Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Lutz Gade' 'Ralf A. Findeis' _publ_contact_author_name 'Prof Lutz Gade' _publ_contact_author_address ; (CNRS UMR 7513), Institut le Bel Universite Louis Pasteur Strasbourg 4 rue Blaise Pascal 67070 Strasbourg Cedex FRANCE ; _publ_contact_author_email 'GADE@CHIMIE.U-STRASBG.FR' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Didentate Phosphine Ligands with Alkenyl and Alkynyl Linker Units as Building Blocks for Dendrimer Fixation ; _publ_section_abstract ; Using dimethyl-2-methylmalonate as a starting material, the two diphosphines HC=C-CH2C(CH3)(CH2PPh2)2 (7) and H2C=CH-CH2C(CH3)(CH2PPh2)2 (13), containing alkynyl and alkenyl unit in the ligand backbone were prepared in multistep syntheses. These two ligands were employed in the synthesis of [{(CH3)3Si-C*C-CH2C(CH3)(CH2PPh2)2}PdCl2] (8) and [{(CH3)3Si-C *C-CH2C(CH3)(CH2PPh2)2}PtCl2] (9) as well as [{H2C=CH-CH2C(CH3)(CH2PPh2)2} PdI2] (14b), all of which were characterized by X-ray diffraction. Reaction of Si[(CH2)3SiMe2Cl]4 (= "G[0]-[SiMe2Cl]4") with four molar equivalents of the in situ lithiated alkynyl diphosphine 7 cleanly yielded the fourfold functionalized derivative G[0]-[C*C-CH2C(CH3)(CH2PPh2)2]4 (15) which was cleanly converted to the metallated derivative G[0]-[C**C-CH2C(CH3)(CH2PPh2)2 PdCl2]4 (16). Since the fixation of the alkenyl-functionalized diphosphine ligand 13 to the Si-H-silane Si[(CH2)3SiMe2H]4 (= "G[0]-[SiMe2H]4") by Pt-catalyzed hydrosilation proved to be unsuccessful due to the negative interference of the phosphine with Karsted's catalyst, the chloro-substituted precursor of 13, H2C=CH-CH2C(CH3)(CH2Cl)2 (12) was used. Hydrosilation of G[0]-[SiMe2H]4 with four molar equivalents of 12 readily gave the functionalized dendrimer G[0]-[CH2CH2CH2C(CH3)(CH2Cl)2]4 (17) which was then reacted with eight equiv. of LiPPh2 to yield the phosphinated derivative G[0]-[CH2CH2CH2C(CH3)(CH2PPh2)2]4 (18) ; _publ_section_exptl_prep ; Crystals grown from dichloromethane/hexane at 293 K ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158-166. ; #==================================================================== #===== data_compound_14b _database_code_CSD 190881 #======================================================================== _audit_creation_date 26-04-02 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C31 H32 I2 P2 Pd' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C31 H32 I2 P2 Pd' _chemical_formula_weight 826.76 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 I ? -0.726 1.812 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Pd ? -1.177 1.007 International_Tables_Vol_IV_Table_2.3.1 #======================================================================== #====== # 6. CRYSTAL DATA _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' 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.9006(2) _cell_length_b 18.1476(4) _cell_length_c 14.2538(4) _cell_angle_alpha 90 _cell_angle_beta 112.264(5) _cell_angle_gamma 90 _cell_volume 3088.3(1) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.78 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 2.722 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.9124 _exptl_absorpt_correction_T_max 1.0000 #======================================================================== #====== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 11822 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 2.0 deg 1 scans of 60 sec per frame. Data collection was divided into 1 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.30 Omega = 0.00 Kappa = 0.00 90 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11822 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7239 _reflns_number_gt 4346 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #======================================================================== #====== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4346 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.063 _refine_ls_R_factor_gt 0.029 _refine_ls_wR_factor_all 0.585 _refine_ls_wR_factor_ref 0.031 _refine_ls_goodness_of_fit_all 20.017 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_shift/su_max 0.010 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.735 _refine_diff_density_min -0.214 #======================================================================== #====== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol PD 0.23071(2) 0.30635(1) 0.34471(2) 0.0227(1) Uani ? ? Pd I1 0.31326(2) 0.18985(1) 0.46138(2) 0.0346(1) Uani ? ? I I2 0.42654(2) 0.32762(1) 0.32884(2) 0.0373(1) Uani ? ? I P1 0.16639(8) 0.40891(5) 0.24849(7) 0.0257(5) Uani ? ? P C1 0.2278(3) 0.4934(2) 0.3154(3) 0.028(2) Uani ? ? C C2 0.1979(3) 0.5618(2) 0.2694(3) 0.033(2) Uani ? ? C C3 0.2390(3) 0.6260(2) 0.3235(3) 0.039(2) Uani ? ? C C4 0.3098(4) 0.6219(2) 0.4234(3) 0.044(2) Uani ? ? C C5 0.3411(4) 0.5544(2) 0.4689(3) 0.042(2) Uani ? ? C C6 0.3006(3) 0.4906(2) 0.4163(3) 0.035(2) Uani ? ? C C7 0.1940(3) 0.4044(2) 0.1327(3) 0.026(2) Uani ? ? C C8 0.1451(3) 0.3472(2) 0.0658(3) 0.037(2) Uani ? ? C C9 0.1690(4) 0.3377(2) -0.0206(3) 0.041(2) Uani ? ? C C10 0.2402(3) 0.3847(2) -0.0406(3) 0.042(2) Uani ? ? C C11 0.2884(3) 0.4425(2) 0.0244(3) 0.047(2) Uani ? ? C C12 0.2662(3) 0.4517(2) 0.1111(3) 0.038(2) Uani ? ? C C13 0.0154(3) 0.4278(2) 0.1973(3) 0.029(2) Uani ? ? C C14 -0.0525(3) 0.4130(2) 0.2644(3) 0.029(2) Uani ? ? C C15 -0.1726(3) 0.4409(2) 0.2010(3) 0.039(2) Uani ? ? C C16 -0.2561(4) 0.4225(3) 0.2459(4) 0.058(3) Uani ? ? C C17 -0.3389(4) 0.3752(3) 0.2061(4) 0.080(3) Uani ? ? C C18 -0.0048(3) 0.4540(2) 0.3653(3) 0.040(2) Uani ? ? C C19 -0.0588(3) 0.3298(2) 0.2787(3) 0.029(2) Uani ? ? C P2 0.06580(8) 0.28020(5) 0.35871(7) 0.0253(5) Uani ? ? P C20 0.0221(3) 0.1867(2) 0.3175(3) 0.027(2) Uani ? ? C C21 0.0086(3) 0.1682(2) 0.2189(3) 0.039(2) Uani ? ? C C22 -0.0194(3) 0.0977(2) 0.1822(3) 0.043(2) Uani ? ? C C23 -0.0375(3) 0.0449(2) 0.2428(3) 0.045(2) Uani ? ? C C24 -0.0262(3) 0.0621(2) 0.3403(3) 0.042(2) Uani ? ? C C25 0.0039(3) 0.1321(2) 0.3781(3) 0.036(2) Uani ? ? C C26 0.0684(3) 0.2917(2) 0.4864(3) 0.028(2) Uani ? ? C C27 -0.0262(3) 0.2756(2) 0.5073(3) 0.040(2) Uani ? ? C C28 -0.0253(4) 0.2877(3) 0.6042(3) 0.057(2) Uani ? ? C C29 0.0676(4) 0.3171(3) 0.6784(3) 0.058(3) Uani ? ? C C30 0.1618(4) 0.3336(2) 0.6587(3) 0.049(3) Uani ? ? C C31 0.1621(3) 0.3207(2) 0.5630(3) 0.038(2) Uani ? ? C H1 0.1489 0.5646 0.2002 0.0433 Uiso calc C2 H H2 0.2181 0.6726 0.2916 0.0503 Uiso calc C3 H H3 0.3373 0.6657 0.4611 0.0583 Uiso calc C4 H H4 0.3914 0.5520 0.5377 0.0621 Uiso calc C5 H H5 0.3224 0.4443 0.4490 0.0482 Uiso calc C6 H H6 0.0949 0.3145 0.0792 0.0472 Uiso calc C8 H H7 0.1356 0.2982 -0.0658 0.0555 Uiso calc C9 H H8 0.2568 0.3778 -0.0995 0.0559 Uiso calc C10 H H9 0.3367 0.4759 0.0095 0.0603 Uiso calc C11 H H10 0.3009 0.4908 0.1564 0.0499 Uiso calc C12 H H11 -0.0170 0.3987 0.1380 0.0396 Uiso calc C13 H H12 0.0063 0.4785 0.1795 0.0396 Uiso calc C13 H H13 -0.1962 0.4193 0.1355 0.0497 Uiso calc C15 H H14 -0.1701 0.4929 0.1952 0.0497 Uiso calc C15 H H15 -0.2495 0.4463 0.3073 0.0779 Uiso calc C16 H H16 -0.3896 0.3659 0.2388 0.1055 Uiso calc C17 H H17 -0.3479 0.3504 0.1448 0.1055 Uiso calc C17 H H18 -0.0024 0.5053 0.3530 0.0514 Uiso calc C18 H H19 -0.0511 0.4456 0.4026 0.0514 Uiso calc C18 H H20 0.0688 0.4367 0.4032 0.0514 Uiso calc C18 H H21 -0.0824 0.3081 0.2132 0.0378 Uiso calc C19 H H22 -0.1143 0.3218 0.3063 0.0378 Uiso calc C19 H H23 0.0190 0.2050 0.1759 0.0505 Uiso calc C21 H H24 -0.0262 0.0859 0.1152 0.0554 Uiso calc C22 H H25 -0.0579 -0.0037 0.2176 0.0601 Uiso calc C23 H H26 -0.0394 0.0253 0.3819 0.0563 Uiso calc C24 H H27 0.0124 0.1431 0.4458 0.0480 Uiso calc C25 H H28 -0.0914 0.2563 0.4555 0.0492 Uiso calc C27 H H29 -0.0892 0.2756 0.6189 0.0685 Uiso calc C28 H H30 0.0671 0.3262 0.7439 0.0750 Uiso calc C29 H H31 0.2262 0.3537 0.7105 0.0684 Uiso calc C30 H H32 0.2271 0.3318 0.5496 0.0489 Uiso calc C31 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PD 0.0229(1) 0.0251(1) 0.0203(1) 0.0008(1) 0.0070(1) -0.0004(1) Pd I1 0.0346(1) 0.0369(1) 0.0323(1) 0.0089(1) 0.0069(1) 0.0086(1) I I2 0.0263(1) 0.0417(1) 0.0472(1) -0.0016(1) 0.0151(1) -0.0004(1) I P1 0.0290(5) 0.0269(5) 0.0219(5) -0.0017(4) 0.0090(4) 0.0015(4) P C1 0.032(2) 0.027(2) 0.026(2) -0.000(2) 0.013(1) -0.001(2) C C2 0.040(2) 0.031(2) 0.030(2) 0.003(2) 0.014(2) 0.003(2) C C3 0.052(2) 0.026(2) 0.044(2) 0.001(2) 0.026(2) 0.002(2) C C4 0.062(3) 0.035(2) 0.040(2) -0.010(2) 0.022(2) -0.011(2) C C5 0.065(3) 0.034(2) 0.034(2) -0.010(2) 0.007(2) -0.005(2) C C6 0.042(2) 0.032(2) 0.032(2) -0.000(2) 0.007(2) 0.001(2) C C7 0.034(2) 0.029(2) 0.018(2) -0.003(2) 0.010(1) -0.001(2) C C8 0.041(2) 0.039(2) 0.030(2) -0.010(2) 0.016(2) 0.003(2) C C9 0.055(3) 0.043(2) 0.028(2) -0.011(2) 0.014(2) -0.008(2) C C10 0.053(2) 0.056(2) 0.026(2) -0.002(2) 0.021(2) 0.000(2) C C11 0.051(2) 0.061(3) 0.033(2) -0.018(2) 0.022(2) 0.003(2) C C12 0.044(2) 0.042(2) 0.031(2) -0.013(2) 0.015(2) -0.007(2) C C13 0.029(2) 0.028(2) 0.030(2) 0.002(2) 0.007(2) -0.002(2) C C14 0.029(2) 0.027(2) 0.030(2) 0.005(2) 0.013(1) 0.004(2) C C15 0.037(2) 0.034(2) 0.046(2) 0.008(2) 0.018(2) 0.005(2) C C16 0.044(3) 0.057(3) 0.079(3) 0.015(2) 0.024(2) 0.002(3) C C17 0.064(3) 0.057(3) 0.139(4) -0.003(3) 0.056(2) -0.011(3) C C18 0.045(2) 0.034(2) 0.042(2) 0.000(2) 0.019(2) 0.003(2) C C19 0.028(2) 0.037(2) 0.024(2) -0.001(2) 0.011(1) -0.003(2) C P2 0.0275(5) 0.0257(4) 0.0229(5) 0.0012(5) 0.0102(4) 0.0018(4) P C20 0.025(2) 0.027(2) 0.030(2) 0.003(2) 0.012(1) 0.000(2) C C21 0.041(2) 0.036(2) 0.039(2) -0.002(2) 0.016(2) -0.003(2) C C22 0.046(2) 0.043(2) 