -0.0016(14) C7 0.0238(16) 0.0142(17) 0.0193(19) 0.0027(13) -0.0009(13) 0.0036(13) C8 0.0195(17) 0.0218(17) 0.0098(15) -0.0003(13) 0.0008(12) -0.0001(13) C9 0.0213(17) 0.0222(19) 0.0146(17) -0.0010(14) 0.0041(13) 0.0045(15) C10 0.0215(17) 0.0255(17) 0.0131(16) 0.0031(14) 0.0031(13) -0.0015(15) C11 0.0307(18) 0.0215(18) 0.0097(16) 0.0059(13) -0.0006(14) -0.0015(15) C12 0.0189(16) 0.0240(16) 0.0123(15) 0.0034(12) -0.0013(15) 0.0046(16) C13 0.035(2) 0.026(2) 0.022(2) -0.0039(16) 0.0067(15) -0.0016(16) C14 0.0171(16) 0.029(2) 0.0243(19) 0.0016(17) -0.0044(13) -0.0007(16) C15 0.033(2) 0.0189(18) 0.041(2) -0.0062(16) 0.011(2) 0.0025(17) C16 0.032(2) 0.024(2) 0.079(4) -0.009(2) -0.007(3) 0.0052(17) C17 0.0258(19) 0.0252(19) 0.026(2) -0.0007(16) -0.0035(15) -0.0060(16) C18 0.028(2) 0.044(3) 0.044(3) 0.017(2) 0.0047(18) 0.0030(18) C19 0.031(2) 0.0259(19) 0.0202(19) 0.0007(15) -0.0028(16) -0.0084(16) C20 0.040(2) 0.026(2) 0.030(2) -0.0002(17) -0.002(2) -0.0127(18) C21 0.031(2) 0.0199(18) 0.0229(19) 0.0062(14) -0.0073(17) -0.0012(16) C22 0.030(2) 0.039(3) 0.055(3) 0.015(2) -0.009(2) 0.003(2) C23 0.0245(16) 0.0247(18) 0.0153(17) 0.0006(16) 0.0015(13) -0.0028(17) C24 0.034(2) 0.046(3) 0.038(2) 0.010(2) 0.0042(18) 0.010(2) C25 0.0321(19) 0.0207(17) 0.0169(16) 0.0046(13) -0.0009(18) -0.0082(17) C26 0.051(2) 0.0252(18) 0.0193(17) 0.0010(15) -0.012(2) -0.0129(19) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== 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 Pt P1 2.2962(9) . . yes Pt P2 2.3874(6) . . yes Pt Si 2.3881(8) . . yes Pt C1 2.096(3) . . yes Ti C1 2.196(3) . . yes Ti C2 2.199(3) . . yes Ti C3 2.212(3) . . yes Ti C4 2.215(3) . . yes Ti C5 2.216(3) . . yes Ti C6 2.196(3) . . yes Ti C7 2.184(3) . . yes Ti C8 2.280(3) . . yes Ti C9 2.293(3) . . yes Ti C10 2.333(3) . . yes Ti C11 2.333(3) . . yes Ti C12 2.301(3) . . yes P1 C15 1.831(4) . . yes P1 C17 1.833(4) . . yes P1 C19 1.842(4) . . yes P2 C21 1.831(4) . . yes P2 C23 1.836(3) . . yes P2 C25 1.837(4) . . yes Si C8 1.890(3) . . yes Si C13 1.906(4) . . yes Si C14 1.892(3) . . yes C1 C2 1.426(4) . . no C1 C7 1.426(4) . . no C2 C3 1.429(4) . . no C3 C4 1.428(4) . . no C4 C5 1.418(5) . . no C5 C6 1.417(5) . . no C6 C7 1.430(5) . . no C8 C9 1.427(4) . . no C8 C12 1.432(5) . . no C9 C10 1.418(5) . . no C10 C11 1.404(5) . . no C11 C12 1.421(5) . . no C15 C16 1.537(6) . . no C17 C18 1.514(6) . . no C19 C20 1.526(5) . . no C21 C22 1.520(6) . . no C23 C24 1.513(6) . . no C25 C26 1.530(5) . . no C2 H21 0.97(3) . . no C3 H31 0.96(3) . . no C4 H41 0.91(4) . . no C5 H51 0.88(4) . . no C6 H61 0.98(3) . . no C7 H71 0.89(3) . . no C9 H91 0.90(3) . . no C10 H101 0.96(5) . . no C11 H111 0.97(4) . . no C12 H121 0.92(4) . . no C13 H131 1.05(4) . . no C13 H132 0.94(4) . . no C13 H133 0.91(5) . . no C14 H141 1.02(5) . . no C14 H142 0.92(5) . . no C14 H143 0.99(4) . . no C15 H151 0.95(4) . . no C15 H152 0.97(4) . . no C16 H161 0.97(5) . . no C16 H162 0.97(5) . . no C16 H163 1.07(4) . . no C17 H171 0.93(4) . . no C17 H172 0.98(4) . . no C18 H181 0.82(4) . . no C18 H182 0.89(5) . . no C18 H183 1.06(4) . . no C19 H191 1.01(4) . . no C19 H192 0.94(4) . . no C20 H201 0.88(5) . . no C20 H202 1.05(4) . . no C20 H203 0.99(5) . . no C21 H211 0.91(4) . . no C21 H212 1.03(4) . . no C22 H221 0.94(5) . . no C22 H222 0.94(4) . . no C22 H223 0.97(5) . . no C23 H231 0.92(4) . . no C23 H232 0.92(4) . . no C24 H241 1.04(6) . . no C24 H242 1.09(5) . . no C24 H243 0.90(5) . . no C25 H251 1.01(3) . . no C25 H252 0.92(5) . . no C26 H261 0.96(5) . . no C26 H262 0.99(4) . . no C26 H263 0.97(5) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt P2 99.42(3) . . . yes P1 Pt Si 92.42(3) . . . yes P1 Pt C1 175.54(9) . . . yes P2 Pt Si 167.00(3) . . . yes P2 Pt C1 