# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1670 data_global # 1. SUBMISSION DETAILS _publ_contact_autor ; Prof. Daniela Belli Dell'Amico Universit di Pisa Dipartimento di Chimica e Chimica Industriale via del Risorgimento 35 56126 Pisa Italia ; _publ_contact_author_phone '+39 050 918206' _publ_contact_author_fax '+39 050 20237' _publ_contact_author_email belli@dcci.unipi.it _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Prof. D. Belli Dell'Amico Dipartimento di Chimica e Chimica Industriale Universita di Pisa Via del Risorgimento 35 I-56126 Pisa Italy e-mail: belli@dcci.unipi.it ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; N,N-diethylcarbamato tertiary phosphines complexes as precursors to carbonato and carbamoyl platinum(II) derivatives ; loop_ _publ_author_names _publ_author_address 'Abram, Ulrich' ; Forschungszentrum Rossendorf, Institute of Radiochemistry, c/o Dresden University of Technology, Institute od Analytical Chemistry, D-01062 Dresden, Germany ; ' Belli Dell'Amico, Daniela' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via del Risorgimento 35 I-56126 Pisa Italy ; ' Calderazzo, Fausto' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via del Risorgimento 35 I-56126 Pisa Italy ; ' Marchetti, Lorella' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via del Risorgimento 35 I-56126 Pisa Italy ; 'Straehle, Joachim' ; Institut fuer Anorganische Chemie Universitaet Tuebingen, Auf der Morgenstelle 18, D-72076 Tuebingen, Germany ; #======================================================================= data_ptpph3 _audit_creation_method SHELXL _chemical_name_systematic ; carbonato(O,O')bis(triphenylphophine)platinum(II) ; _chemical_name_common ? _chemical_formula_moiety '(PPh3)2Pt(CO3) * 2 CHCl3' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H32 Cl6 O3 P2 Pt' _chemical_formula_weight 1018.38 _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' '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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.310(16) _cell_length_b 12.889(18) _cell_length_c 14.930(14) _cell_angle_alpha 106.56(6) _cell_angle_beta 93.57(7) _cell_angle_gamma 116.98(6) _cell_volume 1971(4) _cell_formula_units_Z 2 _cell_measurement_temperature -70 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.27 _cell_measurement_theta_max 13.79 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method ? _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 4.083 _exptl_absorpt_correction_type 'DIFABS' _exptl_absorpt_correction_T_min 0.566 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type 'Mo k\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method 'omega/2 theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 9.9 _diffrn_reflns_number 8292 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 26.91 _reflns_number_total 7083 _reflns_number_observed 6719 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction 'CAD4 SDP' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SCHAKAL' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+4.8317P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refined _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7083 _refine_ls_number_parameters 587 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_obs 0.0258 _refine_ls_wR_factor_all 0.0693 _refine_ls_wR_factor_obs 0.0673 _refine_ls_goodness_of_fit_all 0.934 _refine_ls_goodness_of_fit_obs 0.934 _refine_ls_restrained_S_all 0.934 _refine_ls_restrained_S_obs 0.934 _refine_ls_shift/esd_max 0.087 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.023558(13) 0.489325(11) 0.257839(8) 0.01821(6) Uani 1 d . . P1 P 0.05828(10) 0.32814(8) 0.23723(6) 0.0205(2) Uani 1 d . . C11 C 0.0303(4) 0.2771(3) 0.3401(2) 0.0242(8) Uani 1 d . . C12 C -0.0074(4) 0.3378(4) 0.4127(3) 0.0304(9) Uani 1 d . . H12 H -0.0258(45) 0.3981(44) 0.4081(33) 0.034(12) Uiso 1 d . . C13 C -0.0234(5) 0.3066(4) 0.4949(3) 0.0388(11) Uani 1 d . . H13 H -0.0578(61) 0.3479(60) 0.5403(48) 0.074(20) Uiso 1 d . . C14 C -0.0008(5) 0.2158(4) 0.5055(3) 0.0403(11) Uani 1 d . . H14 H -0.0083(51) 0.1944(51) 0.5625(40) 0.053(15) Uiso 1 d . . C15 C 0.0352(5) 0.1529(5) 0.4332(4) 0.0444(12) Uani 1 d . . H15 H 0.0485(56) 0.0901(57) 0.4376(42) 0.062(17) Uiso 1 d . . C16 C 0.0501(5) 0.1833(4) 0.3509(3) 0.0381(11) Uani 1 d . . H16 H 0.0726(53) 0.1396(52) 0.3022(41) 0.055(16) Uiso 1 d . . C21 C 0.2054(4) 0.3369(3) 0.2166(3) 0.0230(8) Uani 1 d . . C22 C 0.2912(4) 0.3410(4) 0.2846(3) 0.0295(10) Uani 1 d . . H22 H 0.2687(49) 0.3396(48) 0.3429(39) 0.046(14) Uiso 1 d . . C23 C 0.4002(5) 0.3471(5) 0.2636(3) 0.0414(12) Uani 1 d . . H23 H 0.4610(54) 0.3481(49) 0.3056(40) 0.049(15) Uiso 1 d . . C24 C 0.4293(5) 0.3513(5) 0.1766(4) 0.0458(13) Uani 1 d . . H24 H 0.5065(61) 0.3552(54) 0.1671(42) 0.057(18) Uiso 1 d . . C25 C 0.3460(5) 0.3493(5) 0.1092(4) 0.0444(12) Uani 1 d . . H25 H 0.3631(69) 0.3594(68) 0.0452(55) 0.094(24) Uiso 1 d . . C26 C 0.2346(5) 0.3407(4) 0.1280(3) 0.0334(10) Uani 1 d . . H26 H 0.1699(47) 0.3338(44) 0.0791(35) 0.038(13) Uiso 1 d . . C31 C -0.0524(4) 0.2001(3) 0.1292(3) 0.0276(9) Uani 1 d . . C32 C -0.1180(5) 0.2203(4) 0.0650(3) 0.0421(12) Uani 1 d . . H32 H -0.1128(61) 0.2909(62) 0.0783(46) 0.071(20) Uiso 1 d . . C33 C -0.1949(5) 0.1261(5) -0.0207(3) 0.0492(14) Uani 1 d . . H33 H -0.2543(60) 0.1354(56) -0.0557(45) 0.066(18) Uiso 1 d . . C34 C -0.2101(6) 0.0115(5) -0.0415(4) 0.0547(15) Uani 1 d . . H34 H -0.2662(57) -0.0595(57) -0.0999(44) 0.066 Uiso 1 d . . C35 C -0.1480(11) -0.0104(6) 0.0219(6) 0.134(5) Uani 1 d . . H35 H -0.1219(100) -0.0679(102) -0.0051(75) 0.156(42) Uiso 1 d . . C36 C -0.0668(10) 0.0846(6) 0.1069(6) 0.114(4) Uani 1 d . . H36 H -0.0311(89) 0.0665(89) 0.1568(70) 0.139(35) Uiso 1 d . . P2 P 0.21952(9) 0.63574(8) 0.27285(6) 0.0209(2) Uani 1 d . . C41 C 0.3373(4) 0.6312(3) 0.3485(3) 0.0262(9) Uani 1 d . . C42 C 0.3078(5) 0.6069(4) 0.4324(3) 0.0314(10) Uani 1 d . . H42 H 0.2357(44) 0.5938(38) 0.4476(30) 0.020(11) Uiso 1 d . . C43 C 0.3935(5) 0.6068(4) 0.4967(3) 0.0396(12) Uani 1 d . . H43 H 0.3695(52) 0.5903(51) 0.5501(41) 0.053(15) Uiso 1 d . . C44 C 0.5082(5) 0.6285(4) 0.4761(3) 0.0438(13) Uani 1 d . . H44 H 0.5675(57) 0.6288(53) 0.5160(43) 0.059(17) Uiso 1 d . . C45 C 0.5374(5) 0.6494(5) 0.3931(4) 0.0431(12) Uani 1 d . . H45 H 0.6033(60) 0.6519(53) 0.3732(42) 0.051(18) Uiso 1 d . . C46 C 0.4518(4) 0.6517(4) 0.3289(3) 0.0356(11) Uani 1 d . . H46 H 0.4680(40) 0.6648(38) 0.2732(31) 0.023(10) Uiso 1 d . . C51 C 0.2627(4) 0.6422(3) 0.1592(3) 0.0246(8) Uani 1 d . . C52 C 0.1776(4) 0.5539(4) 0.0740(3) 0.0290(9) Uani 1 d . . H52 H 0.1038(42) 0.4917(40) 0.0720(29) 0.022(10) Uiso 1 d . . C53 C 0.2056(5) 0.5578(4) -0.0141(3) 0.0370(10) Uani 1 d . . H53 H 0.1434(50) 0.4989(49) -0.0743(39) 0.048(14) Uiso 1 d . . C54 C 0.3197(5) 0.6507(5) -0.0176(3) 0.0446(12) Uani 1 d . . H54 H 0.3476(49) 0.6544(47) -0.0735(39) 0.046(14) Uiso 1 d . . C55 C 0.4036(5) 0.7398(5) 0.0666(4) 0.0408(11) Uani 1 d . . H55 H 0.4856(52) 0.8022(50) 0.0655(37) 0.050(15) Uiso 1 d . . C56 C 0.3754(4) 0.7374(4) 0.1551(3) 0.0328(10) Uani 1 d . . H56 H 0.4306(48) 0.8047(47) 0.2181(37) 0.043(14) Uiso 1 d . . C61 C 0.2391(4) 0.7902(3) 0.3318(3) 0.0268(9) Uani 1 d . . C62 C 0.1759(4) 0.8305(4) 0.2828(3) 0.0356(10) Uani 1 d . . H62 H 0.1260(46) 0.7796(44) 0.2204(35) 0.038(13) Uiso 1 d . . C63 C 0.1885(5) 0.9467(4) 0.3244(4) 0.0462(13) Uani 1 d . . H63 H 0.1462(59) 0.9740(57) 0.2968(44) 0.064(19) Uiso 1 d . . C64 C 0.2620(5) 1.0231(4) 0.4154(4) 0.0501(14) Uani 1 d . . H64 H 0.2709(53) 1.0997(54) 0.4389(40) 0.054(16) Uiso 1 d . . C65 C 0.3233(5) 0.9831(4) 0.4653(4) 0.0455(12) Uani 1 d . . H65 H 0.3746(59) 1.0338(59) 0.5272(46) 0.069(19) Uiso 1 d . . C66 C 0.3119(5) 0.8668(4) 0.4237(3) 0.0352(10) Uani 1 d . . H66 H 0.3548(46) 0.8470(43) 0.4573(34) 0.033(13) Uiso 1 d . . O1 O -0.1630(3) 0.3949(2) 0.2589(2) 0.0298(6) Uani 1 d . . O2 O -0.0672(3) 0.5907(2) 0.2712(2) 0.0249(6) Uani 1 d . . C3 C -0.1760(5) 0.4955(4) 0.2710(3) 0.0320(11) Uani 1 d . . O3 O -0.2701(4) 0.4994(3) 0.2793(3) 