0.041(2) -0.010(2) 0.019(2) -0.015(2) C C23 0.041(2) 0.037(2) 0.061(3) -0.009(2) 0.020(2) -0.013(2) C C24 0.046(2) 0.028(2) 0.056(3) -0.003(2) 0.020(2) 0.004(2) C C25 0.036(2) 0.034(2) 0.039(2) -0.000(2) 0.012(2) 0.001(2) C C26 0.036(2) 0.025(2) 0.024(2) 0.008(2) 0.014(1) 0.005(2) C C27 0.040(2) 0.043(2) 0.037(2) 0.005(2) 0.023(2) 0.005(2) C C28 0.059(2) 0.067(3) 0.046(2) 0.012(2) 0.035(2) 0.011(2) C C29 0.086(3) 0.069(3) 0.032(2) 0.008(3) 0.038(2) 0.002(2) C C30 0.068(3) 0.059(3) 0.029(2) -0.003(2) 0.015(2) -0.004(2) C C31 0.042(2) 0.043(2) 0.030(2) -0.001(2) 0.016(2) -0.001(2) C # 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 PD I1 2.6508(4) . . ? PD I2 2.6487(5) . . ? PD P1 2.274(1) . . ? PD P2 2.261(1) . . ? P1 C1 1.822(4) . . ? P1 C7 1.818(4) . . ? P1 C13 1.835(5) . . ? C1 C2 1.387(6) . . ? C1 C6 1.389(6) . . ? C2 C3 1.388(6) . . ? C3 C4 1.372(6) . . ? C4 C5 1.372(7) . . ? C5 C6 1.371(6) . . ? C7 C8 1.388(6) . . ? C7 C12 1.384(6) . . ? C8 C9 1.390(6) . . ? C9 C10 1.361(6) . . ? C10 C11 1.382(6) . . ? C11 C12 1.379(6) . . ? C13 C14 1.545(6) . . ? C14 C15 1.553(6) . . ? C14 C18 1.526(6) . . ? C14 C19 1.531(5) . . ? C15 C16 1.486(7) . . ? C16 C17 1.319(8) . . ? C19 P2 1.817(5) . . ? P2 C20 1.814(4) . . ? P2 C26 1.819(4) . . ? C20 C21 1.391(6) . . ? C20 C25 1.392(6) . . ? C21 C22 1.377(6) . . ? C22 C23 1.369(6) . . ? C23 C24 1.377(6) . . ? C24 C25 1.378(6) . . ? C26 C27 1.393(6) . . ? C26 C31 1.389(6) . . ? C27 C28 1.395(7) . . ? C28 C29 1.371(8) . . ? C29 C30 1.379(8) . . ? C30 C31 1.385(6) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 I1 PD I2 90.02(1) . . . ? I1 PD P1 177.63(3) . . . ? I1 PD P2 86.85(3) . . . ? I2 PD P1 88.34(3) . . . ? I2 PD P2 176.26(3) . . . ? P1 PD P2 94.85(4) . . . ? C1 P1 C7 108.5(2) . . . ? C1 P1 C13 103.7(2) . . . ? C7 P1 C13 101.1(2) . . . ? P1 C1 C2 121.1(3) . . . ? P1 C1 C6 120.0(3) . . . ? C2 C1 C6 118.7(4) . . . ? C1 C2 C3 120.6(4) . . . ? C2 C3 C4 119.7(4) . . . ? C3 C4 C5 120.0(4) . . . ? C4 C5 C6 120.8(5) . . . ? C1 C6 C5 120.2(4) . . . ? P1 C7 C8 117.6(3) . . . ? P1 C7 C12 123.6(3) . . . ? C8 C7 C12 118.7(4) . . . ? C7 C8 C9 120.4(4) . . . ? C8 C9 C10 120.1(4) . . . ? C9 C10 C11 120.2(4) . . . ? C10 C11 C12 120.0(5) . . . ? C7 C12 C11 120.6(4) . . . ? P1 C13 C14 119.1(3) . . . ? C13 C14 C15 104.9(4) . . . ? C13 C14 C18 112.2(4) . . . ? C13 C14 C19 108.9(4) . . . ? C15 C14 C18 110.3(4) . . . ? C15 C14 C19 107.9(4) . . . ? C18 C14 C19 112.3(4) . . . ? C14 C15 C16 113.7(4) . . . ? C15 C16 C17 124.2(6) . . . ? C14 C19 P2 119.6(3) . . . ? C19 P2 C20 99.6(2) . . . ? C19 P2 C26 104.3(2) . . . ? C20 P2 C26 108.5(2) . . . ? P2 C20 C21 117.2(3) . . . ? P2 C20 C25 124.8(4) . . . ? C21 C20 C25 118.0(4) . . . ? C20 C21 C22 121.5(4) . . . ? C21 C22 C23 119.6(5) . . . ? C22 C23 C24 120.0(4) . . . ? C23 C24 C25 120.6(4) . . . ? C20 C25 C24 120.2(4) . . . ? P2 C26 C27 120.3(4) . . . ? P2 C26 C31 120.7(4) . . . ? C27 C26 C31 118.9(4) . . . ? C26 C27 C28 119.9(5) . . . ? C27 C28 C29 120.1(5) . . . ? C28 C29 C30 120.5(5) . . . ? C29 C30 C31 119.6(5) . . . ? C26 C31 C30 120.8(5) . . . ? #==================================================================== #===== data_compound8 _database_code_CSD 190882 #======================================================================== _audit_creation_date 26-04-02 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C36 H40 Cl8 P2 Pd Si' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H40 Cl8 P2 Pd Si' _chemical_formula_weight 952.78 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Pd ? -1.177 1.007 International_Tables_Vol_IV_Table_2.3.1 Si ? 0.072 0.071 International_Tables_Vol_IV_Table_2.3.1 #======================================================================== #====== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 16.6775(4) _cell_length_b 18.0163(5) _cell_length_c 14.0010(5) _cell_angle_alpha 90 _cell_angle_beta 92.175(5) _cell_angle_gamma 90 _cell_volume 4203.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.51 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 1.080 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.8106 _exptl_absorpt_correction_T_max 1.0000 #======================================================================== #====== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 16279 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.7 deg 1 scans of 50 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.30 Omega = 0.00 Kappa = 0.00 107 frames Set 2 Theta = -6.30 Kappa = 134.00 Phi = 0.00 14 frames Friedel pairs were averaged. Internal R = 0.05 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16279 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9937 _reflns_number_gt 5302 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #======================================================================== #====== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5302 