84.66(9) . . . yes Si Pt C1 83.70(9) . . . yes C1 Ti C2 37.87(11) . . . yes C1 Ti C3 71.83(11) . . . yes C1 Ti C4 94.58(12) . . . yes C1 Ti C5 94.73(12) . . . yes C1 Ti C6 72.33(12) . . . yes C1 Ti C7 38.01(12) . . . yes C1 Ti C8 87.31(11) . . . yes C1 Ti C9 102.29(12) . . . yes C1 Ti C10 137.72(12) . . . yes C1 Ti C11 145.99(12) . . . yes C1 Ti C12 111.03(12) . . . yes C2 Ti C3 37.80(11) . . . yes C2 Ti C4 71.49(12) . . . yes C2 Ti C5 93.13(12) . . . yes C2 Ti C6 92.75(12) . . . yes C2 Ti C7 70.70(12) . . . yes C2 Ti C8 98.53(12) . . . yes C2 Ti C9 129.34(12) . . . yes C2 Ti C10 157.91(12) . . . yes C2 Ti C11 130.48(13) . . . yes C2 Ti C12 100.22(13) . . . yes C3 Ti C4 37.63(11) . . . yes C3 Ti C5 70.67(12) . . . yes C3 Ti C6 92.07(12) . . . yes C3 Ti C7 92.33(12) . . . yes C3 Ti C8 125.41(12) . . . yes C3 Ti C9 161.78(12) . . . yes C3 Ti C10 148.64(12) . . . yes C3 Ti C11 116.27(12) . . . yes C3 Ti C12 105.87(12) . . . yes C4 Ti C5 37.32(12) . . . yes C4 Ti C6 70.54(13) . . . yes C4 Ti C7 92.92(13) . . . yes C4 Ti C8 159.12(12) . . . yes C4 Ti C9 159.04(12) . . . yes C4 Ti C10 125.46(12) . . . yes C4 Ti C11 111.42(12) . . . yes C4 Ti C12 125.50(12) . . . yes C5 Ti C6 37.48(13) . . . yes C5 Ti C7 71.48(12) . . . yes C5 Ti C8 163.30(12) . . . yes C5 Ti C9 127.50(12) . . . yes C5 Ti C10 108.85(12) . . . yes C5 Ti C11 119.26(13) . . . yes C5 Ti C12 151.82(12) . . . yes C6 Ti C7 38.10(12) . . . yes C6 Ti C8 129.36(12) . . . yes C6 Ti C9 102.68(12) . . . yes C6 Ti C10 105.96(12) . . . yes C6 Ti C11 136.02(13) . . . yes C6 Ti C12 161.95(13) . . . yes C7 Ti C8 101.13(12) . . . yes C7 Ti C9 92.80(12) . . . yes C7 Ti C10 117.74(12) . . . yes C7 Ti C11 151.22(13) . . . yes C7 Ti C12 136.41(12) . . . yes C8 Ti C9 36.37(11) . . . yes C8 Ti C10 60.55(11) . . . yes C8 Ti C11 60.59(12) . . . yes C8 Ti C12 36.44(11) . . . yes C9 Ti C10 35.68(12) . . . yes C9 Ti C11 59.05(12) . . . yes C9 Ti C12 59.33(12) . . . yes C10 Ti C11 35.03(12) . . . yes C10 Ti C12 59.06(12) . . . yes C11 Ti C12 35.71(13) . . . yes Pt P1 C15 112.64(12) . . . yes Pt P1 C17 117.96(12) . . . yes Pt P1 C19 119.16(12) . . . yes C15 P1 C17 102.18(18) . . . yes C15 P1 C19 103.08(17) . . . yes C17 P1 C19 99.33(17) . . . yes Pt P2 C21 118.12(12) . . . yes Pt P2 C23 113.96(11) . . . yes Pt P2 C25 115.58(11) . . . yes C21 P2 C23 103.43(16) . . . yes C21 P2 C25 102.24(17) . . . yes C23 P2 C25 101.31(18) . . . yes Pt Si C8 117.30(10) . . . yes Pt Si C13 119.66(12) . . . yes Pt Si C14 109.78(12) . . . yes C8 Si C13 99.85(15) . . . yes C8 Si C14 101.19(15) . . . yes C13 Si C14 107.04(17) . . . yes Pt C1 Ti 135.09(15) . . . yes Pt C1 C2 117.6(2) . . . yes Pt C1 C7 116.9(2) . . . yes Ti C1 C2 71.18(17) . . . yes Ti C1 C7 70.55(18) . . . yes C2 C1 C7 125.5(3) . . . no Ti C2 C1 70.95(18) . . . yes Ti C2 C3 71.58(18) . . . yes C1 C2 C3 129.8(3) . . . no Ti C3 C2 70.62(18) . . . yes Ti C3 C4 71.33(18) . . . yes C2 C3 C4 129.0(3) . . . no Ti C4 C3 71.04(18) . . . yes Ti C4 C5 71.35(19) . . . yes C3 C4 C5 128.2(3) . . . no Ti C5 C4 71.33(19) . . . yes Ti C5 C6 70.51(19) . . . yes C4 C5 C6 127.9(3) . . . no Ti C6 C5 72.01(19) . . . yes Ti C6 C7 70.51(18) . . . yes C5 C6 C7 129.1(3) . . . no Ti C7 C1 71.44(18) . . . yes Ti C7 C6 71.39(19) . . . yes C1 C7 C6 130.3(3) . . . no Ti C8 Si 114.06(15) . . . yes Ti C8 C9 72.32(19) . . . yes Ti C8 C12 72.60(18) . . . yes Si C8 C9 127.6(2) . . . yes Si C8 C12 126.6(3) . . . yes C9 C8 C12 105.3(3) . . . no Ti C9 C8 71.31(18) . . . yes Ti C9 C10 73.70(19) . . . yes C8 C9 C10 109.7(3) . . . no Ti C10 C9 70.61(18) . . . yes Ti C10 C11 72.45(18) . . . yes C9 C10 C11 107.8(3) . . . no Ti C11 C10 72.51(18) . . . yes Ti C11 C12 70.95(17) . . . yes C10 C11 C12 107.9(3) . . . no Ti C12 C8 70.96(18) . . . yes Ti C12 