# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_sa20 _database_code_depnum_ccdc_archive 'CCDC 807132' #TrackingRef 'SA20.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H14 N4 O6 Pd' _chemical_formula_weight 368.63 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 8.283(2) _cell_length_b 13.376(3) _cell_length_c 11.202(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.499(3) _cell_angle_gamma 90.00 _cell_volume 1233.1(5) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.986 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 1.536 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6693 _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_sigmaI/netI 0.0160 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 26.04 _reflns_number_total 2399 _reflns_number_gt 2291 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+0.5349P] 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 2399 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0209 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0530 _refine_ls_wR_factor_gt 0.0522 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _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 0.237467(18) 0.975591(11) 0.357288(13) 0.02235(7) Uani 1 1 d . . . C1 C 0.2524(3) 1.01765(14) 0.6057(2) 0.0238(4) Uani 1 1 d . . . C2 C 0.3337(3) 1.10512(16) 0.55039(19) 0.0289(4) Uani 1 1 d . . . C3 C 0.2356(2) 1.00877(16) 0.72697(19) 0.0235(4) Uani 1 1 d . . . C4 C 0.2873(2) 1.08671(16) 0.82222(18) 0.0268(4) Uani 1 1 d . . . C5 C 0.1127(3) 0.85700(17) 0.6912(2) 0.0340(5) Uani 1 1 d . . . H5 H 0.0643 0.8002 0.7192 0.041 Uiso 1 1 calc R . . C6 C 0.1250(3) 0.86489(15) 0.56912(19) 0.0294(4) Uani 1 1 d . . . H6 H 0.0835 0.8149 0.5167 0.035 Uiso 1 1 calc R . . C7 C 0.2085(3) 0.84166(16) 0.15693(19) 0.0302(5) Uani 1 1 d . . . H7A H 0.1448 0.7935 0.1069 0.036 Uiso 1 1 calc R . . H7B H 0.3214 0.8209 0.1650 0.036 Uiso 1 1 calc R . . C8 C 0.1907(3) 0.94429(17) 0.10209(19) 0.0305(5) Uani 1 1 d . . . H8A H 0.2358 0.9458 0.0259 0.037 Uiso 1 1 calc R . . H8B H 0.0769 0.9630 0.0884 0.037 Uiso 1 1 calc R . . N1 N 0.1972(2) 0.94496(13) 0.52761(15) 0.0239(3) Uani 1 1 d . . . N2 N 0.1665(2) 0.92648(14) 0.76953(16) 0.0316(4) Uani 1 1 d . . . N3 N 0.1491(2) 0.84833(13) 0.27677(15) 0.0260(4) Uani 1 1 d . . . H3A H 0.1832 0.7950 0.3217 0.031 Uiso 1 1 calc R . . H3B H 0.0397 0.8492 0.2687 0.031 Uiso 1 1 calc R . . N4 N 0.2809(2) 1.01405(13) 0.18921(17) 0.0275(4) Uani 1 1 d . . . H4A H 0.2480 1.0773 0.1733 0.033 Uiso 1 1 calc R . . H4B H 0.3881 1.0104 0.1829 0.033 Uiso 1 1 calc R . . O1 O 0.3360(2) 1.10054(12) 0.43609(13) 0.0374(4) Uani 1 1 d . . . O2 O 0.3916(2) 1.17293(13) 0.61485(15) 0.0472(5) Uani 