# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_PdL1x3H2O _database_code_depnum_ccdc_archive 'CCDC 775336' #TrackingRef '- PdLs cif file in txt format.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H14 N4 O2 Pd, 3(H2 O)' _chemical_formula_sum 'C7 H20 N4 O5 Pd' _chemical_formula_weight 346.67 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.300(2) _cell_length_b 9.177(3) _cell_length_c 18.573(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.52(2) _cell_angle_gamma 90.00 _cell_volume 1227.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 24.3 _cell_measurement_theta_max 25.0 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.530 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type AFC7S _diffrn_measurement_method 'omega/2-theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2307 _diffrn_reflns_av_R_equivalents 0.2395 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2155 _reflns_number_gt 2032 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction ? _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+1.3354P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2155 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.002 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 0.17327(3) 0.08359(2) 0.388910(12) 0.01132(14) Uani 1 1 d . . . O1 O 0.3374(3) -0.3160(3) 0.48328(13) 0.0205(5) Uani 1 1 d . . . O2 O 0.2838(4) 0.1183(3) 0.61471(13) 0.0213(5) Uani 1 1 d . . . O3 O 0.5197(4) -0.4658(4) 0.59822(16) 0.0213(6) Uani 1 1 d . . . H31 H 0.562(8) -0.535(7) 0.580(3) 0.042(15) Uiso 1 1 d . . . H32 H 0.477(8) -0.424(6) 0.577(3) 0.028(19) Uiso 1 1 d . . . O4 O 0.4612(4) 0.0125(3) 0.74470(17) 0.0261(6) Uani 1 1 d . . . H41 H 0.404(7) 0.038(5) 0.706(3) 0.024(12) Uiso 1 1 d . . . H42 H 0.396(7) -0.037(6) 0.758(3) 0.030(14) Uiso 1 1 d . . . O5 O 0.3055(4) 0.3823(4) 0.68349(16) 0.0257(6) Uani 1 1 d . . . H51 H 0.301(6) 0.308(6) 0.666(2) 0.022(12) Uiso 1 1 d . . . H52 H 0.356(7) 0.429(5) 0.660(3) 0.025(14) Uiso 1 1 d . . . N1 N 0.1494(4) 0.0131(3) 0.28314(15) 0.0171(6) Uani 1 1 d . . . H1A H 0.0644 0.0662 0.2537 0.021 Uiso 1 1 calc R . . H1B H 0.2590 0.0204 0.2672 0.021 Uiso 1 1 calc R . . N2 N 0.2230(4) -0.1252(3) 0.41167(15) 0.0144(6) Uani 1 1 d . . . N3 N 0.1929(4) 0.1431(3) 0.49232(15) 0.0147(6) Uani 1 1 d . . . N4 N 0.1313(4) 0.3023(3) 0.36973(16) 0.0166(6) Uani 1 1 d . . . H4A H 0.2394 0.3467 0.3662 0.020 Uiso 1 1 calc R . . H4B H 0.0519 0.3165 0.3278 0.020 Uiso 1 1 calc R . . C1 C 0.0899(5) -0.1421(4) 0.28405(19) 0.0205(7) Uani 1 1 d . . . H1C H 0.1019 -0.1886 0.2382 0.025 Uiso 1 1 calc R . . H1D H -0.0391 -0.1476 0.2905 0.025 Uiso 1 1 calc R . . C2 C 0.2120(5) -0.2183(4) 0.34642(18) 0.0188(7) Uani 1 1 d . . . H2A H 0.1594 -0.3124 0.3554 0.023 Uiso 1 1 calc R . . H2B H 0.3350 -0.2337 0.3346 0.023 Uiso 1 1 calc R . . C3 C 0.2897(4) -0.1827(4) 0.47543(18) 0.0148(7) Uani 1 1 d . . . C4 C 0.3161(5) -0.0916(3) 0.5444(2) 0.0169(8) Uani 1 1 d . . . H4C H 0.4479 -0.0951 0.5636 0.020 Uiso 1 1 calc R . . H4D H 0.2549 -0.1448 0.5788 0.020 Uiso 1 1 calc R . . C5 C 0.2593(5) 0.0664(4) 0.55050(19) 0.0142(7) Uani 1 1 d . . . C6 C 