C11 73.34(19) . . . yes C8 C12 C11 109.3(3) . . . no P1 C15 C16 112.9(3) . . . yes P1 C17 C18 113.3(3) . . . yes P1 C19 C20 118.0(3) . . . yes P2 C21 C22 113.6(3) . . . yes P2 C23 C24 111.5(3) . . . yes P2 C25 C26 115.8(3) . . . yes Ti C2 H21 125(2) . . . no C1 C2 H21 117.1(19) . . . no C3 C2 H21 111.4(19) . . . no Ti C3 H31 127(2) . . . no C2 C3 H31 114.9(19) . . . no C4 C3 H31 114.7(19) . . . no Ti C4 H41 130(3) . . . no C3 C4 H41 115(2) . . . no C5 C4 H41 117(2) . . . no Ti C5 H51 131(2) . . . no C4 C5 H51 117(2) . . . no C6 C5 H51 115(2) . . . no Ti C6 H61 131.1(19) . . . no C5 C6 H61 115.3(18) . . . no C7 C6 H61 115.2(18) . . . no Ti C7 H71 130(2) . . . no C1 C7 H71 116(2) . . . no C6 C7 H71 113(2) . . . no Ti C9 H91 119(2) . . . no C8 C9 H91 126(2) . . . no C10 C9 H91 124(2) . . . no Ti C10 H101 121(2) . . . no C9 C10 H101 127(2) . . . no C11 C10 H101 126(2) . . . no Ti C11 H111 119(2) . . . no C10 C11 H111 128(2) . . . no C12 C11 H111 124(2) . . . no Ti C12 H121 119(2) . . . no C8 C12 H121 125(2) . . . no C11 C12 H121 126(2) . . . no Si C13 H131 116(2) . . . no Si C13 H132 107(3) . . . no Si C13 H133 111(2) . . . no H131 C13 H132 108(4) . . . no H131 C13 H133 107(3) . . . no H132 C13 H133 107(4) . . . no Si C14 H141 114(3) . . . no Si C14 H142 117(3) . . . no Si C14 H143 114(3) . . . no H141 C14 H142 102(4) . . . no H141 C14 H143 102(3) . . . no H142 C14 H143 106(4) . . . no P1 C15 H151 107(2) . . . no P1 C15 H152 111(2) . . . no C16 C15 H151 108(3) . . . no C16 C15 H152 107(2) . . . no H151 C15 H152 110(3) . . . no C15 C16 H161 113(3) . . . no C15 C16 H162 108(3) . . . no C15 C16 H163 111(3) . . . no H161 C16 H162 108(4) . . . no H161 C16 H163 102(4) . . . no H162 C16 H163 115(4) . . . no P1 C17 H171 104(2) . . . no P1 C17 H172 111(2) . . . no C18 C17 H171 111(2) . . . no C18 C17 H172 110(2) . . . no H171 C17 H172 107(3) . . . no C17 C18 H181 109(3) . . . no C17 C18 H182 118(3) . . . no C17 C18 H183 115(2) . . . no H181 C18 H182 110(4) . . . no H181 C18 H183 104(3) . . . no H182 C18 H183 100(3) . . . no P1 C19 H191 109(2) . . . no P1 C19 H192 108(2) . . . no C20 C19 H191 113(2) . . . no C20 C19 H192 110(2) . . . no H191 C19 H192 97(3) . . . no C19 C20 H201 116(2) . . . no C19 C20 H202 114(2) . . . no C19 C20 H203 109(3) . . . no H201 C20 H202 105(4) . . . no H201 C20 H203 106(4) . . . no H202 C20 H203 107(4) . . . no P2 C21 H211 105(2) . . . no P2 C21 H212 106(2) . . . no C22 C21 H211 109(3) . . . no C22 C21 H212 110(2) . . . no H211 C21 H212 113(3) . . . no C21 C22 H221 111(3) . . . no C21 C22 H222 107(3) . . . no C21 C22 H223 111(3) . . . no H221 C22 H222 111(4) . . . no H221 C22 H223 107(4) . . . no H222 C22 H223 110(4) . . . no P2 C23 H231 110(2) . . . no P2 C23 H232 106(2) . . . no C24 C23 H231 110(2) . . . no C24 C23 H232 112(2) . . . no H231 C23 H232 107(3) . . . no C23 C24 H241 111(3) . . . no C23 C24 H242 112(3) . . . no C23 C24 H243 108(3) . . . no H241 C24 H242 113(3) . . . no H241 C24 H243 108(4) . . . no H242 C24 H243 104(4) . . . no P2 C25 H251 107.5(19) . . . no P2 C25 H252 107(2) . . . no C26 C25 H251 112(2) . . . no C26 C25 H252 112(3) . . . no H251 C25 H252 102(3) . . . no C25 C26 H261 110(3) . . . no C25 C26 H262 110(2) . . . no C25 C26 H263 111(2) . . . no H261 C26 H262 101(4) . . . no H261 C26 H263 115(4) . . . no H262 C26 H263 109(4) . . . no # End of Crystallographic Information File # CIF-file generated for KUND 4425-123 # Compound 3b data_KUND-4425-123 _database_code_depnum_ccdc_archive 'CCDC 257303' _audit_creation_date 9-Nov-04 _audit_creation_method 'PLATON
