# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Pombeiro, Armando' 'Bokach, Nadezhda A.' 'Galanski, Mathea S.' 'Garnovskii, Dmitrii A.' 'Haukka, Matti' 'Keppler, Bernhard K.' 'Kukushkin, Vadim Yu.' 'Makarycheva-Mikhailova, Anastassiya V.' _publ_contact_author_name 'Prof Armando Pombeiro' _publ_contact_author_address ; Complexo I Instituto Superior Tecnico Centro de Quimica Estrutural Av. Rovisco Pais Lisbon 1049-001 PORTUGAL ; _publ_contact_author_email 'POMBEIRO@IST.UTL.PT' _publ_section_title ; Platinum(IV)-mediated Coupling of Dione Monoximes and Nitriles: a Novel Reactivity Pattern of the Classic Oxime-based Chelating Ligands ; data_trans_[PtCl4{NH=C(Me)ON=C(Me)C(Me)(O)}2] _database_code_CSD 186192 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'trans_[PtCl4{NH=C(Me)ON=C(Me)C(Me)(O)}2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H20 Cl4 N4 O4 Pt' _chemical_formula_weight 621.21 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' 'Cl' 'Cl' 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.1415(2) _cell_length_b 15.0031(4) _cell_length_c 11.3715(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.215(2) _cell_angle_gamma 90.00 _cell_volume 1027.78(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 7.369 _exptl_absorpt_correction_type 'Semi-empirical (Xprep in Shelxtl 5.1)' _exptl_absorpt_correction_T_min 0.2159 _exptl_absorpt_correction_T_max 0.3204 _exptl_absorpt_process_details 'based on equivalent reflections' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method 'CCD' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13112 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2232 _reflns_number_gt 2069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1999)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _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^)+(0.0155P)^2^+0.7910P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2232 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0173 _refine_ls_R_factor_gt 0.0157 _refine_ls_wR_factor_ref 0.0398 _refine_ls_wR_factor_gt 0.0389 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 Pt1 Pt 0.0000 0.0000 0.0000 0.01709(6) Uani 1 2 d S . . Cl1 Cl 0.15786(10) 0.01910(4) -0.16751(6) 0.02838(12) Uani 1 1 d . . . Cl2 Cl 0.21649(10) -0.12599(4) 0.05123(6) 0.02942(13) Uani 1 1 d . . . N1 N 0.2345(3) 0.08474(13) 0.08420(18) 0.0224(4) Uani 1 1 d . . . C1 C 0.3583(3) 0.08773(14) 0.18746(19) 0.0214(4) Uani 1 1 d . . . C2 C 0.3750(4) 0.02131(18) 0.2852(2) 0.0257(5) Uani 1 1 d . . . O1 O 0.4995(2) 0.15670(10) 0.22123(14) 0.0250(3) Uani 1 1 d . . . N2 N 0.4623(3) 0.22870(12) 0.13670(17) 0.0242(4) Uani 1 1 d . . . C4 C 0.6381(4) 0.27551(14) 0.1434(2) 0.0247(5) Uani 1 1 d . . . C5 C 0.8607(4) 0.25968(19) 0.2193(3) 0.0334(5) Uani 1 1 d . . . C6 C 0.6069(4) 0.35351(15) 0.0566(2) 0.0303(5) Uani 1 1 d . . . C7 C 0.3768(5) 0.37871(19) -0.0037(3) 0.0385(6) Uani 1 1 d . . . O2 O 0.7695(3) 0.39284(13) 0.04103(18) 0.0423(5) Uani 1 1 d . . . H1 H 0.248(4) 0.1276(17) 0.043(2) 0.013(6) Uiso 1 1 d . . . H2A H 0.320(5) 0.048(2) 0.351(3) 0.046(8) Uiso 1 1 d . . . H2B H 0.524(8) 0.0084(19) 0.324(4) 0.053(12) Uiso 1 1 d . . . H2C H 0.295(6) -0.033(3) 0.259(3) 0.050(9) Uiso 1 1 d . . . H5A H 0.863(5) 0.292(2) 0.287(3) 0.042(8) Uiso 1 1 d . . . H5B H 0.971(6) 0.284(2) 0.180(3) 0.063(10) Uiso 1 1 d . . . H5C H 0.884(5) 0.199(2) 0.235(3) 0.047(9) Uiso 1 1 d . . . H7A H 0.281(6) 0.321(2) -0.032(3) 0.061(10) Uiso 1 1 d . . . H7B H 0.299(6) 0.401(3) 0.052(4) 0.073(12) Uiso 1 1 d . . . H7C H 0.388(6) 0.419(3) -0.058(3) 0.061(10) Uiso 1 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 0.01515(8) 0.01658(8) 0.01886(9) -0.00059(3) 0.00163(5) -0.00164(3) Cl1 0.0243(3) 0.0388(3) 0.0233(3) -0.0005(2) 0.0077(2) -0.0055(2) Cl2 0.0297(3) 0.0229(3) 0.0321(3) -0.0027(2) -0.0031(2) 0.0061(2) N1 0.0223(9) 0.0201(9) 0.0242(10) 0.0012(7) 0.0033(7) -0.0033(7) C1 0.0177(10) 0.0208(10) 0.0253(12) -0.0024(8) 0.0030(8) -0.0012(8) C2 0.0271(13) 0.0260(11) 0.0231(13) 0.0017(10) 0.0028(10) -0.0035(10) O1 0.0244(8) 0.0214(7) 0.0265(8) 0.0006(6) -0.0020(6) -0.0054(6) N2 0.0269(10) 0.0184(9) 0.0258(10) 0.0001(7) 0.0010(7) -0.0010(7) C4 0.0275(11) 0.0221(10) 0.0233(12) -0.0037(8) 0.0024(9) -0.0045(9) C5 0.0280(13) 0.0319(14) 0.0370(15) 0.0006(11) -0.0018(10) -0.0076(10) C6 0.0438(15) 0.0207(11) 0.0243(13) -0.0037(9) 0.0015(10) -0.0062(10) C7 0.0458(17) 0.0275(14) 0.0387(17) 0.0034(11) -0.0005(13) 0.0026(12) O2 0.0481(12) 0.0360(10) 0.0409(11) 0.0059(8) 0.0043(9) -0.0164(9) _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 N1 2.0175(18) 3 ? Pt1 N1 2.0175(18) . ? Pt1 Cl1 2.3170(6) . ? Pt1 Cl1 2.3170(6) 3 ? Pt1 Cl2 2.3193(6) 3 ? Pt1 Cl2 2.3193(6) . ? N1 C1 1.270(3) . ? N1 H1 0.81(3) . ? C1 O1 1.356(2) . ? C1 C2 1.482(3) . ? C2 H2A 0.97(3) . ? C2 H2B 0.96(5) . ? C2 H2C 0.96(4) . ? O1 N2 1.434(2) . ? N2 C4 1.277(3) . ? C4 C5 1.488(3) . ? C4 C6 1.519(3) . ? C5 H5A 0.91(3) . ? C5 H5B 0.95(4) . ? C5 H5C 0.93(3) . ? C6 O2 1.202(3) . ? C6 C7 1.494(4) . ? C7 H7A 1.06(4) . ? C7 H7B 0.93(4) . ? C7 H7C 0.88(4) . ? 