# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 729229' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cl2 N2 O6 Pd' _chemical_formula_weight 457.54 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.780(3) _cell_length_b 13.895(3) _cell_length_c 13.596(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.59(3) _cell_angle_gamma 90.00 _cell_volume 3022.0(11) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6834 _cell_measurement_theta_min 1.941 _cell_measurement_theta_max 27.487 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.011 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 1.614 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8056 _exptl_absorpt_correction_T_max 0.8817 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24305 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0674 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.53 _reflns_number_total 6938 _reflns_number_gt 5489 _reflns_threshold_expression >2sigma(I) _computing_data_collection crystalclear _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0343P)^2^+0.3820P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6938 _refine_ls_number_parameters 447 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.050 _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 Pd2 Pd 0.282744(14) 0.70664(2) 0.11585(2) 0.01262(8) Uani 1 1 d . . . Pd1 Pd 0.215821(14) 0.65534(2) 0.86650(2) 0.01284(8) Uani 1 1 d . . . Cl1 Cl 0.15998(5) 0.80713(7) 0.85650(7) 0.01599(19) Uani 1 1 d . . . Cl2 Cl 0.08857(5) 0.59274(7) 0.86250(7) 0.0178(2) Uani 1 1 d . . . Cl3 Cl 0.33761(5) 0.85570(7) 0.10637(7) 0.0174(2) Uani 1 1 d . . . Cl4 Cl 0.40835(5) 0.63783(7) 0.12249(7) 0.0178(2) Uani 1 1 d . . . O1 O 0.53829(14) 0.9350(2) 0.8760(2) 0.0281(7) Uani 1 1 d . . . O2 O 0.40935(15) 0.9788(2) 0.8739(2) 0.0263(7) Uani 1 1 d . . . H2 H 0.4277 1.0332 0.8714 0.039 Uiso 1 1 calc R . . O3 O 0.16018(14) 0.2599(2) 0.8774(2) 0.0263(7) Uani 1 1 d . . . O4 O 0.28201(16) 0.1856(2) 0.8975(3) 0.0253(7) Uani 1 1 d D . . H4A H 0.261(2) 0.1308(15) 0.901(4) 0.030 Uiso 1 1 d D . . O5 O 0.10143(14) 1.0372(2) 0.1372(2) 0.0192(6) Uani 1 1 d . . . H5 H 0.0851 1.0899 0.1503 0.029 Uiso 1 1 calc R . . O6 O -0.03315(14) 0.9978(2) 0.1059(2) 0.0208(6) Uani 1 1 d . . . O7 O 0.34015(15) 0.3153(2) 0.1622(2) 0.0272(7) Uani 1 1 d . . . O8 O 0.21953(15) 0.2407(2) 0.1472(2) 0.0235(7) Uani 1 1 d D . . H8A H 0.248(2) 0.1904(18) 0.145(3) 0.028 Uiso 1 1 d D . . N1 N 0.33186(16) 0.6988(2) 0.8700(2) 0.0122(6) Uani 1 1 d . . . N2 N 0.27114(16) 0.5253(2) 0.8719(2) 0.0143(7) Uani 1 1 d . . . N3 N 0.16766(16) 0.7562(2) 0.1103(2) 0.0136(7) Uani 1 1 d . . . N4 N 0.22643(16) 0.5796(2) 0.1249(2) 0.0130(7) Uani 1 1 d . . . C1 C 0.4686(2) 0.9142(3) 0.8753(3) 0.0182(8) Uani 1 1 d . . . C2 C 0.4398(2) 0.8130(3) 0.8767(3) 0.0170(8) Uani 1 1 d . . . C3 C 0.4954(2) 0.7395(3) 0.8804(3) 0.0189(8) Uani 1 1 d . . . H3 H 0.5507 0.7530 0.8847 0.023 Uiso 1 1 calc R . . C4 C 0.4686(2) 0.6456(3) 0.8777(3) 0.0178(8) Uani 1 1 d . . . H4 H 0.5054 0.5953 0.8788 0.021 Uiso 1 1 calc R . . C5 C 0.3867(2) 0.6263(3) 0.8733(3) 0.0150(8) Uani 1 1 d . . . C6 C 0.3580(2) 0.7899(3) 0.8715(3) 0.0167(8) Uani 1 1 d . . . H6 H 0.3202 0.8395 0.8690 0.020 Uiso 1 1 calc R . . C7 C 0.35363(19) 0.5290(3) 0.8758(3) 0.0133(8) Uani 1 1 d . . . C8 C 0.3999(2) 0.4460(3) 0.8834(3) 0.0198(9) Uani 1 1 d . . . H8 H 0.4557 0.4496 0.8854 0.024 Uiso 1 1 calc R . . C9 C 0.3639(2) 0.3573(3) 0.8879(3) 0.0192(9) Uani 1 1 d . . . H9 H 0.3954 0.3012 0.8946 0.023 Uiso 1 1 calc R . . C10 C 0.2797(2) 0.3534(3) 0.8822(3) 0.0167(8) Uani 1 1 d . . . C11 C 0.2358(2) 0.4395(3) 0.8740(3) 0.0158(8) Uani 1 1 d . . . H11 H 0.1795 0.4372 0.8700 0.019 Uiso 1 1 calc R . . C12 C 0.2346(2) 0.2630(3) 0.8852(3) 0.0185(8) Uani 1 1 d . . . C13 C 0.0384(2) 0.9752(3) 0.1151(3) 0.0169(8) Uani 1 1 d . . . C14 C 0.0636(2) 0.8748(3) 0.1038(3) 0.0149(8) Uani 1 1 d . . . C15 C 0.1452(2) 0.8482(3) 0.1124(3) 0.0148(8) Uani 1 1 d . . . H15 H 0.1855 0.8959 0.1199 0.018 Uiso 1 1 calc R . . C16 C 0.11021(19) 0.6844(3) 0.1042(3) 0.0137(8) Uani 1 1 d . . . C17 C 0.0269(2) 0.7071(3) 0.0889(3) 0.0187(9) Uani 1 1 d . . . H17 H -0.0129 0.6585 0.0791 0.022 Uiso 1 1 calc R . . C18 C 0.0034(2) 0.8024(3) 0.0882(3) 0.0179(8) Uani 1 1 d . . . H18 H -0.0524 0.8184 0.0774 0.021 Uiso 1 1 calc R . . C19 C 0.1436(2) 0.5871(3) 0.1168(3) 0.0155(8) Uani 1 1 d . . . C20 C 0.0979(2) 0.5053(3) 0.1222(3) 0.0186(9) Uani 1 1 d . . . H20 H 0.0418 0.5110 0.1184 0.022 Uiso 1 1 calc R . . C21 C 0.1343(2) 0.4162(3) 0.1332(3) 0.0208(9) Uani 1 1 d . . . H21 H 0.1032 0.3613 0.1356 0.025 Uiso 1 1 calc R . . C22 C 0.2189(2) 0.4089(3) 0.1406(3) 0.0161(8) Uani 1 1 d . . . C23 C 0.2625(2) 0.4935(3) 0.1371(3) 0.0164(8) Uani 1 1 d . . . H23 H 0.3192 0.4896 0.1436 0.020 Uiso 1 1 calc R . . C24 C 0.2658(2) 0.3173(3) 0.1521(3) 0.0174(8) Uani 1 1 d . . . O9 O 0.04368(15) 0.2030(2) 0.1776(2) 0.0241(7) Uani 1 1 d D . . H9A H -0.0095(6) 0.202(3) 0.163(3) 0.036 Uiso 1 1 d D . . H9B H 0.0705(18) 0.215(3) 0.2406(13) 0.036 Uiso 1 1 d D . . O10 O 0.20414(15) 1.0277(2) 0.9344(2) 0.0237(7) Uani 1 1 d D . . H10A H 0.219(2) 0.9701(12) 0.927(4) 0.035 Uiso 1 1 d D . . H10B H 0.1519(8) 1.036(2) 0.922(3) 0.035 Uiso 1 1 d D . . O11 O 0.46338(16) 0.1522(2) 0.8579(2) 0.0247(7) Uani 1 1 d D . . H11A H 0.5164(6) 0.152(3) 0.872(3) 0.037 Uiso 1 1 d D . . H11B H 0.4359(18) 0.161(4) 0.7945(12) 0.037 Uiso 1 1 d D . . O12 O 0.29690(16) 0.0862(2) 0.1392(2) 0.0258(7) Uani 1 1 d D . . H12A H 0.3491(7) 0.092(3) 0.150(3) 0.039 Uiso 1 1 d D . . H12B H 0.2699(18) 0.060(3) 0.082(2) 0.039 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd2 0.01002(13) 0.01312(17) 0.01563(15) 0.00006(12) 0.00524(10) 0.00012(10) Pd1 0.00968(13) 0.01404(18) 0.01536(15) 0.00029(12) 0.00463(10) 0.00087(10) Cl1 0.0137(4) 0.0146(5) 0.0194(5) -0.0013(4) 0.0046(3) 0.0019(3) Cl2 0.0118(4) 0.0194(6) 0.0236(5) -0.0007(4) 0.0076(3) -0.0013(3) Cl3 0.0133(4) 0.0154(5) 0.0241(5) -0.0010(4) 0.0067(3) -0.0021(3) Cl4 0.0128(4) 0.0202(6) 0.0221(5) 0.0004(4) 0.0078(3) 0.0028(3) O1 