Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Mats Tilset' 'Irene Fjeldahl' 'Christian Romming' 'Knut Thorshaug' _publ_contact_author_name 'Prof Mats Tilset' _publ_contact_author_address ; Department of Chemistry University of Oslo P.O.Box 1033 Blindern Oslo 0315 NORWAY ; _publ_contact_author_email MATS.TILSET@KJEMI.UIO.NO _publ_section_title ; Synthesis, characterization, and acid-base properties of (N N)PtIV(CH3)2(OH)2-x(OCH3)x (x = 0, 1) complexes ; data_8 _database_code_CSD 209032 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H28 N2 O4 Pt' _chemical_formula_weight 507.49 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2537(5) _cell_length_b 10.9870(9) _cell_length_c 12.0195(9) _cell_angle_alpha 81.881(3) _cell_angle_beta 87.298(3) _cell_angle_gamma 74.897(4) _cell_volume 915.50(12) _cell_formula_units_Z 2 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 7.683 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19278 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 40.31 _reflns_number_total 10219 _reflns_number_gt 9100 _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^)+(0.0391P)^2^+0.4871P] 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 10219 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.136 _refine_ls_shift/su_mean 0.003 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 0.219572(11) 0.244400(7) 0.765290(6) 0.01620(2) Uani 1 1 d . . . O1 O 0.5043(2) 0.22398(17) 0.76022(15) 0.0220(3) Uani 1 1 d . . . H1 H 0.5266 0.2916 0.7683 0.033 Uiso 1 1 calc R . . O2 O -0.0632(2) 0.25930(18) 0.77749(15) 0.0216(3) Uani 1 1 d . . . H2 H -0.0923 0.2160 0.7343 0.032 Uiso 1 1 calc R . . N1 N 0.2260(3) 0.23424(17) 0.94509(15) 0.0163(3) Uani 1 1 d . . . N2 N 0.2593(3) 0.04447(17) 0.82401(15) 0.0172(3) Uani 1 1 d . . . C1 C 0.2373(3) 0.1184(2) 1.00436(16) 0.0164(3) Uani 1 1 d . . . C2 C 0.2345(4) 0.1010(2) 1.12190(18) 0.0216(4) Uani 1 1 d . . . H2B H 0.2398 0.0211 1.1614 0.026 Uiso 1 1 calc R . . C3 C 0.2236(4) 0.2047(3) 1.1797(2) 0.0250(4) Uani 1 1 d . . . C4 C 0.2209(4) 0.3214(2) 1.1171(2) 0.0244(4) Uani 1 1 d . . . H4A H 0.2197 0.3914 1.1528 0.029 Uiso 1 1 calc R . . C5 C 0.2199(3) 0.3325(2) 1.0008(2) 0.0211(4) Uani 1 1 d . . . H5A H 0.2147 0.4117 0.9597 0.025 Uiso 1 1 calc R . . C6 C 0.2158(5) 0.1906(4) 1.3059(2) 0.0379(7) Uani 1 1 d . . . H6A H 0.3320 0.2010 1.3336 0.057 Uiso 1 1 calc R . . H6B H 0.2010 0.1077 1.3349 0.057 Uiso 1 1 calc R . . H6C H 0.1094 0.2542 1.3298 0.057 Uiso 1 1 calc R . . C7 C 0.2552(3) 0.01255(19) 0.93678(16) 0.0159(3) Uani 1 1 d . . . C8 C 0.2696(3) -0.1126(2) 0.98581(18) 0.0192(3) Uani 1 1 d . . . H8A H 0.2679 -0.1323 1.0636 0.023 Uiso 1 1 calc R . . C9 C 0.2868(3) -0.2085(2) 0.9176(2) 0.0210(4) Uani 1 1 d . . . C10 C 0.2875(4) -0.1729(2) 0.8018(2) 0.0254(4) Uani 1 1 d . . . H10A H 0.2977 -0.2334 0.7535 0.031 Uiso 1 1 calc R . . C11 C 0.2732(4) -0.0471(2) 0.75850(19) 0.0239(4) Uani 1 1 d . . . H11A H 0.2732 -0.0251 0.6809 0.029 Uiso 1 1 calc R . . C12 