# om970661d.cif data_MH0197 #Paper OM970661D #---------------------------------------------------------------- _audit_creation_date 'Wed Jan 29 11:30:27 1997' _audit_creation_method 'from TEXRAY.INF file' #---------------------------------------------------------------- _publ_requested_journal 'Organometallics' _publ_contact_author ; 'Prof. Michael M. Haley' Department of Chemistry, University of Oregon, Eugene, OR 97403 ; _publ_contact_author_phone '541-346-0456' _publ_contact_author_email 'haley@oregon.uoregon.edu' loop_ _publ_author_name _publ_author_address 'Joshua J. Pak' ; Department of Chemistry, University of Oregon, Eugene, OR 97403 ; 'Timothy J. R. Weakley' ;Department of Chemistry, University of Oregon, Eugene, OR 97403 ; 'Michael M.Haley' ;Department of Chemistry, University of Oregon, Eugene, OR 97403 _publ_section_title ; `Synthesis and Crystallographic Characterization of a Platinadehydrobenzo[19]annulene' ; _publ_section_abstract ; The trans-platinum complex (Et~3~P)~2~Pt(C~30~H~12~)(2) was synthesized from hexayne 3 in 65% overall yield via a simple three-step process. The X-ray crystal structure of 2 shows a strained and warped annulenic core upon insertion of the organometallic gragment, with phosphine ligands tilted by about 16\% off the normal to the macrocycle mean plane. UV-Vis data suggest electronic delocalization is present in the macrocycle. ; _publ_section_references ; Cromer, D.T. & Waber, J.T. (1974). In International Tables for X-ray Crystallogarphy, vol. IV, pp. 71, 148. Kynoch Press, Birmingham, England. Enraf-Nonius (1993). CAD4/PC diffractometer software, v.1.2. Enraf-Nonius, Delft, Netherlands. Molecular Structure Corporation (1989). TEXSAN structure analysis software, v.5.0. MSC, 3200A Research Forest Drive, The Woodlands, TX 77381, USA. ; ;#------------------------------------------------------------------- _computing_data_collection 'CAD4/PC (Enraf-Nonius, 1993)' _computing_cell_refinement 'CAD4/PC (Enraf-Nonius, 1993)' _computing_data_reduction 'TEXSAN (Molecular Structure Corp., 1989)' _computing_structure_solution ' 'TEXSAN (Molecular Structure Corp., 1989)' _computing_structure_refinement ' 'TEXSAN (Molecular Structure Corp., 1989)' _computing_publication_material ' 'TEXSAN (Molecular Structure Corp., 1989)' #---------------------------------------------------------------- _cell_length_a 14.446(1) _cell_length_b 17.184(3) _cell_length_c 29.856(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7411(2) _cell_formula_units_Z 8 _cell_measurement_temperature 295 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 28.0 _cell_measurement_theta_max 29.2 #------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_Int_Tables_number 61 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y, +z' ' +x,1/2-y,1/2+z' '1/2+x, +y,1/2-z' #----------------------------------------------------------------------- _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.140 _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 803.83 _chemical_formula_analytical ? _chemical_formula_sum 'C42 H42 P2 Pt ' _chemical_formula_structural 'Pt (C30 H12) (P (C2 H5)2) _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 3.936 _exptl_absorpt_correction_type 'empirical (azimuthal scans)' #------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 295.2 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'sealed X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'CAD4 diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 60 _diffrn_standards_decay_% -9.50 _diffrn_reflns_number 7189 _reflns_number_total 7189 _reflns_number_observed 3772 _reflns_observed_criterion 1.5\s(I) _diffrn_reflns_av_R_equivalents 'no equivalents measured' _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 25.0 _diffrn_orient_matrix_UB_11 -0.03268 _diffrn_orient_matrix_UB_12 0.00320 _diffrn_orient_matrix_UB_13 0.02947 _diffrn_orient_matrix_UB_21 -0.05683 _diffrn_orient_matrix_UB_22 0.01953 _diffrn_orient_matrix_UB_23 -0.01545 _diffrn_orient_matrix_UB_31 -0.02222 _diffrn_orient_matrix_UB_32 -0.05471 _diffrn_orient_matrix_UB_33 -0.00380 #-------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 336 0.002 0.002 'Cromer & Waber (1974)' H 0 336 0.000 0.000 'Cromer & Waber (1974)' P 0 16 0.090 0.095 'Cromer & Waber (1974)' Pt 0 8 -2.352 8.388 'Cromer & Waber (1974)' #------------------------------------------------------------------- _refine_special_details ;Parameters for C(41, 42) did not converge properly during anisotropic refinement. Apparently these atoms had alternative positions which could not be modelled. They were included at observed positions with fixed isotropic thermal parameters. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 4F~o~^2^/[sig^2^(I) + (0.02I)^2^]' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_number_reflns 3772 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.0501 _refine_ls_wR_factor_obs 0.0447 _refine_ls_goodness_of_fit_obs 1.686 _refine_ls_shift/esd_max 0.023 _refine_diff_density_min 0.96 _refine_diff_density_max -1.23 #-------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Pt() 0.19020(3) 0.52607(2) RGET1 0.0505(1) Uij ? ? P(1) 0.1563(2) 0.6187(2) 0.56014(9) 0.0505(9) Uij ? ? P(2) 0.2237(3) 0.4279(2) 0.6610(1) 0.094(1) Uij ? ? C(1) 0.2069(7) 0.4530(6) 0.5611(3) 