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 N1 Pt1 N1 180.00(13) 3 . ? N1 Pt1 Cl1 93.55(6) 3 . ? N1 Pt1 Cl1 86.45(6) . . ? N1 Pt1 Cl1 86.45(6) 3 3 ? N1 Pt1 Cl1 93.55(6) . 3 ? Cl1 Pt1 Cl1 180.00(4) . 3 ? N1 Pt1 Cl2 94.18(6) 3 3 ? N1 Pt1 Cl2 85.82(6) . 3 ? Cl1 Pt1 Cl2 90.22(2) . 3 ? Cl1 Pt1 Cl2 89.78(2) 3 3 ? N1 Pt1 Cl2 85.82(6) 3 . ? N1 Pt1 Cl2 94.18(6) . . ? Cl1 Pt1 Cl2 89.78(2) . . ? Cl1 Pt1 Cl2 90.22(2) 3 . ? Cl2 Pt1 Cl2 180.00(3) 3 . ? C1 N1 Pt1 134.84(17) . . ? C1 N1 H1 113.4(18) . . ? Pt1 N1 H1 111.7(18) . . ? N1 C1 O1 121.6(2) . . ? N1 C1 C2 127.7(2) . . ? O1 C1 C2 110.70(18) . . ? C1 C2 H2A 108.5(19) . . ? C1 C2 H2B 114(2) . . ? H2A C2 H2B 100(3) . . ? C1 C2 H2C 112(2) . . ? H2A C2 H2C 111(3) . . ? H2B C2 H2C 111(3) . . ? C1 O1 N2 112.04(15) . . ? C4 N2 O1 110.60(17) . . ? N2 C4 C5 128.1(2) . . ? N2 C4 C6 112.8(2) . . ? C5 C4 C6 119.0(2) . . ? C4 C5 H5A 105.5(19) . . ? C4 C5 H5B 109(2) . . ? H5A C5 H5B 108(3) . . ? C4 C5 H5C 110.9(19) . . ? H5A C5 H5C 112(3) . . ? H5B C5 H5C 111(3) . . ? O2 C6 C7 123.2(2) . . ? O2 C6 C4 118.1(2) . . ? C7 C6 C4 118.8(2) . . ? C6 C7 H7A 110.7(19) . . ? C6 C7 H7B 110(2) . . ? H7A C7 H7B 100(3) . . ? C6 C7 H7C 107(2) . . ? H7A C7 H7C 118(3) . . ? H7B C7 H7C 111(3) . . ? 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 N1 Pt1 N1 C1 122(76) 3 . . . ? Cl1 Pt1 N1 C1 -138.3(2) . . . . ? Cl1 Pt1 N1 C1 41.7(2) 3 . . . ? Cl2 Pt1 N1 C1 131.2(2) 3 . . . ? Cl2 Pt1 N1 C1 -48.8(2) . . . . ? Pt1 N1 C1 O1 -177.69(15) . . . . ? Pt1 N1 C1 C2 2.7(4) . . . . ? N1 C1 O1 N2 9.8(3) . . . . ? C2 C1 O1 N2 -170.59(18) . . . . ? C1 O1 N2 C4 -155.60(19) . . . . ? O1 N2 C4 C5 3.7(3) . . . . ? O1 N2 C4 C6 -179.31(17) . . . . ? N2 C4 C6 O2 -167.8(2) . . . . ? C5 C4 C6 O2 9.4(4) . . . . ? N2 C4 C6 C7 13.2(3) . . . . ? C5 C4 C6 C7 -169.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.684 _refine_diff_density_min -0.868 _refine_diff_density_rms 0.093 #===END data_trans-(PtCl4{NH=C(Et)ON=C(Me)C(Ph)(=O)}2] _database_code_CSD 186193 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ' trans-(PtCl4{NH=C(Et)ON=C(Me)C(Ph)(=O)}2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 Cl4 N4 O4 Pt' _chemical_formula_weight 773.39 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' 'Cl' 'Cl' 0.1484 0.1585 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8552(2) _cell_length_b 8.5681(2) _cell_length_c 11.6142(3) _cell_angle_alpha 88.8886(12) _cell_angle_beta 74.9911(12) _cell_angle_gamma 73.4238(12) _cell_volume 722.39(3) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 378 _exptl_absorpt_coefficient_mu 5.262 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.23636 _exptl_absorpt_correction_T_max 0.31680 _exptl_absorpt_process_details 'Xprep in Shelxtl v. 5.1 (Bruker AXS, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method 'CCD' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9834 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.94 _diffrn_reflns_theta_max 25.36 _reflns_number_total 2629 _reflns_number_gt 2624 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1999)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _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^)+(0.0475P)^2^+0.3172P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 2629 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.2567(6) -0.2276(6) 0.0464(4) 0.0316(9) Uani 1 1 d . . . C2 C 0.2515(7) -0.2594(6) -0.0775(4) 0.0369(10) Uani 1 1 d . . . H2A H 0.3045 -0.1837 -0.1306 0.044 Uiso 1 1 calc R . . H2B H 0.1220 -0.2392 -0.0801 0.044 Uiso 1 1 calc R . . C3 C 0.3619(9) -0.4384(7) -0.1232(5) 0.0501(13) Uani 1 1 d . . . H3A H 0.4919 -0.4563 -0.1259 0.075 Uiso 1 1 calc R . . H3B H 0.3511 -0.4582 -0.2034 0.075 Uiso 1 1 calc R . . H3C H 0.3124 -0.5134 -0.0690 0.075 Uiso 1 1 calc R . . C4 C 0.0471(6) -0.3483(6) 0.3144(5) 0.0362(10) Uani 1 1 d . . . C5 C -0.0542(8) -0.4523(7) 0.2772(5) 0.0436(12) Uani 1 1 d . . . H5A H -0.1441 -0.3864 0.2376 0.065 Uiso 1 1 calc R . . H5B H -0.1183 -0.4976 0.3477 0.065 Uiso 1 1 calc R . . H5C H 0.0332 -0.5415 0.2218 0.065 Uiso 1 1 calc R . . C6 C 0.0124(7) -0.3066(6) 0.4467(5) 0.0395(11) Uani 1 1 d . . . C7 C 0.1447(7) -0.2491(7) 0.4927(5) 0.0392(11) Uani 1 1 d . . . C8 C 0.3328(8) -0.3017(11) 0.4404(6) 0.068(2) Uani 1 1 d . . . H8 H 0.3812 -0.3714 0.3697 0.081 Uiso 1 1 calc R . . C9 C 0.4488(10) -0.2511(15) 0.4928(8) 0.099(4) Uani 1 1 d . . . H9 H 0.5781 -0.2882 0.4584 0.119 Uiso 1 1 calc R . . C10 C 0.3798(11) -0.1477(11) 0.5941(6) 0.071(2) Uani 1 1 d . . . H10 H 0.4609 -0.1127 0.6286 0.085 Uiso 1 1 calc R . . C11 C 0.1943(8) -0.0960(7) 0.6444(5) 0.0470(13) Uani 1 1 d . . . H11 H 0.1459 -0.0225 0.7131 0.056 Uiso 1 1 calc R . . C12 C 0.0782(8) -0.1491(7) 0.5968(5) 0.0451(12) Uani 1 1 d . . . H12 H -0.0500 -0.1173 0.6354 0.054 Uiso 1 1 calc R . . N1 N 0.3431(5) -0.1404(4) 0.0815(4) 0.0324(8) Uani 1 1 d . . . H1 H 0.3315 -0.1419 0.1589 0.039 Uiso 1 1 calc R . . N2 N 0.1503(6) -0.2750(5) 0.2459(4) 0.0366(9) Uani 1 1 d . . . O1 O 0.1565(5) -0.3089(4) 0.1241(3) 0.0353(7) Uani 1 1 d . . . O2 O -0.1307(6) -0.3166(6) 0.5126(4) 0.0589(11) Uani 1 1 d . . . Cl1 Cl 0.66095(18) -0.18302(16) -0.16238(12) 0.0459(3) Uani 1 1 d . . . Cl2 Cl 0.71346(19) -0.13346(15) 0.10159(13) 0.0456(3) Uani 1 1 d . . . Pt1 Pt 0.5000 0.0000 0.0000 0.02714(11) 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 0.031(2) 0.032(2) 0.032(2) 0.0056(19) -0.0082(18) -0.0101(18) C2 0.043(3) 0.041(3) 0.033(2) 0.008(2) -0.012(2) -0.019(2) C3 0.068(4) 0.041(3) 0.047(3) -0.004(3) -0.019(3) -0.021(3) C4 0.031(2) 0.038(2) 0.041(3) 0.012(2) -0.012(2) -0.0116(19) C5 0.049(3) 0.047(3) 0.043(3) 0.015(2) -0.016(2) -0.026(2) C6 0.040(3) 0.045(3) 0.038(3) 0.014(2) -0.012(2) -0.018(2) C7 0.036(2) 0.051(3) 0.033(3) 0.012(2) -0.009(2) -0.017(2) C8 0.039(3) 0.117(6) 0.045(3) -0.019(4) -0.010(3) -0.020(3) C9 0.043(4) 0.194(11) 0.065(5) -0.033(6) -0.011(3) -0.042(5) C10 0.072(4) 0.111(6) 0.051(4) 0.005(4) -0.028(3) -0.048(4) C11 0.062(3) 0.045(3) 0.034(3) 0.007(2) -0.017(2) -0.012(3) C12 0.050(3) 0.048(3) 0.034(3) 0.012(2) -0.008(2) -0.012(2) N1 0.036(2) 0.0302(19) 0.030(2) 0.0006(16) -0.0059(16) -0.0106(16) N2 0.039(2) 0.044(2) 0.031(2) 0.0064(18) -0.0088(17) -0.0194(18) O1 0.0404(17) 0.0403(18) 0.0336(17) 0.0103(15) -0.0127(14) -0.0225(15) O2 0.048(2) 0.093(3) 0.043(2) 0.016(2) -0.0071(18) -0.036(2) Cl1 0.0467(7) 0.0450(7) 0.0415(7) -0.0123(6) 0.0063(5) -0.0218(5) Cl2 0.0508(7) 0.0385(6) 0.0617(8) 0.0195(6) -0.0322(6) -0.0206(5) Pt1 0.03011(15) 0.02659(14) 0.02565(15) 0.00418(10) -0.00553(9) -0.01151(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 C1 N1 1.276(6) . ? C1 O1 1.356(6) . ? C1 C2 1.483(7) . ? C2 C3 1.555(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N2 1.273(6) . ? C4 C5 1.487(7) . ? C4 C6 1.521(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 O2 1.209(6) . ? C6 C7 1.482(7) . ? C7 C8 1.386(8) . ? C7 C12 1.389(8) . ? C8 C9 1.383(10) . ? C8 H8 0.9500 . ? C9 C10 1.378(12) . ? C9 H9 0.9500 . ? C10 C11 1.365(10) . ? C10 H10 0.9500 . ? C11 C12 1.361(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? N1 Pt1 2.015(4) . ? N1 H1 0.8800 . ? N2 O1 1.436(5) . ? Cl1 Pt1 2.3157(12) . ? Cl2 Pt1 2.3216(12) . ? Pt1 N1 2.015(4) 2_655 ? Pt1 Cl1 2.3157(12) 2_655 ? Pt1 Cl2 2.3216(12) 2_655 ? 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 N1 C1 O1 121.6(4) . . ? N1 C1 C2 127.8(4) . . ? O1 C1 C2 110.6(4) . . ? C1 C2 C3 110.9(4) . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 C5 126.6(5) . . ? N2 C4 C6 114.1(4) . . ? C5 C4 C6 118.9(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O2 C6 C7 121.2(5) . . ? O2 C6 C4 117.3(5) . . ? C7 C6 C4 121.4(4) . . ? C8 C7 C12 119.3(5) . . ? C8 C7 C6 122.2(5) . . ? C12 C7 C6 118.4(5) . . ? C9 C8 C7 118.9(6) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C10 C9 C8 121.1(7) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C11 C10 C9 119.6(6) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C12 C11 C10 120.4(6) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C7 120.8(5) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? C1 N1 Pt1 134.6(4) . . ? C1 N1 H1 112.7 . . ? Pt1 N1 H1 112.7 . . ? C4 N2 O1 109.3(4) . . ? C1 O1 N2 112.4(3) . . ? N1 Pt1 N1 180.0(3) . 2_655 ? N1 Pt1 Cl1 84.93(11) . 2_655 ? N1 Pt1 Cl1 95.07(11) 2_655 2_655 ? N1 Pt1 Cl1 95.07(11) . . ? N1 Pt1 Cl1 84.93(11) 2_655 . ? Cl1 Pt1 Cl1 180.00(9) 2_655 . ? N1 Pt1 Cl2 87.08(12) . . ? N1 Pt1 Cl2 92.92(12) 2_655 . ? Cl1 Pt1 Cl2 91.05(5) 2_655 . ? Cl1 Pt1 Cl2 88.95(5) . . ? N1 Pt1 Cl2 92.92(12) . 