option' _audit_update_record ; 10-Nov-04 Updated by the Author E.H. Text writing by E.H. Checkcif OK 11-Nov-04 Updated by the Author E.H. 24-Nov-04 Updated by the Author E.H. ; #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C26 H46 P2 Pt Si V' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H46 P2 Pt Si V' _chemical_formula_weight 694.68 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 21 21 21' 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 _cell_length_a 7.8629(1) _cell_length_b 17.7086(1) _cell_length_c 20.1938(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2811.80(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 2975 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 25.37 _exptl_crystal_description needle _exptl_crystal_colour blue-grey _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method none _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 5.471 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.214 _exptl_absorpt_correction_T_max 0.579 _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 10 s per film repetition 1 dx 40 1018 films measured in 9 data sets set 1: phi-scan with delta_phi = 1.0 set 2 to 9: omega-scans with delta_omega = 1.0 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Straight forward after integration with the program NPROCESS, source: Nonius (2001b). Hydrogen atoms could be located in the difference Fourier maps and refined freely. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 58165 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.37 _reflns_number_total 5129 _reflns_number_gt 5071 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or 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 sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0104P)^2^+2.1387P] 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 refall _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(3) _chemical_absolute_configuration ad _refine_ls_number_reflns 5129 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0132 _refine_ls_R_factor_gt 0.0128 _refine_ls_wR_factor_ref 0.0294 _refine_ls_wR_factor_gt 0.0293 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.484 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.059 #=================================================================== # 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 _atom_site_calc_flag _atom_site_refinement_flags Pt Pt Uani 0.95333(1) 0.47084(1) 0.13648(1) 1.000 0.0120(1) . . V V Uani 1.19168(6) 0.65255(3) 0.07235(2) 1.000 0.0121(1) . . P1 P Uani 0.82357(9) 0.35595(4) 0.11941(3) 1.000 0.0163(2) . . P2 P Uani 0.95833(9) 0.47174(4) 0.25456(3) 1.000 0.0145(2) . . Si Si Uani 0.94890(11) 0.50044(4) 0.02102(3) 1.000 0.0135(2) . . C1 C Uani 1.0801(3) 0.57429(14) 0.14429(12) 1.000 0.0125(7) . . C2 C Uani 0.9806(3) 0.64148(14) 0.14192(13) 1.000 0.0139(7) . . C3 C Uani 1.0331(4) 0.71880(14) 0.13965(13) 1.000 0.0166(7) . . C4 C Uani 1.1997(4) 0.74942(15) 0.13960(15) 1.000 0.0186(8) . . C5 C Uani 1.3565(4) 0.71057(16) 0.14359(14) 1.000 0.0187(8) . . C6 C Uani 1.3820(4) 0.63191(16) 0.14845(13) 1.000 0.0188(8) . . C7 C Uani 1.2600(3) 0.57256(16) 0.14913(13) 1.000 0.0164(8) . . C8 C Uani 1.0954(3) 0.57884(16) -0.00754(12) 1.000 0.0143(8) . . C9 C Uani 1.2767(3) 0.57801(16) -0.00977(13) 1.000 0.0150(8) . . C10 C Uani 1.3378(3) 0.65142(16) -0.02444(13) 1.000 0.0165(8) . . C11 C Uani 1.1962(4) 0.69917(16) -0.03255(13) 1.000 0.0170(8) . . C12 C Uani 1.0476(4) 0.65486(14) -0.02312(12) 1.000 0.0145(7) . . C13 C Uani 1.0016(4) 0.42436(18) -0.04252(15) 1.000 0.0231(10) . . C14 C Uani 0.7336(4) 0.5404(2) -0.00215(15) 1.000 0.0213(9) . . C15 C Uani 0.9719(4) 0.28373(17) 0.08908(18) 1.000 0.0276(10) . . C16 C Uani 1.1069(5) 0.2620(2) 0.1402(3) 1.000 0.0445(13) . . C17 C Uani 0.6509(4) 0.35154(18) 0.05827(16) 1.000 0.0229(9) . . C18 C Uani 0.4924(4) 0.3942(2) 0.0790(2) 1.000 0.0363(12) . . C19 C Uani 0.7181(4) 0.30797(18) 