0.0466(9) Uani 1 d . . C10 C 0.7939(6) 0.7305(5) 0.2079(4) 0.0468(13) Uani 1 d . . H10 H 0.8113(62) 0.6789(62) 0.2198(46) 0.068(20) Uiso 1 d . . Cl11 Cl 0.89872(14) 0.78329(14) 0.13420(11) 0.0609(4) Uani 1 d . . Cl12 Cl 0.8196(2) 0.8557(2) 0.30841(12) 0.0844(6) Uani 1 d . . Cl13 Cl 0.6404(2) 0.6486(2) 0.14272(12) 0.0814(6) Uani 1 d . . C20 C 0.6244(5) 0.1325(5) 0.2421(4) 0.057(2) Uani 1 d . . H20 H 0.6942(58) 0.2173(57) 0.2637(42) 0.063(17) Uiso 1 d . . Cl21 Cl 0.5580(2) 0.0909(2) 0.12231(12) 0.0861(6) Uani 1 d . . Cl22 Cl 0.5067(3) 0.1081(2) 0.3069(2) 0.1256(11) Uani 1 d . . Cl23 Cl 0.6922(2) 0.0424(2) 0.2530(2) 0.1129(9) Uani 1 d . . 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 Pt1 0.01774(11) 0.01961(7) 0.01842(7) 0.00699(5) 0.00430(5) 0.00990(6) P1 0.0220(6) 0.0219(4) 0.0191(4) 0.0062(3) 0.0046(3) 0.0125(4) C11 0.026(2) 0.026(2) 0.024(2) 0.0099(13) 0.0082(14) 0.014(2) C12 0.040(3) 0.033(2) 0.027(2) 0.012(2) 0.009(2) 0.023(2) C13 0.052(3) 0.047(2) 0.028(2) 0.017(2) 0.019(2) 0.029(2) C14 0.049(3) 0.045(2) 0.034(2) 0.023(2) 0.015(2) 0.023(2) C15 0.062(4) 0.044(2) 0.050(3) 0.030(2) 0.023(2) 0.034(2) C16 0.057(3) 0.037(2) 0.040(2) 0.021(2) 0.026(2) 0.032(2) C21 0.022(2) 0.026(2) 0.025(2) 0.0062(13) 0.0046(14) 0.016(2) C22 0.020(3) 0.041(2) 0.027(2) 0.006(2) 0.002(2) 0.019(2) C23 0.023(3) 0.058(3) 0.040(2) 0.004(2) -0.002(2) 0.026(2) C24 0.029(3) 0.055(3) 0.054(3) 0.010(2) 0.016(2) 0.027(2) C25 0.044(3) 0.060(3) 0.043(3) 0.022(2) 0.025(2) 0.033(3) C26 0.037(3) 0.044(2) 0.032(2) 0.016(2) 0.014(2) 0.028(2) C31 0.025(2) 0.025(2) 0.027(2) 0.0028(14) -0.0003(15) 0.012(2) C32 0.049(3) 0.032(2) 0.038(2) 0.006(2) -0.007(2) 0.019(2) C33 0.047(3) 0.056(3) 0.037(2) 0.004(2) -0.014(2) 0.029(3) C34 0.055(4) 0.044(3) 0.040(3) -0.008(2) -0.014(2) 0.022(2) C35 0.206(11) 0.049(4) 0.099(6) -0.039(4) -0.097(7) 0.078(6) C36 0.171(9) 0.046(3) 0.087(5) -0.027(3) -0.084(6) 0.067(5) P2 0.0218(6) 0.0213(4) 0.0190(4) 0.0072(3) 0.0045(3) 0.0101(4) C41 0.026(2) 0.025(2) 0.025(2) 0.0075(14) 0.0013(15) 0.012(2) C42 0.032(3) 0.034(2) 0.028(2) 0.010(2) 0.004(2) 0.016(2) C43 0.047(3) 0.043(2) 0.028(2) 0.010(2) -0.004(2) 0.024(2) C44 0.038(3) 0.042(2) 0.043(2) 0.009(2) -0.016(2) 0.019(2) C45 0.025(3) 0.047(3) 0.057(3) 0.019(2) 0.002(2) 0.018(2) C46 0.028(3) 0.038(2) 0.039(2) 0.016(2) 0.005(2) 0.013(2) C51 0.027(2) 0.029(2) 0.024(2) 0.0127(14) 0.0084(15) 0.017(2) C52 0.033(3) 0.030(2) 0.025(2) 0.0112(15) 0.008(2) 0.015(2) C53 0.049(3) 0.044(2) 0.024(2) 0.012(2) 0.009(2) 0.027(2) C54 0.060(4) 0.061(3) 0.036(2) 0.029(2) 0.029(2) 0.038(3) C55 0.033(3) 0.052(3) 0.052(3) 0.032(2) 0.022(2) 0.022(2) C56 0.029(2) 0.035(2) 0.036(2) 0.020(2) 0.009(2) 0.012(2) C61 0.025(2) 0.023(2) 0.029(2) 0.0087(14) 0.008(2) 0.010(2) C62 0.036(3) 0.029(2) 0.040(2) 0.009(2) 0.003(2) 0.016(2) C63 0.044(3) 0.032(2) 0.066(3) 0.015(2) 0.006(2) 0.023(2) C64 0.047(3) 0.024(2) 0.068(3) 0.003(2) 0.015(3) 0.016(2) C65 0.040(3) 0.032(2) 0.047(3) -0.003(2) 0.004(2) 0.014(2) C66 0.034(3) 0.032(2) 0.032(2) 0.004(2) 0.002(2) 0.016(2) O1 0.023(2) 0.0277(13) 0.042(2) 0.0149(11) 0.0096(12) 0.0128(12) O2 0.025(2) 0.0258(12) 0.0290(13) 0.0100(10) 0.0051(11) 0.0168(11) C3 0.042(3) 0.038(2) 0.027(2) 0.010(2) 0.009(2) 0.029(2) O3 0.030(2) 0.052(2) 0.071(2) 0.022(2) 0.016(2) 0.029(2) C10 0.062(4) 0.042(2) 0.046(3) 0.022(2) 0.010(2) 0.030(2) Cl11 0.0521(9) 0.0693(8) 0.0605(8) 0.0348(7) 0.0090(6) 0.0227(7) Cl12 0.123(2) 0.0589(9) 0.0636(9) 0.0068(7) 0.0138(10) 0.0479(10) Cl13 0.0496(10) 0.1148(14) 0.0570(9) 0.0297(9) 0.0119(7) 0.0228(9) C20 0.048(3) 0.039(3) 0.052(3) 0.016(2) 0.005(2) -0.002(2) Cl21 0.0989(14) 0.0708(10) 0.0586(9) 0.0254(8) -0.0009(9) 0.0186(9) Cl22 0.175(3) 0.0783(12) 0.135(2) 0.0429(13) 0.115(2) 0.0582(15) Cl23 0.0459(11) 0.0997(15) 0.186(3) 0.071(2) -0.0024(13) 0.0215(10) _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 Pt1 O2 2.050(3) . ? Pt1 O1 2.058(4) . ? Pt1 P2 2.234(3) . ? Pt1 P1 2.247(3) . ? Pt1 C3 2.512(7) . ? P1 C21 1.814(5) . ? P1 C31 1.830(5) . ? P1 C11 1.829(4) . ? C11 C12 