synthesis, structures and properties of novel … ho ∙ yih hsing lo ∙ li liu ∙ hua li ∙...
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Synthesis, Structures and Properties of Novel Platinum(II) Acetylide Complexes and Polymers with Tri(tolyl)phosphine as the Auxiliary Ligand
Abu Ali Ibn Sina ∙ S. M. Ibrahim Al-Rafia ∙ Md. Faruak Ahmad ∙ Ratan
Kumar Paul ∙ S. M. Saiful Islam ∙ Muhammad Younus ∙ Paul R. Raithby ∙
Cheuk-Lam Ho ∙ Yih Hsing Lo ∙ Li Liu ∙ Hua Li ∙ Wai-Yeung Wong
Figure S1. 1H NMR spectrum of 1 in CDCl3.
Figure S2. 13C NMR spectrum of 1 in CDCl3.
Figure S3. 1H NMR spectrum of 2 in CDCl3.
Figure S4. 13C NMR spectrum of 2 in CDCl3.
Figure S5. 1H NMR spectrum of 4 in CDCl3.
Figure S6. 13C NMR spectrum of 4 in CDCl3.
data_publication_text _publ_requested_journal 'J. Inorg. Organomet.' _publ_contact_author_name 'Professor Paul R Raithby' _publ_contact_author_address ;Department of Chemistry University of Bath Bath BA2 7AY UK ; _publ_contact_author_email [email protected] _publ_contact_author_phone +441225383183 _publ_contact_author_fax +441225386231 loop_ _publ_author_name _publ_author_address 'Raithby, Paul R' ;Department of Chemistry University of Bath Bath BA2 7AY UK ; 'Ibn Sina, Abu Ali' 'Department of Chemistry, Shahjalal University of Science and Technology, Sylhet-3114, Bangladesh' 'Al-Rafia, S. M. Ibrahim' 'Department of Chemistry, Shahjalal University of Science and Technology, Sylhet-3114, Bangladesh' 'Ahmad, md. Faruak' 'Department of Chemistry, Shahjalal University of Science and Technology, Sylhet-3114, Bangladesh' 'Kumar Paul, Ratan' 'Department of Chemistry, Shahjalal University of Science and Technology, Sylhet-3114, Bangladesh' 'Islam, S. M. Saiful' 'Department of Chemistry, Shahjalal University of Science and Technology, Sylhet-3114, Bangladesh' 'Younus, Muhammad' 'Department of Chemistry, Shahjalal University of Science and Technology, Sylhet-3114, Bangladesh' 'Wong, Wai-Yeung' 'Department of Chemistry, Hong Kong Baptist University, Hong Kong, PR China' data_p09prr71 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H50 N2 O4 P2 Pt' _chemical_formula_weight 1096.03
loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7956(2) _cell_length_b 11.0876(2) _cell_length_c 11.8791(1) _cell_angle_alpha 93.145(1) _cell_angle_beta 100.602(1) _cell_angle_gamma 115.850(1) _cell_volume 1243.02(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 75973 _cell_measurement_theta_min 2.7028 _cell_measurement_theta_max 32.8766 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 2.935 _exptl_absorpt_correction_T_min 0.82811 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ;
CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 10.3795 _diffrn_reflns_number 88776 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.7028 _diffrn_reflns_theta_max 32.8766 _diffrn_orient_matrix_UB_11 -0.0111447597 _diffrn_orient_matrix_UB_12 -0.0681926819 _diffrn_orient_matrix_UB_13 -0.0032748354 _diffrn_orient_matrix_UB_21 0.0672366789 _diffrn_orient_matrix_UB_22 0.0197491594 _diffrn_orient_matrix_UB_23 -0.0127601228 _diffrn_orient_matrix_UB_31 0.0314007388 _diffrn_orient_matrix_UB_32 0.0117109663 _diffrn_orient_matrix_UB_33 0.0600409445 _reflns_number_total 8851 _reflns_number_gt 8830 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction
; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.4288P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8851 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0136 _refine_ls_R_factor_gt 0.0135 _refine_ls_wR_factor_ref 0.0353 _refine_ls_wR_factor_gt 0.0353 _refine_ls_goodness_of_fit_ref 0.699 _refine_ls_restrained_S_all 0.699 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity
_atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.06926(11) 0.00099(10) 0.14422(9) 0.01673(17) Uani 1 1 d . . . C2 C -0.11289(12) 0.00486(11) 0.23048(10) 0.01937(18) Uani 1 1 d . . . C3 C -0.16910(11) 0.00923(11) 0.33025(9) 0.01812(18) Uani 1 1 d . . . C4 C -0.15680(11) -0.06681(11) 0.41866(9) 0.01770(17) Uani 1 1 d . . . H4 H -0.1102 -0.1216 0.4125 0.021 Uiso 1 1 calc R . . C5 C -0.21186(11) -0.06294(11) 0.51480(9) 0.01870(18) Uani 1 1 d . . . H5 H -0.2035 -0.1145 0.5744 0.022 Uiso 1 1 calc R . . C6 C -0.27938(11) 0.01772(11) 0.52195(9) 0.01916(18) Uani 1 1 d . . . C7 C -0.29244(14) 0.09531(13) 0.43711(11) 0.0249(2) Uani 1 1 d . . . H7 H -0.3381 0.1507 0.4446 0.030 Uiso 1 1 calc R . . C8 C -0.23763(14) 0.09052(13) 0.34114(11) 0.0251(2) Uani 1 1 d . . . H8 H -0.2464 0.1426 0.2821 0.030 Uiso 1 1 calc R . . C9 C -0.13560(11) 0.22372(10) 0.01615(9) 0.01498(16) Uani 1 1 d . . . C10 C -0.26351(11) 0.13411(11) -0.05973(9) 0.01869(18) Uani 1 1 d . . . H10 H -0.2646 0.0715 -0.1182 0.022 Uiso 1 1 calc R . . C11 C -0.38947(12) 0.13592(12) -0.05021(11) 0.0226(2) Uani 1 1 d . . . H11 H -0.4751 0.0764 -0.1039 0.027 Uiso 1 1 calc R . . C12 C -0.39137(12) 0.22395(12) 0.03719(12) 0.0236(2) Uani 1 1 d . . . C13 C -0.26431(13) 0.30977(12) 0.11477(11) 0.0227(2) Uani 1 1 d . . . H13 H -0.2643 0.3687 0.1759 0.027 Uiso 1 1 calc R . . C14 C -0.13701(12) 0.31125(10) 0.10488(10) 0.01843(18) Uani 1 1 d . . . H14 H -0.0514 0.3715 0.1583 0.022 Uiso 1 1 calc R . . C15 C -0.52705(15) 0.22720(16) 0.04887(16) 0.0372(3) Uani 1 1 d . . . H15A H -0.5486 0.1986 0.1225 0.056 Uiso 1 1 calc R . . H15B H -0.6046 0.1655 -0.0154 0.056 