0.1559(5) 0.2982(4) 0.50309(19) 0.0176(7) Uani 1 1 d . . . H6A H 0.2721 0.3498 0.5176 0.021 Uiso 1 1 calc R . . H6B H 0.0820 0.3092 0.5416 0.021 Uiso 1 1 calc R . . C7 C 0.0524(5) 0.3622(4) 0.4326(2) 0.0193(7) Uani 1 1 d . . . H7A H -0.0785 0.3379 0.4274 0.023 Uiso 1 1 calc R . . H7B H 0.0640 0.4675 0.4337 0.023 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 0.0143(2) 0.0097(2) 0.0101(2) 0.00045(8) 0.00252(12) 0.00055(8) O1 0.0304(13) 0.0115(12) 0.0200(12) 0.0027(10) 0.0055(10) 0.0059(10) O2 0.0318(13) 0.0178(12) 0.0140(13) -0.0023(10) 0.0029(10) 0.0020(12) O3 0.0263(14) 0.0180(15) 0.0191(14) 0.0010(14) 0.0027(12) 0.0009(12) O4 0.0242(14) 0.0331(17) 0.0202(15) 0.0064(13) 0.0011(12) -0.0049(13) O5 0.0352(16) 0.0224(14) 0.0221(15) -0.0065(14) 0.0121(12) -0.0055(13) N1 0.0210(14) 0.0168(16) 0.0135(14) 0.0024(11) 0.0028(11) 0.0001(12) N2 0.0182(14) 0.0123(14) 0.0127(14) -0.0016(12) 0.0021(11) 0.0007(12) N3 0.0180(14) 0.0112(14) 0.0152(14) -0.0004(11) 0.0034(11) 0.0006(11) N4 0.0193(14) 0.0141(15) 0.0158(13) 0.0009(12) 0.0014(11) -0.0011(12) C1 0.0266(18) 0.0204(19) 0.0143(17) -0.0027(14) 0.0026(14) -0.0032(15) C2 0.0299(19) 0.0118(16) 0.0151(16) -0.0012(14) 0.0048(14) 0.0007(14) C3 0.0135(15) 0.0138(16) 0.0178(17) -0.0008(14) 0.0047(12) 0.0001(13) C4 0.0213(18) 0.0150(18) 0.0140(17) 0.0013(12) 0.0016(14) 0.0010(12) C5 0.0140(16) 0.0163(17) 0.0122(16) -0.0004(13) 0.0022(13) -0.0014(12) C6 0.0243(17) 0.0113(16) 0.0182(17) -0.0030(13) 0.0063(13) -0.0008(13) C7 0.0242(17) 0.0120(17) 0.0227(18) 0.0015(14) 0.0070(14) 0.0043(14) _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 N3 1.979(3) . ? Pd1 N2 1.983(3) . ? Pd1 N1 2.048(3) . ? Pd1 N4 2.053(3) . ? O1 C3 1.273(4) . ? O2 C5 1.269(4) . ? O3 H31 0.80(7) . ? O3 H32 0.60(6) . ? O4 H41 0.80(6) . ? O4 H42 0.73(6) . ? O5 H51 0.75(5) . ? O5 H52 0.75(5) . ? N1 C1 1.489(5) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C3 1.314(5) . ? N2 C2 1.474(4) . ? N3 C5 1.313(5) . ? N3 C6 1.469(4) . ? N4 C7 1.491(4) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? C1 C2 1.511(5) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.515(5) . ? C4 C5 1.517(5) . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C6 C7 1.517(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? 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 N3 Pd1 N2 94.52(11) . . ? N3 Pd1 N1 177.49(11) . . ? N2 Pd1 N1 83.26(12) . . ? N3 Pd1 N4 83.29(11) . . ? N2 Pd1 N4 177.20(11) . . ? N1 Pd1 N4 98.97(11) . . ? H31 O3 H32 115(7) . . ? H41 O4 H42 102(5) . . ? H51 O5 H52 105(5) . . ? C1 N1 Pd1 105.7(2) . . ? C1 N1 H1A 110.6 . . ? Pd1 N1 H1A 110.6 . . ? C1 N1 H1B 110.6 . . ? Pd1 N1 H1B 110.6 . . ? H1A N1 H1B 108.7 . . ? C3 N2 C2 118.0(3) . . ? C3 N2 Pd1 127.4(2) . . ? C2 N2 Pd1 113.7(2) . . ? C5 N3 C6 117.3(3) . . ? C5 N3 Pd1 127.4(2) . . ? C6 N3 Pd1 114.5(2) . . ? C7 N4 Pd1 106.9(2) . . ? C7 N4 H4A 110.3 . . ? Pd1 N4 H4A 110.3 . . ? C7 N4 H4B 110.3 . . ? Pd1 N4 H4B 110.3 . . ? H4A N4 H4B 108.6 . . ? N1 C1 C2 108.4(3) . . ? N1 C1 H1C 110.0 . . ? C2 C1 H1C 110.0 . . ? N1 C1 H1D 110.0 . . ? C2 C1 H1D 110.0 . . ? H1C C1 H1D 108.4 . . ? N2 C2 C1 