Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Waldemar Priebe' 'Romana Anulewicz-Ostrowska' 'E. Bednarek' 'W. Bocian' 'I. Fokt' 'Leon Fuks' 'Lech Kozerski' 'H. Lewandowska' 'W. Lewandowski' A.P.Mazurek 'T. Przewloka' 'K. Samochocka' 'Jerzy Sitkowski' _publ_contact_author_name 'Prof Waldemar Priebe' _publ_contact_author_address ; The University of Texas M. D. Anderson Cancer Center 1515 Holcombe Blvd., Box 422 Houston TX 77030 UNITED STATES OF AMERICA ; _publ_contact_author_email 'WP@WT.NET ' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Platinum (II) and Palladium(II) Complexes with Methyl 3,4-diamino-2,3,4,6-tetradeoxy-a-L-lyxo-hexopyranoside ; data_cis-PT(II) _database_code_CSD 161953 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; cis-PT(II) complex with methyl-3,4-diamino-2,3,4,6-tetradeoxy- alpha-L-lyxo-heksopyranoside with ethanol (2:1) ; _chemical_formula_sum 'C16 H38 Cl4 N4 O5 Pt2' _chemical_formula_weight 898.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 ORTHORHOMBIC _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.823(2) _cell_length_b 7.827(2) _cell_length_c 43.999(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2694.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISMATIC _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 10.803 _exptl_absorpt_correction_type NUMERICAL _exptl_absorpt_correction_T_min 0.363 _exptl_absorpt_correction_T_max 0.522 _exptl_absorpt_process_details ? _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 KM4CCD _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean 1024 _diffrn_standards_number '1 FRAME' _diffrn_standards_interval_count '50 FRAME' _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 17915 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 28.96 _reflns_number_total 6468 _reflns_number_gt 6198 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrysAlisCCD _computing_cell_refinement CrysAlisRED _computing_data_reduction CrysAlisRED _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-93 _computing_publication_material SHELXTL-97 _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^)+(0.0314P)^2^+19.5064P] 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 SHELXL _refine_ls_extinction_coef 0.00075(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.041(14) _refine_ls_number_reflns 6468 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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 0.16853(4) 0.62283(4) 0.872204(8) 0.02739(10) Uani 1 1 d . . . Cl11 Cl 0.3284(4) 0.7455(4) 0.91045(6) 0.0389(6) Uani 1 1 d . . . Cl12 Cl 0.0219(4) 0.4492(3) 0.90532(6) 0.0382(6) Uani 1 1 d . . . N1 N 0.0371(12) 0.5276(11) 0.83563(18) 0.0313(18) Uani 1 1 d . . . H1A H 0.0700 0.4193 0.8320 0.038 Uiso 1 1 calc R . . H1B H -0.0757 0.5272 0.8397 0.038 Uiso 1 1 calc R . . N2 N 0.2842(11) 0.7689(11) 0.84015(18) 0.0304(17) Uani 1 1 d . . . H2A H 0.2404 0.8752 0.8404 0.036 Uiso 1 1 calc R . . H2B H 0.3970 0.7758 0.8440 0.036 Uiso 1 1 calc R . . O11 O 0.1538(11) 0.4015(10) 0.77512(19) 0.0435(18) Uani 1 1 d . . . C11 C 0.3301(16) 0.4537(16) 0.7753(2) 0.040(3) Uani 1 1 d . . . H11 H 0.4028 0.3523 0.7733 0.13(8) Uiso 1 1 calc R . . C21 C 0.3731(16) 0.5440(15) 0.8042(2) 0.040(2) Uani 1 1 d . . . H211 H 0.3660 0.4639 0.8210 0.05(4) Uiso 1 1 calc R . . H212 H 0.4897 0.5857 0.8032 0.04(3) Uiso 1 1 calc R . . C31 C 0.2557(13) 0.6900(13) 0.8100(2) 0.032(2) Uani 1 1 d . . . H31 H 0.2753 0.7769 0.7944 0.04(3) Uiso 1 1 calc R . . C41 C 0.0707(12) 0.6341(12) 0.8084(2) 0.0286(19) Uani 1 1 d . . . H41 H -0.0025 0.7356 0.8091 0.02(3) Uiso 1 1 calc R . . C51 C 0.0377(14) 0.5400(15) 0.7788(2) 0.036(2) Uani 1 1 d . . . H51 H 0.0534 0.6200 0.7619 0.10(7) Uiso 1 1 calc R . . C61 C 0.350(3) 0.490(3) 0.7223(3) 0.070(5) Uani 1 1 d . . . H611 H 0.3755 0.5744 0.7072 0.07(5) Uiso 1 1 calc R . . H612 H 0.2359 0.4485 0.7195 0.10(7) Uiso 1 1 calc R . . H613 H 0.4294 0.3968 0.7206 0.17(12) Uiso 1 1 calc R . . O21 O 0.3650(12) 0.5644(12) 0.75160(18) 0.051(2) Uani 1 1 d . . . C71 C -0.1420(17) 0.462(2) 0.7766(4) 0.059(4) Uani 1 1 d . . . H711 H -0.1543 0.4050 0.7574 0.06(4) Uiso 1 1 calc R . . H712 H -0.2259 0.5512 0.7782 0.09(6) Uiso 1 1 calc R . . H713 H -0.1581 0.3816 0.7928 0.13(9) Uiso 1 1 calc R . . Pt2 Pt 0.87274(4) 0.91855(4) 0.877789(8) 0.02744(10) Uani 1 1 d . . . Cl21 Cl 0.9954(4) 1.0784(3) 0.83945(6) 0.0390(6) Uani 1 1 d . . . Cl22 Cl 0.6991(3) 0.7722(4) 0.84464(6) 0.0389(6) Uani 1 1 d . . . N3 N 1.0174(14) 1.0341(11) 0.90999(18) 0.0324(19) Uani 1 1 d . . . H3A H 1.1241 0.9910 0.9096 0.039 Uiso 1 1 calc R . . H3B H 1.0238 1.1468 0.9061 0.039 Uiso 1 1 calc R . . N4 N 0.7793(12) 0.7883(11) 0.91368(17) 0.0304(18) Uani 1 1 d . . . H4A H 0.6705 0.8202 0.9171 0.037 Uiso 1 1 calc R . . H4B H 0.7799 0.6757 0.9095 0.037 Uiso 1 1 calc R . . O12 O 0.6517(11) 0.9041(10) 0.97489(18) 0.0435(18) Uani 1 1 d . . . C12 C 0.7055(18) 1.0796(15) 0.9747(3) 0.045(3) Uani 1 1 d . . . H12 H 0.6040 1.1518 0.9769 0.07(5) Uiso 1 1 calc R . . C22 C 0.7908(17) 1.1241(14) 0.9452(2) 0.039(2) Uani 1 1 d . . . H221 H 0.8295 1.2418 0.9456 0.18(12) Uiso 1 1 calc R . . H222 H 0.7103 1.1117 0.9285 0.19(12) Uiso 1 1 calc R . . C32 C 0.9411(15) 1.0063(12) 0.9404(2) 0.030(2) Uani 1 1 d . . . H32 H 1.0273 1.0269 0.9562 0.04(3) Uiso 1 1 calc R . . C42 C 0.8846(14) 0.8217(12) 0.9415(2) 0.032(2) Uani 1 1 d . . . H42 H 0.9864 0.7489 0.9407 0.02(3) Uiso 1 1 calc R . . C52 C 0.7910(16) 0.7868(13) 0.9713(3) 0.037(2) Uani 1 1 d . . . H52 H 0.8712 0.8026 0.9881 0.04(3) Uiso 1 1 calc R . . C62 C 0.736(3) 1.098(2) 1.0279(3) 0.076(5) Uani 1 1 d . . . H621 H 0.8180 1.1240 