Uiso 1 1 calc R . . H15C H -0.5159 0.3196 0.0471 0.056 Uiso 1 1 calc R . . C16 C 0.06281(11) 0.28957(9) -0.13230(8) 0.01452(16) Uani 1 1 d . . . C17 C -0.03700(12) 0.30516(11) -0.21447(9) 0.01901(18) Uani 1 1 d . . . H17 H -0.1281 0.2826 -0.2011 0.023 Uiso 1 1 calc R . . C18 C -0.00388(14) 0.35373(12) -0.31648(10) 0.0237(2) Uani 1 1 d . . . H18 H -0.0734 0.3631 -0.3720 0.028 Uiso 1 1 calc R . . C19 C 0.12865(14) 0.38859(12) -0.33832(10) 0.0240(2) Uani 1 1 d . . . C20 C 0.22905(13) 0.37476(12) -0.25475(10) 0.0224(2) Uani 1 1 d . . . H20 H 0.3210 0.3998 -0.2673 0.027 Uiso 1 1 calc R . . C21 C 0.19672(12) 0.32501(11) -0.15352(10) 0.01849(18) Uani 1 1 d . . . H21 H 0.2661 0.3150 -0.0983 0.022 Uiso 1 1 calc R . . C22 C 0.1633(2) 0.44034(19) -0.44930(14) 0.0416(4) Uani 1 1 d . . . H22A H 0.0755 0.4183 -0.5062 0.062 Uiso 1 1 calc R . . H22B H 0.2151 0.3974 -0.4801 0.062 Uiso 1 1 calc R . . H22C H 0.2219 0.5389 -0.4335 0.062 Uiso 1 1 calc R . . C23 C 0.16600(10) 0.33969(10) 0.11316(8) 0.01433(16) Uani 1 1 d . . . C24 C 0.20730(12) 0.47822(10) 0.11348(10) 0.01957(19) Uani 1 1 d . . . H24 H 0.1642 0.5075 0.0511 0.023 Uiso 1 1 calc R . . C25 C 0.31085(12) 0.57297(11) 0.20433(10) 0.01998(19) Uani 1 1 d . . . H25 H 0.3374 0.6666 0.2038 0.024 Uiso 1 1 calc R . . C26 C 0.37638(11) 0.53245(11) 0.29645(9) 0.01725(17) Uani 1 1 d . . . C27 C 0.33812(12) 0.39460(11) 0.29348(10) 0.02025(19) Uani 1 1 d . . . H27 H 0.3844 0.3658 0.3541 0.024 Uiso 1 1 calc R . . C28 C 0.23340(11) 0.29850(10) 0.20338(9) 0.01721(17) Uani 1 1 d . . . H28 H 0.2079 0.2050 0.2034 0.021 Uiso 1 1 calc R . . C29 C 0.48440(13) 0.63682(12) 0.39583(11) 0.0252(2) Uani 1 1 d . . . H29A H 0.4365 0.6535 0.4529 0.038 Uiso 1 1 calc R . . H29B H 0.5369 0.7214 0.3671 0.038 Uiso 1 1 calc R . .
H29C H 0.5502 0.6036 0.4323 0.038 Uiso 1 1 calc R . . N1 N -0.34164(11) 0.01862(11) 0.62115(9) 0.02442(19) Uani 1 1 d . . . O1 O -0.35645(13) -0.07027(12) 0.68232(9) 0.0350(2) Uani 1 1 d . . . O2 O -0.37824(11) 0.10766(11) 0.63796(9) 0.0322(2) Uani 1 1 d . . . P1 P 0.02430(3) 0.21619(2) -0.00167(2) 0.01260(4) Uani 1 1 d . . . Pt1 Pt 0.0000 0.0000 0.0000 0.01220(2) Uani 1 2 d S . . 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 C1 0.0212(4) 0.0119(4) 0.0176(4) 0.0032(3) 0.0049(4) 0.0077(3) C2 0.0231(5) 0.0155(4) 0.0194(5) 0.0028(3) 0.0065(4) 0.0080(4) C3 0.0198(4) 0.0167(4) 0.0165(4) 0.0011(3) 0.0053(4) 0.0068(4) C4 0.0189(4) 0.0166(4) 0.0167(4) 0.0009(3) 0.0044(3) 0.0073(3) C5 0.0192(4) 0.0186(4) 0.0152(4) 0.0012(3) 0.0035(3) 0.0061(4) C6 0.0184(4) 0.0209(4) 0.0156(4) -0.0012(3) 0.0056(3) 0.0064(4) C7 0.0300(6) 0.0279(5) 0.0244(5) 0.0044(4) 0.0104(4) 0.0183(5) C8 0.0346(6) 0.0280(5) 