Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Armando Pombeiro' 'Cristina M. P. Ferreira' 'M. Fatima C. Guedes da Silva' 'Vadim Yu. Kukushkin' ; R.A.Michelin ; _publ_contact_author_name 'Prof Armando Pombeiro' _publ_contact_author_address ; Centro de Química Estrutural IST Complexo I, Av. Rovisco Pais Lisboa 1049-001 PORTUGAL ; _publ_contact_author_email POMBEIRO@IST.UTL.PT _publ_section_title ; 2-Amino-2-Oxazoline and Trialkylisourea Pt(II) Complexes Derived from Organocyanamides ; data_oxazoline2b _database_code_CSD 199088 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H28 Cl2 N4 O2 Pt' _chemical_formula_weight 550.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 12.192(2) _cell_length_b 8.263(2) _cell_length_c 29.793(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.74(3) _cell_angle_gamma 90.00 _cell_volume 2974.1(11) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12 _cell_measurement_theta_min 20. _cell_measurement_theta_max 24. _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 15.828 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.033 _exptl_absorpt_correction_T_max 0.141 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator beta-filter _diffrn_measurement_device_type 'Syntex P-1' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.1 _diffrn_reflns_number 3551 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 56.08 _reflns_number_total 3360 _reflns_number_gt 3360 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0448P)^2^+7.0325P] 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 SHELXL _refine_ls_extinction_coef 0.00065(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3360 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 0.11426(2) 0.06787(3) 0.092858(8) 0.04724(14) Uani 1 1 d . . . Pt2 Pt 0.5000 0.99201(5) 0.2500 0.05116(15) Uani 1 2 d S . . Cl1 Cl -0.04015(16) 0.2301(2) 0.08070(6) 0.0721(5) Uani 1 1 d . . . Cl2 Cl 0.22950(18) 0.2899(2) 0.10182(7) 0.0788(6) Uani 1 1 d . . . Cl3 Cl 0.37377(17) 0.7974(2) 0.26379(6) 0.0754(5) Uani 1 1 d . . . O1 O -0.1003(4) -0.3349(6) 0.08472(18) 0.0740(14) Uani 1 1 d . . . O2 O 0.3666(4) -0.2842(6) 0.09972(15) 0.0654(12) Uani 1 1 d . . . O3 O 0.2853(4) 1.3637(6) 0.28354(16) 0.0707(13) Uani 1 1 d . . . N1 N 0.0168(4) -0.1291(7) 0.08231(17) 0.0502(12) Uani 1 1 d . . . N2 N -0.0670(5) -0.1884(7) 0.1484(2) 0.0669(16) Uani 1 1 d . . . N3 N 0.2435(4) -0.0879(6) 0.10489(17) 0.0495(13) Uani 1 1 d . . . N4 N 0.3899(5) 1.1692(7) 0.25899(18) 0.0588(14) Uani 1 1 d . . . N5 N 0.3145(5) -0.1444(8) 0.03580(17) 0.0609(14) Uani 1 1 d . . . N6 N 0.3841(5) 1.2163(7) 0.33755(18) 0.0637(15) Uani 1 1 d . . . C1 C -0.0464(5) -0.2073(8) 0.1067(2) 0.0520(16) Uani 1 1 d . . . C2 C -0.0581(8) -0.3542(10) 0.0421(3) 