1.0435 0.08(6) Uiso 1 1 calc R . . H622 H 0.6957 0.9834 1.0304 0.06(5) Uiso 1 1 calc R . . H623 H 0.6418 1.1762 1.0293 0.11(8) Uiso 1 1 calc R . . O22 O 0.8161(13) 1.1152(11) 0.99859(18) 0.052(2) Uani 1 1 d . . . C72 C 0.714(2) 0.6080(17) 0.9734(3) 0.057(4) Uani 1 1 d . . . H721 H 0.6580 0.5948 0.9926 2(2) Uiso 1 1 calc R . . H722 H 0.8039 0.5246 0.9716 0.14(10) Uiso 1 1 calc R . . H723 H 0.6335 0.5920 0.9572 0.04(3) Uiso 1 1 calc R . . O3 O -0.050(2) 0.2995(18) 0.1250(5) 0.123(6) Uani 1 1 d . . . H3 H -0.0651 0.3260 0.1071 0.184 Uiso 1 1 calc R . . C8 C 0.084(2) 0.1704(17) 0.1268(5) 0.078(5) Uani 1 1 d . . . H8A H 0.0622 0.0902 0.1432 0.093 Uiso 1 1 calc R . . H8B H 0.1955 0.2220 0.1297 0.093 Uiso 1 1 calc R . . C9 C 0.070(5) 0.087(4) 0.0966(10) 0.22(2) Uani 1 1 d . . . H9A H 0.0006 -0.0141 0.0983 0.328 Uiso 1 1 calc R . . H9B H 0.1820 0.0554 0.0896 0.328 Uiso 1 1 calc R . . H9C H 0.0187 0.1642 0.0824 0.328 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02904(17) 0.02493(16) 0.02821(18) -0.00038(12) 0.00046(13) 0.00357(13) Cl11 0.0355(13) 0.0451(13) 0.0362(12) -0.0048(10) -0.0056(11) 0.0016(12) Cl12 0.0560(16) 0.0253(11) 0.0333(12) 0.0020(9) 0.0054(11) -0.0012(11) N1 0.030(4) 0.035(4) 0.029(4) -0.009(3) 0.000(3) -0.004(4) N2 0.029(4) 0.031(4) 0.031(4) -0.005(3) 0.001(3) -0.002(3) O11 0.043(4) 0.037(4) 0.051(4) -0.013(3) -0.003(4) 0.006(4) C11 0.040(6) 0.050(6) 0.031(5) -0.011(4) 0.008(5) 0.011(5) C21 0.037(6) 0.049(6) 0.036(5) -0.004(4) 0.006(5) 0.007(5) C31 0.027(5) 0.036(5) 0.033(5) 0.000(4) -0.004(4) 0.000(4) C41 0.026(4) 0.022(4) 0.038(5) -0.003(4) -0.002(4) 0.005(4) C51 0.032(5) 0.047(6) 0.029(5) -0.003(4) 0.003(4) 0.000(5) C61 0.068(11) 0.101(12) 0.042(7) -0.017(8) -0.013(7) 0.013(10) O21 0.049(5) 0.068(6) 0.035(4) -0.011(4) -0.001(4) 0.002(5) C71 0.033(6) 0.078(9) 0.066(9) -0.031(8) -0.008(6) -0.001(7) Pt2 0.02768(17) 0.02644(17) 0.02820(18) -0.00042(12) 0.00025(14) 0.00350(13) Cl21 0.0491(15) 0.0345(12) 0.0335(12) 0.0051(10) 0.0036(11) 0.0002(12) Cl22 0.0276(11) 0.0523(15) 0.0368(12) -0.0061(11) -0.0028(10) -0.0016(11) N3 0.049(5) 0.027(4) 0.021(4) 0.004(3) -0.003(4) -0.001(4) N4 0.036(4) 0.037(4) 0.019(4) 0.002(3) 0.008(3) -0.005(4) O12 0.042(4) 0.043(4) 0.046(4) 0.001(3) 0.011(4) 0.008(4) C12 0.050(7) 0.035(6) 0.050(6) 0.004(5) 0.010(6) 0.012(5) C22 0.057(7) 0.031(5) 0.030(5) -0.001(4) 0.008(5) 0.011(5) C32 0.047(6) 0.025(4) 0.019(4) 0.002(3) -0.001(4) -0.005(4) C42 0.032(5) 0.027(4) 0.038(5) 0.002(4) -0.001(4) 0.002(4) C52 0.043(6) 0.029(5) 0.040(6) 0.007(4) 0.002(5) -0.002(5) C62 0.119(16) 0.069(10) 0.039(7) -0.009(7) 0.027(9) -0.001(11) O22 0.074(6) 0.048(4) 0.034(4) -0.001(3) 0.012(4) 0.000(5) C72 0.077(10) 0.038(6) 0.056(8) 0.004(5) 0.028(7) -0.015(7) O3 0.085(10) 0.082(9) 0.202(19) 0.013(13) 0.027(14) -0.009(8) C8 0.055(8) 0.034(6) 0.144(17) 0.003(9) 0.036(11) 0.006(6) C9 0.16(3) 0.10(2) 0.40(6) -0.02(3) 0.15(4) 0.00(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N2 2.029(9) . ? Pt1 N1 2.050(8) . ? Pt1 Cl12 2.299(3) . ? Pt1 Cl11 2.306(3) . ? N1 C41 1.484(13) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C31 1.478(13) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? O11 C51 1.424(13) . ? O11 C11 1.438(15) . ? C11 O21 1.382(15) . ? C11 C21 1.497(15) . ? C11 H11 0.9800 . ? C21 C31 1.488(15) . ? C21 H211 0.9700 . ? C21 H212 0.9700 . ? C31 C41 1.513(14) . ? C31 H31 0.9800 . ? C41 C51 1.516(14) . ? C41 H41 0.9800 . ? C51 C71 1.535(17) . ? C51 H51 0.9800 . ? C61 O21 1.417(15) . ? C61 H611 0.9600 . ? C61 H612 0.9600 . ? C61 H613 0.9600 . ? C71 H711 0.9600 . ? C71 H712 0.9600 . ? C71 H713 0.9600 . ? Pt2 N4 2.017(8) . ? Pt2 N3 2.026(9) . ? Pt2 Cl22 2.299(3) . ? Pt2 Cl21 2.309(3) . ? N3 C32 1.482(12) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C42 1.497(13) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? O12 C52 1.434(14) . ? O12 C12 1.436(15) . ? C12 O22 1.391(16) . ? C12 C22 1.500(15) . ? C12 H12 0.9800 . ? C22 C32 1.509(15) . ? C22 H221 0.9700 . ? C22 H222 0.9700 . ? C32 C42 1.511(13) . ? C32 H32 0.9800 . ? C42 C52 1.526(15) . ? C42 H42 0.9800 . ? C52 C72 1.525(16) . ? C52 H52 0.9800 . ? C62 O22 1.439(15) . ? C62 H621 0.9600 . ? C62 H622 0.9600 . ? C62 H623 0.9600 . ? C72 H721 0.9600 . ? C72 H722 0.9600 . ? C72 H723 0.9600 . ? O3 C8 1.46(2) . ? O3 H3 0.8200 . ? C8 C9 1.49(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt1 N1 83.3(3) . . ? N2 Pt1 Cl12 175.1(3) . . ? N1 Pt1 Cl12 91.8(3) . . ? N2 Pt1 Cl11 91.8(2) . . ? N1 Pt1 Cl11 175.0(3) . . ? Cl12 Pt1 Cl11 93.11(11) . . ? C41 N1 Pt1 109.9(6) . . ? C41 N1 H1A 109.7 . . ? Pt1 N1 H1A 109.7 . . ? C41 N1 H1B 109.7 . . ? Pt1 N1 H1B 109.7 . . ? H1A N1 H1B 108.2 . . ? C31 N2 Pt1 108.7(6) . . ? C31 N2 H2A 110.0 . . ? Pt1 N2 H2A 110.0 . . ? C31 N2 H2B 110.0 . . ? Pt1 N2 H2B 110.0 . . ? H2A N2 H2B 108.3 . . ? C51 O11 C11 113.3(9) . . ? O21 C11 O11 111.4(10) . . ? O21 C11 C21 107.5(10) . . ? O11 C11 C21 110.7(9) . . ? O21 C11 H11 109.1 . . ? O11 C11 H11 109.1 . . ? C21 C11 H11 109.1 . . ? C31 C21 C11 111.7(10) . . ? C31 C21 H211 109.3 . . ? C11 C21 H211 109.3 . . ? C31 C21 H212 109.3 . . ? C11 C21 H212 109.3 . . ? H211 C21 H212 107.9 . . ? N2 C31 C21 112.4(9) . . ? N2 C31 C41 108.0(8) . . ? C21 C31 C41 111.1(9) . . ? N2 C31 H31 108.4 . . ? C21 C31 H31 108.4 . . ? C41 C31 H31 108.4 . . ? N1 C41 C31 107.0(8) . . ? N1 C41 C51 112.9(8) . . ? C31 C41 C51 110.2(8) . . ? N1 C41 H41 108.9 . . ? C31 C41 H41 108.9 . . ? C51 C41 H41 108.9 . . ? O11 C51 C41 111.1(9) . . ? O11 C51 C71 106.0(10) . . ? C41 C51 C71 113.8(9) . . ? O11 C51 H51 108.6 . . ? C41 C51 H51 108.6 . . ? C71 C51 H51 108.6 . . ? O21 C61 H611 109.5 . . ? O21 C61 H612 109.5 . . ? H611 C61 H612 109.5 . . ? O21 C61 H613 109.5 . . ? H611 C61 H613 109.5 . . ? H612 C61 H613 109.5 . . ? C11 O21 C61 114.2(12) . . ? C51 C71 H711 109.5 . . ? C51 C71 H712 109.5 . . ? H711 C71 H712 109.5 . . ? C51 C71 H713 109.5 . . ? H711 C71 H713 109.5 . . ? H712 C71 H713 109.5 . . ? N4 Pt2 N3 83.1(4) . . ? N4 Pt2 Cl22 91.8(3) . . ? N3 Pt2 Cl22 174.9(3) . . ? N4 Pt2 Cl21 175.2(3) . . ? N3 Pt2 Cl21 92.1(2) . . ? Cl22 Pt2 Cl21 92.99(11) . . ? C32 N3 Pt2 110.0(7) . . ? C32 N3 H3A 109.7 . . ? Pt2 N3 H3A 109.7 . . ? C32 N3 H3B 109.7 . . ? Pt2 N3 H3B 109.7 . . ? H3A N3 H3B 108.2 . . ? C42 N4 Pt2 110.6(6) . . ? C42 N4 H4A 109.5 . . ? Pt2 N4 H4A 109.5 . . ? C42 N4 H4B 109.5 . . ? Pt2 N4 H4B 109.5 . . ? H4A N4 H4B 108.1 . . ? C52 O12 C12 112.9(9) . . ? O22 C12 O12 111.6(9) . . ? O22 C12 C22 109.4(11) . . ? O12 C12 C22 111.0(10) . . ? O22 C12 H12 108.2 . . ? O12 C12 H12 108.2 . . ? C22 C12 H12 108.2 . . ? C12 C22 C32 108.9(9) . . ? C12 C22 H221 109.9 . . ? C32 C22 H221 109.9 . . ? C12 C22 H222 109.9 . . ? C32 C22 H222 109.9 . . ? H221 C22 H222 108.3 . . ? N3 C32 C22 110.4(8) . . ? N3 C32 C42 106.6(8) . . ? C22 C32 C42 110.6(10) . . ? N3 C32 H32 109.7 . . ? C22 C32 H32 109.7 . . ? C42 C32 H32 109.7 . . ? N4 C42 C32 107.6(8) . . ? N4 C42 C52 114.0(9) . . ? C32 C42 C52 109.7(8) . . ? N4 C42 H42 108.5 . . ? C32 C42 H42 108.5 . . ? C52 C42 H42 108.5 . . ? O12 C52 C72 106.4(11) . . ? O12 C52 C42 110.2(8) . . ? C72 C52 C42 113.9(9) . . ? O12 C52 H52 108.7 . . ? C72 C52 H52 108.7 . . ? C42 C52 H52 108.7 . . ? O22 C62 H621 109.5 . . ? O22 C62 H622 109.5 . . ? H621 C62 H622 109.5 . . ? O22 C62 H623 109.5 . . ? H621 C62 H623 109.5 . . ? H622 C62 H623 109.5 . . ? C12 O22 C62 112.9(13) . . ? C52 C72 H721 109.5 . . ? C52 C72 H722 109.5 . . ? H721 C72 H722 109.5 . . ? C52 C72 H723 109.5 . . ? H721 C72 H723 109.5 . . ? H722 C72 H723 109.5 . . ? C8 O3 H3 109.5 . . ? O3 C8 C9 102(2) . . ? O3 C8 H8A 111.4 . . ? C9 C8 H8A 111.4 . . ? O3 C8 H8B 111.4 . . ? C9 C8 H8B 111.4 . . ? H8A C8 H8B 109.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 C41 -10.6(6) . . . . ? Cl12 Pt1 N1 C41 168.8(6) . . . . ? Cl11 Pt1 N1 C41 -9(4) . . . . ? N1 Pt1 N2 C31 -18.3(7) . . . . ? Cl12 Pt1 N2 C31 -25(4) . . . . ? Cl11 Pt1 N2 C31 161.8(6) . . . . ? C51 O11 C11 O21 -61.5(11) . . . . ? C51 O11 C11 C21 58.1(13) . . . . ? O21 C11 C21 C31 67.3(12) . . . . ? O11 C11 C21 C31 -54.6(13) . . . . ? Pt1 N2 C31 C21 -79.5(9) . . . . ? Pt1 N2 C31 C41 43.4(9) . . . . ? C11 C21 C31 N2 173.7(9) . . . . ? C11 C21 C31 C41 52.6(13) . . . . ? Pt1 N1 C41 C31 36.5(9) . . . . ? Pt1 N1 C41 C51 157.9(7) . . . . ? N2 C31 C41 N1 -52.6(10) . . . . ? C21 C31 C41 N1 71.1(10) . . . . ? N2 C31 C41 C51 -175.7(8) . . . . ? C21 C31 C41 C51 -52.0(12) . . . . ? C11 O11 C51 C41 -58.6(12) . . . . ? C11 O11 C51 C71 177.4(10) . . . . ? N1 C41 C51 O11 -65.1(11) . . . . ? C31 C41 C51 O11 54.5(11) . . . . ? N1 C41 C51 C71 54.4(13) . . . . ? C31 C41 C51 C71 174.0(11) . . . . ? O11 C11 O21 C61 -65.8(14) . . . . ? C21 C11 O21 C61 172.7(12) . . . . ? N4 Pt2 N3 C32 -18.1(7) . . . . ? Cl22 Pt2 N3 C32 -22(4) . . . . ? Cl21 Pt2 N3 C32 162.2(6) . . . . ? N3 Pt2 N4 C42 -10.4(7) . . . . ? Cl22 Pt2 N4 C42 169.3(6) . . . . ? Cl21 Pt2 N4 C42 -6(4) . . . . ? C52 O12 C12 O22 -61.9(12) . . . . ? C52 O12 C12 C22 60.4(13) . . . . ? O22 C12 C22 C32 65.8(12) . . . . ? O12 C12 C22 C32 -57.8(14) . . . . ? Pt2 N3 C32 C22 -77.9(9) . . . . ? Pt2 N3 C32 C42 42.3(10) . . . . ? C12 C22 C32 N3 174.0(10) . . . . ? C12 C22 C32 C42 56.2(12) . . . . ? Pt2 N4 C42 C32 36.2(10) . . . . ? Pt2 N4 C42 C52 158.2(7) . . . . ? N3 C32 C42 N4 -50.8(11) . . . . ? C22 C32 C42 N4 69.3(10) . . . . ? N3 C32 C42 C52 -175.3(9) . . . . ? C22 C32 C42 C52 -55.3(11) . . . . ? C12 O12 C52 C72 177.6(10) . . . . ? C12 O12 C52 C42 -58.4(12) . . . . ? N4 C42 C52 O12 -65.5(11) . . . . ? C32 C42 C52 O12 55.3(12) . . . . ? N4 C42 C52 C72 54.0(14) . . . . ? C32 C42 C52 C72 174.8(11) . . . . ? O12 C12 O22 C62 -64.8(14) . . . . ? C22 C12 O22 C62 172.0(11) . . . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 28.96 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 1.072 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.270 data_cis-Pd_(II) _database_code_CSD 161954 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; cis-Pd (II) complex with methyl-3,4-diamino-2,3,4,6-tetradeoxy- alpha-L-lyxo-heksopyranoside with ethanol (2:1) ; _chemical_formula_sum 'C16 H38 Cl4 N4 O5 Pd2' _chemical_formula_weight 721.10 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 ORTHORHOMBIC _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.714(2) _cell_length_b 7.718(2) _cell_length_c 43.528(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2591.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISMATIC _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 1.834 _exptl_absorpt_correction_type NUMERICAL _exptl_absorpt_correction_T_min 0.427 _exptl_absorpt_correction_T_max 0.585 _exptl_absorpt_process_details ? _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 KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 1024 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count '50 frame' _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 14285 _diffrn_reflns_av_R_equivalents 0.0977 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4500 _reflns_number_gt 4412 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrysAlisCCD _computing_cell_refinement CrysAlisRED _computing_data_reduction CrysAlisRED _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-93 _computing_publication_material SHELXTL-97 _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^)+(0.1050P)^2^+19.5427P] 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 SHELXL _refine_ls_extinction_coef 0.0117(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -1.89(15) _refine_ls_number_reflns 4500 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1735 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 4.744 _refine_ls_shift/su_mean 0.235 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 1.16858(8) 0.62283(8) 0.872230(16) 0.0198(3) Uani 1 1 d . . . Cl11 Cl 1.3283(7) 0.7437(8) 0.91070(11) 0.0772(13) Uani 1 1 d . . . Cl12 Cl 1.0223(8) 0.4482(6) 0.90548(11) 0.0777(13) Uani 1 1 d . . . N1 N 1.036(2) 0.517(2) 0.8375(4) 0.073(4) Uani 1 1 d . . . H1A H 1.0724 0.4082 0.8340 0.05(4) Uiso 1 1 calc R . . H1B H 0.9219 0.5140 0.8420 0.6(6) Uiso 1 1 calc R . . N2 N 1.282(2) 0.765(2) 0.8412(3) 0.066(4) Uani 1 1 d . . . H2A H 1.2392 0.8732 0.8418 0.02(2) Uiso 1 1 calc R . . H2B H 1.3967 0.7707 0.8452 0.03(3) Uiso 1 1 calc R . . O11 O 1.1542(19) 0.3989(18) 0.7751(4) 0.090(4) Uani 1 1 d . . . C11 C 1.332(3) 0.453(3) 0.7747(5) 0.073(5) Uani 1 1 d . . . H11 H 1.4054 0.3498 0.7727 0.3(2) Uiso 1 1 calc R . . C21 C 1.370(3) 0.539(3) 0.8047(6) 0.097(7) Uani 1 1 d . . . H211 H 1.4901 0.5758 0.8048 0.07(3) Uiso 1 1 calc R . . H212 H 1.3554 0.4549 0.8211 0.2(6) Uiso 1 1 calc R . . C31 C 1.256(2) 0.692(3) 0.8110(5) 0.076(5) Uani 1 1 d . . . H31 H 1.2809 0.7820 0.7957 0.04(3) Uiso 1 1 calc R . . C41 C 1.068(2) 0.636(3) 0.8073(4) 0.062(4) Uani 1 1 d . . . H41 H 0.9936 0.7384 0.8085 0.00(2) Uiso 1 1 calc R . . C51 C 1.036(3) 0.547(3) 0.7789(4) 0.074(5) Uani 1 1 d . . . H51 H 1.0497 0.6274 0.7617 0.05(4) Uiso 1 1 calc R . . C61 C 1.335(5) 0.471(5) 0.7212(6) 0.130(13) Uani 1 1 d . . . H611 H 1.3681 0.5491 0.7051 0.12(9) Uiso 1 1 calc R . . H612 H 1.2143 0.4429 0.7192 2.0(13) Uiso 1 1 calc R . . H613 H 1.4030 0.3676 0.7200 0.5(7) Uiso 1 1 calc R . . O21 O 1.365(2) 0.558(2) 0.7521(3) 0.097(5) Uani 1 1 d . . . C71 C 0.852(3) 0.466(6) 0.7779(9) 0.148(15) Uani 1 1 d . . . H711 H 0.8343 0.4108 0.7583 0.4(3) Uiso 1 1 calc R . . H712 H 0.7664 0.5545 0.7808 2(5) Uiso 1 1 calc R . . H713 H 0.8411 0.3808 0.7939 0.2(8) Uiso 1 1 calc R . . Pd2 Pd 0.87279(8) 0.91860(8) 0.877783(16) 0.0198(3) Uani 1 1 d . . . Cl21 Cl 0.9957(8) 1.0788(7) 0.83941(11) 0.0791(13) Uani 1 1 d . . . Cl22 Cl 0.6982(7) 0.7730(8) 0.84471(12) 0.0779(13) Uani 1 1 d . . . N3 N 1.010(2) 1.028(2) 0.9094(3) 0.069(4) Uani 1 1 d . . . H3A H 1.1189 0.9878 0.9080 0.04(4) Uiso 1 1 calc R . . H3B H 1.0136 1.1428 0.9054 0.00(2) Uiso 1 1 calc R . . N4 N 0.768(2) 0.789(3) 0.9128(3) 0.075(4) Uani 1 1 d . . . H4A H 0.6589 0.8265 0.9162 0.06(5) Uiso 1 1 calc R . . H4B H 0.7640 0.6751 0.9085 0.15(13) Uiso 1 1 calc R . . O12 O 0.6473(19) 0.909(2) 0.9755(4) 0.095(5) Uani 1 1 d . . . C12 C 0.700(3) 1.075(2) 0.9742(5) 0.072(5) Uani 1 1 d . . . H12 H 0.5970 1.1478 0.9766 0.23(19) Uiso 1 1 calc R . . C22 C 0.783(3) 1.122(3) 0.9444(5) 0.084(6) Uani 1 1 d . . . H221 H 0.8152 1.2433 0.9445 0.19(14) Uiso 1 1 calc R . . H222 H 0.7035 1.1017 0.9276 1.7(12) Uiso 1 1 calc R . . C32 C 0.951(3) 1.005(2) 0.9403(4) 0.085(7) Uani 1 1 d . . . H32 H 1.0410 1.0304 0.9556 0.00(2) Uiso 1 1 calc R . . C42 C 0.885(3) 0.822(2) 0.9423(4) 0.064(4) Uani 1 1 d . . . H42 H 0.9853 0.7453 0.9408 0.01(3) Uiso 1 1 calc R . . C52 C 0.799(3) 0.784(2) 0.9712(5) 0.074(5) Uani 1 1 d . . . H52 H 0.8818 0.8071 0.9878 0.01(2) Uiso 1 1 calc R . . C62 C 0.736(5) 1.090(4) 1.0291(7) 0.117(10) Uani 1 1 d . . . H621 H 0.8243 1.1141 1.0441 0.12(11) Uiso 1 1 calc R . . H622 H 0.6960 0.9729 1.0317 0.6(9) Uiso 1 1 calc R . . H623 H 0.6410 1.1684 1.0319 2(5) Uiso 1 1 calc R . . O22 O 0.808(2) 1.111(2) 0.9981(4) 0.101(5) Uani 1 1 d . . . C72 C 0.727(6) 0.595(4) 0.9760(9) 0.138(16) Uani 1 1 d . . . H721 H 0.6773 0.5857 0.9961 2(6) Uiso 1 1 calc R . . H722 H 0.8206 0.5139 0.9740 2(6) Uiso 1 1 calc R . . H723 H 0.6403 0.5713 0.9608 0.20(12) Uiso 1 1 calc R . . O3 O -0.039(6) 0.289(4) 0.1291(9) 0.62(9) Uiso 1 1 d R . . H111 H -0.0802 0.3717 0.1384 2.0(17) Uiso 1 1 calc R . . C8 C 0.076(12) 0.384(8) 0.0816(15) 0.47(8) Uiso 1 1 d . . . H81 H 0.0076 0.4646 0.0696 2(6) Uiso 1 1 calc R . . H82 H 0.2004 0.4017 0.0804 0.01(2) Uiso 1 1 calc R . . C9 C 0.000(11) 0.166(10) 0.0843(18) 0.8(2) Uiso 1 1 d . . . H91 H 0.0925 0.0928 0.0914 0.00(2) Uiso 1 1 calc R . . H92 H -0.0380 0.1275 0.0644 0.9(5) Uiso 1 1 calc R . . H93 H -0.0947 0.1608 0.0985 0.9(5) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0211(4) 0.0171(4) 0.0212(4) 0.0002(3) 0.0003(3) 0.0037(3) Cl11 0.072(3) 0.090(3) 0.070(3) -0.008(2) -0.007(2) 0.002(3) Cl12 0.101(4) 0.059(2) 0.073(3) 0.002(2) 0.010(3) 0.001(3) N1 0.064(9) 0.068(9) 0.086(11) -0.015(8) 0.005(8) -0.002(8) N2 0.059(8) 0.062(9) 0.076(9) -0.012(8) -0.002(7) 0.002(8) O11 0.082(9) 0.068(8) 0.121(11) -0.022(7) -0.010(8) -0.002(8) C11 0.060(11) 0.084(13) 0.074(12) 0.004(10) 0.010(9) 0.018(10) C21 0.056(11) 0.128(18) 0.107(16) -0.032(14) 0.000(11) 0.030(12) C31 0.057(10) 0.062(11) 0.109(16) 0.003(11) -0.016(10) -0.008(9) C41 0.054(9) 0.064(10) 0.069(10) 0.004(9) 0.001(7) 0.006(9) C51 0.067(11) 0.088(13) 0.065(11) 0.001(10) 0.010(9) 0.021(11) C61 0.11(3) 0.20(3) 0.084(16) -0.014(19) -0.020(16) 0.08(3) O21 0.092(10) 0.131(13) 0.068(8) -0.012(9) 0.006(7) 0.009(12) C71 0.111(17) 0.21(4) 0.12(2) -0.09(3) -0.038(17) -0.02(2) Pd2 0.0202(4) 0.0182(4) 0.0209(4) -0.0001(3) -0.0002(3) 0.0037(3) Cl21 0.095(3) 0.068(3) 0.075(3) 0.007(2) 0.009(3) -0.001(3) Cl22 0.063(3) 0.096(3) 0.074(3) -0.008(3) -0.003(2) 0.000(3) N3 0.084(11) 0.058(8) 0.064(8) 0.002(7) 0.004(8) 0.000(8) N4 