# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © 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 'Sanz Miguel, Pablo J.' _publ_contact_author_address ;Department of Bioinorganic Chemistry TU Dortmund University Otto-Hahn-Strasse 6 44227 Dortmund, Germany ; # Address of author for correspondence _publ_contact_author_email pablo.sanz@uni-dortmund.de _publ_contact_author_fax 49(231)7553797 _publ_contact_author_phone 49(231)7555034 _publ_section_title ; Coordination of two different metal ions as reason for N-chirality in m-amide complexes. ; # Attachment '- CCDC_819877_revised.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-10-27 at 16:08:18 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : 1 #TrackingRef '- CCDC_819877_revised.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2009-10-27 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? loop_ _publ_author_name P.Brandi-Blanco 'P.Sanz Miguel' Lippert #============================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 819877' #TrackingRef '- CCDC_819877_revised.cif' _audit_creation_date 2009-10-27T16:08:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H30 N10 Pd2 Pt, 2(N O3)' _chemical_formula_sum 'C12 H30 N12 O6 Pd2 Pt' _chemical_formula_weight 846.37 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 15.7994(8) _cell_length_b 10.6355(4) _cell_length_c 15.0356(8) _cell_angle_alpha 90 _cell_angle_beta 114.114(6) _cell_angle_gamma 90 _cell_volume 2306.02(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4665 _cell_measurement_theta_min 2.3719 _cell_measurement_theta_max 29.012 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prisms _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.393 _exptl_absorpt_correction_T_max 0.465 _exptl_absorpt_process_details sadabs #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_unetI/netI 0.0718 _diffrn_reflns_number 10493 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 29.08 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.853 _reflns_number_total 5276 _reflns_number_gt 3613 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2010)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5276 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0337 _refine_ls_wR_factor_gt 0.0324 _refine_ls_goodness_of_fit_ref 0.827 _refine_ls_restrained_S_all 0.827 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.044 _refine_diff_density_min -1.158 _refine_diff_density_rms 0.171 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.246001(17) 0.790590(16) 0.001986(17) 0.01121(4) Uani 1 1 d . . . Pd1 Pd 0.05053(3) 0.96855(3) -0.11558(3) 0.01212(9) Uani 1 1 d . . . Pd2 Pd 0.44054(3) 0.60957(3) 0.11609(3) 0.01219(9) Uani 1 1 d . . . N11 N 0.1888(3) 0.9518(3) -0.0726(3) 0.0129(9) Uani 1 1 d . . . H11 H 0.2158 1.0182 -0.0303 0.015 Uiso 1 1 calc R . . C12 C 0.2121(3) 0.9696(4) -0.1568(3) 0.0201(12) Uani 1 1 d . . . H12A H 0.1899 1.0521 -0.1861 0.03 Uiso 1 1 calc R . . H12B H 0.1825 0.9036 -0.2051 0.03 Uiso 1 1 calc R . . H12C H 0.2795 0.965 -0.1355 0.03 Uiso 1 1 calc R . . N21 N 0.3036(3) 0.6294(3) 0.0768(3) 0.0134(9) Uani 1 1 d . . . H21 H 0.2755 0.5632 0.0346 0.016 Uiso 1 1 calc R . . C22 C 0.2814(3) 0.6114(4) 0.1618(3) 0.0174(11) Uani 1 1 d . . . H22A H 0.3045 0.5293 0.1913 0.026 Uiso 1 1 calc R . . H22B H 0.2141 0.6151 0.1412 0.026 Uiso 1 1 calc R . . H22C H 0.311 0.6779 0.2097 0.026 Uiso 1 1 calc R . . N31 N 0.3716(3) 0.8689(3) 0.0608(3) 0.0116(9) Uani 1 1 d . . . N32 N 0.4494(3) 0.7957(3) 0.1047(3) 0.0143(10) Uani 1 1 d . . . C33 C 0.5236(3) 0.8710(4) 0.1318(3) 0.0149(11) Uani 1 1 d . . . H33A H 0.5861 0.8437 0.1628 0.018 Uiso 1 1 calc R . . C34 C 0.4961(4) 0.9939(4) 0.1083(3) 0.0186(12) Uani 1 1 d . . . H34A H 0.5343 1.0663 0.1203 0.022 Uiso 1 1 calc R . . C35 C 0.3997(3) 0.9883(4) 0.0630(3) 0.0191(12) Uani 1 1 d . . . H35A H 0.3598 1.0585 0.0375 0.023 Uiso 1 1 calc R . . N41 N 0.1215(3) 0.7112(3) -0.0582(3) 0.0128(9) Uani 1 1 d . . . N42 N 0.0432(3) 0.7806(3) -0.1081(3) 0.0124(10) Uani 