# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address 'Biprajit Sarkar' ;Institut f\"ur Anorganische Chemie Universit\"at Stuttgart Pfaffenwaldring 55 70569 Stuttgart ; 'Ingo Hartenbach' '' 'Ralph Hubner' '' 'Roberto Pattacini' '' _publ_contact_author_name 'Biprajit Sarkar' _publ_contact_author_email SARKAR@IAC.UNI-STUTTGART.DE _publ_section_title ; Combining Two Non-Innocent Ligands in Isomeric Complexes [Pt(pap)mQn]0 (pap = Phenylazopyridine, Q = 3,5-Di-tert-butyl-benzoquinone ; _publ_contact_author_address ;Institut f\"ur Anorganische Chemie Universit\"at Stuttgart Pfaffenwaldring 55 70569 Stuttgart Germany ; _publ_contact_author_fax '+49 711 68564165' _publ_contact_author_phone '+49 711 68564235' # Attachment '1a_revised.cif' data_Bipro2 _database_code_depnum_ccdc_archive 'CCDC 719277' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H29 N3 O2 Pt' _chemical_formula_sum 'C25 H29 N3 O2 Pt' _chemical_formula_weight 598.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9677(3) _cell_length_b 10.7867(6) _cell_length_c 15.6342(7) _cell_angle_alpha 101.695(2) _cell_angle_beta 95.843(3) _cell_angle_gamma 91.407(2) _cell_volume 1143.44(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6022 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 6.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.423 _exptl_absorpt_correction_T_max 0.540 _exptl_absorpt_process_details 'L. Spek, J. Appl.Cryst. 2003, 36, 7, B. Blessing, Acta Cryst, 1995, A51, 33' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9059 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 29.99 _reflns_number_total 6626 _reflns_number_gt 5701 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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^)+(0.0620P)^2^+0.0000P] 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 6626 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_restrained_S_all 1.206 _refine_ls_shift/su_max 0.002 _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 0.25582(3) 0.11812(2) 0.463629(13) 0.01971(8) Uani 1 1 d . . . O1 O 0.2755(7) 0.1539(4) 0.3445(3) 0.0247(9) Uani 1 1 d . . . O2 O 0.2758(6) -0.0581(4) 0.4017(3) 0.0249(9) Uani 1 1 d . . . N1 N 0.2345(7) 0.2885(5) 0.5379(3) 0.0208(10) Uani 1 1 d . . . N2 N 0.2359(7) 0.0778(5) 0.5796(3) 0.0200(10) Uani 1 1 d . . . N3 N 0.2201(8) 0.2979(5) 0.6216(3) 0.0249(11) Uani 1 1 d . . . C1 C 0.2797(9) 0.0456(6) 0.2828(4) 0.0221(12) Uani 1 1 d . . . C2 C 0.2833(8) -0.0685(6) 0.3145(4) 0.0213(11) Uani 1 1 d . . . C3 C 0.2870(9) -0.1845(6) 0.2581(4) 0.0244(12) Uani 1 1 d . . . H3 H 0.2940 -0.2581 0.2804 0.029 Uiso 1 1 calc R . . C4 C 0.2802(9) -0.1917(6) 0.1677(4) 0.0243(12) Uani 1 1 d . . . C5 C 0.2759(9) -0.0782(6) 0.1378(4) 0.0264(13) Uani 1 1 d . . . H5 H 0.2724 -0.0825 0.0777 0.032 Uiso 1 1 calc R . . C6 C 0.2765(9) 0.0404(6) 0.1922(4) 0.0235(12) Uani 1 1 d . . . C7 C 0.2766(9) -0.3219(6) 0.1060(4) 0.0263(13) Uani 1 1 d . . . C8 C 0.1018(13) -0.4031(8) 0.1201(5) 0.047(2) Uani 1 1 d . . . H8A H 0.1082 -0.4083 0.1809 0.070 Uiso 1 1 calc R . . H8B H 0.1040 -0.4866 0.0846 0.070 Uiso 1 1 calc R . . H8C H -0.0155 -0.3647 0.1038 0.070 Uiso 1 1 calc R . . C9 C 0.4618(14) -0.3919(8) 0.1261(5) 0.055(2) Uani 1 1 d . . . H9A H 0.5721 -0.3456 0.1143 0.083 Uiso 1 1 calc R . . H9B H 0.4529 -0.4754 0.0897 0.083 Uiso 1 1 calc R . . H9C H 0.4752 -0.3981 0.1868 0.083 Uiso 1 1 calc R . . C10 C 0.2540(11) -0.3136(7) 0.0088(4) 0.0361(16) Uani 1 1 d . . . H10A H 0.1334 -0.2770 -0.0050 0.054 Uiso 1 1 calc R . . H10B H 0.2559 -0.3971 -0.0270 0.054 Uiso 1 1 calc R . . H10C H 0.3584 -0.2616 -0.0025 0.054 Uiso 1 1 calc R . . C11 C 0.2661(10) 0.1633(7) 0.1558(4) 0.0292(14) Uani 1 1 d . . . C12 C 0.0763(11) 0.2280(7) 0.1775(5) 0.0354(15) Uani 1 1 d . . . H12A H 0.0724 0.2465 0.2400 0.053 Uiso 1 1 calc R . . H12B H -0.0319 0.1724 0.1499 0.053 Uiso 1 1 calc R . . H12C H 0.0706 0.3054 0.1561 0.053 Uiso 1 1 calc R . . C13 C 0.4407(11) 0.2542(7) 0.1972(5) 0.0397(18) Uani 1 1 d . . . H13A H 0.4407 0.2741 0.2599 0.060 Uiso 1 1 calc R . . H13B H 0.4320 0.3307 0.1749 0.060 Uiso 1 1 calc R . . H13C H 0.5581 0.2142 0.1826 0.060 Uiso 1 1 calc R . . C14 C 0.2640(11) 0.1364(7) 0.0548(5) 0.0364(16) Uani 1 1 d . . . H14A H 0.2784 0.2150 0.0357 0.055 Uiso 1 1 calc R . . H14B H 0.1436 0.0938 0.0280 0.055 Uiso 1 1 calc R . . H14C H 0.3686 0.0838 0.0379 0.055 Uiso 1 1 calc R . . C15 C 0.2179(9) 0.1802(6) 0.6449(4) 0.0237(12) Uani 1 1 d . . . C16 C 0.1948(10) 0.1689(7) 0.7285(4) 0.0303(14) Uani 1 1 d . . . H16 H 0.1786 0.2402 0.7714 0.036 Uiso 1 1 calc R . . C17 C 0.1959(10) 0.0495(7) 0.7486(5) 0.0329(15) Uani 1 1 d . . . H17 H 0.1823 0.0396 0.8055 0.039 Uiso 1 1 calc R . . C18 C 0.2177(10) -0.0545(7) 0.6830(4) 0.0307(14) Uani 1 1 d . . . H18 H 0.2199 -0.1354 0.6953 0.037 Uiso 1 1 calc R . . C19 C 0.2361(9) -0.0372(6) 0.5989(4) 0.0272(13) Uani 1 1 d . . . H19 H 0.2489 -0.1075 0.5546 0.033 Uiso 1 1 calc R . . C20 C 0.2399(9) 0.4088(6) 0.5122(4) 0.0244(12) Uani 1 1 d . . . C21 C 0.3189(9) 0.5154(6) 0.5707(4) 0.0249(12) Uani 1 1 d . . . H21 H 0.3653 0.5115 0.6280 0.030 Uiso 1 1 calc R . . C22 C 