2_655 ? N1 Pt1 Cl2 87.08(12) 2_655 2_655 ? Cl1 Pt1 Cl2 88.95(5) 2_655 2_655 ? Cl1 Pt1 Cl2 91.05(5) . 2_655 ? Cl2 Pt1 Cl2 180.00(7) . 2_655 ? 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 N1 C1 C2 C3 108.8(6) . . . . ? O1 C1 C2 C3 -69.8(5) . . . . ? N2 C4 C6 O2 152.0(5) . . . . ? C5 C4 C6 O2 -21.6(7) . . . . ? N2 C4 C6 C7 -25.4(7) . . . . ? C5 C4 C6 C7 161.0(5) . . . . ? O2 C6 C7 C8 150.1(7) . . . . ? C4 C6 C7 C8 -32.6(8) . . . . ? O2 C6 C7 C12 -24.9(8) . . . . ? C4 C6 C7 C12 152.4(5) . . . . ? C12 C7 C8 C9 -0.9(12) . . . . ? C6 C7 C8 C9 -175.8(8) . . . . ? C7 C8 C9 C10 -1.2(15) . . . . ? C8 C9 C10 C11 0.8(15) . . . . ? C9 C10 C11 C12 1.6(12) . . . . ? C10 C11 C12 C7 -3.7(9) . . . . ? C8 C7 C12 C11 3.3(9) . . . . ? C6 C7 C12 C11 178.4(5) . . . . ? O1 C1 N1 Pt1 -178.7(3) . . . . ? C2 C1 N1 Pt1 2.8(8) . . . . ? C5 C4 N2 O1 -0.4(7) . . . . ? C6 C4 N2 O1 -173.5(4) . . . . ? N1 C1 O1 N2 4.2(6) . . . . ? C2 C1 O1 N2 -177.1(4) . . . . ? C4 N2 O1 C1 176.8(4) . . . . ? C1 N1 Pt1 N1 -71(100) . . . 2_655 ? C1 N1 Pt1 Cl1 137.1(5) . . . 2_655 ? C1 N1 Pt1 Cl1 -42.9(5) . . . . ? C1 N1 Pt1 Cl2 -131.6(4) . . . . ? C1 N1 Pt1 Cl2 48.4(4) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.935 _refine_diff_density_min -1.059 _refine_diff_density_rms 0.142 #===END======================================================================== data_trans-(PtCl4{NH=C(Et)ON=C(Me)C(C6H4F-p)(=O)}2] _database_code_CSD 186194 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'trans-(PtCl4{NH=C(Et)ON=C(Me)C(C6H4F-p)(=O)}2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H26 Cl4 F2 N4 O4 Pt' _chemical_formula_weight 809.38 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' 'F' 'F' 0.0171 0.0103 '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' '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4829(15) _cell_length_b 12.489(3) _cell_length_c 16.111(3) _cell_angle_alpha 71.07(3) _cell_angle_beta 86.40(3) _cell_angle_gamma 86.11(3) _cell_volume 1419.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'yellow' _exptl_crystal_colour 'block' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 5.370 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.19631 _exptl_absorpt_correction_T_max 0.28248 _exptl_absorpt_process_details 'Xprep in Shelxtl v. 5.1 (Bruker AXS, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method 'CCD' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19480 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.06 _reflns_number_total 4975 _reflns_number_gt 3868 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1999)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _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^)+(0.0250P)^2^+8.9393P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 4975 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _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 Pt1 Pt 0.5000 0.0000 0.5000 0.02611(11) Uani 1 2 d S . . Cl1 Cl 0.6035(2) 0.08392(15) 0.35611(11) 0.0399(4) Uani 1 1 d . . . Cl2 Cl 0.3123(2) -0.11145(15) 0.45790(12) 0.0391(4) Uani 1 1 d . . . N1 N 0.3035(7) 0.1205(5) 0.4957(3) 0.0316(12) Uani 1 1 d . . . H1 H 0.2993 0.1427 0.5424 0.038 Uiso 1 1 calc R . . C1 C 0.1839(9) 0.1724(6) 0.4418(4) 0.0335(15) Uani 1 1 d . . . C2 C 0.1454(12) 0.1566(8) 0.3574(5) 0.056(2) Uani 1 1 d . . . H2A H 0.2565 0.1259 0.3348 0.068 Uiso 1 1 calc R . . H2B H 0.0551 0.0984 0.3696 0.068 Uiso 1 1 calc R . . C3 C 0.0806(17) 0.2563(9) 0.2881(6) 0.080(3) Uani 1 1 d . . . H3A H -0.0279 0.2893 0.3096 0.119 Uiso 1 1 calc R . . H3B H 0.0529 0.2346 0.2373 0.119 Uiso 1 1 calc R . . H3C H 0.1731 0.3122 0.2708 0.119 Uiso 1 1 calc R . . O1 O 0.0669(6) 0.2502(4) 0.4598(3) 0.0340(11) Uani 1 1 d . . . N2 N 0.0777(7) 0.2516(5) 0.5489(3) 0.0307(12) Uani 1 1 d . . . C4 C -0.0405(8) 0.3208(6) 0.5639(4) 0.0305(14) Uani 1 1 d . . . C5 C -0.1696(10) 0.3957(6) 0.5024(5) 0.0407(17) Uani 1 1 d . . . H5A H -0.1165 0.4169 0.4424 0.061 Uiso 1 1 calc R . . H5B H -0.1988 0.4641 0.5186 0.061 Uiso 1 1 calc R . . H5C H -0.2793 0.3557 0.5052 0.061 Uiso 1 1 calc R . . C6 C -0.0388(9) 0.3272(6) 0.6569(5) 0.0331(15) Uani 1 1 d . . . O2 O -0.0779(7) 0.4192(4) 0.6657(3) 0.0485(13) Uani 1 1 d . . . C7 C 0.0052(8) 0.2248(6) 0.7316(4) 0.0295(14) Uani 1 1 d . . . C8 C -0.0084(8) 0.1142(6) 0.7293(4) 0.0297(14) Uani 1 1 d . . . H8 H -0.0465 0.1029 0.6778 0.036 Uiso 1 1 calc R . . C9 C 0.0330(9) 0.0224(6) 