0.069(10) 0.096(13) 0.059(9) -0.002(8) 0.011(8) -0.006(9) O12 0.070(9) 0.093(11) 0.122(12) 0.017(9) 0.015(8) 0.000(9) C12 0.077(12) 0.042(8) 0.098(14) -0.001(8) -0.004(11) 0.016(9) C22 0.121(17) 0.061(11) 0.070(11) -0.014(9) 0.012(11) 0.031(12) C32 0.15(2) 0.055(10) 0.053(10) 0.012(8) -0.009(11) -0.021(12) C42 0.078(11) 0.056(9) 0.060(10) -0.006(7) -0.005(9) 0.005(9) C52 0.082(13) 0.048(9) 0.092(13) -0.004(9) -0.001(11) 0.004(10) C62 0.15(3) 0.095(19) 0.11(2) 0.003(16) 0.03(2) 0.040(19) O22 0.130(14) 0.085(10) 0.086(10) 0.003(8) 0.006(10) 0.025(12) C72 0.20(5) 0.07(2) 0.14(3) -0.011(19) 0.07(3) -0.01(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 Pd1 N2 1.950(16) . ? Pd1 N1 2.001(16) . ? Pd1 Cl11 2.279(5) . ? Pd1 Cl12 2.277(5) . ? Pd1 Pd2 3.2367(10) . ? N1 C41 1.62(2) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C31 1.44(2) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? O11 C51 1.47(2) . ? O11 C11 1.43(2) . ? C11 O21 1.30(2) . ? C11 C21 1.49(3) . ? C11 H11 0.9800 . ? C21 C31 1.50(3) . ? C21 H211 0.9700 . ? C21 H212 0.9700 . ? C31 C41 1.52(2) . ? C31 H31 0.9800 . ? C41 C51 1.44(3) . ? C41 H41 0.9800 . ? C51 C71 1.55(3) . ? C51 H51 0.9800 . ? C61 O21 1.52(3) . ? C61 H611 0.9600 . ? C61 H612 0.9600 . ? C61 H613 0.9600 . ? C71 H711 0.9600 . ? C71 H712 0.9600 . ? C71 H713 0.9600 . ? Pd2 N3 1.931(16) . ? Pd2 N4 1.994(15) . ? Pd2 Cl22 2.269(5) . ? Pd2 Cl21 2.284(5) . ? N3 C32 1.43(2) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C42 1.59(2) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? O12 C12 1.34(2) . ? O12 C52 1.53(2) . ? C12 O22 1.36(3) . ? C12 C22 1.49(3) . ? C12 H12 0.9800 . ? C22 C32 1.59(3) . ? C22 H221 0.9700 . ? C22 H222 0.9700 . ? C32 C42 1.50(3) . ? C32 H32 0.9800 . ? C42 C52 1.45(3) . ? C42 H42 0.9800 . ? C52 C72 1.57(4) . ? C52 H52 0.9800 . ? C62 O22 1.47(3) . ? C62 H621 0.9600 . ? C62 H622 0.9600 . ? C62 H623 0.9600 . ? C72 H721 0.9600 . ? C72 H722 0.9600 . ? C72 H723 0.9600 . ? O3 C8 2.37(8) . ? O3 H111 0.8200 . ? C8 C9 1.78(10) . ? C8 H81 0.9700 . ? C8 H82 0.9700 . ? C9 H91 0.9600 . ? C9 H92 0.9600 . ? C9 H93 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd1 N1 86.3(7) . . ? N2 Pd1 Cl11 92.0(4) . . ? N1 Pd1 Cl11 178.0(5) . . ? N2 Pd1 Cl12 175.5(5) . . ? N1 Pd1 Cl12 89.2(5) . . ? Cl11 Pd1 Cl12 92.5(2) . . ? N2 Pd1 Pd2 88.4(5) . . ? N1 Pd1 Pd2 89.0(5) . . ? Cl11 Pd1 Pd2 92.15(14) . . ? Cl12 Pd1 Pd2 91.18(15) . . ? C41 N1 Pd1 107.6(11) . . ? C41 N1 H1A 110.2 . . ? Pd1 N1 H1A 110.1 . . ? C41 N1 H1B 110.3 . . ? Pd1 N1 H1B 110.2 . . ? H1A N1 H1B 108.5 . . ? C31 N2 Pd1 110.4(13) . . ? C31 N2 H2A 109.4 . . ? Pd1 N2 H2A 109.4 . . ? C31 N2 H2B 109.7 . . ? Pd1 N2 H2B 109.7 . . ? H2A N2 H2B 108.1 . . ? C51 O11 C11 111.8(16) . . ? O21 C11 O11 112.3(18) . . ? O21 C11 C21 110(2) . . ? O11 C11 C21 108.0(17) . . ? O21 C11 H11 108.7 . . ? O11 C11 H11 108.9 . . ? C21 C11 H11 108.9 . . ? C11 C21 C31 113.2(19) . . ? C11 C21 H211 109.0 . . ? C31 C21 H211 109.0 . . ? C11 C21 H212 108.8 . . ? C31 C21 H212 109.0 . . ? H211 C21 H212 107.8 . . ? N2 C31 C41 110.0(17) . . ? N2 C31 C21 112.9(18) . . ? C41 C31 C21 108.2(17) . . ? N2 C31 H31 108.6 . . ? C41 C31 H31 108.6 . . ? C21 C31 H31 108.6 . . ? C51 C41 C31 113.3(16) . . ? C51 C41 N1 113.5(16) . . ? C31 C41 N1 103.1(15) . . ? C51 C41 H41 108.9 . . ? C31 C41 H41 109.0 . . ? N1 C41 H41 108.9 . . ? O11 C51 C71 104(2) . . ? O11 C51 C41 111.0(16) . . ? C71 C51 C41 112.4(17) . . ? O11 C51 H51 110.3 . . ? C71 C51 H51 108.4 . . ? C41 C51 H51 110.2 . . ? O21 C61 H611 109.7 . . ? O21 C61 H612 109.7 . . ? H611 C61 H612 109.5 . . ? O21 C61 H613 109.1 . . ? H611 C61 H613 109.5 . . ? H612 C61 H613 109.5 . . ? C11 O21 C61 111(2) . . ? C51 C71 H711 109.9 . . ? C51 C71 H712 111.2 . . ? H711 C71 H712 109.5 . . ? C51 C71 H713 107.3 . . ? H711 C71 H713 109.5 . . ? H712 C71 H713 109.5 . . ? N3 Pd2 N4 84.2(7) . . ? N3 Pd2 Cl22 173.9(5) . . ? N4 Pd2 Cl22 89.7(5) . . ? N3 Pd2 Cl21 93.2(5) . . ? N4 Pd2 Cl21 177.0(6) . . ? Cl22 Pd2 Cl21 92.9(2) . . ? N3 Pd2 Pd1 88.7(5) . . ? N4 Pd2 Pd1 89.4(6) . . ? Cl22 Pd2 Pd1 91.25(15) . . ? Cl21 Pd2 Pd1 91.98(15) . . ? C32 N3 Pd2 116.2(14) . . ? C32 N3 H3A 108.1 . . ? Pd2 N3 H3A 108.2 . . ? C32 N3 H3B 108.5 . . ? Pd2 N3 H3B 108.2 . . ? H3A N3 H3B 107.3 . . ? C42 N4 Pd2 107.8(12) . . ? C42 N4 H4A 110.2 . . ? Pd2 N4 H4A 110.1 . . ? C42 N4 H4B 110.1 . . ? Pd2 N4 H4B 110.2 . . ? H4A N4 H4B 108.5 . . ? C12 O12 C52 111.4(16) . . ? O22 C12 O12 110.6(17) . . ? O22 C12 C22 110.3(19) . . ? O12 C12 C22 113.5(18) . . ? O22 C12 H12 107.4 . . ? O12 C12 H12 107.2 . . ? C22 C12 H12 107.6 . . ? C12 C22 C32 108.1(16) . . ? C12 C22 H221 109.9 . . ? C32 C22 H221 110.2 . . ? C12 C22 H222 110.1 . . ? C32 C22 H222 110.0 . . ? H221 C22 H222 108.5 . . ? C42 C32 N3 106.2(15) . . ? C42 C32 C22 104.4(19) . . ? N3 C32 C22 107.0(16) . . ? C42 C32 H32 113.0 . . ? N3 C32 H32 112.8 . . ? C22 C32 H32 112.9 . . ? C32 C42 C52 113.3(15) . . ? C32 C42 N4 107.3(15) . . ? C52 C42 N4 114.1(17) . . ? C32 C42 H42 107.1 . . ? C52 C42 H42 107.4 . . ? N4 C42 H42 107.1 . . ? C42 C52 O12 109.0(16) . . ? C42 C52 C72 117.6(19) . . ? O12 C52 C72 108(2) . . ? C42 C52 H52 107.2 . . ? O12 C52 H52 107.2 . . ? C72 C52 H52 107.8 . . ? O22 C62 H621 109.7 . . ? O22 C62 H622 108.9 . . ? H621 C62 H622 109.5 . . ? O22 C62 H623 109.8 . . ? H621 C62 H623 109.5 . . ? H622 C62 H623 109.5 . . ? C12 O22 C62 116(2) . . ? C52 C72 H721 109.0 . . ? C52 C72 H722 109.7 . . ? H721 C72 H722 109.5 . . ? C52 C72 H723 109.7 . . ? H721 C72 H723 109.5 . . ? H722 C72 H723 109.5 . . ? C8 O3 H111 108.5 . . ? C9 C8 O3 62(4) . . ? C9 C8 H81 118.3 . . ? O3 C8 H81 118.5 . . ? C9 C8 H82 116.3 . . ? O3 C8 H82 117.2 . . ? H81 C8 H82 114.7 . . ? C8 C9 H91 110.5 . . ? C8 C9 H92 110.0 . . ? H91 C9 H92 109.5 . . ? C8 C9 H93 108.0 . . ? H91 C9 H93 109.5 . . ? H92 C9 H93 109.5 . . ? 