C 0.3022(4) -0.3434(2) 0.9680(3) 0.0287(5) Uani 1 1 d . . . H12A H 0.1787 -0.3523 0.9941 0.043 Uiso 1 1 calc R . . H12B H 0.3889 -0.3658 1.0299 0.043 Uiso 1 1 calc R . . H12C H 0.3489 -0.3988 0.9121 0.043 Uiso 1 1 calc R . . C13 C 0.1690(4) 0.4370(2) 0.7268(2) 0.0251(4) Uani 1 1 d . . . H13A H 0.1529 0.4602 0.6471 0.038 Uiso 1 1 calc R . . H13B H 0.2752 0.4639 0.7501 0.038 Uiso 1 1 calc R . . H13C H 0.0552 0.4776 0.7650 0.038 Uiso 1 1 calc R . . C14 C 0.2171(4) 0.2397(3) 0.5963(2) 0.0285(5) Uani 1 1 d . . . H14A H 0.2454 0.1530 0.5819 0.043 Uiso 1 1 calc R . . H14B H 0.3115 0.2793 0.5600 0.043 Uiso 1 1 calc R . . H14C H 0.0933 0.2847 0.5674 0.043 Uiso 1 1 calc R . . O21 O 0.7845(3) 0.1177(2) 0.63563(19) 0.0326(4) Uani 1 1 d . . . H21 H 0.6841 0.1471 0.6680 0.049 Uiso 1 1 calc R . . C21 C 0.7608(6) 0.1520(5) 0.5187(3) 0.0490(9) Uani 1 1 d . . . H21A H 0.7463 0.2418 0.5000 0.074 Uiso 1 1 calc R . . H21B H 0.6492 0.1307 0.4961 0.074 Uiso 1 1 calc R . . H21C H 0.8709 0.1067 0.4802 0.074 Uiso 1 1 calc R . . O22 O -0.3493(3) 0.45914(19) 0.75201(17) 0.0274(3) Uani 1 1 d . . . H22 H -0.2592 0.3959 0.7628 0.041 Uiso 1 1 calc R . . C22 C -0.3626(5) 0.5045(3) 0.6361(3) 0.0376(6) Uani 1 1 d . . . H22A H -0.4284 0.5932 0.6257 0.056 Uiso 1 1 calc R . . H22B H -0.4318 0.4578 0.6000 0.056 Uiso 1 1 calc R . . H22C H -0.2367 0.4933 0.6038 0.056 Uiso 1 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 Pt1 0.01653(3) 0.01718(3) 0.01470(3) 0.00062(2) -0.00087(2) -0.00531(2) O1 0.0168(7) 0.0239(7) 0.0254(7) -0.0006(6) 0.0000(5) -0.0066(6) O2 0.0167(7) 0.0256(7) 0.0228(7) -0.0029(6) -0.0010(5) -0.0060(6) N1 0.0167(7) 0.0160(6) 0.0170(7) -0.0024(5) -0.0009(5) -0.0050(5) N2 0.0188(7) 0.0171(7) 0.0158(7) -0.0015(5) -0.0009(5) -0.0048(6) C1 0.0169(8) 0.0182(8) 0.0149(7) -0.0019(6) -0.0006(6) -0.0060(6) C2 0.0270(10) 0.0242(9) 0.0157(8) -0.0030(7) 0.0019(7) -0.0105(8) C3 0.0288(11) 0.0323(11) 0.0181(9) -0.0086(8) 0.0019(7) -0.0128(9) C4 0.0257(10) 0.0260(10) 0.0247(10) -0.0105(8) 0.0017(8) -0.0087(8) C5 0.0219(9) 0.0193(8) 0.0236(9) -0.0053(7) -0.0008(7) -0.0068(7) C6 0.0526(19) 0.0489(17) 0.0196(11) -0.0125(11) 0.0050(10) -0.0229(14) C7 0.0160(8) 0.0162(7) 0.0157(7) -0.0011(6) -0.0004(5) -0.0047(6) C8 0.0199(9) 0.0183(8) 0.0189(8) 0.0011(6) -0.0003(6) -0.0062(7) C9 0.0203(9) 0.0181(8) 0.0250(9) -0.0018(7) -0.0001(7) -0.0064(7) C10 0.0333(12) 0.0204(9) 0.0238(10) -0.0061(8) -0.0008(8) -0.0071(8) C11 0.0346(12) 0.0207(9) 0.0165(8) -0.0040(7) -0.0009(7) -0.0067(8) C12 0.0309(12) 0.0173(9) 0.0382(13) -0.0006(9) 0.0015(10) -0.0084(8) C13 0.0253(11) 0.0182(9) 0.0312(11) 0.0025(8) -0.0028(8) -0.0073(8) C14 0.0366(13) 0.0341(12) 0.0154(9) 0.0010(8) -0.0016(8) -0.0122(10) O21 0.0274(9) 0.0364(10) 0.0352(10) -0.0127(8) 0.0012(7) -0.0063(8) C21 0.0391(18) 0.075(3) 0.0328(16) -0.0204(17) 0.0022(12) -0.0077(17) O22 0.0275(9) 0.0242(8) 0.0295(9) -0.0032(7) -0.0041(7) -0.0044(7) C22 0.0407(16) 0.0336(14) 0.0349(14) 