1 1 d . . . C43 C -0.0300(3) 0.7070(4) -0.1345(3) 0.0175(11) Uani 1 1 d . . . H43A H -0.0924 0.7337 -0.169 0.021 Uiso 1 1 calc R . . C44 C -0.0030(3) 0.5862(4) -0.1048(3) 0.0175(12) Uani 1 1 d . . . H44A H -0.0412 0.514 -0.1144 0.021 Uiso 1 1 calc R . . C45 C 0.0922(3) 0.5930(4) -0.0581(3) 0.0164(12) Uani 1 1 d . . . H45A H 0.1317 0.5234 -0.0296 0.02 Uiso 1 1 calc R . . N51 N -0.0905(3) 0.9993(3) -0.1687(3) 0.0159(10) Uani 1 1 d . . . H51A H -0.1207 0.9489 -0.2221 0.019 Uiso 1 1 calc R . . H51B H -0.1116 0.9794 -0.1218 0.019 Uiso 1 1 calc R . . C52 C -0.1098(4) 1.1323(4) -0.1963(4) 0.0372(16) Uani 1 1 d . . . H52A H -0.1172 1.1438 -0.2645 0.045 Uiso 1 1 calc R . . H52B H -0.1685 1.1574 -0.1924 0.045 Uiso 1 1 calc R . . C53 C -0.0354(3) 1.2110(4) -0.1328(4) 0.0315(14) Uani 1 1 d . . . H53A H -0.0404 1.22 -0.0696 0.038 Uiso 1 1 calc R . . H53B H -0.0414 1.2958 -0.162 0.038 Uiso 1 1 calc R . . N54 N 0.0553(3) 1.1595(3) -0.1161(3) 0.0179(10) Uani 1 1 d . . . H54A H 0.0986 1.1878 -0.0572 0.021 Uiso 1 1 calc R . . H54B H 0.0727 1.1864 -0.1643 0.021 Uiso 1 1 calc R . . N61 N 0.5808(3) 0.5740(3) 0.1643(3) 0.0167(10) Uani 1 1 d . . . H61A H 0.5995 0.5878 0.1146 0.02 Uiso 1 1 calc R . . H61B H 0.6137 0.6271 0.2149 0.02 Uiso 1 1 calc R . . C62 C 0.5989(4) 0.4423(4) 0.1970(4) 0.0259(14) Uani 1 1 d . . . H62A H 0.6037 0.4351 0.2645 0.031 Uiso 1 1 calc R . . H62B H 0.6583 0.4141 0.1962 0.031 Uiso 1 1 calc R . . C63 C 0.5220(3) 0.3623(5) 0.1310(4) 0.0268(13) Uani 1 1 d . . . H63A H 0.5246 0.3567 0.0665 0.032 Uiso 1 1 calc R . . H63B H 0.5281 0.2764 0.1582 0.032 Uiso 1 1 calc R . . N64 N 0.4325(3) 0.4175(3) 0.1203(3) 0.0172(10) Uani 1 1 d . . . H64A H 0.4191 0.3938 0.172 0.021 Uiso 1 1 calc R . . H64B H 0.3858 0.3888 0.0639 0.021 Uiso 1 1 calc R . . N10 N 0.2510(3) 0.1578(4) 0.3899(3) 0.0231(11) Uani 1 1 d . . . O11 O 0.1766(3) 0.1907(3) 0.3267(3) 0.0347(10) Uani 1 1 d . . . O12 O 0.2699(2) 0.0434(3) 0.4049(2) 0.0287(9) Uani 1 1 d . . . O13 O 0.3093(3) 0.2372(3) 0.4398(3) 0.0366(11) Uani 1 1 d . . . N20 N 0.2431(3) 0.2402(4) 0.1136(3) 0.0193(10) Uani 1 1 d . . . O21 O 0.2156(2) 0.1293(3) 0.0956(2) 0.0316(10) Uani 1 1 d . . . O22 O 0.2006(3) 0.3261(3) 0.0587(3) 0.0395(11) Uani 1 1 d . . . O23 O 0.3145(3) 0.2627(3) 0.1862(3) 0.0367(10) 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 Pt1 0.00855(10) 0.01154(8) 0.01184(9) 0.00166(9) 0.00242(7) 0.00114(8) Pd1 0.0097(2) 0.0109(2) 0.0137(2) 0.00278(17) 0.00269(19) 0.00100(16) Pd2 0.0102(2) 0.0124(2) 0.0125(2) 0.00195(18) 0.00312(18) 0.00151(16) N11 0.012(2) 0.010(2) 0.016(2) -0.0014(18) 0.005(2) 0.0020(17) C12 0.019(3) 0.024(3) 0.017(3) 0.006(2) 0.008(3) 0.010(2) N21 0.014(2) 0.013(2) 0.011(2) 0.0004(18) 0.003(2) 0.0036(17) C22 0.013(3) 0.023(3) 0.014(3) 0.000(2) 0.003(2) 0.002(2) N31 0.012(2) 0.009(2) 0.011(2) 0.0056(18) 0.0024(19) 0.0039(17) N32 0.009(2) 0.017(2) 0.015(2) -0.002(2) 0.003(2) 0.002(2) C33 0.005(3) 0.021(3) 0.015(3) 0.001(2) -0.001(2) -0.002(2) C34 0.013(3) 0.017(3) 0.024(3) -0.005(2) 0.007(3) -0.006(2) C35 0.013(3) 0.017(3) 0.027(3) -0.001(2) 0.008(3) 0.003(2) N41 0.012(2) 0.011(2) 0.013(2) 0.0037(19) 0.0034(19) 0.0049(18) N42 0.007(2) 0.011(2) 0.018(3) 0.0023(19) 0.005(2) 0.0002(18) C43 0.012(3) 0.019(3) 0.019(3) 0.005(3) 0.004(2) 0.003(2) C44 0.015(3) 0.019(3) 0.016(3) 0.000(2) 0.003(3) -0.005(2) C45 0.015(3) 0.009(3) 0.022(3) 0.001(2) 0.005(3) 0.001(2) N51 0.016(3) 0.016(2) 0.018(2) 0.0033(19) 0.009(2) 0.0008(18) C52 0.022(4) 0.019(3) 0.066(5) -0.005(3) 0.013(4) 0.000(3) C53 0.019(3) 0.021(3) 0.047(4) 0.003(3) 0.005(3) 0.011(3) N54 0.014(2) 0.020(2) 0.019(2) -0.0025(19) 0.005(2) -0.0021(18) N61 0.014(3) 0.018(2) 0.017(2) -0.0027(18) 0.005(2) 0.0003(18) C62 0.025(4) 0.024(3) 0.031(4) 0.007(3) 0.015(3) 0.016(3) C63 0.024(4) 0.024(3) 0.030(3) -0.005(3) 0.010(3) 0.008(3) N64 0.019(3) 0.013(2) 0.018(2) -0.0005(18) 0.005(2) 0.0033(18) N10 0.024(3) 0.030(3) 0.020(3) 0.007(2) 0.014(3) 0.005(2) O11 0.026(3) 0.043(2) 0.023(2) 0.0013(19) -0.003(2) 0.020(2) O12 0.040(3) 0.021(2) 0.035(2) 