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.107 _refine_ls_R_factor_gt 0.049 _refine_ls_wR_factor_all 1.020 _refine_ls_wR_factor_ref 0.072 _refine_ls_goodness_of_fit_all 22.664 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_shift/su_max 0.003 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 1.094 _refine_diff_density_min -0.183 #======================================================================== #====== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol PD 0.41344(3) 0.19178(2) 0.29381(3) 0.0208(2) 1.000 Uani ? ? Pd CL1 0.39267(9) 0.29172(8) 0.39776(9) 0.0367(8) 1.000 Uani ? ? Cl CL2 0.53945(9) 0.16503(8) 0.36721(9) 0.0342(7) 1.000 Uani ? ? Cl P1 0.29397(9) 0.22372(8) 0.23007(9) 0.0240(7) 1.000 Uani ? ? P C1 0.2112(3) 0.2047(3) 0.3091(4) 0.031(3) 1.000 Uani ? ? C C2 0.2277(4) 0.1764(3) 0.4007(4) 0.040(3) 1.000 Uani ? ? C C3 0.1669(4) 0.1585(4) 0.4581(4) 0.054(4) 1.000 Uani ? ? C C4 0.0892(4) 0.1649(5) 0.4252(5) 0.064(4) 1.000 Uani ? ? C C5 0.0710(4) 0.1943(5) 0.3358(5) 0.057(5) 1.000 Uani ? ? C C6 0.1323(4) 0.2139(4) 0.2775(4) 0.044(4) 1.000 Uani ? ? C C7 0.2912(3) 0.3219(3) 0.1986(4) 0.028(3) 1.000 Uani ? ? C C8 0.2313(4) 0.3700(3) 0.2317(4) 0.038(3) 1.000 Uani ? ? C C9 0.2312(4) 0.4433(3) 0.2008(5) 0.053(4) 1.000 Uani ? ? C C10 0.2889(5) 0.4684(3) 0.1419(5) 0.053(4) 1.000 Uani ? ? C C11 0.3480(4) 0.4218(4) 0.1098(4) 0.049(4) 1.000 Uani ? ? C C12 0.3490(4) 0.3476(3) 0.1394(4) 0.038(3) 1.000 Uani ? ? C P2 0.43199(9) 0.09383(8) 0.19696(9) 0.0219(7) 1.000 Uani ? ? P C13 0.4330(3) 0.0065(3) 0.2614(4) 0.027(3) 1.000 Uani ? ? C C14 0.4183(4) 0.0050(3) 0.3591(4) 0.035(3) 1.000 Uani ? ? C C15 0.4184(4) -0.0617(3) 0.4088(4) 0.045(4) 1.000 Uani ? ? C C16 0.4336(4) -0.1278(3) 0.3621(5) 0.049(4) 1.000 Uani ? ? C C17 0.4473(4) -0.1263(3) 0.2639(5) 0.041(3) 1.000 Uani ? ? C C18 0.4472(4) -0.0599(3) 0.2141(4) 0.036(3) 1.000 Uani ? ? C C19 0.5277(3) 0.1018(3) 0.1410(3) 0.023(3) 1.000 Uani ? ? C C20 0.5370(3) 0.1556(3) 0.0714(4) 0.029(3) 1.000 Uani ? ? C C21 0.6090(4) 0.1660(3) 0.0294(4) 0.038(3) 1.000 Uani ? ? C C22 0.6742(4) 0.1226(4) 0.0565(4) 0.050(4) 1.000 Uani ? ? C C23 0.6667(4) 0.0690(4) 0.1266(4) 0.042(3) 1.000 Uani ? ? C C24 0.5934(4) 0.0577(3) 0.1694(4) 0.034(3) 1.000 Uani ? ? C C25 0.2632(3) 0.1827(3) 0.1164(3) 0.024(3) 1.000 Uani ? ? C C26 0.2741(4) 0.0979(3) 0.1038(3) 0.028(3) 1.000 Uani ? ? C C27 0.3631(3) 0.0795(3) 0.0931(3) 0.025(3) 1.000 Uani ? ? C C28 0.2387(4) 0.0524(3) 0.1831(4) 0.035(3) 1.000 Uani ? ? C C29 0.2295(4) 0.0784(3) 0.0066(4) 0.035(3) 1.000 Uani ? ? C C30 0.1421(4) 0.0976(4) 0.0079(4) 0.043(3) 1.000 Uani ? ? C C31 0.0723(4) 0.1137(4) 0.0154(5) 0.045(4) 1.000 Uani ? ? C SI -0.0334(1) 0.1284(1) 0.0336(1) 0.051(1) 1.000 Uani ? ? Si C32 -0.0654(5) 0.0637(5) 0.1272(6) 0.076(5) 1.000 Uani ? ? C C33 -0.0495(5) 0.2244(4) 0.0749(6) 0.071(5) 1.000 Uani ? ? C C34 -0.0882(5) 0.1113(6) -0.0801(6) 0.082(6) 1.000 Uani ? ? C C35 -0.2608(5) 0.3049(5) -0.1656(7) 0.084(6) 1.000 Uani ? ? C CL3 -0.1761(2) 0.3449(2) -0.2118(2) 0.110(2) 1.000 Uani ? ? Cl CL4 -0.2715(2) 0.2130(2) -0.2003(3) 0.131(2) 1.000 Uani ? ? Cl CL5 -0.2525(2) 0.3077(2) -0.0405(2) 0.104(2) 1.000 Uani ? ? Cl C36 0.895(1) 0.042(1) 0.614(1) 0.08(1) 0.500 Uani ? ? C CL6 0.9024(3) 0.0445(3) 0.4910(3) 0.080(3) 0.500 Uani ? ? Cl CL7 0.9833(5) 0.0664(4) 0.6684(3) 0.130(5) 0.500 Uani ? ? Cl CL8 0.8206(4) 0.0896(4) 0.6546(4) 0.179(4) 0.500 Uani ? ? Cl H1 0.2817 0.1697 0.4229 0.0527 1.000 Uiso calc C2 H H2 0.1784 0.1414 0.5213 0.0720 1.000 Uiso calc C3 H H3 0.0471 0.1490 0.4642 0.0836 1.000 Uiso calc C4 H H4 0.0166 0.2010 0.3147 0.0813 1.000 Uiso calc C5 H H5 0.1203 0.2336 0.2156 0.0604 1.000 Uiso calc C6 H H6 0.1922 0.3527 0.2739 0.0494 1.000 Uiso calc C8 H H7 0.1906 0.4763 0.2208 0.0717 1.000 Uiso calc C9 H H8 0.2883 0.5190 0.1226 0.0792 1.000 Uiso calc C10 H H9 0.3874 0.4399 0.0683 0.0648 1.000 Uiso calc C11 H H10 0.3896 0.3150 0.1187 0.0504 1.000 Uiso calc C12 H H11 0.4081 0.0500 0.3918 0.0471 1.000 Uiso calc C14 H H12 0.4081 -0.0621 0.4751 0.0619 1.000 Uiso calc C15 H H13 0.4348 -0.1734 0.3961 0.0671 1.000 Uiso calc C16 H H14 0.4567 -0.1715 0.2312 0.0571 1.000 Uiso calc C17 H H15 0.4568 -0.0596 0.1476 0.0470 1.000 Uiso calc C18 H H16 0.4925 0.1859 0.0524 0.0383 1.000 Uiso calc C20 H H17 0.6141 0.2030 -0.0183 0.0499 1.000 Uiso calc C21 H H18 0.7242 0.1295 0.0272 0.0657 1.000 Uiso calc C22 H H19 0.7119 0.0397 0.1458 0.0561 1.000 Uiso calc C23 H H20 0.5882 0.0206 0.2170 0.0447 1.000 Uiso calc C24 H H21 0.2930 0.2064 0.0686 0.0321 1.000 Uiso calc C25 H H22 0.2077 0.1932 0.1059 0.0321 1.000 Uiso calc C25 H H23 0.3663 0.0286 0.0759 0.0339 1.000 Uiso calc C27 H H24 0.3818 0.1093 0.0426 0.0339 1.000 Uiso calc C27 H H25 0.2348 0.0267 -0.0049 0.0455 1.000 