0.18964(15) 1.000 0.0231(9) . . C20 C Uani 0.6368(5) 0.23125(18) 0.17636(18) 1.000 0.0290(11) . . C21 C Uani 1.0696(4) 0.39490(16) 0.29754(15) 1.000 0.0216(9) . . C22 C Uani 1.2616(5) 0.3961(2) 0.2881(2) 1.000 0.0378(14) . . C23 C Uani 0.7465(3) 0.4716(2) 0.29247(14) 1.000 0.0194(8) . . C24 C Uani 0.6359(5) 0.5340(3) 0.26402(19) 1.000 0.0373(11) . . C25 C Uani 1.0532(5) 0.55630(16) 0.29273(13) 1.000 0.0199(8) . . C26 C Uani 1.0420(5) 0.56071(18) 0.36823(15) 1.000 0.0284(9) . . H21 H Uiso 0.853(3) 0.6345(15) 0.1301(15) 1.000 0.014(7) . . H31 H Uiso 0.936(4) 0.7548(15) 0.1295(15) 1.000 0.016(7) . . H41 H Uiso 1.205(3) 0.8010(17) 0.1287(15) 1.000 0.015(7) . . H51 H Uiso 1.455(4) 0.7400(16) 0.1361(14) 1.000 0.019(7) . . H61 H Uiso 1.496(3) 0.6144(15) 0.1456(14) 1.000 0.009(7) . . H71 H Uiso 1.308(3) 0.5283(17) 0.1443(13) 1.000 0.014(7) . . H91 H Uiso 1.344(3) 0.5374(19) 0.0000(13) 1.000 0.012(7) . . H101 H Uiso 1.445(5) 0.6675(17) -0.0247(15) 1.000 0.024(8) . . H111 H Uiso 1.202(4) 0.7522(18) -0.0415(14) 1.000 0.020(8) . . H121 H Uiso 0.942(4) 0.6731(15) -0.0247(13) 1.000 0.009(7) . . H131 H Uiso 0.927(4) 0.3778(19) -0.0451(16) 1.000 0.028(9) . . H132 H Uiso 0.999(4) 0.447(2) -0.0860(18) 1.000 0.040(10) . . H133 H Uiso 1.119(4) 0.4059(19) -0.0389(16) 1.000 0.024(9) . . H141 H Uiso 0.692(4) 0.580(2) 0.0298(17) 1.000 0.030(9) . . H142 H Uiso 0.645(4) 0.5050(19) -0.0020(16) 1.000 0.030(9) . . H143 H Uiso 0.732(5) 0.563(2) -0.043(2) 1.000 0.042(11) . . H151 H Uiso 1.020(5) 0.3032(19) 0.0514(17) 1.000 0.034(10) . . H152 H Uiso 0.910(4) 0.2368(18) 0.0736(14) 1.000 0.021(8) . . H161 H Uiso 1.170(5) 0.311(2) 0.1544(19) 1.000 0.050(12) . . H162 H Uiso 1.192(6) 0.229(2) 0.117(2) 1.000 0.056(12) . . H163 H Uiso 1.056(7) 0.240(3) 0.180(2) 1.000 0.074(15) . . H171 H Uiso 0.692(4) 0.3735(17) 0.0167(16) 1.000 0.019(8) . . H172 H Uiso 0.627(4) 0.2993(19) 0.0491(15) 1.000 0.024(8) . . H181 H Uiso 0.444(5) 0.3723(18) 0.1147(17) 1.000 0.030(9) . . H182 H Uiso 0.506(5) 0.445(2) 0.091(2) 1.000 0.057(13) . . H183 H Uiso 0.400(5) 0.401(2) 0.043(2) 1.000 0.059(13) . . H191 H Uiso 0.634(4) 0.3472(19) 0.2062(16) 1.000 0.028(9) . . H192 H Uiso 0.802(4) 0.3029(18) 0.2222(17) 1.000 0.025(8) . . H201 H Uiso 0.553(5) 0.2334(19) 0.1475(18) 1.000 0.037(10) . . H202 H Uiso 0.589(5) 0.211(2) 0.215(2) 1.000 0.048(11) . . H203 H Uiso 0.719(6) 0.197(2) 0.158(2) 1.000 0.061(14) . . H211 H Uiso 1.020(4) 0.3492(18) 0.2804(15) 1.000 0.021(8) . . H212 H Uiso 1.042(4) 0.3980(16) 0.3443(15) 1.000 0.022(8) . . H221 H Uiso 1.313(6) 0.350(3) 0.302(2) 1.000 0.059(13) . . H222 H Uiso 1.290(5) 0.407(2) 0.242(2) 1.000 0.046(11) . . H223 H Uiso 1.307(6) 0.435(3) 0.314(2) 1.000 0.066(14) . . H231 H Uiso 0.755(4) 0.4779(18) 0.3388(15) 1.000 0.021(8) . . H232 H Uiso 0.701(4) 0.4237(18) 0.2872(14) 1.000 0.014(8) . . H241 H Uiso 0.620(6) 0.529(3) 0.214(2) 1.000 0.077(14) . . H242 H Uiso 0.518(4) 0.534(2) 0.2860(17) 1.000 0.040(10) . . H243 H Uiso 0.686(5) 0.580(3) 0.2726(19) 1.000 0.045(12) . . H251 H Uiso 1.009(4) 0.6039(17) 0.2727(14) 1.000 0.016(8) . . H252 H Uiso 1.166(5) 0.557(2) 0.2791(17) 1.000 0.034(10) . . H261 H Uiso 1.096(4) 0.518(2) 0.3880(17) 1.000 0.037(10) . . H262 H Uiso 1.112(4) 0.602(2) 0.3850(16) 1.000 0.032(9) . . H263 H Uiso 0.922(6) 0.566(3) 0.385(2) 1.000 0.081(16) . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.0138(1) 0.0103(1) 0.0119(1) 0.0010(1) 0.0000(1) -0.0001(1) V 0.0138(2) 0.0120(2) 0.0104(2) 0.0013(2) 0.0001(2) 0.0001(2) P1 0.0191(3) 0.0117(3) 0.0182(4) -0.0004(3) 0.0003(3) -0.0013(3) P2 0.0181(3) 0.0134(3) 0.0119(3) 0.0030(3) -0.0020(3) -0.0025(4) Si 0.0141(3) 0.0146(3) 0.0118(3) -0.0007(3) 0.0000(3) 0.0005(3) C1 0.0152(13) 0.0119(13) 0.0104(12) 0.0014(10) -0.0004(10) -0.0007(9) C2 0.0168(13) 0.0140(13) 0.0108(12) 0.0000(11) 0.0010(11) -0.0034(10) C3 0.0228(13) 0.0144(13) 0.0127(12) 0.0004(11) 0.0012(14) 0.0044(12) C4 0.0298(15) 0.0132(14) 0.0127(13) -0.0017(12) 0.0014(13) -0.0035(11) C5 0.0199(14) 0.0214(14) 0.0148(14) 0.0017(12) -0.0041(12) -0.0095(11) C6 0.0164(13) 0.0250(15) 0.0150(15) 0.0042(11) -0.0024(11) -0.0009(12) C7 0.0197(14) 0.0138(15) 0.0158(15) 0.0032(11) -0.0002(11) 0.0023(11) C8 0.0165(14) 0.0190(15) 0.0074(12) 0.0018(10) -0.0002(10) 0.0003(11) C9 0.0177(14) 0.0165(15) 0.0108(13) -0.0008(11) 0.0016(10) 0.0027(12) C10 0.0146(14) 0.0237(15) 0.0113(13) 0.0013(11) 0.0039(11) -0.0015(12) C11 0.0232(14) 0.0159(15) 0.0119(14) 0.0051(11) 0.0002(11) -0.0033(12) C12 0.0151(13) 0.0192(13) 0.0093(12) 0.0008(10) -0.0035(12) 0.0027(13) C13 0.0294(19) 0.0210(17) 0.0190(16) -0.0043(12) 0.0061(11) -0.0041(12) C14 0.0173(14) 0.0268(19) 0.0197(15) -0.0007(14) -0.0031(11) 0.0021(14) C15 0.0272(16) 0.0148(15) 0.0408(19) -0.0043(14) 0.0058(16) -0.0003(13) C16 0.0297(18) 0.0269(19) 0.077(3) -0.001(2) -0.008(2) 0.0059(15) C17 0.0264(16) 0.0201(16) 0.0221(16) 0.0016(13) -0.0043(13) -0.0046(13) C18 0.026(2) 0.041(2) 0.042(2) 0.0168(18) 0.0028(15) 0.0047(15) C19 0.0283(17) 0.0230(16) 0.0181(15) 0.0007(12) -0.0019(13) -0.0095(13) C20 0.0359(19) 0.0207(17) 0.0305(19) 0.0021(14) -0.0021(16) -0.0105(15) C21 0.0268(17) 0.0175(15) 0.0205(15) 0.0043(11) -0.0077(14) -0.0027(13) C22 0.0285(19) 0.033(2) 0.052(3) 0.0143(19) -0.0072(17) 0.0064(16) C23 0.0207(14) 0.0220(15) 0.0155(14) 0.0011(13) 0.0036(11) -0.0054(14) C24 0.0298(18) 0.043(2) 0.039(2) 0.0102(19) 0.0047(15) 0.011(2) C25 0.0274(16) 0.0160(14) 0.0163(14) 0.0016(11) 0.0005(15) -0.0061(14) C26 0.0454(18) 0.0254(16) 0.0145(14) 0.0017(13) -0.0057(19) -0.0140(16) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== 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 Pt P1 2.3020(7) . . yes Pt P2 2.3849(6) . . yes Pt Si 2.3900(6) . . yes Pt C1 2.092(2) . . yes V C1 2.191(2) . . yes V C2 2.183(3) . . yes V C3 2.186(3) . . yes V C4 2.189(3) . . yes V C5 2.192(3) . . yes V C6 2.176(3) . . yes V C7 2.168(3) . . yes V C8 2.209(3) . . yes V C9 2.222(3) . . yes V C10 2.267(3) . . yes V C11 2.274(3) . . yes V C12 2.236(3) . . yes P1 C15 1.836(3) . . yes P1 C17 1.837(3) . . yes P1 C19 1.850(3) . . yes P2 C21 1.836(3) . . yes P2 C23 1.833(3) . . yes P2 C25 1.842(3) . . yes Si C8 1.894(3) . . yes Si C13 1.906(3) . . yes Si C14 1.894(3) . . yes C1 C2 1.425(3) . . no C1 C7 1.418(3) . . no C2 C3 1.431(4) . . no C3 C4 1.418(4) . . no C4 C5 1.414(4) . . no C5 C6 1.411(4) . . no C6 C7 1.423(4) . . no C8 C9 1.426(3) . . no C8 C12 1.433(4) . . no C9 C10 1.417(4) . . no C10 C11 1.408(4) . . no C11 C12 1.420(4) . . no C15 C16 1.530(6) . . no C17 C18 1.516(5) . . no C19 C20 1.525(5) . . no C21 C22 1.522(5) . . no C23 C24 1.519(6) . . no C25 C26 1.529(4) . . no C2 H21 1.04(2) . . no C3 H31 1.02(3) . . no C4 H41 0.94(3) . . no C5 H51 0.95(3) . . no C6 H61 0.95(2) . . no C7 H71 0.88(3) . . no C9 H91 0.91(3) . . no C10 H101 0.89(4) . . no C11 H111 0.96(3) . . no C12 H121 0.89(3) . . no C13 H131 1.01(3) . . no C13 H132 0.97(4) . . no C13 H133 0.98(3) . . no C14 H141 1.01(4) . . no C14 H142 0.94(3) . . no C14 H143 0.92(4) . . no C15 H151 0.92(4) . . no C15 H152 1.01(3) . . no C16 H161 1.04(4) . . no C16 H162 1.00(4) . . no C16 H163 0.98(4) . . no C17 H171 0.98(3) . . no C17 H172 0.96(3) . . no C18 H181 0.90(3) . . no C18 H182 0.94(4) . . no C18 H183 1.03(4) . . no C19 H191 1.02(3) . . no C19 H192 0.94(3) . . no C20 H201 0.88(4) . . no C20 H202 0.94(4) . . no C20 H203 0.96(4) . . no C21 H211 0.96(3) . . no C21 H212 0.97(3) . . no C22 H221 0.95(5) . . no C22 H222 0.98(4) . . no C22 H223 0.94(5) . . no C23 H231 0.94(3) . . no C23 H232 0.93(3) . . no C24 H241 