0.3269(9) 0.6272(6) 0.5419(4) 0.0272(13) Uani 1 1 d . . . H22 H 0.3818 0.6998 0.5801 0.033 Uiso 1 1 calc R . . C23 C 0.2553(9) 0.6344(6) 0.4577(4) 0.0301(15) Uani 1 1 d . . . H23 H 0.2621 0.7112 0.4396 0.036 Uiso 1 1 calc R . . C24 C 0.1736(10) 0.5275(6) 0.4002(4) 0.0284(13) Uani 1 1 d . . . H24 H 0.1241 0.5325 0.3435 0.034 Uiso 1 1 calc R . . C25 C 0.1652(9) 0.4136(6) 0.4266(4) 0.0249(12) Uani 1 1 d . . . H25 H 0.1108 0.3411 0.3882 0.030 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 0.02222(13) 0.01504(12) 0.02116(12) 0.00269(8) 0.00114(8) 0.00085(8) O1 0.033(2) 0.017(2) 0.025(2) 0.0034(17) 0.0059(17) 0.0025(18) O2 0.035(2) 0.018(2) 0.022(2) 0.0041(16) 0.0015(17) 0.0022(18) N1 0.023(2) 0.015(2) 0.023(2) -0.0006(19) 0.0010(19) 0.0029(19) N2 0.017(2) 0.017(2) 0.025(2) 0.0049(19) -0.0013(18) 0.0020(18) N3 0.029(3) 0.018(3) 0.027(3) 0.003(2) 0.004(2) 0.003(2) C1 0.022(3) 0.014(3) 0.028(3) 0.001(2) 0.000(2) 0.001(2) C2 0.022(3) 0.021(3) 0.021(3) 0.004(2) 0.000(2) 0.001(2) C3 0.030(3) 0.018(3) 0.025(3) 0.006(2) 0.003(2) 0.001(2) C4 0.026(3) 0.019(3) 0.025(3) 0.000(2) 0.001(2) -0.001(2) C5 0.036(3) 0.021(3) 0.022(3) 0.004(2) 0.006(2) 0.003(3) C6 0.026(3) 0.015(3) 0.028(3) 0.004(2) 0.002(2) 0.001(2) C7 0.033(3) 0.023(3) 0.021(3) 0.002(2) 0.002(2) 0.000(3) C8 0.063(5) 0.032(4) 0.038(4) -0.011(3) 0.014(4) -0.021(4) C9 0.074(6) 0.037(5) 0.043(4) -0.012(4) -0.010(4) 0.026(4) C10 0.051(4) 0.030(4) 0.024(3) -0.003(3) 0.006(3) 0.000(3) C11 0.039(4) 0.025(3) 0.026(3) 0.012(3) 0.001(3) 0.003(3) C12 0.042(4) 0.030(4) 0.036(4) 0.011(3) 0.002(3) 0.010(3) C13 0.052(5) 0.031(4) 0.038(4) 0.015(3) 0.000(3) -0.011(3) C14 0.050(4) 0.030(4) 0.032(4) 0.012(3) 0.006(3) 0.004(3) C15 0.022(3) 0.023(3) 0.026(3) 0.003(2) 0.002(2) 0.001(2) C16 0.035(4) 0.030(4) 0.026(3) 0.005(3) 0.007(3) 0.001(3) C17 0.036(4) 0.035(4) 0.029(3) 0.008(3) 0.004(3) -0.002(3) C18 0.034(3) 0.029(4) 0.031(3) 0.011(3) 0.002(3) 0.002(3) C19 0.034(3) 0.016(3) 0.033(3) 0.008(2) 0.005(3) 0.000(2) C20 0.023(3) 0.022(3) 0.029(3) 0.004(2) 0.005(2) 0.003(2) C21 0.024(3) 0.020(3) 0.030(3) 0.003(2) 0.005(2) 0.002(2) C22 0.028(3) 0.020(3) 0.033(3) -0.001(2) 0.009(3) 0.003(2) C23 0.034(4) 0.020(3) 0.039(4) 0.008(3) 0.010(3) 0.004(3) C24 0.035(3) 0.019(3) 0.033(3) 0.007(3) 0.007(3) 0.007(3) C25 0.021(3) 0.019(3) 0.035(3) 0.005(2) 0.004(2) 0.005(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 N2 1.966(5) . ? Pt1 O2 1.966(5) . ? Pt1 N1 1.983(5) . ? Pt1 O1 1.994(4) . ? O1 C1 1.360(7) . ? O2 C2 1.353(7) . ? N1 N3 1.307(7) . ? N1 C20 1.435(8) . ? N2 C19 1.334(8) . ? N2 C15 1.362(8) . ? N3 C15 1.390(8) . ? C1 C6 1.405(9) . ? C1 C2 1.416(8) . ? C2 C3 1.379(9) . ? C3 C4 1.395(8) . ? C3 H3 0.9300 . ? C4 C5 1.396(9) . ? C4 C7 1.532(9) . ? C5 C6 1.385(9) . ? C5 H5 0.9300 . ? C6 C11 1.545(8) . ? C7 C10 1.533(8) . ? C7 C8 1.542(9) . ? C7 C9 1.548(10) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C13 1.544(10) . ? C11 C14 1.545(9) . ? C11 C12 1.546(10) . ? 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 . ? C15 C16 1.362(9) . ? C16 C17 1.386(10) . ? C16 H16 0.9300 . ? C17 C18 1.381(10) . ? C17 H17 0.9300 . ? C18 C19 1.384(9) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.379(9) . ? C20 C25 1.397(9) . ? C21 C22 1.373(9) . ? C21 H21 0.9300 . ? C22 C23 1.378(9) . ? C22 H22 0.9300 . ? C23 C24 1.380(9) . ? C23 H23 0.9300 . ? C24 C25 1.375(8) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? 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 N2 Pt1 O2 95.60(19) . . ? N2 Pt1 N1 78.1(2) . . ? O2 Pt1 N1 173.74(17) . . ? N2 Pt1 O1 178.42(18) . . ? O2 Pt1 O1 82.84(17) . . ? N1 Pt1 O1 103.4(2) . . ? C1 O1 Pt1 111.8(4) . . ? C2 O2 Pt1 112.5(4) . . ? N3 N1 C20 113.3(5) . . ? N3 N1 Pt1 118.7(4) . . ? C20 N1 Pt1 128.0(4) . . ? C19 N2 C15 118.7(5) . . ? C19 N2 Pt1 126.7(5) . . ? C15 N2 Pt1 114.5(4) . . ? N1 N3 C15 112.1(5) . . ? O1 C1 C6 124.7(5) . . ? O1 C1 C2 115.9(5) . . ? C6 C1 C2 119.4(6) . . ? O2 C2 C3 121.9(5) . . ? O2 C2 C1 116.8(5) . . ? C3 C2 C1 121.2(5) . . ? C2 C3 C4 120.2(6) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 117.6(6) . . ? C3 C4 C7 119.4(5) . . ? C5 C4 C7 123.0(5) . . ? C6 C5 C4 124.1(6) . . ? C6 C5 H5 117.9 . . ? C4 C5 H5 117.9 . . ? C5 C6 C1 117.4(5) . . ? C5 C6 C11 122.2(6) . . ? C1 C6 C11 120.4(6) . . ? C4 C7 C10 112.7(5) . . ? C4 C7 C8 109.2(5) . . ? C10 C7 C8 106.8(6) . . ? C4 C7 C9 110.7(5) . . ? C10 C7 C9 109.4(6) . . ? C8 C7 C9 107.9(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C6 110.1(5) . . ? C13 C11 C14 108.8(6) . . ? C6 C11 C14 112.0(6) . . ? C13 C11 C12 109.8(6) . . ? C6 C11 C12 109.2(5) . . ? C14 C11 C12 107.0(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 122.2(6) . . ? N2 C15 N3 116.5(5) . . ? C16 C15 N3 121.2(6) . . ? C15 C16 C17 119.0(7) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C18 C17 C16 119.0(6) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C19 119.3(6) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? N2 C19 C18 121.7(6) . . ? N2 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C21 C20 C25 121.7(6) . . ? C21 C20 N1 120.2(6) . . ? C25 C20 N1 118.0(5) . . ? C22 C21 C20 118.0(6) . . ? C22 C21 H21 121.0 . . ? C20 C21 H21 121.0 . . ? C21 C22 C23 121.5(6) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C24 120.0(6) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.1(6) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C20 118.8(6) . . ? C24 C25 H25 120.6 . . ? C20 C25 H25 120.6 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.627 _refine_diff_density_min -2.276 _refine_diff_density_rms 0.436 # Attachment '1b_revised.cif' data_bsapr08 _database_code_depnum_ccdc_archive 'CCDC 719278' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H29 N3 O2 Pt' _chemical_formula_sum 'C25 H29 N3 O2 Pt' _chemical_formula_weight 598.