Uiso calc C29 H H26 0.2534 0.1054 -0.0432 0.0455 1.000 Uiso calc C29 H H27 -0.1208 0.0708 0.1376 0.1001 1.000 Uiso calc C32 H H28 -0.0566 0.0141 0.1073 0.1001 1.000 Uiso calc C32 H H29 -0.0352 0.0731 0.1849 0.1001 1.000 Uiso calc C32 H H30 -0.1049 0.2320 0.0844 0.0977 1.000 Uiso calc C33 H H31 -0.0199 0.2323 0.1333 0.0977 1.000 Uiso calc C33 H H32 -0.0318 0.2582 0.0281 0.0977 1.000 Uiso calc C33 H H33 -0.1440 0.1187 -0.0722 0.1136 1.000 Uiso calc C34 H H34 -0.0699 0.1446 -0.1271 0.1136 1.000 Uiso calc C34 H H35 -0.0792 0.0616 -0.1000 0.1136 1.000 Uiso calc C34 H H36 0.1837 0.0648 0.1883 0.0457 1.000 Uiso calc C28 H H37 0.2435 0.0011 0.1687 0.0457 1.000 Uiso calc C28 H H38 0.2668 0.0629 0.2418 0.0457 1.000 Uiso calc C28 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PD 0.0228(2) 0.0230(2) 0.0171(2) -0.0013(2) -0.0028(2) -0.0005(2) Pd CL1 0.0410(9) 0.0414(8) 0.0290(6) 0.0016(7) -0.0057(6) -0.0152(6) Cl CL2 0.0310(8) 0.0404(7) 0.0319(7) 0.0016(7) -0.0107(6) -0.0012(6) Cl P1 0.0232(8) 0.0281(7) 0.0212(6) 0.0004(7) -0.0015(6) -0.0024(6) P C1 0.026(3) 0.040(3) 0.027(3) -0.001(3) 0.003(2) -0.009(2) C C2 0.046(4) 0.046(3) 0.031(3) -0.004(3) 0.010(3) -0.001(3) C C3 0.059(5) 0.070(4) 0.038(3) -0.011(4) 0.018(3) -0.002(3) C C4 0.062(5) 0.082(5) 0.051(4) -0.013(4) 0.035(3) -0.010(4) C C5 0.030(4) 0.090(6) 0.068(4) -0.006(4) 0.013(3) -0.021(4) C C6 0.029(4) 0.065(4) 0.046(3) 0.003(3) 0.005(3) -0.006(3) C C7 0.032(3) 0.028(3) 0.025(3) 0.002(3) -0.011(2) -0.001(2) C C8 0.043(4) 0.033(3) 0.037(3) 0.009(3) -0.007(3) -0.009(3) C C9 0.070(5) 0.036(3) 0.057(4) 0.023(4) -0.024(3) -0.014(3) C C10 0.093(6) 0.025(3) 0.062(4) -0.000(4) -0.027(4) 0.001(3) C C11 0.064(5) 0.039(3) 0.046(3) -0.007(4) -0.006(3) 0.007(3) C C12 0.047(4) 0.031(3) 0.039(3) 0.004(3) 0.006(3) 0.001(3) C P2 0.0244(8) 0.0225(6) 0.0192(6) 0.0016(6) -0.0010(6) 0.0013(5) P C13 0.030(3) 0.024(3) 0.025(2) 0.002(3) 0.003(2) 0.002(2) C C14 0.047(4) 0.032(3) 0.029(3) 0.005(3) 0.000(3) 0.006(3) C C15 0.071(5) 0.035(3) 0.037(3) -0.001(4) 0.009(3) 0.010(3) C C16 0.065(5) 0.030(3) 0.060(4) -0.002(4) 0.004(4) 0.019(3) C C17 0.049(4) 0.024(3) 0.059(4) 0.002(3) 0.004(3) -0.002(3) C C18 0.045(4) 0.028(3) 0.036(3) 0.003(3) 0.002(3) 0.001(3) C C19 0.022(3) 0.025(2) 0.022(2) 0.002(3) -0.001(2) -0.001(2) C C20 0.022(3) 0.030(3) 0.036(3) 0.000(3) -0.001(2) 0.001(2) C C21 0.039(4) 0.039(3) 0.037(3) 0.000(3) 0.006(3) 0.009(3) C C22 0.038(4) 0.063(4) 0.052(4) 0.003(4) 0.016(3) 0.009(3) C C23 0.031(3) 0.050(4) 0.049(3) 0.016(3) 0.010(3) 0.010(3) C C24 0.034(3) 0.038(3) 0.031(3) 0.008(3) 0.005(2) 0.005(3) C C25 0.022(3) 0.032(3) 0.020(2) -0.000(3) -0.001(2) -0.004(2) C C26 0.032(3) 0.034(3) 0.022(2) -0.008(3) -0.007(2) -0.005(2) C C27 0.036(3) 0.023(2) 0.018(2) -0.005(3) -0.003(2) 0.000(2) C C28 0.032(3) 0.034(3) 0.039(3) -0.009(3) 0.005(3) -0.003(3) C C29 0.035(3) 0.035(3) 0.034(3) -0.009(3) -0.005(3) -0.010(3) C C30 0.045(4) 0.046(3) 0.039(3) -0.006(3) -0.009(3) -0.012(3) C C31 0.029(4) 0.057(4) 0.057(4) -0.000(3) -0.011(3) -0.014(3) C SI 0.033(1) 0.056(1) 0.072(1) 0.002(1) -0.006(1) -0.013(1) Si C32 0.077(6) 0.065(5) 0.089(5) 0.002(5) 0.008(5) -0.014(4) C C33 0.061(5) 0.053(4) 0.112(6) 0.011(5) 0.010(5) -0.007(5) C C34 0.053(5) 0.128(8) 0.080(5) 0.012(6) -0.015(4) -0.011(6) C C35 0.066(6) 0.082(6) 0.109(6) -0.008(5) 0.033(5) 0.019(5) C CL3 0.078(2) 0.103(2) 0.166(2) 0.003(2) 0.044(2) 0.045(2) Cl CL4 0.118(2) 0.103(2) 0.185(3) -0.008(2) 0.005(2) -0.015(2) Cl CL5 0.070(2) 0.133(2) 0.122(2) -0.024(2) -0.011(1) 0.038(2) Cl C36 0.08(1) 0.07(1) 0.09(1) -0.01(1) 0.01(1) 0.01(1) C CL6 0.070(3) 0.092(3) 0.080(2) -0.019(3) -0.004(2) -0.011(2) Cl CL7 0.200(6) 0.179(6) 0.062(3) 0.056(5) -0.014(3) 0.001(4) Cl CL8 0.190(5) 0.198(5) 0.153(3) 0.074(5) 0.108(3) 0.109(3) Cl # 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 PD CL1 2.349(1) . . ? PD CL2 2.354(2) . . ? PD P1 2.228(2) . . ? PD P2 2.254(1) . . ? P1 C1 1.834(6) . . ? P1 C7 1.822(6) . . ? P1 C25 1.811(5) . . ? C1 C2 1.398(8) . . ? C1 C6 1.382(9) . . ? C2 C3 1.356(9) . . ? C3 C4 1.36(1) . . ? C4 C5 1.38(1) . . ? C5 C6 1.38(1) . . ? C7 C8 1.414(8) . . ? C7 C12 1.376(8) . . ? C8 C9 1.390(9) . . ? C9 C10 1.37(1) . . ? C10 C11 1.38(1) . . ? C11 C12 1.400(9) . . ? P2 C13 1.813(5) . . ? P2 C19 1.810(6) . . ? P2 C27 1.837(5) . . ? C13 C14 1.400(8) . . ? C13 C18 1.392(8) . . ? C14 C15 1.389(8) . . ? C15 C16 1.386(9) . . ? C16 C17 1.402(9) . . ? C17 C18 1.386(8) . . ? C19 C20 1.389(8) . . ? C19 C24 1.398(8) . . ? C20 C21 1.371(8) . . ? C21 C22 1.381(9) . . ? C22 C23 1.386(9) . . ? C23 C24 1.396(8) . . ? C25 C26 1.549(8) . . ? C26 C27 1.534(8) . . ? C26 C28 1.517(8) . . ? C26 C29 1.565(8) . . ? C29 C30 1.50(1) . . ? C30 C31 1.207(9) . . ? C31 SI 1.810(8) . . ? SI C32 1.846(9) . . ? SI C33 1.847(9) . . ? SI C34 1.832(9) . . ? C35 CL3 1.733(9) . . ? C35 