0.054(3) Uij ? ? C(2) 0.2307(7) 0.4139(6) 0.5300(4) 0.056(4) Uij ? ? C(3) 0.2640(8) 0.3720(6) 0.4908(3) 0.053(4) Uij ? ? C(4) 0.2008(8) 0.3394(7) 0.4611(3) 0.067(4) Uij ? ? C(5) 0.2317(9) 0.3001(8) 0.4237(4) 0.082(5) Uij ? ? C(6) 0.3262(8) 0.2930(7) 0.4144(3) 0.073(4) Uij ? ? C(7) 0.3868(7) 0.3267(6) 0.4434(3) 0.055(3) Uij ? ? C(8) 0.3582(7) 0.3636(6) 0.4820(3) 0.049(3) Uij ? ? C(9) 0.4237(7) 0.3956(6) 0.5125(3) 0.054(4) Uij ? ? C(10) 0.4843(8) 0.4185(6) 0.5370(3) 0.059(4) Uij ? ? C(11) 0.5567(8) 0.4423(6) 0.5644(3) 0.060(4) Uij ? ? C(12) 0.6174(8) 0.4638(7) 0.5870(3) 0.060(4) Uij ? ? C(13) 0.6957(8) 0.4869(6) 0.6121(3) 0.057(3) Uij ? ? C(14) 0.7863(9) 0.4617(8) 0.5991(4) 0.084(5) Uij ? ? C(15) 0.8643(9) 0.4817(9) 0.6219(4) 0.095(5) Uij ? ? C(16) 0.8581(8) 0.5287(9) 0.6581(5) 0.096(5) Uij ? ? C(17) 0.773(1) 0.5563(8) 0.6720(4) 0.091(5) Uij ? ? C(18) 0.6903(8) 0.5350(6) 0.6498(3) 0.058(3) Uij ? ? C(19) 0.6062(9) 0.5657(7) 0.6650(4) 0.063(4) Uij ? ? C(20) 0.5390(8) 0.5960(7) 0.6806(3) 0.060(4) Uij ? ? C(21) 0.4636(8) 0.6319(7) 0.7012(4) 0.061(4) Uij ? ? C(22) 0.4001(8) 0.6635(7) 0.7203(3) 0.059(4) Uij ? ? C(23) 0.3301(7) 0.7015(6) 0.7443(3) 0.049(3) Uij ? ? C(24) 0.3517(8) 0.7477(7) 0.7811(4) 0.069(4) Uij ? ? C(25) 0.284(1) 0.7860(7) 0.8043(4) 0.080(5) Uij ? ? C(26) 0.191(1) 0.7778(7) 0.7917(4) 0.077(5) Uij ? ? C(27) 0.1663(8) 0.7313(6) 0.7556(3) 0.062(4) Uij ? ? C(28) 0.2355(8) 0.6929(6) 0.7315(3) 0.051(3) Uij ? ? C(29) 0.2116(7) 0.6452(6) 0.6940(3) 0.052(4) Uij ? ? C(30) 0.1963(8) 0.6014(6) 0.6630(3) 0.059(4) Uij ? ? C(31) 0.0659(7) 0.5851(6) 0.5221(3) 0.057(3) Uij ? ? C(32) 0.0387(8) 0.6407(7) 0.4855(4) 0.081(5) Uij ? ? C(33) 0.2552(9) 0.6385(7) 0.5236(4) 0.077(4) Uij ? ? C(34) 0.3385(8) 0.6676(9) 0.5480(5) 0.119(6) Uij ? ?C42 C(35) 0.1197(8) 0.7121(6) 0.5809(3) 0.066(4) Uij ? ? C(36) 0.0293(9) 0.7099(7) 0.6059(4) 0.095(5) Uij ? ? C(37) 0.179(1) 0.3317(8) 0.6445(4) 0.113(6) Uij ? ? C(38) 0.080(1) 0.3267(10) 0.6363(5) 0.131(7) Uij ? ? C(39) 0.191(2) 0.441(1) 0.7185(5) 0.20(1) Uij ? ? C(40) 0.097(2) 0.457(1) 0.7254(7) 0.18(1) Uij ? ? C(41) 0.3494 0.3892 0.6564 0.1520 Uiso ? ? C(42) 0.3909 0.4240 0.6586 0.1900 Uiso ? ? H(1) 0.1363 0.3443 0.4666 0.0806 Uiso calc C4 H(2) 0.1879 0.2775 0.4039 0.0986 Uiso calc C5 H(3) 0.3473 0.2655 0.3887 0.0879 Uiso calc C6 H(4) 0.4511 0.3247 0.4369 0.0660 Uiso calc C7 H(5) 0.7922 0.4295 0.5734 0.1009 Uiso calc C14 H(6) 0.9228 0.4627 0.6125 0.1142 Uiso calc C15 H(7) 0.9125 0.5429 0.6740 0.1152 Uiso calc C16 H(8) 0.7695 0.5903 0.6970 0.1098 Uiso calc C17 H(9) 0.4145 0.7528 0.7902 0.0834 Uiso calc C24 H(10) 0.3002 0.8181 0.8291 0.0957 Uiso calc C25 H(11) 0.1443 0.8044 0.8080 0.0922 