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 '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' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P42/mbc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'y+1/2, x+1/2, -z+1/2' 'y, -x, z+1/2' '-y, x, z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-y-1/2, -x-1/2, z-1/2' '-y, x, -z-1/2' 'y, -x, -z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 26.8885(12) _cell_length_b 26.8885(12) _cell_length_c 6.7983(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4915.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6242 _cell_measurement_theta_min 23.11 _cell_measurement_theta_max 0.998 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 5.734 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.36 _exptl_absorpt_correction_T_max 0.71 _exptl_absorpt_process_details 'SCALEPACK (W. Minor & Z. Otwinowski)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius Kappa-CCD' _diffrn_measurement_method 'four-circle, ccd detector' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6555 _diffrn_reflns_av_R_equivalents 0.1097 _diffrn_reflns_av_sigmaI/netI 0.0870 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 23.24 _reflns_number_total 1938 _reflns_number_gt 1388 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'DENZO (W. Minor & Z. Otwinowski)' _computing_data_reduction 'DENZO & SCALEPACK (Minor & Otwinowski)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. The crystals of 1b were of poor quality. This resulted in a low maximum theta ?value. The thermal parameters of several atoms where then refined with restrained anisotropic parameters (Shelxl SIMU and ISOR). The structure was solved in the monoclinic system (P21/a) in order to check the correctness of the P42/mbc assignement. A PLATON ADDSYM procedure confirmed the chosen Tetragonal space group. Although solvent accessible voids were found, no atom was found in the difference map, the highest peak included in those coordinates bein 0.8 e/A3. ; _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^)+(0.0444P)^2^+17.9226P] 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 SHELXL _refine_ls_extinction_coef 0.00054(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1938 _refine_ls_number_parameters 186 _refine_ls_number_restraints 168 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.008 _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 Pt Pt 0.28882(2) 0.25773(2) 0.0000 0.0218(2) Uani 1 2 d S . . N1 N 0.2202(4) 0.2841(4) 0.0000 0.019(3) Uani 1 2 d SU . . N2 N 0.2494(4) 0.1974(4) 0.0000 0.027(3) Uani 1 2 d S . . N3 N 0.1846(4) 0.2529(4) 0.0000 0.017(3) Uani 1 2 d SU . . O1 O 0.3539(3) 0.2228(3) 0.0000 0.025(2) Uani 1 2 d SU . . O2 O 0.3306(3) 0.3185(3) 0.0000 0.022(2) Uani 1 2 d SU . . C1 C 0.3928(5) 0.2552(5) 0.0000 0.018(3) Uani 1 2 d SU . . C2 C 0.3800(5) 0.3050(5) 0.0000 0.022(3) Uani 1 2 d SU . . C3 C 0.4160(5) 0.3429(5) 0.0000 0.027(3) Uani 1 2 d SU . . H3 H 0.4065 0.3761 0.0000 0.032 Uiso 1 2 calc SR . . C4 C 0.4662(5) 0.3300(5) 0.0000 0.024(3) Uani 1 2 d SU . . C5 C 0.4787(5) 0.2789(5) 0.0000 0.020(3) Uani 1 2 d SU . . H5 H 0.5121 0.2699 0.0000 0.024 Uiso 1 2 calc SR . . C6 C 0.4429(6) 0.2415(5) 0.0000 0.031(3) Uani 1 2 d SU . . C7 C 0.5082(5) 0.3675(5) 0.0000 0.017(3) Uani 1 2 d SU . . C8 C 0.4899(5) 0.4221(6) 0.0000 0.044(5) Uani 1 2 d S . . H8A H 0.4777 0.4306 -0.1284 0.066 Uiso 0.50 1 calc PR . . H8B H 0.5170 0.4438 0.0338 0.066 Uiso 0.50 1 calc PR . . H8C H 0.4637 0.4259 0.0946 0.066 Uiso 0.50 1 calc PR . . C9 C 0.5402(3) 0.3603(4) 0.1837(15) 0.032(3) Uani 1 1 d . . . H9A H 0.5215 0.3697 0.2980 0.048 Uiso 1 1 calc R . . H9B H 0.5694 0.3807 0.1742 0.048 Uiso 1 1 calc R . . H9C H 0.5498 0.3260 0.1942 0.048 Uiso 1 1 calc R . . C11 C 0.4571(5) 0.1848(5) 0.0000 0.019(3) Uani 1 2 d SU . . C12 C 0.5153(5) 0.1779(6) 0.0000 0.036(4) Uani 1 2 d S . . H12A H 0.5232 0.1432 0.0127 0.055 Uiso 0.50 1 calc PR . . H12B H 0.5294 0.1959 0.1084 0.055 Uiso 0.50 1 calc PR . . H12C H 0.5288 0.1904 -0.1211 0.055 Uiso 0.50 1 calc PR . . C13 C 0.4354(4) 0.1607(4) -0.1861(15) 0.036(3) Uani 1 1 d . . . H13A H 0.4436 0.1260 -0.1879 0.054 Uiso 1 1 calc R . . H13B H 0.4491 0.1766 -0.3003 0.054 Uiso 1 1 calc R . . H13C H 0.3999 0.1645 -0.1863 0.054 Uiso 1 1 calc R . . C15 C 0.1993(5) 0.2050(5) 0.0000 0.019(3) Uani 1 2 d SU . . C16 C 0.1655(6) 0.1644(6) 0.0000 0.034(4) Uani 1 2 d SU . . H16 H 0.1314 0.1700 0.0000 