0.082(2) Uani 1 1 d . . . C3 C 0.0085(6) -0.2020(9) 0.0376(2) 0.0666(19) Uani 1 1 d . . . C4 C 0.3032(5) -0.1654(8) 0.0793(2) 0.0512(16) Uani 1 1 d . . . C5 C 0.3438(6) -0.2967(9) 0.1462(2) 0.069(2) Uani 1 1 d . . . C6 C 0.2643(6) -0.1588(11) 0.1505(2) 0.069(2) Uani 1 1 d . . . C7 C 0.3581(5) 1.2412(8) 0.2937(2) 0.0549(16) Uani 1 1 d . . . C8 C 0.2689(8) 1.3773(11) 0.2346(3) 0.085(2) Uani 1 1 d . . . C9A C 0.3551(15) 1.271(2) 0.2167(6) 0.067(5) Uiso 0.50 1 d P . . C9B C 0.3177(14) 1.224(2) 0.2188(5) 0.061(4) Uiso 0.50 1 d P . . C10 C -0.0176(6) -0.0585(9) 0.1785(3) 0.0656(19) Uani 1 1 d . . . C11 C -0.1041(8) 0.0564(11) 0.1914(3) 0.086(3) Uani 1 1 d . . . C12 C -0.1190(8) -0.3223(10) 0.1713(3) 0.088(3) Uani 1 1 d . . . C13 C -0.0398(10) -0.4562(11) 0.1858(4) 0.104(3) Uani 1 1 d . . . C14 C 0.2618(6) -0.0158(10) 0.0078(2) 0.0620(18) Uani 1 1 d . . . C15 C 0.3417(7) 0.1169(11) 0.0009(3) 0.083(2) Uani 1 1 d . . . C16 C 0.3778(6) -0.2653(10) 0.0132(2) 0.072(2) Uani 1 1 d . . . C17 C 0.3095(8) -0.4134(11) -0.0007(3) 0.088(3) Uani 1 1 d . . . C18 C 0.3410(8) 1.3290(10) 0.3703(3) 0.079(2) Uani 1 1 d . . . C19 C 0.4115(11) 1.4762(13) 0.3783(4) 0.115(4) Uani 1 1 d . . . C20 C 0.4563(6) 1.0859(10) 0.3572(2) 0.071(2) Uani 1 1 d . . . C21 C 0.3959(8) 0.9572(11) 0.3789(3) 0.091(3) Uani 1 1 d . . . H21 H -0.0228 -0.4596 0.0422 0.080 Uiso 1 1 d . . . H22 H -0.1086 -0.3788 0.0159 0.080 Uiso 1 1 d . . . H31 H 0.0812 -0.2300 0.0309 0.080 Uiso 1 1 d . . . H32 H -0.0283 -0.1308 0.0151 0.080 Uiso 1 1 d . . . H51 H 0.3171 -0.4027 0.1516 0.080 Uiso 1 1 d . . . H52 H 0.4091 -0.2764 0.1675 0.080 Uiso 1 1 d . . . H61 H 0.1962 -0.1849 0.1614 0.080 Uiso 1 1 d . . . H62 H 0.3103 -0.0975 0.1734 0.080 Uiso 1 1 d . . . H81 H 0.2778 1.4861 0.2249 0.080 Uiso 1 1 d . . . H82 H 0.1892 1.3838 0.2262 0.080 Uiso 1 1 d . . . H101 H 0.0371 -0.0056 0.1639 0.080 Uiso 1 1 d . . . H102 H 0.0204 -0.1081 0.2055 0.080 Uiso 1 1 d . . . H111 H -0.1220 0.1202 0.1647 0.080 Uiso 1 1 d . . . H112 H -0.1585 0.0040 0.2068 0.080 Uiso 1 1 d . . . H113 H -0.0575 0.1301 0.2106 0.080 Uiso 1 1 d . . . H121 H -0.1446 -0.2765 0.1974 0.080 Uiso 1 1 d . . . H122 H -0.1791 -0.3705 0.1514 0.080 Uiso 1 1 d . . . H131 H 0.0135 -0.4849 0.1666 0.080 Uiso 1 1 d . . . H132 H -0.0721 -0.5472 0.1993 0.080 Uiso 1 1 d . . . H133 H 0.0281 -0.4110 0.2007 0.080 Uiso 1 1 d . . . H141 H 0.2005 0.0229 0.0212 0.080 Uiso 1 1 d . . . H142 H 0.2288 -0.0662 -0.0201 0.080 Uiso 1 1 d . . . H151 H 0.3064 0.1974 -0.0197 0.080 Uiso 1 1 d . . . H152 H 0.4017 0.0686 -0.0117 0.080 Uiso 1 1 d . . . H153 H 0.3514 0.1862 0.0272 0.080 Uiso 1 1 d . . . H161 H 0.4494 -0.2788 0.0306 0.080 Uiso 1 1 d . . . H162 H 0.3916 -0.2251 -0.0157 0.080 Uiso 1 1 d . . . H171 H 0.2812 -0.4547 0.0254 0.080 