0.0221(5) 0.0082(4) 0.0117(5) 0.0200(5) C9 0.0179(4) 0.0132(4) 0.0157(4) 0.0041(3) 0.0045(3) 0.0082(3) C10 0.0193(4) 0.0174(4) 0.0180(4) 0.0035(3) 0.0045(4) 0.0070(4) C11 0.0172(4) 0.0219(5) 0.0268(5) 0.0079(4) 0.0041(4) 0.0071(4) C12 0.0220(5) 0.0213(5) 0.0349(6) 0.0126(4) 0.0114(4) 0.0139(4) C13 0.0270(5) 0.0188(5) 0.0298(6) 0.0062(4) 0.0112(4) 0.0151(4) C14 0.0222(5) 0.0152(4) 0.0204(5) 0.0022(3) 0.0050(4) 0.0108(4) C15 0.0262(6) 0.0349(7) 0.0605(10) 0.0124(6) 0.0154(6) 0.0201(5) C16 0.0190(4) 0.0112(4) 0.0137(4) 0.0025(3) 0.0033(3) 0.0073(3) C17 0.0208(5) 0.0187(4) 0.0177(4) 0.0068(3) 0.0035(4) 0.0091(4) C18 0.0300(6) 0.0248(5) 0.0180(5) 0.0092(4) 0.0046(4) 0.0138(4) C19 0.0363(6) 0.0212(5) 0.0201(5) 0.0092(4) 0.0122(4) 0.0154(5) C20 0.0281(5) 0.0209(5) 0.0248(5) 0.0082(4) 0.0136(4) 0.0135(4) C21 0.0216(5) 0.0172(4) 0.0201(5) 0.0053(3) 0.0067(4) 0.0109(4) C22 0.0575(10) 0.0540(9) 0.0317(7) 0.0274(7) 0.0262(7) 0.0331(8) C23 0.0170(4) 0.0125(4) 0.0135(4) 0.0022(3) 0.0022(3) 0.0072(3) C24 0.0228(5) 0.0133(4) 0.0187(5) 0.0027(3) -0.0021(4) 0.0073(4) C25 0.0214(5) 0.0130(4) 0.0213(5) 0.0016(3) 0.0006(4) 0.0059(4) C26 0.0154(4) 0.0170(4) 0.0162(4) 0.0005(3) 0.0023(3) 0.0053(3) C27 0.0226(5) 0.0190(4) 0.0165(4) 0.0029(3) -0.0012(4) 0.0094(4) C28 0.0202(4) 0.0150(4) 0.0164(4) 0.0037(3) 0.0016(3) 0.0089(4) C29 0.0221(5) 0.0229(5) 0.0212(5) -0.0026(4) -0.0020(4) 0.0054(4) N1 0.0219(4) 0.0295(5) 0.0182(4) -0.0027(4) 0.0064(3) 0.0085(4) O1 0.0449(6) 0.0406(6) 0.0241(4) 0.0085(4) 0.0190(4) 0.0189(5) O2 0.0318(5) 0.0394(5) 0.0295(5) -0.0035(4) 0.0115(4) 0.0193(4) P1 0.01569(10) 0.01057(9) 0.01194(10) 0.00208(8) 0.00247(8) 0.00656(8) Pt1 0.01624(3) 0.00966(2) 0.01178(3) 0.00241(1) 0.00383(2) 0.00653(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.2100(15) . ? C1 Pt1 1.9926(11) . ? C2 C3 1.4350(15) . ? C3 C4 1.4054(15) . ? C3 C8 1.4072(16) . ? C4 C5 1.3878(14) . ? C4 H4 0.9500 . ? C5 C6 1.3861(16) . ? C5 H5 0.9500 . ? C6 C7 1.3872(17) . ? C6 N1 1.4618(14) . ? C7 C8 1.3862(16) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.3977(15) . ? C9 C14 1.3999(14) . ? C9 P1 1.8138(10) . ? C10 C11 1.3937(16) . ? C10 H10 0.9500 . ? C11 C12 1.3947(18) . ? C11 H11 0.9500 . ? C12 C13 1.3917(18) . ? C12 C15 1.5120(17) . ? C13 C14 1.3938(15) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.3920(14) . ? C16 C21 1.3990(14) . ? C16 P1 1.8232(10) . ? C17 C18 1.3962(15) . ? C17 H17 0.9500 . ? C18 C19 1.3889(18) . ? C18 H18 0.9500 . ? C19 C20 1.3963(17) . ? C19 C22 1.5115(17) . ? C20 C21 1.3898(15) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C28 1.3940(13) . ? C23 C24 1.3998(14) . ? C23 P1 1.8101(10) . ? C24 C25 1.3877(15) . ?