0.0167(13) 0.0227(19) 0.045(2) -0.0016(15) 0.0098(12) -0.0059(12) O2 0.0246(14) 0.0170(18) 0.0391(19) -0.0056(15) 0.0126(13) -0.0042(12) O3 0.0156(13) 0.0239(19) 0.0406(19) 0.0049(15) 0.0102(12) 0.0001(12) O4 0.0216(14) 0.0123(17) 0.0426(19) 0.0027(14) 0.0105(13) 0.0015(11) O5 0.0171(12) 0.0141(17) 0.0273(16) -0.0025(13) 0.0080(11) 0.0007(10) O6 0.0121(12) 0.0232(18) 0.0263(16) -0.0009(13) 0.0043(10) 0.0059(11) O7 0.0182(13) 0.0192(18) 0.046(2) -0.0001(15) 0.0128(13) 0.0017(11) O8 0.0198(14) 0.0124(17) 0.0389(18) 0.0017(14) 0.0095(12) 0.0030(11) N1 0.0123(13) 0.0164(19) 0.0077(15) -0.0014(13) 0.0025(11) 0.0025(12) N2 0.0138(14) 0.019(2) 0.0113(15) -0.0009(13) 0.0049(11) 0.0026(12) N3 0.0130(13) 0.0181(19) 0.0111(15) -0.0012(13) 0.0058(11) -0.0023(12) N4 0.0111(13) 0.0160(19) 0.0126(15) 0.0009(13) 0.0046(11) -0.0007(12) C1 0.0164(17) 0.017(2) 0.020(2) -0.0030(17) 0.0035(14) -0.0008(15) C2 0.0173(17) 0.018(2) 0.016(2) -0.0006(16) 0.0046(14) -0.0031(15) C3 0.0129(17) 0.021(2) 0.024(2) 0.0002(18) 0.0067(14) -0.0011(15) C4 0.0142(17) 0.020(2) 0.021(2) -0.0004(17) 0.0071(14) 0.0032(15) C5 0.0138(16) 0.016(2) 0.0159(19) 0.0008(16) 0.0060(14) 0.0018(14) C6 0.0146(17) 0.022(2) 0.0134(19) 0.0030(16) 0.0050(13) 0.0041(15) C7 0.0097(15) 0.016(2) 0.0138(18) -0.0005(15) 0.0032(13) 0.0000(13) C8 0.0152(17) 0.019(2) 0.026(2) -0.0004(18) 0.0073(15) 0.0013(15) C9 0.0189(18) 0.018(2) 0.021(2) 0.0007(17) 0.0063(15) 0.0032(15) C10 0.0158(17) 0.019(2) 0.0161(19) -0.0023(16) 0.0054(14) -0.0020(15) C11 0.0142(16) 0.017(2) 0.0161(19) 0.0012(16) 0.0041(13) 0.0017(14) C12 0.0196(18) 0.019(2) 0.018(2) 0.0002(17) 0.0065(15) 0.0003(16) C13 0.0176(17) 0.017(2) 0.0152(19) 0.0012(16) 0.0043(14) -0.0005(15) C14 0.0168(17) 0.015(2) 0.0134(18) 0.0014(15) 0.0051(14) 0.0026(14) C15 0.0154(17) 0.017(2) 0.0121(18) 0.0003(16) 0.0050(13) 0.0006(14) C16 0.0127(16) 0.016(2) 0.0129(18) -0.0014(15) 0.0051(13) 0.0015(14) C17 0.0132(16) 0.021(2) 0.021(2) -0.0006(17) 0.0046(14) -0.0025(15) C18 0.0131(17) 0.017(2) 0.024(2) 0.0019(17) 0.0073(14) 0.0016(14) C19 0.0153(17) 0.017(2) 0.0135(18) -0.0011(16) 0.0031(13) 0.0013(14) C20 0.0128(17) 0.021(3) 0.023(2) -0.0018(18) 0.0064(14) -0.0001(15) C21 0.0181(18) 0.018(2) 0.027(2) -0.0010(18) 0.0079(16) -0.0046(15) C22 0.0190(17) 0.011(2) 0.018(2) 0.0040(16) 0.0059(14) 0.0027(14) C23 0.0156(17) 0.017(2) 0.0170(19) 0.0020(16) 0.0053(14) -0.0003(15) C24 0.0236(19) 0.011(2) 0.019(2) -0.0001(16) 0.0080(15) -0.0006(15) O9 0.0139(13) 0.0198(18) 0.0378(19) -0.0018(14) 0.0064(12) 0.0017(11) O10 0.0184(13) 0.0160(17) 0.0374(18) -0.0012(14) 0.0097(12) 0.0007(11) O11 0.0178(13) 0.0218(18) 0.0360(18) -0.0028(15) 0.0105(12) -0.0031(12) O12 0.0205(14) 0.0234(19) 0.0329(18) -0.0038(14) 0.0071(12) -0.0006(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 Pd2 N4 2.023(3) . ? Pd2 N3 2.030(3) . ? Pd2 Cl3 2.2859(10) . ? Pd2 Cl4 2.2911(9) . ? Pd1 N2 2.022(3) . ? Pd1 N1 2.025(3) . ? Pd1 Cl2 2.2910(9) . ? Pd1 Cl1 2.2953(10) . ? O1 C1 1.202(4) . ? O2 C1 1.336(4) . ? O2 H2 0.8200 . ? O3 C12 1.221(4) . ? O4 C12 1.319(5) . ? O4 H4A 0.847(10) . ? O5 C13 1.326(4) . ? O5 H5 0.8200 . ? O6 C13 1.210(4) . ? O7 C24 1.214(4) . ? O8 C24 1.307(5) . ? O8 H8A 0.852(10) . ? N1 C6 1.339(5) . ? N1 C5 1.355(5) . ? N2 C11 1.337(5) . ? N2 C7 1.370(4) . ? N3 C15 1.335(5) . ? N3 C16 1.372(5) . ? N4 C23 1.329(5) . ? N4 C19 1.365(4) . ? C1 C2 1.489(5) . ? C2 C3 1.375(5) . ? C2 C6 1.390(5) . ? C3 C4 1.377(6) . ? C3 H3 0.9300 . ? C4 C5 1.384(4) . ? C4 H4 0.9300 . ? C5 C7 1.466(5) . ? C6 H6 0.9300 . ? C7 C8 1.377(5) . ? C8 C9 1.382(5) . ? C8 H8 0.9300 . ? C9 C10 1.392(4) . ? C9 H9 0.9300 . ? C10 C11 1.393(5) . ? C10 C12 1.473(5) . ? C11 H11 0.9300 . ? C13 C14 1.480(5) . ? C14 C15 1.389(4) . ? C14 C18 1.396(5) . ? C15 H15 0.9300 . ? C16 C17 1.387(4) . ? C16 C19 1.454(5) . ? C17 C18 1.381(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.385(5) . ? C20 C21 1.369(5) . ? C20 H20 0.9300 . ? C21 C22 1.396(5) . ? C21 H21 0.9300 . ? C22 C23 1.394(5) . ? C22 C24 1.479(5) . ? C23 H23 0.9300 . ? O9 H9A 0.854(10) . ? O9 H9B 0.854(10) . ? O10 H10A 0.855(10) . ? O10 H10B 0.849(10) . ? O11 H11A 0.852(10) . ? O11 H11B 0.853(10) . ? O12 H12A 0.847(10) . ? O12 H12B 0.856(10) . ? 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 Pd2 N3 80.88(12) . . ? N4 Pd2 Cl3 175.76(8) . . ? N3 Pd2 Cl3 94.89(9) . . ? N4 Pd2 Cl4 94.28(8) . . ? N3 Pd2 Cl4 175.16(10) . . ? Cl3 Pd2 Cl4 89.94(3) . . ? N2 Pd1 N1 80.67(12) . . ? N2 Pd1 Cl2 94.36(8) . . ? N1 Pd1 Cl2 175.02(9) . . ? N2 Pd1 Cl1 176.17(8) . . ? N1 Pd1 Cl1 95.74(9) . . ? Cl2 Pd1 Cl1 89.23(3) . . ? C1 O2 H2 109.5 . . ? C12 O4 H4A 120(3) . . ? C13 O5 H5 109.5 . . ? C24 O8 H8A 110(3) . . ? C6 N1 C5 119.1(3) . . ? C6 N1 Pd1 126.2(2) . . ? C5 N1 Pd1 114.7(3) . . ? C11 N2 C7 118.8(3) . . ? C11 N2 Pd1 126.6(2) . . ? C7 N2 Pd1 114.6(3) . . ? C15 N3 C16 120.0(3) . . ? C15 N3 Pd2 126.5(2) . . ? C16 N3 Pd2 113.5(2) . . ? C23 N4 C19 119.5(3) . . ? C23 N4 Pd2 126.1(2) . . ? C19 N4 Pd2 114.3(3) . . ? O1 C1 O2 123.8(4) . . ? O1 C1 C2 123.1(3) . . ? O2 C1 C2 113.1(3) . . ? C3 C2 C6 118.7(4) . . ? C3 C2 C1 118.8(3) . . ? C6 C2 C1 122.5(3) . . ? C2 C3 C4 119.3(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.8(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 120.9(4) . . ? N1 C5 C7 115.3(3) . . ? C4 C5 C7 123.7(3) . . ? N1 C6 C2 122.2(3) . . ? N1 C6 H6 118.9 . . ? C2 C6 H6 118.9 . . ? N2 C7 C8 120.8(3) . . ? N2 C7 C5 114.7(3) . . ? C8 C7 C5 124.4(3) . . ? C7 C8 C9 120.4(3) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C10 118.8(4) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C9 C10 C11 118.4(4) . . ? C9 C10 C12 123.6(4) . . ? C11 C10 C12 118.0(3) . . ? N2 C11 C10 122.7(3) . . ? N2 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? O3 C12 O4 123.0(4) . . ? O3 C12 C10 123.3(4) . . ? O4 C12 C10 113.8(3) . . ? O6 C13 O5 123.6(4) . . ? O6 C13 C14 122.7(3) . . ? O5 C13 C14 113.7(3) . . ? C15 C14 C18 118.1(4) . . ? C15 C14 C13 123.3(3) . . ? C18 C14 C13 118.6(3) . . ? N3 C15 C14 122.0(3) . . ? N3 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? N3 C16 C17 120.2(4) . . ? N3 C16 C19 115.5(3) . . ? C17 C16 C19 124.3(3) . . ? C18 C17 C16 119.4(3) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C14 119.9(3) . . ? C17 C18 H18 120.1 . . ? C14 C18 H18 120.1 . . ? N4 C19 C20 120.0(3) . . ? N4 C19 C16 115.2(3) . . ? C20 C19 C16 124.7(3) . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 119.0(4) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C23 C22 C21 118.0(4) . . ? C23 C22 C24 117.5(3) . . ? C21 C22 C24 124.5(3) . . ? N4 C23 C22 122.7(3) . . ? N4 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? O7 C24 O8 124.2(4) . . ? O7 C24 C22 121.8(3) . . ? O8 C24 C22 114.0(3) . . ? H9A O9 H9B 115.4(18) . . ? H10A O10 H10B 115.6(18) . . ? H11A O11 H11B 115.5(18) . . ? H12A O12 H12B 115.8(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pd1 N1 C6 -178.1(3) . . . . ? Cl2 Pd1 N1 C6 180(32) . . . . ? Cl1 Pd1 N1 C6 3.3(3) . . . . ? N2 Pd1 N1 C5 0.4(3) . . . . ? Cl2 Pd1 N1 C5 -1.8(12) . . . . ? Cl1 Pd1 N1 C5 -178.3(2) . . . . ? N1 Pd1 N2 C11 179.0(3) . . . . ? Cl2 Pd1 N2 C11 -1.2(3) . . . . ? Cl1 Pd1 N2 C11 -160.8(11) . . . . ? N1 Pd1 N2 C7 0.5(3) . . . . ? Cl2 Pd1 N2 C7 -179.7(2) . . . . ? Cl1 Pd1 N2 C7 20.7(15) . . . . ? N4 Pd2 N3 C15 173.3(3) . . . . ? Cl3 Pd2 N3 C15 -6.3(3) . . . . ? Cl4 Pd2 N3 C15 175.7(8) . . . . ? N4 Pd2 N3 C16 -6.4(2) . . . . ? Cl3 Pd2 N3 C16 174.0(2) . . . . ? Cl4 Pd2 N3 C16 -4.0(12) . . . . ? N3 Pd2 N4 C23 -176.6(3) . . . . ? Cl3 Pd2 N4 C23 -170.6(10) . . . . ? Cl4 Pd2 N4 C23 3.6(3) . . . . ? N3 Pd2 N4 C19 3.8(3) . . . . ? Cl3 Pd2 N4 C19 9.8(14) . . . . ? Cl4 Pd2 N4 C19 -176.0(2) . . . . ? O1 C1 C2 C3 0.9(6) . . . . ? O2 C1 C2 C3 -178.6(4) . . . . ? O1 C1 C2 C6 -177.2(4) . . . . ? O2 C1 C2 C6 3.2(6) . . . . ? C6 C2 C3 C4 0.7(6) . . . . ? C1 C2 C3 C4 -177.5(4) . . . . ? C2 C3 C4 C5 -1.2(6) . . . . ? C6 N1 C5 C4 -0.4(5) . . . . ? Pd1 N1 C5 C4 -178.9(3) . . . . ? C6 N1 C5 C7 177.5(3) . . . . ? Pd1 N1 C5 C7 -1.1(4) . . . . ? C3 C4 C5 N1 1.1(6) . . . . ? C3 C4 C5 C7 -176.6(4) . . . . ? C5 N1 C6 C2 -0.2(5) . . . . ? Pd1 N1 C6 C2 178.2(3) . . . . ? C3 C2 C6 N1 0.0(6) . . . . ? C1 C2 C6 N1 178.1(3) . . . . ? C11 N2 C7 C8 -1.0(5) . . . . ? Pd1 N2 C7 C8 177.7(3) . . . . ? C11 N2 C7 C5 -179.8(3) . . . . ? Pd1 N2 C7 C5 -1.1(4) . . . . ? N1 C5 C7 N2 1.5(5) . . . . ? C4 C5 C7 N2 179.2(3) . . . . ? N1 C5 C7 C8 -177.4(4) . . . . ? C4 C5 C7 C8 0.4(6) . . . . ? N2 C7 C8 C9 -0.5(6) . . . . ? C5 C7 C8 C9 178.3(4) . . . . ? C7 C8 C9 C10 1.5(6) . . . . ? C8 C9 C10 C11 -1.2(6) . . . . ? C8 C9 C10 C12 179.4(4) . . . . ? C7 N2 C11 C10 1.3(5) . . . . ? Pd1 N2 C11 C10 -177.2(3) . . . . ? C9 C10 C11 N2 -0.2(6) . . . . ? C12 C10 C11 N2 179.2(3) . . . . ? C9 C10 C12 O3 -177.9(4) . . . . ? C11 C10 C12 O3 2.7(6) . . . . ? C9 C10 C12 O4 2.2(6) . . . . ? C11 C10 C12 O4 -177.2(3) . . . . ? O6 C13 C14 C15 178.8(4) . . . . ? O5 C13 C14 C15 -1.9(5) . . . . ? O6 C13 C14 C18 -4.0(6) . . . . ? O5 C13 C14 C18 175.3(3) . . . . ? C16 N3 C15 C14 -3.1(5) . . . . ? Pd2 N3 C15 C14 177.3(3) . . . . ? C18 C14 C15 N3 -2.7(6) . . . . ? C13 C14 C15 N3 174.5(3) . . . . ? C15 N3 C16 C17 7.1(5) . . . . ? Pd2 N3 C16 C17 -173.2(3) . . . . ? C15 N3 C16 C19 -171.7(3) . . . . ? Pd2 N3 C16 C19 8.0(4) . . . . ? N3 C16 C17 C18 -5.2(6) . . . . ? C19 C16 C17 C18 173.5(4) . . . . ? C16 C17 C18 C14 -0.6(6) . . . . ? C15 C14 C18 C17 4.5(6) . . . . ? C13 C14 C18 C17 -172.9(3) . . . . ? C23 N4 C19 C20 0.6(5) . . . . ? Pd2 N4 C19 C20 -179.8(3) . . . . ? C23 N4 C19 C16 179.7(3) . . . . ? Pd2 N4 C19 C16 -0.6(4) . . . . ? N3 C16 C19 N4 -4.9(5) . . . . ? C17 C16 C19 N4 176.3(3) . . . . ? N3 C16 C19 C20 174.2(3) . . . . ? C17 C16 C19 C20 -4.6(6) . . . . ? N4 C19 C20 C21 -1.6(6) . . . . ? C16 C19 C20 C21 179.3(4) . . . . ? C19 C20 C21 C22 1.1(6) . . . . ? C20 C21 C22 C23 0.4(6) . . . . ? C20 C21 C22 C24 -179.7(4) . . . . ? C19 N4 C23 C22 1.0(6) . . . . ? Pd2 N4 C23 C22 -178.7(3) . . . . ? C21 C22 C23 N4 -1.5(6) . . . . ? C24 C22 C23 N4 178.6(3) . . . . ? C23 C22 C24 O7 2.8(6) . . . . ? C21 C22 C24 O7 -177.1(4) . . . . ? C23 C22 C24 O8 -175.3(3) . . . . ? C21 C22 C24 O8 4.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.858 _refine_diff_density_min -1.353 _refine_diff_density_rms 0.142 data_2 _database_code_depnum_ccdc_archive 'CCDC 729232' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cl2 N2 O6 Pt' _chemical_formula_weight 546.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.640(2) _cell_length_b 13.7906(18) _cell_length_c 13.6697(19) _cell_angle_alpha 90.00 _cell_angle_beta 106.052(3) _cell_angle_gamma 90.00 _cell_volume 3014.6(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 9.696 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6977 _exptl_absorpt_correction_T_max 0.9093 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18633 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5314 _reflns_number_gt 4172 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+16.4685P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5314 _refine_ls_number_parameters 418 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.014 _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 C2 C 0.3559(6) 0.6580(7) 0.3883(7) 0.028(2) Uani 1 1 d . . . H2 H 0.3164 0.6091 0.3836 0.034 Uiso 1 1 calc R . . C7 C 0.3543(6) 0.9163(7) 0.3834(7) 0.023(2) Uani 1 1 d . . . C8 C 0.3992(7) 0.9997(8) 0.3795(7) 0.034(3) Uani 1 1 d U . . H8 H 0.4554 0.9951 0.3818 0.040 Uiso 1 1 calc R . . C3 C 0.4346(6) 0.6324(8) 0.3944(7) 0.026(2) Uani 1 1 d . . . C12 C 0.2375(6) 1.0087(7) 0.3656(7) 0.026(2) Uani 1 1 d . . . H12 H 0.1805 1.0123 0.3596 0.032 Uiso 1 1 calc R . . C5 C 0.4701(7) 0.7977(9) 0.4069(8) 0.037(3) Uani 1 1 d . . . H5 H 0.5091 0.8474 0.4142 0.045 Uiso 1 1 calc R . . C10 C 0.2776(7) 1.0920(8) 0.3629(8) 0.034(3) Uani 1 1 d . . . C11 C 0.2312(8) 1.1852(8) 0.3554(9) 0.038(3) Uani 1 1 d . . . C9 C 0.3623(7) 1.0889(9) 0.3723(8) 0.043(3) Uani 1 1 d . . . H9 H 0.3931 1.1454 0.3738 0.051 Uiso 1 1 calc R . . C18 C 0.1477(6) 0.9669(9) 0.6218(7) 0.033(3) Uani 1 1 d . . . C17 C 0.1011(7) 1.0487(9) 