0.0134(19) 0.025(2) 0.0136(18) O13 0.035(3) 0.039(2) 0.031(3) -0.012(2) 0.009(2) -0.021(2) N20 0.019(3) 0.024(3) 0.018(3) 0.000(2) 0.011(2) -0.004(2) O21 0.037(3) 0.027(2) 0.038(3) -0.014(2) 0.024(2) -0.0208(19) O22 0.039(3) 0.044(3) 0.034(3) 0.017(2) 0.014(2) 0.017(2) O23 0.031(3) 0.037(2) 0.025(2) 0.0043(19) -0.006(2) -0.0176(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N41 1.986(4) . ? Pt1 N31 1.995(4) . ? Pt1 N11 2.046(3) . ? Pt1 N21 2.048(3) . ? Pd1 N42 2.008(3) . ? Pd1 N11 2.017(4) . ? Pd1 N54 2.033(3) . ? Pd1 N51 2.062(4) . ? Pd2 N32 1.997(3) . ? Pd2 N21 2.008(4) . ? Pd2 N64 2.049(3) . ? Pd2 N61 2.066(4) . ? N11 C12 1.468(5) . ? N11 H11 0.93 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? N21 C22 1.469(5) . ? N21 H21 0.93 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? N31 C35 1.342(5) . ? N31 N32 1.375(5) . ? N32 C33 1.338(5) . ? C33 C34 1.377(6) . ? C33 H33A 0.95 . ? C34 C35 1.392(6) . ? C34 H34A 0.95 . ? C35 H35A 0.95 . ? N41 C45 1.340(5) . ? N41 N42 1.371(5) . ? N42 C43 1.317(5) . ? C43 C44 1.370(6) . ? C43 H43A 0.95 . ? C44 C45 1.377(6) . ? C44 H44A 0.95 . ? C45 H45A 0.95 . ? N51 C52 1.471(5) . ? N51 H51A 0.92 . ? N51 H51B 0.92 . ? C52 C53 1.442(6) . ? C52 H52A 0.99 . ? C52 H52B 0.99 . ? C53 N54 1.456(5) . ? C53 H53A 0.99 . ? C53 H53B 0.99 . ? N54 H54A 0.92 . ? N54 H54B 0.92 . ? N61 C62 1.473(5) . ? N61 H61A 0.92 . ? N61 H61B 0.92 . ? C62 C63 1.483(6) . ? C62 H62A 0.99 . ? C62 H62B 0.99 . ? C63 N64 1.478(5) . ? C63 H63A 0.99 . ? C63 H63B 0.99 . ? N64 H64A 0.92 . ? N64 H64B 0.92 . ? N10 O11 1.222(5) . ? N10 O13 1.249(5) . ? N10 O12 1.252(4) . ? N20 O22 1.230(5) . ? N20 O23 1.231(5) . ? N20 O21 1.248(4) . ? 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 N41 Pt1 N31 179.04(15) . . ? N41 Pt1 N11 88.45(15) . . ? N31 Pt1 N11 91.72(14) . . ? N41 Pt1 N21 91.67(14) . . ? N31 Pt1 N21 88.16(15) . . ? N11 Pt1 N21 179.9(2) . . ? N42 Pd1 N11 88.47(15) . . ? N42 Pd1 N54 176.34(15) . . ? N11 Pd1 N54 93.04(14) . . ? N42 Pd1 N51 95.85(15) . . ? N11 Pd1 N51 174.40(13) . . ? N54 Pd1 N51 82.86(14) . . ? N32 Pd2 N21 88.62(15) . . ? N32 Pd2 N64 176.61(15) . . ? N21 Pd2 N64 92.34(14) . . ? N32 Pd2 N61 96.23(15) . . ? N21 Pd2 N61 174.40(13) . . ? N64 Pd2 N61 82.97(14) . . ? C12 N11 Pd1 109.4(3) . . ? C12 N11 Pt1 111.8(3) . . ? Pd1 N11 Pt1 115.34(16) . . ? C12 N11 H11 106.6 . . ? Pd1 N11 H11 106.6 . . ? Pt1 N11 H11 106.6 . . ? N11 C12 H12A 109.5 . . ? N11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 N21 Pd2 110.0(3) . . ? C22 N21 Pt1 112.1(3) . . ? Pd2 N21 Pt1 115.63(16) . . ? C22 N21 H21 106.1 . . ? Pd2 N21 H21 106.1 . . ? Pt1 N21 H21 106.1 . . ? N21 C22 H22A 109.5 . . ? N21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C35 N31 N32 107.6(4) . . ? C35 N31 Pt1 131.7(3) . . ? N32 N31 Pt1 120.6(3) . . ? C33 N32 N31 107.9(4) . . ? C33 N32 Pd2 130.6(3) . . ? N31 N32 Pd2 121.5(3) . . ? N32 C33 C34 110.2(4) . . ? N32 C33 H33A 124.9 . . ? C34 C33 H33A 124.9 . . ? C33 C34 C35 104.7(4) . . ? C33 C34 H34A 127.7 . . ? C35 C34 H34A 127.7 . . ? N31 C35 C34 109.7(4) . . ? N31 C35 H35A 125.2 . . ? C34 C35 H35A 125.2 . . ? C45 N41 N42 105.7(4) . . ? C45 N41 Pt1 132.6(3) . . ? N42 N41 Pt1 121.6(3) . . ? C43 N42 N41 109.3(4) . . ? C43 N42 Pd1 129.7(3) . . ? N41 N42 Pd1 120.5(3) . . ? N42 C43 C44 109.9(4) . . ? N42 C43 H43A 125 . . ? C44 C43 H43A 125 . . ? C43 C44 C45 104.3(4) . . ? C43 C44 H44A 127.9 . . ? C45 C44 H44A 127.9 . . ? N41 C45 C44 110.8(4) . . ? N41 C45 H45A 124.6 . . ? C44 C45 H45A 124.6 . . ? C52 N51 Pd1 109.2(3) . . ? C52 N51 H51A 109.8 . . ? Pd1 N51 H51A 109.8 . . ? C52 N51 H51B 109.8 . . ? Pd1 N51 H51B 109.8 . . ? H51A N51 H51B 108.3 . . ? C53 C52 N51 110.6(4) . . ? C53 C52 H52A 109.5 . . ? N51 C52 H52A 109.5 . . ? C53 C52 H52B 109.5 . . ? N51 C52 H52B 109.5 . . ? H52A C52 H52B 108.1 . . ? C52 C53 N54 112.0(4) . . ? C52 C53 H53A 109.2 . . ? N54 C53 H53A 109.2 . . ? C52 C53 H53B 109.2 . . ? N54 C53 H53B 109.2 . . ? H53A C53 H53B 107.9 . . ? C53 N54 Pd1 110.0(3) . . ? C53 N54 H54A 109.7 . . ? Pd1 N54 H54A 