1.382(6) . ? C11 C16 1.387(6) . ? C12 C13 1.396(6) . ? C13 C14 1.366(7) . ? C14 C15 1.379(7) . ? C15 C16 1.391(6) . ? C21 C22 1.390(6) . ? C21 C26 1.401(6) . ? C22 C23 1.370(7) . ? C23 C24 1.377(7) . ? C24 C25 1.378(8) . ? C25 C26 1.378(8) . ? C31 C32 1.370(6) . ? C31 C36 1.352(7) . ? C32 C33 1.389(6) . ? C33 C34 1.339(8) . ? C34 C35 1.347(9) . ? C35 C36 1.398(8) . ? P2 C41 1.815(5) . ? P2 C51 1.823(4) . ? P2 C61 1.826(5) . ? C41 C46 1.378(7) . ? C41 C42 1.405(6) . ? C42 C43 1.382(7) . ? C43 C44 1.382(8) . ? C44 C45 1.377(8) . ? C45 C46 1.395(7) . ? C51 C52 1.391(6) . ? C51 C56 1.395(6) . ? C52 C53 1.390(6) . ? C53 C54 1.388(7) . ? C54 C55 1.380(8) . ? C55 C56 1.391(6) . ? C61 C62 1.386(6) . ? C61 C66 1.391(6) . ? C62 C63 1.379(7) . ? C63 C64 1.382(8) . ? C64 C65 1.375(8) . ? C65 C66 1.385(7) . ? O1 C3 1.340(6) . ? O2 C3 1.344(6) . ? C3 O3 1.195(6) . ? C10 Cl13 1.734(7) . ? C10 Cl12 1.748(6) . ? C10 Cl11 1.773(6) . ? C20 Cl21 1.740(6) . ? C20 Cl23 1.744(7) . ? C20 Cl22 1.752(7) . ? 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 O2 Pt1 O1 64.47(15) . . ? O2 Pt1 P2 100.87(15) . . ? O1 Pt1 P2 164.74(9) . . ? O2 Pt1 P1 160.97(9) . . ? O1 Pt1 P1 96.58(13) . . ? P2 Pt1 P1 98.15(12) . . ? O2 Pt1 C3 32.28(13) . . ? O1 Pt1 C3 32.21(14) . . ? P2 Pt1 C3 132.93(13) . . ? P1 Pt1 C3 128.78(11) . . ? C21 P1 C31 101.6(2) . . ? C21 P1 C11 105.8(2) . . ? C31 P1 C11 108.6(2) . . ? C21 P1 Pt1 122.47(13) . . ? C31 P1 Pt1 108.4(2) . . ? C11 P1 Pt1 109.21(14) . . ? C12 C11 C16 118.0(4) . . ? C12 C11 P1 118.9(3) . . ? C16 C11 P1 123.0(3) . . ? C11 C12 C13 121.0(4) . . ? C14 C13 C12 120.3(4) . . ? C13 C14 C15 119.6(4) . . ? C14 C15 C16 120.1(4) . . ? C11 C16 C15 121.0(4) . . ? C22 C21 C26 118.2(4) . . ? C22 C21 P1 123.3(3) . . ? C26 C21 P1 118.4(3) . . ? C23 C22 C21 120.0(4) . . ? C22 C23 C24 121.8(5) . . ? C25 C24 C23 118.8(5) . . ? C26 C25 C24 120.4(5) . . ? C25 C26 C21 120.8(4) . . ? C32 C31 C36 117.6(4) . . ? C32 C31 P1 120.6(3) . . ? C36 C31 P1 121.6(4) . . ? C31 C32 C33 121.1(5) . . ? C34 C33 C32 120.8(5) . . ? C33 C34 C35 118.7(5) . . ? C34 C35 C36 121.2(6) . . ? C31 C36 C35 120.5(5) . . ? C41 P2 C51 110.0(2) . . ? C41 P2 C61 104.0(2) . . ? C51 P2 C61 103.0(2) . . ? C41 P2 Pt1 114.3(2) . . ? C51 P2 Pt1 114.2(2) . . ? C61 P2 Pt1 110.3(2) . . ? C46 C41 C42 119.5(4) . . ? C46 C41 P2 124.0(3) . . ? C42 C41 P2 116.5(4) . . ? C43 C42 C41 120.8(5) . . ? C44 C43 C42 118.8(5) . . ? C45 C44 C43 121.1(5) . . ? C44 C45 C46 120.1(6) . . ? C41 C46 C45 119.6(5) . . ? C52 C51 C56 119.0(4) . . ? C52 C51 P2 119.1(3) . . ? C56 C51 P2 121.8(3) . . ? C53 C52 C51 120.8(4) . . ? C54 C53 C52 119.8(4) . . ? C55 C54 C53 119.7(4) . . ? C54 C55 C56 120.8(4) . . ? C55 C56 C51 119.8(4) . . ? C62 C61 C66 119.2(4) . . ? C62 C61 P2 118.0(3) . . ? C66 C61 P2 122.8(3) . . ? C63 C62 C61 119.9(4) . . ? C64 C63 C62 120.7(5) . . ? C63 C64 C65 119.8(5) . . ? C64 C65 C66 119.9(5) . . ? C65 C66 C61 120.5(5) . . ? C3 O1 Pt1 92.9(3) . . ? C3 O2 Pt1 93.2(3) . . ? O3 C3 O1 125.2(4) . . ? O3 C3 O2 125.4(4) . . ? O1 C3 O2 109.4(4) . . ? O3 C3 Pt1 178.6(3) . . ? O1 C3 Pt1 54.9(2) . . ? O2 C3 Pt1 54.6(2) . . ? Cl13 C10 Cl12 111.9(4) . . ? Cl13 C10 Cl11 110.5(3) . . ? Cl12 C10 Cl11 110.2(3) . . ? Cl21 C20 Cl23 110.1(4) . . ? Cl21 C20 Cl22 108.6(4) . . ? Cl23 C20 Cl22 109.7(3) . . ? _refine_diff_density_max 1.201 _refine_diff_density_min -1.214 _refine_diff_density_rms 0.101 #===END data_Pt(PPh3)2ClCONEt2 _audit_creation_method SHELXL _chemical_name_systematic ; trans-chloro(N,N-diethylcarbamoyl)bis(triphenilphosphine)platinum(II) ; _chemical_name_common ? _chemical_formula_moiety 'trans- * 2 C7H8' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C55 H56 Cl N O P2 Pt' _chemical_formula_weight 1039.49 _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' '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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'O' 'O' 0.0106 0.0060 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.739(3) _cell_length_b 12.428(5) _cell_length_c 17.982(3) _cell_angle_alpha 96.75(2) _cell_angle_beta 91.82(2) _cell_angle_gamma 95.62(3) _cell_volume 2369.