0.040 Uiso 1 2 calc SR . . C17 C 0.1834(6) 0.1178(6) 0.0000 0.035(4) Uani 1 2 d SU . . H17 H 0.1616 0.0910 0.0000 0.042 Uiso 1 2 calc SR . . C18 C 0.2338(6) 0.1095(6) 0.0000 0.032(4) Uani 1 2 d SU . . H18 H 0.2458 0.0771 0.0000 0.039 Uiso 1 2 calc SR . . C19 C 0.2667(6) 0.1490(5) 0.0000 0.024(4) Uani 1 2 d SU . . H19 H 0.3008 0.1430 0.0000 0.029 Uiso 1 2 calc SR . . C20 C 0.2058(5) 0.3347(5) 0.0000 0.031(4) Uani 1 2 d SU . . C21 C 0.1553(6) 0.3466(6) 0.0000 0.053(4) Uani 1 2 d SU . . H21 H 0.1318 0.3211 0.0000 0.064 Uiso 1 2 calc SR . . C22 C 0.1398(6) 0.3951(6) 0.0000 0.045(4) Uani 1 2 d SU . . H22 H 0.1060 0.4023 0.0000 0.053 Uiso 1 2 calc SR . . C23 C 0.1722(5) 0.4319(5) 0.0000 0.034(4) Uani 1 2 d SU . . H23 H 0.1615 0.4648 0.0000 0.041 Uiso 1 2 calc SR . . C24 C 0.2221(6) 0.4210(6) 0.0000 0.053(4) Uani 1 2 d SU . . H24 H 0.2454 0.4465 0.0000 0.064 Uiso 1 2 calc SR . . C25 C 0.2373(6) 0.3728(6) 0.0000 0.053(4) Uani 1 2 d SU . . H25 H 0.2713 0.3662 0.0000 0.063 Uiso 1 2 calc SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.0113(4) 0.0245(4) 0.0297(4) 0.000 0.000 0.0007(3) N1 0.006(5) 0.030(6) 0.022(5) 0.000 0.000 -0.006(5) N2 0.029(9) 0.024(8) 0.029(7) 0.000 0.000 -0.002(5) N3 0.005(6) 0.022(7) 0.024(6) 0.000 0.000 -0.001(5) O1 0.008(5) 0.025(5) 0.043(5) 0.000 0.000 0.002(4) O2 0.010(4) 0.025(5) 0.031(4) 0.000 0.000 -0.003(4) C1 0.016(6) 0.014(6) 0.026(6) 0.000 0.000 0.004(5) C2 0.014(8) 0.021(7) 0.032(8) 0.000 0.000 0.001(6) C3 0.022(8) 0.025(8) 0.033(8) 0.000 0.000 0.008(6) C4 0.024(7) 0.025(7) 0.023(7) 0.000 0.000 0.000(6) C5 0.010(7) 0.024(8) 0.027(7) 0.000 0.000 0.008(6) C6 0.024(7) 0.025(8) 0.044(7) 0.000 0.000 -0.002(6) C7 0.013(6) 0.017(6) 0.020(6) 0.000 0.000 -0.001(5) C8 0.021(10) 0.043(11) 0.068(12) 0.000 0.000 0.012(8) C9 0.021(6) 0.033(7) 0.043(7) -0.001(6) 0.010(6) -0.002(5) C11 0.013(5) 0.020(6) 0.025(6) 0.000 0.000 0.003(5) C12 0.018(9) 0.041(11) 0.050(10) 0.000 0.000 0.002(8) C13 0.027(7) 0.030(7) 0.050(7) -0.002(6) -0.005(6) -0.003(5) C15 0.015(6) 0.018(6) 0.022(6) 0.000 0.000 -0.002(5) C16 0.029(8) 0.028(8) 0.044(8) 0.000 0.000 0.003(7) C17 0.038(9) 0.028(8) 0.039(8) 0.000 0.000 -0.003(7) C18 0.026(8) 0.031(8) 0.039(8) 0.000 0.000 -0.005(7) C19 0.023(8) 0.030(9) 0.021(7) 0.000 0.000 0.007(7) C20 0.024(8) 0.019(8) 0.049(8) 0.000 0.000 0.004(6) C21 0.032(9) 0.028(9) 0.099(11) 0.000 0.000 0.006(7) C22 0.016(8) 0.026(9) 0.091(10) 0.000 0.000 0.011(7) C23 0.021(8) 0.017(8) 0.065(9) 0.000 0.000 0.005(6) C24 0.017(8) 0.029(9) 0.113(11) 0.000 0.000 0.002(7) C25 0.016(8) 0.031(9) 0.111(11) 0.000 0.000 0.008(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt N2 1.938(12) . ? Pt N1 1.976(11) . ? Pt O2 1.985(9) . ? Pt O1 1.986(9) . ? N1 N3 1.274(15) . ? N1 C20 1.416(16) . ? N2 C15 1.361(16) . ? N2 C19 1.382(17) . ? N3 C15 1.346(16) . ? O1 C1 1.363(15) . ? O2 C2 1.375(15) . ? C1 C2 1.384(17) . ? C1 C6 1.394(18) . ? C2 C3 1.407(19) . ? C3 C4 1.394(18) . ? C3 H3 0.9300 . ? C4 C5 1.415(18) . ? C4 C7 1.514(18) . ? C5 C6 1.391(18) . ? C5 H5 0.9300 . ? C6 C11 1.574(19) . ? C7 C9 1.528(12) . ? C7 C9 1.529(12) 11 ? C7 C8 1.548(18) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C11 C13 1.536(12) . ? C11 C13 1.536(12) 11 ? C11 C12 1.576(17) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C15 C16 1.421(18) . ? C16 C17 1.341(19) . ? C16 H16 0.9300 . ? C17 C18 1.371(19) . ? C17 H17 0.9300 . ? C18 C19 1.383(19) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C25 1.33(2) . ? C20 C21 1.396(19) . ? C21 C22 1.371(19) . ? C21 H21 0.9300 . ? C22 C23 1.318(19) . ? C22 H22 0.9300 . ? C23 C24 1.372(18) . ? C23 H23 0.9300 . ? C24 C25 1.36(2) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? 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 N2 Pt N1 77.8(5) . . ? N2 Pt O2 178.7(4) . . ? N1 Pt O2 103.5(4) . . ? N2 Pt O1 94.9(4) . . ? N1 Pt O1 172.7(4) . . ? O2 Pt O1 83.7(4) . . ? N3 N1 C20 115.4(12) . . ? N3 N1 Pt 117.8(9) . . ? C20 N1 Pt 126.8(9) . . ? C15 N2 C19 118.4(13) . . ? C15 N2 Pt 114.5(9) . . ? C19 N2 Pt 127.1(10) . . ? N1 N3 C15 114.1(11) . . ? C1 O1 Pt 111.9(8) . . ? C2 O2 Pt 109.2(8) . . ? O1 C1 C2 115.3(12) . . ? O1 C1 C6 124.9(12) . . ? C2 C1 C6 119.8(13) . . ? O2 C2 C1 119.8(12) . . ? O2 C2 C3 118.3(12) . . ? C1 C2 C3 121.9(13) . . ? C4 C3 C2 119.2(13) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 118.1(13) . . ? C3 C4 C7 123.8(13) . . ? C5 C4 C7 118.1(12) . . ? C6 C5 C4 122.5(13) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C1 118.6(14) . . ? C5 C6 C11 122.1(13) . . ? C1 C6 C11 119.3(12) . . ? C4 C7 C9 109.6(7) . . ? C4 C7 C9 109.6(7) . 11 ? C9 C7 C9 109.6(10) . 11 ? C4 C7 C8 113.3(12) . . ? C9 C7 C8 107.4(8) . . ? C9 C7 C8 107.4(8) 11 . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C13 C11 C13 110.9(11) . 