C24 H24 0.9500 . ? C25 C26 1.3950(15) . ? C25 H25 0.9500 . ? C26 C27 1.3951(15) . ? C26 C29 1.5032(15) . ? C27 C28 1.3922(15) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? N1 O1 1.2283(16) . ? N1 O2 1.2320(15) . ? P1 Pt1 2.2964(2) . ? Pt1 C1 1.9926(11) 2 ? Pt1 P1 2.2964(2) 2 ? 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_3 _geom_angle_publ_flag C2 C1 Pt1 177.71(9) . . ? C1 C2 C3 177.96(12) . . ? C4 C3 C8 118.80(10) . . ? C4 C3 C2 120.96(10) . . ? C8 C3 C2 120.24(10) . . ? C5 C4 C3 120.86(10) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 118.58(10) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C5 C6 C7 122.30(10) . . ? C5 C6 N1 118.76(10) . . ? C7 C6 N1 118.92(10) . . ? C8 C7 C6 118.77(11) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C7 C8 C3 120.68(11) . . ? C7 C8 H8 119.7 . . ? C3 C8 H8 119.7 . . ? C10 C9 C14 118.87(10) . . ? C10 C9 P1 118.14(8) . . ? C14 C9 P1 122.94(8) . . ? C11 C10 C9 120.52(10) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 120.85(11) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 118.30(10) . . ? C13 C12 C15 120.14(12) . . ? C11 C12 C15 121.56(12) . . ?
C12 C13 C14 121.53(11) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C13 C14 C9 119.88(10) . . ? C13 C14 H14 120.1 . . ? C9 C14 H14 120.1 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 118.69(9) . . ? C17 C16 P1 123.04(8) . . ? C21 C16 P1 118.18(8) . . ? C16 C17 C18 120.31(10) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 121.30(11) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 118.12(10) . . ? C18 C19 C22 120.95(12) . . ? C20 C19 C22 120.94(12) . . ? C21 C20 C19 121.08(11) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C16 120.49(10) . . ? C20 C21 H21 119.8 . . ? C16 C21 H21 119.8 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 119.13(9) . . ? C28 C23 P1 120.73(7) . . ? C24 C23 P1 120.13(8) . . ? C25 C24 C23 120.40(10) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.85(10) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C27 118.39(10) . . ? C25 C26 C29 119.72(10) . . ? C27 C26 C29 121.89(10) . . ? C28 C27 C26 121.24(10) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C23 119.93(9) . . ? C27 C28 H28 120.0 . . ? C23 C28 H28 120.0 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 N1 O2 123.51(11) . . ? O1 N1 C6 118.38(10) . . ? O2 N1 C6 118.10(11) . . ? C23 P1 C9 106.11(5) . . ? C23 P1 C16 103.48(5) . . ? C9 P1 C16 105.65(5) . . ? C23 P1 Pt1 113.59(3) . . ? C9 P1 Pt1 111.01(3) . . ? C16 P1 Pt1 116.13(3) . . ? C1 Pt1 C1 180.00(6) . 2 ? C1 Pt1 P1 86.67(3) . . ? C1 Pt1 P1 93.33(3) 2 . ? C1 Pt1 P1 93.33(3) . 2 ? C1 Pt1 P1 86.67(3) 2 2 ? P1 Pt1 P1 180.000(13) . 2 ? 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 Pt1 C1 C2 C3 44(5) . . . . ? C1 C2 C3 C4 138(3) . . . . ? C1 C2 C3 C8 -42(3) . . . . ? C8 C3 C4 C5 0.43(16) . . . . ? C2 C3 C4 C5 -179.68(10) . . . . ? C3 C4 C5 C6 -0.03(16) . . . . ? C4 C5 C6 C7 -0.63(17) . . . . ? C4 C5 C6 N1 177.99(10) . . . . ? C5 C6 C7 C8 0.87(19) . . . . ? N1 C6 C7 C8 -177.75(11) . . . . ? C6 C7 C8 C3 -0.44(19) . . . . ? C4 C3 C8 C7 -0.19(18) . . . . ? C2 C3 C8 C7 179.92(12) . . . . ? C14 C9 C10 C11 2.70(15) . . . . ? P1 C9 C10 C11 -179.75(8) . . . . ? C9 C10 C11 C12 -2.02(17) . . . . ? C10 C11 C12 C13 -0.11(17) . . . . ? C10 C11 C12 C15 -179.95(12) . . . . ? C11 C12 C13 C14 1.52(17) . . . . ? C15 C12 C13 C14 -178.63(12) . . . . ? C12 C13 C14 C9 -0.81(17) . . . . ? C10 C9 C14 C13 -1.31(15) . . . . ? P1 C9 C14 C13 -178.73(8) . . . . ? C21 C16 C17 C18 0.76(16) . . . . ? P1 C16 C17 C18 -175.73(9) . . . . ? C16 C17 C18 C19 -0.52(18) . . . . ? C17 C18 C19 C20 -0.49(18) . . . . ?