Uiso calc C26 H(12) 0.1031 0.7257 0.7474 0.0741 Uiso calc C27 H(13) 0.0870 0.5384 0.5084 0.0683 Uiso calc C31 H(14) 0.0122 0.5743 0.5394 0.0683 Uiso calc C31 H(15) 0.0914 0.6527 0.4678 0.0972 Uiso calc C32 H(16) -0.0074 0.6174 0.4672 0.0972 Uiso calc C32 H(17) 0.0149 0.6871 0.4984 0.0972 Uiso calc C32 H(18) 0.2714 0.5917 0.5086 0.0926 Uiso calc C33 H(19) 0.2373 0.6766 0.5023 0.0926 Uiso calc C33 H(20) 0.3597 0.6288 0.5682 0.1424 Uiso calc C34 H(21) 0.3860 0.6794 0.5270 0.1424 Uiso calc C34 H(22) 0.3228 0.7133 0.5642 0.1424 Uiso calc C34 H(23) 0.1661 0.7313 0.6006 0.0793 Uiso calc C35 H(24) 0.1133 0.7465 0.5562 0.0793 Uiso calc C35 H(25) 0.0128 0.7612 0.6148 0.1137 Uiso calc C36 H(26) -0.0175 0.6892 0.5870 0.1137 Uiso calc C36 H(27) 0.0356 0.6780 0.6317 0.1137 Uiso calc C36 H(28) 0.2099 0.3167 0.6178 0.1356 Uiso calc C37 H(29) 0.1936 0.2961 0.6677 0.1356 Uiso calc C37 H(30) 0.0477 0.3412 0.6626 0.1566 Uiso calc C38 H(31) 0.0641 0.3608 0.6125 0.1566 Uiso calc C38 H(32) 0.0647 0.2748 0.6283 0.1566 Uiso calc C38 H(33) 0.2063 0.3945 0.7343 0.2392 Uiso calc C39 H(34) 0.2263 0.4829 0.7304 0.2392 Uiso calc C39 H(35) 0.0855 0.4624 0.7566 0.2179 Uiso calc C40 H(36) 0.0810 0.5036 0.7104 0.2179 Uiso calc C40 H(37) 0.0609 0.4151 0.7140 0.2179 Uiso calc C40 H(38) 0.3589 0.3523 0.6796 0.1824 Uiso calc C41 H(39) 0.3561 0.3643 0.6282 0.1824 Uiso calc C41 H(40) 0.4503 0.4005 0.6563 0.2280 Uiso calc C42 H(41) 0.3834 0.4609 0.6352 0.2280 Uiso calc C42 H(42) 0.3855 0.4494 0.6867 0.2280 Uiso calc C42 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 Pt() 0.0555(2) 0.0527(2) 0.0433(2) 0.0069(3) -0.0049(3) -0.0047(3) P(1) 0.053(2) 0.049(2) 0.050(2) -0.006(1) -0.001(1) -0.001(1) P(2) 0.115(3) 0.087(3) 0.079(2) 0.038(2) -0.029(2) 0.011(2) C(1) 0.060(7) 0.052(7) 0.049(6) 0.001(6) 0.002(6) -0.007(5) C(2) 0.044(7) 0.064(8) 0.061(7) 0.007(6) -0.007(6) -0.005(6) C(3) 0.063(8) 0.048(7) 0.048(6) 0.005(6) -0.010(6) -0.006(6) C(4) 0.058(7) 0.082(8) 0.062(7) 0.004(7) -0.004(7) -0.026(6) C(5) 0.070(9) 0.11(1) 0.064(8) -0.002(8) -0.022(7) -0.039(8) C(6) 0.080(10) 0.094(9) 0.046(6) 0.007(8) -0.014(7) -0.026(7) C(7) 0.049(7) 0.075(8) 0.041(6) -0.001(6) 0.003(5) -0.019(6) C(8) 0.050(7) 0.050(7) 0.046(6) 0.000(6) -0.009(6) -0.005(6) C(9) 0.056(7) 0.057(8) 0.048(7) -0.007(6) 0.004(6) -0.007(6) C(10) 0.073(8) 0.062(8) 0.042(6) 0.000(7) 0.000(6) -0.003(6) C(11) 0.062(8) 0.067(8) 0.052(7) -0.011(6) -0.001(6) -0.015(6) C(12) 0.060(7) 0.069(8) 0.052(7) -0.004(7) 0.005(6) -0.011(7) C(13) 0.060(6) 0.060(7) 0.050(5) 0.003(7) -0.010(7) -0.006(6) C(14) 0.08(1) 0.11(1) 0.064(8) 0.022(8) -0.008(7) -0.025(7) C(15) 0.060(9) 0.14(1) 0.09(1) 