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.30 _cell_measurement_theta_max 12.68 _exptl_crystal_description cube _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method ? _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 3.124 _exptl_absorpt_correction_type 'PSI SCAN' _exptl_absorpt_correction_T_min 0.9317 _exptl_absorpt_correction_T_max 0.9999 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4' _diffrn_measurement_method 'omega/2 theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 2.1 _diffrn_reflns_number 11976 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 26.95 _reflns_number_total 10309 _reflns_number_observed 8657 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction 'CAD4 SDP' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SCHAKAL _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 190 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 'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+29.2847P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10119 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_obs 0.0499 _refine_ls_wR_factor_all 0.3845 _refine_ls_wR_factor_obs 0.1314 _refine_ls_goodness_of_fit_all 1.093 _refine_ls_goodness_of_fit_obs 0.979 _refine_ls_restrained_S_all 2.755 _refine_ls_restrained_S_obs 0.979 _refine_ls_shift/esd_max 0.008 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt Pt 0.22468(3) 0.17265(2) 0.21220(2) 0.01761(10) Uani 1 d . . Cl Cl 0.0436(2) 0.2538(2) 0.26189(12) 0.0314(4) Uani 1 d . . C10 C 0.3828(7) 0.1164(6) 0.1725(4) 0.0210(15) Uani 1 d . . O O 0.3815(5) 0.0325(5) 0.1314(4) 0.0297(13) Uani 1 d . . N N 0.4935(6) 0.1808(6) 0.1912(4) 0.031(2) Uani 1 d . . C20 C 0.6068(8) 0.1502(9) 0.1574(6) 0.041(2) Uani 1 d . . H20A H 0.6610(8) 0.2161(9) 0.1532(6) 0.049 Uiso 1 calc R . H20B H 0.5852(8) 0.1151(9) 0.1069(6) 0.049 Uiso 1 calc R . C30 C 0.5014(9) 0.2819(8) 0.2422(6) 0.042(2) Uani 1 d . . H30A H 0.4176(9) 0.3033(8) 0.2484(6) 0.051 Uiso 1 calc R . H30B H 0.5493(9) 0.3384(8) 0.2192(6) 0.051 Uiso 1 calc R . C50 C 0.5601(14) 0.2762(11) 0.3183(7) 0.069(4) Uani 1 d . . H50A H 0.5614(14) 0.3458(11) 0.3480(7) 0.103 Uiso 1 calc R . H50B H 0.6441(14) 0.2572(11) 0.3132(7) 0.103 Uiso 1 calc R . H50C H 0.5121(14) 0.2221(11) 0.3424(7) 0.103 Uiso 1 calc R . C40 C 0.6787(11) 0.0771(13) 0.1967(9) 0.074(5) Uani 1 d . . H40A H 0.7518(11) 0.0621(13) 0.1696(9) 0.111 Uiso 1 calc R . H40B H 0.6275(11) 0.0102(13) 0.1999(9) 0.111 Uiso 1 calc R . H40C H 0.7036(11) 0.1115(13) 0.2463(9) 0.111 Uiso 1 calc R . P1 P 0.2128(2) 0.26299(15) 0.10736(11) 0.0181(4) Uani 1 d . . C11 C 0.1922(7) 0.4064(6) 0.1248(4) 0.0216(15) Uani 1 d . . C12 C 0.2277(8) 0.4642(7) 0.1949(5) 0.030(2) Uani 1 d . . H12 H 0.2558(8) 0.4277(7) 0.2335(5) 0.036 Uiso 1 calc R . C13 C 0.2212(10) 0.5749(7) 0.2074(6) 0.039(2) Uani 1 d . . H13 H 0.2454(10) 0.6125(7) 0.2542(6) 0.046 Uiso 1 calc R . C14 C 0.1791(9) 0.6310(7) 0.1508(6) 0.036(2) Uani 1 d . . H14 H 0.1751(9) 0.7058(7) 0.1597(6) 0.043 Uiso 1 calc R . C15 C 0.1432(10) 0.5752(7) 0.0816(6) 0.039(2) Uani 1 d . . H15 H 0.1149(10) 0.6122(7) 0.0434(6) 0.047 Uiso 1 calc R . C16 C 0.1494(9) 0.4643(7) 0.0690(6) 0.036(2) Uani 1 d . . H16 H 0.1244(9) 0.4273(7) 0.0222(6) 0.043 Uiso 1 calc R . C21 C 0.3484(7) 0.2615(6) 0.0474(5) 0.024(2) Uani 1 d . . C22 C 0.4346(8) 0.3542(7) 0.0497(5) 0.031(2) Uani 1 d . . H22 H 0.4216(8) 0.4184(7) 0.0792(5) 0.037 Uiso 1 calc R . C23 C 0.5402(9) 0.3482(8) 0.0068(6) 0.041(2) Uani 1 d . . H23 H 0.5989(9) 0.4088(8) 0.0086(6) 0.049 Uiso 1 calc R . C24 C 0.5589(9) 0.2549(8) -0.0378(6) 0.040(2) Uani 1 d . . H24 H 0.6291(9) 0.2532(8) -0.0668(6) 0.048 Uiso 1 calc R . C25 C 0.4742(9) 0.1623(8) -0.0405(6) 0.037(2) Uani 1 d . . H25 H 0.4867(9) 0.0985(8) -0.0707(6) 0.044 Uiso 1 calc R . C26 C 0.3692(8) 0.1681(7) 0.0039(5) 0.030(2) Uani 1 d . . H26 H 0.3124(8) 0.1066(7) 0.0036(5) 0.036 Uiso 1 calc R . C31 C 0.0819(7) 0.2023(6) 0.0425(4) 0.0191(14) Uani 