0.0089(11) -0.0072(12) -0.0089(12) _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 2.0149(17) . ? Pt1 O1 2.0177(17) . ? Pt1 C14 2.040(2) . ? Pt1 C13 2.040(2) . ? Pt1 N1 2.1503(18) . ? Pt1 N2 2.1582(19) . ? O1 H1 0.8200 . ? O2 H2 0.8200 . ? N1 C5 1.339(3) . ? N1 C1 1.352(3) . ? N2 C11 1.344(3) . ? N2 C7 1.352(3) . ? C1 C2 1.399(3) . ? C1 C7 1.486(3) . ? C2 C3 1.398(3) . ? C2 H2B 0.9300 . ? C3 C4 1.388(4) . ? C3 C6 1.503(4) . ? C4 C5 1.385(3) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.397(3) . ? C8 C9 1.401(3) . ? C8 H8A 0.9300 . ? C9 C10 1.392(4) . ? C9 C12 1.498(3) . ? C10 C11 1.385(4) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? O21 C21 1.410(4) . ? O21 H21 0.8200 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? O22 C22 1.410(4) . ? O22 H22 0.8200 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? 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 177.24(7) . . ? O2 Pt1 C14 91.32(10) . . ? O1 Pt1 C14 90.85(10) . . ? O2 Pt1 C13 90.57(9) . . ? O1 Pt1 C13 91.27(9) . . ? C14 Pt1 C13 86.35(11) . . ? O2 Pt1 N1 88.64(7) . . ? O1 Pt1 N1 89.07(7) . . ? C14 Pt1 N1 175.75(9) . . ? C13 Pt1 N1 97.89(9) . . ? O2 Pt1 N2 86.78(7) . . ? O1 Pt1 N2 91.19(7) . . ? C14 Pt1 N2 99.44(10) . . ? C13 Pt1 N2 173.67(9) . . ? N1 Pt1 N2 76.31(7) . . ? Pt1 O1 H1 109.5 . . ? Pt1 O2 H2 109.5 . . ? C5 N1 C1 118.83(19) . . ? C5 N1 Pt1 125.10(16) . . ? C1 N1 Pt1 116.07(13) . . ? C11 N2 C7 118.43(19) . . ? C11 N2 Pt1 125.56(15) . . ? C7 N2 Pt1 115.82(13) . . ? N1 C1 C2 121.29(19) . . ? N1 C1 C7 115.80(17) . . ? C2 C1 C7 122.90(19) . . ? C3 C2 C1 119.6(2) . . ? C3 C2 H2B 120.2 . . ? C1 C2 H2B 120.2 . . ? C4 C3 C2 118.1(2) . . ? C4 C3 C6 120.7(2) . . ? C2 C3 C6 121.2(3) . . ? C5 C4 C3 119.3(2) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? N1 C5 C4 122.8(2) . . ? N1 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 121.69(18) . . ? N2 C7 C1 115.74(18) . . ? C8 C7 C1 122.56(18) . . ? C7 C8 C9 119.9(2) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C10 C9 C8 117.3(2) . . ? C10 C9 C12 121.7(2) . . ? C8 C9 C12 121.0(2) . . ? C11 C10 C9 120.0(2) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? N2 C11 C10 122.7(2) . . ? N2 C11 H11A 118.6 . . ? C10 C11 H11A 118.6 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Pt1 C13 H13A 109.5 . . ? Pt1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Pt1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Pt1 C14 H14A 109.5 . . ? Pt1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Pt1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C21 O21 H21 109.5 . . ? O21 C21 H21A 109.5 . . ? O21 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O21 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 O22 H22 109.5 . . ? O22 C22 H22A 109.5 . . ? O22 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O22 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 40.31 _diffrn_measured_fraction_theta_full 0.885 _refine_diff_density_max 3.787 _refine_diff_density_min -2.630 _refine_diff_density_rms 0.166