# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Vadim Kukushkin' _publ_contact_author_email kukushkin@VK2100.spb.edu _publ_section_title ; Unexpectedly Efficient Activation of Push-Pull Nitriles by a PtII Center toward Dipolar Cycloaddition of Z-Nitrones ; loop_ _publ_author_name V.Kukushkin N.Bokach # Attachment '- all.cif' #Unexpectedly Efficient Activation of Push-Pull Nitriles by a PtII Center #toward #Dipolar Cycloaddition of Z-Nitrones #by Andrey S. Krytchankou, Nadezhda A. Bokach, Matti Haukka and #Vadim Yu. Kukushkin data_2a _database_code_depnum_ccdc_archive 'CCDC 803620' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H34 Cl2 N6 O2 Pt' _chemical_formula_sum 'C24 H34 Cl2 N6 O2 Pt' _chemical_formula_weight 704.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.0916(4) _cell_length_b 9.3706(2) _cell_length_c 18.3895(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.5729(13) _cell_angle_gamma 90.00 _cell_volume 2771.87(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11953 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 5.287 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5144 _exptl_absorpt_correction_T_max 0.7318 _exptl_absorpt_process_details 'SADABS-2008/1 (Sheldrick, 2008)' _publ_section_exptl_refinement ; Hydrogen atoms were positioned geometrically and were constrained to ride on their parent atoms, with C---H = 0.95-1.00 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 1.46 \%A from atom Cl2 and the deepest hole is located 0.85 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45783 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6354 _reflns_number_gt 4734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2008)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.2c (Brandenburg, 2009)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0226P)^2^+1.8805P] 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 6354 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.004 _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 0.747098(8) 0.044917(13) 0.998272(7) 0.01685(5) Uani 1 1 d . . . Cl1 Cl 0.66492(6) 0.23006(10) 0.95473(5) 0.0304(2) Uani 1 1 d . . . Cl2 Cl 0.82445(6) -0.14672(10) 1.04195(4) 0.0264(2) Uani 1 1 d . . . O1 O 0.84771(17) 0.0007(3) 0.78959(13) 0.0330(6) Uani 1 1 d . . . O2 O 0.65350(15) 0.0848(3) 1.20943(12) 0.0242(6) Uani 1 1 d . . . N1 N 0.78447(18) 0.0049(3) 0.89631(15) 0.0201(6) Uani 1 1 d . . . N2 N 0.7792(2) -0.1073(4) 0.78706(16) 0.0338(8) Uani 1 1 d . . . N3 N 0.91889(19) 0.1079(3) 0.88194(15) 0.0277(7) Uani 1 1 d . . . N4 N 0.70922(18) 0.0899(3) 1.09944(14) 0.0208(7) Uani 1 1 d . . . N5 N 0.72425(18) 0.1875(3) 1.21282(15) 0.0241(7) Uani 1 1 d . . . N6 N 0.60968(19) -0.0869(3) 1.13049(15) 0.0240(7) Uani 1 1 d . . . C1 C 0.7230(2) -0.0447(4) 0.84089(18) 0.0249(8) Uani 1 1 d . . . H1 H 0.6925 0.0386 0.8191 0.030 Uiso 1 1 calc R . . C2 C 0.8500(2) 0.0411(4) 0.86041(18) 0.0220(8) Uani 1 1 d . . . C3 C 0.7327(2) 0.2248(4) 1.13514(17) 0.0211(8) Uani 1 1 d . . . H3 H 0.6921 0.3014 1.1210 0.025 Uiso 1 1 calc R . . C4 C 0.6584(2) 0.0246(4) 1.14224(18) 0.0198(8) Uani 1 1 d . . . C5 C 0.6627(2) -0.1560(4) 0.86435(17) 0.0231(8) Uani 1 1 d . . . C6 C 0.6892(2) -0.2846(4) 0.89417(19) 0.0300(9) Uani 1 1 d . . . H6 H 0.7468 -0.2999 0.9042 0.036 Uiso 1 1 calc R . . C7 C 0.6320(2) -0.3918(4) 0.9095(2) 0.0305(9) Uani 1 1 d . . . H7 H 0.6509 -0.4795 0.9299 0.037 Uiso 1 1 calc R . . C8 C 0.5481(2) -0.3707(4) 0.89514(19) 0.0280(9) Uani 1 1 d . . . C9 C 0.5221(3) -0.2404(5) 0.8679(2) 0.0409(11) Uani 1 1 d . . . H9 H 0.4644 -0.2227 0.8600 0.049 Uiso 1 1 calc R . . C10 C 0.5791(2) -0.1355(4) 0.8522(2) 0.0364(10) Uani 1 1 d . . . H10 H 0.5600 -0.0473 0.8324 0.044 Uiso 1 1 calc R . . C11 C 0.4847(3) -0.4876(5) 0.9070(3) 0.0456(12) Uani 1 1 d . . . H11A H 0.4408 -0.4515 0.9381 0.068 Uiso 1 1 calc R . . H11B H 0.5120 -0.5694 0.9307 0.068 Uiso 1 1 calc R . . H11C H 0.4602 -0.5173 0.8600 0.068 Uiso 1 1 calc R . . C12 C 0.7453(3) -0.1026(5) 0.7132(2) 0.0476(12) Uani 1 1 d . . . H12A H 0.7284 -0.0047 0.7012 0.071 Uiso 1 1 calc R . . H12B H 0.6969 -0.1658 0.7090 0.071 Uiso 1 1 calc R . . H12C H 0.7876 -0.1341 0.6794 0.071 Uiso 1 1 calc R . . C13 C 0.9307(2) 0.1624(4) 0.95610(19) 0.0342(10) Uani 1 1 d . . . H13A H 0.8921 0.2416 0.9638 0.051 Uiso 1 1 calc R . . H13B H 0.9880 0.1961 0.9632 0.051 Uiso 1 1 calc R . . H13C H 0.9198 0.0860 0.9909 0.051 Uiso 1 1 calc R . . C14 C 0.9828(2) 0.1460(4) 0.8301(2) 0.0339(9) Uani 1 1 d . . . H14A H 0.9796 0.0808 0.7885 0.051 Uiso 1 1 calc R . . H14B H 1.0379 0.1387 0.8539 0.051 Uiso 1 1 calc R . . H14C H 0.9737 0.2441 0.8132 0.051 Uiso 1 1 calc R . . C15 C 0.8201(2) 0.2751(4) 1.12365(17) 0.0219(8) Uani 1 1 d . . . C16 C 0.8352(2) 0.4141(4) 1.1027(2) 0.0277(9) Uani 1 1 d . . . H16 H 0.7901 0.4771 1.0926 0.033 Uiso 1 1 calc R . . C17 C 0.9168(3) 0.4617(4) 1.0966(2) 0.0327(10) Uani 1 1 d . . . H17 H 0.9264 0.5575 1.0823 0.039 Uiso 1 1 calc R . . C18 C 0.9839(2) 0.3732(4) 1.1109(2) 0.0310(9) Uani 1 1 d . . . C19 C 0.9676(2) 0.2329(4) 1.13172(19) 0.0294(9) Uani 1 1 d . . . H19 H 1.0128 0.1698 1.1415 0.035 Uiso 1 1 calc R . . C20 C 0.8869(2) 0.1840(4) 1.13839(18) 0.0253(8) Uani 1 1 d . . . H20 H 0.8771 0.0884 1.1530 0.030 Uiso 1 1 calc R . . C21 C 1.0724(3) 0.4228(5) 1.1040(3) 0.0487(12) Uani 1 1 d . . . H21A H 1.0987 0.3700 1.0648 0.073 Uiso 1 1 calc R . . H21B H 1.1032 0.4057 1.1499 0.073 Uiso 1 1 calc R . . H21C H 1.0730 0.5251 1.0928 0.073 Uiso 1 1 calc R . . C22 C 0.6951(3) 0.3083(4) 1.2560(2) 0.0350(10) Uani 1 1 d . . . H22A H 0.7356 0.3861 1.2544 0.053 Uiso 1 1 calc R . . H22B H 0.6887 0.2779 1.3066 0.053 Uiso 1 1 calc R . . H22C H 0.6414 0.3414 1.2360 0.053 Uiso 1 1 calc R . . C23 C 0.5915(3) -0.1444(5) 1.05809(19) 0.0374(10) Uani 1 1 d . . . H23A H 0.6036 -0.0719 1.0214 0.056 Uiso 1 1 calc R . . H23B H 0.5327 -0.1712 1.0540 0.056 Uiso 1 1 calc R . . H23C H 0.6261 -0.2288 1.0502 0.056 Uiso 1 1 calc R . . C24 C 0.5768(3) -0.1688(4) 1.19146(19) 0.0314(9) Uani 1 1 d . . . H24A H 0.6065 -0.2598 1.1959 0.047 Uiso 1 1 calc R . . H24B H 0.5174 -0.1869 1.1826 0.047 Uiso 1 1 calc