107.9(3) . . ? N2 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? N2 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? O1 C3 N2 122.8(3) . . ? O1 C3 C4 116.1(3) . . ? N2 C3 C4 121.1(3) . . ? C3 C4 C5 126.3(3) . . ? C3 C4 H4C 105.7 . . ? C5 C4 H4C 105.7 . . ? C3 C4 H4D 105.7 . . ? C5 C4 H4D 105.7 . . ? H4C C4 H4D 106.2 . . ? O2 C5 N3 123.2(3) . . ? O2 C5 C4 115.5(3) . . ? N3 C5 C4 121.3(3) . . ? N3 C6 C7 109.5(3) . . ? N3 C6 H6A 109.8 . . ? C7 C6 H6A 109.8 . . ? N3 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? N4 C7 C6 109.3(3) . . ? N4 C7 H7A 109.8 . . ? C6 C7 H7A 109.8 . . ? N4 C7 H7B 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.638 _refine_diff_density_min -1.535 _refine_diff_density_rms 0.253 data_PdL2x6H2O _database_code_depnum_ccdc_archive 'CCDC 775337' #TrackingRef '- PdLs cif file in txt format.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H18 N4 O2 Pd, 6(H2 O)' _chemical_formula_sum 'C10 H30 N4 O8 Pd' _chemical_formula_weight 440.78 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.2560(2) _cell_length_b 24.9406(6) _cell_length_c 9.5763(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.208(2) _cell_angle_gamma 90.00 _cell_volume 1731.73(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 1.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8293 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34985 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.0153 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 33.14 _reflns_number_total 6523 _reflns_number_gt 6093 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+1.2653P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6523 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0627 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.561093(12) 0.198970(4) 0.353558(9) 0.01230(3) Uani 1 1 d . . . O1 O 0.47313(14) 0.33428(4) 0.59657(10) 0.01821(18) Uani 1 1 d . . . O2 O 0.48214(14) 0.33479(4) 0.10521(10) 0.01774(18) Uani 1 1 d . . . N1 N 0.60186(16) 0.14659(5) 0.51635(12) 0.01582(19) Uani 1 1 d . . . N2 N 0.51851(16) 0.25129(5) 0.50490(11) 0.01523(19) Uani 1 1 d . . . N3 N 0.51917(16) 0.25149(5) 0.19954(11) 0.01501(19) Uani 1 1 d . . . N4 N 0.59884(16) 0.14641(5) 0.19335(12) 0.01625(19) Uani 1 1 d . . . C1 C 0.4895(2) 0.16779(6) 0.63106(14) 0.0186(2) Uani 1 1 d . . . C2 C 0.52181(19) 0.22784(6) 0.64615(14) 0.0173(2) Uani 1 1 d . . . C3 C 0.49682(18) 0.30324(5) 0.49248(14) 0.0148(2) Uani 1 1 d . . . C4 C 0.5018(2) 0.33106(6) 0.35194(14) 0.0183(2) Uani 1 1 d . . . C5 C 0.50117(18) 0.30357(5) 0.21040(14) 0.0144(2) Uani 1 1 d . . . C6 C 0.52187(19) 0.22777(6) 0.05860(14) 0.0173(2) Uani 1 1 d . . . C7 C 0.4862(2) 0.16805(6) 0.07299(15) 0.0193(2) Uani 1 1 d . . . C8 C 0.5573(2) 0.08918(6) 0.22115(16) 0.0205(2) Uani 1 1 d . . . C9 C 0.6521(2) 0.06921(6) 0.35622(17) 0.0223(3) Uani 1 1 d . . . C10 C 0.5640(2) 0.08895(6) 0.48873(16) 0.0203(2) Uani 1 1 d . . . H1N H 0.716(3) 0.1490(8) 0.538(2) 0.017(5) Uiso 1 1 d . . . H3N H 0.707(3) 0.1484(8) 0.173(2) 0.018(5) Uiso 1 1 d . . . H1A H 0.366(3) 0.1613(8) 0.606(2) 0.018(5) Uiso 1 1 d . . . H1B H 0.515(3) 