1 1 d . . . O3 O 0.18272(19) 1.15113(12) 0.83827(14) 0.0361(4) Uani 1 1 d . . . O4 O 0.42299(19) 1.07524(14) 0.87995(15) 0.0408(4) Uani 1 1 d . . . O5 O 0.6489(2) 0.29840(13) 0.57623(16) 0.0352(4) Uani 1 1 d . . . O6 O 0.5273(3) 0.18405(16) 0.0901(2) 0.0509(5) Uani 1 1 d . . . H5B H 0.571(4) 0.267(2) 0.576(3) 0.061 Uiso 1 1 d . . . H6B H 0.506(4) 0.146(2) 0.025(3) 0.061 Uiso 1 1 d . . . H5A H 0.662(4) 0.309(3) 0.514(3) 0.061 Uiso 1 1 d . . . H6A H 0.612(4) 0.180(3) 0.105(3) 0.061 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 0.03005(11) 0.02034(10) 0.01690(10) -0.00043(5) 0.00375(7) -0.00144(5) C1 0.0263(11) 0.0224(11) 0.0230(10) -0.0025(8) 0.0039(8) -0.0021(7) C2 0.0371(11) 0.0257(10) 0.0251(10) -0.0023(9) 0.0085(9) -0.0082(9) C3 0.0234(10) 0.0264(10) 0.0208(11) 0.0006(8) 0.0038(8) 0.0007(8) C4 0.0272(10) 0.0333(11) 0.0208(10) -0.0022(9) 0.0065(8) -0.0054(8) C5 0.0454(13) 0.0276(11) 0.0297(11) 0.0037(9) 0.0073(10) -0.0089(9) C6 0.0374(12) 0.0233(10) 0.0276(11) -0.0014(9) 0.0046(9) -0.0062(8) C7 0.0367(11) 0.0288(11) 0.0255(11) -0.0069(9) 0.0050(9) 0.0008(9) C8 0.0346(12) 0.0376(12) 0.0190(10) -0.0002(9) 0.0023(9) 0.0021(9) N1 0.0296(9) 0.0218(8) 0.0201(8) -0.0007(7) 0.0028(7) -0.0022(7) N2 0.0400(10) 0.0322(10) 0.0230(9) 0.0010(8) 0.0054(8) -0.0073(8) N3 0.0306(9) 0.0243(8) 0.0227(9) -0.0006(7) 0.0008(7) -0.0005(7) N4 0.0366(10) 0.0254(9) 0.0213(10) 0.0014(7) 0.0066(8) 0.0011(7) O1 0.0615(11) 0.0290(8) 0.0232(8) -0.0027(6) 0.0106(7) -0.0160(7) O2 0.0702(12) 0.0414(10) 0.0324(9) -0.0118(8) 0.0162(8) -0.0312(9) O3 0.0320(8) 0.0411(9) 0.0352(9) -0.0127(7) 0.0035(7) 0.0036(7) O4 0.0302(9) 0.0553(11) 0.0352(9) -0.0142(8) -0.0039(7) 0.0039(8) O5 0.0381(9) 0.0370(9) 0.0299(8) 0.0028(7) 0.0016(7) -0.0092(7) O6 0.0489(11) 0.0499(11) 0.0507(12) -0.0090(9) -0.0082(9) 0.0164(10) _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 2.0157(17) . ? Pd1 O1 2.0189(16) . ? Pd1 N4 2.0229(19) . ? Pd1 N3 2.0243(17) . ? C1 N1 1.352(3) . ? C1 C3 1.387(3) . ? C1 C2 1.516(3) . ? C2 O2 1.223(3) . ? C2 O1 1.284(3) . ? C3 N2 1.352(3) . ? C3 C4 1.518(3) . ? C4 O4 1.241(3) . ? C4 O3 1.249(3) . ? C5 N2 1.320(3) . ? C5 C6 1.387(3) . ? C6 N1 1.335(3) . ? C7 N3 1.484(3) . ? C7 C8 1.504(3) . ? C8 N4 1.489(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 N1 Pd1 O1 81.74(7) . . ? N1 Pd1 N4 176.88(7) . . ? O1 Pd1 N4 95.21(7) . . ? N1 Pd1 N3 99.24(7) . . ? O1 Pd1 N3 177.35(7) . . ? N4 Pd1 N3 83.83(7) . . ? N1 C1 C3 120.53(18) . . ? N1 C1 C2 115.08(19) . . ? C3 C1 C2 124.39(19) . . ? O2 C2 O1 125.09(19) . . ? O2 C2 C1 119.57(19) . . ? O1 C2 C1 115.33(18) . . ? N2 C3 C1 120.59(19) . . ? N2 C3 C4 114.09(18) . . ? C1 C3 C4 125.32(18) . . ? O4 C4 O3 