Uiso 1 1 d . . . H172 H 0.3563 -0.4705 -0.0189 0.080 Uiso 1 1 d . . . H173 H 0.2575 -0.3679 -0.0245 0.080 Uiso 1 1 d . . . H181 H 0.2654 1.3628 0.3634 0.080 Uiso 1 1 d . . . H182 H 0.3401 1.2811 0.3993 0.080 Uiso 1 1 d . . . H191 H 0.3712 1.5341 0.3993 0.080 Uiso 1 1 d . . . H192 H 0.4256 1.5171 0.3501 0.080 Uiso 1 1 d . . . H193 H 0.4862 1.4401 0.3883 0.080 Uiso 1 1 d . . . H201 H 0.5126 1.1407 0.3775 0.080 Uiso 1 1 d . . . H202 H 0.5004 1.0619 0.3345 0.080 Uiso 1 1 d . . . H211 H 0.4368 0.8672 0.3923 0.080 Uiso 1 1 d . . . H212 H 0.3476 1.0098 0.3971 0.080 Uiso 1 1 d . . . H213 H 0.3305 0.9272 0.3578 0.080 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 0.0588(2) 0.03938(19) 0.04239(19) 0.00089(10) 0.00281(12) -0.00624(12) Pt2 0.0617(3) 0.0566(3) 0.0360(2) 0.000 0.00941(17) 0.000 Cl1 0.0896(13) 0.0539(10) 0.0703(11) 0.0006(8) 0.0012(9) 0.0146(9) Cl2 0.1005(14) 0.0580(11) 0.0743(12) 0.0009(9) -0.0016(10) -0.0313(10) Cl3 0.0928(13) 0.0776(13) 0.0578(10) 0.0023(9) 0.0175(9) -0.0217(10) O1 0.076(3) 0.060(3) 0.089(4) -0.014(3) 0.022(3) -0.027(3) O2 0.073(3) 0.069(3) 0.055(3) 0.006(2) 0.010(2) 0.008(3) O3 0.086(3) 0.064(3) 0.064(3) 0.004(3) 0.017(3) 0.017(3) N1 0.049(3) 0.054(3) 0.047(3) -0.001(3) 0.007(2) -0.001(3) N2 0.072(4) 0.060(4) 0.074(4) -0.004(3) 0.032(3) -0.008(3) N3 0.052(3) 0.049(3) 0.047(3) 0.001(2) 0.005(3) -0.005(2) N4 0.067(4) 0.068(4) 0.041(3) 0.009(3) 0.005(3) 0.005(3) N5 0.068(3) 0.072(4) 0.043(3) 0.004(3) 0.008(3) 0.001(3) N6 0.080(4) 0.066(4) 0.047(3) -0.002(3) 0.013(3) 0.008(3) C1 0.046(3) 0.048(4) 0.063(4) -0.001(3) 0.011(3) 0.002(3) C2 0.110(6) 0.056(5) 0.080(5) -0.016(4) 0.011(5) -0.022(5) C3 0.079(5) 0.061(5) 0.058(4) -0.005(3) 0.005(4) -0.017(4) C4 0.050(4) 0.051(4) 0.049(4) 0.007(3) -0.004(3) -0.008(3) C5 0.087(5) 0.067(5) 0.050(4) 0.006(3) 0.008(4) 0.009(4) C6 0.069(4) 0.093(6) 0.045(4) 0.008(4) 0.004(3) 0.018(4) C7 0.062(4) 0.055(4) 0.050(4) 0.002(3) 0.014(3) -0.003(3) C8 0.107(6) 0.075(6) 0.074(5) 0.014(4) 0.011(5) 0.022(5) C10 0.070(5) 0.067(5) 0.063(4) -0.003(4) 0.021(4) -0.001(4) C11 0.099(6) 0.071(6) 0.091(6) -0.004(5) 0.023(5) 0.010(5) C12 0.113(7) 0.063(5) 0.098(6) -0.001(5) 0.055(5) -0.016(5) C13 0.152(9) 0.064(6) 0.108(8) 0.018(5) 0.055(7) -0.013(6) C14 0.060(4) 0.075(5) 0.052(4) 0.014(4) 0.013(3) 0.002(4) C15 0.093(6) 0.070(5) 0.089(6) 0.007(5) 0.026(5) -0.009(5) C16 0.083(5) 0.077(5) 0.056(4) -0.001(4) 0.017(4) -0.007(4) C17 0.125(8) 0.072(6) 0.068(5) -0.002(4) 0.017(5) -0.015(5) C18 0.117(7) 0.064(5) 0.060(4) -0.009(4) 0.028(4) -0.001(5) C19 0.166(11) 0.090(7) 0.095(7) -0.029(6) 0.036(7) -0.022(7) C20 0.074(5) 0.089(6) 0.050(4) -0.002(4) 0.009(4) 0.010(4) C21 0.114(7) 0.086(6) 0.077(6) 0.027(5) 0.026(5) 0.033(5) _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(5) . ? Pt1 