0.8010(4) 0.0339(15) Uani 1 1 d . . . H9 H 0.0224 -0.0526 0.8001 0.041 Uiso 1 1 calc R . . C10 C 0.0898(9) 0.0416(7) 0.8736(5) 0.0389(17) Uani 1 1 d . . . C11 C 0.1023(10) 0.1467(7) 0.8807(5) 0.0410(18) Uani 1 1 d . . . H11 H 0.1394 0.1561 0.9331 0.049 Uiso 1 1 calc R . . C12 C 0.0592(9) 0.2387(6) 0.8087(5) 0.0366(16) Uani 1 1 d . . . H12 H 0.0663 0.3131 0.8117 0.044 Uiso 1 1 calc R . . F3 F 0.1340(6) -0.0501(4) 0.9438(3) 0.0520(11) Uani 1 1 d . . . Pt1B Pt 1.0000 -0.5000 0.0000 0.03927(13) Uani 1 2 d S . . Cl2B Cl 1.2028(3) -0.4626(2) 0.08723(16) 0.0636(6) Uani 1 1 d . . . Cl1B Cl 1.1138(4) -0.68561(19) 0.03395(15) 0.0667(7) Uani 1 1 d . . . N1B N 0.8263(9) -0.5301(6) 0.1057(4) 0.0492(17) Uani 1 1 d . . . H1B H 0.8199 -0.4752 0.1290 0.059 Uiso 1 1 calc R . . C1B C 0.7244(11) -0.6096(7) 0.1462(6) 0.055(2) Uani 1 1 d . . . C2B C 0.7034(14) -0.7189(8) 0.1292(7) 0.073(3) Uani 1 1 d . . . H2B1 H 0.7852 -0.7222 0.0793 0.087 Uiso 1 1 calc R . . H2B2 H 0.7392 -0.7826 0.1815 0.087 Uiso 1 1 calc R . . C3B C 0.5307(16) -0.7322(11) 0.1105(8) 0.101(5) Uani 1 1 d . . . H3B1 H 0.4526 -0.7436 0.1634 0.151 Uiso 1 1 calc R . . H3B2 H 0.5289 -0.7982 0.0904 0.151 Uiso 1 1 calc R . . H3B3 H 0.4880 -0.6642 0.0642 0.151 Uiso 1 1 calc R . . O1B O 0.6216(8) -0.6051(4) 0.2177(4) 0.0544(15) Uani 1 1 d . . . N2B N 0.6279(8) -0.4972(5) 0.2311(4) 0.0412(15) Uani 1 1 d . . . C4B C 0.5386(9) -0.4982(6) 0.3021(4) 0.0338(15) Uani 1 1 d . . . C5B C 0.4480(10) -0.5936(6) 0.3661(5) 0.0385(16) Uani 1 1 d . . . H5B1 H 0.3233 -0.5924 0.3503 0.058 Uiso 1 1 calc R . . H5B2 H 0.4505 -0.5867 0.4249 0.058 Uiso 1 1 calc R . . H5B3 H 0.5099 -0.6651 0.3657 0.058 Uiso 1 1 calc R . . C6B C 0.5418(8) -0.3860(6) 0.3209(4) 0.0305(14) Uani 1 1 d . . . O2B O 0.5810(7) -0.3918(4) 0.3948(3) 0.0431(12) Uani 1 1 d . . . C7B C 0.4959(8) -0.2787(6) 0.2525(4) 0.0288(14) Uani 1 1 d . . . C8B C 0.4286(9) -0.2722(6) 0.1713(4) 0.0354(16) Uani 1 1 d . . . H8B H 0.4136 -0.3398 0.1581 0.043 Uiso 1 1 calc R . . C9B C 0.3847(9) -0.1697(6) 0.1112(4) 0.0381(16) Uani 1 1 d . . . H9B H 0.3390 -0.1649 0.0563 0.046 Uiso 1 1 calc R . . C10B C 0.4084(10) -0.0728(6) 0.1324(5) 0.0391(17) Uani 1 1 d . . . C11B C 0.4709(9) -0.0741(6) 0.2106(5) 0.0376(16) Uani 1 1 d . . . H11B H 0.4837 -0.0059 0.2232 0.045 Uiso 1 1 calc R . . C12B C 0.5147(8) -0.1784(6) 0.2706(4) 0.0330(15) Uani 1 1 d . . . H12B H 0.5587 -0.1819 0.3256 0.040 Uiso 1 1 calc R . . F1B F 0.3640(6) 0.0294(4) 0.0724(3) 0.0545(12) Uani 1 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 0.0272(2) 0.0315(2) 0.02291(19) -0.01408(16) 0.00437(14) -0.00241(14) Cl1 0.0480(10) 0.0449(10) 0.0262(8) -0.0129(8) 0.0100(7) -0.0027(8) Cl2 0.0350(9) 0.0470(10) 0.0453(10) -0.0282(9) 0.0000(7) -0.0060(7) N1 0.029(3) 0.042(3) 0.024(3) -0.012(3) 0.006(2) -0.004(3) C1 0.035(4) 0.041(4) 0.025(3) -0.013(3) 0.004(3) -0.001(3) C2 0.064(6) 0.071(6) 0.042(5) -0.032(4) -0.014(4) 0.019(5) C3 0.133(10) 0.071(7) 0.037(5) -0.017(5) -0.032(6) 0.010(6) O1 0.037(3) 0.041(3) 0.025(2) -0.015(2) 0.0007(19) 0.004(2) N2 0.031(3) 0.038(3) 0.026(3) -0.015(3) 0.004(2) -0.001(2) C4 0.028(3) 0.033(4) 0.029(3) -0.009(3) 0.005(3) -0.005(3) C5 0.039(4) 0.042(4) 0.038(4) -0.011(3) 0.004(3) 0.004(3) C6 0.030(4) 0.032(4) 0.038(4) -0.014(3) 0.008(3) 0.000(3) O2 0.063(4) 0.036(3) 0.045(3) -0.015(2) 0.016(3) 0.003(2) C7 0.024(3) 0.039(4) 0.026(3) -0.014(3) 0.003(3) 0.000(3) C8 0.028(3) 0.037(4) 0.029(3) -0.017(3) 0.000(3) -0.002(3) C9 0.037(4) 0.031(4) 0.035(4) -0.013(3) -0.001(3) 0.002(3) C10 0.031(4) 0.051(4) 0.031(4) -0.010(3) 0.003(3) 0.002(3) C11 0.040(4) 0.061(5) 0.028(4) -0.024(4) 0.001(3) -0.002(4) C12 0.035(4) 0.044(4) 0.039(4) -0.024(4) 0.008(3) -0.010(3) F3 0.065(3) 0.053(3) 0.031(2) -0.006(2) -0.007(2) 0.010(2) Pt1B 0.0425(2) 0.0455(3) 0.0413(2) -0.0311(2) 0.01924(18) -0.01495(18) Cl2B 0.0566(13) 0.0917(17) 0.0659(14) -0.0575(14) 0.0061(10) -0.0121(12) Cl1B 0.0991(18) 0.0508(12) 0.0557(13) -0.0301(11) 0.0244(12) -0.0014(12) N1B 0.053(4) 0.051(4) 0.057(4) -0.038(4) 0.026(3) -0.020(3) C1B 0.055(5) 0.056(5) 0.065(6) -0.036(5) 0.032(4) -0.019(4) C2B 0.086(7) 0.065(6) 0.079(7) -0.045(6) 0.045(6) -0.030(5) C3B 0.102(9) 0.127(10) 0.113(10) -0.094(9) 0.058(8) -0.068(8) O1B 0.070(4) 0.044(3) 0.058(3) -0.032(3) 0.041(3) -0.022(3) N2B 0.051(4) 0.035(3) 0.044(4) -0.024(3) 0.018(3) -0.010(3) C4B 0.035(4) 0.037(4) 0.031(4) -0.016(3) 0.007(3) -0.001(3) C5B 0.045(4) 0.036(4) 0.035(4) -0.016(3) 0.015(3) -0.005(3) C6B 0.029(3) 0.035(4) 0.027(3) -0.011(3) 