127.7(2) . . ? O4 C4 C3 116.62(19) . . ? O3 C4 C3 115.44(18) . . ? N2 C5 C6 123.0(2) . . ? N1 C6 C5 119.36(19) . . ? N3 C7 C8 106.69(16) . . ? N4 C8 C7 106.58(17) . . ? C6 N1 C1 118.90(18) . . ? C6 N1 Pd1 128.40(15) . . ? C1 N1 Pd1 112.70(14) . . ? C5 N2 C3 117.60(18) . . ? C7 N3 Pd1 108.25(13) . . ? C8 N4 Pd1 108.77(13) . . ? C2 O1 Pd1 115.12(13) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.332 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.153 data_ta022m _database_code_depnum_ccdc_archive 'CCDC 807133' #TrackingRef 'TA02.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H30 N6 O12 Pd2' _chemical_formula_weight 735.28 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2309(5) _cell_length_b 12.1884(9) _cell_length_c 14.6252(11) _cell_angle_alpha 103.8740(10) _cell_angle_beta 94.0380(10) _cell_angle_gamma 93.7760(10) _cell_volume 1243.69(16) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.963 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 1.520 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details . _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7011 _diffrn_reflns_av_R_equivalents 0.0110 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 26.02 _reflns_number_total 4755 _reflns_number_gt 3932 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+0.7664P] 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 4755 _refine_ls_number_parameters 367 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.003 _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 0.16833(3) 0.657495(16) 0.923815(13) 0.01758(8) Uani 1 1 d . . . Pd2 Pd 0.68186(3) 0.661188(16) 0.428976(14) 0.01768(8) Uani 1 1 d . . . C1 C 0.3026(4) 0.5521(2) 1.08098(19) 0.0220(6) Uani 1 1 d . . . H1 H 0.3193 0.6250 1.1202 0.026 Uiso 1 1 calc R . . C2 C 0.3498(4) 0.4607(3) 1.1168(2) 0.0260(7) Uani 1 1 d . . . H2 H 0.3970 0.4723 1.1795 0.031 Uiso 1 1 calc R . . C3 C 0.3258(4) 0.3528(2) 1.0582(2) 0.0234(6) Uani 1 1 d . . . H3 H 0.3570 0.2911 1.0813 0.028 Uiso 1 1 calc R . . C4 C 0.2544(4) 0.3363(2) 0.96400(19) 0.0193(6) Uani 1 1 d . . . C5 C 0.2422(4) 0.2168(2) 0.90052(19) 0.0216(6) Uani 1 1 d . . . C6 C 0.2089(4) 0.4304(2) 0.93314(19) 0.0174(6) Uani 1 1 d . . . C7 C 0.1250(4) 0.4252(2) 0.83386(19) 0.0195(6) Uani 1 1 d . . . C8 C 0.2829(4) 0.8948(3) 0.9853(2) 0.0306(7) Uani 1 1 d . . . H8A H 0.3996 0.8909 0.9563 0.037 Uiso 1 1 calc R . . H8B H 0.2882 0.9657 1.0333 0.037 Uiso 1 1 calc R . . C9 C 0.1222(5) 0.8881(3) 0.9115(2) 0.0293(7) Uani 1 1 d . . . H9A H 0.0078 0.9026 0.9415 0.035 Uiso 1 1 calc R . . H9B H 0.1452 0.9440 0.8754 0.035 Uiso 1 1 calc R . . C10 C 0.7998(4) 0.5468(3) 0.58436(19) 0.0227(6) Uani 1 1 d . . . H10 H 0.8168 