1.02(4) . . no C24 H242 1.03(3) . . no C24 H243 0.92(5) . . no C25 H251 1.00(3) . . no C25 H252 0.93(4) . . no C26 H261 0.95(3) . . no C26 H262 0.98(3) . . no C26 H263 1.01(5) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt P2 99.38(2) . . . yes P1 Pt Si 92.37(2) . . . yes P1 Pt C1 175.31(7) . . . yes P2 Pt Si 166.95(3) . . . yes P2 Pt C1 84.89(7) . . . yes Si Pt C1 83.59(7) . . . yes C1 V C2 38.02(9) . . . yes C1 V C3 72.47(9) . . . yes C1 V C4 95.50(10) . . . yes C1 V C5 95.63(10) . . . yes C1 V C6 72.59(10) . . . yes C1 V C7 37.97(9) . . . yes C1 V C8 88.47(9) . . . yes C1 V C9 103.86(10) . . . yes C1 V C10 140.25(10) . . . yes C1 V C11 148.61(10) . . . yes C1 V C12 112.35(10) . . . yes C2 V C3 38.23(10) . . . yes C2 V C4 72.12(10) . . . yes C2 V C5 93.97(10) . . . yes C2 V C6 93.05(10) . . . yes C2 V C7 70.70(9) . . . yes C2 V C8 99.00(9) . . . yes C2 V C9 130.96(10) . . . yes C2 V C10 159.91(9) . . . yes C2 V C11 130.09(11) . . . yes C2 V C12 99.86(10) . . . yes C3 V C4 37.82(11) . . . yes C3 V C5 71.19(11) . . . yes C3 V C6 92.49(11) . . . yes C3 V C7 92.72(10) . . . yes C3 V C8 125.15(10) . . . yes C3 V C9 162.61(10) . . . yes C3 V C10 146.07(10) . . . yes C3 V C11 113.16(10) . . . yes C3 V C12 103.72(11) . . . yes C4 V C5 37.67(11) . . . yes C4 V C6 70.95(11) . . . yes C4 V C7 93.51(11) . . . yes C4 V C8 157.84(11) . . . yes C4 V C9 156.89(11) . . . yes C4 V C10 121.81(11) . . . yes C4 V C11 107.04(11) . . . yes C4 V C12 122.35(10) . . . yes C5 V C6 37.68(11) . . . yes C5 V C7 71.96(10) . . . yes C5 V C8 163.52(10) . . . yes C5 V C9 126.18(10) . . . yes C5 V C10 105.68(10) . . . yes C5 V C11 115.59(11) . . . yes C5 V C12 148.94(10) . . . yes C6 V C7 38.25(10) . . . yes C6 V C8 130.71(10) . . . yes C6 V C9 102.73(10) . . . yes C6 V C10 105.00(10) . . . yes C6 V C11 135.09(11) . . . yes C6 V C12 163.79(11) . . . yes C7 V C8 102.78(10) . . . yes C7 V C9 94.07(10) . . . yes C7 V C10 119.03(10) . . . yes C7 V C11 154.12(10) . . . yes C7 V C12 138.94(10) . . . yes C8 V C9 37.55(9) . . . yes C8 V C10 62.54(9) . . . yes C8 V C11 62.58(10) . . . yes C8 V C12 37.59(9) . . . yes C9 V C10 36.78(10) . . . yes C9 V C11 61.04(10) . . . yes C9 V C12 61.32(10) . . . yes C10 V C11 36.12(10) . . . yes C10 V C12 60.90(10) . . . yes C11 V C12 36.70(11) . . . yes Pt P1 C15 112.58(10) . . . yes Pt P1 C17 117.76(10) . . . yes Pt P1 C19 119.33(10) . . . yes C15 P1 C17 102.46(15) . . . yes C15 P1 C19 102.75(15) . . . yes C17 P1 C19 99.47(14) . . . yes Pt P2 C21 118.40(10) . . . yes Pt P2 C23 113.74(9) . . . yes Pt P2 C25 115.50(9) . . . yes C21 P2 C23 103.57(14) . . . yes C21 P2 C25 102.22(14) . . . yes C23 P2 C25 101.20(16) . . . yes Pt Si C8 116.68(8) . . . yes Pt Si C13 119.90(10) . . . yes Pt Si C14 109.64(10) . . . yes C8 Si C13 100.42(13) . . . yes C8 Si C14 101.22(13) . . . yes C13 Si C14 106.99(14) . . . yes Pt C1 V 134.01(12) . . . yes Pt C1 C2 117.85(17) . . . yes Pt C1 C7 117.49(18) . . . yes V C1 C2 70.69(14) . . . yes V C1 C7 70.12(15) . . . yes C2 C1 C7 124.6(2) . . . no V C2 C1 71.29(14) . . . yes V C2 C3 70.98(15) . . . yes C1 C2 C3 129.9(2) . . . no V C3 C2 70.79(15) . . . yes V C3 C4 71.20(17) . . . yes C2 C3 C4 129.2(3) . . . no V C4 C3 70.98(16) . . . yes V C4 C5 71.29(16) . . . yes C3 C4 C5 128.3(2) . . . no V C5 C4 71.05(17) . . . yes V C5 C6 70.54(17) . . . yes C4 C5 C6 127.5(3) . . . no V C6 C5 71.78(17) . . . yes V C6 C7 70.57(16) . . . yes C5 C6 C7 129.4(3) . . . no V C7 C1 71.91(15) . . . yes V C7 C6 71.19(16) . . . yes C1 C7 C6 131.0(3) . . . no V C8 Si 114.78(12) . . . yes V C8 C9 71.74(15) . . . yes V C8 C12 72.24(15) . . . yes Si C8 C9 127.6(2) . . . yes Si C8 C12 126.6(2) . . . yes C9 C8 C12 105.4(2) . . . no V C9 C8 70.71(15) . . . yes V C9 C10 