0.6136(8) 0.041(3) Uani 1 1 d . . . H17 H 0.0445 1.0455 0.6097 0.050 Uiso 1 1 calc R . . C16 C 0.1396(7) 1.1360(8) 0.6113(8) 0.036(3) Uani 1 1 d . . . H16 H 0.1087 1.1931 0.6046 0.043 Uiso 1 1 calc R . . C15 C 0.2214(6) 1.1395(8) 0.6187(8) 0.031(3) Uani 1 1 d . . . C14 C 0.2650(6) 1.0556(9) 0.6264(8) 0.037(3) Uani 1 1 d . . . H14 H 0.3219 1.0585 0.6319 0.045 Uiso 1 1 calc R . . C13 C 0.2669(7) 1.2313(9) 0.6172(8) 0.037(3) Uani 1 1 d . . . C19 C 0.1137(6) 0.8693(8) 0.6238(7) 0.026(2) Uani 1 1 d . . . C6 C 0.3868(6) 0.8192(8) 0.3950(8) 0.031(3) Uani 1 1 d . . . C24 C 0.1448(7) 0.7082(8) 0.6267(7) 0.032(3) Uani 1 1 d . . . H24 H 0.1836 0.6590 0.6299 0.039 Uiso 1 1 calc R . . C23 C 0.0394(7) 0.5793(10) 0.6228(9) 0.045(3) Uani 1 1 d . . . C1 C 0.4590(7) 0.5303(8) 0.3849(7) 0.034(3) Uani 1 1 d . . . C22 C 0.0640(7) 0.6826(8) 0.6210(8) 0.032(3) Uani 1 1 d . . . C4 C 0.4949(7) 0.7037(9) 0.4079(8) 0.041(3) Uani 1 1 d . . . H4 H 0.5509 0.6879 0.4175 0.049 Uiso 1 1 calc R . . C21 C 0.0084(7) 0.7557(9) 0.6157(8) 0.039(3) Uani 1 1 d . . . H21 H -0.0472 0.7409 0.6102 0.047 Uiso 1 1 calc R . . C20 C 0.0322(6) 0.8495(9) 0.6182(8) 0.039(3) Uani 1 1 d . . . H20 H -0.0059 0.8993 0.6161 0.047 Uiso 1 1 calc R . . Cl1 Cl 0.16200(16) 0.6471(2) 0.3903(2) 0.0375(7) Uani 1 1 d . . . Cl2 Cl 0.08967(15) 0.8624(2) 0.3750(2) 0.0369(7) Uani 1 1 d . . . Cl3 Cl 0.41332(15) 0.9031(2) 0.6376(2) 0.0359(7) Uani 1 1 d . . . Cl4 Cl 0.34137(16) 0.68949(19) 0.6419(2) 0.0340(6) Uani 1 1 d . . . H13A H 0.566(5) 0.855(4) 0.167(7) 0.041 Uiso 1 1 d D . . H13B H 0.569(5) 0.772(6) 0.226(5) 0.051 Uiso 1 1 d D . . N1 N 0.2715(5) 0.9221(6) 0.3760(6) 0.0243(19) Uani 1 1 d . . . N2 N 0.3311(5) 0.7492(6) 0.3885(6) 0.0252(19) Uani 1 1 d . . . N3 N 0.2293(5) 0.9696(6) 0.6263(6) 0.025(2) Uani 1 1 d . . . N4 N 0.1701(5) 0.7976(6) 0.6279(6) 0.0255(19) Uani 1 1 d . . . O1 O 0.5312(5) 0.5102(6) 0.3942(6) 0.047(2) Uani 1 1 d . . . H1 H 0.5349 0.4527 0.3807 0.071 Uiso 1 1 calc R . . O2 O 0.3989(5) 0.4691(5) 0.3643(6) 0.043(2) Uani 1 1 d . . . O3 O 0.2769(5) 1.2610(6) 0.3604(7) 0.057(2) Uani 1 1 d . . . H3A H 0.2487 1.3096 0.3612 0.086 Uiso 1 1 calc R . . O4 O 0.1576(5) 1.1864(6) 0.3417(7) 0.060(3) Uani 1 1 d . . . O7 O 0.3408(5) 1.2332(6) 0.6274(7) 0.059(3) Uani 1 1 d . . . O8 O 0.2193(5) 1.3070(6) 0.6031(7) 0.056(2) Uani 1 1 d . . . H8B H 0.2462 1.3547 0.5946 0.084 Uiso 1 1 calc R . . O9 O 0.0953(5) 0.5175(6) 0.6279(6) 0.049(2) Uani 1 1 d . . . O10 O -0.0336(5) 0.5615(6) 0.6191(7) 0.065(3) Uani 1 1 d . . . H10A H -0.0394 0.5028 0.6243 0.097 Uiso 1 1 calc R . . O13 O 0.5425(5) 0.8015(6) 0.1723(7) 0.053(2) Uani 1 1 d D . . O15 O 0.2976(5) 0.4662(5) 0.5744(5) 0.070(3) Uani 1 1 d G . . H15A H 0.3465 0.4697 0.5667 0.104 Uiso 1 1 d G . . H15B H 0.2769 0.5228 0.5719 0.104 Uiso 1 1 d G . . O16 O 0.0391(4) 0.1559(5) 0.1452(5) 0.055(2) Uani 1 1 d G . . H16A H -0.0119 0.1652 0.1134 0.083 Uiso 1 1 d G . . H16B H 0.0460 0.1649 0.2085 0.083 Uiso 1 1 d G . . O14 O 0.1957(4) 0.4158(4) 0.3631(4) 0.058(2) Uani 1 1 d G . . H14A H 0.1506 0.4236 0.3797 0.087 Uiso 1 1 d G . . H14B H 0.2366 0.4376 0.4100 0.087 Uiso 1 1 d G . . Pt1 Pt 0.21668(2) 0.79679(3) 0.38275(3) 0.02898(13) Uani 1 1 d . . . Pt2 Pt 0.28521(2) 0.84065(3) 0.63260(3) 0.02881(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2 0.035(6) 0.010(6) 0.038(6) 0.006(5) 0.008(5) -0.007(5) C7 0.022(6) 0.026(7) 0.021(5) 0.000(4) 0.005(4) 0.003(4) C8 0.033(3) 0.033(3) 0.034(3) 0.0003(10) 0.0096(12) 0.0002(10) C3 0.026(6) 0.031(7) 0.023(5) 0.001(5) 0.007(4) 0.007(5) C12 0.023(6) 0.013(6) 0.045(6) 0.002(5) 0.014(5) -0.008(4) C5 0.029(6) 0.041(8) 0.045(7) 0.000(6) 0.014(5) -0.006(5) C10 0.038(7) 0.022(7) 0.043(7) 0.009(5) 0.013(5) 0.009(5) C11 0.043(8) 0.025(8) 0.048(7) -0.006(5) 0.014(6) 0.006(5) C9 0.034(7) 0.043(9) 0.054(7) 0.005(6) 0.017(5) -0.013(6) C18 0.025(6) 0.047(8) 0.028(6) 0.002(5) 0.009(4) 0.005(5) C17 0.019(6) 0.048(9) 0.060(8) 0.000(6) 0.016(5) 0.002(5) C16 0.034(7) 0.026(7) 0.049(7) 0.004(5) 0.013(5) 0.009(5) C15 0.021(6) 0.037(8) 0.034(6) 0.000(5) 0.006(4) 0.004(5) C14 0.019(6) 0.054(9) 0.037(6) 0.003(6) 0.005(5) -0.007(5) C13 0.039(8) 0.033(8) 0.042(7) 0.002(5) 0.013(5) -0.005(5) C19 0.021(6) 0.039(8) 0.019(5) -0.002(5) 0.007(4) 0.005(5) C6 0.027(6) 0.033(8) 0.035(6) -0.007(5) 0.013(5) -0.005(5) C24 0.035(7) 0.029(8) 0.032(6) -0.003(5) 0.009(5) 0.005(5) C23 0.030(7) 0.056(10) 0.048(7) -0.009(6) 0.009(5) -0.009(6) C1 0.045(8) 0.032(8) 0.022(6) 0.006(5) 0.005(5) 0.017(6) C22 0.039(7) 0.019(7) 0.035(6) -0.006(5) 0.005(5) -0.003(5) C4 0.021(6) 0.052(9) 0.052(7) 0.005(6) 0.012(5) 0.008(6) C21 0.027(6) 0.042(9) 0.051(7) -0.001(6) 0.013(5) -0.011(6) C20 0.023(6) 0.041(9) 0.058(8) 0.001(6) 0.017(5) -0.001(5) Cl1 0.0309(15) 0.0258(17) 0.0580(18) 0.0001(13) 0.0158(12) -0.0063(11) Cl2 0.0233(14) 0.0388(19) 0.0518(17) 0.0017(13) 0.0157(12) 0.0034(11) Cl3 0.0204(14) 0.0381(19) 0.0527(17) -0.0021(13) 0.0157(12) -0.0002(11) Cl4 0.0283(15) 0.0288(17) 0.0447(16) 0.0003(12) 0.0097(11) 0.0063(11) N1 0.030(5) 0.012(5) 0.031(5) 0.001(4) 0.007(4) -0.001(4) N2 0.019(4) 0.030(6) 0.030(5) 0.004(4) 0.011(3) -0.004(4) N3 0.017(4) 0.030(6) 0.028(5) 0.001(4) 0.009(3) 0.004(4) N4 0.026(5) 0.020(6) 0.033(5) -0.003(4) 0.013(4) 0.002(4) O1 0.039(5) 0.031(5) 0.070(6) 0.000(4) 0.012(4) 0.017(4) O2 0.035(5) 0.024(5) 0.070(6) -0.005(4) 0.016(4) -0.002(4) O3 0.057(6) 0.021(5) 0.097(7) 0.004(5) 0.026(5) -0.002(4) O4 0.045(6) 0.028(6) 0.113(8) -0.007(5) 0.033(5) -0.002(4) O7 0.028(5) 0.037(6) 0.109(7) 0.014(5) 0.016(5) -0.004(4) O8 0.040(5) 0.028(5) 0.104(7) 0.015(5) 0.028(5) 0.008(4) O9 0.037(5) 0.037(6) 0.077(6) -0.002(4) 0.024(4) 0.002(4) O10 0.039(6) 0.037(6) 0.115(8) 0.000(5) 0.015(5) -0.017(4) O13 0.039(5) 0.033(6) 0.088(7) 0.017(5) 0.019(4) 0.000(4) O15 0.040(5) 0.034(6) 0.133(8) -0.006(5) 0.021(5) -0.004(4) O16 0.035(5) 0.042(6) 0.090(7) 0.000(5) 0.021(4) 0.005(4) O14 0.045(6) 0.034(6) 0.094(7) -0.009(5) 0.019(5) 0.002(4) Pt1 0.0243(2) 0.0307(3) 0.0340(2) -0.0009(2) 0.01151(17) -0.00072(19) Pt2 0.0235(2) 0.0321(3) 0.0318(2) 0.0001(2) 0.00914(16) 