1 d . . C32 C 0.0853(8) 0.2066(7) -0.0350(5) 0.029(2) Uani 1 d . . H32 H 0.1547(8) 0.2410(7) -0.0554(5) 0.035 Uiso 1 calc R . C33 C -0.0146(9) 0.1597(7) -0.0801(6) 0.035(2) Uani 1 d . . H33 H -0.0120(9) 0.1606(7) -0.1317(6) 0.042 Uiso 1 calc R . C34 C -0.1193(9) 0.1109(8) -0.0504(6) 0.038(2) Uani 1 d . . H34 H -0.1867(9) 0.0793(8) -0.0820(6) 0.046 Uiso 1 calc R . C35 C -0.1244(10) 0.1089(10) 0.0243(6) 0.050(3) Uani 1 d . . H35 H -0.1964(10) 0.0775(10) 0.0439(6) 0.059 Uiso 1 calc R . C36 C -0.0238(9) 0.1529(8) 0.0724(6) 0.038(2) Uani 1 d . . H36 H -0.0271(9) 0.1494(8) 0.1236(6) 0.045 Uiso 1 calc R . P2 P 0.2236(2) 0.0616(2) 0.30655(11) 0.0191(4) Uani 1 d . . C41 C 0.3591(7) -0.0138(6) 0.3185(5) 0.025(2) Uani 1 d . . C42 C 0.4381(8) 0.0057(8) 0.3824(5) 0.035(2) Uani 1 d . . H42 H 0.4233(8) 0.0597(8) 0.4205(5) 0.042 Uiso 1 calc R . C43 C 0.5390(9) -0.0547(9) 0.3897(6) 0.043(2) Uani 1 d . . H43 H 0.5910(9) -0.0417(9) 0.4328(6) 0.051 Uiso 1 calc R . C44 C 0.5617(9) -0.1340(10) 0.3330(7) 0.047(3) Uani 1 d . . H44 H 0.6291(9) -0.1746(10) 0.3380(7) 0.056 Uiso 1 calc R . C45 C 0.4852(9) -0.1535(8) 0.2688(6) 0.039(2) Uani 1 d . . H45 H 0.5007(9) -0.2073(8) 0.2308(6) 0.047 Uiso 1 calc R . C46 C 0.3848(8) -0.0925(7) 0.2613(5) 0.030(2) Uani 1 d . . H46 H 0.3343(8) -0.1045(7) 0.2176(5) 0.036 Uiso 1 calc R . C51 C 0.0940(7) -0.0474(6) 0.2945(4) 0.024(2) Uani 1 d . . C52 C 0.1094(8) -0.1515(7) 0.3120(5) 0.030(2) Uani 1 d . . H52 H 0.1860(8) -0.1668(7) 0.3315(5) 0.036 Uiso 1 calc R . C53 C 0.0089(9) -0.2331(7) 0.3001(5) 0.034(2) Uani 1 d . . H53 H 0.0193(9) -0.3029(7) 0.3114(5) 0.040 Uiso 1 calc R . C54 C -0.1044(8) -0.2110(7) 0.2718(5) 0.034(2) Uani 1 d . . H54 H -0.1701(8) -0.2661(7) 0.2632(5) 0.040 Uiso 1 calc R . C55 C -0.1216(8) -0.1066(8) 0.2561(5) 0.034(2) Uani 1 d . . H55 H -0.1991(8) -0.0914(8) 0.2378(5) 0.041 Uiso 1 calc R . C56 C -0.0223(8) -0.0247(7) 0.2678(5) 0.028(2) Uani 1 d . . H56 H -0.0338(8) 0.0454(7) 0.2576(5) 0.034 Uiso 1 calc R . C61 C 0.2073(7) 0.1313(6) 0.4004(4) 0.023(2) Uani 1 d . . C62 C 0.1627(8) 0.0750(7) 0.4579(5) 0.029(2) Uani 1 d . . H62 H 0.1365(8) 0.0009(7) 0.4484(5) 0.034 Uiso 1 calc R . C63 C 0.1571(9) 0.1287(8) 0.5291(5) 0.034(2) Uani 1 d . . H63 H 0.1265(9) 0.0906(8) 0.5673(5) 0.041 Uiso 1 calc R . C64 C 0.1964(9) 0.2384(8) 0.5442(5) 0.037(2) Uani 1 d . . H64 H 0.1925(9) 0.2744(8) 0.5923(5) 0.044 Uiso 1 calc R . C65 C 0.2420(10) 0.2948(8) 0.4864(6) 0.042(2) Uani 1 d . . H65 H 0.2703(10) 0.3684(8) 0.4962(6) 0.051 Uiso 1 calc R . C66 C 0.2452(9) 0.2419(7) 0.4153(5) 0.032(2) Uani 1 d . . H66 H 0.2730(9) 0.2806(7) 0.3767(5) 0.039 Uiso 1 calc R . C91 C 0.7836(11) 0.5013(9) 0.2804(8) 0.055(3) Uani 1 d . . C92 C 0.8257(20) 0.4915(11) 0.2124(8) 0.085(5) Uani 1 d . . H92 H 0.9006(20) 0.4597(11) 0.2103(8) 0.101 Uiso 1 calc R . C93 C 0.7900(30) 0.5144(24) 0.1502(13) 0.161(14) Uani 1 d . . H93 H 0.8324(30) 0.5036(24) 0.1061(13) 0.193 Uiso 1 calc R . C94 C 0.6727(25) 0.5603(16) 0.1578(17) 0.133(11) Uani 1 d . . H94 H 0.6351(25) 0.5802(16) 0.1148(17) 0.159 Uiso 1 calc R . C95 C 0.6068(16) 0.5785(11) 0.2286(17) 0.109(9) Uani 1 d . . H95 H 0.5310(16) 0.6086(11) 0.2312(17) 0.131 Uiso 1 calc R . C96 C 0.6664(13) 0.5474(9) 0.2897(11) 0.077(5) Uani 1 d . . H96 H 0.6318(13) 0.5560(9) 0.3365(11) 0.093 Uiso 1 calc R . C97 C 0.8397(7) 0.4746(6) 0.3474(4) 0.098(6) Uani 1 d . . H97A H 0.7866(7) 0.4908(6) 0.3883(4) 0.147 Uiso 1 calc R . H97B H 0.9197(7) 0.5165(6) 0.3573(4) 0.147 Uiso 1 calc R . H97C H 0.8508(7) 0.3984(6) 0.3419(4) 0.147 Uiso 1 calc R . C01 C 0.2020(7) 0.7219(6) 0.5072(4) 0.071(4) Uani 1 d R . C02 C 0.1377(7) 0.6219(6) 0.4599(4) 0.095(6) Uani 1 d R . H02 H 0.0512(7) 0.6084(6) 0.4616(4) 0.114 Uiso 1 calc R . C06 C 0.3301(7) 0.7419(6) 0.4873(4) 0.083(5) Uani 1 d R . H06 H 0.3752(7) 0.8088(6) 0.5033(4) 0.100 Uiso 1 calc R . C07 C 0.1471(7) 0.8019(6) 0.5594(4) 0.091(5) Uani 1 d R . H07A H 0.0616(7) 0.7763(6) 0.5667(4) 0.137 Uiso 1 calc R . H07B H 0.1502(7) 0.8701(6) 0.5392(4) 0.137 Uiso 1 calc R . H07C H 0.1936(7) 0.8116(6) 