0.008(3) -0.001(3) O2B 0.051(3) 0.053(3) 0.029(3) -0.020(2) -0.001(2) 0.006(2) C7B 0.023(3) 0.037(4) 0.030(3) -0.015(3) 0.004(3) -0.003(3) C8B 0.035(4) 0.044(4) 0.034(4) -0.021(3) 0.001(3) -0.006(3) C9B 0.040(4) 0.046(4) 0.027(3) -0.009(3) -0.004(3) -0.006(3) C10B 0.038(4) 0.036(4) 0.038(4) -0.007(3) 0.001(3) 0.004(3) C11B 0.040(4) 0.035(4) 0.042(4) -0.020(3) 0.002(3) -0.001(3) C12B 0.026(3) 0.047(4) 0.030(3) -0.021(3) 0.003(3) 0.001(3) F1B 0.065(3) 0.042(3) 0.048(3) -0.003(2) -0.005(2) -0.002(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 Pt1 N1 2.019(5) 2_656 ? Pt1 N1 2.019(5) . ? Pt1 Cl2 2.3167(17) . ? Pt1 Cl2 2.3167(17) 2_656 ? Pt1 Cl1 2.3194(18) 2_656 ? Pt1 Cl1 2.3194(18) . ? N1 C1 1.277(8) . ? N1 H1 0.8800 . ? C1 O1 1.352(8) . ? C1 C2 1.484(10) . ? C2 C3 1.454(12) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O1 N2 1.449(6) . ? N2 C4 1.262(8) . ? C4 C5 1.479(9) . ? C4 C6 1.528(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 O2 1.217(8) . ? C6 C7 1.479(9) . ? C7 C12 1.396(9) . ? C7 C8 1.404(9) . ? C8 C9 1.371(9) . ? C8 H8 0.9500 . ? C9 C10 1.367(10) . ? C9 H9 0.9500 . ? C10 F3 1.362(8) . ? C10 C11 1.363(11) . ? C11 C12 1.379(10) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? Pt1B N1B 2.026(6) 2_745 ? Pt1B N1B 2.026(6) . ? Pt1B Cl2B 2.299(2) 2_745 ? Pt1B Cl2B 2.299(2) . ? Pt1B Cl1B 2.316(2) . ? Pt1B Cl1B 2.316(2) 2_745 ? N1B C1B 1.270(10) . ? N1B H1B 0.8800 . ? C1B O1B 1.359(9) . ? C1B C2B 1.496(11) . ? C2B C3B 1.378(15) . ? C2B H2B1 0.9900 . ? C2B H2B2 0.9900 . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C3B H3B3 0.9800 . ? O1B N2B 1.436(7) . ? N2B C4B 1.284(8) . ? C4B C5B 1.472(10) . ? C4B C6B 1.530(9) . ? C5B H5B1 0.9800 . ? C5B H5B2 0.9800 . ? C5B H5B3 0.9800 . ? C6B O2B 1.221(8) . ? C6B C7B 1.467(9) . ? C7B C12B 1.393(9) . ? C7B C8B 1.408(9) . ? C8B C9B 1.365(10) . ? C8B H8B 0.9500 . ? C9B C10B 1.385(10) . ? C9B H9B 0.9500 . ? C10B F1B 1.362(8) . ? C10B C11B 1.366(10) . ? C11B C12B 1.380(10) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? 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 N1 Pt1 N1 180.0(3) 2_656 . ? N1 Pt1 Cl2 87.31(16) 2_656 . ? N1 Pt1 Cl2 92.69(16) . . ? N1 Pt1 Cl2 92.69(16) 2_656 2_656 ? N1 Pt1 Cl2 87.31(16) . 2_656 ? Cl2 Pt1 Cl2 180.00(6) . 2_656 ? N1 Pt1 Cl1 94.55(16) 2_656 2_656 ? N1 Pt1 Cl1 85.45(16) . 2_656 ? Cl2 Pt1 Cl1 88.30(7) . 2_656 ? Cl2 Pt1 Cl1 91.70(7) 2_656 2_656 ? N1 Pt1 Cl1 85.45(16) 2_656 . ? N1 Pt1 Cl1 94.55(16) . . ? Cl2 Pt1 Cl1 91.70(7) . . ? Cl2 Pt1 Cl1 88.30(7) 2_656 . ? Cl1 Pt1 Cl1 180.0 2_656 . ? C1 N1 Pt1 135.6(5) . . ? C1 N1 H1 112.2 . . ? Pt1 N1 H1 112.2 . . ? N1 C1 O1 120.8(6) . . ? N1 C1 C2 128.2(6) . . ? O1 C1 C2 111.0(6) . . ? C3 C2 C1 116.9(7) . . ? C3 C2 H2A 108.1 . . ? C1 C2 H2A 108.1 . . ? C3 C2 H2B 108.1 . . ? C1 C2 H2B 108.1 . . ? H2A C2 H2B 107.3 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 O1 N2 112.3(5) . . ? C4 N2 O1 109.7(5) . . ? N2 C4 C5 128.0(6) . . ? N2 C4 C6 113.2(6) . . ? C5 C4 C6 118.8(6) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O2 C6 C7 122.7(6) . . ? O2 C6 C4 116.7(6) . . ? C7 C6 C4 120.5(6) . . ? C12 C7 C8 118.5(6) . . ? C12 C7 C6 118.5(6) . . ? C8 C7 C6 123.1(6) . . ? C9 C8 C7 120.5(6) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 118.3(6) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? F3 C10 C11 118.0(6) . . ? F3 C10 C9 117.9(7) . . ? C11 C10 C9 124.1(7) . . ? C10 C11 C12 117.4(6) . . ? C10 C11 H11 121.3 . . ? C12 C11 H11 121.3 . . ? C11 C12 C7 121.2(7) . . ? C11 C12 H12 119.4 . . ? C7 C12 H12 119.4 . . ? N1B Pt1B N1B 180.0(4) 2_745 . ? N1B Pt1B Cl2B 86.3(2) 2_745 2_745 ? N1B Pt1B Cl2B 93.7(2) . 2_745 ? N1B Pt1B Cl2B 93.7(2) 2_745 . ? N1B Pt1B Cl2B 86.3(2) . . ? Cl2B Pt1B Cl2B 180.0 2_745 . ? N1B Pt1B Cl1B 84.8(2) 2_745 . ? N1B Pt1B Cl1B 95.2(2) . . ? Cl2B Pt1B Cl1B 89.13(10) 2_745 . ? Cl2B Pt1B Cl1B 90.87(10) . . ? N1B Pt1B Cl1B 95.2(2) 2_745 2_745 ? N1B Pt1B Cl1B 84.8(2) . 2_745 ? Cl2B Pt1B Cl1B 90.87(10) 2_745 2_745 ? Cl2B Pt1B Cl1B 89.13(10) . 2_745 ? Cl1B Pt1B Cl1B 180.0 . 