R . . H24C H 0.5846 -0.1142 1.2366 0.047 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 0.02002(8) 0.01663(8) 0.01406(7) -0.00032(6) 0.00352(5) -0.00071(6) Cl1 0.0418(6) 0.0247(5) 0.0249(4) 0.0053(4) 0.0053(4) 0.0111(4) Cl2 0.0314(5) 0.0263(5) 0.0213(4) 0.0000(4) -0.0014(4) 0.0078(4) O1 0.0337(16) 0.0474(17) 0.0184(13) -0.0048(12) 0.0083(12) -0.0106(14) O2 0.0227(14) 0.0329(15) 0.0172(12) -0.0032(11) 0.0039(10) -0.0043(11) N1 0.0211(16) 0.0227(16) 0.0165(15) -0.0031(12) 0.0023(12) -0.0030(13) N2 0.0324(19) 0.045(2) 0.0246(17) -0.0028(15) 0.0081(14) -0.0111(16) N3 0.0257(18) 0.036(2) 0.0224(16) -0.0040(14) 0.0082(13) -0.0086(15) N4 0.0238(17) 0.0225(16) 0.0162(14) -0.0017(12) 0.0027(12) -0.0022(13) N5 0.0226(17) 0.0302(18) 0.0199(15) -0.0058(13) 0.0056(13) -0.0066(14) N6 0.0266(17) 0.0267(17) 0.0191(15) 0.0003(13) 0.0077(13) -0.0048(14) C1 0.026(2) 0.030(2) 0.0187(18) -0.0015(15) 0.0007(15) 0.0008(17) C2 0.028(2) 0.023(2) 0.0156(17) -0.0001(15) 0.0062(16) 0.0037(17) C3 0.0206(19) 0.0222(19) 0.0207(17) -0.0032(15) 0.0024(14) 0.0007(15) C4 0.0220(19) 0.024(2) 0.0132(17) 0.0001(14) 0.0039(15) 0.0037(16) C5 0.027(2) 0.025(2) 0.0173(17) -0.0074(15) 0.0009(15) -0.0028(16) C6 0.025(2) 0.034(2) 0.032(2) -0.0010(18) 0.0027(17) 0.0045(18) C7 0.039(2) 0.019(2) 0.034(2) 0.0029(17) 0.0041(18) 0.0068(18) C8 0.031(2) 0.025(2) 0.0275(19) -0.0057(17) -0.0028(17) -0.0053(18) C9 0.024(2) 0.035(3) 0.063(3) 0.008(2) -0.009(2) -0.0018(19) C10 0.032(2) 0.026(2) 0.052(3) 0.006(2) -0.0053(19) -0.0007(19) C11 0.044(3) 0.033(2) 0.059(3) 0.007(2) -0.006(2) -0.017(2) C12 0.048(3) 0.071(4) 0.024(2) -0.004(2) 0.002(2) -0.013(3) C13 0.029(2) 0.046(3) 0.028(2) -0.0099(19) 0.0061(17) -0.010(2) C14 0.033(2) 0.040(2) 0.030(2) 0.0011(19) 0.0111(17) -0.009(2) C15 0.0223(19) 0.024(2) 0.0193(17) -0.0090(15) 0.0035(15) -0.0007(16) C16 0.027(2) 0.024(2) 0.032(2) -0.0030(17) -0.0005(17) 0.0020(17) C17 0.034(2) 0.028(2) 0.036(2) 0.0004(18) 0.0021(19) -0.0105(19) C18 0.027(2) 0.037(2) 0.030(2) -0.0106(19) 0.0065(16) -0.0056(19) C19 0.027(2) 0.030(2) 0.031(2) -0.0086(17) 0.0024(17) 0.0025(18) C20 0.028(2) 0.024(2) 0.0236(18) -0.0056(15) 0.0047(16) -0.0004(17) C21 0.031(3) 0.054(3) 0.061(3) -0.004(2) 0.008(2) -0.011(2) C22 0.035(2) 0.041(3) 0.029(2) -0.0164(18) 0.0042(18) -0.006(2) C23 0.046(3) 0.041(2) 0.025(2) -0.0060(19) 0.0080(18) -0.024(2) C24 0.037(2) 0.031(2) 0.0261(19) 0.0078(17) 0.0081(17) -0.0079(19) _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 N4 2.018(3) . yes Pt1 N1 2.020(3) . yes Pt1 Cl1 2.3112(9) . yes Pt1 Cl2 2.3162(9) . yes O1 C2 1.356(4) . yes O1 N2 1.496(4) . yes O2 C4 1.363(4) . yes O2 N5 1.490(4) . yes N1 C2 1.305(5) . yes N1 C1 1.475(4) . yes N2 C12 1.451(5) . ? N2 C1 1.480(5) . yes N3 C2 1.323(5) . ? N3 C13 1.464(4) . ? N3 C14 1.466(4) . ? N4 C4 1.303(4) . yes N4 C3 1.469(4) . yes N5 C22 1.468(5) . ? N5 C3 1.480(4) . yes N6 C4 1.320(5) . ? N6 C23 1.459(4) . ? N6 C24 1.469(4) . ? C1 C5 1.496(5) . ? C1 H1 1.0000 . ? C3 C15 1.504(5) . ? C3 H3 1.0000 . ? C5 C10 1.371(5) . ? C5 C6 1.387(5) . ? C6 C7 1.397(5) . ? C6 H6 0.9500 . ? C7 C8 1.384(5) . ? C7 H7 0.9500 . ? C8 C9 1.380(5) . ? C8 C11 1.516(5) . ? C9 C10 1.381(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? 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 1.381(5) . ? C15 C20 1.394(5) . ? C16 C17 1.394(5) . ? C16 H16 0.9500 . ? C17 C18 1.381(5) . ? C17 H17 0.9500 . ? C18 C19 1.396(6) . ? C18 C21 1.508(5) . ? C19 C20 1.386(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 N4 Pt1 N1 178.60(12) . . ? N4 Pt1 Cl1 88.75(9) . . ? N1 Pt1 Cl1 89.99(9) . . ? N4 Pt1 Cl2 90.87(9) . . ? N1 Pt1 Cl2 90.41(9) . . ? Cl1 Pt1 Cl2 177.56(3) . . ? C2 O1 N2 102.7(3) . . ? C4 O2 N5 104.0(2) . . ? C2 N1 C1 105.6(3) . . ? C2 N1 Pt1 133.4(2) . . ? C1 N1 Pt1 119.3(2) . . ? C12 N2 C1 113.2(3) . . ? C12 N2 O1 105.5(3) . . ? C1 N2 O1 100.0(3) . . ? C2 N3 C13 122.0(3) . . ? C2 N3 C14 121.1(3) . . ? C13 N3 C14 116.5(3) . . ? C4 N4 C3 107.0(3) . . ? C4 N4 Pt1 132.0(2) . . ? C3 N4 Pt1 120.8(2) . . ? C22 N5 C3 112.3(3) . . ? C22 N5 O2 105.4(3) . . ? C3 N5 O2 101.7(2) . . ? C4 N6 C23 123.0(3) . . ? C4 N6 C24 120.9(3) . . ? C23 N6 C24 115.9(3) . . ? N1 C1 N2 100.2(3) . . ? N1 C1 C5 116.6(3) . . ? N2 C1 C5 109.3(3) . . ? N1 C1 H1 110.1 . . ? N2 C1 H1 110.1 . . ? C5 C1 H1 110.1 . . ? N1 C2 N3 130.8(3) . . ? N1 C2 O1 114.3(3) . . ? N3 C2 O1 114.9(3) . . ? N4 C3 N5 101.5(3) . . ? N4 C3 C15 115.9(3) . . ? N5 C3 C15 108.7(3) . . ? N4 C3 H3 110.1 . . ? N5 C3 H3 110.1 . . ? C15 C3 H3 110.1 . . ? N4 C4 N6 130.7(3) . . ? N4 C4 O2 114.0(3) . . ? N6 C4 O2 115.3(3) . . ? C10 C5 C6 118.5(4) . . ? C10 C5 C1 119.8(3) . . ? C6 C5 C1 121.6(3) . . ? C5 C6 C7 120.5(4) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 120.3(4) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C9 C8 C7 118.7(4) . . ? C9 C8 C11 119.5(4) . . ? C7 C8 C11 121.8(4) . . ? C8 C9 C10 120.6(4) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C5 C10 C9 121.4(4) . . ? C5 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 119.4(3) . . ? C16 C15 C3 120.5(3) . . ? C20 C15 C3 120.0(3) . . ? C15 C16 C17 119.8(4) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 121.7(4) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C19 117.8(4) . . ? C17 C18 C21 122.3(4) . . ? C19 C18 C21 119.9(4) . . ? C20 C19 C18 121.2(4) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C15 120.0(4) . . ? C19 C20 H20 120.0 . . ? C15 C20 H20 120.0 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N5 C22 H22A 109.5 . . ? N5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N6 C23 H23A 109.5 . . ? N6 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N6 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N6 C24 H24A 109.5 . . ? N6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.758 _refine_diff_density_min -1.109 _refine_diff_density_rms 0.141 #===END======================================================================== data_2c _database_code_depnum_ccdc_archive 'CCDC 803621' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H34 Cl2 N6 O2 Pt' _chemical_formula_sum 'C30 H42 Cl2 N6 O2 Pt' _chemical_formula_weight 784.