11 ? C13 C11 C6 108.5(8) . . ? C13 C11 C6 108.5(8) 11 . ? C13 C11 C12 109.1(7) . . ? C13 C11 C12 109.1(7) 11 . ? C6 C11 C12 110.8(11) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C15 N2 115.8(12) . . ? N3 C15 C16 123.2(13) . . ? N2 C15 C16 121.1(13) . . ? C17 C16 C15 119.2(15) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 120.4(16) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C19 120.5(15) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? N2 C19 C18 120.4(14) . . ? N2 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C25 C20 C21 116.5(14) . . ? C25 C20 N1 124.5(14) . . ? C21 C20 N1 119.0(14) . . ? C22 C21 C20 120.8(16) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C23 C22 C21 120.9(15) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 119.0(15) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 119.9(16) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C20 C25 C24 122.8(16) . . ? C20 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.933 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.168 # Attachment '1a+1b.cif' data_gklger15 _database_code_depnum_ccdc_archive 'CCDC 719347' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H29 N3 O2 Pt' _chemical_formula_sum 'C25 H29 N3 O2 Pt' _chemical_formula_weight 598.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 '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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7992(3) _cell_length_b 13.6690(4) _cell_length_c 16.6581(6) _cell_angle_alpha 107.050(3) _cell_angle_beta 98.301(3) _cell_angle_gamma 101.033(2) _cell_volume 2254.17(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9939 _cell_measurement_theta_min 3.0354 _cell_measurement_theta_max 32.4503 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 6.251 _exptl_absorpt_correction_T_min 0.3535 _exptl_absorpt_correction_T_max 0.4540 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21767 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 26.50 _reflns_number_total 9287 _reflns_number_gt 6498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0160P)^2^+0.0000P] 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 9287 _refine_ls_number_parameters 575 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0526 _refine_ls_wR_factor_gt 0.0499 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.002 _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 0.803548(18) 0.049912(15) 0.899606(13) 0.02055(6) Uani 1 1 d . . . N1 N 0.9805(4) 0.1061(3) 0.9719(3) 0.0231(10) Uani 1 1 d . . . N2 N 0.7702(4) 0.1058(3) 1.0145(3) 0.0222(10) Uani 1 1 d . . . N3 N 0.9941(4) 0.1501(3) 1.0536(3) 0.0211(10) Uani 1 1 d . . . O1 O 0.8300(3) -0.0077(3) 0.7820(2) 0.0270(9) Uani 1 1 d . . . O2 O 0.6208(3) 0.0003(3) 0.8402(2) 0.0259(8) Uani 1 1 d . . . C1 C 0.7163(4) -0.0475(4) 0.7217(3) 0.0230(12) Uani 1 1 d . . . C2 C 0.6052(5) -0.0425(4) 0.7548(3) 0.0218(12) Uani 1 1 d . . . C3 C 0.4834(4) -0.0813(4) 0.6993(3) 0.0236(12) Uani 1 1 d . . . H3 H 0.4078 -0.0792 0.7221 0.028 Uiso 1 1 calc R . . C4 C 0.4725(4) -0.1228(4) 0.6117(3) 0.0227(12) Uani 1 1 d . . . C5 C 0.5871(4) -0.1265(4) 0.5810(3) 0.0227(12) Uani 1 1 d . . . H5 H 0.5799 -0.1555 0.5208 0.027 Uiso 1 1 calc R . . C6 C 0.7096(4) -0.0902(4) 0.6334(3) 0.0220(12) Uani 1 1 d . . . C7 C 0.3405(4) -0.1710(4) 0.5492(3) 0.0257(12) Uani 1 1 d . . . C8 C 0.2984(6) -0.2880(5) 0.5406(4) 0.0520(19) Uani 1 1 d . . . H8A H 0.2110 -0.3185 0.5049 0.078 Uiso 1 1 calc R . . H8B H 0.2991 -0.2945 0.5977 0.078 Uiso 1 1 calc R . . H8C H 0.3582 -0.3257 0.5137 0.078 Uiso 1 1 calc R . . C9 C 0.3446(5) -0.1633(5) 0.4608(4) 0.0397(15) Uani 1 1 d . . . H9A H 0.2574 -0.1901 0.4246 0.059 Uiso 1 1 calc R . . H9B H 0.4014 -0.2053 0.4349 0.059 Uiso 1 1 calc R . . H9C H 0.3777 -0.0893 0.4658 0.059 Uiso 1 1 calc R . . C10 C 0.2387(5) -0.1170(5) 0.5830(4) 0.0485(18) Uani 1 1 d . . . H10A H 0.2652 -0.0415 0.5909 0.073 Uiso 1 1 calc R . . H10B H 0.2295 -0.1263 0.6382 0.073 Uiso 1 1 calc R . . H10C H 0.1559 -0.1485 0.5417 0.073 Uiso 1 1 calc R . . C11 C 0.8331(4) -0.0965(4) 0.5984(3) 0.0240(12) Uani 1 1 d . . . C12 C 0.9222(5) 0.0151(4) 0.6218(4) 0.0343(14) Uani 1 1 d . . . H12A H 0.9441 0.0487 0.6844 0.051 Uiso 1 1 calc R . . H12B H 0.8777 0.0576 0.5953 0.051 Uiso 1 1 calc R . . H12C H 1.0015 0.0096 0.6005 0.051 Uiso 1 1 calc R . . C13 C 0.9033(5) -0.1663(4) 0.6360(4) 0.0304(13) Uani 1 1 d . . . H13A H 0.9279 -0.1346 0.6987 0.046 Uiso 1 1 calc R . . H13B H 0.9809 -0.1720 0.6127 0.046 Uiso 1 1 calc R . . H13C H 0.8457 -0.2368 0.6205 0.046 Uiso 1 1 calc R . . C14 C 0.8025(5) -0.1457(4) 0.5000(3) 0.0334(14) Uani 1 1 d . . . H14A H 0.8828 -0.1511 0.4801 0.050 Uiso 1 1 calc R . . H14B H 0.7608 -0.1010 0.4743 0.050 Uiso 1 1 calc R . . H14C H 0.7444 -0.2162 0.4827 0.050 Uiso 1 1 calc R . . C15 C 0.8783(5) 0.1517(4) 1.0788(3) 0.0217(11) Uani 1 1 d . . . C16 C 0.8721(5) 0.1969(4) 1.1633(3) 0.0241(12) Uani 1 1 d . . . H16 H 0.9489 0.2275 1.2068 0.029 Uiso 1 1 calc R . . C17 C 0.7530(5) 0.1971(4) 1.1837(4) 0.0300(13) Uani 1 1 d . . . H17 H 0.7465 0.2284 1.2414 0.036 Uiso 1 1 calc R . . C18 C 0.6425(5) 0.1508(4) 1.1189(3) 0.0264(13) Uani 1 1 d . . . H18 H 0.5596 0.1493 1.1320 0.032 Uiso 1 1 calc R . . C19 C 0.6542(5) 0.1073(4) 1.0358(3) 0.0230(12) Uani 1 1 d . . . H19 H 0.5781 0.0773 0.9917 0.028 Uiso 1 1 calc R . . C20 C 1.1031(5) 0.1068(4) 0.9458(4) 0.0218(12) Uani 1 1 d . . . C21 C 1.2195(4) 0.1506(4) 1.0055(4) 0.0236(12) Uani 1 1 d . . . H21 