109.7 . . ? C53 N54 H54B 109.7 . . ? Pd1 N54 H54B 109.7 . . ? H54A N54 H54B 108.2 . . ? C62 N61 Pd2 109.0(3) . . ? C62 N61 H61A 109.9 . . ? Pd2 N61 H61A 109.9 . . ? C62 N61 H61B 109.9 . . ? Pd2 N61 H61B 109.9 . . ? H61A N61 H61B 108.3 . . ? N61 C62 C63 109.1(4) . . ? N61 C62 H62A 109.9 . . ? C63 C62 H62A 109.9 . . ? N61 C62 H62B 109.9 . . ? C63 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? N64 C63 C62 109.3(4) . . ? N64 C63 H63A 109.8 . . ? C62 C63 H63A 109.8 . . ? N64 C63 H63B 109.8 . . ? C62 C63 H63B 109.8 . . ? H63A C63 H63B 108.3 . . ? C63 N64 Pd2 109.3(3) . . ? C63 N64 H64A 109.8 . . ? Pd2 N64 H64A 109.8 . . ? C63 N64 H64B 109.8 . . ? Pd2 N64 H64B 109.8 . . ? H64A N64 H64B 108.3 . . ? O11 N10 O13 120.9(5) . . ? O11 N10 O12 120.1(5) . . ? O13 N10 O12 119.0(5) . . ? O22 N20 O23 120.1(4) . . ? O22 N20 O21 120.7(5) . . ? O23 N20 O21 119.2(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 N42 Pd1 N11 C12 103.9(3) . . . . ? N54 Pd1 N11 C12 -79.4(3) . . . . ? N42 Pd1 N11 Pt1 -23.13(19) . . . . ? N54 Pd1 N11 Pt1 153.53(18) . . . . ? N41 Pt1 N11 C12 -103.9(3) . . . . ? N31 Pt1 N11 C12 75.1(3) . . . . ? N41 Pt1 N11 Pd1 21.94(18) . . . . ? N31 Pt1 N11 Pd1 -159.01(18) . . . . ? N32 Pd2 N21 C22 -106.2(3) . . . . ? N64 Pd2 N21 C22 77.0(3) . . . . ? N32 Pd2 N21 Pt1 22.02(19) . . . . ? N64 Pd2 N21 Pt1 -154.72(18) . . . . ? N41 Pt1 N21 C22 -76.7(3) . . . . ? N31 Pt1 N21 C22 104.3(3) . . . . ? N41 Pt1 N21 Pd2 156.18(18) . . . . ? N31 Pt1 N21 Pd2 -22.87(18) . . . . ? N11 Pt1 N31 C35 11.2(4) . . . . ? N21 Pt1 N31 C35 -168.8(4) . . . . ? N11 Pt1 N31 N32 -164.9(3) . . . . ? N21 Pt1 N31 N32 15.1(3) . . . . ? C35 N31 N32 C33 -0.8(5) . . . . ? Pt1 N31 N32 C33 176.1(3) . . . . ? C35 N31 N32 Pd2 -179.2(3) . . . . ? Pt1 N31 N32 Pd2 -2.2(4) . . . . ? N21 Pd2 N32 C33 169.7(4) . . . . ? N61 Pd2 N32 C33 -7.5(4) . . . . ? N21 Pd2 N32 N31 -12.3(3) . . . . ? N61 Pd2 N32 N31 170.5(3) . . . . ? N31 N32 C33 C34 1.2(5) . . . . ? Pd2 N32 C33 C34 179.4(3) . . . . ? N32 C33 C34 C35 -1.1(5) . . . . ? N32 N31 C35 C34 0.1(5) . . . . ? Pt1 N31 C35 C34 -176.4(3) . . . . ? C33 C34 C35 N31 0.6(5) . . . . ? N11 Pt1 N41 C45 172.4(4) . . . . ? N21 Pt1 N41 C45 -7.6(4) . . . . ? N11 Pt1 N41 N42 -11.2(3) . . . . ? N21 Pt1 N41 N42 168.8(3) . . . . ? C45 N41 N42 C43 1.5(5) . . . . ? Pt1 N41 N42 C43 -175.7(3) . . . . ? C45 N41 N42 Pd1 173.5(3) . . . . ? Pt1 N41 N42 Pd1 -3.7(4) . . . . ? N11 Pd1 N42 C43 -173.4(4) . . . . ? N51 Pd1 N42 C43 3.1(4) . . . . ? N11 Pd1 N42 N41 16.5(3) . . . . ? N51 Pd1 N42 N41 -167.1(3) . . . . ? N41 N42 C43 C44 -1.2(5) . . . . ? Pd1 N42 C43 C44 -172.2(3) . . . . ? N42 C43 C44 C45 0.3(5) . . . . ? N42 N41 C45 C44 -1.3(5) . . . . ? Pt1 N41 C45 C44 175.5(3) . . . . ? C43 C44 C45 N41 0.6(5) . . . . ? N42 Pd1 N51 C52 -171.7(3) . . . . ? N54 Pd1 N51 C52 11.7(3) . . . . ? Pd1 N51 C52 C53 -33.2(5) . . . . ? N51 C52 C53 N54 44.6(6) . . . . ? C52 C53 N54 Pd1 -33.5(5) . . . . ? N11 Pd1 N54 C53 -172.6(3) . . . . ? N51 Pd1 N54 C53 11.3(3) . . . . ? N32 Pd2 N61 C62 169.7(3) . . . . ? N64 Pd2 N61 C62 -13.6(3) . . . . ? Pd2 N61 C62 C63 37.9(4) . . . . ? N61 C62 C63 N64 -50.3(5) . . . . ? C62 C63 N64 Pd2 37.7(5) . . . . ? N21 Pd2 N64 C63 169.9(3) . . . . ? N61 Pd2 N64 C63 -13.1(3) . . . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment '- CCDC_819878_revised.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-04-01 at 11:22:59 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : 1 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# #TrackingRef '- CCDC_819878_revised.cif' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_2 _database_code_depnum_ccdc_archive 'CCDC 819878' #TrackingRef '- CCDC_819878_revised.cif' _audit_creation_date 2011-04-01T11:22:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H30 N10 Pd2 Pt, 2(N O3), 3(H2 O)' _chemical_formula_sum 'C12 H36 N12 O9 Pd2 Pt' _chemical_formula_weight 900.42 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.0711(10) _cell_length_b 18.8743(10) _cell_length_c 14.5114(8) _cell_angle_alpha 90 _cell_angle_beta 94.729(5) _cell_angle_gamma 90 _cell_volume 5478.