0.1490(9) 0.717(2) 0.026(5) Uiso 1 1 d . . . H2A H 0.427(3) 0.2431(8) 0.701(2) 0.017(4) Uiso 1 1 d . . . H2B H 0.640(3) 0.2364(8) 0.692(2) 0.021(5) Uiso 1 1 d . . . H4A H 0.397(3) 0.3559(9) 0.348(2) 0.026(5) Uiso 1 1 d . . . H4B H 0.612(3) 0.3536(10) 0.359(2) 0.028(6) Uiso 1 1 d . . . H6A H 0.640(3) 0.2350(8) 0.020(2) 0.020(5) Uiso 1 1 d . . . H6B H 0.428(3) 0.2439(9) -0.004(2) 0.027(5) Uiso 1 1 d . . . H7A H 0.358(3) 0.1625(8) 0.092(2) 0.018(5) Uiso 1 1 d . . . H7B H 0.516(3) 0.1489(8) -0.009(2) 0.021(5) Uiso 1 1 d . . . H8A H 0.595(3) 0.0675(9) 0.146(2) 0.028(6) Uiso 1 1 d . . . H8B H 0.431(3) 0.0855(9) 0.224(2) 0.026(5) Uiso 1 1 d . . . H9A H 0.651(3) 0.0323(10) 0.360(2) 0.033(6) Uiso 1 1 d . . . H9B H 0.778(3) 0.0773(9) 0.361(2) 0.026(5) Uiso 1 1 d . . . H10A H 0.431(3) 0.0849(9) 0.481(2) 0.026(5) Uiso 1 1 d . . . H10B H 0.611(3) 0.0685(9) 0.563(2) 0.031(6) Uiso 1 1 d . . . O3 O 0.6430(2) 0.35913(6) 0.85267(13) 0.0360(3) Uani 1 1 d . . . O4 O 0.36151(19) 0.51733(5) 0.17719(14) 0.0309(3) Uani 1 1 d . . . O5 O 0.61471(19) 0.43976(5) 0.11455(14) 0.0296(2) Uani 1 1 d . . . O6 O 0.8173(2) 0.44233(7) 0.36703(16) 0.0404(3) Uani 1 1 d . . . O7 O 0.5155(2) 0.44186(5) 0.56326(15) 0.0364(3) Uani 1 1 d . . . O8 O 0.1983(2) 0.44908(8) 0.37463(17) 0.0480(4) Uani 1 1 d . . . H31 H 0.5973 0.3463 0.9225 0.050 Uiso 1 1 d . . . H32 H 0.5992 0.3458 0.7806 0.050 Uiso 1 1 d . . . H41 H 0.4219 0.4974 0.1624 0.050 Uiso 0.50 1 d P . . H42 H 0.3932 0.5356 0.2257 0.050 Uiso 0.50 1 d P . . H43 H 0.3451 0.5331 0.1122 0.050 Uiso 1 1 d . . . H51 H 0.5446 0.4538 0.1218 0.050 Uiso 0.50 1 d P . . H52 H 0.6557 0.4403 0.1840 0.050 Uiso 0.50 1 d P . . H53 H 0.5735 0.4109 0.1101 0.050 Uiso 1 1 d . . . H61 H 0.9009 0.4493 0.3806 0.050 Uiso 0.50 1 d P . . H62 H 0.7562 0.4478 0.4367 0.050 Uiso 1 1 d . . . H63 H 0.7711 0.4463 0.2941 0.050 Uiso 0.50 1 d P . . H71 H 0.5200 0.4526 0.6344 0.050 Uiso 0.50 1 d P . . H73 H 0.5084 0.4089 0.5744 0.050 Uiso 1 1 d . . . H72 H 0.4172 0.4446 0.5599 0.050 Uiso 0.50 1 d P . . H81 H 0.0920 0.4546 0.3735 0.050 Uiso 0.50 1 d P . . H82 H 0.2234 0.4719 0.3184 0.050 Uiso 1 1 d . . . H83 H 0.2777 0.4534 0.4348 0.050 Uiso 0.50 1 d P . . 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 0.01195(5) 0.01355(5) 0.01144(5) -0.00037(3) 0.00116(3) 0.00032(3) O1 0.0222(5) 0.0180(4) 0.0146(4) -0.0037(3) 0.0026(3) 0.0002(3) O2 0.0197(4) 0.0190(4) 0.0146(4) 0.0032(3) 0.0006(3) -0.0005(3) N1 0.0148(5) 0.0167(5) 0.0160(5) 0.0008(4) 0.0006(4) 0.0002(4) N2 0.0174(5) 0.0169(5) 0.0115(4) -0.0002(4) 0.0022(3) 0.0012(4) N3 0.0172(5) 0.0166(5) 0.0113(4) -0.0004(4) 0.0009(3) 0.0007(4) N4 0.0160(5) 0.0162(5) 0.0167(5) -0.0019(4) 0.0032(4) -0.0003(4) C1 0.0211(6) 0.0199(6) 0.0151(5) 0.0025(4) 0.0034(4) 0.0003(5) C2 0.0194(6) 0.0207(6) 0.0118(5) 0.0008(4) 0.0013(4) 0.0016(4) C3 0.0137(5) 0.0174(6) 0.0134(5) -0.0013(4) 0.0012(4) -0.0001(4) C4 0.0257(6) 0.0154(5) 0.0140(5) -0.0005(4) 0.0014(4) 0.0002(5) C5 0.0121(5) 0.0171(6) 0.0142(5) 0.0008(4) 0.0010(4) -0.0003(4) C6 0.0198(6) 0.0200(6) 0.0122(5) -0.0016(4) 0.0011(4) 0.0014(4) C7 0.0217(6) 0.0211(6) 0.0150(5) -0.0036(4) -0.0014(4) -0.0003(5) C8 