0.031(9) -0.015(7) -0.024(10) C(16) 0.045(8) 0.13(1) 0.11(1) 0.011(9) -0.031(8) -0.04(1) C(17) 0.080(10) 0.10(1) 0.091(10) -0.007(9) -0.032(8) -0.040(8) C(18) 0.056(6) 0.068(7) 0.050(6) 0.009(8) 0.002(6) -0.009(6) C(19) 0.062(8) 0.064(8) 0.062(8) -0.014(7) 0.002(7) -0.015(7) C(20) 0.061(8) 0.061(8) 0.059(8) 0.003(7) -0.007(6) -0.008(6) C(21) 0.064(8) 0.057(8) 0.063(8) -0.011(7) -0.006(7) -0.002(6) C(22) 0.060(8) 0.064(8) 0.053(7) -0.012(7) 0.005(6) -0.001(6) C(23) 0.059(8) 0.052(7) 0.035(6) 0.000(6) 0.003(5) 0.000(5) C(24) 0.093(9) 0.065(8) 0.051(7) -0.006(8) -0.002(7) -0.006(6) C(25) 0.15(1) 0.055(8) 0.038(7) -0.012(9) 0.015(8) -0.009(6) C(26) 0.11(1) 0.064(8) 0.053(8) 0.004(9) 0.035(9) 0.002(6) C(27) 0.078(9) 0.057(7) 0.050(7) 0.016(7) 0.020(6) 0.000(6) C(28) 0.072(8) 0.050(7) 0.031(5) -0.012(6) -0.003(6) 0.003(5) C(29) 0.050(8) 0.061(8) 0.045(6) 0.002(6) -0.003(5) 0.011(6) C(30) 0.060(7) 0.062(8) 0.054(7) 0.010(7) 0.001(7) 0.002(6) C(31) 0.050(7) 0.061(7) 0.060(7) -0.012(6) -0.009(6) 0.002(6) C(32) 0.095(10) 0.084(10) 0.065(8) 0.002(8) -0.010(7) 0.009(7) C(33) 0.083(9) 0.078(9) 0.071(8) -0.019(8) 0.014(8) 0.014(7) C(34) 0.056(9) 0.18(2) 0.12(1) -0.037(9) 0.009(8) -0.02(1) C(35) 0.076(9) 0.057(8) 0.064(8) -0.002(7) -0.008(7) -0.007(6) C(36) 0.09(1) 0.093(10) 0.10(1) 0.026(8) -0.015(9) -0.029(8) C(37) 0.20(2) 0.066(9) 0.077(9) 0.05(1) 0.01(1) 0.010(7) C(38) 0.17(2) 0.10(1) 0.12(1) -0.01(1) 0.01(1) 0.00(1) C(39) 0.46(4) 0.08(1) 0.051(10) 0.03(2) -0.06(2) 0.007(9) C(40) 0.30(3) 0.13(2) 0.11(1) 0.00(2) 0.10(2) -0.02(1) #------------------------------------------------------------- _geom_special_details ? 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 2.283(3) ? ? yes Pt P2 2.277(4) ? ? yes Pt C1 1.996(10) ? ? yes Pt C30 1.99(1) ? ? yes P1 C31 1.826(9) ? ? yes P1 C33 1.83(1) ? ? yes P1 C35 1.80(1) ? ? yes P2 C37 1.84(2) ? ? yes P2 C39 1.79(2) ? ? yes P2 C41 1.94(1) ? ? yes C1 C2 1.20(1) ? ? yes C2 C3 1.46(1) ? ? yes C3 C4 1.39(1) ? ? yes C3 C8 1.39(1) ? ? yes C4 C5 1.38(1) ? ? yes C5 C6 1.40(1) ? ? yes C6 C7 1.36(1) ? ? yes C7 C8 1.38(1) ? ? yes C8 C9 1.42(1) ? ? yes C9 C10 1.21(1) ? ? yes C10 C11 1.39(1) ? ? yes C11 C12 1.17(1) ? ? yes C12 C13 1.41(1) ? ? yes C13 C14 1.43(1) ? ? yes C13 C18 1.40(1) ? ? yes C14 C15 1.36(2) ? ? yes C15 C16 1.35(2) ? ? yes C16 C17 1.39(2) ? ? yes C17 C18 1.41(1) ? ? yes C18 C19 1.40(1) ? ? yes C19 C20 1.20(1) ? ? yes C20 C21 1.39(1) ? ? yes C21 C22 1.21(1) ? ? yes C22 C23 1.40(1) ? ? yes C23 C24 1.39(1) ? ? yes C23 C28 1.43(1) ? ? yes C24 C25 1.37(2) ? ? yes C25 C26 1.41(2) ? ? yes C26 C27 1.39(1) ? ? yes C27 C28 1.40(1) ? ? yes C28 C29 1.43(1) ? ? yes C29 C30 1.21(1) ? ? yes C31 C32 