0.00296(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 C2 N2 1.324(12) . ? C2 C3 1.337(14) . ? C2 H2 0.9300 . ? C7 N1 1.356(12) . ? C7 C8 1.380(14) . ? C7 C6 1.437(14) . ? C8 C9 1.366(15) . ? C8 H8 0.9300 . ? C3 C4 1.380(15) . ? C3 C1 1.481(14) . ? C12 N1 1.313(12) . ? C12 C10 1.334(13) . ? C12 H12 0.9300 . ? C5 C4 1.359(15) . ? C5 C6 1.382(14) . ? C5 H5 0.9300 . ? C10 C9 1.380(14) . ? C10 C11 1.488(14) . ? C11 O4 1.188(13) . ? C11 O3 1.284(13) . ? C9 H9 0.9300 . ? C18 N3 1.343(12) . ? C18 C17 1.355(15) . ? C18 C19 1.463(15) . ? C17 C16 1.368(15) . ? C17 H17 0.9300 . ? C16 C15 1.338(14) . ? C16 H16 0.9300 . ? C15 C14 1.354(15) . ? C15 C13 1.479(15) . ? C14 N3 1.326(13) . ? C14 H14 0.9300 . ? C13 O7 1.198(13) . ? C13 O8 1.292(13) . ? C19 N4 1.354(12) . ? C19 C20 1.363(13) . ? C6 N2 1.324(12) . ? C24 N4 1.301(12) . ? C24 C22 1.371(15) . ? C24 H24 0.9300 . ? C23 O10 1.227(13) . ? C23 O9 1.249(14) . ? C23 C22 1.484(16) . ? C1 O1 1.205(12) . ? C1 O2 1.279(13) . ? C22 C21 1.356(15) . ? C4 H4 0.9300 . ? C21 C20 1.352(15) . ? C21 H21 0.9300 . ? C20 H20 0.9300 . ? Cl1 Pt1 2.270(3) . ? Cl2 Pt1 2.274(3) . ? Cl3 Pt2 2.282(3) . ? Cl4 Pt2 2.274(3) . ? N1 Pt1 1.968(8) . ? N2 Pt1 1.995(8) . ? N3 Pt2 1.998(8) . ? N4 Pt2 1.990(8) . ? O1 H1 0.8200 . ? O3 H3A 0.8200 . ? O8 H8B 0.8200 . ? O10 H10A 0.8200 . ? O13 H13A 0.846(10) . ? O13 H13B 0.846(10) . ? O15 H15A 0.8502 . ? O15 H15B 0.8498 . ? O16 H16A 0.8499 . ? O16 H16B 0.8499 . ? O14 H14A 0.8499 . ? O14 H14B 0.8501 . ? 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 C2 C3 123.4(10) . . ? N2 C2 H2 118.3 . . ? C3 C2 H2 118.3 . . ? N1 C7 C8 119.9(9) . . ? N1 C7 C6 114.0(9) . . ? C8 C7 C6 126.2(10) . . ? C9 C8 C7 121.1(11) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C2 C3 C4 119.0(10) . . ? C2 C3 C1 122.2(10) . . ? C4 C3 C1 118.8(10) . . ? N1 C12 C10 125.6(10) . . ? N1 C12 H12 117.2 . . ? C10 C12 H12 117.2 . . ? C4 C5 C6 119.8(11) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C12 C10 C9 118.5(10) . . ? C12 C10 C11 119.4(10) . . ? C9 C10 C11 122.0(11) . . ? O4 C11 O3 124.6(11) . . ? O4 C11 C10 121.0(11) . . ? O3 C11 C10 114.3(11) . . ? C8 C9 C10 117.5(11) . . ? C8 C9 H9 121.3 . . ? C10 C9 H9 121.3 . . ? N3 C18 C17 121.8(11) . . ? N3 C18 C19 114.6(9) . . ? C17 C18 C19 123.5(10) . . ? C18 C17 C16 118.4(11) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C15 C16 C17 120.1(11) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C15 C14 119.2(11) . . ? C16 C15 C13 123.0(10) . . ? C14 C15 C13 117.8(10) . . ? N3 C14 C15 122.2(10) . . ? N3 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? O7 C13 O8 124.5(11) . . ? O7 C13 C15 122.0(11) . . ? O8 C13 C15 113.5(10) . . ? N4 C19 C20 121.6(10) . . ? N4 C19 C18 113.9(9) . . ? C20 C19 C18 124.5(10) . . ? N2 C6 C5 120.8(10) . . ? N2 C6 C7 115.9(9) . . ? C5 C6 C7 123.2(10) . . ? N4 C24 C22 123.6(10) . . ? N4 C24 H24 118.2 . . ? C22 C24 H24 118.2 . . ? O10 C23 O9 125.4(13) . . ? O10 C23 C22 117.8(12) . . ? O9 C23 C22 116.8(11) . . ? O1 C1 O2 124.6(11) . . ? O1 C1 C3 119.9(11) . . ? O2 C1 C3 115.5(10) . . ? C21 C22 C24 117.1(11) . . ? C21 C22 C23 121.8(11) . . ? C24 C22 C23 121.1(10) . . ? C5 C4 C3 118.0(10) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C20 C21 C22 121.2(11) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C21 C20 C19 118.2(11) . . ? C21 C20 H20 120.9 . . ? C19 C20 H20 120.9 . . ? C12 N1 C7 117.4(8) . . ? C12 N1 Pt1 127.8(7) . . ? C7 N1 Pt1 114.8(6) . . ? C6 N2 C2 118.7(9) . . ? C6 N2 Pt1 113.9(7) . . ? C2 N2 Pt1 127.3(7) . . ? C14 N3 C18 118.2(9) . . ? C14 N3 Pt2 126.4(7) . . ? C18 N3 Pt2 115.4(7) . . ? C24 N4 C19 118.2(9) . . ? C24 N4 Pt2 126.1(7) . . ? C19 N4 Pt2 115.7(7) . . ? C1 O1 H1 109.5 . . ? C11 O3 H3A 109.5 . . ? C13 O8 H8B 109.5 . . ? C23 O10 H10A 109.5 . . ? H13A O13 H13B 110.7(19) . . ? H15A O15 H15B 109.5 . . ? H16A O16 H16B 109.5 . . ? H14A O14 H14B 109.6 . . ? N1 Pt1 N2 80.9(3) . . ? N1 Pt1 Cl1 176.0(2) . . ? N2 Pt1 Cl1 95.1(3) . . ? N1 Pt1 Cl2 94.9(2) . . ? N2 Pt1 Cl2 175.8(3) . . ? Cl1 Pt1 Cl2 89.12(10) . . ? N4 Pt2 N3 80.3(3) . . ? N4 Pt2 Cl4 96.0(3) . . ? N3 Pt2 Cl4 176.3(2) . . ? N4 Pt2 Cl3 175.2(3) . . ? N3 Pt2 Cl3 94.9(2) . . ? Cl4 Pt2 Cl3 88.75(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C7 C8 C9 2.6(15) . . . . ? C6 C7 C8 C9 -177.4(10) . . . . ? N2 C2 C3 C4 4.1(16) . . . . ? N2 C2 C3 C1 -174.5(9) . . . . ? N1 C12 C10 C9 -0.4(17) . . . . ? N1 C12 C10 C11 -177.2(10) . . . . ? C12 C10 C11 O4 -7.5(17) . . . . ? C9 C10 C11 O4 175.8(11) . . . . ? C12 C10 C11 O3 175.5(10) . . . . ? C9 C10 C11 O3 -1.2(16) . . . . ? C7 C8 C9 C10 -3.9(16) . . . . ? C12 C10 C9 C8 2.8(16) . . . . ? C11 C10 C9 C8 179.5(10) . . . . ? N3 C18 C17 C16 -0.9(16) . . . . ? C19 C18 C17 C16 -179.2(10) . . . . ? C18 C17 C16 C15 -1.1(17) . . . . ? C17 C16 C15 C14 1.3(16) . . . . ? C17 C16 C15 C13 -179.7(10) . . . . ? C16 C15 C14 N3 0.4(16) . . . . ? C13 C15 C14 N3 -178.7(9) . . . . ? C16 C15 C13 O7 177.4(11) . . . . ? C14 C15 C13 O7 -3.6(16) . . . . ? C16 C15 C13 O8 -3.3(15) . . . . ? C14 C15 C13 O8 175.8(10) . . . . ? N3 C18 C19 N4 -1.3(12) . . . . ? C17 C18 C19 N4 177.2(10) . . . . ? N3 C18 C19 C20 -178.7(9) . . . . ? C17 C18 C19 C20 -0.3(16) . . . . ? C4 C5 C6 N2 2.7(16) . . . . ? C4 C5 C6 C7 -173.9(10) . . . . ? N1 C7 C6 N2 5.3(13) . . . . ? C8 C7 C6 N2 -174.7(9) . . . . ? N1 C7 C6 C5 -178.0(9) . . . . ? C8 C7 C6 C5 2.0(16) . . . . ? C2 C3 C1 O1 -177.6(10) . . . . ? C4 C3 C1 O1 3.7(15) . . . . ? C2 C3 C1 O2 4.1(14) . . . . ? C4 C3 C1 O2 -174.6(9) . . . . ? N4 C24 C22 C21 0.5(16) . . . . ? N4 C24 C22 C23 -178.3(9) . . . . ? O10 C23 C22 C21 0.1(17) . . . . ? O9 C23 C22 C21 -179.9(11) . . . . ? O10 C23 C22 C24 178.8(10) . . . . ? O9 C23 C22 C24 -1.1(16) . . . . ? C6 C5 C4 C3 1.5(17) . . . . ? C2 C3 C4 C5 -4.8(16) . . . . ? C1 C3 C4 C5 173.9(10) . . . . ? C24 C22 C21 C20 -1.4(16) . . . . ? C23 C22 C21 C20 177.4(10) . . . . ? C22 C21 C20 C19 1.5(17) . . . . ? N4 C19 C20 C21 -0.6(15) . . . . ? C18 C19 C20 C21 176.7(10) . . . . ? C10 C12 N1 C7 -0.9(15) . . . . ? C10 C12 N1 Pt1 178.9(8) . . . . ? C8 C7 