CL4 1.73(1) . . ? C35 CL5 1.75(1) . . ? C36 CL6 1.73(2) . . ? C36 CL7 1.69(2) . . ? C36 CL8 1.63(2) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag CL1 PD CL2 92.10(5) . . . ? CL1 PD P1 84.24(5) . . . ? CL1 PD P2 178.47(6) . . . ? CL2 PD P1 176.30(6) . . . ? CL2 PD P2 87.80(5) . . . ? P1 PD P2 95.87(5) . . . ? C1 P1 C7 108.3(3) . . . ? C1 P1 C25 105.0(3) . . . ? C7 P1 C25 100.4(3) . . . ? P1 C1 C2 119.7(5) . . . ? P1 C1 C6 120.9(5) . . . ? C2 C1 C6 119.3(6) . . . ? C1 C2 C3 120.3(7) . . . ? C2 C3 C4 120.2(7) . . . ? C3 C4 C5 120.8(7) . . . ? C4 C5 C6 119.4(7) . . . ? C1 C6 C5 119.9(7) . . . ? P1 C7 C8 121.9(5) . . . ? P1 C7 C12 117.4(5) . . . ? C8 C7 C12 120.7(5) . . . ? C7 C8 C9 118.3(6) . . . ? C8 C9 C10 120.6(7) . . . ? C9 C10 C11 121.5(6) . . . ? C10 C11 C12 118.9(7) . . . ? C7 C12 C11 120.0(6) . . . ? C13 P2 C19 107.0(3) . . . ? C13 P2 C27 105.4(2) . . . ? C19 P2 C27 101.8(2) . . . ? P2 C13 C14 120.3(4) . . . ? P2 C13 C18 120.5(4) . . . ? C14 C13 C18 119.2(5) . . . ? C13 C14 C15 120.7(5) . . . ? C14 C15 C16 120.2(6) . . . ? C15 C16 C17 119.1(5) . . . ? C16 C17 C18 120.9(5) . . . ? C13 C18 C17 120.0(5) . . . ? P2 C19 C20 118.8(4) . . . ? P2 C19 C24 121.8(4) . . . ? C20 C19 C24 119.3(5) . . . ? C19 C20 C21 121.2(6) . . . ? C20 C21 C22 120.0(6) . . . ? C21 C22 C23 119.8(6) . . . ? C22 C23 C24 120.7(6) . . . ? C19 C24 C23 119.0(5) . . . ? P1 C25 C26 118.2(4) . . . ? C25 C26 C27 110.0(5) . . . ? C25 C26 C28 113.5(5) . . . ? C25 C26 C29 105.5(5) . . . ? C27 C26 C28 111.1(5) . . . ? C27 C26 C29 107.2(4) . . . ? C28 C26 C29 109.2(5) . . . ? P2 C27 C26 118.1(4) . . . ? C26 C29 C30 111.5(5) . . . ? C29 C30 C31 175.7(7) . . . ? C30 C31 SI 173.8(7) . . . ? C31 SI C32 108.5(4) . . . ? C31 SI C33 109.6(4) . . . ? C31 SI C34 108.0(4) . . . ? C32 SI C33 108.6(4) . . . ? C32 SI C34 111.3(5) . . . ? C33 SI C34 110.8(5) . . . ? CL3 C35 CL4 111.6(5) . . . ? CL3 C35 CL5 109.1(6) . . . ? CL4 C35 CL5 108.2(5) . . . ? CL6 C36 CL7 110(1) . . . ? CL6 C36 CL8 114(1) . . . ? CL7 C36 CL8 111(1) . . . ? #======================================================================= data_compound9 _database_code_CSD 190883 #========================================================================== _audit_creation_date 26-04-02 # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C36 H42 Cl6 P2 Pt Si' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H42 Cl6 P2 Pt Si' _chemical_formula_weight 972.58 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Pt ? -2.352 8.388 International_Tables_Vol_IV_Table_2.3.1 Si ? 0.072 0.071 International_Tables_Vol_IV_Table_2.3.1 #=========================================================================== #=== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 16.4406(3) _cell_length_b 17.8845(5) _cell_length_c 13.8996(5) _cell_angle_alpha 90 _cell_angle_beta 90.946(5) _cell_angle_gamma 90 _cell_volume 4086.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.58 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 3.958 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.6705 _exptl_absorpt_correction_T_max 1.0000 #=========================================================================== #=== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 16896 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 0.7 deg 1 scans of 50 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.30 Omega = 0.00 Kappa = 0.00 259 frames Set 2 Theta = -6.30 Kappa = -169.00 Phi = 0.00 57 frames Friedel pairs were averaged. Internal R = 0.00 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16896 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9581 _reflns_number_gt 5880 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=========================================================================== #=== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5880 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.069 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_all 0.174 _refine_ls_wR_factor_ref 0.050 _refine_ls_goodness_of_fit_all 4.439 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.753 _refine_diff_density_min -0.227 #=========================================================================== #=== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol PT 0.40928(1) 0.19152(1) 0.79230(2) 0.0240(1) Uani ? ? Pt CL1 0.3900(1) 0.29228(8) 0.8981(1) 0.0399(8) Uani ? ? Cl CL2 0.53534(9) 0.16596(8) 0.8682(1) 0.0394(8) Uani ? ? Cl P1 0.28973(9) 0.22433(8) 0.7295(1) 0.0280(7) Uani ? ? P C1 0.2052(4) 0.2045(3) 0.8081(5) 0.038(3) Uani ? ? C C2 0.2195(4) 0.1743(4) 0.8996(5) 0.045(4) Uani ? ? C C3 0.1562(5) 0.1523(4) 0.9549(6) 0.061(5) Uani ? ? C C4 0.0772(5) 0.1585(5) 0.9219(6) 0.070(5) Uani ? ? C C5 0.0617(5) 0.1900(5) 0.8356(7) 0.062(5) Uani ? ? C C6 0.1248(4) 0.2136(4) 0.7749(6) 0.050(4) Uani ? ? C