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 C41 -12.0(11) . . . . ? Cl11 Pd1 N1 C41 -48(16) . . . . ? Cl12 Pd1 N1 C41 167.6(11) . . . . ? Pd2 Pd1 N1 C41 76.4(11) . . . . ? N1 Pd1 N2 C31 -16.5(13) . . . . ? Cl11 Pd1 N2 C31 162.3(12) . . . . ? Cl12 Pd1 N2 C31 -20(8) . . . . ? Pd2 Pd1 N2 C31 -105.6(12) . . . . ? C51 O11 C11 O21 -61(2) . . . . ? C51 O11 C11 C21 61(2) . . . . ? O21 C11 C21 C31 64(3) . . . . ? O11 C11 C21 C31 -59(3) . . . . ? Pd1 N2 C31 C41 43.7(18) . . . . ? Pd1 N2 C31 C21 -77.2(19) . . . . ? C11 C21 C31 N2 174.5(19) . . . . ? C11 C21 C31 C41 53(3) . . . . ? N2 C31 C41 C51 -174.3(17) . . . . ? C21 C31 C41 C51 -51(2) . . . . ? N2 C31 C41 N1 -51.3(19) . . . . ? C21 C31 C41 N1 72(2) . . . . ? Pd1 N1 C41 C51 158.8(13) . . . . ? Pd1 N1 C41 C31 35.9(16) . . . . ? C11 O11 C51 C71 178(2) . . . . ? C11 O11 C51 C41 -60(2) . . . . ? C31 C41 C51 O11 54(2) . . . . ? N1 C41 C51 O11 -63(2) . . . . ? C31 C41 C51 C71 171(2) . . . . ? N1 C41 C51 C71 54(3) . . . . ? O11 C11 O21 C61 -62(2) . . . . ? C21 C11 O21 C61 177.5(19) . . . . ? N2 Pd1 Pd2 N3 -90.0(6) . . . . ? N1 Pd1 Pd2 N3 -176.3(7) . . . . ? Cl11 Pd1 Pd2 N3 2.0(5) . . . . ? Cl12 Pd1 Pd2 N3 94.5(5) . . . . ? N2 Pd1 Pd2 N4 -174.2(7) . . . . ? N1 Pd1 Pd2 N4 99.5(6) . . . . ? Cl11 Pd1 Pd2 N4 -82.2(5) . . . . ? Cl12 Pd1 Pd2 N4 10.4(5) . . . . ? N2 Pd1 Pd2 Cl22 96.1(5) . . . . ? N1 Pd1 Pd2 Cl22 9.8(5) . . . . ? Cl11 Pd1 Pd2 Cl22 -171.9(2) . . . . ? Cl12 Pd1 Pd2 Cl22 -79.36(19) . . . . ? N2 Pd1 Pd2 Cl21 3.2(4) . . . . ? N1 Pd1 Pd2 Cl21 -83.2(5) . . . . ? Cl11 Pd1 Pd2 Cl21 95.2(2) . . . . ? Cl12 Pd1 Pd2 Cl21 -172.3(2) . . . . ? N4 Pd2 N3 C32 -14.3(15) . . . . ? Cl22 Pd2 N3 C32 -14(6) . . . . ? Cl21 Pd2 N3 C32 164.2(14) . . . . ? Pd1 Pd2 N3 C32 -103.9(14) . . . . ? N3 Pd2 N4 C42 -12.2(12) . . . . ? Cl22 Pd2 N4 C42 167.8(12) . . . . ? Cl21 Pd2 N4 C42 -42(11) . . . . ? Pd1 Pd2 N4 C42 76.5(12) . . . . ? C52 O12 C12 O22 -64(2) . . . . ? C52 O12 C12 C22 60(2) . . . . ? O22 C12 C22 C32 63(2) . . . . ? O12 C12 C22 C32 -62(2) . . . . ? Pd2 N3 C32 C42 38(2) . . . . ? Pd2 N3 C32 C22 -73.3(17) . . . . ? C12 C22 C32 C42 57(2) . . . . ? C12 C22 C32 N3 169.2(17) . . . . ? N3 C32 C42 C52 -172.2(18) . . . . ? C22 C32 C42 C52 -59(2) . . . . ? N3 C32 C42 N4 -45(2) . . . . ? C22 C32 C42 N4 67.5(18) . . . . ? Pd2 N4 C42 C32 35.0(18) . . . . ? Pd2 N4 C42 C52 161.5(12) . . . . ? C32 C42 C52 O12 58(2) . . . . ? N4 C42 C52 O12 -65(2) . . . . ? C32 C42 C52 C72 -179(3) . . . . ? N4 C42 C52 C72 58(3) . . . . ? C12 O12 C52 C42 -56(2) . . . . ? C12 O12 C52 C72 175(2) . . . . ? O12 C12 O22 C62 -60(2) . . . . ? C22 C12 O22 C62 173.3(18) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.124 _refine_diff_density_min -1.236 _refine_diff_density_rms 0.241 data_cis-Pd(II) _database_code_CSD 161955 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; cis-Pd(II) complex with methyl-3,4-diamino-2,3,4,6-teradeoxy- alpha-L-lyxo-hexopyranoside with wather (1:1) ; _chemical_formula_sum 'C14 H36 Cl4 N4 O6 Pd2' _chemical_formula_weight 711.04 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 12.345(2) _cell_length_b 28.136(6) _cell_length_c 7.734(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2686.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.770 _exptl_absorpt_correction_type NUMERICAL _exptl_absorpt_correction_T_min 0.488 _exptl_absorpt_correction_T_max 0.623 _exptl_absorpt_process_details ? _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 KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 1024 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count '50 frames' _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 17973 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 28.84 _reflns_number_total 6426 _reflns_number_gt 5128 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrysAlisCCD _computing_cell_refinement CrysAlisRED _computing_data_reduction CrysAlisRED _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-93 _computing_publication_material SHELXTL-97 _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^)+(0.1153P)^2^+9.8454P] 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 SHELXL _refine_ls_extinction_coef 0.0069(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(8) _refine_ls_number_reflns 6426 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.2114 _refine_ls_wR_factor_gt 0.1932 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 Pd1 Pd 0.47644(6) 0.81286(3) 0.73598(9) 0.0422(2) Uani 1 1 d . . . Cl1 Cl 0.3609(2) 0.86126(12) 0.8901(4) 0.0626(8) Uani 1 1 d . . . Cl2 Cl 0.5464(3) 0.87502(10) 0.5769(4) 0.0615(8) Uani 1 1 d . . . N1 N 0.5795(7) 0.7664(3) 0.6222(11) 0.0442(18) Uani 1 1 d . . . H1A H 0.5580 0.7605 0.5131 0.05(3) Uiso 1 1 calc R . . H1B H 0.6467 0.7789 0.6187 0.06(4) Uiso 1 1 calc R . . N2 N 0.4231(8) 0.7538(3) 0.8672(14) 0.054(2) Uani 1 1 d . . . H2A H 0.4468 0.7548 0.9772 0.16(10) Uiso 1 1 calc R . . H2B H 0.3503 0.7534 0.8687 0.12(7) Uiso 1 1 calc R . . O11 O 0.5583(7) 0.6687(3) 0.4774(9) 0.0538(18) Uani 1 1 d . . . C11 C 0.4497(8) 0.6564(4) 0.5267(16) 0.052(2) Uani 1 1 d . . . H11 H 0.4077 0.6512 0.4209 0.05(3) Uiso 1 1 calc R . . C21 C 0.3977(9) 0.6972(4) 0.6256(17) 0.054(3) Uani 1 1 d . . . H211 H 0.3916 0.7247 0.5506 0.10(6) Uiso 1 1 calc R . . H212 H 0.3254 0.6881 0.6617 0.06(4) Uiso 1 1 calc R . . C31 C 0.4644(8) 0.7098(3) 0.7815(13) 0.043(2) Uani 1 1 d . . . H31 H 0.4645 0.6833 0.8637 0.10(6) Uiso 1 1 calc R . . C41 C 