1.50(1) ? ? yes C33 C34 1.49(2) ? ? yes C35 C36 1.50(1) ? ? yes C37 C38 1.45(2) ? ? yes C39 C40 1.40(3) ? ? yes C41 C42 0.849 ? ? yes#------------------------------------------------------------------ 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 176.3(1) ? ? ? yes P1 Pt C1 86.5(3) ? ? ? yes P1 Pt C30 94.3(3) ? ? ? yes P2 Pt C1 89.8(3) ? ? ? yes P2 Pt C30 89.4(3) ? ? ? yes C1 Pt C30 170.4(4) ? ? ? yes Pt P1 C31 111.0(3) ? ? ? yes Pt P1 C33 111.7(4) ? ? ? yes Pt P1 C35 116.6(4) ? ? ? yes C31 P1 C33 104.3(5) ? ? ? yes C31 P1 C35 106.7(5) ? ? ? yes C33 P1 C35 105.6(5) ? ? ? yes Pt P2 C37 114.8(5) ? ? ? yes Pt P2 C39 117.6(6) ? ? ? yes Pt P2 C41 114(1) ? ? ? yes C37 P2 C39 106.0(9) ? ? ? yes C37 P2 C41 90(1) ? ? ? yes C39 P2 C41 111(1) ? ? ? yes Pt C1 C2 169.7(9) ? ? ? yes C1 C2 C3 175(1) ? ? ? yes C2 C3 C4 119(1) ? ? ? yes C2 C3 C8 121.6(10) ? ? ? yes C4 C3 C8 118(1) ? ? ? yes C3 C4 C5 120(1) ? ? ? yes C4 C5 C6 121(1) ? ? ? yes C5 C6 C7 117.6(10) ? ? ? yes C6 C7 C8 122.3(10) ? ? ? yes C3 C8 C7 119.8(10) ? ? ? yes C3 C8 C9 119.3(10) ? ? ? yes C7 C8 C9 120.8(10) ? ? ? yes C8 C9 C10 174(1) ? ? ? yes C9 C10 C11 177(1) ? ? ? yes C10 C11 C12 178(1) ? ? ? yes C11 C12 C13 175(1) ? ? ? yes C12 C13 C14 120.2(10) ? ? ? yes C12 C13 C18 123(1) ? ? ? yes C14 C13 C18 116.6(10) ? ? ? yes C13 C14 C15 123(1) ? ? ? yes C14 C15 C16 119(1) ? ? ? yes C15 C16 C17 120(1) ? ? ? yes C16 C17 C18 121(1) ? ? ? yes C13 C18 C17 118(1) ? ? ? yes C13 C18 C19 122(1) ? ? ? yes C17 C18 C19 118.8(10) ? ? ? yes C18 C19 C20 174(1) ? ? ? yes C19 C20 C21 176(1) ? ? ? yes C20 C21 C22 177(1) ? ? ? yes C21 C22 C23 176(1) ? ? ? yes C22 C23 C24 120(1) ? ? ? yes C22 C23 C28 120.3(9) ? ? ? yes C24 C23 C28 119.2(10) ? ? ? yes C23 C24 C25 121(1) ? ? ? yes C24 C25 C26 119(1) ? ? ? yes C25 C26 C27 120(1) ? ? ? yes C26 C27 C28 119(1) ? ? ? yes C23 C28 C27 119.8(9) ? ? ? yes C23 C28 C29 120.1(10) ? ? ? yes C27 C28 C29 120.1(10) ? ? ? yes C28 C29 C30 175(1) ? ? ? yes Pt C30 C29 171(1) ? ? ? yes P1 C31 C32 115.9(8) ? ? ? yes P1 C33 C34 113.7(8) ? ? ? yes P1 C35 C36 113.8(8) ? ? ? yes P2 C37 C38 116(1) ? ? ? yes P2 C39 C40 114(1) ? ? ? yes P2 C41 C42 115(2) ? ? ? yes #----------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pt P1 C31 C32 -178.9(7) ? ? ? ? no Pt P1 C33 C34 -60(1) ? ? ? ? no Pt P1 C35 C36 -64.6(9) ? ? ? ? no Pt P2 C37 C38 -56(1) ? ? ? ? no Pt P2 C39 C40 56(2) ? ? ? ? no Pt P2 C41 C42 54(1) ? ? ? ? no Pt C1 C2 C3 -38(17) ? ? ? ? no Pt C30 C29 C28 -27(19) ? ? ? ? no P1 Pt P2 C37 -28(2) ? ? ? ? no P1 Pt P2 C39 -153(2) ? ? ? ? no P1 Pt P2 C41 74(2) ? ? ? ? no P1 Pt C1 C2 84(5) ? ? ? ? no P1 Pt C30 C29 -113(7) ? ? ? ? no P2 Pt P1 C31 43(2) ? ? ? ? no