0.6066(4) 0.137 Uiso 1 calc R . C04 C 0.3181(7) 0.5619(6) 0.4065(4) 0.100(6) Uani 1 d R . H04 H 0.3532(7) 0.5071(6) 0.3769(4) 0.120 Uiso 1 calc R . C03 C 0.1893(7) 0.5619(6) 0.4222(4) 0.118(9) Uani 1 d R . H03 H 0.1381(7) 0.5029(6) 0.3976(4) 0.142 Uiso 1 calc R . C05 C 0.3866(7) 0.6619(6) 0.4444(4) 0.112(7) Uani 1 d R . H05 H 0.4728(7) 0.6723(6) 0.4395(4) 0.135 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.01922(15) 0.01634(14) 0.01841(15) 0.00666(9) 0.00168(9) 0.00180(9) Cl 0.0346(11) 0.0338(10) 0.0304(10) 0.0112(8) 0.0116(8) 0.0143(8) C10 0.027(4) 0.021(4) 0.016(3) 0.008(3) -0.002(3) 0.004(3) O 0.027(3) 0.025(3) 0.038(3) 0.005(3) 0.004(2) 0.005(2) N 0.020(3) 0.031(4) 0.042(4) 0.015(3) 0.001(3) -0.001(3) C20 0.020(4) 0.052(6) 0.054(6) 0.022(5) 0.004(4) -0.001(4) C30 0.033(5) 0.028(5) 0.061(7) 0.007(4) -0.016(5) -0.014(4) C50 0.086(10) 0.057(7) 0.056(8) 0.019(6) -0.025(7) -0.028(7) C40 0.037(6) 0.106(11) 0.097(11) 0.060(9) 0.015(6) 0.032(7) P1 0.0194(9) 0.0157(8) 0.0203(9) 0.0075(7) 0.0010(7) 0.0006(7) C11 0.024(4) 0.016(3) 0.025(4) 0.004(3) 0.004(3) 0.001(3) C12 0.039(5) 0.020(4) 0.032(5) 0.007(3) 0.001(4) 0.006(3) C13 0.051(6) 0.026(4) 0.038(5) -0.001(4) -0.003(4) 0.006(4) C14 0.040(5) 0.017(4) 0.053(6) 0.005(4) 0.008(4) 0.008(3) C15 0.048(6) 0.027(4) 0.045(6) 0.015(4) -0.002(4) 0.008(4) C16 0.042(5) 0.018(4) 0.047(6) 0.009(4) -0.005(4) 0.003(4) C21 0.019(4) 0.025(4) 0.031(4) 0.013(3) 0.002(3) -0.001(3) C22 0.030(4) 0.020(4) 0.043(5) 0.006(3) 0.011(4) -0.004(3) C23 0.036(5) 0.039(5) 0.047(6) 0.015(4) 0.013(4) -0.009(4) C24 0.031(5) 0.048(6) 0.046(6) 0.017(5) 0.021(4) 0.007(4) C25 0.035(5) 0.036(5) 0.040(5) 0.004(4) 0.013(4) 0.008(4) C26 0.030(4) 0.023(4) 0.038(5) 0.008(3) 0.007(4) -0.002(3) C31 0.024(4) 0.019(3) 0.015(3) 0.008(3) -0.001(3) 0.000(3) C32 0.026(4) 0.030(4) 0.033(5) 0.011(3) 0.003(3) 0.002(3) C33 0.036(5) 0.030(4) 0.039(5) 0.003(4) -0.004(4) 0.004(4) C34 0.034(5) 0.036(5) 0.044(6) 0.007(4) -0.013(4) -0.002(4) C35 0.032(5) 0.070(7) 0.044(6) 0.016(5) -0.003(4) -0.019(5) C36 0.029(4) 0.045(5) 0.037(5) 0.009(4) -0.004(4) -0.008(4) P2 0.0207(9) 0.0190(9) 0.0186(9) 0.0074(7) 0.0004(7) 0.0010(7) C41 0.020(4) 0.026(4) 0.031(4) 0.016(3) 0.004(3) 0.002(3) C42 0.028(4) 0.044(5) 0.035(5) 0.015(4) -0.001(4) 0.005(4) C43 0.027(5) 0.059(6) 0.046(6) 0.023(5) -0.006(4) 0.005(4) C44 0.031(5) 0.063(7) 0.058(7) 0.040(6) 0.010(5) 0.022(5) C45 0.037(5) 0.034(5) 0.051(6) 0.018(4) 0.015(4) 0.014(4) C46 0.031(4) 0.025(4) 0.037(5) 0.014(3) 0.003(4) 0.006(3) C51 0.027(4) 0.021(4) 0.024(4) 0.004(3) 0.002(3) -0.001(3) C52 0.025(4) 0.025(4) 0.042(5) 0.017(4) 0.004(3) -0.004(3) C53 0.040(5) 0.023(4) 0.040(5) 0.013(4) 0.013(4) -0.003(4) C54 0.032(4) 0.026(4) 0.041(5) 0.004(4) 0.010(4) -0.011(3) C55 0.022(4) 0.042(5) 0.038(5) 0.011(4) -0.004(4) -0.004(4) C56 0.025(4) 0.028(4) 0.035(5) 0.013(3) 0.003(3) 0.000(3) C61 0.023(4) 0.024(4) 0.022(4) 0.003(3) 0.000(3) 0.002(3) C62 0.034(4) 0.030(4) 0.021(4) 0.008(3) 0.005(3) -0.003(3) C63 0.040(5) 0.043(5) 0.019(4) 0.007(4) 0.007(3) -0.003(4) C64 0.039(5) 0.041(5) 0.027(5) -0.003(4) -0.005(4) 0.004(4) C65 0.058(6) 0.027(5) 0.038(5) -0.000(4) 0.005(5) -0.008(4) C66 0.047(5) 0.027(4) 0.023(4) 0.008(3) 0.004(4) -0.003(4) C91 0.049(6) 0.034(5) 0.076(9) 0.014(5) -0.024(6) -0.018(5) C92 0.153(17) 0.053(8) 0.045(8) -0.001(6) 0.034(9) -0.002(9) C93 0.198(29) 0.181(26) 0.078(14) 0.041(15) -0.061(17) -0.115(23) C94 0.117(18) 0.069(12) 0.194(28) -0.009(14) -0.107(20) -0.014(12) C95 0.059(9) 0.025(6) 0.233(27) -0.003(11) -0.046(13) -0.003(6) C96 0.058(8) 0.022(5) 0.146(15) 0.003(7) -0.007(9) -0.013(5) C97 0.134(16) 0.056(9) 0.098(13) 0.018(9) -0.023(12) -0.017(9) C01 0.068(9) 0.095(11) 0.056(8) 0.047(8) -0.012(7) -0.002(8) C02 0.075(11) 0.108(15) 0.104(14) 0.056(12) -0.038(10) -0.014(10) C06 0.084(11) 0.094(12) 0.068(10) 0.018(9) 0.012(8) -0.021(9) C07 0.086(12) 0.121(15) 0.080(11) 0.041(11) 0.003(9) 0.034(11) C04 0.122(16) 0.074(11) 0.105(15) 0.015(10) -0.007(12) 0.014(11) C03 0.093(15) 0.103(16) 0.166(24) 0.066(16) -0.038(15) 