73.33(16) . . . yes C8 C9 C10 109.6(2) . . . no V C10 C9 69.89(15) . . . yes V C10 C11 72.19(15) . . . yes C9 C10 C11 107.9(2) . . . no V C11 C10 71.69(15) . . . yes V C11 C12 70.22(15) . . . yes C10 C11 C12 107.7(2) . . . no V C12 C8 70.16(14) . . . yes V C12 C11 73.08(16) . . . yes C8 C12 C11 109.4(3) . . . no P1 C15 C16 113.0(3) . . . yes P1 C17 C18 113.6(2) . . . yes P1 C19 C20 117.5(2) . . . yes P2 C21 C22 113.8(2) . . . yes P2 C23 C24 111.2(2) . . . yes P2 C25 C26 115.8(2) . . . yes V C2 H21 126.7(17) . . . no C1 C2 H21 116.0(15) . . . no C3 C2 H21 112.7(15) . . . no V C3 H31 129.8(17) . . . no C2 C3 H31 113.0(16) . . . no C4 C3 H31 117.0(16) . . . no V C4 H41 128.1(19) . . . no C3 C4 H41 114.4(15) . . . no C5 C4 H41 116.6(15) . . . no V C5 H51 129.6(17) . . . no C4 C5 H51 115.9(18) . . . no C6 C5 H51 116.0(18) . . . no V C6 H61 131.4(17) . . . no C5 C6 H61 116.9(16) . . . no C7 C6 H61 113.3(16) . . . no V C7 H71 127.8(17) . . . no C1 C7 H71 116.2(16) . . . no C6 C7 H71 111.7(17) . . . no V C9 H91 118.7(17) . . . no C8 C9 H91 125.4(17) . . . no C10 C9 H91 124.8(17) . . . no V C10 H101 119(2) . . . no C9 C10 H101 128(2) . . . no C11 C10 H101 124(2) . . . no V C11 H111 122.2(17) . . . no C10 C11 H111 125.0(19) . . . no C12 C11 H111 127.3(19) . . . no V C12 H121 120.6(17) . . . no C8 C12 H121 126.3(18) . . . no C11 C12 H121 124.1(18) . . . no Si C13 H131 118.9(19) . . . no Si C13 H132 108(2) . . . no Si C13 H133 112.9(19) . . . no H131 C13 H132 106(3) . . . no H131 C13 H133 106(3) . . . no H132 C13 H133 103(3) . . . no Si C14 H141 113.1(19) . . . no Si C14 H142 114(2) . . . no Si C14 H143 113(2) . . . no H141 C14 H142 103(3) . . . no H141 C14 H143 106(3) . . . no H142 C14 H143 107(3) . . . no P1 C15 H151 106(2) . . . no P1 C15 H152 111.7(18) . . . no C16 C15 H151 112(2) . . . no C16 C15 H152 109.6(18) . . . no H151 C15 H152 105(3) . . . no C15 C16 H161 108(2) . . . no C15 C16 H162 107(2) . . . no C15 C16 H163 112(3) . . . no H161 C16 H162 107(3) . . . no H161 C16 H163 108(4) . . . no H162 C16 H163 115(4) . . . no P1 C17 H171 108.4(19) . . . no P1 C17 H172 108.3(19) . . . no C18 C17 H171 108.0(18) . . . no C18 C17 H172 111.8(19) . . . no H171 C17 H172 106(3) . . . no C17 C18 H181 111(2) . . . no C17 C18 H182 117(2) . . . no C17 C18 H183 116(2) . . . no H181 C18 H182 105(3) . . . no H181 C18 H183 108(3) . . . no H182 C18 H183 99(3) . . . no P1 C19 H191 103.3(18) . . . no P1 C19 H192 105(2) . . . no C20 C19 H191 113.2(19) . . . no C20 C19 H192 109(2) . . . no H191 C19 H192 107(3) . . . no C19 C20 H201 113(2) . . . no C19 C20 H202 111(2) . . . no C19 C20 H203 110(2) . . . no H201 C20 H202 106(3) . . . no H201 C20 H203 106(3) . . . no H202 C20 H203 110(3) . . . no P2 C21 H211 105.1(19) . . . no P2 C21 H212 108.2(18) . . . no C22 C21 H211 111.6(19) . . . no C22 C21 H212 110.1(19) . . . no H211 C21 H212 108(3) . . . no C21 C22 H221 112(3) . . . no C21 C22 H222 110(2) . . . no C21 C22 H223 109(3) . . . no H221 C22 H222 111(3) . . . no H221 C22 H223 108(4) . . . no H222 C22 H223 107(3) . . . no P2 C23 H231 110.4(19) . . . no P2 C23 H232 107.7(19) . . . no C24 C23 H231 109.2(19) . . . no C24 C23 H232 113.7(19) . . . no H231 C23 H232 104(3) . . . no C23 C24 H241 112(3) . . . no C23 C24 H242 111(2) . . . no C23 C24 H243 109(3) . . . no H241 C24 H242 108(3) . . . no H241 C24 H243 108(4) . . . no H242 C24 H243 108(3) . . . no P2 C25 H251 112.1(17) . . . no P2 C25 H252 106(2) . . . no C26 C25 H251 109.9(17) . . . no C26 C25 H252 110(2) . . . no H251 C25 H252 102(3) . . . no C25 C26 H261 111(2) . . . no C25 C26 H262 110.6(19) . . . no C25 C26 H263 113(2) . . . no H261 C26 H262 101(3) . . . no H261 C26 H263 110(3) . . . no H262 C26 H263 110(3) . . . no # End of Crystallographic Information File