0.0253(6) 0.0160(6) 0.0205(6) -0.0032(5) 0.0037(5) -0.0018(5) C9 0.0249(7) 0.0170(6) 0.0251(7) -0.0004(5) 0.0029(5) 0.0033(5) C10 0.0244(6) 0.0160(6) 0.0206(6) 0.0020(5) 0.0015(5) -0.0013(5) O3 0.0402(7) 0.0509(8) 0.0169(5) 0.0000(5) 0.0008(5) -0.0184(6) O4 0.0332(6) 0.0256(6) 0.0343(6) 0.0075(5) 0.0086(5) 0.0023(5) O5 0.0332(6) 0.0202(5) 0.0359(6) -0.0020(4) 0.0087(5) -0.0011(4) O6 0.0381(7) 0.0476(9) 0.0360(7) 0.0022(6) 0.0087(6) -0.0025(6) O7 0.0511(8) 0.0207(6) 0.0378(7) -0.0008(5) 0.0080(6) -0.0024(5) O8 0.0385(8) 0.0641(11) 0.0414(8) 0.0209(8) 0.0013(6) -0.0119(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 1.9832(11) . ? Pd1 N3 1.9872(11) . ? Pd1 N4 2.0444(11) . ? Pd1 N1 2.0466(12) . ? O1 C3 1.2789(16) . ? O2 C5 1.2765(16) . ? N1 C10 1.4856(18) . ? N1 C1 1.4897(18) . ? N1 H1N 0.85(2) . ? N2 C3 1.3101(17) . ? N2 C2 1.4730(17) . ? N3 C5 1.3100(17) . ? N3 C6 1.4744(17) . ? N4 C8 1.4850(18) . ? N4 C7 1.4883(19) . ? N4 H3N 0.82(2) . ? C1 C2 1.522(2) . ? C1 H1A 0.93(2) . ? C1 H1B 0.96(2) . ? C2 H2A 0.96(2) . ? C2 H2B 0.97(2) . ? C3 C4 1.5159(19) . ? C4 C5 1.5189(19) . ? C4 H4A 0.98(2) . ? C4 H4B 0.98(2) . ? C6 C7 1.519(2) . ? C6 H6A 0.96(2) . ? C6 H6B 0.98(2) . ? C7 H7A 0.96(2) . ? C7 H7B 0.95(2) . ? C8 C9 1.525(2) . ? C8 H8A 0.95(2) . ? C8 H8B 0.92(2) . ? C9 C10 1.524(2) . ? C9 H9A 0.92(2) . ? C9 H9B 0.94(2) . ? C10 H10A 0.97(2) . ? C10 H10B 0.93(2) . ? O3 H31 0.82 . ? O3 H32 0.82 . ? O4 H41 0.68 . ? O4 H42 0.68 . ? O4 H43 0.74 . ? O5 H51 0.62 . ? O5 H52 0.72 . ? O5 H53 0.78 . ? O6 H61 0.64 . ? O6 H62 0.83 . ? O6 H63 0.77 . ? O7 H71 0.73 . ? O7 H73 0.83 . ? O7 H72 0.72 . ? O8 H81 0.78 . ? O8 H82 0.81 . ? O8 H83 0.81 . ? 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 N3 94.88(5) . . ? N2 Pd1 N4 178.09(5) . . ? N3 Pd1 N4 83.50(5) . . ? N2 Pd1 N1 83.41(5) . . ? N3 Pd1 N1 178.28(5) . . ? N4 Pd1 N1 98.21(5) . . ? C10 N1 C1 111.85(11) . . ? C10 N1 Pd1 117.50(9) . . ? C1 N1 Pd1 105.55(8) . . ? C10 N1 H1N 106.5(14) . . ? C1 N1 H1N 110.4(14) . . ? Pd1 N1 H1N 104.8(14) . . ? C3 N2 C2 118.28(11) . . ? C3 N2 Pd1 127.30(9) . . ? C2 N2 Pd1 114.35(9) . . ? C5 N3 C6 118.38(11) . . ? C5 N3 Pd1 127.41(9) . . ? C6 N3 Pd1 114.08(9) . . ? C8 N4 C7 112.23(11) . . ? C8 N4 Pd1 116.60(9) . . ? C7 N4 Pd1 105.26(8) . . ? C8 N4 H3N 107.7(14) . . ? C7 N4 H3N 107.1(14) . . ? Pd1 N4 H3N 107.5(14) . . ? N1 C1 C2 109.43(11) . . ? N1 C1 H1A 107.3(13) . . ? C2 C1 H1A 109.7(13) . . ? N1 C1 H1B 111.5(13) . . ? C2 C1 H1B 112.0(13) . . ? H1A C1 H1B 106.8(18) . . ? N2 C2 C1 107.85(11) . . ? N2 C2 H2A 110.7(12) . . ? C1 C2 H2A 109.4(12) . . ? N2 C2 H2B 108.2(12) . . ? C1 C2 H2B 113.0(12) . . ? H2A C2 H2B 107.7(17) . . ? O1 C3 N2 123.17(12) . . ? O1 C3 C4 115.06(11) . . ? N2 C3 C4 121.77(12) . . ? C3 C4 C5 125.89(12) . . ? C3 C4 H4A 106.1(13) . . ? C5 C4 H4A 105.9(13) . . ? C3 C4 H4B 104.7(13) . . ? C5 C4 H4B 107.0(13) . . ? H4A C4 H4B 105.7(19) . . ? O2 C5 N3 123.39(12) . . ? O2 C5 C4 115.16(11) . . ? N3 C5 C4 121.44(12) . . ? N3 C6 C7 107.58(11) . . ? N3 C6 H6A 108.9(12) . . ? C7 C6 H6A 112.0(12) . . ? N3 C6 H6B 111.5(13) . . ? C7 C6 H6B 110.0(13) . . ? H6A C6 