2_745 ? C1B N1B Pt1B 135.0(5) . . ? C1B N1B H1B 112.5 . . ? Pt1B N1B H1B 112.5 . . ? N1B C1B O1B 120.9(7) . . ? N1B C1B C2B 128.6(7) . . ? O1B C1B C2B 110.5(7) . . ? C3B C2B C1B 113.1(9) . . ? C3B C2B H2B1 109.0 . . ? C1B C2B H2B1 109.0 . . ? C3B C2B H2B2 109.0 . . ? C1B C2B H2B2 109.0 . . ? H2B1 C2B H2B2 107.8 . . ? C2B C3B H3B1 109.5 . . ? C2B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C2B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C1B O1B N2B 111.6(5) . . ? C4B N2B O1B 110.0(5) . . ? N2B C4B C5B 128.0(6) . . ? N2B C4B C6B 112.7(6) . . ? C5B C4B C6B 119.2(6) . . ? C4B C5B H5B1 109.5 . . ? C4B C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? C4B C5B H5B3 109.5 . . ? H5B1 C5B H5B3 109.5 . . ? H5B2 C5B H5B3 109.5 . . ? O2B C6B C7B 123.3(6) . . ? O2B C6B C4B 116.6(6) . . ? C7B C6B C4B 120.1(6) . . ? C12B C7B C8B 118.6(6) . . ? C12B C7B C6B 117.9(6) . . ? C8B C7B C6B 123.6(6) . . ? C9B C8B C7B 120.7(6) . . ? C9B C8B H8B 119.7 . . ? C7B C8B H8B 119.7 . . ? C8B C9B C10B 118.2(6) . . ? C8B C9B H9B 120.9 . . ? C10B C9B H9B 120.9 . . ? F1B C10B C11B 118.3(6) . . ? F1B C10B C9B 118.1(6) . . ? C11B C10B C9B 123.6(7) . . ? C10B C11B C12B 117.5(6) . . ? C10B C11B H11B 121.3 . . ? C12B C11B H11B 121.3 . . ? C11B C12B C7B 121.5(6) . . ? C11B C12B H12B 119.3 . . ? C7B C12B H12B 119.3 . . ? 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 N1 Pt1 N1 C1 89(100) 2_656 . . . ? Cl2 Pt1 N1 C1 -46.2(7) . . . . ? Cl2 Pt1 N1 C1 133.8(7) 2_656 . . . ? Cl1 Pt1 N1 C1 -134.3(7) 2_656 . . . ? Cl1 Pt1 N1 C1 45.7(7) . . . . ? Pt1 N1 C1 O1 179.0(4) . . . . ? Pt1 N1 C1 C2 1.8(12) . . . . ? N1 C1 C2 C3 -147.5(9) . . . . ? O1 C1 C2 C3 35.0(11) . . . . ? N1 C1 O1 N2 -9.0(9) . . . . ? C2 C1 O1 N2 168.6(6) . . . . ? C1 O1 N2 C4 -176.4(6) . . . . ? O1 N2 C4 C5 -2.6(9) . . . . ? O1 N2 C4 C6 179.8(5) . . . . ? N2 C4 C6 O2 146.0(7) . . . . ? C5 C4 C6 O2 -31.9(9) . . . . ? N2 C4 C6 C7 -35.1(9) . . . . ? C5 C4 C6 C7 147.0(6) . . . . ? O2 C6 C7 C12 -20.7(10) . . . . ? C4 C6 C7 C12 160.5(6) . . . . ? O2 C6 C7 C8 158.0(7) . . . . ? C4 C6 C7 C8 -20.8(9) . . . . ? C12 C7 C8 C9 -0.9(9) . . . . ? C6 C7 C8 C9 -179.5(6) . . . . ? C7 C8 C9 C10 -0.9(10) . . . . ? C8 C9 C10 F3 -178.7(6) . . . . ? C8 C9 C10 C11 2.3(11) . . . . ? F3 C10 C11 C12 179.3(6) . . . . ? C9 C10 C11 C12 -1.8(11) . . . . ? C10 C11 C12 C7 -0.2(10) . . . . ? C8 C7 C12 C11 1.4(10) . . . . ? C6 C7 C12 C11 -179.9(6) . . . . ? N1B Pt1B N1B C1B 151(100) 2_745 . . . ? Cl2B Pt1B N1B C1B 50.1(9) 2_745 . . . ? Cl2B Pt1B N1B C1B -129.9(9) . . . . ? Cl1B Pt1B N1B C1B -39.4(9) . . . . ? Cl1B Pt1B N1B C1B 140.6(9) 2_745 . . . ? Pt1B N1B C1B O1B 179.5(6) . . . . ? Pt1B N1B C1B C2B 2.8(17) . . . . ? N1B C1B C2B C3B -120.8(12) . . . . ? O1B C1B C2B C3B 62.2(12) . . . . ? N1B C1B O1B N2B 7.6(12) . . . . ? C2B C1B O1B N2B -175.2(8) . . . . ? C1B O1B N2B C4B -176.0(7) . . . . ? O1B N2B C4B C5B 3.2(11) . . . . ? O1B N2B C4B C6B 179.3(6) . . . . ? N2B C4B C6B O2B -130.3(7) . . . . ? C5B C4B C6B O2B 46.2(9) . . . . ? N2B C4B C6B C7B 50.8(8) . . . . ? C5B C4B C6B C7B -132.7(7) . . . . ? O2B C6B C7B C12B 6.2(9) . . . . ? C4B C6B C7B C12B -175.0(6) . . . . ? O2B C6B C7B C8B -171.6(6) . . . . ? C4B C6B C7B C8B 7.3(9) . . . . ? C12B C7B C8B C9B 0.7(10) . . . . ? C6B C7B C8B C9B 178.5(6) . . . . ? C7B C8B C9B C10B 0.1(10) . . . . ? C8B C9B C10B F1B -179.8(6) . . . . ? C8B C9B C10B C11B -1.0(11) . . . . ? F1B C10B C11B C12B 179.8(6) . . . . ? C9B C10B C11B C12B 1.0(11) . . . . ? C10B C11B C12B C7B -0.1(10) . . . . ? C8B C7B C12B C11B -0.7(9) . . . . ? C6B C7B C12B C11B -178.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.470 _refine_diff_density_min -1.779 _refine_diff_density_rms 0.137 #===END======================================================================== data_trans-[PtCl2{NH=C(Et)ON=C(Me)C(Me)(=O)}2] _database_code_CSD 186195 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common trans-[PtCl2{NH=C(Et)ON=C(Me)C(Me)(=O)}2] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H24 Cl2 N4 O4 Pt' _chemical_formula_weight 578.36 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' 'Cl' 'Cl' 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.14820(10) _cell_length_b 9.4605(2) _cell_length_c 17.0184(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.5058(9) _cell_angle_gamma 90.00 _cell_volume 983.50(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2101 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.373 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.953 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 7.431 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.11968 _exptl_absorpt_correction_T_max 0.17958 _exptl_absorpt_process_details 'Xprep in Shelxtl v. 6.12 (Bruker AXS, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method 'CCD' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11539 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.26 _diffrn_reflns_theta_max 26.36 _reflns_number_total 