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6768(2) _cell_length_b 12.1702(2) _cell_length_c 26.9509(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.1540(11) _cell_angle_gamma 90.00 _cell_volume 3155.68(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11953 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 4.653 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5144 _exptl_absorpt_correction_T_max 0.7318 _exptl_absorpt_process_details 'SADABS-2008/1 (Sheldrick, 2008)' _publ_section_exptl_refinement ; Hydrogen atoms were positioned geometrically and were constrained to ride on their parent atoms, with C---H = 0.95-1.00 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.95 \%A from atom H1 and the deepest hole is located 0.84 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44178 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 30.06 _reflns_number_total 9211 _reflns_number_gt 7209 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2008)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.2c (Brandenburg, 2009)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0199P)^2^+2.3980P] 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 9211 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0611 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.491388(11) 0.694010(9) 0.127929(4) 0.01391(4) Uani 1 1 d . . . Cl1 Cl 0.32677(8) 0.82944(7) 0.13363(3) 0.02645(18) Uani 1 1 d . . . Cl2 Cl 0.65351(8) 0.55542(6) 0.12494(3) 0.02045(16) Uani 1 1 d . . . O1 O 0.7518(2) 0.93316(18) 0.19942(7) 0.0248(5) Uani 1 1 d . . . O2 O 0.1494(2) 0.50214(18) 0.07011(7) 0.0190(5) Uani 1 1 d . . . N1 N 0.6417(3) 0.8031(2) 0.15060(9) 0.0172(5) Uani 1 1 d . . . N2 N 0.7720(3) 0.9653(2) 0.14791(9) 0.0255(6) Uani 1 1 d . . . N3 N 0.6901(3) 0.7800(2) 0.23974(9) 0.0230(6) Uani 1 1 d . . . N4 N 0.3373(2) 0.5878(2) 0.10743(8) 0.0156(5) Uani 1 1 d . . . N5 N 0.1229(3) 0.5136(2) 0.12255(8) 0.0194(6) Uani 1 1 d . . . N6 N 0.2942(3) 0.5779(2) 0.01838(8) 0.0195(6) Uani 1 1 d . . . C1 C 0.6591(3) 0.9019(3) 0.11950(11) 0.0222(7) Uani 1 1 d . . . H1 H 0.5717 0.9462 0.1178 0.027 Uiso 1 1 calc R . . C2 C 0.6896(3) 0.8328(3) 0.19618(11) 0.0191(7) Uani 1 1 d . . . C3 C 0.2657(3) 0.5342(3) 0.14691(10) 0.0181(6) Uani 1 1 d . . . H3 H 0.2611 0.5867 0.1752 0.022 Uiso 1 1 calc R . . C4 C 0.2678(3) 0.5613(2) 0.06506(10) 0.0159(6) Uani 1 1 d . . . C5 C 0.6921(3) 0.8801(3) 0.06679(11) 0.0205(7) Uani 1 1 d . . . C6 C 0.7549(3) 0.7852(3) 0.05230(12) 0.0227(7) Uani 1 1 d . . . H6 H 0.7684 0.7251 0.0748 0.027 Uiso 1 1 calc R . . C7 C 0.7984(3) 0.7774(3) 0.00494(13) 0.0261(8) Uani 1 1 d . . . H7 H 0.8407 0.7115 -0.0048 0.031 Uiso 1 1 calc R . . C8 C 0.7807(3) 0.8656(3) -0.02878(11) 0.0250(7) Uani 1 1 d . . . C9 C 0.7121(3) 0.9577(3) -0.01428(11) 0.0257(7) Uani 1 1 d . . . H9 H 0.6950 1.0171 -0.0370 0.031 Uiso 1 1 calc R . . C10 C 0.6679(3) 0.9649(3) 0.03266(12) 0.0248(7) Uani 1 1 d . . . H10 H 0.6202 1.0289 0.0417 0.030 Uiso 1 1 calc R . . C11 C 0.8415(4) 0.8603(3) -0.07789(13) 0.0370(9) Uani 1 1 d . . . H11A H 0.7918 0.9115 -0.1015 0.055 Uiso 1 1 calc R . . H11B H 0.8321 0.7854 -0.0912 0.055 Uiso 1 1 calc R . . H11C H 0.9401 0.8804 -0.0728 0.055 Uiso 1 1 calc R . . C12 C 0.9140(3) 0.9277(3) 0.14210(13) 0.0316(8) Uani 1 1 d . . . H12A H 0.9797 0.9627 0.1675 0.047 Uiso 1 1 calc R . . H12B H 0.9378 0.9476 0.1088 0.047 Uiso 1 1 calc R . . H12C H 0.9191 0.8477 0.1461 0.047 Uiso 1 1 calc R . . C13 C 0.7256(4) 0.8384(3) 0.28758(11) 0.0282(8) Uani 1 1 d . . . H13A H 0.7756 0.9074 0.2817 0.034 Uiso 1 1 calc R . . H13B H 0.7871 0.7920 0.3106 0.034 Uiso 1 1 calc R . . C14 C 0.5933(3) 0.8642(3) 0.31055(12) 0.0242(7) Uani 1 1 d . . . H14A H 0.5361 0.9159 0.2887 0.029 Uiso 1 1 calc R . . H14B H 0.6169 0.9004 0.3433 0.029 Uiso 1 1 calc R . . C15 C 0.5097(4) 0.7605(3) 0.31768(11) 0.0259(7) Uani 1 1 d . . . H15A H 0.4202 0.7803 0.3300 0.031 Uiso 1 1 calc R . . H15B H 0.5617 0.7127 0.3429 0.031 Uiso 1 1 calc R . . C16 C 0.4820(3) 0.6981(3) 0.26832(11) 0.0240(7) Uani 1 1 d . . . H16A H 0.4354 0.6276 0.2741 0.029 Uiso 1 1 calc R . . H16B H 0.4193 0.7419 0.2445 0.029 Uiso 1 1 calc R . . C17 C 0.6164(4) 0.6761(3) 0.24624(12) 0.0238(7) Uani 1 1 d . . . H17A H 0.6759 0.6268 0.2686 0.029 Uiso 1 1 calc R . . H17B H 0.5963 0.6391 0.2135 0.029 Uiso 1 1 calc R . . C18 C 0.3326(3) 0.4287(3) 0.16644(10) 0.0193(7) Uani 1 1 d . . . C19 C 0.3269(3) 0.4002(3) 0.21629(11) 0.0231(7) Uani 1 1 d . . . H19 H 0.2902 0.4509 0.2383 0.028 Uiso 1 1 calc R . . C20 C 0.3742(3) 0.2985(3) 0.23411(12) 0.0277(8) Uani 1 1 d . . . H20 H 0.3698 0.2806 0.2682 0.033 Uiso 1 1 calc R . . C21 C 0.4279(3) 0.2226(3) 0.20299(13) 0.0274(8) Uani 1 1 d . . . C22 C 0.4367(3) 0.2523(3) 0.15375(12) 0.0254(7) Uani 1 1 d . . . H22 H 0.4759 0.2023 0.1321 0.031 Uiso 1 1 calc R . . C23 C 0.3892(3) 0.3538(3) 0.13566(12) 0.0226(7) Uani 1 1 d . . . H23 H 0.3956 0.3721 0.1017 0.027 Uiso 1 1 calc R . . C24 C 0.4757(4) 0.1104(3) 0.22207(15) 0.0411(10) Uani 1 1 d . . . H24A H 0.5655 0.1173 0.2424 0.062 Uiso 1 1 calc R . . H24B H 0.4856 0.0617 0.1937 0.062 Uiso 1 1 calc R . . H24C H 0.4070 0.0797 0.2424 0.062 Uiso 1 1 calc R . . C25 C 0.0347(3) 0.6111(3) 0.12341(12) 0.0246(7) Uani 1 1 d . . . H25A H 0.0821 0.6742 0.1103 0.037 Uiso 1 1 calc R . . H25B H 0.0161 0.6262 0.1578 0.037 Uiso 1 1 calc R . . H25C H -0.0533 0.5981 0.1027 0.037 Uiso 1 1 calc R . . C26 C 0.1843(3) 0.5673(3) -0.02355(10) 0.0244(7) Uani 1 1 d . . . H26A H 0.1011 0.5329 -0.0118 0.029 Uiso 1 1 calc R . . H26B H 0.2170 0.5195 -0.0496 0.029 Uiso 1 1 calc R . . C27 C 0.1470(3) 0.6800(3) -0.04527(12) 0.0285(8) Uani 1 1 d . . . H27A H 0.1060 0.7253 -0.0201 0.034 Uiso 1 1 calc R . . H27B H 0.0768 0.6721 -0.0746 0.034 Uiso 1 1 calc R . . C28 C 0.2752(4) 0.7374(3) -0.06092(12) 0.0271(8) Uani 1 1 d . . . H28A H 0.2502 0.8124 -0.0730 0.032 Uiso 1 1 calc R . . H28B H 0.3106 0.6963 -0.0886 0.032 Uiso 1 1 calc R . . C29 C 0.3885(3) 0.7441(3) -0.01689(12) 0.0223(7) Uani 1 1 d . . . H29A H 0.4737 0.7765 -0.0282 0.027 Uiso 1 1 calc R . . H29B H 0.3571 0.7925 0.0092 0.027 Uiso 1 1 