0.6185 0.6256 0.027 Uiso 1 1 calc R . . C11 C 0.8390(4) 0.4532(3) 0.6178(2) 0.0263(7) Uani 1 1 d . . . H11 H 0.8795 0.4616 0.6811 0.032 Uiso 1 1 calc R . . C12 C 0.8171(4) 0.3470(2) 0.5560(2) 0.0227(6) Uani 1 1 d . . . H12 H 0.8441 0.2834 0.5774 0.027 Uiso 1 1 calc R . . C13 C 0.7541(4) 0.3352(2) 0.46116(19) 0.0189(6) Uani 1 1 d . . . C14 C 0.7419(4) 0.2179(2) 0.39352(19) 0.0205(6) Uani 1 1 d . . . C15 C 0.7139(4) 0.4318(2) 0.43300(19) 0.0167(6) Uani 1 1 d . . . C16 C 0.6347(4) 0.4310(2) 0.33355(19) 0.0188(6) Uani 1 1 d . . . C17 C 0.7808(4) 0.9000(3) 0.5007(2) 0.0288(7) Uani 1 1 d . . . H17A H 0.9005 0.9030 0.4749 0.035 Uiso 1 1 calc R . . H17B H 0.7760 0.9681 0.5507 0.035 Uiso 1 1 calc R . . C18 C 0.6249(4) 0.8916(3) 0.4239(2) 0.0283(7) Uani 1 1 d . . . H18A H 0.5061 0.8977 0.4509 0.034 Uiso 1 1 calc R . . H18B H 0.6438 0.9521 0.3920 0.034 Uiso 1 1 calc R . . N1 N 0.1066(4) 0.7724(2) 0.84869(17) 0.0239(5) Uani 1 1 d . . . H1A H 0.1852 0.7696 0.8033 0.029 Uiso 1 1 calc R . . H1B H -0.0100 0.7552 0.8205 0.029 Uiso 1 1 calc R . . N2 N 0.2505(3) 0.7972(2) 1.02819(17) 0.0217(5) Uani 1 1 d . . . H2A H 0.1621 0.8111 1.0689 0.026 Uiso 1 1 calc R . . H2B H 0.3558 0.7865 1.0603 0.026 Uiso 1 1 calc R . . N3 N 0.6280(3) 0.7793(2) 0.35634(17) 0.0222(5) Uani 1 1 d . . . H3A H 0.7163 0.7829 0.3165 0.027 Uiso 1 1 calc R . . H3B H 0.5173 0.7600 0.3220 0.027 Uiso 1 1 calc R . . N4 N 0.7546(3) 0.7977(2) 0.53809(17) 0.0206(5) Uani 1 1 d . . . H4A H 0.6650 0.8065 0.5783 0.025 Uiso 1 1 calc R . . H4B H 0.8609 0.7876 0.5698 0.025 Uiso 1 1 calc R . . N5 N 0.2334(3) 0.5368(2) 0.99088(16) 0.0180(5) Uani 1 1 d . . . N6 N 0.7377(3) 0.5366(2) 0.49362(16) 0.0178(5) Uani 1 1 d . . . O1 O 0.3901(3) 0.18844(19) 0.86650(16) 0.0353(6) Uani 1 1 d . . . O2 O 0.0914(3) 0.15677(17) 0.89055(15) 0.0278(5) Uani 1 1 d . . . O3 O 0.0958(3) 0.33398(16) 0.77525(13) 0.0233(4) Uani 1 1 d . . . O4 O 0.0847(3) 0.52074(17) 0.81857(14) 0.0235(4) Uani 1 1 d . . . O5 O 0.8873(3) 0.19157(18) 0.35509(14) 0.0275(5) Uani 1 1 d . . . O6 O 0.5928(3) 0.15639(17) 0.38615(15) 0.0257(5) Uani 1 1 d . . . O7 O 0.6030(3) 0.34025(16) 0.27394(13) 0.0232(4) Uani 1 1 d . . . O8 O 0.6021(3) 0.52811(17) 0.31985(14) 0.0235(4) Uani 1 1 d . . . O9 O 0.7406(3) 0.2103(2) 0.7348(2) 0.0447(6) Uani 1 1 d D . . O10 O 0.2692(4) 0.2018(2) 0.2232(2) 0.0543(8) Uani 1 1 d D . . O11 O 0.9633(5) 0.9607(3) 0.3007(2) 0.0642(9) Uani 1 1 d D . . O12 O 0.4606(5) 1.0044(3) 0.2217(3) 0.0847(14) Uani 1 1 d D . . H10B H 0.364(4) 0.247(3) 0.246(4) 0.102 Uiso 1 1 d D . . H9OB H 0.852(3) 0.238(3) 0.740(4) 0.102 Uiso 1 1 d D . . H9OA H 0.730(6) 0.1391(9) 0.716(4) 0.102 Uiso 1 1 d D . . H10A H 0.293(6) 0.1331(13) 0.213(4) 