C7 0.2859(4) 0.3228(3) 0.6979(4) 0.034(3) Uani ? ? C C8 0.3465(4) 0.3497(3) 0.6379(5) 0.043(4) Uani ? ? C C9 0.3478(5) 0.4246(3) 0.6100(5) 0.052(4) Uani ? ? C C10 0.2883(5) 0.4718(3) 0.6412(6) 0.055(4) Uani ? ? C C11 0.2286(5) 0.4467(4) 0.7007(6) 0.057(4) Uani ? ? C C12 0.2264(4) 0.3726(3) 0.7305(5) 0.044(4) Uani ? ? C P2 0.43117(9) 0.09404(7) 0.6956(1) 0.0252(7) Uani ? ? P C13 0.4320(3) 0.0051(3) 0.7589(4) 0.029(3) Uani ? ? C C14 0.4134(4) 0.0021(3) 0.8562(5) 0.044(4) Uani ? ? C C15 0.4133(5) -0.0645(4) 0.9044(5) 0.052(4) Uani ? ? C C16 0.4309(5) -0.1309(4) 0.8551(6) 0.058(4) Uani ? ? C C17 0.4481(5) -0.1281(3) 0.7592(6) 0.048(4) Uani ? ? C C18 0.4486(4) -0.0607(3) 0.7103(5) 0.039(3) Uani ? ? C C19 0.5296(3) 0.1033(3) 0.6389(4) 0.026(3) Uani ? ? C C20 0.5392(4) 0.1593(3) 0.5705(4) 0.033(3) Uani ? ? C C21 0.6140(4) 0.1715(3) 0.5300(5) 0.039(3) Uani ? ? C C22 0.6799(4) 0.1280(4) 0.5563(5) 0.045(4) Uani ? ? C C23 0.6718(4) 0.0739(4) 0.6265(5) 0.046(4) Uani ? ? C C24 0.5967(4) 0.0599(3) 0.6661(5) 0.038(3) Uani ? ? C C25 0.2612(3) 0.1823(3) 0.6152(4) 0.027(3) Uani ? ? C C26 0.2721(3) 0.0972(3) 0.6028(4) 0.027(3) Uani ? ? C C27 0.3623(3) 0.0804(3) 0.5920(4) 0.026(3) Uani ? ? C C28 0.2358(4) 0.0515(3) 0.6861(5) 0.041(3) Uani ? ? C C29 0.2285(4) 0.0762(3) 0.5085(5) 0.037(3) Uani ? ? C C30 0.1412(4) 0.0953(3) 0.5091(5) 0.049(4) Uani ? ? C C31 0.0700(4) 0.1098(4) 0.5180(6) 0.053(4) Uani ? ? C SI -0.0390(1) 0.1294(1) 0.5333(2) 0.051(1) Uani ? ? Si C32 -0.0771(5) 0.0709(5) 0.6321(7) 0.074(5) Uani ? ? C C33 -0.0546(6) 0.2281(5) 0.5637(8) 0.087(6) Uani ? ? C C34 -0.0895(5) 0.1086(5) 0.4173(7) 0.070(5) Uani ? ? C C35 0.0893(8) -0.0446(7) 0.8527(8) 0.110(8) Uani ? ? C CL3 0.1356(3) -0.0629(2) 0.9614(3) 0.161(3) Uani ? ? Cl CL4 -0.0081(2) -0.0680(2) 0.8428(3) 0.162(3) Uani ? ? Cl C36 0.2832(7) -0.2645(7) 0.7128(8) 0.109(8) Uani ? ? C CL5 0.2288(3) -0.2081(3) 0.7870(4) 0.197(4) Uani ? ? Cl CL6 0.2240(3) -0.3085(2) 0.6260(5) 0.199(4) Uani ? ? Cl H1 0.2737 0.1691 0.9233 0.0607 Uiso calc C2 H H2 0.1668 0.1324 1.0172 0.0806 Uiso calc C3 H H3 0.0338 0.1407 0.9598 0.0935 Uiso calc C4 H H4 0.0068 0.1966 0.8149 0.0902 Uiso calc C5 H H5 0.1131 0.2348 0.7136 0.0687 Uiso calc C6 H H6 0.3874 0.3166 0.6159 0.0572 Uiso calc C8 H H7 0.3896 0.4427 0.5698 0.0702 Uiso calc C9 H H8 0.2884 0.5227 0.6213 0.0818 Uiso calc C10 H H9 0.1881 0.4805 0.7221 0.0779 Uiso calc C11 H H10 0.1851 0.3558 0.7723 0.0578 Uiso calc C12 H H11 0.4007 0.0469 0.8895 0.0591 Uiso calc C14 H H12 0.4014 -0.0658 0.9710 0.0715 Uiso calc C15 H H13 0.4308 -0.1775 0.8881 0.0774 Uiso calc C16 H H14 0.4599 -0.1731 0.7257 0.0706 Uiso calc C17 H H15 0.4602 -0.0595 0.6436 0.0512 Uiso calc C18 H H16 0.4939 0.1893 0.5516 0.0430 Uiso calc C20 H H17 0.6201 0.2100 0.4836 0.0514 Uiso calc C21 H H18 0.7308 0.1352 0.5263 0.0583 Uiso calc C22 H H19 0.7181 0.0463 0.6477 0.0606 Uiso calc C23 H H20 0.5908 0.0208 0.7117 0.0495 Uiso calc C24 H H21 0.2926 0.2059 0.5672 0.0358 Uiso calc C25 H H22 0.2052 0.1929 0.6041 0.0358 Uiso calc C25 H H23 0.3667 0.0295 0.5735 0.0338 Uiso calc C27 H H24 0.3815 0.1114 0.5417 0.0338 Uiso calc C27 H H25 0.1797 0.0629 0.6915 0.0533 Uiso calc C28 H H26 0.2422 -0.0004 0.6735 0.0533 Uiso calc C28 H H27 0.2634 0.0639 0.7446 0.0533 Uiso calc C28 H H28 0.2338 0.0238 0.4987 0.0487 Uiso calc C29 H H29 0.2534 0.1022 0.4571 0.0487 Uiso calc C29 H H30 -0.1333 0.0805 0.6407 0.0966 Uiso calc C32 H H31 -0.0696 0.0196 0.6167 0.0966 Uiso calc C32 H H32 -0.0479 0.0823 0.6898 0.0966 Uiso calc C32 H H33 -0.1110 0.2373 0.5713 0.1156 Uiso calc C33 H H34 -0.0263 0.2394 0.6220 0.1156 Uiso calc C33 H H35 -0.0345 0.2587 0.5135 0.1156 Uiso calc C33 H H36 -0.1461 0.1180 0.4220 0.0944 Uiso calc C34 H H37 -0.0673 0.1395 0.3686 0.0944 Uiso calc C34 H H38 -0.0810 0.0576 0.4014 0.0944 Uiso calc C34 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PT 0.0302(1) 0.02375(9) 0.0193(1) 0.00001(9) -0.00249(9) -0.0007(1) Pt CL1 0.0485(9) 0.0415(7) 0.0315(8) 0.0040(7) -0.0043(8) -0.0144(7) Cl CL2 0.0414(8) 0.0411(7) 0.0358(9) 0.0050(7) -0.0140(7) -0.0034(7) Cl P1 0.0309(8) 0.0310(7) 0.0230(8) 0.0021(6) 0.0002(7) -0.0039(7) P C1 0.037(3) 0.046(3) 0.032(4) -0.002(3) -0.001(3) -0.009(3) C C2 0.054(4) 0.058(4) 0.028(4) -0.001(3) 0.001(3) 0.002(3) C C3 0.069(5) 0.073(5) 0.044(4) -0.010(4) 0.023(4) 0.004(4) C C4 0.069(5) 0.095(5) 0.053(5) -0.002(5) 0.041(4) 0.004(5) C C5 0.033(4) 0.113(6) 0.063(5) -0.004(4) 0.020(4) -0.013(5) C C6 0.033(4) 0.078(4) 0.048(4) -0.002(3) 0.008(3) -0.010(4) C C7 0.043(3) 0.033(3) 0.028(3) 0.006(3) -0.014(3) -0.009(3) C C8 0.050(4) 0.032(3) 0.049(4) 0.001(3) -0.002(4) 0.005(3) C C9 0.074(5) 0.038(3) 0.050(4) -0.009(3) -0.014(4) 0.011(3) C C10 0.088(5) 0.026(3) 0.073(5) 0.006(3) -0.025(5) 0.003(3) C C11 0.077(5) 0.040(3) 0.062(5) 0.020(3) -0.031(4) -0.020(3) C C12 0.053(4) 0.041(3) 