calc R . . C30 C 0.4212(3) 0.6305(3) 0.00477(11) 0.0181(6) Uani 1 1 d . . . H30A H 0.4628 0.5847 -0.0201 0.022 Uiso 1 1 calc R . . H30B H 0.4896 0.6369 0.0347 0.022 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 0.01367(6) 0.01143(6) 0.01663(6) -0.00043(5) 0.00169(4) -0.00058(5) Cl1 0.0197(4) 0.0179(4) 0.0422(5) -0.0012(3) 0.0055(3) 0.0042(3) Cl2 0.0176(4) 0.0151(4) 0.0288(4) 0.0007(3) 0.0034(3) 0.0022(3) O1 0.0308(13) 0.0212(13) 0.0225(11) -0.0045(9) 0.0032(9) -0.0092(10) O2 0.0167(11) 0.0236(13) 0.0167(10) 0.0003(9) 0.0024(8) -0.0053(9) N1 0.0154(12) 0.0132(13) 0.0230(12) -0.0010(11) 0.0021(10) -0.0026(11) N2 0.0263(15) 0.0236(16) 0.0269(14) -0.0009(12) 0.0036(12) -0.0085(13) N3 0.0255(15) 0.0244(16) 0.0191(13) -0.0044(11) 0.0026(11) -0.0049(12) N4 0.0134(12) 0.0144(13) 0.0186(12) 0.0016(10) 0.0001(10) -0.0036(10) N5 0.0176(13) 0.0238(15) 0.0170(12) 0.0010(11) 0.0024(10) -0.0005(11) N6 0.0183(13) 0.0236(15) 0.0165(12) 0.0007(11) 0.0012(10) -0.0058(12) C1 0.0245(17) 0.0145(17) 0.0274(16) 0.0022(13) 0.0015(13) -0.0012(14) C2 0.0150(15) 0.0184(17) 0.0245(15) -0.0056(13) 0.0043(12) -0.0012(13) C3 0.0165(15) 0.0180(17) 0.0194(14) 0.0009(12) 0.0005(12) -0.0023(13) C4 0.0154(15) 0.0117(15) 0.0204(14) 0.0004(12) 0.0015(11) -0.0004(12) C5 0.0202(16) 0.0171(17) 0.0237(15) 0.0010(13) 0.0002(13) -0.0049(13) C6 0.0199(17) 0.0205(19) 0.0272(16) 0.0062(13) 0.0008(13) -0.0026(13) C7 0.0215(18) 0.0189(18) 0.0382(19) -0.0037(15) 0.0044(15) -0.0008(14) C8 0.0254(18) 0.027(2) 0.0232(16) 0.0007(14) 0.0048(13) -0.0063(15) C9 0.0326(19) 0.0200(18) 0.0242(16) 0.0085(14) 0.0013(14) 0.0007(15) C10 0.0278(18) 0.0159(17) 0.0305(17) 0.0005(14) 0.0022(14) 0.0005(14) C11 0.041(2) 0.040(2) 0.0319(19) 0.0007(17) 0.0110(16) -0.0011(19) C12 0.0286(19) 0.033(2) 0.0334(18) -0.0037(16) 0.0043(15) -0.0119(17) C13 0.0287(19) 0.031(2) 0.0238(16) -0.0073(15) -0.0008(14) -0.0059(16) C14 0.0288(19) 0.0214(19) 0.0222(15) -0.0027(14) 0.0010(13) 0.0002(15) C15 0.0300(19) 0.026(2) 0.0215(15) -0.0002(14) 0.0040(14) -0.0009(16) C16 0.0272(18) 0.0218(18) 0.0226(15) 0.0018(14) 0.0012(13) -0.0065(15) C17 0.0338(19) 0.0149(18) 0.0222(15) 0.0020(13) 0.0005(14) 0.0001(14) C18 0.0152(15) 0.0212(18) 0.0210(14) 0.0050(13) -0.0004(12) -0.0015(13) C19 0.0207(17) 0.0264(19) 0.0222(15) 0.0033(14) 0.0030(13) -0.0013(14) C20 0.0237(18) 0.031(2) 0.0271(16) 0.0130(15) -0.0023(14) -0.0022(16) C21 0.0193(17) 0.026(2) 0.0375(19) 0.0097(15) 0.0041(15) 0.0025(14) C22 0.0227(18) 0.0202(19) 0.0338(18) 0.0010(15) 0.0053(14) 0.0013(14) C23 0.0210(17) 0.0221(18) 0.0251(16) 0.0068(14) 0.0040(13) -0.0025(14) C24 0.039(2) 0.030(2) 0.055(2) 0.0192(19) 0.0064(19) 0.0088(18) C25 0.0168(16) 0.029(2) 0.0277(16) -0.0006(14) 0.0021(13) 0.0024(14) C26 0.0261(17) 0.032(2) 0.0143(14) -0.0025(14) 0.0002(12) -0.0117(15) C27 0.0228(18) 0.037(2) 0.0246(16) -0.0032(15) -0.0032(13) 0.0043(16) C28 0.0304(19) 0.0212(18) 0.0281(17) 0.0052(14) -0.0037(14) 0.0003(15) C29 0.0237(18) 0.0153(17) 0.0276(16) 0.0044(14) 0.0012(13) -0.0006(14) C30 0.0176(16) 0.0170(17) 0.0204(14) 0.0014(12) 0.0055(12) 0.0000(13) _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 N4 2.006(2) . yes Pt1 N1 2.016(2) . yes Pt1 Cl1 2.3087(8) . yes Pt1 Cl2 2.3108(7) . yes O1 C2 1.361(4) . yes O1 N2 1.475(3) . yes O2 C4 1.372(3) . yes O2 N5 1.470(3) . yes N1 C2 1.316(4) . yes N1 C1 1.485(4) . yes N2 C12 1.473(4) . ? N2 C1 1.482(4) . yes N3 C2 1.338(4) . ? N3 C17 1.471(4) . ? N3 C13 1.481(4) . ? N4 C4 1.302(4) . yes N4 C3 1.482(4) . yes N5 C25 1.464(4) . ? N5 C3 1.486(4) . yes N6 C4 1.326(3) . ? N6 C30 1.467(4) . ? N6 C26 1.472(4) . ? C1 C5 1.512(4) . ? C1 H1 1.0000 . ? C3 C18 1.507(4) . ? C3 H3 1.0000 . ? C5 C6 1.380(4) . ? C5 C10 1.386(4) . ? C6 C7 1.389(4) . ? C6 H6 0.9500 . ? C7 C8 1.405(5) . ? C7 H7 0.9500 . ? C8 C9 1.381(5) . ? C8 C11 1.506(4) . ? C9 C10 1.381(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.514(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.522(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.530(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.511(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.385(4) . ? C18 C19 1.395(4) . ? C19 C20 1.387(5) . ? C19 H19 0.9500 . ? C20 C21 1.385(5) . ? C20 H20 0.9500 . ? C21 C22 1.387(5) . ? C21 C24 1.514(5) . ? C22 C23 1.388(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.520(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.523(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.529(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.521(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? 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 N4 Pt1 N1 177.74(9) . . ? N4 Pt1 Cl1 88.90(7) . . ? N1 Pt1 Cl1 89.44(7) . . ? N4 Pt1 Cl2 90.41(7) . . ? N1 Pt1 Cl2 91.19(7) . . ? Cl1 Pt1 Cl2 177.81(3) . . ? C2 O1 N2 106.2(2) . . ? C4 O2 N5 106.2(2) . . ? C2 N1 C1 104.8(2) . . ? C2 N1 Pt1 129.3(2) . . ? C1 N1 Pt1 118.93(19) . . ? C12 N2 O1 103.7(2) . . ? C12 N2 C1 115.3(3) . . ? O1 N2 C1 100.6(2) . . ? C2 N3 C17 124.1(3) . . ? C2 N3 C13 120.8(3) . . ? C17 N3 C13 112.3(2) . . ? C4 N4 C3 106.5(2) . . ? C4 N4 Pt1 134.4(2) . . ? C3 N4 Pt1 118.47(18) . . ? C25 N5 O2 104.7(2) . . ? C25 N5 C3 111.8(2) . . ? O2 N5 C3 101.0(2) . . ? C4 N6 C30 123.8(2) . . ? C4 N6 C26 121.2(2) . . ? C30 N6 C26 113.7(2) . . ? N2 C1 N1 104.6(2) . . ? N2 C1 C5 111.0(2) . . ? N1 C1 C5 115.9(3) . . ? N2 C1 H1 108.4 . . ? N1 C1 H1 108.4 . . ? C5 C1 H1 108.4 . . ? N1 C2 N3 130.9(3) . . ? N1 C2 O1 114.5(3) . . ? N3 C2 O1 114.5(3) . . ? N4 C3 N5 104.0(2) . . ? N4 C3 C18 114.1(2) . . ? N5 C3 C18 110.8(2) . . ? N4 C3 H3 109.3 . . ? N5 C3 H3 109.3 . . ? C18 C3 H3 109.3 . . ? N4 C4 N6 131.3(3) . . ? N4 C4 O2 113.7(2) . . ? N6 C4 O2 115.0(2) . . ? C6 C5 C10 118.9(3) . . ? C6 C5 C1 123.8(3) . . ? C10 C5 C1 117.1(3) . . ? C5 C6 C7 120.2(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C8 120.9(3) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C7 117.8(3) . . ? C9 C8 C11 121.9(3) . . ? C7 C8 C11 120.3(3) . . ? C8 C9 C10 121.1(3) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C9 C10 C5 120.9(3) . . ? C9 C10 H10 119.6 . . ? C5 C10 H10 119.6 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 109.1(3) . . ? N3 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? N3 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C13 C14 C15 111.4(3) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C16 110.3(3) . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C15 110.7(3) . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N3 C17 C16 110.1(3) . . ? N3 C17 H17A 109.7 . . ? C16 C17 H17A 109.7 . . ? N3 C17 H17B 109.7 . . ? C16 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C23 C18 C19 118.2(3) . . ? C23 C18 C3 122.3(3) . . ? C19 C18 C3 119.2(3) . . ? C20 C19 C18 120.7(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 121.1(3) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 118.1(3) . . ? C20 C21 C24 121.1(3) . . ? C22 C21 C24 120.8(3) . . ? C21 C22 C23 121.1(3) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C18 C23 C22 120.9(3) . . ? C18 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 H25A 109.5 . . ? N5 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N5 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N6 C26 C27 109.8(3) . . ? N6 C26 H26A 109.7 . . ? C27 C26 H26A 109.7 . . ? N6 C26 H26B 109.7 . . ? C27 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C26 C27 C28 110.7(3) . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 C29 110.3(3) . . ? C27 C28 H28A 109.6 . . ? C29 C28 H28A 109.6 . . ? C27 C28 H28B 109.6 . . ? C29 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C30 C29 C28 110.6(3) . . ? C30 C29 H29A 109.5 . . ? C28 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? N6 C30 C29 110.4(2) . . ? N6 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? N6 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.361 _refine_diff_density_min -1.167 _refine_diff_density_rms 0.147 #===END======================================================================== data_2d _database_code_depnum_ccdc_archive 'CCDC 803622' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H42 Cl2 N6 O4 Pt' _chemical_formula_sum 'C36 H42 Cl2 N6 O4 Pt' _chemical_formula_weight 888.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4287(7) _cell_length_b 11.1631(8) _cell_length_c 19.8266(14) _cell_angle_alpha 90.00 _cell_angle_beta 97.669(4) _cell_angle_gamma 90.00 _cell_volume 1848.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4335 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 3.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5259 _exptl_absorpt_correction_T_max 0.7733 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _publ_section_exptl_refinement ; The hydrogen atoms were positioned geometrically and constrained to ride on their parent atoms, with C---H = 0.95-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.97 \%A from atom Pt1 and the deepest hole is located 0.94 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11105 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.25 _reflns_number_total 3320 _reflns_number_gt 2381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2008)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.2c (Brandenburg, 2009)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+17.6262P] 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 3320 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 1.0000 0.5000 0.03773(15) Uani 1 2 d S . . Cl1 Cl 0.6847(3) 1.1007(2) 0.44513(12) 0.0528(6) Uani 1 1 d . . . O1 O 0.7825(9) 1.0665(10) 0.6883(4) 0.103(4) Uani 1 1 d . . . O3 O 0.7807(11) 0.4658(7) 0.5256(5) 0.082(3) Uani 1 1 d . . . N1 N 0.6507(8) 1.0194(6) 0.5877(3) 0.0423(18) Uani 1 1 d . . . N2 N 0.8878(10) 0.9777(8) 0.6603(4) 0.056(2) Uani 1 1 d . . . N3 N 0.5491(11) 1.1616(11) 0.6582(4) 0.086(4) Uani 1 1 d . . . C1 C 0.8050(12) 0.9579(9) 0.5890(5) 0.052(3) Uani 1 1 d . . . H1 H 0.8681 0.9979 0.5561 0.062 Uiso 1 1 calc R . . C2 C 0.6513(11) 1.0837(11) 0.6414(4) 0.054(3) Uani 1 1 d . . . C5 C 0.7940(12) 0.8275(10) 0.5735(5) 0.053(2) Uani 1 1 d . . . C6 C 0.8859(14) 0.7784(11) 0.5287(6) 0.067(3) Uani 1 1 d . . . H6 H 0.9569 0.8280 0.5078 0.080 Uiso 1 1 calc R . . C7 C 0.8767(15) 0.6595(11) 0.5138(6) 0.070(3) Uani 1 1 d . . . H7 H 0.9396 0.6272 0.4818 0.084 Uiso 1 1 calc R . . C8 C 0.7788(13) 0.5868(9) 0.5439(5) 0.054(3) Uani 1 1 d . . . C9 C 0.6856(13) 0.6298(11) 0.5910(6) 0.065(3) Uani 1 1 d . . . H9 H 0.6191 0.5782 0.6131 0.079 Uiso 1 1 calc R . . C10 C 0.6941(12) 0.7568(10) 0.6051(5) 0.058(3) Uani 1 1 d . . . H10 H 0.6304 0.7910 0.6363 0.070 Uiso 1 1 calc R . . C11 C 0.6769(16) 0.3890(11) 0.5569(8) 0.093(4) Uani 1 1 d . . . H11A H 0.7051 0.3922 0.6064 0.139 Uiso 1 1 calc R . . H11B H 0.6883 0.3067 0.5411 0.139 Uiso 1 1 calc R . . H11C H 0.5659 0.4153 0.5446 0.139 Uiso 1 1 calc R . . C12 C 1.0376(11) 1.0342(10) 0.6598(5) 0.059(3) Uani 1 1 d . . . H12A H 1.0200 1.1170 0.6425 0.071 Uiso 1 1 calc R . . H12B H 1.0987 0.9907 0.6282 0.071 Uiso 1 1 calc R . . C13 C 1.1353(12) 1.0384(11) 0.7292(5) 0.067(3) Uani 1 1 d . . . C14 C 1.2508(17) 0.9507(14) 0.7450(7) 0.097(5) Uani 1 1 d . . . H14 H 1.2627 0.8887 0.7132 0.117 Uiso 1 1 calc R . . C15 C 1.3502(19) 0.9530(16) 0.8078(7) 0.123(6) Uani 1 1 d . . . H15 H 1.4331 0.8955 0.8179 0.147 Uiso 1 1 calc R . . C16 C 1.3248(17) 1.0410(17) 0.8546(7) 0.109(6) Uani 1 1 d . . . H16 H 1.3893 1.0431 0.8977 0.131 Uiso 1 1 calc R . . C17 C 1.2097(18) 1.1231(17) 0.8392(7) 0.107(5) Uani 1 1 d . . . H17 H 1.1931 1.1833 0.8714 0.128 Uiso 1 1 calc R . . C18 C 1.1144(15) 1.1205(14) 0.7765(7) 0.099(5) Uani 1 1 d . . . H18 H 1.0322 1.1787 0.7668 0.118 Uiso 1 1 calc R . . C19 C 0.4067(12) 1.1970(11) 0.6131(6) 0.068(3) Uani 1 1 d . . . H19A H 0.4213 1.1792 0.5659 0.102 Uiso 1 1 calc R . . H19B H 0.3886 1.2831 0.6179 0.102 Uiso 1 1 calc R . . H19C H 0.3141 1.1526 0.6250 0.102 Uiso 1 1 calc R . . C20 C 0.5650(16) 1.2122(18) 0.7279(6) 0.147(9) Uani 1 1 d . . . H20A H 0.6403 1.1635 0.7584 0.221 Uiso 1 1 calc R . . H20B H 0.4603 1.2120 0.7443 0.221 Uiso 1 1 calc R . . H20C H 0.6051 1.2945 0.7273 0.221 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 0.0417(3) 0.0375(2) 