0.003(12) C05 0.102(15) 0.143(19) 0.090(14) 0.045(13) 0.002(11) -0.032(13) _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 Pt C10 2.018(8) . ? Pt P2 2.309(2) . ? Pt P1 2.311(2) . ? Pt Cl 2.425(2) . ? C10 O 1.204(10) . ? C10 N 1.375(10) . ? N C20 1.442(12) . ? N C30 1.460(12) . ? C20 C40 1.474(14) . ? C30 C50 1.50(2) . ? P1 C11 1.809(8) . ? P1 C21 1.840(8) . ? P1 C31 1.841(8) . ? C11 C16 1.393(12) . ? C11 C12 1.398(12) . ? C12 C13 1.376(12) . ? C13 C14 1.387(14) . ? C14 C15 1.376(14) . ? C15 C16 1.378(12) . ? C21 C26 1.363(12) . ? C21 C22 1.400(11) . ? C22 C23 1.395(13) . ? C23 C24 1.367(14) . ? C24 C25 1.390(14) . ? C25 C26 1.405(12) . ? C31 C36 1.390(12) . ? C31 C32 1.404(11) . ? C32 C33 1.363(12) . ? C33 C34 1.378(14) . ? C34 C35 1.350(15) . ? C35 C36 1.388(13) . ? P2 C41 1.826(8) . ? P2 C61 1.826(8) . ? P2 C51 1.834(8) . ? C41 C46 1.386(12) . ? C41 C42 1.390(12) . ? C42 C43 1.389(13) . ? C43 C44 1.38(2) . ? C44 C45 1.38(2) . ? C45 C46 1.390(12) . ? C51 C56 1.390(11) . ? C51 C52 1.391(11) . ? C52 C53 1.399(12) . ? C53 C54 1.368(13) . ? C54 C55 1.389(13) . ? C55 C56 1.392(12) . ? C61 C66 1.387(11) . ? C61 C62 1.388(11) . ? C62 C63 1.377(12) . ? C63 C64 1.380(13) . ? C64 C65 1.394(14) . ? C65 C66 1.370(13) . ? C91 C92 1.31(2) . ? C91 C97 1.418(13) . ? C91 C96 1.44(2) . ? C92 C93 1.24(3) . ? C93 C94 1.44(4) . ? C94 C95 1.48(3) . ? C95 C96 1.37(3) . ? C01 C06 1.44 . ? C01 C07 1.47 . ? C01 C02 1.51 . ? C02 C03 1.14 . ? C06 C05 1.39 . ? C04 C03 1.42 . ? C04 C05 1.46 . ? 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 C10 Pt P2 91.3(2) . . ? C10 Pt P1 87.7(2) . . ? P2 Pt P1 172.11(7) . . ? C10 Pt Cl 175.6(2) . . ? P2 Pt Cl 90.68(7) . . ? P1 Pt Cl 90.88(7) . . ? O C10 N 120.4(7) . . ? O C10 Pt 122.3(6) . . ? N C10 Pt 117.3(6) . . ? C10 N C20 119.3(8) . . ? C10 N C30 122.9(7) . . ? C20 N C30 117.8(8) . . ? N C20 C40 116.4(9) . . ? N C30 C50 115.1(9) . . ? C11 P1 C21 102.9(4) . . ? C11 P1 C31 105.5(3) . . ? C21 P1 C31 103.1(4) . . ? C11 P1 Pt 115.9(3) . . ? C21 P1 Pt 116.4(3) . . ? C31 P1 Pt 111.7(2) . . ? C16 C11 C12 117.8(7) . . ? C16 C11 P1 122.3(6) . . ? C12 C11 P1 119.8(6) . . ? C13 C12 C11 120.5(8) . . ? C12 C13 C14 120.7(9) . . ? C15 C14 C13 119.6(8) . . ? C14 C15 C16 119.8(9) . . ? C15 C16 C11 121.6(9) . . ? C26 C21 C22 119.8(8) . . ? C26 C21 P1 119.9(6) . . ? C22 C21 P1 120.2(6) . . ? C23 C22 C21 118.7(8) . . ? C24 C23 C22 121.1(8) . . ? C23 C24 C25 120.8(8) . . ? C24 C25 C26 117.9(9) . . ? C21 C26 C25 121.8(8) . . ? C36 C31 C32 119.8(7) . . ? C36 C31 P1 118.3(6) . . ? C32 C31 P1 121.9(6) . . ? C33 C32 C31 119.1(8) . . ? C32 C33 C34 121.0(9) . . ? C35 C34 C33 120.1(9) . . ? C34 C35 C36 121.0(9) . . ? C35 C36 C31 118.9(9) . . ? C41 P2 C61 103.1(4) . . ? C41 P2 C51 102.2(4) . . ? C61 P2 C51 104.5(4) . . ? C41 P2 Pt 118.0(3) . . ? C61 P2 Pt 114.6(3) . . ? C51 P2 Pt 112.7(3) . . ? C46 C41 C42 118.9(8) . . ? C46 C41 P2 118.8(6) . . ? C42 C41 P2 122.3(7) . . ? C43 C42 C41 120.5(9) . . ? C44 C43 C42 119.8(9) . . ? C43 C44 C45 120.5(9) . . ? C44 C45 C46 119.7(10) . . ? C41 C46 C45 120.6(9) . . ? C56 C51 C52 119.5(7) . . ? C56 C51 P2 119.0(6) . . ? C52 C51 P2 121.5(6) . . ? C51 C52 C53 119.7(8) . . ? C54 C53 C52 120.5(8) . . ? C53 C54 C55 120.2(8) . . ? C54 C55 C56 119.7(8) . . ? C51 C56 C55 120.3(8) . . ? C66 C61 C62 119.3(8) . . ? C66 C61 P2 119.4(6) . . ? C62 C61 P2 121.3(6) . . ? C63 C62 C61 120.0(8) . . ? C62 C63 C64 120.7(8) . . ? C63 C64 C65 119.2(9) . . ? C66 C65 C64 120.2(9) . . ? C65 C66 C61 120.6(8) . . ? C92 C91 C97 128.6(14) . . ? C92 C91 C96 116.7(15) . . ? C97 C91 C96 114.7(13) . . ? C93 C92 C91 135.7(26) . . ? C92 C93 C94 108.8(28) . . ? C93 C94 C95 125.2(21) . . ? C96 C95 C94 114.7(16) . . ? C95 C96 C91 119.0(18) . . ? C06 C01 C07 120.0 . . ? C06 C01 C02 110.7 . . ? C07 C01 C02 128.8 . . ? C03 C02 C01 123.8 . . ? C05 C06 C01 120.3 . . ? C03 C04 C05 108.9 . . ? C02 C03 C04 131.1 . . ? C06 C05 C04 123.5 . . ? _refine_diff_density_max 3.636 _refine_diff_density_min -4.095 _refine_diff_density_rms 0.230 #===END