0.102 Uiso 1 1 d D . . H12B H 0.507(6) 0.9408(18) 0.205(4) 0.102 Uiso 1 1 d D . . H11B H 1.013(7) 1.024(2) 0.292(3) 0.102 Uiso 1 1 d D . . H12A H 0.548(5) 1.054(3) 0.216(4) 0.102 Uiso 1 1 d D . . H11A H 0.908(6) 0.926(3) 0.2477(18) 0.102 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01932(13) 0.01543(14) 0.01671(13) 0.00136(9) 0.00136(9) 0.00212(9) Pd2 0.01930(13) 0.01508(14) 0.01728(13) 0.00125(9) 0.00104(9) 0.00222(9) C1 0.0246(15) 0.0209(15) 0.0172(13) -0.0005(11) 0.0007(11) -0.0011(11) C2 0.0255(15) 0.0337(18) 0.0172(14) 0.0040(13) -0.0014(11) 0.0029(13) C3 0.0252(15) 0.0238(16) 0.0218(14) 0.0061(12) 0.0017(11) 0.0056(12) C4 0.0156(13) 0.0224(15) 0.0185(13) 0.0019(11) 0.0039(10) 0.0002(11) C5 0.0224(14) 0.0219(15) 0.0200(14) 0.0041(12) 0.0000(11) 0.0042(12) C6 0.0148(13) 0.0214(15) 0.0148(13) 0.0017(11) 0.0031(10) 0.0010(11) C7 0.0187(14) 0.0217(15) 0.0163(13) 0.0019(11) -0.0006(10) 0.0001(11) C8 0.0318(17) 0.0205(16) 0.0376(18) 0.0066(13) -0.0025(14) -0.0029(13) C9 0.0397(18) 0.0181(16) 0.0286(16) 0.0040(13) -0.0015(14) 0.0036(13) C10 0.0251(15) 0.0239(15) 0.0156(13) -0.0013(11) 0.0009(11) -0.0008(12) C11 0.0275(15) 0.0319(18) 0.0176(14) 0.0038(13) -0.0012(12) 0.0004(13) C12 0.0248(15) 0.0237(16) 0.0210(14) 0.0080(12) 0.0012(11) 0.0030(12) C13 0.0157(13) 0.0215(15) 0.0179(13) 0.0022(11) 0.0026(10) -0.0003(11) C14 0.0246(15) 0.0193(15) 0.0179(14) 0.0047(11) 0.0007(11) 0.0048(11) C15 0.0147(13) 0.0192(14) 0.0152(13) 0.0025(11) 0.0020(10) -0.0009(10) C16 0.0210(14) 0.0191(15) 0.0154(13) 0.0030(11) 0.0005(10) 0.0012(11) C17 0.0327(17) 0.0181(15) 0.0332(17) 0.0054(13) -0.0046(13) -0.0034(12) C18 0.0374(18) 0.0162(15) 0.0293(16) 0.0032(12) -0.0036(13) 0.0040(13) N1 0.0297(13) 0.0215(13) 0.0202(12) 0.0044(10) 0.0012(10) 0.0052(10) N2 0.0209(12) 0.0187(13) 0.0235(12) 0.0017(10) 0.0009(10) 0.0018(10) N3 0.0244(12) 0.0217(13) 0.0203(12) 0.0045(10) 0.0014(10) 0.0035(10) N4 0.0197(12) 0.0186(13) 0.0217(12) 0.0018(10) 0.0001(9) 0.0010(9) N5 0.0176(11) 0.0172(12) 0.0172(11) 0.0009(9) 0.0001(9) 0.0002(9) N6 0.0187(12) 0.0167(12) 0.0171(11) 0.0025(9) 0.0023(9) -0.0001(9) O1 0.0238(11) 0.0336(13) 0.0387(13) -0.0108(10) -0.0004(9) 0.0072(9) O2 0.0310(12) 0.0199(11) 0.0304(11) 0.0019(9) 0.0072(9) -0.0016(9) O3 0.0280(11) 0.0186(10) 0.0199(10) -0.0003(8) -0.0007(8) -0.0015(8) O4 0.0297(11) 0.0201(11) 0.0191(10) 0.0030(8) -0.0029(8) 0.0025(8) O5 0.0240(11) 0.0272(12) 0.0276(11) -0.0011(9) 0.0021(9) 0.0059(9) O6 0.0269(11) 0.0181(11) 0.0296(11) 0.0015(9) 0.0051(9) -0.0032(8) O7 0.0286(11) 0.0184(10) 0.0193(10) 0.0004(8) -0.0021(8) -0.0009(8) O8 0.0294(11) 0.0193(11) 0.0199(10) 0.0026(8) -0.0036(8) 0.0027(8) O9 0.0335(13) 0.0345(14) 0.0648(17) 