H6B 106.8(18) . . ? N4 C7 C6 109.61(11) . . ? N4 C7 H7A 107.7(12) . . ? C6 C7 H7A 109.1(12) . . ? N4 C7 H7B 108.9(13) . . ? C6 C7 H7B 111.8(13) . . ? H7A C7 H7B 109.7(17) . . ? N4 C8 C9 112.20(12) . . ? N4 C8 H8A 110.2(14) . . ? C9 C8 H8A 109.1(14) . . ? N4 C8 H8B 107.9(14) . . ? C9 C8 H8B 111.3(14) . . ? H8A C8 H8B 106(2) . . ? C10 C9 C8 114.24(12) . . ? C10 C9 H9A 106.9(15) . . ? C8 C9 H9A 110.6(15) . . ? C10 C9 H9B 109.3(14) . . ? C8 C9 H9B 112.2(14) . . ? H9A C9 H9B 103(2) . . ? N1 C10 C9 112.34(12) . . ? N1 C10 H10A 106.9(13) . . ? C9 C10 H10A 110.6(13) . . ? N1 C10 H10B 109.6(15) . . ? C9 C10 H10B 107.9(15) . . ? H10A C10 H10B 109.5(19) . . ? H31 O3 H32 111 . . ? H41 O4 H42 115 . . ? H41 O4 H43 107 . . ? H42 O4 H43 104 . . ? H51 O5 H52 101 . . ? H51 O5 H53 102 . . ? H52 O5 H53 102 . . ? H61 O6 H62 109 . . ? H61 O6 H63 121 . . ? H62 O6 H63 119 . . ? H71 O7 H73 104 . . ? H71 O7 H72 91 . . ? H73 O7 H72 92 . . ? H81 O8 H82 97 . . ? H81 O8 H83 132 . . ? H82 O8 H83 102 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.247 _refine_diff_density_min -1.143 _refine_diff_density_rms 0.084 data_PdL3x5H2O _database_code_depnum_ccdc_archive 'CCDC 775338' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H16 N4 O2 Pd, 5(H2 O)' _chemical_formula_sum 'C9 H26 N4 O7 Pd' _chemical_formula_weight 408.74 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.144(4) _cell_length_b 7.728(4) _cell_length_c 23.565(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.11(3) _cell_angle_gamma 90.00 _cell_volume 1652.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.159 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8240 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11109 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3958 _reflns_number_gt 3723 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+1.9236P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3958 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.191 _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 0.740661(18) 0.56921(2) 0.787944(7) 0.01726(7) Uani 1 1 d . . . O1 O 0.4707(2) 0.4394(2) 0.64011(8) 0.0228(4) Uani 1 1 d . . . O2 O 0.9850(2) 0.4203(2) 0.66050(9) 0.0284(4) Uani 1 1 d . . . O3 O 0.2021(2) 0.6026(3) 0.62327(11) 0.0375(5) Uani 1 1 d . . . H31 H 0.1543 0.5558 0.6411 0.056 Uiso 1 1 d . . . H32 H 0.2792 0.5527 0.6281 0.056 Uiso 1 1 d . . . O4 O 0.0393(2) 0.6676(3) 0.51991(10) 0.0403(5) Uani 1 1 d . . . H41 H 0.0955 0.6452 0.5556 0.061 Uiso 1 1 d . . . H42 H 0.1081 0.7254 0.4992 0.061 Uiso 1 1 d . . . H43 H 0.0125 0.5539 0.5064 0.061 Uiso 0.50 1 d P . . O5 O 0.2403(2) 0.1982(3) 0.45893(9) 0.0363(5) Uani 1 1 d . . . H51 H 0.3170 0.2394 0.4790 0.054 Uiso 1 1 d . . . H52 H 0.1534 0.2551 0.4658 0.054 Uiso 1 1 d . . . O6 O 0.2463(3) 0.8385(3) 0.45832(10) 0.0432(5) Uani 1 1 d . . . H61 H 0.3284 0.7846 0.4625 0.065 Uiso 1 1 d . . . H62 H 0.2440 0.9606 0.4585 0.065 Uiso 1 1 d . . . O7 O 0.4846(2) 0.3452(3) 0.52852(8) 0.0314(4) Uani 1 1 d . . . H71 H 0.4678 0.3783 0.5646 0.047 Uiso 1 1 d . . . H72 H 0.4951 0.4511 0.5090 0.047 Uiso 0.50 1 d P . . N1 N 0.5939(2) 0.5776(3) 0.84483(9) 