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6511 _cell_measurement_theta_min 2.3776 _cell_measurement_theta_max 29.1206 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prisms _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 2.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3472 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.112 _exptl_absorpt_correction_T_max 0.275 _exptl_absorpt_process_details sadabs #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_unetI/netI 0.0741 _diffrn_reflns_number 12745 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 29.16 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.85 _reflns_number_total 6294 _reflns_number_gt 4700 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2010)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. ISOR and DFIX restraints were used to model the disorder of the N30 nitrate. ; _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^)+(0.0387P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6294 _refine_ls_number_parameters 346 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.483 _refine_diff_density_min -2.294 _refine_diff_density_rms 0.22 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.191949(12) 0.110571(14) 0.454788(17) 0.01431(8) Uani 1 1 d . . . Pd1 Pd 0.04336(2) 0.14768(3) 0.52162(3) 0.01517(12) Uani 1 1 d . . . Pd2 Pd 0.28005(2) -0.03038(3) 0.49243(3) 0.01736(12) Uani 1 1 d . . . N11 N 0.0988(3) 0.1448(3) 0.4118(4) 0.0175(12) Uani 1 1 d . . . H11 H 0.0798 0.1111 0.3709 0.021 Uiso 1 1 calc R . . C12 C 0.0963(3) 0.2129(4) 0.3631(5) 0.0277(18) Uani 1 1 d . . . H12A H 0.0523 0.2188 0.3294 0.042 Uiso 1 1 calc R . . H12B H 0.131 0.2141 0.3194 0.042 Uiso 1 1 calc R . . H12C H 0.1039 0.2515 0.408 0.042 Uiso 1 1 calc R . . N21 N 0.2860(2) 0.0754(3) 0.4982(4) 0.0166(12) Uani 1 1 d . . . H21 H 0.2951 0.0885 0.5597 0.02 Uiso 1 1 calc R . . C22 C 0.3395(3) 0.1038(4) 0.4453(5) 0.0300(19) Uani 1 1 d . . . H22A H 0.3829 0.0869 0.4726 0.045 Uiso 1 1 calc R . . H22B H 0.3385 0.1557 0.447 0.045 Uiso 1 1 calc R . . H22C H 0.3327 0.0876 0.381 0.045 Uiso 1 1 calc R . . N31 N 0.1961(3) 0.0435(3) 0.3501(4) 0.0174(12) Uani 1 1 d . . . N32 N 0.2313(3) -0.0183(3) 0.3666(4) 0.0172(12) Uani 1 1 d . . . C33 C 0.2266(3) -0.0561(4) 0.2884(5) 0.0259(17) Uani 1 1 d . . . H33A H 0.2475 -0.1006 0.2804 0.031 Uiso 1 1 calc R . . C34 C 0.1870(3) -0.0210(4) 0.2212(5) 0.0240(17) Uani 1 1 d . . . H34A H 0.1748 -0.0361 0.1596 0.029 Uiso 1 1 calc R . . C35 C 0.1691(3) 0.0413(4) 0.2635(4) 0.0206(15) Uani 1 1 d . . . H35A H 0.1414 0.0771 0.2346 0.025 Uiso 1 1 calc R . . N41 N 0.1859(3) 0.1751(3) 0.5619(4) 0.0207(13) Uani 1 1 d . . . N42 N 0.1247(3) 0.1868(3) 0.5947(3) 0.0157(12) Uani 1 1 d . . . C43 C 0.1346(3) 0.2236(4) 0.6716(4) 0.0229(16) Uani 1 1 d . . . H43A H 0.1004 0.2395 0.7079 0.027 Uiso 1 1 calc R . . C44 C 0.2025(4) 0.2357(4) 0.6920(5) 0.0262(17) Uani 1 1 d . . . H44A H 0.2236 0.2602 0.7437 0.031 Uiso 1 1 calc R . . C45 C 0.2325(3) 0.2041(4) 0.6201(4) 0.0221(16) Uani 1 1 d . . . H45A H 0.2792 0.2033 0.6134 0.026 Uiso 1 1 calc R . . N51 N 0.3335(3) -0.0430(3) 0.6158(4) 0.0287(15) Uani 1 1 d . . . H51A H 0.3782 -0.0362 0.609 0.034 Uiso 1 1 calc R . . H51B H 0.3202 -0.01 0.6573 0.034 Uiso 1 1 calc R . . C52 C 0.3226(4) -0.1151(4) 0.6510(5) 0.0314(19) Uani 1 1 d . . . H52A H 0.2793 -0.1175 0.6789 0.038 Uiso 1 1 calc R . . H52B H 0.3586 -0.1275 0.6991 0.038 Uiso 1 1 calc R . . C53 C 0.3227(4) -0.1655(4) 0.5727(5) 0.0306(18) Uani 1 1 d . . . H53A H 0.3104 -0.2135 0.593 0.037 Uiso 1 1 calc R . . H53B H 0.3678 -0.1678 0.55 0.037 Uiso 1 1 calc R . . N54 N 0.2733(3) -0.1403(3) 0.4977(4) 0.0222(13) Uani 1 1 d . . . H54A H 0.2308 -0.1536 0.5098 0.027 Uiso 1 1 calc R . . H54B H 0.2825 -0.1596 0.442 0.027 Uiso 1 1 calc R . . N61 N -0.0400(3) 0.1090(3) 0.4497(4) 0.0190(12) Uani 1 1 d . . . H61A H -0.0599 0.144 0.4128 0.023 Uiso 1 1 calc R . . H61B H -0.0286 0.0723 0.4122 0.023 Uiso 1 