0.039(4) 0.004(3) -0.011(3) -0.019(3) C P2 0.0311(8) 0.0223(6) 0.0231(8) 0.0008(6) -0.0011(7) 0.0024(6) P C13 0.032(3) 0.029(3) 0.026(3) -0.000(2) -0.001(3) 0.007(3) C C14 0.060(4) 0.036(3) 0.040(4) 0.006(3) 0.004(4) -0.000(3) C C15 0.084(5) 0.039(3) 0.042(4) 0.007(3) 0.009(4) 0.016(3) C C16 0.076(5) 0.040(3) 0.063(5) -0.001(3) 0.007(4) 0.023(3) C C17 0.066(5) 0.023(3) 0.074(5) 0.007(3) 0.002(4) 0.006(3) C C18 0.050(4) 0.033(3) 0.035(4) -0.002(3) 0.003(3) 0.001(3) C C19 0.032(3) 0.027(3) 0.020(3) 0.003(2) -0.005(3) -0.000(2) C C20 0.038(3) 0.033(3) 0.028(3) 0.002(3) -0.007(3) -0.000(3) C C21 0.050(4) 0.039(3) 0.029(3) -0.000(3) 0.005(3) 0.005(3) C C22 0.041(4) 0.052(4) 0.042(4) 0.002(3) 0.013(3) 0.000(3) C C23 0.037(3) 0.054(4) 0.049(4) 0.018(3) 0.002(3) -0.003(3) C C24 0.039(3) 0.039(3) 0.036(3) 0.011(3) 0.008(3) 0.004(3) C C25 0.025(3) 0.037(3) 0.021(3) -0.001(2) 0.002(2) -0.001(3) C C26 0.035(3) 0.025(2) 0.024(3) -0.002(2) -0.002(3) -0.002(2) C C27 0.031(3) 0.026(2) 0.021(3) 0.000(2) -0.000(2) 0.000(2) C C28 0.045(4) 0.040(3) 0.039(4) -0.006(3) 0.006(3) 0.003(3) C C29 0.042(3) 0.037(3) 0.033(3) -0.005(3) -0.005(3) -0.009(3) C C30 0.049(4) 0.042(3) 0.058(4) -0.009(3) -0.015(4) -0.009(3) C C31 0.035(4) 0.053(4) 0.082(6) -0.003(3) -0.016(4) -0.007(4) C SI 0.036(1) 0.049(1) 0.077(2) -0.0002(9) -0.002(1) 0.003(1) Si C32 0.064(5) 0.071(5) 0.088(6) 0.002(4) -0.012(5) -0.002(5) C C33 0.081(6) 0.067(5) 0.120(8) 0.004(5) 0.031(6) -0.007(5) C C34 0.048(5) 0.089(5) 0.081(6) 0.003(4) 0.004(5) 0.008(5) C C35 0.14(1) 0.136(8) 0.069(7) -0.030(7) 0.013(7) 0.006(7) C CL3 0.165(3) 0.123(2) 0.204(4) -0.019(2) -0.060(3) -0.003(3) Cl CL4 0.118(2) 0.225(3) 0.160(3) 0.016(2) 0.011(2) 0.102(2) Cl C36 0.088(7) 0.147(9) 0.102(8) 0.001(7) 0.026(6) -0.010(8) C CL5 0.148(3) 0.244(4) 0.211(5) 0.084(3) 0.019(3) -0.031(4) Cl CL6 0.186(3) 0.126(3) 0.339(6) 0.039(2) -0.128(4) -0.047(3) Cl # 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 CL1 2.351(1) . . ? PT CL2 2.355(2) . . ? PT P1 2.216(2) . . ? PT P2 2.234(1) . . ? P1 C1 1.817(7) . . ? P1 C7 1.817(6) . . ? P1 C25 1.813(6) . . ? C1 C2 1.40(1) . . ? C1 C6 1.40(1) . . ? C2 C3 1.36(1) . . ? C3 C4 1.38(1) . . ? C4 C5 1.35(1) . . ? C5 C6 1.41(1) . . ? C7 C8 1.395(9) . . ? C7 C12 1.404(9) . . ? C8 C9 1.395(9) . . ? C9 C10 1.37(1) . . ? C10 C11 1.37(1) . . ? C11 C12 1.39(1) . . ? P2 C13 1.817(6) . . ? P2 C19 1.820(6) . . ? P2 C27 1.833(6) . . ? C13 C14 1.392(9) . . ? C13 C18 1.386(9) . . ? C14 C15 1.367(9) . . ? C15 C16 1.40(1) . . ? C16 C17 1.37(1) . . ? C17 C18 1.385(9) . . ? C19 C20 1.392(8) . . ? C19 C24 1.396(8) . . ? C20 C21 1.378(9) . . ? C21 C22 1.378(9) . . ? C22 C23 1.38(1) . . ? C23 C24 1.384(9) . . ? C25 C26 1.542(8) . . ? C26 C27 1.523(8) . . ? C26 C28 1.545(9) . . ? C26 C29 1.532(8) . . ? C29 C30 1.48(1) . . ? C30 C31 1.21(1) . . ? C31 SI 1.841(8) . . ? SI C32 1.85(1) . . ? SI C33 1.83(1) . . ? SI C34 1.84(1) . . ? C35 CL3 1.71(1) . . ? C35 CL4 1.66(1) . . ? C36 CL5 1.71(1) . . ? C36 CL6 1.73(1) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag CL1 PT CL2 89.72(6) . . . ? CL1 PT P1 85.16(6) . . . ? CL1 PT P2 177.81(6) . . . ? CL2 PT P1 174.87(5) . . . ? CL2 PT P2 88.20(6) . . . ? P1 PT P2 96.92(6) . . . ? C1 P1 C7 108.1(3) . . . ? C1 P1 C25 104.9(3) . . . ? C7 P1 C25 100.5(3) . . . ? P1 C1 C2 120.2(5) . . . ? P1 C1 C6 120.4(6) . . . ? C2 C1 C6 119.2(7) . . . ? C1 C2 C3 120.5(7) . . . ? C2 C3 C4 120.9(8) . . . ? C3 C4 C5 119.7(8) . . . ? C4 C5 C6 121.8(8) . . . ? C1 C6 C5 117.8(8) . . . ? P1 C7 C8 117.2(5) . . . ? P1 C7 C12 123.9(6) . . . ? C8 C7 C12 118.9(6) . . . ? C7 C8 C9 120.7(7) . . . ? C8 C9 C10 119.4(8) . . . ? C9 C10 C11 120.8(7) . . . ? C10 C11 C12 121.0(7) . . . ? C7 C12 C11 119.2(7) . . . ? C13 P2 C19 106.8(3) . . . ? C13 P2 C27 105.3(3) . . . ? C19 P2 C27 102.3(3) . . . ? P2 C13 C14 120.3(4) . . . ? P2 C13 C18 120.4(5) . . . ? C14 C13 C18 119.3(5) . . . ? C13 C14 C15 120.8(6) . . . ? C14 C15 C16 119.8(7) . . . ? C15 C16 C17 119.5(6) . . . ? C16 C17 C18 120.9(6) . . . ? C13 C18 C17 119.8(6) . . . ? P2 C19 C20 118.2(4) . . . ? P2 C19 C24 122.4(5) . . . ? C20 C19 C24 119.2(6) . . . ? C19 C20 C21 120.2(6) . . . ? C20 C21 C22 120.4(6) . . . ? C21 C22 C23 119.8(6) . . . ? C22 C23 C24 120.3(6) . . . ? C19 C24 C23 119.8(6) . . . ? P1 C25 C26 118.5(4) . . . ? C25 C26 C27 108.7(5) . . . ? C25 C26 C28 113.0(5) . . . ? C25 C26 C29 106.5(5) . . . ? C27 C26 C28 111.0(5) . . . ? C27 C26 C29 108.1(5) . . . ? C28 C26 C29 109.3(5) . . . ? P2 C27 C26 119.0(4) . . . ? C26 C29 C30 112.3(6) . . . ? C29 C30 C31 174.3(9) . . . ? C30 C31 SI 178.5(7) . . . ? C31 SI C32 108.7(4) . . . ? C31 SI C33 110.5(4) . . . ? C31 SI C34 106.7(4) . . . ? C32 SI C33 108.9(5) . . . ? C32 SI C34 112.6(4) . . . ? C33 SI C34 109.5(5) . . . ? CL3 C35 CL4 116.1(7) . . . ? CL5 C36 CL6 113.4(7) . . . ? #===END