C17 C18 C19 C22 179.65(13) . . . . ? C18 C19 C20 C21 1.26(18) . . . . ? C22 C19 C20 C21 -178.89(13) . . . . ? C19 C20 C21 C16 -1.03(17) . . . . ? C17 C16 C21 C20 0.00(15) . . . . ? P1 C16 C21 C20 176.66(8) . . . . ? C28 C23 C24 C25 -2.04(16) . . . . ? P1 C23 C24 C25 176.68(9) . . . . ? C23 C24 C25 C26 0.46(18) . . . . ? C24 C25 C26 C27 1.75(17) . . . . ? C24 C25 C26 C29 -177.78(11) . . . . ? C25 C26 C27 C28 -2.40(17) . . . . ? C29 C26 C27 C28 177.11(11) . . . . ? C26 C27 C28 C23 0.84(17) . . . . ? C24 C23 C28 C27 1.39(16) . . . . ? P1 C23 C28 C27 -177.32(8) . . . . ? C5 C6 N1 O1 -13.89(16) . . . . ? C7 C6 N1 O1 164.78(12) . . . . ? C5 C6 N1 O2 167.07(11) . . . . ? C7 C6 N1 O2 -14.25(16) . . . . ? C28 C23 P1 C9 111.54(9) . . . . ? C24 C23 P1 C9 -67.16(10) . . . . ? C28 C23 P1 C16 -137.48(9) . . . . ? C24 C23 P1 C16 43.82(10) . . . . ? C28 C23 P1 Pt1 -10.70(10) . . . . ? C24 C23 P1 Pt1 170.61(8) . . . . ? C10 C9 P1 C23 -177.78(8) . . . . ? C14 C9 P1 C23 -0.33(10) . . . . ? C10 C9 P1 C16 72.78(9) . . . . ? C14 C9 P1 C16 -109.78(9) . . . . ? C10 C9 P1 Pt1 -53.92(9) . . . . ? C14 C9 P1 Pt1 123.52(8) . . . . ? C17 C16 P1 C23 -128.88(9) . . . . ? C21 C16 P1 C23 54.62(9) . . . . ? C17 C16 P1 C9 -17.56(10) . . . . ? C21 C16 P1 C9 165.93(8) . . . . ? C17 C16 P1 Pt1 105.96(8) . . . . ? C21 C16 P1 Pt1 -70.55(8) . . . . ? C2 C1 Pt1 C1 -158(44) . . . 2 ? C2 C1 Pt1 P1 27(3) . . . . ? C2 C1 Pt1 P1 -153(3) . . . 2 ? C23 P1 Pt1 C1 69.80(5) . . . . ? C9 P1 Pt1 C1 -49.67(5) . . . . ? C16 P1 Pt1 C1 -170.36(5) . . . . ? C23 P1 Pt1 C1 -110.20(5) . . . 2 ? C9 P1 Pt1 C1 130.33(5) . . . 2 ? C16 P1 Pt1 C1 9.64(5) . . . 2 ? C23 P1 Pt1 P1 24.77(4) . . . 2 ? C9 P1 Pt1 P1 -94.71(4) . . . 2 ? C16 P1 Pt1 P1 144.60(4) . . . 2 ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 32.94 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.655 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.064