H 1.2199 0.1765 1.0651 0.028 Uiso 1 1 calc R . . C22 C 1.3347(5) 0.1565(4) 0.9782(4) 0.0289(14) Uani 1 1 d . . . H22 H 1.4142 0.1878 1.0190 0.035 Uiso 1 1 calc R . . C23 C 1.3350(5) 0.1171(4) 0.8920(4) 0.0304(13) Uani 1 1 d . . . H23 H 1.4143 0.1214 0.8733 0.036 Uiso 1 1 calc R . . C24 C 1.2197(5) 0.0715(4) 0.8333(4) 0.0342(14) Uani 1 1 d . . . H24 H 1.2195 0.0428 0.7740 0.041 Uiso 1 1 calc R . . C25 C 1.1039(5) 0.0671(4) 0.8602(4) 0.0283(13) Uani 1 1 d . . . H25 H 1.0246 0.0366 0.8191 0.034 Uiso 1 1 calc R . . Pt1B Pt 0.780052(18) 0.374276(15) 1.030396(13) 0.02127(6) Uani 1 1 d . . . N1B N 0.7421(4) 0.3184(3) 0.9059(3) 0.0272(11) Uani 1 1 d . . . N2B N 0.9543(4) 0.3774(3) 1.0074(3) 0.0215(10) Uani 1 1 d . . . N3B N 0.8365(4) 0.3032(3) 0.8654(3) 0.0292(11) Uani 1 1 d . . . O1B O 0.8363(3) 0.4350(3) 1.1552(2) 0.0245(8) Uani 1 1 d . . . O2B O 0.6049(3) 0.3622(2) 1.0551(2) 0.0228(8) Uani 1 1 d . . . C1B C 0.7338(4) 0.4368(4) 1.1953(3) 0.0198(11) Uani 1 1 d . . . C2B C 0.6109(5) 0.3958(4) 1.1411(3) 0.0230(12) Uani 1 1 d . . . C3B C 0.5003(4) 0.3892(4) 1.1752(3) 0.0249(12) Uani 1 1 d . . . H3B H 0.4177 0.3586 1.1378 0.030 Uiso 1 1 calc R . . C4B C 0.5101(5) 0.4266(4) 1.2625(3) 0.0237(12) Uani 1 1 d . . . C5B C 0.6344(5) 0.4710(4) 1.3156(3) 0.0242(12) Uani 1 1 d . . . H5B H 0.6413 0.4979 1.3760 0.029 Uiso 1 1 calc R . . C6B C 0.7482(5) 0.4779(4) 1.2848(3) 0.0221(12) Uani 1 1 d . . . C7B C 0.3904(5) 0.4253(4) 1.3016(4) 0.0316(13) Uani 1 1 d . . . C8B C 0.4124(6) 0.4101(7) 1.3883(4) 0.078(3) Uani 1 1 d . . . H8D H 0.3341 0.4117 1.4115 0.117 Uiso 1 1 calc R . . H8E H 0.4844 0.4669 1.4277 0.117 Uiso 1 1 calc R . . H8F H 0.4330 0.3418 1.3820 0.117 Uiso 1 1 calc R . . C9B C 0.3535(7) 0.5302(5) 1.3092(6) 0.085(3) Uani 1 1 d . . . H9D H 0.2723 0.5289 1.3291 0.127 Uiso 1 1 calc R . . H9E H 0.3429 0.5402 1.2530 0.127 Uiso 1 1 calc R . . H9F H 0.4219 0.5886 1.3505 0.127 Uiso 1 1 calc R . . C10B C 0.2759(5) 0.3373(4) 1.2455(4) 0.0364(14) Uani 1 1 d . . . H10D H 0.2971 0.2691 1.2383 0.055 Uiso 1 1 calc R . . H10E H 0.2548 0.3460 1.1892 0.055 Uiso 1 1 calc R . . H10F H 0.2015 0.3399 1.2728 0.055 Uiso 1 1 calc R . . C11B C 0.8823(5) 0.5297(4) 1.3454(3) 0.0251(12) Uani 1 1 d . . . C12B C 0.9496(5) 0.6235(4) 1.3220(4) 0.0362(14) Uani 1 1 d . . . H12D H 0.8974 0.6754 1.3282 0.054 Uiso 1 1 calc R . . H12E H 0.9598 0.5989 1.2624 0.054 Uiso 1 1 calc R . . H12F H 1.0348 0.6562 1.3604 0.054 Uiso 1 1 calc R . . C13B C 0.9665(4) 0.4483(4) 1.3357(3) 0.0273(12) Uani 1 1 d . . . H13D H 1.0509 0.4813 1.3751 0.041 Uiso 1 1 calc R . . H13E H 0.9784 0.4250 1.2765 0.041 Uiso 1 1 calc R . . H13F H 0.9234 0.3873 1.3496 0.041 Uiso 1 1 calc R . . C14B C 0.8741(5) 0.5674(4) 1.4394(3) 0.0322(14) Uani 1 1 d . . . H14D H 0.9613 0.5975 1.4754 0.048 Uiso 1 1 calc R . . H14E H 0.8308 0.5076 1.4547 0.048 Uiso 1 1 calc R . . H14F H 0.8247 0.6214 1.4487 0.048 Uiso 1 1 calc R . . C15B C 0.9534(5) 0.3332(4) 0.9222(4) 0.0280(13) Uani 1 1 d . . . C16B C 1.0683(5) 0.3237(4) 0.8945(4) 0.0337(14) Uani 1 1 d . . . H16B H 1.0671 0.2923 0.8353 0.040 Uiso 1 1 calc R . . C17B C 1.1818(6) 0.3605(5) 0.9541(4) 0.0391(16) Uani 1 1 d . . . H17B H 1.2607 0.3542 0.9366 0.047 Uiso 1 1 calc R . . C18B C 1.1820(5) 0.4067(4) 1.0394(4) 0.0319(14) Uani 1 1 d . . . H18B H 1.2614 0.4342 1.0806 0.038 Uiso 1 1 calc R . . C19B C 1.0673(5) 0.4132(4) 1.0653(4) 0.0263(13) Uani 1 1 d . . . H19B H 1.0679 0.4433 1.1246 0.032 Uiso 1 1 calc R . . C20B C 0.6188(5) 0.2911(4) 0.8473(3) 0.0245(12) Uani 1 1 d . . . C21B C 0.5906(5) 0.2089(4) 0.7700(3) 0.0301(13) Uani 1 1 d . . . H21B H 0.6503 0.1671 0.7559 0.036 Uiso 1 1 calc R . . C22B C 0.4746(6) 0.1890(4) 0.7142(4) 0.0387(15) Uani 1 1 d . . . H22B H 0.4526 0.1310 0.6621 0.046 Uiso 1 1 calc R . . C23B C 0.3900(6) 0.2518(5) 0.7326(4) 0.0397(16) Uani 1 1 d . . . H23B H 0.3116 0.2385 0.6925 0.048 Uiso 1 1 calc R . . C24B C 0.4192(5) 0.3343(4) 0.8097(4) 0.0321(14) Uani 1 1 d . . . H24B H 0.3609 0.3777 0.8223 0.039 Uiso 1 1 calc R . . C25B C 0.5329(5) 0.3536(4) 0.8682(3) 0.0285(13) Uani 1 1 d . . . H25B H 0.5522 0.4088 0.9218 0.034 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 0.01761(11) 0.02185(12) 0.02016(14) 0.00610(10) 0.00357(10) 0.00181(9) N1 0.025(2) 0.018(2) 0.026(3) 0.0080(19) 0.010(2) 0.0024(19) N2 0.023(2) 0.017(2) 0.024(3) 0.0049(19) 0.006(2) 0.0016(19) N3 0.022(2) 0.021(2) 0.018(3) 0.0034(19) 0.0053(19) 0.0045(18) O1 0.0165(18) 0.032(2) 0.027(2) 0.0059(17) 0.0030(16) -0.0012(16) O2 0.0200(18) 0.033(2) 0.020(2) 0.0044(16) 0.0025(16) 0.0031(16) C1 0.014(2) 0.028(3) 0.026(3) 0.011(2) 0.001(2) 0.001(2) C2 0.023(3) 0.021(3) 0.022(3) 0.008(2) 0.004(2) 0.004(2) C3 0.016(2) 0.032(3) 0.023(3) 0.009(2) 0.007(2) 0.003(2) C4 0.015(2) 0.026(3) 0.030(3) 0.014(2) 0.003(2) 0.004(2) C5 0.018(2) 0.029(3) 0.020(3) 0.008(2) 0.004(2) 0.004(2) C6 0.016(2) 0.025(3) 0.023(3) 0.007(2) 0.005(2) 0.002(2) C7 0.016(2) 0.032(3) 0.027(3) 0.009(2) 0.004(2) 0.002(2) C8 0.041(4) 0.044(4) 0.057(5) 0.020(3) -0.015(3) -0.010(3) C9 0.022(3) 0.060(4) 0.033(4) 0.016(3) 0.001(3) 0.003(3) C10 0.021(3) 0.076(5) 0.039(4) 0.006(3) 0.001(3) 0.015(3) C11 0.017(3) 