N3 2.029(5) . ? Pt1 Cl1 2.2996(19) . ? Pt1 Cl2 2.3042(18) . ? Pt2 N4 2.029(6) 2_655 ? Pt2 N4 2.029(6) . ? Pt2 Cl3 2.3008(19) . ? Pt2 Cl3 2.3008(19) 2_655 ? O1 C1 1.362(8) . ? O1 C2 1.441(9) . ? O2 C4 1.344(8) . ? O2 C5 1.451(8) . ? O3 C7 1.353(8) . ? O3 C8 1.450(9) . ? N1 C1 1.301(8) . ? N1 C3 1.453(9) . ? N2 C1 1.307(8) . ? N2 C10 1.475(9) . ? N2 C12 1.486(9) . ? N3 C4 1.293(8) . ? N3 C6 1.471(8) . ? N4 C7 1.297(8) . ? N4 C9B 1.459(16) . ? N4 C9A 1.526(18) . ? N5 C4 1.332(8) . ? N5 C14 1.447(9) . ? N5 C16 1.480(10) . ? N6 C7 1.319(8) . ? N6 C20 1.462(9) . ? N6 C18 1.494(9) . ? C2 C3 1.513(11) . ? C5 C6 1.513(10) . ? C8 C9B 1.502(18) . ? C8 C9A 1.521(18) . ? C9A C9B 0.61(2) . ? C10 C11 1.506(11) . ? C12 C13 1.494(14) . ? C14 C15 1.499(11) . ? C16 C17 1.506(11) . ? C18 C19 1.490(13) . ? C20 C21 1.490(12) . ? 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 N3 86.7(2) . . ? N1 Pt1 Cl1 89.61(16) . . ? N3 Pt1 Cl1 175.96(15) . . ? N1 Pt1 Cl2 177.22(15) . . ? N3 Pt1 Cl2 92.15(15) . . ? Cl1 Pt1 Cl2 91.58(8) . . ? N4 Pt2 N4 87.6(3) 2_655 . ? N4 Pt2 Cl3 176.95(15) 2_655 . ? N4 Pt2 Cl3 90.60(17) . . ? N4 Pt2 Cl3 90.60(17) 2_655 2_655 ? N4 Pt2 Cl3 176.95(16) . 2_655 ? Cl3 Pt2 Cl3 91.32(11) . 2_655 ? C1 O1 C2 107.7(5) . . ? C4 O2 C5 108.2(5) . . ? C7 O3 C8 106.3(5) . . ? C1 N1 C3 109.5(6) . . ? C1 N1 Pt1 134.1(5) . . ? C3 N1 Pt1 116.4(4) . . ? C1 N2 C10 123.4(6) . . ? C1 N2 C12 119.6(6) . . ? C10 N2 C12 115.2(6) . . ? C4 N3 C6 107.9(5) . . ? C4 N3 Pt1 134.1(4) . . ? C6 N3 Pt1 116.7(4) . . ? C7 N4 C9B 107.5(8) . . ? C7 N4 C9A 109.1(8) . . ? C9B N4 C9A 23.4(8) . . ? C7 N4 Pt2 135.3(5) . . ? C9B N4 Pt2 116.9(7) . . ? C9A N4 Pt2 113.8(7) . . ? C4 N5 C14 124.1(6) . . ? C4 N5 C16 118.9(6) . . ? C14 N5 C16 116.8(5) . . ? C7 N6 C20 124.3(6) . . ? C7 N6 C18 119.4(6) . . ? C20 N6 C18 116.3(6) . . ? N1 C1 N2 132.4(6) . . ? N1 C1 O1 113.5(6) . . ? N2 C1 O1 114.1(6) . . ? O1 C2 C3 104.2(6) . . ? N1 C3 C2 103.6(6) . . ? N3 C4 N5 130.5(6) . . ? N3 C4 O2 115.4(6) . . ? N5 C4 O2 114.1(6) . . ? O2 C5 C6 103.6(5) . . ? N3 C6 C5 104.6(5) . . ? N4 C7 N6 131.3(7) . . ? N4 C7 O3 115.0(6) . . ? N6 C7 O3 113.7(6) . . ? O3 C8 C9B 104.0(8) . . ? O3 C8 C9A 107.4(8) . . ? C9B C8 C9A 23.2(8) . . ? C9B C9A C8 77(3) . . ? C9B C9A N4 72(3) . . ? C8 C9A N4 99.0(10) . . ? C9A C9B N4 85(3) . . ? C9A C9B C8 80(3) . . ? N4 C9B C8 103.0(10) . . ? N2 C10 C11 111.8(7) . . ? N2 C12 C13 112.6(7) . . ? N5 C14 C15 111.7(6) . . ? N5 C16 C17 111.8(7) . . ? C19 C18 N6 111.5(7) . . ? N6 C20 C21 113.1(7) . . ? _diffrn_measured_fraction_theta_max 0.865 _diffrn_reflns_theta_full 56.08 _diffrn_measured_fraction_theta_full 0.865 _refine_diff_density_max 1.345 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.093