0.5800(8) 0.7212(3) 0.7254(14) 0.044(2) Uani 1 1 d . . . H41 H 0.6244 0.7260 0.8290 0.06(4) Uiso 1 1 calc R . . C51 C 0.6269(8) 0.6792(4) 0.6219(12) 0.044(2) Uani 1 1 d . . . H511 H 0.6292 0.6513 0.6975 0.02(2) Uiso 1 1 calc R . . C61 C 0.4807(16) 0.5746(5) 0.521(3) 0.086(4) Uani 1 1 d . . . H611 H 0.4781 0.5467 0.5919 0.10(6) Uiso 1 1 calc R . . H612 H 0.5532 0.5791 0.4789 0.5(4) Uiso 1 1 calc R . . H613 H 0.4324 0.5707 0.4243 0.11(7) Uiso 1 1 calc R . . O21 O 0.4484(7) 0.6151(3) 0.6201(12) 0.062(2) Uani 1 1 d . . . C71 C 0.7394(9) 0.6883(4) 0.5544(17) 0.056(3) Uani 1 1 d . . . H711 H 0.7641 0.6611 0.4910 0.008(15) Uiso 1 1 calc R . . H712 H 0.7875 0.6942 0.6496 0.10(6) Uiso 1 1 calc R . . H713 H 0.7384 0.7155 0.4795 0.20(12) Uiso 1 1 calc R . . Pd2 Pd 0.67282(6) 0.83888(3) 1.01571(9) 0.0421(2) Uani 1 1 d . . . Cl3 Cl 0.6276(3) 0.77139(10) 1.1699(4) 0.0567(7) Uani 1 1 d . . . Cl4 Cl 0.7945(2) 0.80107(9) 0.8354(4) 0.0512(6) Uani 1 1 d . . . N3 N 0.7049(7) 0.9026(3) 0.8963(12) 0.0470(19) Uani 1 1 d . . . H3A H 0.7725 0.9122 0.9221 0.10(6) Uiso 1 1 calc R . . H3B H 0.6999 0.8992 0.7809 0.11(6) Uiso 1 1 calc R . . N4 N 0.5687(8) 0.8790(3) 1.1565(11) 0.0461(19) Uani 1 1 d . . . H4A H 0.5008 0.8747 1.1173 0.05(3) Uiso 1 1 calc R . . H4B H 0.5708 0.8698 1.2679 0.12(7) Uiso 1 1 calc R . . O12 O 0.7564(7) 0.9975(3) 1.0467(10) 0.0541(18) Uani 1 1 d . . . C12 C 0.7371(10) 0.9896(3) 1.2259(15) 0.053(3) Uani 1 1 d . . . H12 H 0.8047 0.9940 1.2904 0.07(4) Uiso 1 1 calc R . . C22 C 0.6950(9) 0.9405(4) 1.2562(16) 0.053(2) Uani 1 1 d . . . H221 H 0.6750 0.9371 1.3769 0.05(3) Uiso 1 1 calc R . . H222 H 0.7521 0.9177 1.2320 0.06(4) Uiso 1 1 calc R . . C32 C 0.5974(9) 0.9290(4) 1.1441(13) 0.048(2) Uani 1 1 d . . . H32 H 0.5357 0.9487 1.1791 0.05(3) Uiso 1 1 calc R . . C42 C 0.6249(9) 0.9385(3) 0.9574(13) 0.045(2) Uani 1 1 d . . . H42 H 0.5586 0.9349 0.8889 0.07(4) Uiso 1 1 calc R . . C52 C 0.6665(10) 0.9897(4) 0.9339(15) 0.053(2) Uani 1 1 d . . . H52 H 0.6084 1.0115 0.9672 0.04(3) Uiso 1 1 calc R . . C62 C 0.6985(12) 1.0693(4) 1.305(2) 0.070(4) Uani 1 1 d . . . H621 H 0.6416 1.0893 1.3482 0.11(7) Uiso 1 1 calc R . . H622 H 0.7216 1.0807 1.1938 0.06(4) Uiso 1 1 calc R . . H623 H 0.7585 1.0699 1.3837 0.22(15) Uiso 1 1 calc R . . O22 O 0.6590(7) 1.0212(3) 1.2883(10) 0.0565(19) Uani 1 1 d . . . C72 C 0.7022(17) 1.0022(5) 0.7524(19) 0.083(5) Uani 1 1 d . . . H721 H 0.7266 1.0346 0.7497 0.10(6) Uiso 1 1 calc R . . H722 H 0.6424 0.9984 0.6743 0.24(16) Uiso 1 1 calc R . . H723 H 0.7603 0.9816 0.7180 0.10(6) Uiso 1 1 calc R . . O3 O 0.5992(9) 0.6466(5) 1.1114(16) 0.092(4) Uani 1 1 d . . . O4 O 0.9345(11) 0.9123(5) 0.979(3) 0.139(7) 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 Pd1 0.0443(4) 0.0409(4) 0.0413(4) -0.0026(3) -0.0009(3) 0.0030(3) Cl1 0.0468(14) 0.0660(18) 0.0749(19) -0.0249(14) -0.0034(13) 0.0098(12) Cl2 0.094(2) 0.0474(14) 0.0432(12) 0.0067(10) -0.0042(13) -0.0059(14) N1 0.046(5) 0.037(4) 0.050(5) 0.007(3) 0.007(4) 0.000(3) N2 0.058(6) 0.045(5) 0.059(6) -0.003(4) 0.016(5) 0.001(4) O11 0.072(5) 0.047(4) 0.042(4) 0.000(3) 0.003(3) -0.001(3) C11 0.030(4) 0.062(6) 0.062(6) -0.014(5) 0.005(4) -0.007(4) C21 0.033(5) 0.051(6) 0.077(7) -0.008(5) 0.001(5) 0.008(4) C31 0.042(5) 0.040(5) 0.046(5) 0.004(4) 0.006(4) 0.002(4) C41 0.045(5) 0.040(5) 0.047(5) 0.008(4) 0.006(4) -0.005(4) C51 0.041(5) 0.058(6) 0.033(4) 0.006(4) 0.000(4) 0.004(4) C61 0.096(11) 0.047(7) 0.114(12) -0.014(8) -0.019(11) 0.002(7) O21 0.069(5) 0.040(4) 0.076(5) 0.004(4) 0.000(4) -0.015(4) C71 0.043(5) 0.048(6) 0.076(7) -0.004(5) 0.008(5) 0.017(4) Pd2 0.0458(4) 0.0395(4) 0.0411(4) 0.0002(3) -0.0029(3) 0.0010(3) Cl3 0.0759(19) 0.0434(13) 0.0507(13) 0.0028(10) -0.0036(12) -0.0084(12) Cl4 0.0526(14) 0.0474(13) 0.0535(13) -0.0027(10) 0.0005(11) 0.0083(10) N3 0.043(5) 0.047(5) 0.052(5) 0.002(4) -0.001(4) -0.004(3) N4 0.051(5) 0.048(5) 0.039(4) 0.003(4) -0.003(4) 0.002(4) O12 0.050(4) 0.048(4) 0.065(4) 0.000(4) 0.005(4) 0.003(3) C12 0.057(6) 0.035(5) 0.066(7) -0.014(5) -0.009(5) -0.001(4) C22 0.053(6) 0.051(6) 0.054(6) 0.000(5) -0.008(5) -0.001(4) C32 0.047(5) 0.053(6) 0.043(5) -0.005(4) 0.000(4) 0.005(4) C42 0.051(5) 0.039(5) 0.046(5) -0.001(4) -0.007(4) 0.016(4) C52 0.051(6) 0.039(5) 0.069(6) 0.001(4) 0.005(5) 0.002(5) C62 0.071(9) 0.030(5) 0.109(11) -0.009(6) -0.001(7) -0.007(5) O22 0.064(5) 0.050(4) 0.056(4) -0.005(3) 0.002(4) 0.008(3) C72 0.130(15) 0.043(6) 0.076(8) 0.015(7) 0.018(10) 0.003(7) O3 0.065(6) 0.109(9) 0.102(8) -0.037(7) -0.001(6) -0.009(6) O4 0.077(8) 0.080(8) 0.26(2) -0.052(11) 0.031(12) 0.012(6) _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 2.024(8) . ? Pd1 N2 2.056(9) . ? Pd1 Cl1 2.305(3) . ? Pd1 Cl2 2.306(3) . ? N1 C41 1.503(12) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C31 1.494(13) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? O11 C51 1.433(12) . ? O11 C11 1.435(13) . ? C11 O21 1.367(15) . ? C11 C21 1.521(15) . ? C11 H11 0.9800 . ? C21 C31 1.502(16) . ? C21 H211 0.9700 . ? C21 H212 0.9700 . ? C31 C41 1.526(14) . ? C31 H31 0.9800 . ? C41 C51 1.539(15) . ? C41 H41 0.9800 . ? C51 C71 1.506(15) . ? C51 H511 0.9800 . ? C61 O21 1.434(17) . ? C61 H611 0.9600 . ? C61 H612 0.9600 . ? C61 H613 0.9600 . ? C71 H711 0.9600 . ? C71 H712 0.9600 . ? C71 H713 0.9600 . ? Pd2 N4 2.027(9) . ? Pd2 N3 2.055(9) . ? Pd2 Cl4 2.309(3) . ? Pd2 Cl3 2.311(3) . ? N3 C42 1.491(13) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C32 1.456(14) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? O12 C12 1.424(14) . ? O12 C52 1.429(15) . ? C12 O22 1.397(13) . ? C12 C22 1.497(15) . ? C12 H12 0.9800 . ? C22 C32 1.519(15) . ? C22 