0.033(3) 0.020(3) 0.007(2) 0.006(2) 0.003(2) C12 0.021(3) 0.044(4) 0.040(4) 0.021(3) 0.009(3) 0.003(3) C13 0.018(3) 0.040(3) 0.035(4) 0.012(3) 0.010(2) 0.008(2) C14 0.027(3) 0.051(4) 0.023(3) 0.011(3) 0.010(3) 0.011(3) C15 0.023(3) 0.018(3) 0.025(3) 0.011(2) 0.003(2) 0.001(2) C16 0.027(3) 0.029(3) 0.014(3) 0.006(2) 0.001(2) 0.006(2) C17 0.039(3) 0.030(3) 0.025(3) 0.013(3) 0.016(3) 0.007(3) C18 0.029(3) 0.027(3) 0.027(3) 0.012(2) 0.012(3) 0.007(2) C19 0.022(3) 0.024(3) 0.023(3) 0.009(2) 0.005(2) 0.004(2) C20 0.022(3) 0.012(3) 0.027(3) 0.004(2) 0.003(2) 0.000(2) C21 0.022(3) 0.022(3) 0.025(3) 0.005(2) 0.004(2) 0.005(2) C22 0.018(3) 0.031(3) 0.036(4) 0.011(3) 0.001(3) 0.009(2) C23 0.023(3) 0.031(3) 0.039(4) 0.014(3) 0.010(3) 0.007(3) C24 0.025(3) 0.045(4) 0.029(4) 0.007(3) 0.010(3) 0.005(3) C25 0.016(3) 0.032(3) 0.028(3) 0.003(3) -0.002(2) 0.003(2) Pt1B 0.02298(12) 0.02284(13) 0.02033(14) 0.00969(10) 0.00725(10) 0.00515(10) N1B 0.029(3) 0.022(2) 0.036(3) 0.016(2) 0.010(2) 0.008(2) N2B 0.024(2) 0.019(2) 0.025(3) 0.0110(19) 0.003(2) 0.0079(19) N3B 0.039(3) 0.025(3) 0.030(3) 0.013(2) 0.014(2) 0.013(2) O1B 0.0186(18) 0.031(2) 0.026(2) 0.0118(17) 0.0069(16) 0.0046(16) O2B 0.0179(17) 0.027(2) 0.018(2) 0.0049(16) -0.0008(16) 0.0007(15) C1B 0.020(3) 0.023(3) 0.020(3) 0.010(2) 0.003(2) 0.009(2) C2B 0.027(3) 0.022(3) 0.019(3) 0.006(2) 0.006(2) 0.004(2) C3B 0.016(2) 0.031(3) 0.025(3) 0.007(2) 0.006(2) 0.001(2) C4B 0.023(3) 0.024(3) 0.025(3) 0.008(2) 0.008(2) 0.008(2) C5B 0.029(3) 0.024(3) 0.018(3) 0.004(2) 0.006(2) 0.007(2) C6B 0.020(3) 0.021(3) 0.022(3) 0.007(2) 0.002(2) 0.003(2) C7B 0.022(3) 0.038(3) 0.031(4) 0.006(3) 0.010(3) 0.005(3) C8B 0.030(4) 0.159(8) 0.023(4) 0.018(5) 0.012(3) -0.009(4) C9B 0.058(5) 0.046(5) 0.162(9) 0.022(5) 0.079(5) 0.018(4) C10B 0.023(3) 0.046(4) 0.035(4) 0.011(3) 0.008(3) -0.001(3) C11B 0.026(3) 0.028(3) 0.018(3) 0.006(2) 0.002(2) 0.002(2) C12B 0.032(3) 0.031(3) 0.038(4) 0.013(3) -0.001(3) -0.005(3) C13B 0.021(3) 0.035(3) 0.022(3) 0.008(2) -0.004(2) 0.007(2) C14B 0.025(3) 0.036(3) 0.026(3) 0.004(3) -0.002(3) 0.001(3) C15B 0.035(3) 0.027(3) 0.033(4) 0.019(3) 0.014(3) 0.015(3) C16B 0.046(4) 0.036(3) 0.034(4) 0.021(3) 0.027(3) 0.019(3) C17B 0.035(3) 0.042(4) 0.063(5) 0.037(3) 0.027(3) 0.020(3) C18B 0.027(3) 0.040(4) 0.044(4) 0.031(3) 0.011(3) 0.015(3) C19B 0.026(3) 0.031(3) 0.033(4) 0.020(3) 0.014(3) 0.011(3) C20B 0.032(3) 0.028(3) 0.019(3) 0.014(2) 0.008(3) 0.008(3) C21B 0.038(3) 0.031(3) 0.024(3) 0.011(3) 0.011(3) 0.006(3) C22B 0.050(4) 0.035(4) 0.026(4) 0.008(3) 0.007(3) 0.000(3) C23B 0.042(4) 0.049(4) 0.026(4) 0.018(3) 0.002(3) 0.001(3) C24B 0.034(3) 0.035(3) 0.035(4) 0.020(3) 0.014(3) 0.008(3) C25B 0.036(3) 0.027(3) 0.022(3) 0.009(2) 0.007(3) 0.003(3) _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 N2 1.956(4) . ? Pt1 O2 1.966(3) . ? Pt1 O1 1.970(4) . ? Pt1 N1 1.981(4) . ? N1 N3 1.289(5) . ? N1 C20 1.452(6) . ? N2 C19 1.354(6) . ? N2 C15 1.366(6) . ? N3 C15 1.378(6) . ? O1 C1 1.372(5) . ? O2 C2 1.340(6) . ? C1 C2 1.396(7) . ? C1 C6 1.399(7) . ? C2 C3 1.401(6) . ? C3 C4 1.380(7) . ? C3 H3 0.9500 . ? C4 C5 1.410(6) . ? C4 C7 1.536(6) . ? C5 C6 1.386(6) . ? C5 H5 0.9500 . ? C6 C11 1.539(7) . ? C7 C9 1.513(7) . ? C7 C10 1.521(7) . ? C7 C8 1.534(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.537(7) . ? C11 C13 1.539(7) . ? C11 C12 1.544(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.379(7) . ? C16 C17 1.378(7) . ? C16 H16 0.9500 . ? C17 C18 1.388(7) . ? C17 H17 0.9500 . ? C18 C19 1.372(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.372(7) . ? C20 C21 1.389(6) . ? C21 C22 1.381(7) . ? C21 H21 0.9500 . ? C22 C23 1.378(7) . ? C22 H22 0.9500 . ? C23 C24 1.374(7) . ? C23 H23 0.9500 . ? C24 C25 1.385(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? Pt1B N1B 1.938(5) . ? Pt1B O1B 1.952(3) . ? Pt1B N2B 1.969(4) . ? Pt1B O2B 1.980(3) . ? N1B N3B 1.318(6) . ? N1B C20B 1.444(6) . ? N2B C19B 1.346(6) . ? N2B C15B 1.367(6) . ? N3B C15B 1.373(7) . ? O1B C1B 1.373(6) . ? O2B C2B 1.358(6) . ? C1B C2B 1.401(6) . ? C1B C6B 1.404(7) . ? C2B C3B 1.394(7) . ? C3B C4B 1.374(7) . ? C3B H3B 0.9500 . ? C4B C5B 1.408(6) . ? C4B C7B 1.528(7) . ? C5B C6B 1.396(7) . ? C5B H5B 0.9500 . ? C6B C11B 1.544(7) . ? C7B C8B 1.511(8) . ? C7B C10B 1.512(7) . ? C7B C9B 1.536(8) . ? C8B H8D 0.9800 . ? C8B H8E 0.9800 . ? C8B H8F 0.9800 . ? C9B H9D 0.9800 . ? C9B H9E 0.9800 . ? C9B H9F 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11B C14B 1.521(7) . ? C11B C12B 1.530(7) . ? C11B C13B 1.554(7) . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 0.9800 . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B C16B 1.400(7) . ? C16B C17B 1.364(8) . ? C16B H16B 0.9500 . ? C17B C18B 1.376(8) . ? C17B H17B 0.9500 . ? C18B C19B 1.380(7) . ? C18B H18B 0.9500 . ? C19B H19B 0.9500 . ? C20B C21B 1.386(7) . ? C20B C25B 1.390(7) . ? C21B C22B 1.377(7) . ? C21B H21B 0.9500 . ? C22B C23B 1.376(8) . ? C22B H22B 0.9500 . ? C23B C24B 1.384(8) . ? C23B H23B 0.9500 . ? C24B C25B 1.381(7) . ? C24B H24B 0.9500 . ? C25B H25B 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 N2 Pt1 O2 95.45(15) . . ? N2 Pt1 O1 177.83(14) . . ? O2 Pt1 O1 82.38(13) . . ? N2 Pt1 N1 77.88(17) . . ? O2 Pt1 N1 173.33(16) . . ? O1 Pt1 N1 104.29(15) . . ? N3 N1 C20 112.7(4) . . ? N3 N1 Pt1 118.6(3) . . ? C20 N1 Pt1 128.7(3) . . ? C19 N2 C15 117.8(5) . . ? C19 N2 Pt1 127.3(4) . . ? C15 N2 Pt1 114.9(3) . . ? N1 N3 C15 113.1(4) . . ? C1 O1 Pt1 112.6(3) . . ? C2 O2 Pt1 112.6(3) . . ? O1 C1 C2 114.9(5) . . ? O1 C1 C6 123.6(4) . . ? C2 C1 C6 121.6(4) . . ? O2 C2 C1 117.5(4) . . ? O2 C2 C3 122.5(4) . . ? C1 C2 C3 119.9(5) . . ? C4 C3 C2 120.3(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 117.9(4) . . ? C3 C4 C7 121.8(4) . . ? C5 C4 C7 120.2(5) . . ? C6 C5 C4 123.9(5) . . ? C6 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? C5 C6 C1 116.4(4) . . ? C5 C6 C11 122.9(5) . . ? C1 C6 C11 120.7(4) . . ? C9 C7 C10 108.3(4) . . ? C9 C7 C8 108.5(5) . . ? C10 C7 C8 108.1(5) . . ? C9 C7 C4 112.4(4) . . ? C10 C7 C4 111.1(4) . . ? C8 C7 C4 108.4(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C6 111.6(4) . . ? C14 C11 C13 107.9(4) . . ? C6 C11 C13 109.2(4) . . ? C14 C11 C12 107.3(4) . . ? C6 C11 C12 110.4(4) . . ? C13 C11 C12 110.4(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 N3 115.6(5) . . ? N2 C15 C16 122.4(5) . . ? N3 C15 C16 122.1(5) . . ? C17 C16 C15 118.9(5) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 C18 119.2(5) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 119.4(5) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? N2 C19 C18 122.3(5) . . ? N2 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? C25 C20 C21 119.5(5) . . ? C25 C20 N1 119.2(4) . . ? C21 C20 N1 121.2(5) . . ? C22 C21 C20 119.9(5) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.4(5) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 119.5(5) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 120.4(5) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C20 C25 C24 120.3(5) . . ? C20 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? N1B Pt1B O1B 174.30(16) . . ? N1B Pt1B N2B 78.70(18) . . ? O1B Pt1B N2B 95.76(16) . . ? N1B Pt1B O2B 101.89(16) . . ? O1B Pt1B O2B 83.74(13) . . ? N2B Pt1B O2B 176.13(14) . . ? N3B N1B C20B 112.3(4) . . ? N3B N1B Pt1B 119.6(3) . . ? C20B N1B Pt1B 128.2(3) . . ? C19B N2B C15B 119.6(5) . . ? C19B N2B Pt1B 127.4(4) . . ? C15B N2B Pt1B 113.0(3) . . ? N1B N3B C15B 111.3(5) . . ? C1B O1B Pt1B 112.0(3) . . ? C2B O2B Pt1B 110.9(3) . . ? O1B C1B C2B 115.9(5) . . ? O1B C1B C6B 123.3(4) . . ? C2B C1B C6B 120.8(5) . . ? O2B C2B C3B 122.0(5) . . ? O2B C2B C1B 117.3(4) . . ? C3B C2B C1B 120.6(5) . . ? C4B C3B C2B 120.3(5) . . ? C4B C3B H3B 119.8 . . ? C2B C3B H3B 119.8 . . ? C3B C4B C5B 118.0(5) . . ? C3B C4B C7B 121.5(4) . . ? C5B C4B C7B 120.4(5) . . ? C6B C5B C4B 123.9(5) . . ? C6B C5B H5B 118.1 . . ? C4B C5B H5B 118.1 . . ? C5B C6B C1B 116.2(4) . . ? C5B C6B C11B 122.0(5) . . ? C1B C6B C11B 121.7(4) . . ? C8B C7B C10B 106.4(5) . . ? C8B C7B C4B 112.4(4) . . ? C10B C7B C4B 112.3(4) . . ? C8B C7B C9B 110.5(6) . . ? C10B C7B C9B 107.5(5) . . ? C4B C7B C9B 107.7(5) . . ? C7B C8B H8D 109.5 . . ? C7B C8B H8E 109.5 . . ? H8D C8B H8E 109.5 . . ? C7B C8B H8F 109.5 . . ? H8D C8B H8F 109.5 . . ? H8E C8B H8F 109.5 . . ? C7B C9B H9D 109.5 . . ? C7B C9B H9E 109.5 . . ? H9D C9B H9E 109.5 . . ? C7B C9B H9F 109.5 . . ? H9D C9B H9F 109.5 . . ? H9E C9B H9F 109.5 . . ? C7B C10B H10D 109.5 . . ? C7B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C7B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C14B C11B C12B 109.1(4) . . ? C14B C11B C6B 112.4(4) . . ? C12B C11B C6B 109.6(4) . . ? C14B C11B C13B 106.9(4) . . ? C12B C11B C13B 108.9(4) . . ? C6B C11B C13B 109.9(4) . . ? C11B C12B H12D 109.5 . . ? C11B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C11B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C11B C13B H13D 109.5 . . ? C11B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C11B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C11B C14B H14D 109.5 . . ? C11B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C11B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? N2B C15B N3B 117.2(5) . . ? N2B C15B C16B 120.9(5) . . ? N3B C15B C16B 121.9(6) . . ? C17B C16B C15B 118.7(6) . . ? C17B C16B H16B 120.6 . . ? C15B C16B H16B 120.6 . . ? C16B C17B C18B 119.9(5) . . ? C16B C17B H17B 120.0 . . ? C18B C17B H17B 120.0 . . ? C17B C18B C19B 120.2(6) . . ? C17B C18B H18B 119.9 . . ? C19B C18B H18B 119.9 . . ? N2B C19B C18B 120.6(6) . . ? N2B C19B H19B 119.7 . . ? C18B C19B H19B 119.7 . . ? C21B C20B C25B 121.1(5) . . ? C21B C20B N1B 120.7(5) . . ? C25B C20B N1B 118.2(5) . . ? C22B C21B C20B 118.7(5) . . ? C22B C21B H21B 120.6 . . ? C20B C21B H21B 120.6 . . ? C23B C22B C21B 121.0(6) . . ? C23B C22B H22B 119.5 . . ? C21B C22B H22B 119.5 . . ? C22B C23B C24B 119.9(6) . . ? C22B C23B H23B 120.1 . . ? C24B C23B H23B 120.1 . . ? C25B C24B C23B 120.2(5) . . ? C25B C24B H24B 119.9 . . ? C23B C24B H24B 119.9 . . ? C24B C25B C20B 119.0(5) . . ? C24B C25B H25B 120.5 . . ? C20B C25B H25B 120.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.411 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.140