1984 _reflns_number_gt 1751 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997-2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0000P)^2^+1.4142P] 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 1984 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0195 _refine_ls_R_factor_gt 0.0160 _refine_ls_wR_factor_ref 0.0406 _refine_ls_wR_factor_gt 0.0386 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.0000 0.0000 0.0000 0.01550(6) Uani 1 2 d S . . Cl1 Cl -0.24607(11) -0.13079(7) -0.08244(4) 0.02483(15) Uani 1 1 d . . . N1 N -0.0272(4) 0.1634(2) -0.07642(13) 0.0188(5) Uani 1 1 d . . . H1 H 0.0678 0.1670 -0.1113 0.023 Uiso 1 1 calc R . . C1 C -0.1684(4) 0.2615(3) -0.07892(15) 0.0195(5) Uani 1 1 d . . . C2 C -0.3400(5) 0.2770(3) -0.02435(17) 0.0256(6) Uani 1 1 d . . . H2A H -0.3604 0.1857 0.0023 0.031 Uiso 1 1 calc R . . H2B H -0.4807 0.3032 -0.0550 0.031 Uiso 1 1 calc R . . C3 C -0.2742(6) 0.3910(4) 0.03789(19) 0.0345(7) Uani 1 1 d . . . H3A H -0.1384 0.3629 0.0698 0.052 Uiso 1 1 calc R . . H3B H -0.3908 0.4021 0.0722 0.052 Uiso 1 1 calc R . . H3C H -0.2515 0.4809 0.0114 0.052 Uiso 1 1 calc R . . O1 O -0.1812(3) 0.3720(2) -0.13114(11) 0.0224(4) Uani 1 1 d . . . N2 N -0.0141(4) 0.3700(2) -0.18335(13) 0.0208(5) Uani 1 1 d . . . C4 C -0.0395(5) 0.4776(3) -0.22931(17) 0.0197(6) Uani 1 1 d . . . C5 C -0.2095(5) 0.5892(3) -0.22868(18) 0.0251(6) Uani 1 1 d . . . H5A H -0.3536 0.5489 -0.2463 0.038 Uiso 1 1 calc R . . H5B H -0.1782 0.6659 -0.2644 0.038 Uiso 1 1 calc R . . H5C H -0.2088 0.6264 -0.1749 0.038 Uiso 1 1 calc R . . C6 C 0.1311(5) 0.4891(3) -0.28684(18) 0.0219(6) Uani 1 1 d . . . C7 C 0.2706(5) 0.3638(3) -0.2973(2) 0.0327(7) Uani 1 1 d . . . H7A H 0.3709 0.3852 -0.3365 0.049 Uiso 1 1 calc R . . H7B H 0.1777 0.2834 -0.3156 0.049 Uiso 1 1 calc R . . H7C H 0.3552 0.3401 -0.2467 0.049 Uiso 1 1 calc R . . O2 O 0.1491(4) 0.6006(2) -0.32063(12) 0.0290(5) Uani 1 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 0.01842(9) 0.01483(9) 0.01404(9) 0.00090(5) 0.00534(6) 0.00106(5) Cl1 0.0262(3) 0.0258(3) 0.0223(3) -0.0011(3) 0.0019(3) -0.0039(3) N1 0.0223(11) 0.0197(11) 0.0156(11) 0.0002(9) 0.0068(9) 0.0001(9) C1 0.0233(13) 0.0182(13) 0.0174(13) 0.0004(11) 0.0039(11) -0.0013(11) C2 0.0273(15) 0.0242(15) 0.0274(15) 0.0036(12) 0.0126(12) 0.0038(12) C3 0.0411(18) 0.0383(18) 0.0257(16) -0.0031(14) 0.0114(14) 0.0097(15) O1 0.0264(10) 0.0207(9) 0.0218(10) 0.0049(8) 0.0103(8) 0.0051(8) N2 0.0227(11) 0.0201(11) 0.0210(11) 0.0005(10) 0.0086(9) -0.0014(10) C4 0.0222(14) 0.0188(12) 0.0176(14) -0.0002(11) 0.0002(12) -0.0027(11) C5 0.0290(15) 0.0217(14) 0.0248(14) 0.0047(12) 0.0041(12) 0.0040(12) C6 0.0246(15) 0.0217(15) 0.0193(15) -0.0021(11) 0.0021(12) -0.0048(11) C7 0.0352(17) 0.0310(16) 0.0349(17) 0.0076(14) 0.0171(14) 0.0063(14) O2 0.0384(12) 0.0228(11) 0.0270(11) 0.0036(9) 0.0091(9) -0.0068(9) _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 N1 2.015(2) 3 ? Pt1 N1 2.015(2) . ? Pt1 Cl1 2.3037(7) 3 ? Pt1 Cl1 2.3037(7) . ? N1 C1 1.268(4) . ? C1 O1 1.368(3) . ? C1 C2 1.490(4) . ? C2 C3 1.533(4) . ? O1 N2 1.432(3) . ? N2 C4 1.283(4) . ? C4 C5 1.487(4) . ? C4 C6 1.518(4) . ? C6 O2 1.212(3) . ? C6 C7 1.486(4) . ? 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 N1 Pt1 N1 180.00(12) 3 . ? N1 Pt1 Cl1 91.04(6) 3 3 ? N1 Pt1 Cl1 88.96(6) . 3 ? N1 Pt1 Cl1 88.96(6) 3 . ? N1 Pt1 Cl1 91.04(6) . . ? Cl1 Pt1 Cl1 180.00(4) 3 . ? C1 N1 Pt1 126.13(19) . . ? N1 C1 O1 124.7(2) . . ? N1 C1 C2 125.6(2) . . ? O1 C1 C2 109.7(2) . . ? C1 C2 C3 110.5(2) . . ? C1 O1 N2 113.60(19) . . ? C4 N2 O1 108.8(2) . . ? N2 C4 C5 126.6(3) . . ? N2 C4 C6 113.9(2) . . ? C5 C4 C6 119.4(2) . . ? O2 C6 C7 123.5(3) . . ? O2 C6 C4 118.4(3) . . ? C7 C6 C4 118.1(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 N1 Pt1 N1 C1 154(84) 3 . . . ? Cl1 Pt1 N1 C1 -92.7(2) 3 . . . ? Cl1 Pt1 N1 C1 87.3(2) . . . . ? Pt1 N1 C1 O1 179.33(18) . . . . ? Pt1 N1 C1 C2 1.4(4) . . . . ? N1 C1 C2 C3 102.3(3) . . . . ? O1 C1 C2 C3 -75.9(3) . . . . ? N1 C1 O1 N2 -1.4(4) . . . . ? C2 C1 O1 N2 176.8(2) . . . . ? C1 O1 N2 C4 -179.6(2) . . . . ? O1 N2 C4 C5 1.2(4) . . . . ? O1 N2 C4 C6 178.9(2) . . . . ? N2 C4 C6 O2 -164.7(3) . . . . ? C5 C4 C6 O2 13.2(4) . . . . ? N2 C4 C6 C7 13.9(4) . . . . ? C5 C4 C6 C7 -168.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.381 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.101 #===END======================================================================== _eof # End of Crystallographic Information File