Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Adilia Charmier' _publ_contact_author_address ; Centro de Qu\'imica Estrutural, Complexo 1 Instituto Superior T\'ecnico Av. Rovisco Pais Lisbon 1049-001 PORTUGAL ; _publ_contact_author_email ADILIA.CHARMIER@IST.UTL.PT _publ_section_title ;Direct synthesis of (imine)platinum(II) complexes by iminoacylation of ketoximes with activated organonitrile ligands ; loop_ _publ_author_name 'Adilia Charmier' 'M.F.C.G.da Silva' 'Jamal Lasri' 'Armando J. L. Pombeiro' # Attachment 'jl31pf1.cif' data_jl31pf1 _database_code_depnum_ccdc_archive 'CCDC 617145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Pt Cl4 O2 N4 C12 H22' _chemical_formula_sum 'C12 H22 Cl4 N4 O2 Pt' _chemical_formula_weight 591.23 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 Tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 10.9223 _cell_length_b 10.9223 _cell_length_c 34.2519(39) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4086.1(5) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 4904 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 30.08 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 7.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4965 _exptl_absorpt_correction_T_max 0.5889 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and onega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18448 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 35.54 _reflns_number_total 4617 _reflns_number_gt 3045 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'WinGX v.1.70.01 (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 v.1.08 (Farrugia, 1997)' _computing_publication_material ? _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^)+(0.0452P)^2^+0.3924P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4617 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 0.7730(4) 0.6417(4) 0.45297(12) 0.0430(9) Uani 1 1 d . . . C2 C 0.8275(4) 0.6303(6) 0.49210(12) 0.0640(15) Uani 1 1 d . . . H2A H 0.9160 0.6263 0.4899 0.077 Uiso 1 1 calc R . . H2B H 0.7994 0.5552 0.5043 0.077 Uiso 1 1 calc R . . C11 C 0.4906(4) 0.5841(5) 0.41445(14) 0.0512(11) Uani 1 1 d . . . C12 C 0.4261(6) 0.5916(7) 0.37599(15) 0.0721(18) Uani 1 1 d . . . H12A H 0.3611 0.6519 0.3773 0.087 Uiso 1 1 calc R . . H12B H 0.4832 0.6164 0.3558 0.087 Uiso 1 1 calc R . . C13 C 0.3767(11) 0.4753(14) 0.3670(3) 0.171(5) Uani 1 1 d . . . H13A H 0.3356 0.4789 0.3423 0.256 Uiso 1 1 calc R . . H13B H 0.3195 0.4518 0.3869 0.256 Uiso 1 1 calc R . . H13C H 0.4416 0.4161 0.3657 0.256 Uiso 1 1 calc R . . C14 C 0.4240(5) 0.5399(8) 0.44948(19) 0.108(3) Uani 1 1 d . . . H14A H 0.4779 0.5409 0.4716 0.162 Uiso 1 1 calc R . . H14B H 0.3957 0.4579 0.4450 0.162 Uiso 1 1 calc R . . H14C H 0.3552 0.5923 0.4545 0.162 Uiso 1 1 calc R . . N1 N 0.8297(3) 0.6821(3) 0.42335(9) 0.0332(6) Uani 1 1 d . . . N11 N 0.6011(4) 0.6155(5) 0.41422(11) 0.0650(13) Uani 1 1 d . . . O11 O 0.6552(3) 0.6015(3) 0.45297(8) 0.0554(8) Uani 1 1 d . . . Cl1 Cl 0.92174(10) 0.94644(9) 0.42397(3) 0.0396(2) Uani 1 1 d . . . Pt1 Pt 1.0000 0.7500 0.423077(5) 0.02826(6) Uani 1 2 d S . . Cl2 Cl 0.7868(3) 0.7548(2) 0.52100(6) 0.1552(11) Uani 1 1 d . . . H1 H 0.795(4) 0.676(3) 0.4002(12) 0.027(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 C1 0.0319(19) 0.061(3) 0.0361(19) 0.0085(18) -0.0024(15) -0.0120(17) C2 0.044(2) 0.114(5) 0.034(2) 0.025(2) -0.0035(18) -0.026(3) C11 0.037(2) 0.067(3) 0.050(3) 0.005(2) 0.0006(18) -0.012(2) C12 0.052(3) 0.109(5) 0.056(3) -0.008(3) -0.005(2) -0.028(3) C13 0.113(8) 0.265(17) 0.135(9) -0.060(9) -0.021(6) -0.013(9) C14 0.030(2) 0.215(9) 0.080(4) 0.063(5) -0.006(3) -0.027(4) N1 0.0307(15) 0.0442(18) 0.0246(13) 0.0034(12) -0.0042(11) -0.0066(13) N11 0.046(2) 0.110(4) 0.039(2) 0.012(2) -0.0053(16) -0.032(2) O11 0.0382(15) 0.091(3) 0.0369(15) 0.0149(15) -0.0005(12) -0.0210(15) Cl1 0.0436(5) 0.0392(5) 0.0359(4) -0.0028(4) 0.0039(4) 0.0026(4) Pt1 0.02595(10) 0.03503(11) 0.02380(8) 0.000 0.000 -0.00355(7) Cl2 0.274(3) 0.1423(19) 0.0496(9) -0.0238(11) -0.0477(15) 0.024(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.268(5) . ? C1 O11 1.359(5) . ? C1 C2 1.472(6) . ? C2 Cl2 1.740(6) . ? C11 N11 1.255(5) . ? C11 C14 1.484(7) . ? C11 C12 1.496(7) . ? C12 C13 1.414(14) . ? N1 Pt1 2.002(3) . ? N11 O11 1.461(5) . ? Cl1 Pt1 2.3098(10) . ? Pt1 N1 2.002(3) 2_765 ? Pt1 Cl1 2.3098(10) 2_765 ? 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 O11 125.1(4) . . ? N1 C1 C2 124.1(4) . . ? O11 C1 C2 110.8(3) . . ? C1 C2 Cl2 110.4(4) . . ? N11 C11 C14 124.4(5) . . ? N11 C11 C12 115.6(4) . . ? C14 C11 C12 120.0(4) . . ? C13 C12 C11 108.8(7) . . ? C1 N1 Pt1 125.9(3) . . ? C11 N11 O11 110.8(4) . . ? C1 O11 N11 110.5(3) . . ? N1 Pt1 N1 179.47(17) . 2_765 ? N1 Pt1 Cl1 89.99(10) . 2_765 ? N1 Pt1 Cl1 90.01(10) 2_765 2_765 ? N1 Pt1 Cl1 90.01(10) . . ? N1 Pt1 Cl1 89.99(10) 2_765 . ? Cl1 Pt1 Cl1 178.48(5) 2_765 . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 35.54 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.242 _refine_diff_density_min -1.109 _refine_diff_density_rms 0.146