1 calc R . . C62 C -0.0872(3) 0.0833(4) 0.5160(5) 0.0258(17) Uani 1 1 d . . . H62A H -0.0728 0.0365 0.541 0.031 Uiso 1 1 calc R . . H62B H -0.1327 0.0784 0.4845 0.031 Uiso 1 1 calc R . . C63 C -0.0876(3) 0.1362(4) 0.5922(5) 0.0282(18) Uani 1 1 d . . . H63A H -0.1085 0.1808 0.5687 0.034 Uiso 1 1 calc R . . H63B H -0.1137 0.1178 0.642 0.034 Uiso 1 1 calc R . . N64 N -0.0176(3) 0.1494(3) 0.6287(4) 0.0195(13) Uani 1 1 d . . . H64A H -0.0042 0.1152 0.6714 0.023 Uiso 1 1 calc R . . H64B H -0.0146 0.1928 0.6576 0.023 Uiso 1 1 calc R . . N10 N 0.6350(3) 0.2428(4) 0.6350(4) 0.0277(15) Uani 1 1 d . . . O11 O 0.6616(3) 0.1869(3) 0.6630(4) 0.0431(16) Uani 1 1 d . . . O12 O 0.5743(3) 0.2517(3) 0.6350(4) 0.0461(16) Uani 1 1 d . . . O13 O 0.6702(3) 0.2911(4) 0.6076(4) 0.0484(16) Uani 1 1 d . . . N20 N 0 -0.0268(5) 0.75 0.0221(19) Uani 1 2 d S . . O21 O 0 -0.0931(4) 0.75 0.0276(17) Uani 1 2 d S . . O22 O 0.0068(3) 0.0064(3) 0.6776(3) 0.0391(15) Uani 1 1 d . . . N30 N 0.0066(9) 0.3310(6) 0.7321(8) 0.046(5) Uani 0.5 1 d PDU A -1 O31 O -0.0266(11) 0.3039(8) 0.6600(9) 0.061(6) Uani 0.5 1 d PDU A -1 O32 O 0.0203(8) 0.3995(5) 0.7363(11) 0.099(7) Uani 0.5 1 d PDU A -1 O33 O 0.0229(8) 0.2937(7) 0.8069(8) 0.029(3) Uani 0.5 1 d PDU A -1 O1W O 0.3754(3) 0.1029(3) 0.6839(4) 0.0514(17) Uani 1 1 d . . . O2W O 0.5015(5) 0.1181(7) 0.6141(10) 0.164(5) Uani 1 1 d . . . O3W O -0.0283(5) 0.4454(8) 0.5611(10) 0.206(7) Uani 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 Pt1 0.01471(12) 0.01385(13) 0.01386(13) 0.00081(13) -0.00182(8) -0.00054(11) Pd1 0.0150(2) 0.0151(3) 0.0151(2) 0.0028(2) -0.00045(18) 0.0003(2) Pd2 0.0179(3) 0.0160(3) 0.0178(3) 0.0008(2) -0.00068(19) 0.0033(2) N11 0.016(3) 0.021(3) 0.016(3) 0.001(3) -0.001(2) 0.000(2) C12 0.025(4) 0.033(5) 0.025(4) 0.009(4) -0.001(3) 0.007(3) N21 0.017(3) 0.012(3) 0.021(3) 0.000(3) -0.002(2) 0.002(2) C22 0.020(4) 0.040(5) 0.030(4) 0.015(4) -0.006(3) -0.004(4) N31 0.019(3) 0.014(3) 0.018(3) -0.005(3) -0.003(2) 0.000(2) N32 0.017(3) 0.019(3) 0.016(3) -0.001(3) 0.002(2) -0.002(2) C33 0.024(4) 0.026(4) 0.027(4) -0.008(4) 0.000(3) -0.001(3) C34 0.028(4) 0.029(5) 0.015(3) -0.012(3) 0.004(3) 0.000(3) C35 0.018(3) 0.024(4) 0.019(4) -0.002(4) -0.003(3) -0.001(3) N41 0.023(3) 0.020(3) 0.020(3) -0.003(3) 0.001(2) -0.004(3) N42 0.016(3) 0.012(3) 0.018(3) 0.000(3) -0.002(2) -0.001(2) C43 0.029(4) 0.022(4) 0.018(4) -0.002(3) 0.005(3) 0.002(3) C44 0.037(4) 0.021(4) 0.019(4) -0.010(4) -0.007(3) -0.005(3) C45 0.017(3) 0.021(4) 0.026(4) -0.012(4) -0.008(3) 0.001(3) N51 0.029(3) 0.025(4) 0.031(4) -0.001(3) -0.001(3) 0.008(3) C52 0.037(4) 0.027(5) 0.029(4) 0.009(4) -0.004(3) 0.003(4) C53 0.033(4) 0.022(4) 0.037(4) 0.002(4) 0.002(3) 0.009(3) N54 0.030(3) 0.014(3) 0.023(3) 0.007(3) 0.006(2) 0.006(3) N61 0.017(3) 0.018(3) 0.021(3) 0.003(3) 0.000(2) 0.000(3) C62 0.018(4) 0.028(4) 0.031(4) 0.004(4) 0.000(3) -0.002(3) C63 0.019(4) 0.034(5) 0.034(4) 0.001(4) 0.009(3) 0.003(3) N64 0.020(3) 0.020(3) 0.018(3) -0.001(3) 0.000(2) 0.000(3) N10 0.030(4) 0.037(4) 0.015(3) 0.002(3) 0.000(2) 0.007(3) O11 0.054(4) 0.042(4) 0.033(3) 0.015(3) 0.005(3) 0.029(3) O12 0.025(3) 0.050(4) 0.064(4) 0.019(4) 0.009(3) 0.016(3) O13 0.041(4) 0.048(4) 0.056(4) 0.012(4) -0.001(3) -0.007(3) N20 0.024(4) 0.020(5) 0.020(5) 0 -0.009(3) 0 O21 0.038(4) 0.018(4) 0.024(4) 0 -0.009(3) 0 O22 0.070(4) 0.022(3) 0.025(3) 0.011(3) 0.001(3) 0.010(3) N30 0.031(8) 0.042(7) 0.066(10) -0.008(7) 0.009(7) 0.013(7) O31 0.063(8) 0.034(8) 0.084(10) 0.015(7) -0.015(8) 0.015(6) O32 0.090(11) 0.065(8) 0.140(10) 0.014(8) -0.012(8) 0.006(7) O33 0.031(6) 0.024(6) 0.032(6) 0.000(6) 0.001(5) -0.006(5) O1W 0.048(4) 0.044(4) 0.061(4) -0.010(4) 0.002(3) -0.007(3) O2W 0.058(6) 0.167(12) 0.269(15) 0.001(10) 0.025(8) -0.024(7) O3W 0.048(6) 0.287(18) 0.289(16) 0.134(14) 0.052(8) 0.045(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N31 1.985(5) . ? Pt1 N41 1.987(5) . ? Pt1 N11 2.027(5) . ? Pt1 N21 2.051(5) . ? Pt1 Pd2 3.2161(6) . ? Pd1 N42 2.012(5) . ? Pd1 N11 2.019(5) . ? Pd1 N61 2.033(5) . ? Pd1 