P2 Pt P1 C33 -73(2) ? ? ? ? no P2 Pt P1 C35 166(2) ? ? ? ? no P2 Pt C1 C2 -96(5) ? ? ? ? no P2 Pt C30 C29 67(7) ? ? ? ? no C1 Pt P1 C31 52.4(4) ? ? ? ? no C1 Pt P1 C33 -63.6(5) ? ? ? ? no C1 Pt P1 C35 174.8(5) ? ? ? ? no C1 Pt P2 C37 -36.8(7) ? ? ? ? no C1 Pt P2 C39 -163(1) ? ? ? ? no C1 Pt P2 C41 65(1) ? ? ? ? no C1 Pt C30 C29 -18(8) ? ? ? ? no C1 C2 C3 C4 -122(13) ? ? ? ? no C1 C2 C3 C8 58(13) ? ? ? ? no C2 C1 Pt C30 -11(7) ? ? ? ? no C2 C3 C4 C5 180(1) ? ? ? ? no C2 C3 C8 C7 -177(1) ? ? ? ? no C2 C3 C8 C9 1(2) ? ? ? ? no C3 C4 C5 C6 -1(2) ? ? ? ? no C3 C8 C7 C6 -4(2) ? ? ? ? no C3 C8 C9 C10 157(12) ? ? ? ? no C4 C3 C8 C7 3(2) ? ? ? ? no C4 C3 C8 C9 -179(1) ? ? ? ? no C4 C5 C6 C7 0(2) ? ? ? ? no C5 C4 C3 C8 0(2) ? ? ? ? no C5 C6 C7 C8 3(2) ? ? ? ? no C6 C7 C8 C9 178(1) ? ? ? ? no C7 C8 C9 C10 -25(13) ? ? ? ? no C8 C9 C10 C11 1(36) ? ? ? ? no C9 C10 C11 C12 119(48) ? ? ? ? no C10 C11 C12 C13 -103(48) ? ? ? ? no C11 C12 C13 C14 -2(17) ? ? ? ? no C11 C12 C13 C18 177(16) ? ? ? ? no C12 C13 C14 C15 -180(1) ? ? ? ? no C12 C13 C18 C17 -179(1) ? ? ? ? no C12 C13 C18 C19 -2(2) ? ? ? ? no C13 C14 C15 C16 -1(2) ? ? ? ? no C13 C18 C17 C16 -2(2) ? ? ? ? no C13 C18 C19 C20 -171(12) ? ? ? ? no C14 C13 C18 C17 1(2) ? ? ? ? no C14 C13 C18 C19 178(1) ? ? ? ? no C14 C15 C16 C17 0(2) ? ? ? ? no C15 C14 C13 C18 1(2) ? ? ? ? no C15 C16 C17 C18 1(2) ? ? ? ? no C16 C17 C18 C19 -179(1) ? ? ? ? no C17 C18 C19 C20 5(13) ? ? ? ? no C18 C19 C20 C21 -27(32) ? ? ? ? no C19 C20 C21 C22 3(48) ? ? ? ? no C20 C21 C22 C23 11(49) ? ? ? ? no C21 C22 C23 C24 7(22) ? ? ? ? no C21 C22 C23 C28 -172(21) ? ? ? ? no C22 C23 C24 C25 179(1) ? ? ? ? no C22 C23 C28 C27 -179.8(9) ? ? ? ? no C22 C23 C28 C29 0(1) ? ? ? ? no C23 C24 C25 C26 1(2) ? ? ? ? no C23 C28 C27 C26 0(1) ? ? ? ? no C23 C28 C29 C30 34(14) ? ? ? ? no C24 C23 C28 C27 1(1) ? ? ? ? no C24 C23 C28 C29 -179.5(9) ? ? ? ? no C24 C25 C26 C27 0(2) ? ? ? ? no C25 C24 C23 C28 -1(2) ? ? ? ? no C25 C26 C27 C28 -1(2) ? ? ? ? no C26 C27 C28 C29 -179.5(9) ? ? ? ? no C27 C28 C29 C30 -146(14) ? ? ? ? no C30 Pt P1 C31 -137.2(5) ? ? ? ? no C30 Pt P1 C33 106.9(5) ? ? ? ? no C30 Pt P1 C35 -14.7(5) ? ? ? ? no C30 Pt P2 C37 152.7(7) ? ? ? ? no C30 Pt P2 C39 27(1) ? ? ? ? no C30 Pt P2 C41 -105(1) ? ? ? ? no C31 P1 C33 C34 180(1) ? ? ? ? no C31 P1 C35 C36 60.1(9) ? ? ? ? no C32 C31 P1 C33 -58.5(9) ? ? ? ? no C32 C31 P1 C35 53.0(9) ? ? ? ? no C33 P1 C35 C36 170.7(8) ? ? ? ? no C34 C33 P1 C35 67(1) ? ? ? ? no C37 P2 C39 C40 -74(2) ? ? ? ? no C37 P2 C41 C42 171.1(4) ? ? ? ? no C38 C37 P2 C39 76(2) ? ? ? ? no C38 C37 P2 C41 -172(2) ? ? ? ? no C39 P2 C41 C42 -82(2) ? ? ? ? no C40 C39 P2 C41 -170(2) ? ? ? ? no