0.0298(2) -0.0016(3) -0.01047(17) -0.0027(3) Cl1 0.0565(15) 0.0523(13) 0.0476(13) 0.0011(11) -0.0008(11) -0.0117(12) O1 0.044(4) 0.213(11) 0.045(4) -0.052(6) -0.020(3) 0.013(5) O3 0.084(6) 0.064(6) 0.098(7) -0.006(4) 0.014(5) 0.007(4) N1 0.046(4) 0.040(5) 0.037(4) -0.002(3) -0.012(3) 0.002(3) N2 0.059(5) 0.068(6) 0.037(4) -0.005(4) -0.017(4) -0.011(4) N3 0.050(6) 0.155(10) 0.049(5) -0.051(6) -0.010(4) 0.024(6) C1 0.048(6) 0.068(7) 0.037(5) -0.004(4) -0.001(4) -0.008(5) C2 0.035(5) 0.093(8) 0.031(5) -0.013(5) -0.009(4) -0.005(5) C5 0.043(6) 0.073(7) 0.037(5) 0.003(5) -0.012(4) 0.001(5) C6 0.062(7) 0.072(8) 0.064(7) 0.019(6) -0.003(6) 0.010(6) C7 0.073(8) 0.068(8) 0.068(7) 0.008(6) 0.006(6) 0.019(6) C8 0.054(7) 0.049(6) 0.055(6) -0.008(5) -0.008(5) 0.013(5) C9 0.044(6) 0.084(9) 0.066(7) 0.012(6) -0.001(5) -0.008(6) C10 0.052(6) 0.079(8) 0.039(5) -0.015(5) -0.008(5) 0.013(6) C11 0.079(9) 0.064(8) 0.133(13) 0.026(9) 0.003(9) -0.023(7) C12 0.043(6) 0.082(8) 0.049(6) -0.011(5) -0.001(5) 0.006(5) C13 0.037(6) 0.114(10) 0.048(6) -0.029(6) -0.002(5) -0.005(6) C14 0.078(9) 0.130(12) 0.072(8) -0.030(8) -0.036(7) 0.005(8) C15 0.106(12) 0.172(18) 0.078(10) -0.036(10) -0.030(9) 0.021(11) C16 0.073(9) 0.186(19) 0.063(8) -0.028(10) -0.017(7) -0.010(10) C17 0.084(10) 0.172(16) 0.058(8) -0.042(9) -0.011(7) 0.012(11) C18 0.059(8) 0.147(14) 0.085(9) -0.051(10) -0.009(7) 0.015(8) C19 0.046(6) 0.086(8) 0.068(7) -0.025(6) -0.009(5) -0.003(6) C20 0.071(10) 0.29(2) 0.074(9) -0.108(13) -0.027(7) 0.028(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 N1 2.023(7) 3_676 ? Pt1 N1 2.023(7) . yes Pt1 Cl1 2.307(2) . yes Pt1 Cl1 2.307(2) 3_676 ? O1 C2 1.360(11) . yes O1 N2 1.487(11) . yes O3 C8 1.399(13) . ? O3 C11 1.424(13) . ? N1 C2 1.285(11) . yes N1 C1 1.468(12) . yes N2 C12 1.413(12) . ? N2 C1 1.508(11) . yes N3 C2 1.298(13) . ? N3 C19 1.453(13) . ? N3 C20 1.483(13) . ? C1 C5 1.488(14) . ? C1 H1 1.0000 . ? C5 C10 1.366(14) . ? C5 C6 1.368(14) . ? C6 C7 1.361(15) . ? C6 H6 0.9500 . ? C7 C8 1.351(15) . ? C7 H7 0.9500 . ? C8 C9 1.385(14) . ? C9 C10 1.444(15) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.507(13) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.339(15) . ? C13 C14 1.387(17) . ? C14 C15 1.404(18) . ? C14 H14 0.9500 . ? C15 C16 1.388(19) . ? C15 H15 0.9500 . ? C16 C17 1.34(2) . ? C16 H16 0.9500 . ? C17 C18 1.388(17) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N1 179.999(2) 3_676 . ? N1 Pt1 Cl1 91.9(2) 3_676 . ? N1 Pt1 Cl1 88.1(2) . . ? N1 Pt1 Cl1 88.1(2) 3_676 3_676 ? N1 Pt1 Cl1 91.9(2) . 3_676 ? Cl1 Pt1 Cl1 179.999(1) . 3_676 ? C2 O1 N2 108.1(7) . . ? C8 O3 C11 116.1(10) . . ? C2 N1 C1 110.0(7) . . ? C2 N1 Pt1 134.9(7) . . ? C1 N1 Pt1 114.7(5) . . ? C12 N2 O1 106.5(8) . . ? C12 N2 C1 111.1(8) . . ? O1 N2 C1 102.9(7) . . ? C2 N3 C19 123.1(8) . . ? C2 N3 C20 120.9(10) . . ? C19 N3 C20 115.8(10) . . ? N1 C1 C5 115.1(8) . . ? N1 C1 N2 104.3(7) . . ? C5 C1 N2 110.2(8) . . ? N1 C1 H1 109.0 . . ? C5 C1 H1 109.0 . . ? N2 C1 H1 109.0 . . ? N1 C2 N3 131.1(9) . . ? N1 C2 O1 113.6(9) . . ? N3 C2 O1 115.2(9) . . ? C10 C5 C6 120.2(10) . . ? C10 C5 C1 119.7(10) . . ? C6 C5 C1 120.0(10) . . ? C7 C6 C5 120.8(11) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 C6 120.7(11) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 121.7(10) . . ? C7 C8 O3 115.9(10) . . ? C9 C8 O3 122.4(11) . . ? C8 C9 C10 116.9(10) . . ? C8 C9 H9 121.5 . . ? C10 C9 H9 121.5 . . ? C5 C10 C9 119.7(10) . . ? C5 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? O3 C11 H11A 109.5 . . ? O3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C13 112.7(8) . . ? N2 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? N2 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C18 C13 C14 118.7(11) . . ? C18 C13 C12 123.6(11) . . ? C14 C13 C12 117.8(10) . . ? C13 C14 C15 120.3(13) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 118.6(15) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C17 C16 C15 120.3(13) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.3(14) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 121.8(14) . . ? C13 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.605 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.126 #===END======================================================================== data_1b _database_code_depnum_ccdc_archive 'CCDC 803623' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H31 Cl2 N5 O Pt' _chemical_formula_sum 'C19 H31 Cl2 N5 O Pt' _chemical_formula_weight 611.48 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2227(2) _cell_length_b 11.0745(3) _cell_length_c 13.7740(4) _cell_angle_alpha 102.4393(13) _cell_angle_beta 99.8321(14) _cell_angle_gamma 102.6972(13) _cell_volume 1163.15(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6069 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 6.280 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4011 _exptl_absorpt_correction_T_max 0.7319 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _publ_section_exptl_refinement ; The N,N'-diethylcyanamide ligand was heavily disordered. The N5, C6, and C7 atoms were disordered over two sites with occupancies 0.9 and 0.1. The C4 and C5 carbon atoms were disordered over three sites with occupacies 0.7, 0.2, and 0.1 respectively. The anisotropic displacement pameters of the disordered atoms were constrained to be similar. Also, the C---C and N---C distances in the N,N'-diethylcyanamide ligand were restrained to be similar. Hydrogen atoms were positioned geometrically and constrained to ride on their parent carbon atoms, with C---H = 0.95-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.30 \%A from atom C7B and the deepest hole is located 0.45 \%A from atom C6A. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_measurement_device '62mm x 62mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 16 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16522 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5325 _reflns_number_gt 5044 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2008)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.2c (Brandenburg, 2009)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0144P)^2^+4.1458P] 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 5325 _refine_ls_number_parameters 284 _refine_ls_number_restraints 73 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0572 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.105 _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 0.986452(16) 0.793885(12) 0.297224(10) 0.01403(5) Uani 1 1 d . . . Cl1 Cl 0.85400(12) 0.78295(9) 0.13332(7) 0.02217(18) Uani 1 1 d . . . Cl2 Cl 1.11814(13) 0.79774(10) 0.45965(7) 0.0270(2) Uani 1 1 d . . . O1 O 1.4142(3) 1.1031(2) 0.3484(2) 0.0173(5) Uani 1 1 d . . . N4 N 0.8141(4) 0.6372(3) 0.2912(3) 0.0237(7) Uani 1 1 d . A . C3 C 0.7189(6) 0.5442(4) 0.2892(5) 0.0397(12) Uani 1 1 d D . . N5A N 0.6159(8) 0.4379(5) 0.2984(6) 0.064(2) Uani 0.90 1 d PD A 1 C6A C 0.4691(10) 0.3705(8) 0.2274(6) 0.0658(19) Uani 0.90 1 d PDU A 1 H6A1 H 0.3757 0.4109 0.2394 0.079 Uiso 0.90 1 calc PR A 1 H6A2 H 0.4355 0.2818 0.2341 0.079 Uiso 0.90 1 calc PR A 1 C7A C 0.4930(10) 0.3676(8) 0.1267(6) 0.0528(19) Uani 0.90 1 d PDU A 1 H7A1 H 0.5117 0.4544 0.1172 0.079 Uiso 0.90 1 calc PR A 1 H7A2 H 0.3908 0.3109 0.0765 0.079 Uiso 0.90 1 calc PR A 1 H7A3 H 0.5927 0.3356 0.1171 0.079 Uiso 0.90 1 calc PR A 1 C4A C 0.6568(11) 0.3895(8) 0.3941(7) 0.0456(18) Uani 0.70 1 d PDU A 1 H4A1 H 0.5479 0.3511 0.4108 0.055 Uiso 0.70 1 calc PR A 1 H4A2 H 0.7152 0.3208 0.3783 0.055 Uiso 0.70 1 calc PR A 1 C5A C 0.7577(16) 0.4828(12) 0.4783(10) 0.086(3) Uani 0.70 1 d PDU A 1 H5A1 H 0.8702 0.5157 0.4649 0.128 Uiso 0.70 1 calc PR A 1 H5A2 H 0.7718 0.4464 0.5370 0.128 Uiso 0.70 1 calc PR A 1 H5A3 H 0.7034 0.5529 0.4930 0.128 Uiso 0.70 1 calc PR A 1 C4B C 0.646(4) 0.455(3) 0.4231(14) 0.0456(18) Uani 0.20 1 d PDU A 1 H4B1 H 0.7325 0.4057 0.4289 0.055 Uiso 0.20 1 calc PR A 1 H4B2 H 0.7154 0.5453 0.4446 0.055 Uiso 0.20 1 calc PR A 1 C5B C 0.605(6) 0.451(4) 0.511(2) 0.086(3) Uani 0.20 1 d PDU A 1 H5B1 H 0.6294 0.5387 0.5543 0.128 Uiso 0.20 1 calc PR A 1 H5B2 H 0.6714 0.4029 0.5454 0.128 Uiso 0.20 1 calc PR A 1 H5B3 H 0.4822 0.4089 0.4987 0.128 Uiso 0.20 1 calc PR A 1 N5B N 0.583(6) 0.440(4) 0.247(3) 0.064(2) Uani 0.10 1 d PD A 2 C6B C 0.527(14) 0.362(7) 0.145(3) 0.0658(19) Uani 0.10 1 d PDU A 2 H6B1 H 0.4122 0.3054 0.1377 0.079 Uiso 0.10 1 calc PR A 2 H6B2 H 0.6051 0.3064 0.1343 0.079 Uiso 0.10 1 calc PR A 2 C7B C 0.516(8) 0.431(6) 0.056(4) 0.0528(19) Uani 0.10 1 d PDU A 2 H7B1 H 0.6315 0.4767 0.0542 0.079 Uiso 0.10 1 calc PR A 2 H7B2 H 0.4465 0.4914 0.0671 0.079 Uiso 0.10 1 calc PR A 2 H7B3 H 0.4633 0.3662 -0.0096 0.079 Uiso 0.10 1 calc PR A 2 C4C C 0.565(7) 0.366(3) 0.337(4) 0.0456(18) Uani 0.10 1 d PDU A 2 H4C1 H 0.4452 0.3158 0.3258 0.055 Uiso 0.10 1 calc PR A 2 H4C2 H 0.6390 0.3065 0.3347 0.055 Uiso 0.10 1 calc PR A 2 C5C C 0.614(13) 0.455(6) 0.430(3) 0.086(3) Uani 0.10 1 d PDU A 2 H5C1 H 0.5702 0.4158 0.4812 0.128 Uiso 0.10 1 calc PR A 2 H5C2 H 0.5664 0.5282 0.4255 0.128 Uiso 0.10 1 calc PR A 2 H5C3 H 0.7389 0.4851 0.4507 0.128 Uiso 0.10 1 calc PR A 2 N1 N 1.1613(4) 0.9571(3) 0.3090(2) 0.0132(6) Uani 1 1 d . . . N2 N 1.3110(4) 1.1600(3) 0.4135(2) 0.0171(6) Uani 1 1 d . . . N3 N 1.4055(4) 0.9056(3) 0.2554(2) 0.0184(6) Uani 1 1 d . . . C1 C 1.1372(4) 1.0835(3) 0.3557(3) 0.0143(7) Uani 1 1 d . . . H1 H 1.0581 1.0746 0.4030 0.017 Uiso 1 1 calc R . . C8 C 1.0746(5) 1.1515(3) 0.2781(3) 0.0173(7) Uani 1 1 d . . . C9 C 1.0346(6) 1.2652(4) 0.3158(3) 0.0268(9) Uani 1 1 d . . . H9 H 1.0335 1.2916 0.3860 0.032 Uiso 1 1 calc R . . C10 C 0.9963(6) 1.3407(4) 0.2512(3) 0.0271(9) Uani 1 1 d . . . H10 H 0.9708 1.4191 0.2782 0.033 Uiso 1 1 calc R . . C11 C 0.9945(5) 1.3043(4) 0.1487(3) 0.0207(8) Uani 1 1 d . . . C14 C 0.9556(6) 1.3876(4) 0.0789(3) 0.0269(9) Uani 1 1 d . . . H14A H 0.9682 1.4746 0.1199 0.040 Uiso 1 1 calc R . . H14B H 0.8379 1.3517 0.0379 0.040 Uiso 1 1 calc R . . H14C H 1.0353 1.3905 0.0335 0.040 Uiso 1 1 calc R . . C12 C 1.0316(5) 1.1885(4) 0.1107(3) 0.0195(7) Uani 1 1 d . . . H12 H 1.0295 1.1608 0.0402 0.023 Uiso 1 1 calc R . . C13 C 1.0716(5) 1.1132(3) 0.1756(3) 0.0173(7) Uani 1 1 d . . . H13 H 1.0970 1.0348 0.1489 0.021 Uiso 1 1 calc R . . C15 C 1.3610(5) 1.1340(4) 0.5126(3) 0.0234(8) Uani 1 1 d . . . H15A H 1.3372 1.0411 0.5038 0.035 Uiso 1 1 calc R . . H15C H 1.2956 1.1696 0.5593 0.035 Uiso 1 1 calc R . . H15B H 1.4836 1.1739 0.5411 0.035 Uiso 1 1 calc R . . C2 C 1.3201(4) 0.9800(3) 0.3019(3) 0.0144(7) Uani 1 1 d . . . C18 C 1.5867(5) 0.9603(4) 0.2543(3) 0.0232(8) Uani 1 1 d . . . H18A H 1.6463 0.8914 0.2475 0.028 Uiso 1 1 calc R . . H18B H 1.6445 1.0253 0.3198 0.028 Uiso 1 1 calc R . . C19 C 1.5982(6) 1.0222(5) 0.1663(4) 0.0361(11) Uani 1 1 d . . . H19A H 1.5413 0.9578 0.1015 0.054 Uiso 1 1 calc R . . H19B H 1.7188 1.0568 0.1667 0.054 Uiso 1 1 calc R . . H19C H 1.5418 1.0919 0.1741 0.054 Uiso 1 1 calc R . . C16 C 1.3190(5) 0.7798(4) 0.1847(3) 0.0264(9) Uani 1 1 d . . . H16A H 1.3651 0.7715 0.1224 0.032 Uiso 1 1 calc R . . H16B H 1.1952 0.7729 0.1643 0.032 Uiso 1 1 calc R . . C17 C 1.3428(7) 0.6717(4) 0.2321(5) 0.0503(16) Uani 1 1 d . . . H17A H 1.4653 0.6794 0.2538 0.075 Uiso 1 1 calc R . . H17B H 1.2872 0.5892 0.1817 0.075 Uiso 1 1 calc R . . H17C H 1.2912 0.6766 0.2914 0.075 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 0.01160(7) 0.01240(7) 0.01772(8) 0.00382(5) 0.00507(5) 0.00124(5) Cl1 0.0195(4) 0.0223(4) 0.0198(4) 0.0032(3) -0.0007(3) 0.0018(3) Cl2 0.0312(5) 0.0268(5) 0.0208(5) 0.0133(4) 0.0034(4) -0.0016(4) O1 0.0155(12) 0.0170(12) 0.0183(13) 0.0038(10) 0.0047(10) 0.0023(10) N4 0.0171(15) 0.0186(16) 0.0333(19) 0.0054(14) 0.0080(14) 0.0003(13) C3 0.022(2) 0.018(2) 0.077(4) 0.003(2) 0.020(2) 0.0024(17) N5A 0.038(3) 0.025(2) 0.118(6) -0.001(3) 0.033(4) -0.005(2) C6A 0.060(3) 0.059(3) 0.078(3) 0.022(3) 0.011(3) 0.014(3) C7A 0.042(3) 0.047(3) 0.057(3) 0.003(2) 0.004(2) 0.003(2) C4A 0.052(3) 0.037(3) 0.051(3) 0.019(2) 0.021(2) 0.006(2) C5A 0.094(4) 0.081(4) 0.082(4) 0.028(3) 0.021(3) 0.018(3) C4B 0.052(3) 0.037(3) 0.051(3) 0.019(2) 0.021(2) 0.006(2) C5B 0.094(4) 0.081(4) 0.082(4) 0.028(3) 0.021(3) 0.018(3) N5B 0.038(3) 0.025(2) 0.118(6) -0.001(3) 0.033(4) -0.005(2) C6B 0.060(3) 0.059(3) 0.078(3) 0.022(3) 0.011(3) 0.014(3) C7B 0.042(3) 0.047(3) 0.057(3) 0.003(2) 0.004(2) 0.003(2) C4C 0.052(3) 0.037(3) 0.051(3) 0.019(2) 0.021(2) 0.006(2) C5C 0.094(4) 0.081(4) 0.082(4) 0.028(3) 0.021(3) 0.018(3) N1 0.0134(14) 0.0123(14) 0.0145(14) 0.0039(11) 0.0059(11) 0.0021(11) N2 0.0187(15) 0.0165(15) 0.0156(15) 0.0034(12) 0.0049(12) 0.0038(12) N3 0.0096(14) 0.0216(16) 0.0221(16) 0.0032(13) 0.0051(12) 0.0016(12) C1 0.0164(16) 0.0112(16) 0.0170(17) 0.0041(13) 0.0066(14) 0.0043(13) C8 0.0168(17) 0.0176(17) 0.0200(18) 0.0077(14) 0.0058(14) 0.0055(14) C9 0.040(2) 0.029(2) 0.021(2) 0.0106(17) 0.0126(18) 0.0206(19) C10 0.037(2) 0.028(2) 0.026(2) 0.0112(17) 0.0125(18) 0.0205(19) C11 0.0184(18) 0.0233(19) 0.024(2) 0.0128(16) 0.0057(15) 0.0061(15) C14 0.031(2) 0.029(2) 0.026(2) 0.0153(17) 0.0060(17) 0.0104(18) C12 0.0187(18) 0.0219(19) 0.0160(17) 0.0074(15) 0.0032(14) 0.0000(15) C13 0.0170(17) 0.0143(17) 0.0186(18) 0.0037(14) 0.0041(14) 0.0005(13) C15 0.029(2) 0.0227(19) 0.0139(18) 0.0031(15) -0.0004(15) 0.0025(16) C2 0.0150(16) 0.0147(16) 0.0124(16) 0.0050(13) 0.0025(13) 0.0008(13) C18 0.0131(17) 0.033(2) 0.025(2) 0.0076(17) 0.0076(15) 0.0071(16) C19 0.025(2) 0.052(3) 0.038(3) 0.021(2) 0.015(2) 0.010(2) C16 0.0170(18) 0.029(2) 0.025(2) -0.0096(17) 0.0028(16) 0.0056(16) C17 0.035(3) 0.020(2) 0.078(4) -0.010(2) -0.010(3) 0.011(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 N4 1.960(3) . yes Pt1 N1 2.003(3) . yes Pt1 Cl1 2.2983(9) . yes Pt1 Cl2 2.3002(10) . yes O1 C2 1.364(4) . yes O1 N2 1.474(4) . yes N4 C3 1.141(5) . yes C3 N5A 1.335(7) . yes C3 N5B 1.35(2) . yes N5A C6A 1.363(10) . ? N5A C4A 1.540(10) . ? N5A C4B 1.655(17) . ? C6A C7A 1.428(12) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C4A C5A 1.371(14) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? C4B C5B 1.32(2) . ? C4B H4B1 0.9900 . ? C4B H4B2 0.9900 . ? C5B H5B1 0.9800 . ? C5B H5B2 0.9800 . ? C5B H5B3 0.9800 . ? N5B C6B 1.42(2) . ? N5B C4C 1.64(2) . ? C6B C7B 1.57(2) . ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? C4C C5C 1.38(2) . ? C4C H4C1 0.9900 . ? C4C H4C2 0.9900 . ? C5C H5C1 0.9800 . ? C5C H5C2 0.9800 . ? C5C H5C3 0.9800 . ? N1 C2 1.299(4) . yes N1 C1 1.480(4) . yes N2 C15 1.465(5) . ? N2 C1 1.478(5) . yes N3 C2 1.328(5) . ? N3 C16 1.461(5) . ? N3 C18 1.484(5) . ? C1 C8 1.517(5) . ? C1 H1 1.0000 . ? C8 C13 1.379(5) . ? C8 C9 1.386(5) . ? C9 C10 1.390(5) . ? C9 H9 0.9500 . ? C10 C11 1.379(6) . ? C10 H10 0.9500 . ? C11 C12 1.396(5) . ? C11 C14 1.511(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C12 C13 1.394(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C15 H15A 0.9800 . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C18 C19 1.523(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C16 C17 1.514(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 N4 Pt1 N1 177.65(13) . . ? N4 Pt1 Cl1 88.99(11) . . ? N1 Pt1 Cl1 92.65(9) . . ? N4 Pt1 Cl2 89.67(11) . . ? N1 Pt1 Cl2 88.74(9) . . ? Cl1 Pt1 Cl2 178.13(3) . . ? C2 O1 N2 105.8(2) . . ? C3 N4 Pt1 177.3(4) . . ? N4 C3 N5A 173.3(7) . . ? N4 C3 N5B 155.2(18) . . ? N5A C3 N5B 31.4(16) . . ? C3 N5A C6A 122.7(7) . . ? C3 N5A C4A 120.2(6) . . ? C6A N5A C4A 117.1(6) . . ? C3 N5A C4B 104.7(10) . . ? C6A N5A C4B 125.7(12) . . ? C4A N5A C4B 28.0(11) . . ? N5A C6A C7A 110.6(7) . . ? N5A C6A H6A1 109.5 . . ? C7A C6A H6A1 109.5 . . ? N5A C6A H6A2 109.5 . . ? C7A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 108.1 . . ? C5A C4A N5A 114.1(8) . . ? C5A C4A H4A1 108.7 . . ? N5A C4A H4A1 108.7 . . ? C5A C4A H4A2 108.7 . . ? N5A C4A H4A2 108.7 . . ? H4A1 C4A H4A2 107.6 . . ? C5B C4B N5A 158(3) . . ? C5B C4B H4B1 96.9 . . ? N5A C4B H4B1 96.9 . . ? C5B C4B H4B2 96.9 . . ? N5A C4B H4B2 96.9 . . ? H4B1 C4B H4B2 103.5 . . ? C3 N5B C6B 130(6) . . ? C3 N5B C4C 104.7(18) . . ? C6B N5B C4C 116(4) . . ? N5B C6B C7B 118(5) . . ? N5B C6B H6B1 107.8 . . ? C7B C6B H6B1 107.8 . . ? N5B C6B H6B2 107.8 . . ? C7B C6B H6B2 107.8 . . ? H6B1 C6B H6B2 107.2 . . ? C6B C7B H7B1 109.5 . . ? C6B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C6B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C5C C4C N5B 109(3) . . ? C5C C4C H4C1 109.8 . . ? N5B C4C H4C1 109.8 . . ? C5C C4C H4C2 109.8 . . ? N5B C4C H4C2 109.8 . . ? H4C1 C4C H4C2 108.3 . . ? C4C C5C H5C1 109.5 . . ? C4C C5C H5C2 109.5 . . ? H5C1 C5C H5C2 109.5 . . ? C4C C5C H5C3 109.5 . . ? H5C1 C5C H5C3 109.5 . . ? H5C2 C5C H5C3 109.5 . . ? C2 N1 C1 105.4(3) . . ? C2 N1 Pt1 131.9(2) . . ? C1 N1 Pt1 121.2(2) . . ? C15 N2 O1 105.8(3) . . ? C15 N2 C1 113.3(3) . . ? O1 N2 C1 100.1(2) . . ? C2 N3 C16 122.1(3) . . ? C2 N3 C18 119.8(3) . . ? C16 N3 C18 116.6(3) . . ? N2 C1 N1 103.9(3) . . ? N2 C1 C8 108.0(3) . . ? N1 C1 C8 113.6(3) . . ? N2 C1 H1 110.4 . . ? N1 C1 H1 110.4 . . ? C8 C1 H1 110.4 . . ? C13 C8 C9 119.1(3) . . ? C13 C8 C1 123.7(3) . . ? C9 C8 C1 116.9(3) . . ? C8 C9 C10 120.2(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 121.4(4) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C11 C12 118.2(3) . . ? C10 C11 C14 121.3(4) . . ? C12 C11 C14 120.5(4) . . ? 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 . . ? C13 C12 C11 120.5(4) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C8 C13 C12 120.6(3) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? N2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? N1 C2 N3 131.4(3) . . ? N1 C2 O1 114.1(3) . . ? N3 C2 O1 114.5(3) . . ? N3 C18 C19 110.9(3) . . ? N3 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.0 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C16 C17 111.8(4) . . ? N3 C16 H16A 109.3 . . ? C17 C16 H16A 109.3 . . ? N3 C16 H16B 109.3 . . ? C17 C16 H16B 109.3 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.177 _refine_diff_density_min -0.898 _refine_diff_density_rms 0.128 # start Validation Reply Form _vrf_PUBL220_GLOBAL ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min)... 5.90 Ratio RESPONSE: Large Non-Solvent C is due to the disorder. ; #===END========================================================================