0.0158(13) -0.0117(12) -0.0023(11) O10 0.0386(15) 0.0417(16) 0.085(2) 0.0318(16) -0.0233(14) -0.0075(12) O11 0.089(2) 0.0474(18) 0.0440(16) -0.0101(14) -0.0237(16) 0.0286(17) O12 0.084(2) 0.065(2) 0.076(2) -0.0365(19) -0.046(2) 0.0478(18) _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 O4 2.005(2) . ? Pd1 N5 2.016(2) . ? Pd1 N2 2.019(2) . ? Pd1 N1 2.030(2) . ? Pd2 O8 2.0041(19) . ? Pd2 N6 2.019(2) . ? Pd2 N4 2.021(2) . ? Pd2 N3 2.025(2) . ? C1 N5 1.341(3) . ? C1 C2 1.391(4) . ? C2 C3 1.379(4) . ? C3 C4 1.400(4) . ? C4 C6 1.380(4) . ? C4 C5 1.522(4) . ? C5 O1 1.246(3) . ? C5 O2 1.252(3) . ? C6 N5 1.360(3) . ? C6 C7 1.519(4) . ? C7 O3 1.226(3) . ? C7 O4 1.285(3) . ? C8 N2 1.485(4) . ? C8 C9 1.514(4) . ? C9 N1 1.479(4) . ? C10 N6 1.345(3) . ? C10 C11 1.383(4) . ? C11 C12 1.382(4) . ? C12 C13 1.400(4) . ? C13 C15 1.379(4) . ? C13 C14 1.525(4) . ? C14 O5 1.251(3) . ? C14 O6 1.254(3) . ? C15 N6 1.362(3) . ? C15 C16 1.523(4) . ? C16 O7 1.229(3) . ? C16 O8 1.281(3) . ? C17 N4 1.484(4) . ? C17 C18 1.514(4) . ? C18 N3 1.487(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Pd1 N5 81.57(9) . . ? O4 Pd1 N2 178.85(8) . . ? N5 Pd1 N2 99.57(9) . . ? O4 Pd1 N1 95.42(9) . . ? N5 Pd1 N1 176.44(9) . . ? N2 Pd1 N1 83.44(10) . . ? O8 Pd2 N6 81.81(9) . . ? O8 Pd2 N4 178.14(8) . . ? N6 Pd2 N4 99.49(9) . . ? O8 Pd2 N3 94.96(9) . . ? N6 Pd2 N3 176.42(8) . . ? N4 Pd2 N3 83.78(10) . . ? N5 C1 C2 121.2(3) . . ? C3 C2 C1 119.2(3) . . ? C2 C3 C4 119.9(3) . . ? C6 C4 C3 117.9(3) . . ? C6 C4 C5 124.0(2) . . ? C3 C4 C5 118.0(2) . . ? O1 C5 O2 127.1(3) . . ? O1 C5 C4 114.5(2) . . ? O2 C5 C4 118.3(2) . . ? N5 C6 C4 122.1(2) . . ? N5 C6 C7 114.1(2) . . ? C4 C6 C7 123.8(2) . . ? O3 C7 O4 124.3(2) . . ? O3 C7 C6 120.3(3) . . ? O4 C7 C6 115.3(2) . . ? N2 C8 C9 107.1(2) . . ? N1 C9 C8 107.2(2) . . ? N6 C10 C11 121.6(3) . . ? C12 C11 C10 119.1(3) . . ? C11 C12 C13 119.9(3) . . ? C15 C13 C12 117.9(3) . . ? C15 C13 C14 123.4(2) . . ? C12 C13 C14 118.7(2) . . ? O5 C14 O6 127.1(3) . . ? O5 C14 C13 115.4(2) . . ? O6 C14 C13 117.3(2) . . ? N6 C15 C13 122.2(2) . . ? N6 C15 C16 114.2(2) . . ? C13 C15 C16 123.6(2) . . ? O7 C16 O8 125.0(2) . . ? O7 C16 C15 119.5(2) . . ? O8 C16 C15 115.5(2) . . ? N4 C17 C18 107.1(2) . . ? N3 C18 C17 106.9(2) . . ? C9 N1 Pd1 110.42(18) . . ? C8 N2 Pd1 108.61(18) . . ? C18 N3 Pd2 109.38(18) . . ? C17 N4 Pd2 109.03(18) . . ? C1 N5 C6 119.7(2) . . ? C1 N5 Pd1 127.3(2) . . ? C6 N5 Pd1 112.88(18) . . ? C10 N6 C15 119.3(2) . . ? C10 N6 Pd2 128.1(2) . . ? C15 N6 Pd2 112.51(18) . . ? C7 O4 Pd1 115.44(17) . . ? C16 O8 Pd2 115.47(17) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.137 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.091