H221 0.9700 . ? C22 H222 0.9700 . ? C32 C42 1.507(15) . ? C32 H32 0.9800 . ? C42 C52 1.539(15) . ? C42 H42 0.9800 . ? C52 C72 1.513(17) . ? C52 H52 0.9800 . ? C62 O22 1.444(13) . ? C62 H621 0.9600 . ? C62 H622 0.9600 . ? C62 H623 0.9600 . ? C72 H721 0.9600 . ? C72 H722 0.9600 . ? C72 H723 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 83.9(3) . . ? N1 Pd1 Cl1 174.3(3) . . ? N2 Pd1 Cl1 91.4(3) . . ? N1 Pd1 Cl2 91.3(2) . . ? N2 Pd1 Cl2 175.2(3) . . ? Cl1 Pd1 Cl2 93.42(13) . . ? C41 N1 Pd1 108.6(6) . . ? C41 N1 H1A 110.0 . . ? Pd1 N1 H1A 110.0 . . ? C41 N1 H1B 110.0 . . ? Pd1 N1 H1B 110.0 . . ? H1A N1 H1B 108.4 . . ? C31 N2 Pd1 110.0(6) . . ? C31 N2 H2A 109.7 . . ? Pd1 N2 H2A 109.7 . . ? C31 N2 H2B 109.7 . . ? Pd1 N2 H2B 109.7 . . ? H2A N2 H2B 108.2 . . ? C51 O11 C11 113.2(8) . . ? O21 C11 O11 110.8(9) . . ? O21 C11 C21 111.7(10) . . ? O11 C11 C21 110.2(9) . . ? O21 C11 H11 108.0 . . ? O11 C11 H11 108.0 . . ? C21 C11 H11 108.0 . . ? C31 C21 C11 110.5(9) . . ? C31 C21 H211 109.6 . . ? C11 C21 H211 109.6 . . ? C31 C21 H212 109.6 . . ? C11 C21 H212 109.6 . . ? H211 C21 H212 108.1 . . ? N2 C31 C21 111.4(9) . . ? N2 C31 C41 105.7(8) . . ? C21 C31 C41 109.5(9) . . ? N2 C31 H31 110.1 . . ? C21 C31 H31 110.1 . . ? C41 C31 H31 110.1 . . ? N1 C41 C31 109.0(8) . . ? N1 C41 C51 112.1(8) . . ? C31 C41 C51 109.8(8) . . ? N1 C41 H41 108.7 . . ? C31 C41 H41 108.7 . . ? C51 C41 H41 108.7 . . ? O11 C51 C71 108.1(8) . . ? O11 C51 C41 110.0(8) . . ? C71 C51 C41 113.4(9) . . ? O11 C51 H511 108.4 . . ? C71 C51 H511 108.4 . . ? C41 C51 H511 108.4 . . ? O21 C61 H611 109.5 . . ? O21 C61 H612 109.5 . . ? H611 C61 H612 109.5 . . ? O21 C61 H613 109.5 . . ? H611 C61 H613 109.5 . . ? H612 C61 H613 109.5 . . ? C11 O21 C61 112.9(11) . . ? C51 C71 H711 109.5 . . ? C51 C71 H712 109.5 . . ? H711 C71 H712 109.5 . . ? C51 C71 H713 109.5 . . ? H711 C71 H713 109.5 . . ? H712 C71 H713 109.5 . . ? N4 Pd2 N3 83.0(4) . . ? N4 Pd2 Cl4 173.2(3) . . ? N3 Pd2 Cl4 90.3(3) . . ? N4 Pd2 Cl3 91.5(3) . . ? N3 Pd2 Cl3 174.4(3) . . ? Cl4 Pd2 Cl3 95.19(11) . . ? C42 N3 Pd2 108.8(6) . . ? C42 N3 H3A 109.9 . . ? Pd2 N3 H3A 109.9 . . ? C42 N3 H3B 109.9 . . ? Pd2 N3 H3B 109.9 . . ? H3A N3 H3B 108.3 . . ? C32 N4 Pd2 110.4(7) . . ? C32 N4 H4A 109.6 . . ? Pd2 N4 H4A 109.6 . . ? C32 N4 H4B 109.6 . . ? Pd2 N4 H4B 109.6 . . ? H4A N4 H4B 108.1 . . ? C12 O12 C52 116.1(9) . . ? O22 C12 O12 110.6(9) . . ? O22 C12 C22 107.2(10) . . ? O12 C12 C22 110.7(9) . . ? O22 C12 H12 109.4 . . ? O12 C12 H12 109.4 . . ? C22 C12 H12 109.4 . . ? C12 C22 C32 112.4(10) . . ? C12 C22 H221 109.1 . . ? C32 C22 H221 109.1 . . ? C12 C22 H222 109.1 . . ? C32 C22 H222 109.1 . . ? H221 C22 H222 107.8 . . ? N4 C32 C42 106.8(8) . . ? N4 C32 C22 111.1(9) . . ? C42 C32 C22 109.3(10) . . ? N4 C32 H32 109.9 . . ? C42 C32 H32 109.9 . . ? C22 C32 H32 109.9 . . ? N3 C42 C32 109.4(8) . . ? N3 C42 C52 112.1(9) . . ? C32 C42 C52 110.8(9) . . ? N3 C42 H42 108.2 . . ? C32 C42 H42 108.2 . . ? C52 C42 H42 108.2 . . ? O12 C52 C72 107.7(12) . . ? O12 C52 C42 109.4(9) . . ? C72 C52 C42 115.2(10) . . ? O12 C52 H52 108.1 . . ? C72 C52 H52 108.1 . . ? C42 C52 H52 108.1 . . ? O22 C62 H621 109.5 . . ? O22 C62 H622 109.5 . . ? H621 C62 H622 109.5 . . ? O22 C62 H623 109.5 . . ? H621 C62 H623 109.5 . . ? H622 C62 H623 109.5 . . ? C12 O22 C62 113.2(10) . . ? C52 C72 H721 109.5 . . ? C52 C72 H722 109.5 . . ? H721 C72 H722 109.5 . . ? C52 C72 H723 109.5 . . ? H721 C72 H723 109.5 . . ? H722 C72 H723 109.5 . . ? 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 C41 -14.6(7) . . . . ? Cl1 Pd1 N1 C41 20(3) . . . . ? Cl2 Pd1 N1 C41 165.5(6) . . . . ? N1 Pd1 N2 C31 -14.3(7) . . . . ? Cl1 Pd1 N2 C31 168.9(7) . . . . ? Cl2 Pd1 N2 C31 -14(5) . . . . ? C51 O11 C11 O21 -64.6(11) . . . . ? C51 O11 C11 C21 59.7(12) . . . . ? O21 C11 C21 C31 66.5(11) . . . . ? O11 C11 C21 C31 -57.2(13) . . . . ? Pd1 N2 C31 C21 -79.8(10) . . . . ? Pd1 N2 C31 C41 39.1(10) . . . . ? C11 C21 C31 N2 172.4(8) . . . . ? C11 C21 C31 C41 55.9(11) . . . . ? Pd1 N1 C41 C31 40.7(9) . . . . ? Pd1 N1 C41 C51 162.4(7) . . . . ? N2 C31 C41 N1 -52.3(11) . . . . ? C21 C31 C41 N1 67.8(10) . . . . ? N2 C31 C41 C51 -175.4(8) . . . . ? C21 C31 C41 C51 -55.3(10) . . . . ? C11 O11 C51 C71 176.4(9) . . . . ? C11 O11 C51 C41 -59.4(11) . . . . ? N1 C41 C51 O11 -64.9(11) . . . . ? C31 C41 C51 O11 56.3(10) . . . . ? N1 C41 C51 C71 56.2(11) . . . . ? C31 C41 C51 C71 177.4(8) . . . . ? O11 C11 O21 C61 -66.0(13) . . . . ? C21 C11 O21 C61 170.6(11) . . . . ? N4 Pd2 N3 C42 -8.8(7) . . . . ? Cl4 Pd2 N3 C42 170.4(6) . . . . ? Cl3 Pd2 N3 C42 -19(3) . . . . ? N3 Pd2 N4 C32 -19.3(7) . . . . ? Cl4 Pd2 N4 C32 -26(3) . . . . ? Cl3 Pd2 N4 C32 159.7(6) . . . . ? C52 O12 C12 O22 -63.0(11) . . . . ? C52 O12 C12 C22 55.7(12) . . . . ? O22 C12 C22 C32 68.2(12) . . . . ? O12 C12 C22 C32 -52.6(13) . . . . ? Pd2 N4 C32 C42 42.7(10) . . . . ? Pd2 N4 C32 C22 -76.5(9) . . . . ? C12 C22 C32 N4 171.2(9) . . . . ? C12 C22 C32 C42 53.6(12) . . . . ? Pd2 N3 C42 C32 34.5(10) . . . . ? Pd2 N3 C42 C52 157.8(7) . . . . ? N4 C32 C42 N3 -50.8(11) . . . . ? C22 C32 C42 N3 69.5(11) . . . . ? N4 C32 C42 C52 -174.8(9) . . . . ? C22 C32 C42 C52 -54.5(12) . . . . ? C12 O12 C52 C72 177.2(9) . . . . ? C12 O12 C52 C42 -56.9(11) . . . . ? N3 C42 C52 O12 -67.1(11) . . . . ? C32 C42 C52 O12 55.5(11) . . . . ? N3 C42 C52 C72 54.4(14) . . . . ? C32 C42 C52 C72 176.9(12) . . . . ? O12 C12 O22 C62 -72.8(13) . . . . ? C22 C12 O22 C62 166.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 28.84 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 2.149 _refine_diff_density_min -1.406 _refine_diff_density_rms 0.202