N1 C12 -0.2(13) . . . . ? C6 C7 N1 C12 179.8(9) . . . . ? C8 C7 N1 Pt1 179.9(7) . . . . ? C6 C7 N1 Pt1 0.0(10) . . . . ? C5 C6 N2 C2 -3.5(15) . . . . ? C7 C6 N2 C2 173.3(8) . . . . ? C5 C6 N2 Pt1 175.3(8) . . . . ? C7 C6 N2 Pt1 -7.8(11) . . . . ? C3 C2 N2 C6 0.1(15) . . . . ? C3 C2 N2 Pt1 -178.6(7) . . . . ? C15 C14 N3 C18 -2.3(15) . . . . ? C15 C14 N3 Pt2 177.9(8) . . . . ? C17 C18 N3 C14 2.5(15) . . . . ? C19 C18 N3 C14 -179.0(9) . . . . ? C17 C18 N3 Pt2 -177.6(8) . . . . ? C19 C18 N3 Pt2 0.9(11) . . . . ? C22 C24 N4 C19 0.4(15) . . . . ? C22 C24 N4 Pt2 -178.4(7) . . . . ? C20 C19 N4 C24 -0.3(14) . . . . ? C18 C19 N4 C24 -177.9(9) . . . . ? C20 C19 N4 Pt2 178.6(8) . . . . ? C18 C19 N4 Pt2 1.1(10) . . . . ? C12 N1 Pt1 N2 177.1(9) . . . . ? C7 N1 Pt1 N2 -3.1(6) . . . . ? C12 N1 Pt1 Cl1 174(3) . . . . ? C7 N1 Pt1 Cl1 -7(4) . . . . ? C12 N1 Pt1 Cl2 -2.8(8) . . . . ? C7 N1 Pt1 Cl2 177.0(6) . . . . ? C6 N2 Pt1 N1 6.0(7) . . . . ? C2 N2 Pt1 N1 -175.2(9) . . . . ? C6 N2 Pt1 Cl1 -174.2(7) . . . . ? C2 N2 Pt1 Cl1 4.6(8) . . . . ? C6 N2 Pt1 Cl2 8(4) . . . . ? C2 N2 Pt1 Cl2 -173(3) . . . . ? C24 N4 Pt2 N3 178.4(9) . . . . ? C19 N4 Pt2 N3 -0.5(6) . . . . ? C24 N4 Pt2 Cl4 -2.4(8) . . . . ? C19 N4 Pt2 Cl4 178.7(6) . . . . ? C24 N4 Pt2 Cl3 179(44) . . . . ? C19 N4 Pt2 Cl3 0(3) . . . . ? C14 N3 Pt2 N4 179.6(9) . . . . ? C18 N3 Pt2 N4 -0.2(7) . . . . ? C14 N3 Pt2 Cl4 167(3) . . . . ? C18 N3 Pt2 Cl4 -13(4) . . . . ? C14 N3 Pt2 Cl3 -0.3(8) . . . . ? C18 N3 Pt2 Cl3 179.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.794 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.178 data_3 _database_code_depnum_ccdc_archive 'CCDC 733797' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Cl2 N2 O5 Pd' _chemical_formula_weight 439.52 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' Pd Pd -0.9988 1.0072 '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 7.2791(15) _cell_length_b 8.0941(16) _cell_length_c 12.513(3) _cell_angle_alpha 103.02(3) _cell_angle_beta 102.91(3) _cell_angle_gamma 90.52(3) _cell_volume 698.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2502 _cell_measurement_theta_min 2.876 _cell_measurement_theta_max 27.853 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 1.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8737 _exptl_absorpt_correction_T_max 0.9338 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5067 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2443 _reflns_number_gt 2174 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0414P)^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 2443 _refine_ls_number_parameters 201 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _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 Pd1 Pd 0.21804(3) 0.57381(2) 0.497519(16) 0.00949(9) Uani 1 1 d . . . Cl1 Cl 0.22359(10) 0.85146(8) 0.59485(6) 0.01629(16) Uani 1 1 d . . . Cl2 Cl 0.40912(9) 0.51197(8) 0.65430(6) 0.01471(16) Uani 1 1 d . . . N1 N 0.0513(3) 0.6109(3) 0.35457(19) 0.0103(5) Uani 1 1 d . . . N2 N 0.2094(3) 0.3383(3) 0.39799(19) 0.0109(5) Uani 1 1 d . . . O1 O -0.3717(3) 0.7935(2) 0.04235(18) 0.0220(5) Uani 1 1 d . . . H1 H -0.4483 0.7907 -0.0171 0.033 Uiso 1 1 calc R . . O2 O -0.3108(3) 0.5370(3) -0.04859(18) 0.0229(5) Uani 1 1 d . . . O3 O 0.1299(3) -0.1443(3) 0.05667(18) 0.0295(5) Uani 1 1 d . . . O4 O 0.3141(3) -0.2382(2) 0.19719(17) 0.0199(5) Uani 1 1 d . . . H4 H 0.3105 -0.3250 0.1479 0.030 Uiso 1 1 calc R . . C1 C -0.0384(4) 0.7514(3) 0.3431(2) 0.0135(6) Uani 1 1 d . . . H1A H -0.0232 0.8425 0.4054 0.016 Uiso 1 1 calc R . . C2 C -0.1521(4) 0.7660(3) 0.2426(2) 0.0137(6) Uani 1 1 d . . . H2 H -0.2146 0.8647 0.2379 0.016 Uiso 1 1 calc R . . C3 C -0.1731(4) 0.6335(3) 0.1487(2) 0.0132(6) Uani 1 1 d . . . C4 C -0.0825(4) 0.4849(3) 0.1597(2) 0.0110(6) Uani 1 1 d . . . H4A H -0.0959 0.3933 0.0978 0.013 Uiso 1 1 calc R . . C5 C 0.0271(4) 0.4751(3) 0.2630(2) 0.0104(5) Uani 1 1 d . . . C6 C 0.1205(3) 0.3239(3) 0.2876(2) 0.0099(5) Uani 1 1 d . . . C7 C 0.1192(4) 0.1743(3) 0.2071(2) 0.0118(6) Uani 1 1 d . . . H7 H 0.0582 0.1651 0.1321 0.014 Uiso 1 1 calc R . . C8 C 0.2119(4) 0.0377(3) 0.2412(2) 0.0112(6) Uani 1 1 d . . . C9 C 0.2967(4) 0.0524(3) 0.3532(2) 0.0131(6) Uani 1 1 d . . . H9 H 0.3553 -0.0387 0.3774 0.016 Uiso 1 1 calc R . . C10 C 0.2932(4) 0.2058(3) 0.4294(2) 0.0125(6) Uani 1 1 d . . . H10 H 0.3514 0.2163 0.5050 0.015 Uiso 1 1 calc R . . C11 C -0.2919(4) 0.6476(4) 0.0364(2) 0.0150(6) Uani 1 1 d . . . C12 C 0.2126(4) -0.1228(3) 0.1534(2) 0.0146(6) Uani 1 1 d . . . O5 O 0.4136(3) 0.8305(3) 0.86028(19) 0.0368(6) Uani 1 1 d D . . H5A H 0.3640 0.9254 0.8572 0.044 Uiso 1 1 d RD . . H5B H 0.3971 0.7563 0.8006 0.044 Uiso 1 1 d RD . . 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 Pd1 0.01060(14) 0.00924(13) 0.00727(14) 0.00014(9) 0.00104(9) 0.00058(8) Cl1 0.0203(4) 0.0115(3) 0.0126(4) -0.0023(3) -0.0003(3) 0.0026(3) Cl2 0.0155(3) 0.0174(3) 0.0097(3) 0.0030(3) -0.0002(3) 0.0005(3) N1 0.0102(11) 0.0092(11) 0.0115(13) 0.0003(9) 0.0043(9) -0.0028(9) N2 0.0089(11) 0.0122(11) 0.0104(12) 0.0000(9) 0.0022(9) -0.0014(9) O1 0.0335(13) 0.0143(10) 0.0143(11) 0.0025(8) -0.0023(9) 0.0135(9) O2 0.0358(13) 0.0178(10) 0.0104(11) -0.0002(8) -0.0010(9) 0.0115(9) O3 0.0484(15) 0.0189(11) 0.0135(12) -0.0010(9) -0.0045(10) 0.0145(10) O4 0.0284(12) 0.0116(10) 0.0152(11) -0.0015(8) 0.0001(9) 0.0123(9) C1 0.0161(14) 0.0091(13) 0.0147(15) 0.0008(11) 0.0043(12) 0.0033(11) C2 0.0176(14) 0.0083(13) 0.0153(16) 0.0014(11) 0.0052(12) 0.0027(11) C3 0.0164(14) 0.0118(13) 0.0129(15) 0.0045(11) 0.0049(12) 0.0026(11) C4 0.0121(13) 0.0095(13) 0.0104(14) -0.0002(11) 0.0029(11) 0.0004(11) C5 0.0111(13) 0.0087(12) 0.0118(15) 0.0017(11) 0.0045(11) 0.0002(10) C6 0.0068(12) 0.0106(13) 0.0120(15) 0.0025(11) 0.0021(11) -0.0030(10) C7 0.0113(13) 0.0143(13) 0.0093(14) 0.0027(11) 0.0013(11) 0.0007(11) C8 0.0108(13) 0.0085(13) 0.0141(15) 0.0011(11) 0.0038(11) 0.0005(10) C9 0.0130(13) 0.0117(13) 0.0140(15) 0.0040(11) 0.0013(11) 0.0012(11) C10 0.0120(14) 0.0149(14) 0.0099(14) 0.0050(11) -0.0009(11) 0.0012(11) C11 0.0183(15) 0.0113(14) 0.0143(15) 0.0011(11) 0.0034(12) 0.0029(11) C12 0.0179(14) 0.0123(14) 0.0137(16) 0.0029(11) 0.0040(12) 0.0034(11) O5 0.0581(17) 0.0304(13) 0.0144(13) 0.0014(10) -0.0041(11) 0.0186(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 Pd1 N1 2.010(2) . ? Pd1 N2 2.020(2) . ? Pd1 Cl2 2.2957(10) . ? Pd1 Cl1 2.2974(10) . ? N1 C1 1.336(3) . ? N1 C5 1.376(3) . ? N2 C10 1.331(3) . ? N2 C6 1.366(4) . ? O1 C11 1.315(3) . ? O1 H1 0.8200 . ? O2 C11 1.207(4) . ? O3 C12 1.198(3) . ? O4 C12 1.334(3) . ? O4 H4 0.8200 . ? C1 C2 1.372(4) . ? C1 H1A 0.9300 . ? C2 C3 1.379(4) . ? C2 H2 0.9300 . ? C3 C4 1.396(4) . ? C3 C11 1.505(4) . ? C4 C5 1.379(4) . ? C4 H4A 0.9300 . ? C5 C6 1.465(4) . ? C6 C7 1.388(4) . ? C7 C8 1.400(4) . ? C7 H7 0.9300 . ? C8 C9 1.376(4) . ? C8 C12 1.502(4) . ? C9 C10 1.390(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? O5 H5A 0.8572 . ? O5 H5B 0.8302 . ? 