0.0200(4) Uani 1 1 d . . . N2 N 0.5739(2) 0.5208(3) 0.72925(9) 0.0196(4) Uani 1 1 d . . . N3 N 0.8972(2) 0.5126(3) 0.74174(9) 0.0220(4) Uani 1 1 d . . . N4 N 0.9022(2) 0.5916(3) 0.85348(9) 0.0232(4) Uani 1 1 d . . . C1 C 0.4637(3) 0.4775(4) 0.81744(11) 0.0249(5) Uani 1 1 d . . . C2 C 0.4329(3) 0.5225(4) 0.75376(11) 0.0240(5) Uani 1 1 d . . . C3 C 0.5821(3) 0.4805(3) 0.67562(10) 0.0187(4) Uani 1 1 d . . . C4 C 0.7301(3) 0.4855(4) 0.65177(11) 0.0235(5) Uani 1 1 d . . . C5 C 0.8812(3) 0.4707(3) 0.68724(11) 0.0207(5) Uani 1 1 d . . . C6 C 1.0404(3) 0.4920(4) 0.77754(12) 0.0261(5) Uani 1 1 d . . . C7 C 1.0107(3) 0.4585(4) 0.83933(12) 0.0267(5) Uani 1 1 d . . . C8 C 0.8325(3) 0.5761(4) 0.90736(11) 0.0281(6) Uani 1 1 d . . . C9 C 0.6779(3) 0.4960(4) 0.89647(11) 0.0253(5) Uani 1 1 d . . . H1N H 0.567(3) 0.684(4) 0.8521(12) 0.019(7) Uiso 1 1 d . . . H4N H 0.947(4) 0.704(5) 0.8520(14) 0.036(9) Uiso 1 1 d . . . H1A H 0.387(3) 0.498(4) 0.8372(13) 0.027(8) Uiso 1 1 d . . . H1B H 0.494(4) 0.361(5) 0.8235(14) 0.032(8) Uiso 1 1 d . . . H2A H 0.364(4) 0.442(4) 0.7350(13) 0.025(8) Uiso 1 1 d . . . H2B H 0.396(3) 0.639(4) 0.7500(13) 0.026(8) Uiso 1 1 d . . . H4A H 0.723(4) 0.590(5) 0.6293(15) 0.032(9) Uiso 1 1 d . . . H4B H 0.720(3) 0.406(4) 0.6251(14) 0.026(8) Uiso 1 1 d . . . H6A H 1.104(4) 0.599(5) 0.7741(14) 0.034(9) Uiso 1 1 d . . . H6B H 1.097(4) 0.401(5) 0.7646(15) 0.036(9) Uiso 1 1 d . . . H7A H 0.971(3) 0.348(5) 0.8425(13) 0.028(8) Uiso 1 1 d . . . H7B H 1.098(4) 0.460(5) 0.8628(15) 0.035(9) Uiso 1 1 d . . . H8A H 0.825(4) 0.691(5) 0.9220(15) 0.040(9) Uiso 1 1 d . . . H8B H 0.893(4) 0.512(5) 0.9367(15) 0.035(9) Uiso 1 1 d . . . H9A H 0.630(3) 0.507(4) 0.9276(13) 0.022(7) Uiso 1 1 d . . . H9B H 0.692(3) 0.384(4) 0.8887(13) 0.022(7) Uiso 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 0.01496(10) 0.01769(10) 0.01910(10) -0.00106(6) 0.00196(7) -0.00053(6) O1 0.0209(8) 0.0250(9) 0.0220(8) -0.0017(7) 0.0005(7) -0.0021(7) O2 0.0249(9) 0.0277(10) 0.0352(10) -0.0032(8) 0.0139(8) 0.0020(7) O3 0.0242(10) 0.0318(11) 0.0569(14) 0.0125(10) 0.0067(9) 0.0019(8) O4 0.0388(11) 0.0338(12) 0.0468(12) 0.0007(9) -0.0010(9) 0.0018(9) O5 0.0358(11) 0.0362(11) 0.0348(11) -0.0018(9) -0.0040(8) 0.0008(9) O6 0.0485(13) 0.0330(12) 0.0470(13) -0.0030(10) 0.0015(10) 0.0062(10) O7 0.0368(10) 0.0328(11) 0.0240(9) -0.0015(8) 0.0021(8) -0.0012(8) N1 0.0215(10) 0.0190(10) 0.0201(10) -0.0018(8) 0.0055(8) 0.0004(8) N2 0.0145(9) 0.0234(10) 0.0215(10) -0.0020(8) 0.0043(7) 0.0002(8) N3 0.0148(9) 0.0257(11) 0.0259(10) 0.0000(9) 0.0039(8) 0.0006(8) N4 0.0209(10) 0.0237(11) 0.0244(10) 0.0005(8) 0.0003(8) -0.0026(8) C1 0.0193(11) 0.0293(14) 0.0273(13) -0.0032(10) 0.0077(10) -0.0044(10) C2 0.0173(11) 0.0289(13) 0.0262(12) -0.0037(10) 0.0043(9) -0.0010(10) C3 0.0187(11) 0.0153(10) 0.0219(11) 0.0007(9) 0.0020(9) 0.0000(8) C4 0.0221(12) 0.0302(14) 0.0189(11) -0.0032(10) 0.0055(9) 0.0003(10) C5 0.0193(11) 0.0153(10) 0.0284(12) 0.0015(9) 0.0069(9) -0.0010(9) C6 0.0162(11) 0.0290(13) 0.0325(14) -0.0018(11) 0.0010(10) -0.0002(10) C7 0.0214(12) 0.0269(13) 0.0303(13) 0.0032(10) -0.0025(10) 0.0003(10) C8 