N64 2.056(5) . ? Pd2 N21 2.002(6) . ? Pd2 N32 2.012(5) . ? Pd2 N51 2.024(6) . ? Pd2 N54 2.080(6) . ? N11 C12 1.465(9) . ? N11 H11 0.93 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? N21 C22 1.470(8) . ? N21 H21 0.93 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? N31 C35 1.328(8) . ? N31 N32 1.374(7) . ? N32 C33 1.338(8) . ? C33 C34 1.376(10) . ? C33 H33A 0.95 . ? C34 C35 1.387(10) . ? C34 H34A 0.95 . ? C35 H35A 0.95 . ? N41 C45 1.327(8) . ? N41 N42 1.371(7) . ? N42 C43 1.316(8) . ? C43 C44 1.389(9) . ? C43 H43A 0.95 . ? C44 C45 1.382(9) . ? C44 H44A 0.95 . ? C45 H45A 0.95 . ? N51 C52 1.476(9) . ? N51 H51A 0.92 . ? N51 H51B 0.92 . ? C52 C53 1.481(10) . ? C52 H52A 0.99 . ? C52 H52B 0.99 . ? C53 N54 1.490(9) . ? C53 H53A 0.99 . ? C53 H53B 0.99 . ? N54 H54A 0.92 . ? N54 H54B 0.92 . ? N61 C62 1.487(8) . ? N61 H61A 0.92 . ? N61 H61B 0.92 . ? C62 C63 1.490(10) . ? C62 H62A 0.99 . ? C62 H62B 0.99 . ? C63 N64 1.481(8) . ? C63 H63A 0.99 . ? C63 H63B 0.99 . ? N64 H64A 0.92 . ? N64 H64B 0.92 . ? N10 O12 1.231(7) . ? N10 O11 1.235(8) . ? N10 O13 1.239(8) . ? N20 O22 1.240(6) . ? N20 O22 1.241(6) 2_556 ? N20 O21 1.251(10) . ? N30 O31 1.299(9) . ? N30 O33 1.311(8) . ? N30 O32 1.322(8) . ? 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 N31 Pt1 N41 177.9(2) . . ? N31 Pt1 N11 93.6(2) . . ? N41 Pt1 N11 86.0(2) . . ? N31 Pt1 N21 86.2(2) . . ? N41 Pt1 N21 94.2(2) . . ? N11 Pt1 N21 179.7(2) . . ? N31 Pt1 Pd2 62.96(16) . . ? N41 Pt1 Pd2 116.30(16) . . ? N11 Pt1 Pd2 142.78(17) . . ? N21 Pt1 Pd2 36.96(16) . . ? N42 Pd1 N11 87.1(2) . . ? N42 Pd1 N61 178.9(2) . . ? N11 Pd1 N61 93.9(2) . . ? N42 Pd1 N64 96.0(2) . . ? N11 Pd1 N64 176.9(2) . . ? N61 Pd1 N64 83.0(2) . . ? N21 Pd2 N32 87.0(2) . . ? N21 Pd2 N51 93.1(2) . . ? N32 Pd2 N51 177.1(2) . . ? N21 Pd2 N54 175.5(2) . . ? N32 Pd2 N54 96.8(2) . . ? N51 Pd2 N54 83.2(2) . . ? N21 Pd2 Pt1 38.02(15) . . ? N32 Pd2 Pt1 62.11(16) . . ? N51 Pd2 Pt1 119.43(18) . . ? N54 Pd2 Pt1 142.57(16) . . ? C12 N11 Pd1 110.9(4) . . ? C12 N11 Pt1 115.0(4) . . ? Pd1 N11 Pt1 108.7(2) . . ? C12 N11 H11 107.3 . . ? Pd1 N11 H11 107.3 . . ? Pt1 N11 H11 107.3 . . ? N11 C12 H12A 109.5 . . ? N11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 N21 Pd2 112.7(5) . . ? C22 N21 Pt1 114.5(4) . . ? Pd2 N21 Pt1 105.0(2) . . ? C22 N21 H21 108.1 . . ? Pd2 N21 H21 108.1 . . ? Pt1 N21 H21 108.1 . . ? N21 C22 H22A 109.5 . . ? N21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C35 N31 N32 107.6(5) . . ? C35 N31 Pt1 134.8(5) . . ? N32 N31 Pt1 117.4(4) . . ? C33 N32 N31 107.8(5) . . ? C33 N32 Pd2 134.7(5) . . ? N31 N32 Pd2 117.4(4) . . ? N32 C33 C34 109.9(7) . . ? N32 C33 H33A 125 . . ? C34 C33 H33A 125 . . ? C33 C34 C35 104.5(6) . . ? C33 C34 H34A 127.7 . . ? C35 C34 H34A 127.7 . . ? N31 C35 C34 110.1(7) . . ? N31 C35 H35A 124.9 . . ? C34 C35 H35A 124.9 . . ? C45 N41 N42 108.6(5) . . ? C45 N41 Pt1 131.7(5) . . ? N42 N41 Pt1 119.0(4) . . ? C43 N42 N41 107.5(5) . . ? C43 N42 Pd1 134.5(5) . . ? N41 N42 Pd1 118.0(4) . . ? N42 C43 C44 110.2(6) . . ? N42 C43 H43A 124.9 . . ? C44 C43 H43A 124.9 . . ? C45 C44 C43 104.4(6) . . ? C45 C44 H44A 127.8 . . ? C43 C44 H44A 127.8 . . ? N41 C45 C44 109.3(6) . . ? N41 C45 H45A 125.4 . . ? C44 C45 H45A 125.4 . . ? C52 N51 Pd2 109.4(5) . . ? C52 N51 H51A 109.8 . . ? Pd2 N51 H51A 109.8 . . ? C52 N51 H51B 109.8 . . ? Pd2 N51 H51B 109.8 . . ? H51A N51 H51B 108.2 . . ? N51 C52 C53 108.5(6) . . ? N51 C52 H52A 110 . . ? C53 C52 H52A 110 . . ? N51 C52 H52B 110 . . ? C53 C52 H52B 110 . . ? H52A C52 H52B 108.4 . . ? C52 C53 N54 108.2(6) . . ? C52 C53 H53A 110.1 . . ? N54 C53 H53A 110.1 . . ? C52 C53 H53B 110.1 . . ? N54 C53 H53B 110.1 . . ? H53A C53 H53B 108.4 . . ? C53 N54 Pd2 107.7(4) . . ? C53 N54 H54A 110.2 . . ? Pd2 N54 H54A 110.2 . . ? C53 N54 H54B 110.2 . . ? Pd2 N54 H54B 110.2 . . ? H54A N54 H54B 108.5 . . ? C62 N61 Pd1 109.1(4) . . ? C62 N61 H61A 109.9 . . ? Pd1 N61 H61A 109.9 . . ? C62 N61 H61B 109.9 . . ? Pd1 N61 H61B 109.9 . . ? H61A N61 H61B 108.3 . . ? N61 C62 C63 107.7(6) . . ? N61 C62 H62A 110.2 . . ? C63 C62 H62A 110.2 . . ? N61 C62 H62B 110.2 . . ? C63 C62 H62B 110.2 . . ? H62A C62 H62B 108.5 . . ? N64 C63 C62 108.4(6) . . ? N64 C63 H63A 110 . . ? C62 C63 H63A 110 . . ? N64 C63 H63B 110 . . ? C62 C63 H63B 110 . . ? H63A C63 H63B 108.4 . . ? C63 N64 Pd1 109.5(4) . . ? C63 N64 H64A 109.8 . . ? Pd1 N64 H64A 109.8 . . ? C63 N64 H64B 109.8 . . ? Pd1 N64 H64B 109.8 . . ? H64A N64 H64B 108.2 . . ? O12 N10 O11 121.2(7) . . ? O12 N10 O13 119.4(7) . . ? O11 N10 O13 119.4(7) . . ? O22 N20 O22 119.2(9) . 