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 Pd1 N2 80.58(9) . . ? N1 Pd1 Cl2 175.99(6) . . ? N2 Pd1 Cl2 95.40(7) . . ? N1 Pd1 Cl1 94.45(7) . . ? N2 Pd1 Cl1 174.36(7) . . ? Cl2 Pd1 Cl1 89.56(4) . . ? C1 N1 C5 119.0(2) . . ? C1 N1 Pd1 125.86(18) . . ? C5 N1 Pd1 115.16(17) . . ? C10 N2 C6 119.5(2) . . ? C10 N2 Pd1 125.68(19) . . ? C6 N2 Pd1 114.57(17) . . ? C11 O1 H1 109.5 . . ? C12 O4 H4 109.5 . . ? N1 C1 C2 122.3(2) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C1 C2 C3 119.7(3) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 118.7(3) . . ? C2 C3 C11 121.0(2) . . ? C4 C3 C11 120.3(2) . . ? C5 C4 C3 119.4(2) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? N1 C5 C4 120.8(2) . . ? N1 C5 C6 114.1(2) . . ? C4 C5 C6 125.0(2) . . ? N2 C6 C7 121.1(2) . . ? N2 C6 C5 115.0(2) . . ? C7 C6 C5 123.8(2) . . ? C6 C7 C8 118.5(3) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C9 C8 C7 119.8(2) . . ? C9 C8 C12 122.0(2) . . ? C7 C8 C12 118.2(2) . . ? C8 C9 C10 118.8(2) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N2 C10 C9 122.2(3) . . ? N2 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? O2 C11 O1 124.4(3) . . ? O2 C11 C3 123.4(3) . . ? O1 C11 C3 112.2(2) . . ? O3 C12 O4 124.7(3) . . ? O3 C12 C8 123.8(3) . . ? O4 C12 C8 111.5(2) . . ? H5A O5 H5B 117.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pd1 N1 C1 173.2(2) . . . . ? Cl2 Pd1 N1 C1 172.0(7) . . . . ? Cl1 Pd1 N1 C1 -9.5(2) . . . . ? N2 Pd1 N1 C5 -5.12(17) . . . . ? Cl2 Pd1 N1 C5 -6.3(9) . . . . ? Cl1 Pd1 N1 C5 172.18(16) . . . . ? N1 Pd1 N2 C10 -178.6(2) . . . . ? Cl2 Pd1 N2 C10 1.3(2) . . . . ? Cl1 Pd1 N2 C10 152.9(5) . . . . ? N1 Pd1 N2 C6 6.70(17) . . . . ? Cl2 Pd1 N2 C6 -173.39(16) . . . . ? Cl1 Pd1 N2 C6 -21.8(7) . . . . ? C5 N1 C1 C2 -0.8(4) . . . . ? Pd1 N1 C1 C2 -179.10(19) . . . . ? N1 C1 C2 C3 -1.4(4) . . . . ? C1 C2 C3 C4 2.2(4) . . . . ? C1 C2 C3 C11 -178.1(2) . . . . ? C2 C3 C4 C5 -0.8(4) . . . . ? C11 C3 C4 C5 179.4(2) . . . . ? C1 N1 C5 C4 2.2(4) . . . . ? Pd1 N1 C5 C4 -179.34(18) . . . . ? C1 N1 C5 C6 -175.6(2) . . . . ? Pd1 N1 C5 C6 2.8(3) . . . . ? C3 C4 C5 N1 -1.4(4) . . . . ? C3 C4 C5 C6 176.2(2) . . . . ? C10 N2 C6 C7 -1.2(4) . . . . ? Pd1 N2 C6 C7 173.77(19) . . . . ? C10 N2 C6 C5 177.9(2) . . . . ? Pd1 N2 C6 C5 -7.1(3) . . . . ? N1 C5 C6 N2 2.9(3) . . . . ? C4 C5 C6 N2 -174.9(2) . . . . ? N1 C5 C6 C7 -178.1(2) . . . . ? C4 C5 C6 C7 4.2(4) . . . . ? N2 C6 C7 C8 -0.2(4) . . . . ? C5 C6 C7 C8 -179.3(2) . . . . ? C6 C7 C8 C9 1.9(4) . . . . ? C6 C7 C8 C12 -179.0(2) . . . . ? C7 C8 C9 C10 -2.0(4) . . . . ? C12 C8 C9 C10 178.9(2) . . . . ? C6 N2 C10 C9 1.1(4) . . . . ? Pd1 N2 C10 C9 -173.33(19) . . . . ? C8 C9 C10 N2 0.6(4) . . . . ? C2 C3 C11 O2 178.1(3) . . . . ? C4 C3 C11 O2 -2.1(4) . . . . ? C2 C3 C11 O1 -2.0(4) . . . . ? C4 C3 C11 O1 177.8(2) . . . . ? C9 C8 C12 O3 174.9(3) . . . . ? C7 C8 C12 O3 -4.2(4) . . . . ? C9 C8 C12 O4 -4.2(4) . . . . ? C7 C8 C12 O4 176.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.584 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.088 data_4 _database_code_depnum_ccdc_archive 'CCDC 733798' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Cl2 N2 O5 Pt' _chemical_formula_weight 528.21 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3879(15) _cell_length_b 7.9746(16) _cell_length_c 12.542(3) _cell_angle_alpha 102.29(3) _cell_angle_beta 103.83(3) _cell_angle_gamma 92.87(3) _cell_volume 697.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2531 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 25.01 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 10.473 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2544 _exptl_absorpt_correction_T_max 0.4207 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4748 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0729 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2452 _reflns_number_gt 2142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0330P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2452 _refine_ls_number_parameters 201 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.020 _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 Pt1 Pt 0.78460(4) 0.42121(3) 0.00247(2) 0.01412(12) Uani 1 1 d . . . Cl1 Cl 0.6004(3) 0.4786(2) -0.15860(15) 0.0178(4) Uani 1 1 d . . . Cl2 Cl 0.7844(3) 0.1439(2) -0.09750(15) 0.0208(5) Uani 1 1 d . . . O1 O 0.6777(8) 1.2289(6) 0.3002(4) 0.0231(14) Uani 1 1 d . . . H1 H 0.6809 1.3157 0.3496 0.035 Uiso 1 1 calc R . . O2 O 0.8631(9) 1.1382(7) 0.4427(4) 0.0308(16) Uani 1 1 d . . . O3 O 1.3131(9) 0.4690(6) 0.5519(4) 0.0255(14) Uani 1 1 d . . . O4 O 1.3651(9) 0.2081(6) 0.4612(4) 0.0254(14) Uani 1 1 d . . . H4 H 1.4336 0.2076 0.5231 0.038 Uiso 1 1 calc R . . N1 N 0.7876(9) 0.6550(7) 0.1018(5) 0.0113(13) Uani 1 1 d . . . N2 N 0.9453(10) 0.3860(7) 0.1471(5) 0.0156(15) Uani 1 1 d . . . C1 C 0.7025(11) 0.7857(8) 0.0703(6) 0.0175(18) Uani 1 1 d . . . H1A H 0.6459 0.7748 -0.0058 0.021 Uiso 1 1 calc R . . C2 C 0.6941(11) 0.9372(9) 0.1455(6) 0.0165(17) Uani 1 1 d . . . H2 H 0.6296 1.0248 0.1209 0.020 Uiso 1 1 calc R . . C3 C 0.7831(11) 0.9560(8) 0.2578(6) 0.0125(16) Uani 1 1 d . . . C4 C 0.8737(11) 0.8208(8) 0.2925(6) 0.0143(17) Uani 1 1 d . . . H4A H 0.9317 0.8307 0.3683 0.017 Uiso 1 1 calc R . . C5 C 0.8770(12) 0.6722(9) 0.2138(6) 0.0161(18) Uani 1 1 d . . . C6 C 0.9673(11) 0.5222(9) 0.2385(6) 0.0139(17) Uani 1 1 d . . . C7 C 1.0795(11) 0.5150(8) 0.3431(6) 0.0136(17) Uani 1 1 d . . . H7 H 1.0941 0.6069 0.4052 0.016 Uiso 1 1 calc R . . C8 C 1.1693(11) 0.3687(8) 0.3533(6) 0.0142(17) Uani 1 1 d . . . C9 C 1.1462(11) 0.2346(9) 0.2603(6) 0.0172(18) Uani 1 1 d . . . H9 H 1.2067 0.1362 0.2664 0.021 Uiso 1 1 calc R . . C10 C 1.0334(11) 0.2465(8) 0.1584(6) 0.0155(18) Uani 1 1 d . . . H10 H 1.0182 0.1552 0.0959 0.019 Uiso 1 1 calc R . . C11 C 0.7764(12) 1.1155(9) 0.3447(6) 0.0179(18) Uani 1 1 d . . . C12 C 1.2909(12) 0.3563(9) 0.4665(6) 0.0174(18) Uani 1 1 d . . . O5 O 0.4114(10) 0.8387(7) 0.3626(4) 0.0412(19) Uani 1 1 d D . . H5A H 0.4912 0.8640 0.3281 0.062 Uiso 1 1 d RD . . H5B H 0.3437 0.9198 0.3802 0.062 Uiso 1 1 d RD . . 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 0.0168(2) 0.01375(19) 0.00906(18) -0.00057(12) 0.00081(13) 0.00144(12) Cl1 0.0189(12) 0.0220(10) 0.0104(9) 0.0031(7) 0.0004(8) 0.0022(8) Cl2 0.0264(13) 0.0166(9) 0.0126(9) -0.0028(7) -0.0028(9) 0.0039(8) O1 0.031(4) 0.015(3) 0.017(3) -0.004(2) 0.000(3) 0.012(3) O2 0.049(5) 0.024(3) 0.012(3) -0.002(2) -0.004(3) 0.013(3) O3 0.041(4) 0.016(3) 0.011(3) -0.005(2) -0.004(3) 0.011(3) O4 0.035(4) 0.021(3) 0.017(3) 0.004(2) -0.003(3) 0.017(3) N1 0.008(4) 0.014(3) 0.010(3) 0.004(2) -0.001(3) 0.000(3) N2 0.027(4) 0.006(3) 0.013(3) -0.002(2) 0.009(3) 0.000(3) C1 0.022(5) 0.015(4) 0.010(4) 0.002(3) -0.008(3) 0.007(3) C2 0.014(5) 0.014(4) 0.019(4) 0.002(3) 0.001(3) 0.002(3) C3 0.016(5) 0.012(4) 0.011(4) 0.004(3) 0.005(3) 0.003(3) C4 0.018(5) 0.016(4) 0.008(4) 0.003(3) 0.002(3) 0.003(3) C5 0.017(5) 0.014(4) 0.016(4) 0.002(3) 0.003(4) 0.000(3) C6 0.011(5) 0.019(4) 0.014(4) 0.001(3) 0.009(3) -0.003(3) C7 0.015(5) 0.013(4) 0.011(4) -0.001(3) 0.003(3) 0.003(3) C8 0.016(5) 0.014(4) 0.009(4) 0.003(3) -0.004(3) 0.005(3) C9 0.017(5) 0.010(4) 0.021(4) 0.003(3) -0.002(4) 0.001(3) C10 0.022(5) 0.011(4) 0.012(4) -0.002(3) 0.003(4) 0.001(3) C11 0.021(5) 0.017(4) 0.014(4) -0.003(3) 0.006(4) 0.007(3) C12 0.021(5) 0.018(4) 0.016(4) 0.010(3) 0.004(4) 0.004(3) O5 0.071(6) 0.030(3) 0.014(3) -0.002(3) -0.002(3) 0.020(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 2.000(6) . ? Pt1 N1 2.005(6) . ? Pt1 Cl2 2.2982(19) . ? Pt1 Cl1 2.299(2) . ? O1 C11 1.322(9) . ? O1 H1 0.8200 . ? O2 C11 1.213(9) . ? O3 C12 1.214(9) . ? O4 C12 1.323(9) . ? O4 H4 0.8200 . ? N1 C1 1.327(9) . ? N1 C5 1.376(9) . ? N2 C10 1.333(9) . ? N2 C6 1.373(8) . ? C1 C2 1.379(10) . ? C1 H1A 0.9300 . ? C2 C3 1.377(10) . ? C2 H2 0.9300 . ? C3 C4 1.390(10) . ? C3 C11 1.500(9) . ? C4 C5 1.377(9) . ? C4 H4A 0.9300 . ? C5 C6 1.453(10) . ? C6 C7 1.388(10) . ? C7 C8 1.385(10) . ? C7 H7 0.9300 . ? C8 C9 1.374(9) . ? C8 C12 1.514(10) . ? C9 C10 1.374(10) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? O5 H5A 0.8493 . ? O5 H5B 0.8608 . ? 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 N1 80.8(2) . . ? N2 Pt1 Cl2 94.85(16) . . ? N1 Pt1 Cl2 175.00(17) . . ? N2 Pt1 Cl1 176.61(15) . . ? N1 Pt1 Cl1 95.87(18) . . ? Cl2 Pt1 Cl1 88.54(7) . . ? C11 O1 H1 109.5 . . ? C12 O4 H4 109.5 . . ? C1 N1 C5 118.9(6) . . ? C1 N1 Pt1 126.0(5) . . ? C5 N1 Pt1 114.9(5) . . ? C10 N2 C6 119.9(7) . . ? C10 N2 Pt1 125.1(5) . . ? C6 N2 Pt1 115.0(5) . . ? N1 C1 C2 123.0(7) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C3 C2 C1 118.6(7) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 119.3(6) . . ? C2 C3 C11 121.5(7) . . ? C4 C3 C11 119.1(6) . . ? C5 C4 C3 119.6(7) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? N1 C5 C4 120.6(7) . . ? N1 C5 C6 114.3(6) . . ? C4 C5 C6 125.1(7) . . ? N2 C6 C7 120.4(7) . . ? N2 C6 C5 114.8(6) . . ? C7 C6 C5 124.7(6) . . ? C8 C7 C6 118.9(6) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 119.6(7) . . ? C9 C8 C12 120.3(6) . . ? C7 C8 C12 120.1(6) . . ? C8 C9 C10 119.7(7) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 121.5(6) . . ? N2 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? O2 C11 O1 125.3(7) . . ? O2 C11 C3 122.2(7) . . ? O1 C11 C3 112.3(6) . . ? O3 C12 O4 124.7(7) . . ? O3 C12 C8 123.1(7) . . ? O4 C12 C8 112.1(6) . . ? H5A O5 H5B 114.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pt1 N1 C1 179.6(7) . . . . ? Cl2 Pt1 N1 C1 -151.6(18) . . . . ? Cl1 Pt1 N1 C1 0.0(7) . . . . ? N2 Pt1 N1 C5 -5.0(5) . . . . ? Cl2 Pt1 N1 C5 24(3) . . . . ? Cl1 Pt1 N1 C5 175.4(5) . . . . ? N1 Pt1 N2 C10 -173.6(7) . . . . ? Cl2 Pt1 N2 C10 8.8(6) . . . . ? Cl1 Pt1 N2 C10 -167(3) . . . . ? N1 Pt1 N2 C6 4.1(5) . . . . ? Cl2 Pt1 N2 C6 -173.4(5) . . . . ? Cl1 Pt1 N2 C6 11(4) . . . . ? C5 N1 C1 C2 -2.1(12) . . . . ? Pt1 N1 C1 C2 173.1(6) . . . . ? N1 C1 C2 C3 2.2(12) . . . . ? C1 C2 C3 C4 -1.8(12) . . . . ? C1 C2 C3 C11 -178.6(7) . . . . ? C2 C3 C4 C5 1.6(12) . . . . ? C11 C3 C4 C5 178.5(7) . . . . ? C1 N1 C5 C4 1.9(11) . . . . ? Pt1 N1 C5 C4 -173.9(6) . . . . ? C1 N1 C5 C6 -179.3(7) . . . . ? Pt1 N1 C5 C6 4.9(8) . . . . ? C3 C4 C5 N1 -1.6(12) . . . . ? C3 C4 C5 C6 179.7(7) . . . . ? C10 N2 C6 C7 -0.6(11) . . . . ? Pt1 N2 C6 C7 -178.4(6) . . . . ? C10 N2 C6 C5 175.2(7) . . . . ? Pt1 N2 C6 C5 -2.7(8) . . . . ? N1 C5 C6 N2 -1.5(10) . . . . ? C4 C5 C6 N2 177.3(7) . . . . ? N1 C5 C6 C7 174.0(7) . . . . ? C4 C5 C6 C7 -7.2(12) . . . . ? N2 C6 C7 C8 0.3(11) . . . . ? C5 C6 C7 C8 -175.0(7) . . . . ? C6 C7 C8 C9 0.2(12) . . . . ? C6 C7 C8 C12 -179.3(7) . . . . ? C7 C8 C9 C10 -0.4(12) . . . . ? C12 C8 C9 C10 179.1(7) . . . . ? C6 N2 C10 C9 0.3(11) . . . . ? Pt1 N2 C10 C9 177.9(6) . . . . ? C8 C9 C10 N2 0.2(12) . . . . ? C2 C3 C11 O2 -175.6(8) . . . . ? C4 C3 C11 O2 7.6(12) . . . . ? C2 C3 C11 O1 0.1(11) . . . . ? C4 C3 C11 O1 -176.7(7) . . . . ? C9 C8 C12 O3 -178.4(8) . . . . ? C7 C8 C12 O3 1.1(12) . . . . ? C9 C8 C12 O4 0.2(11) . . . . ? C7 C8 C12 O4 179.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.688 _refine_diff_density_min -2.142 _refine_diff_density_rms 0.246