0.0314(14) 0.0312(15) 0.0208(12) 0.0003(10) -0.0007(10) -0.0013(11) C9 0.0317(13) 0.0246(13) 0.0204(12) 0.0019(10) 0.0064(10) 0.0018(11) _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 N3 1.952(2) . ? Pd1 N2 1.963(2) . ? Pd1 N4 2.008(2) . ? Pd1 N1 2.012(2) . ? O1 C3 1.276(3) . ? O2 C5 1.264(3) . ? O3 H31 0.74 . ? O3 H32 0.80 . ? O4 H41 0.95 . ? O4 H42 0.95 . ? O4 H43 0.96 . ? O5 H51 0.86 . ? O5 H52 0.94 . ? O6 H61 0.85 . ? O6 H62 0.94 . ? O7 H71 0.92 . ? O7 H72 0.95 . ? N1 C9 1.496(3) . ? N1 C1 1.497(3) . ? N1 H1N 0.88(3) . ? N2 C3 1.313(3) . ? N2 C2 1.477(3) . ? N3 C5 1.315(3) . ? N3 C6 1.476(3) . ? N4 C8 1.494(4) . ? N4 C7 1.496(4) . ? N4 H4N 0.96(4) . ? C1 C2 1.532(4) . ? C1 H1A 0.91(3) . ? C1 H1B 0.95(4) . ? C2 H2A 0.95(3) . ? C2 H2B 0.96(3) . ? C3 C4 1.529(3) . ? C4 C5 1.528(4) . ? C4 H4A 0.96(4) . ? C4 H4B 0.88(3) . ? C6 C7 1.536(4) . ? C6 H6A 1.02(4) . ? C6 H6B 0.95(4) . ? C7 H7A 0.94(3) . ? C7 H7B 0.92(4) . ? C8 C9 1.536(4) . ? C8 H8A 0.96(4) . ? C8 H8B 0.97(4) . ? C9 H9A 0.90(3) . ? C9 H9B 0.90(3) . ? 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 N3 Pd1 N2 97.09(9) . . ? N3 Pd1 N4 85.87(9) . . ? N2 Pd1 N4 172.44(9) . . ? N3 Pd1 N1 167.01(9) . . ? N2 Pd1 N1 87.23(9) . . ? N4 Pd1 N1 88.43(9) . . ? H31 O3 H32 105 . . ? H41 O4 H42 103 . . ? H41 O4 H43 103 . . ? H42 O4 H43 115 . . ? H51 O5 H52 113 . . ? H61 O6 H62 121 . . ? H71 O7 H72 104 . . ? C9 N1 C1 115.7(2) . . ? C9 N1 Pd1 102.18(16) . . ? C1 N1 Pd1 104.86(15) . . ? C9 N1 H1N 111.3(18) . . ? C1 N1 H1N 110.0(18) . . ? Pd1 N1 H1N 112.5(19) . . ? C3 N2 C2 122.3(2) . . ? C3 N2 Pd1 126.28(16) . . ? C2 N2 Pd1 111.25(15) . . ? C5 N3 C6 121.0(2) . . ? C5 N3 Pd1 126.81(17) . . ? C6 N3 Pd1 111.42(17) . . ? C8 N4 C7 119.9(2) . . ? C8 N4 Pd1 107.23(16) . . ? C7 N4 Pd1 102.39(16) . . ? C8 N4 H4N 109(2) . . ? C7 N4 H4N 108(2) . . ? Pd1 N4 H4N 109(2) . . ? N1 C1 C2 110.2(2) . . ? N1 C1 H1A 109(2) . . ? C2 C1 H1A 114(2) . . ? N1 C1 H1B 103(2) . . ? C2 C1 H1B 112(2) . . ? H1A C1 H1B 108(3) . . ? N2 C2 C1 108.5(2) . . ? N2 C2 H2A 112.0(19) . . ? C1 C2 H2A 109.7(19) . . ? N2 C2 H2B 106.6(18) . . ? C1 C2 H2B 108.8(18) . . ? H2A C2 H2B 111(3) . . ? O1 C3 N2 123.7(2) . . ? O1 C3 C4 115.9(2) . . ? N2 C3 C4 120.4(2) . . ? C5 C4 C3 125.3(2) . . ? C5 C4 H4A 111(2) . . ? C3 C4 H4A 103(2) . . ? C5 C4 H4B 110(2) . . ? C3 C4 H4B 103(2) . . ? H4A C4 H4B 102(3) . . ? O2 C5 N3 124.3(2) . . ? O2 C5 C4 115.7(2) . . ? N3 C5 C4 120.0(2) . . ? N3 C6 C7 108.2(2) . . ? N3 C6 H6A 110.0(19) . . ? C7 C6 H6A 112.5(19) . . ? N3 C6 H6B 112(2) . . ? C7 C6 H6B 110(2) . . ? H6A C6 H6B 104(3) . . ? N4 C7 C6 107.2(2) . . ? N4 C7 H7A 110(2) . . ? C6 C7 H7A 110.1(19) . . ? N4 C7 H7B 114(2) . . ? C6 C7 H7B 109(2) . . ? H7A C7 H7B 107(3) . . ? N4 C8 C9 111.8(2) . . ? N4 C8 H8A 107(2) . . ? C9 C8 H8A 109(2) . . ? N4 C8 H8B 112(2) . . ? C9 C8 H8B 110(2) . . ? H8A C8 H8B 106(3) . . ? N1 C9 C8 109.6(2) . . ? N1 C9 H9A 111.8(19) . . ? C8 C9 H9A 110.8(19) . . ? N1 C9 H9B 108.2(19) . . ? C8 C9 H9B 105.9(19) . . ? H9A C9 H9B 110(3) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.522 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.091