2_556 ? O22 N20 O21 120.4(4) . . ? O22 N20 O21 120.4(4) 2_556 . ? O31 N30 O33 122.1(9) . . ? O31 N30 O32 120.8(9) . . ? O33 N30 O32 116.8(9) . . ? 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 N31 Pt1 Pd2 N21 123.6(3) . . . . ? N41 Pt1 Pd2 N21 -58.5(3) . . . . ? N11 Pt1 Pd2 N21 180.0(3) . . . . ? N31 Pt1 Pd2 N32 -1.8(2) . . . . ? N41 Pt1 Pd2 N32 176.0(2) . . . . ? N11 Pt1 Pd2 N32 54.5(3) . . . . ? N21 Pt1 Pd2 N32 -125.5(3) . . . . ? N31 Pt1 Pd2 N51 175.4(3) . . . . ? N41 Pt1 Pd2 N51 -6.8(3) . . . . ? N11 Pt1 Pd2 N51 -128.3(3) . . . . ? N21 Pt1 Pd2 N51 51.7(3) . . . . ? N31 Pt1 Pd2 N54 -63.7(3) . . . . ? N41 Pt1 Pd2 N54 114.1(3) . . . . ? N11 Pt1 Pd2 N54 -7.4(3) . . . . ? N21 Pt1 Pd2 N54 172.7(4) . . . . ? N42 Pd1 N11 C12 -86.6(4) . . . . ? N61 Pd1 N11 C12 93.0(4) . . . . ? N42 Pd1 N11 Pt1 40.8(3) . . . . ? N61 Pd1 N11 Pt1 -139.6(3) . . . . ? N31 Pt1 N11 C12 -100.6(5) . . . . ? N41 Pt1 N11 C12 81.5(5) . . . . ? Pd2 Pt1 N11 C12 -148.5(4) . . . . ? N31 Pt1 N11 Pd1 134.4(3) . . . . ? N41 Pt1 N11 Pd1 -43.5(3) . . . . ? Pd2 Pt1 N11 Pd1 86.4(3) . . . . ? N32 Pd2 N21 C22 -79.2(4) . . . . ? N51 Pd2 N21 C22 98.0(5) . . . . ? Pt1 Pd2 N21 C22 -125.3(5) . . . . ? N32 Pd2 N21 Pt1 46.1(2) . . . . ? N51 Pd2 N21 Pt1 -136.8(3) . . . . ? N31 Pt1 N21 C22 76.1(5) . . . . ? N41 Pt1 N21 C22 -106.0(5) . . . . ? Pd2 Pt1 N21 C22 124.1(6) . . . . ? N31 Pt1 N21 Pd2 -48.0(2) . . . . ? N41 Pt1 N21 Pd2 129.9(3) . . . . ? N11 Pt1 N31 C35 28.8(7) . . . . ? N21 Pt1 N31 C35 -151.4(7) . . . . ? Pd2 Pt1 N31 C35 178.5(7) . . . . ? N11 Pt1 N31 N32 -147.0(4) . . . . ? N21 Pt1 N31 N32 32.8(4) . . . . ? Pd2 Pt1 N31 N32 2.7(4) . . . . ? C35 N31 N32 C33 1.9(7) . . . . ? Pt1 N31 N32 C33 178.7(4) . . . . ? C35 N31 N32 Pd2 178.8(4) . . . . ? Pt1 N31 N32 Pd2 -4.3(6) . . . . ? N21 Pd2 N32 C33 148.4(6) . . . . ? N54 Pd2 N32 C33 -34.1(7) . . . . ? Pt1 Pd2 N32 C33 178.6(7) . . . . ? N21 Pd2 N32 N31 -27.5(4) . . . . ? N54 Pd2 N32 N31 150.0(4) . . . . ? Pt1 Pd2 N32 N31 2.7(4) . . . . ? N31 N32 C33 C34 -1.8(8) . . . . ? Pd2 N32 C33 C34 -178.0(5) . . . . ? N32 C33 C34 C35 1.1(8) . . . . ? N32 N31 C35 C34 -1.2(7) . . . . ? Pt1 N31 C35 C34 -177.3(5) . . . . ? C33 C34 C35 N31 0.1(8) . . . . ? N11 Pt1 N41 C45 -159.1(7) . . . . ? N21 Pt1 N41 C45 21.1(7) . . . . ? Pd2 Pt1 N41 C45 52.1(7) . . . . ? N11 Pt1 N41 N42 32.0(5) . . . . ? N21 Pt1 N41 N42 -147.8(5) . . . . ? Pd2 Pt1 N41 N42 -116.9(4) . . . . ? C45 N41 N42 C43 0.9(8) . . . . ? Pt1 N41 N42 C43 172.2(5) . . . . ? C45 N41 N42 Pd1 -179.2(5) . . . . ? Pt1 N41 N42 Pd1 -7.9(6) . . . . ? N11 Pd1 N42 C43 158.7(7) . . . . ? N64 Pd1 N42 C43 -20.7(7) . . . . ? N11 Pd1 N42 N41 -21.1(5) . . . . ? N64 Pd1 N42 N41 159.5(5) . . . . ? N41 N42 C43 C44 -1.1(8) . . . . ? Pd1 N42 C43 C44 179.0(5) . . . . ? N42 C43 C44 C45 0.9(9) . . . . ? N42 N41 C45 C44 -0.3(8) . . . . ? Pt1 N41 C45 C44 -170.2(5) . . . . ? C43 C44 C45 N41 -0.3(9) . . . . ? N21 Pd2 N51 C52 162.3(5) . . . . ? N54 Pd2 N51 C52 -15.0(5) . . . . ? Pt1 Pd2 N51 C52 133.3(4) . . . . ? Pd2 N51 C52 C53 41.1(7) . . . . ? N51 C52 C53 N54 -53.3(8) . . . . ? C52 C53 N54 Pd2 39.1(7) . . . . ? N32 Pd2 N54 C53 163.8(4) . . . . ? N51 Pd2 N54 C53 -13.3(4) . . . . ? Pt1 Pd2 N54 C53 -144.5(4) . . . . ? N11 Pd1 N61 C62 163.2(5) . . . . ? N64 Pd1 N61 C62 -17.4(5) . . . . ? Pd1 N61 C62 C63 42.2(6) . . . . ? N61 C62 C63 N64 -51.9(8) . . . . ? C62 C63 N64 Pd1 36.7(7) . . . . ? N42 Pd1 N64 C63 168.9(5) . . . . ? N61 Pd1 N64 C63 -10.7(5) . . . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF