# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_mo_11110a _database_code_depnum_ccdc_archive 'CCDC 913613' #TrackingRef 'Complex-1 Pd-Sm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H17 Cl4 N4 O10 Pd2 Sm' _chemical_formula_weight 1026.37 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' Sm Sm -0.1638 3.4418 '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 9.1629(8) _cell_length_b 14.7835(12) _cell_length_c 16.1693(14) _cell_angle_alpha 67.0610(10) _cell_angle_beta 87.9300(10) _cell_angle_gamma 77.1940(10) _cell_volume 1963.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9961 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.29 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 982 _exptl_absorpt_coefficient_mu 2.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3761 _exptl_absorpt_correction_T_max 0.7376 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.32 _diffrn_reflns_number 15207 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9573 _reflns_number_gt 8791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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^)+(0.0995P)^2^+5.8707P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9573 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1434 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 Sm1 Sm 0.27382(2) -0.001694(14) 1.003538(14) 0.00874(8) Uani 1 1 d . . . Pd1 Pd 0.52430(4) 0.53299(2) 0.59688(2) 0.01187(10) Uani 1 1 d . . . Pd2 Pd 0.00417(4) 0.56665(2) 0.88382(2) 0.01236(10) Uani 1 1 d . . . Cl1 Cl 0.74860(13) 0.46625(9) 0.67989(8) 0.0207(2) Uani 1 1 d . . . Cl2 Cl 0.62784(13) 0.65302(9) 0.49011(8) 0.0197(2) Uani 1 1 d . . . Cl3 Cl 0.23947(13) 0.47628(9) 0.87650(10) 0.0223(2) Uani 1 1 d . . . Cl4 Cl 0.10323(14) 0.70252(9) 0.86375(9) 0.0213(2) Uani 1 1 d . . . O1 O 0.4200(4) 0.1037(3) 0.9077(2) 0.0171(7) Uani 1 1 d . . . O2 O 0.6307(4) 0.1516(2) 0.8647(2) 0.0157(6) Uani 1 1 d . . . O3 O -0.0321(5) 0.8062(3) 0.2929(3) 0.0357(11) Uani 1 1 d . . . O4 O 0.2073(4) 0.8217(3) 0.2944(3) 0.0289(9) Uani 1 1 d . . . O5 O 0.1016(4) 0.1587(3) 0.9484(3) 0.0188(7) Uani 1 1 d . . . O6 O -0.1159(4) 0.1123(2) 0.9804(2) 0.0170(7) Uani 1 1 d . . . O7 O -0.3460(4) 0.9146(3) 0.9124(2) 0.0172(7) Uani 1 1 d . . . O8 O -0.5759(4) 0.8853(2) 0.9425(2) 0.0156(6) Uani 1 1 d . . . O9 O 0.1775(4) 0.0295(3) 0.8487(2) 0.0185(7) Uani 1 1 d . . . O10 O 0.1163(4) -0.0065(3) 1.1388(2) 0.0167(6) Uani 1 1 d . . . N1 N 0.4184(4) 0.4280(3) 0.6796(3) 0.0119(7) Uani 1 1 d . . . N2 N 0.3159(4) 0.5890(3) 0.5360(3) 0.0142(7) Uani 1 1 d . . . N3 N -0.1017(4) 0.4546(3) 0.8979(3) 0.0130(7) Uani 1 1 d . . . N4 N -0.2092(4) 0.6391(3) 0.8892(3) 0.0136(7) Uani 1 1 d . . . C1 C 0.4865(5) 0.3386(3) 0.7426(3) 0.0140(8) Uani 1 1 d . . . H1 H 0.5918 0.3242 0.7542 0.017 Uiso 1 1 calc R . . C2 C 0.4070(5) 0.2670(3) 0.7910(3) 0.0130(8) Uani 1 1 d . . . C3 C 0.2512(5) 0.2894(3) 0.7753(3) 0.0147(8) Uani 1 1 d . . . H3 H 0.1940 0.2425 0.8093 0.018 Uiso 1 1 calc R . . C4 C 0.1823(5) 0.3807(4) 0.7095(3) 0.0159(9) Uani 1 1 d . . . H4 H 0.0768 0.3973 0.6975 0.019 Uiso 1 1 calc R . . C5 C 0.2683(5) 0.4479(3) 0.6611(3) 0.0134(8) Uani 1 1 d . . . C6 C 0.2094(5) 0.5405(3) 0.5813(3) 0.0131(8) Uani 1 1 d . . . C7 C 0.0600(5) 0.5739(4) 0.5509(3) 0.0174(9) Uani 1 1 d . . . H7 H -0.0140 0.5423 0.5858 0.021 Uiso 1 1 calc R . . C8 C 0.0201(5) 0.6543(4) 0.4687(3) 0.0189(9) Uani 1 1 d . . . H8 H -0.0811 0.6771 0.4454 0.023 Uiso 1 1 calc R . . C9 C 0.1301(5) 0.7010(4) 0.4208(3) 0.0168(9) Uani 1 1 d . . . C10 C 0.2772(5) 0.6673(3) 0.4570(3) 0.0162(9) Uani 1 1 d . . . H10 H 0.3517 0.7007 0.4250 0.019 Uiso 1 1 calc R . . C11 C 0.4904(5) 0.1676(3) 0.8582(3) 0.0112(8) Uani 1 1 d . . . C12 C 0.0929(6) 0.7816(4) 0.3293(3) 0.0205(10) Uani 1 1 d . . . C13 C -0.0359(5) 0.3590(3) 0.9123(3) 0.0141(8) Uani 1 1 d . . . H13 H 0.0701 0.3403 0.9117 0.017 Uiso 1 1 calc R . . C14 C -0.1186(5) 0.2868(3) 0.9279(3) 0.0109(8) Uani 1 1 d . . . C15 C -0.2734(5) 0.3141(3) 0.9257(3) 0.0156(9) Uani 1 1 d . . . H15 H -0.3318 0.2654 0.9359 0.019 Uiso 1 1 calc R . . C16 C -0.3428(5) 0.4150(3) 0.9082(3) 0.0151(8) Uani 1 1 d . . . H16 H -0.4490 0.4364 0.9041 0.018 Uiso 1 1 calc R . . C17 C -0.2535(5) 0.4824(3) 0.8972(3) 0.0141(8) Uani 1 1 d . . . C18 C -0.3138(5) 0.5861(3) 0.8890(3) 0.0145(8) Uani 1 1 d . . . C19 C -0.4656(6) 0.6277(4) 0.8876(4) 0.0181(9) Uani 1 1 d . . . H19 H -0.5381 0.5922 0.8839 0.022 Uiso 1 1 calc R . . C20 C -0.5102(6) 0.7220(3) 0.8917(3) 0.0172(9) Uani 1 1 d . . . H20 H -0.6137 0.7525 0.8891 0.021 Uiso 1 1 calc R . . C21 C -0.4024(5) 0.7713(3) 0.8997(3) 0.0156(9) Uani 1 1 d . . . C22 C -0.2528(5) 0.7294(3) 0.8948(3) 0.0161(9) Uani 1 1 d . . . H22 H -0.1792 0.7655 0.8954 0.019 Uiso 1 1 calc R . . C23 C -0.0410(5) 0.1780(3) 0.9534(3) 0.0107(7) Uani 1 1 d . . . C24 C -0.4457(5) 0.8661(3) 0.9186(3) 0.0128(8) 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 Sm1 0.00802(12) 0.00495(12) 0.01198(13) -0.00209(9) 0.00022(8) -0.00119(8) Pd1 0.00933(17) 0.01102(16) 0.01249(17) -0.00113(13) 0.00042(12) -0.00330(12) Pd2 0.00936(17) 0.01112(16) 0.01829(18) -0.00718(13) 0.00112(12) -0.00304(12) Cl1 0.0121(5) 0.0244(6) 0.0199(5) -0.0015(4) -0.0023(4) -0.0057(4) Cl2 0.0168(5) 0.0181(5) 0.0199(5) -0.0006(4) 0.0031(4) -0.0086(4) Cl3 0.0100(5) 0.0227(5) 0.0375(7) -0.0158(5) 0.0028(4) -0.0031(4) Cl4 0.0183(5) 0.0204(5) 0.0318(6) -0.0140(5) 0.0049(5) -0.0112(4) O1 0.0187(17) 0.0133(15) 0.0167(16) -0.0020(12) 0.0041(13) -0.0064(13) O2 0.0104(15) 0.0122(14) 0.0175(16) 0.0001(12) -0.0036(12) 0.0008(11) O3 0.023(2) 0.037(2) 0.029(2) 0.0110(18) -0.0146(17) -0.0121(18) O4 0.0198(19) 0.031(2) 0.0206(18) 0.0070(16) -0.0004(15) -0.0065(16) O5 0.0118(16) 0.0119(14) 0.0258(18) -0.0032(13) 0.0038(13) 0.0024(12) O6 0.0161(16) 0.0118(14) 0.0240(17) -0.0060(13) -0.0003(13) -0.0065(12) O7 0.0172(16) 0.0159(15) 0.0251(17) -0.0139(14) 0.0046(13) -0.0067(13) O8 0.0115(15) 0.0138(15) 0.0251(17) -0.0117(13) 0.0017(13) -0.0023(12) O9 0.0168(16) 0.0200(16) 0.0159(16) -0.0054(13) -0.0035(13) -0.0010(13) O10 0.0154(16) 0.0179(15) 0.0174(16) -0.0066(13) 0.0024(13) -0.0061(13) N1 0.0109(17) 0.0113(16) 0.0125(17) -0.0038(14) -0.0004(13) -0.0021(13) N2 0.0104(17) 0.0121(16) 0.0167(18) -0.0022(14) 0.0014(14) -0.0023(13) N3 0.0146(18) 0.0103(16) 0.0149(17) -0.0062(14) 0.0008(14) -0.0022(14) N4 0.0129(18) 0.0134(17) 0.0170(18) -0.0087(14) 0.0023(14) -0.0028(14) C1 0.0119(19) 0.0110(19) 0.015(2) -0.0002(16) -0.0008(16) -0.0029(15) C2 0.014(2) 0.0115(19) 0.0105(19) -0.0012(16) -0.0016(16) -0.0028(16) C3 0.011(2) 0.014(2) 0.017(2) -0.0029(17) 0.0029(16) -0.0058(16) C4 0.011(2) 0.018(2) 0.018(2) -0.0042(17) 0.0011(16) -0.0055(17) C5 0.012(2) 0.0096(18) 0.0122(19) 0.0007(15) 0.0008(15) 0.0000(15) C6 0.016(2) 0.0085(18) 0.0094(18) 0.0018(15) -0.0006(16) -0.0017(15) C7 0.012(2) 0.021(2) 0.016(2) -0.0024(18) 0.0033(17) -0.0058(17) C8 0.012(2) 0.019(2) 0.022(2) -0.0032(19) -0.0022(17) -0.0041(17) C9 0.015(2) 0.016(2) 0.013(2) 0.0001(17) -0.0003(17) -0.0037(17) C10 0.017(2) 0.014(2) 0.015(2) -0.0023(17) 0.0007(17) -0.0049(17) C11 0.015(2) 0.0070(17) 0.0125(19) -0.0042(15) 0.0011(15) -0.0028(15) C12 0.021(2) 0.016(2) 0.016(2) 0.0027(18) -0.0039(18) -0.0024(18) C13 0.013(2) 0.0113(19) 0.018(2) -0.0054(16) 0.0019(16) -0.0025(16) C14 0.012(2) 0.0086(18) 0.0119(18) -0.0044(15) 0.0006(15) -0.0021(15) C15 0.010(2) 0.013(2) 0.024(2) -0.0075(17) 0.0008(17) -0.0016(16) C16 0.0079(19) 0.0118(19) 0.023(2) -0.0069(17) -0.0019(16) 0.0028(15) C17 0.014(2) 0.0106(19) 0.018(2) -0.0076(16) 0.0000(16) 0.0001(16) C18 0.018(2) 0.0096(19) 0.017(2) -0.0063(16) 0.0013(17) -0.0029(16) C19 0.017(2) 0.017(2) 0.027(2) -0.0131(19) 0.0015(18) -0.0080(18) C20 0.015(2) 0.013(2) 0.024(2) -0.0094(18) -0.0008(18) -0.0002(16) C21 0.017(2) 0.0063(17) 0.021(2) -0.0042(16) 0.0002(17) 0.0008(15) C22 0.014(2) 0.014(2) 0.021(2) -0.0078(17) 0.0023(17) -0.0034(16) C23 0.0087(18) 0.0086(17) 0.0123(18) -0.0036(15) -0.0008(14) 0.0022(14) C24 0.015(2) 0.0097(18) 0.0134(19) -0.0058(15) -0.0010(16) -0.0004(15) _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 Sm1 O1 2.349(3) . ? Sm1 O6 2.351(3) 2_557 ? Sm1 O5 2.389(3) . ? Sm1 O7 2.398(3) 2_567 ? Sm1 O2 2.410(3) 2_657 ? Sm1 O8 2.415(3) 1_645 ? Sm1 O9 2.519(3) . ? Sm1 O10 2.563(3) . ? Sm1 C11 3.066(4) 2_657 ? Pd1 N1 2.024(4) . ? Pd1 N2 2.025(4) . ? Pd1 Cl1 2.2950(12) . ? Pd1 Cl2 2.2955(11) . ? Pd2 N4 2.027(4) . ? Pd2 N3 2.034(4) . ? Pd2 Cl4 2.2898(11) . ? Pd2 Cl3 2.2968(12) . ? O1 C11 1.262(5) . ? O2 C11 1.255(6) . ? O2 Sm1 2.410(3) 2_657 ? O3 C12 1.219(7) . ? O4 C12 1.320(6) . ? O5 C23 1.281(5) . ? O6 C23 1.244(5) . ? O6 Sm1 2.351(3) 2_557 ? O7 C24 1.259(6) . ? O7 Sm1 2.398(3) 2_567 ? O8 C24 1.247(6) . ? O8 Sm1 2.415(3) 1_465 ? N1 C1 1.342(6) . ? N1 C5 1.360(6) . ? N2 C10 1.340(6) . ? N2 C6 1.361(6) . ? N3 C13 1.339(6) . ? N3 C17 1.360(6) . ? N4 C22 1.344(6) . ? N4 C18 1.367(6) . ? C1 C2 1.385(6) . ? C2 C3 1.401(6) . ? C2 C11 1.498(6) . ? C3 C4 1.380(6) . ? C4 C5 1.384(6) . ? C5 C6 1.475(6) . ? C6 C7 1.386(6) . ? C7 C8 1.388(7) . ? C8 C9 1.388(7) . ? C9 C10 1.393(7) . ? C9 C12 1.486(6) . ? C11 Sm1 3.067(4) 2_657 ? C13 C14 1.382(6) . ? C14 C15 1.384(6) . ? C14 C23 1.503(6) . ? C15 C16 1.405(6) . ? C16 C17 1.381(6) . ? C17 C18 1.464(6) . ? C18 C19 1.387(7) . ? C19 C20 1.391(6) . ? C20 C21 1.388(7) . ? C21 C22 1.387(6) . ? C21 C24 1.514(6) . ? 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 O1 Sm1 O6 147.07(13) . 2_557 ? O1 Sm1 O5 77.71(12) . . ? O6 Sm1 O5 102.06(12) 2_557 . ? O1 Sm1 O7 74.83(12) . 2_567 ? O6 Sm1 O7 137.62(12) 2_557 2_567 ? O5 Sm1 O7 75.79(13) . 2_567 ? O1 Sm1 O2 125.06(12) . 2_657 ? O6 Sm1 O2 73.42(12) 2_557 2_657 ? O5 Sm1 O2 144.91(12) . 2_657 ? O7 Sm1 O2 84.68(12) 2_567 2_657 ? O1 Sm1 O8 79.49(12) . 1_645 ? O6 Sm1 O8 79.39(12) 2_557 1_645 ? O5 Sm1 O8 137.73(13) . 1_645 ? O7 Sm1 O8 130.64(12) 2_567 1_645 ? O2 Sm1 O8 76.66(12) 2_657 1_645 ? O1 Sm1 O9 76.55(12) . . ? O6 Sm1 O9 72.16(12) 2_557 . ? O5 Sm1 O9 72.69(12) . . ? O7 Sm1 O9 141.02(12) 2_567 . ? O2 Sm1 O9 133.88(12) 2_657 . ? O8 Sm1 O9 67.63(12) 1_645 . ? O1 Sm1 O10 136.89(11) . . ? O6 Sm1 O10 72.73(12) 2_557 . ? O5 Sm1 O10 76.83(12) . . ? O7 Sm1 O10 65.53(11) 2_567 . ? O2 Sm1 O10 68.55(11) 2_657 . ? O8 Sm1 O10 140.17(11) 1_645 . ? O9 Sm1 O10 126.57(12) . . ? O1 Sm1 C11 102.41(12) . 2_657 ? O6 Sm1 C11 92.40(12) 2_557 2_657 ? O5 Sm1 C11 152.62(12) . 2_657 ? O7 Sm1 C11 77.85(12) 2_567 2_657 ? O2 Sm1 C11 22.68(11) 2_657 2_657 ? O8 Sm1 C11 67.45(12) 1_645 2_657 ? O9 Sm1 C11 134.42(11) . 2_657 ? O10 Sm1 C11 85.65(11) . 2_657 ? N1 Pd1 N2 80.18(16) . . ? N1 Pd1 Cl1 95.38(11) . . ? N2 Pd1 Cl1 174.03(12) . . ? N1 Pd1 Cl2 173.59(11) . . ? N2 Pd1 Cl2 94.59(11) . . ? Cl1 Pd1 Cl2 90.08(4) . . ? N4 Pd2 N3 80.94(16) . . ? N4 Pd2 Cl4 94.31(11) . . ? N3 Pd2 Cl4 174.95(12) . . ? N4 Pd2 Cl3 176.12(11) . . ? N3 Pd2 Cl3 95.28(11) . . ? Cl4 Pd2 Cl3 89.45(5) . . ? C11 O1 Sm1 174.1(3) . . ? C11 O2 Sm1 109.5(3) . 2_657 ? C23 O5 Sm1 128.2(3) . . ? C23 O6 Sm1 166.9(3) . 2_557 ? C24 O7 Sm1 134.9(3) . 2_567 ? C24 O8 Sm1 138.9(3) . 1_465 ? C1 N1 C5 119.3(4) . . ? C1 N1 Pd1 125.2(3) . . ? C5 N1 Pd1 115.1(3) . . ? C10 N2 C6 119.3(4) . . ? C10 N2 Pd1 125.7(3) . . ? C6 N2 Pd1 115.1(3) . . ? C13 N3 C17 119.6(4) . . ? C13 N3 Pd2 126.4(3) . . ? C17 N3 Pd2 113.9(3) . . ? C22 N4 C18 119.7(4) . . ? C22 N4 Pd2 126.5(3) . . ? C18 N4 Pd2 113.8(3) . . ? N1 C1 C2 121.7(4) . . ? C1 C2 C3 119.1(4) . . ? C1 C2 C11 119.0(4) . . ? C3 C2 C11 122.0(4) . . ? C4 C3 C2 119.0(4) . . ? C3 C4 C5 119.3(4) . . ? N1 C5 C4 121.6(4) . . ? N1 C5 C6 114.8(4) . . ? C4 C5 C6 123.4(4) . . ? N2 C6 C7 121.7(4) . . ? N2 C6 C5 114.4(4) . . ? C7 C6 C5 123.8(4) . . ? C6 C7 C8 118.9(4) . . ? C7 C8 C9 119.1(4) . . ? C8 C9 C10 119.4(4) . . ? C8 C9 C12 120.1(4) . . ? C10 C9 C12 120.4(4) . . ? N2 C10 C9 121.5(4) . . ? O2 C11 O1 121.8(4) . . ? O2 C11 C2 117.9(4) . . ? O1 C11 C2 120.3(4) . . ? O2 C11 Sm1 47.8(2) . 2_657 ? O1 C11 Sm1 74.5(3) . 2_657 ? C2 C11 Sm1 163.0(3) . 2_657 ? O3 C12 O4 125.5(5) . . ? O3 C12 C9 121.6(5) . . ? O4 C12 C9 112.9(4) . . ? N3 C13 C14 121.6(4) . . ? C13 C14 C15 119.6(4) . . ? C13 C14 C23 120.4(4) . . ? C15 C14 C23 119.9(4) . . ? C14 C15 C16 118.9(4) . . ? C17 C16 C15 118.6(4) . . ? N3 C17 C16 121.6(4) . . ? N3 C17 C18 115.5(4) . . ? C16 C17 C18 122.8(4) . . ? N4 C18 C19 120.8(4) . . ? N4 C18 C17 115.3(4) . . ? C19 C18 C17 123.7(4) . . ? C18 C19 C20 119.1(4) . . ? C21 C20 C19 119.5(4) . . ? C22 C21 C20 118.8(4) . . ? C22 C21 C24 120.2(4) . . ? C20 C21 C24 120.9(4) . . ? N4 C22 C21 121.7(4) . . ? O6 C23 O5 123.9(4) . . ? O6 C23 C14 119.4(4) . . ? O5 C23 C14 116.7(4) . . ? O8 C24 O7 126.9(4) . . ? O8 C24 C21 115.7(4) . . ? O7 C24 C21 117.3(4) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.048 0.000 0.500 608.3 92.5 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 6.106 _refine_diff_density_min -1.371 _refine_diff_density_rms 0.319 data_mo_11125a _database_code_depnum_ccdc_archive 'CCDC 913614' #TrackingRef 'Complex-2 Pd-Eu.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H17 Cl4 Eu N4 O10 Pd2' _chemical_formula_weight 1027.98 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' Eu Eu -0.1578 3.6682 '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 9.1669(5) _cell_length_b 14.7619(8) _cell_length_c 16.2021(8) _cell_angle_alpha 66.9840(10) _cell_angle_beta 87.9180(10) _cell_angle_gamma 77.1600(10) _cell_volume 1964.37(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9513 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.26 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 2.802 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4971 _exptl_absorpt_correction_T_max 0.8069 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.96 _diffrn_reflns_number 13922 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.01 _reflns_number_total 8443 _reflns_number_gt 7591 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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^)+(0.1010P)^2^+8.2182P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8443 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1519 _refine_ls_wR_factor_gt 0.1408 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 Eu1 Eu 0.27359(3) -0.001584(18) 1.003515(17) 0.00894(10) Uani 1 1 d . . . Pd1 Pd 0.52387(5) 0.53313(3) 0.59666(3) 0.01223(12) Uani 1 1 d . . . Pd2 Pd 0.00392(5) 0.56676(3) 0.88406(3) 0.01263(12) Uani 1 1 d . . . Cl1 Cl 0.74787(16) 0.46623(12) 0.67992(10) 0.0213(3) Uani 1 1 d . . . Cl2 Cl 0.62786(17) 0.65307(11) 0.49022(10) 0.0204(3) Uani 1 1 d . . . Cl3 Cl 0.23891(16) 0.47632(12) 0.87639(12) 0.0225(3) Uani 1 1 d . . . Cl4 Cl 0.10333(17) 0.70275(12) 0.86400(11) 0.0222(3) Uani 1 1 d . . . O1 O 0.4180(5) 0.1035(3) 0.9079(3) 0.0175(9) Uani 1 1 d . . . O2 O 0.6290(5) 0.1502(3) 0.8651(3) 0.0161(8) Uani 1 1 d . . . O3 O -0.0304(6) 0.8058(4) 0.2930(4) 0.0369(14) Uani 1 1 d . . . O4 O 0.2071(6) 0.8215(4) 0.2934(3) 0.0292(11) Uani 1 1 d . . . O5 O 0.0991(5) 0.1582(3) 0.9494(3) 0.0172(8) Uani 1 1 d . . . O6 O -0.1174(5) 0.1114(3) 0.9798(3) 0.0173(9) Uani 1 1 d . . . O7 O -0.3460(5) 0.9149(3) 0.9138(3) 0.0175(9) Uani 1 1 d . . . O8 O -0.5777(5) 0.8863(3) 0.9430(3) 0.0154(8) Uani 1 1 d . . . O9 O 0.1779(5) 0.0286(3) 0.8501(3) 0.0183(9) Uani 1 1 d . . . O10 O 0.1170(5) -0.0070(3) 1.1380(3) 0.0157(8) Uani 1 1 d . . . N1 N 0.4173(6) 0.4283(4) 0.6791(3) 0.0135(9) Uani 1 1 d . . . N2 N 0.3152(6) 0.5894(4) 0.5358(3) 0.0141(9) Uani 1 1 d . . . N3 N -0.1025(6) 0.4550(4) 0.8975(3) 0.0133(9) Uani 1 1 d . . . N4 N -0.2101(6) 0.6395(4) 0.8894(3) 0.0148(9) Uani 1 1 d . . . C1 C 0.4863(7) 0.3395(4) 0.7430(4) 0.0134(11) Uani 1 1 d . . . H1 H 0.5912 0.3261 0.7557 0.016 Uiso 1 1 calc R . . C2 C 0.4059(6) 0.2664(4) 0.7913(4) 0.0132(11) Uani 1 1 d . . . C3 C 0.2512(7) 0.2895(4) 0.7755(4) 0.0145(11) Uani 1 1 d . . . H3 H 0.1935 0.2429 0.8097 0.017 Uiso 1 1 calc R . . C4 C 0.1828(7) 0.3808(4) 0.7099(4) 0.0164(11) Uani 1 1 d . . . H4 H 0.0773 0.3978 0.6980 0.020 Uiso 1 1 calc R . . C5 C 0.2692(7) 0.4475(4) 0.6613(4) 0.0139(11) Uani 1 1 d . . . C6 C 0.2101(7) 0.5399(4) 0.5815(4) 0.0163(11) Uani 1 1 d . . . C7 C 0.0591(7) 0.5749(5) 0.5497(4) 0.0169(12) Uani 1 1 d . . . H7 H -0.0149 0.5430 0.5841 0.020 Uiso 1 1 calc R . . C8 C 0.0183(7) 0.6557(5) 0.4682(4) 0.0181(12) Uani 1 1 d . . . H8 H -0.0833 0.6799 0.4457 0.022 Uiso 1 1 calc R . . C9 C 0.1309(7) 0.7010(5) 0.4196(4) 0.0178(12) Uani 1 1 d . . . C10 C 0.2769(7) 0.6678(4) 0.4577(4) 0.0154(11) Uani 1 1 d . . . H10 H 0.3513 0.7022 0.4270 0.018 Uiso 1 1 calc R . . C11 C 0.4900(7) 0.1665(4) 0.8589(4) 0.0123(10) Uani 1 1 d . . . C12 C 0.0930(7) 0.7819(5) 0.3286(4) 0.0197(12) Uani 1 1 d . . . C13 C -0.0361(7) 0.3588(4) 0.9115(4) 0.0140(11) Uani 1 1 d . . . H13 H 0.0698 0.3404 0.9101 0.017 Uiso 1 1 calc R . . C14 C -0.1187(6) 0.2860(4) 0.9277(4) 0.0115(10) Uani 1 1 d . . . C15 C -0.2732(7) 0.3147(4) 0.9248(4) 0.0162(11) Uani 1 1 d . . . H15 H -0.3320 0.2663 0.9345 0.019 Uiso 1 1 calc R . . C16 C -0.3424(7) 0.4152(4) 0.9074(4) 0.0164(11) Uani 1 1 d . . . H16 H -0.4486 0.4363 0.9030 0.020 Uiso 1 1 calc R . . C17 C -0.2546(7) 0.4833(4) 0.8966(4) 0.0159(11) Uani 1 1 d . . . C18 C -0.3141(7) 0.5863(4) 0.8886(4) 0.0158(11) Uani 1 1 d . . . C19 C -0.4645(7) 0.6281(5) 0.8882(4) 0.0186(12) Uani 1 1 d . . . H19 H -0.5366 0.5924 0.8842 0.022 Uiso 1 1 calc R . . C20 C -0.5114(7) 0.7209(5) 0.8935(4) 0.0179(12) Uani 1 1 d . . . H20 H -0.6150 0.7504 0.8920 0.022 Uiso 1 1 calc R . . C21 C -0.4012(7) 0.7708(4) 0.9010(4) 0.0138(11) Uani 1 1 d . . . C22 C -0.2528(7) 0.7291(4) 0.8951(4) 0.0160(11) Uani 1 1 d . . . H22 H -0.1790 0.7652 0.8952 0.019 Uiso 1 1 calc R . . C23 C -0.0408(6) 0.1772(4) 0.9531(4) 0.0122(10) Uani 1 1 d . . . C24 C -0.4449(6) 0.8658(4) 0.9198(4) 0.0126(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.00773(15) 0.00455(15) 0.01277(16) -0.00186(11) 0.00108(10) -0.00085(10) Pd1 0.0091(2) 0.0106(2) 0.0135(2) -0.00073(17) 0.00137(15) -0.00295(16) Pd2 0.0090(2) 0.0107(2) 0.0194(2) -0.00700(17) 0.00206(16) -0.00252(16) Cl1 0.0127(7) 0.0234(7) 0.0209(7) -0.0003(6) -0.0023(5) -0.0055(5) Cl2 0.0165(7) 0.0192(7) 0.0212(7) -0.0013(6) 0.0054(5) -0.0088(5) Cl3 0.0110(6) 0.0217(7) 0.0371(8) -0.0150(6) 0.0032(6) -0.0022(5) Cl4 0.0177(7) 0.0203(7) 0.0352(8) -0.0149(6) 0.0062(6) -0.0105(6) O1 0.021(2) 0.0108(19) 0.018(2) -0.0017(16) 0.0066(17) -0.0053(16) O2 0.0109(19) 0.0138(19) 0.016(2) 0.0007(16) -0.0026(15) 0.0016(15) O3 0.023(3) 0.038(3) 0.031(3) 0.011(2) -0.011(2) -0.015(2) O4 0.020(2) 0.032(3) 0.020(2) 0.006(2) -0.0007(19) -0.007(2) O5 0.012(2) 0.0104(19) 0.024(2) -0.0035(17) 0.0030(16) 0.0004(15) O6 0.013(2) 0.013(2) 0.024(2) -0.0046(17) -0.0014(16) -0.0042(16) O7 0.016(2) 0.019(2) 0.027(2) -0.0160(18) 0.0064(17) -0.0084(17) O8 0.0109(19) 0.0135(19) 0.026(2) -0.0136(17) 0.0046(16) -0.0012(15) O9 0.018(2) 0.021(2) 0.0139(19) -0.0040(17) -0.0061(16) -0.0027(17) O10 0.013(2) 0.017(2) 0.0137(19) -0.0030(16) 0.0003(15) -0.0034(16) N1 0.014(2) 0.013(2) 0.017(2) -0.0074(19) 0.0043(18) -0.0056(19) N2 0.011(2) 0.013(2) 0.016(2) -0.0038(19) 0.0062(18) -0.0028(18) N3 0.015(2) 0.011(2) 0.016(2) -0.0071(19) 0.0052(18) -0.0038(18) N4 0.012(2) 0.013(2) 0.019(2) -0.0062(19) 0.0007(18) -0.0018(18) C1 0.012(3) 0.011(3) 0.013(3) 0.000(2) 0.002(2) -0.003(2) C2 0.013(3) 0.011(3) 0.014(3) -0.005(2) 0.002(2) -0.002(2) C3 0.014(3) 0.015(3) 0.012(3) -0.001(2) 0.001(2) -0.006(2) C4 0.011(3) 0.015(3) 0.019(3) -0.002(2) 0.001(2) -0.003(2) C5 0.015(3) 0.012(3) 0.009(2) 0.001(2) -0.001(2) -0.001(2) C6 0.016(3) 0.012(3) 0.015(3) 0.001(2) 0.003(2) -0.002(2) C7 0.012(3) 0.016(3) 0.016(3) 0.000(2) 0.005(2) -0.001(2) C8 0.011(3) 0.014(3) 0.025(3) -0.002(2) -0.002(2) -0.004(2) C9 0.018(3) 0.016(3) 0.013(3) 0.000(2) -0.001(2) -0.002(2) C10 0.015(3) 0.011(3) 0.017(3) -0.002(2) 0.003(2) -0.003(2) C11 0.014(3) 0.009(2) 0.016(3) -0.007(2) 0.004(2) -0.004(2) C12 0.022(3) 0.015(3) 0.016(3) 0.000(2) -0.004(2) -0.003(2) C13 0.013(3) 0.007(2) 0.021(3) -0.006(2) 0.005(2) -0.002(2) C14 0.012(3) 0.009(3) 0.011(2) -0.003(2) -0.0006(19) 0.001(2) C15 0.013(3) 0.015(3) 0.023(3) -0.010(2) 0.002(2) -0.005(2) C16 0.009(3) 0.013(3) 0.023(3) -0.005(2) 0.001(2) 0.000(2) C17 0.016(3) 0.014(3) 0.017(3) -0.006(2) -0.002(2) -0.001(2) C18 0.020(3) 0.013(3) 0.016(3) -0.007(2) 0.002(2) -0.006(2) C19 0.015(3) 0.018(3) 0.026(3) -0.010(2) 0.001(2) -0.006(2) C20 0.018(3) 0.015(3) 0.024(3) -0.012(2) 0.003(2) -0.002(2) C21 0.017(3) 0.006(2) 0.018(3) -0.006(2) 0.001(2) 0.001(2) C22 0.017(3) 0.011(3) 0.019(3) -0.006(2) 0.001(2) -0.003(2) C23 0.013(3) 0.009(2) 0.013(2) -0.004(2) 0.003(2) -0.002(2) C24 0.012(3) 0.009(2) 0.018(3) -0.008(2) 0.005(2) 0.000(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 Eu1 O6 2.326(4) 2_557 ? Eu1 O1 2.333(4) . ? Eu1 O7 2.379(4) 2_567 ? Eu1 O5 2.387(4) . ? Eu1 O8 2.394(4) 1_645 ? Eu1 O2 2.399(4) 2_657 ? Eu1 O9 2.503(4) . ? Eu1 O10 2.550(4) . ? Eu1 O1 3.005(5) 2_657 ? Eu1 C11 3.059(6) 2_657 ? Eu1 Eu1 4.1585(6) 2_657 ? Pd1 N1 2.024(5) . ? Pd1 N2 2.028(5) . ? Pd1 Cl2 2.2936(14) . ? Pd1 Cl1 2.2955(15) . ? Pd2 N4 2.033(5) . ? Pd2 N3 2.035(5) . ? Pd2 Cl4 2.2909(15) . ? Pd2 Cl3 2.2957(15) . ? O1 C11 1.261(7) . ? O1 Eu1 3.005(5) 2_657 ? O2 C11 1.244(7) . ? O2 Eu1 2.399(4) 2_657 ? O3 C12 1.203(8) . ? O4 C12 1.316(8) . ? O5 C23 1.255(7) . ? O6 C23 1.256(7) . ? O6 Eu1 2.326(4) 2_557 ? O7 C24 1.259(7) . ? O7 Eu1 2.379(4) 2_567 ? O8 C24 1.267(7) . ? O8 Eu1 2.394(4) 1_465 ? N1 C5 1.342(8) . ? N1 C1 1.344(7) . ? N2 C10 1.329(8) . ? N2 C6 1.360(8) . ? N3 C13 1.346(7) . ? N3 C17 1.363(8) . ? N4 C22 1.332(8) . ? N4 C18 1.367(8) . ? C1 C2 1.405(8) . ? C2 C3 1.391(8) . ? C2 C11 1.503(8) . ? C3 C4 1.375(8) . ? C4 C5 1.383(8) . ? C5 C6 1.473(7) . ? C6 C7 1.405(8) . ? C7 C8 1.383(8) . ? C8 C9 1.403(8) . ? C9 C10 1.395(9) . ? C9 C12 1.482(8) . ? C11 Eu1 3.059(6) 2_657 ? C13 C14 1.387(8) . ? C14 C15 1.382(8) . ? C14 C23 1.501(7) . ? C15 C16 1.396(8) . ? C16 C17 1.380(9) . ? C17 C18 1.451(8) . ? C18 C19 1.379(9) . ? C19 C20 1.377(8) . ? C20 C21 1.411(8) . ? C21 C22 1.380(8) . ? C21 C24 1.515(7) . ? 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 O6 Eu1 O1 147.17(16) 2_557 . ? O6 Eu1 O7 137.60(15) 2_557 2_567 ? O1 Eu1 O7 74.76(15) . 2_567 ? O6 Eu1 O5 101.55(15) 2_557 . ? O1 Eu1 O5 78.30(15) . . ? O7 Eu1 O5 76.00(16) 2_567 . ? O6 Eu1 O8 79.51(15) 2_557 1_645 ? O1 Eu1 O8 79.45(15) . 1_645 ? O7 Eu1 O8 130.52(15) 2_567 1_645 ? O5 Eu1 O8 138.00(15) . 1_645 ? O6 Eu1 O2 73.89(15) 2_557 2_657 ? O1 Eu1 O2 124.66(15) . 2_657 ? O7 Eu1 O2 84.20(15) 2_567 2_657 ? O5 Eu1 O2 144.43(15) . 2_657 ? O8 Eu1 O2 76.84(15) 1_645 2_657 ? O6 Eu1 O9 72.21(15) 2_557 . ? O1 Eu1 O9 76.53(15) . . ? O7 Eu1 O9 141.20(15) 2_567 . ? O5 Eu1 O9 73.04(15) . . ? O8 Eu1 O9 67.36(15) 1_645 . ? O2 Eu1 O9 134.11(15) 2_657 . ? O6 Eu1 O10 72.35(15) 2_557 . ? O1 Eu1 O10 137.15(14) . . ? O7 Eu1 O10 65.90(14) 2_567 . ? O5 Eu1 O10 76.42(14) . . ? O8 Eu1 O10 140.04(14) 1_645 . ? O2 Eu1 O10 68.54(14) 2_657 . ? O9 Eu1 O10 126.55(14) . . ? O6 Eu1 O1 114.28(13) 2_557 2_657 ? O1 Eu1 O1 78.39(15) . 2_657 ? O7 Eu1 O1 69.03(14) 2_567 2_657 ? O5 Eu1 O1 141.90(13) . 2_657 ? O8 Eu1 O1 64.81(13) 1_645 2_657 ? O2 Eu1 O1 46.28(13) 2_657 2_657 ? O9 Eu1 O1 128.99(13) . 2_657 ? O10 Eu1 O1 101.75(12) . 2_657 ? O6 Eu1 C11 92.60(15) 2_557 2_657 ? O1 Eu1 C11 102.28(16) . 2_657 ? O7 Eu1 C11 77.57(15) 2_567 2_657 ? O5 Eu1 C11 152.39(15) . 2_657 ? O8 Eu1 C11 67.61(15) 1_645 2_657 ? O2 Eu1 C11 22.44(15) 2_657 2_657 ? O9 Eu1 C11 134.33(14) . 2_657 ? O10 Eu1 C11 85.66(14) . 2_657 ? O1 Eu1 C11 23.98(13) 2_657 2_657 ? O6 Eu1 Eu1 140.22(11) 2_557 2_657 ? O1 Eu1 Eu1 45.06(11) . 2_657 ? O7 Eu1 Eu1 66.05(10) 2_567 2_657 ? O5 Eu1 Eu1 117.06(10) . 2_657 ? O8 Eu1 Eu1 65.78(10) 1_645 2_657 ? O2 Eu1 Eu1 79.61(10) 2_657 2_657 ? O9 Eu1 Eu1 108.91(10) . 2_657 ? O10 Eu1 Eu1 123.94(9) . 2_657 ? O1 Eu1 Eu1 33.33(8) 2_657 2_657 ? C11 Eu1 Eu1 57.25(11) 2_657 2_657 ? N1 Pd1 N2 80.0(2) . . ? N1 Pd1 Cl2 173.54(15) . . ? N2 Pd1 Cl2 94.75(14) . . ? N1 Pd1 Cl1 95.53(15) . . ? N2 Pd1 Cl1 173.84(14) . . ? Cl2 Pd1 Cl1 90.01(6) . . ? N4 Pd2 N3 80.8(2) . . ? N4 Pd2 Cl4 94.43(15) . . ? N3 Pd2 Cl4 174.80(15) . . ? N4 Pd2 Cl3 176.03(15) . . ? N3 Pd2 Cl3 95.39(15) . . ? Cl4 Pd2 Cl3 89.38(6) . . ? C11 O1 Eu1 174.6(4) . . ? C11 O1 Eu1 80.4(3) . 2_657 ? Eu1 O1 Eu1 101.61(15) . 2_657 ? C11 O2 Eu1 110.1(4) . 2_657 ? C23 O5 Eu1 129.0(4) . . ? C23 O6 Eu1 167.7(4) . 2_557 ? C24 O7 Eu1 135.4(4) . 2_567 ? C24 O8 Eu1 138.9(4) . 1_465 ? C5 N1 C1 119.5(5) . . ? C5 N1 Pd1 115.6(4) . . ? C1 N1 Pd1 124.5(4) . . ? C10 N2 C6 120.0(5) . . ? C10 N2 Pd1 125.5(4) . . ? C6 N2 Pd1 114.5(4) . . ? C13 N3 C17 120.0(5) . . ? C13 N3 Pd2 126.0(4) . . ? C17 N3 Pd2 113.9(4) . . ? C22 N4 C18 120.3(5) . . ? C22 N4 Pd2 126.3(4) . . ? C18 N4 Pd2 113.5(4) . . ? N1 C1 C2 121.0(5) . . ? C3 C2 C1 118.7(5) . . ? C3 C2 C11 122.5(5) . . ? C1 C2 C11 118.7(5) . . ? C4 C3 C2 119.2(5) . . ? C3 C4 C5 119.3(5) . . ? N1 C5 C4 122.0(5) . . ? N1 C5 C6 114.6(5) . . ? C4 C5 C6 123.2(5) . . ? N2 C6 C7 120.4(5) . . ? N2 C6 C5 114.9(5) . . ? C7 C6 C5 124.7(5) . . ? C8 C7 C6 120.0(5) . . ? C7 C8 C9 118.2(6) . . ? C10 C9 C8 119.1(5) . . ? C10 C9 C12 121.4(6) . . ? C8 C9 C12 119.5(6) . . ? N2 C10 C9 122.0(5) . . ? O2 C11 O1 122.4(5) . . ? O2 C11 C2 118.2(5) . . ? O1 C11 C2 119.4(5) . . ? O2 C11 Eu1 47.4(3) . 2_657 ? O1 C11 Eu1 75.6(3) . 2_657 ? C2 C11 Eu1 162.9(4) . 2_657 ? O3 C12 O4 125.6(6) . . ? O3 C12 C9 121.5(6) . . ? O4 C12 C9 112.9(5) . . ? N3 C13 C14 121.5(5) . . ? C15 C14 C13 118.8(5) . . ? C15 C14 C23 120.8(5) . . ? C13 C14 C23 120.3(5) . . ? C14 C15 C16 119.7(5) . . ? C17 C16 C15 119.1(6) . . ? N3 C17 C16 120.7(5) . . ? N3 C17 C18 115.6(5) . . ? C16 C17 C18 123.6(6) . . ? N4 C18 C19 119.9(5) . . ? N4 C18 C17 115.8(5) . . ? C19 C18 C17 124.1(6) . . ? C20 C19 C18 120.8(6) . . ? C19 C20 C21 118.1(6) . . ? C22 C21 C20 118.8(5) . . ? C22 C21 C24 120.7(5) . . ? C20 C21 C24 120.4(5) . . ? N4 C22 C21 121.8(6) . . ? O5 C23 O6 124.4(5) . . ? O5 C23 C14 116.8(5) . . ? O6 C23 C14 118.7(5) . . ? O7 C24 O8 126.3(5) . . ? O7 C24 C21 117.6(5) . . ? O8 C24 C21 116.0(5) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.048 0.000 0.500 608.6 17.9 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 5.409 _refine_diff_density_min -1.636 _refine_diff_density_rms 0.320 data_mo_11129a _database_code_depnum_ccdc_archive 'CCDC 913615' #TrackingRef 'Complex-3 Pd-Gd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H17 Cl4 Gd N4 O10 Pd2' _chemical_formula_weight 1033.27 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' Gd Gd -0.1653 3.9035 '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 9.1605(8) _cell_length_b 14.7381(13) _cell_length_c 16.2023(15) _cell_angle_alpha 66.9550(10) _cell_angle_beta 87.9010(10) _cell_angle_gamma 77.0700(10) _cell_volume 1958.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7415 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 28.21 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 986 _exptl_absorpt_coefficient_mu 2.902 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4764 _exptl_absorpt_correction_T_max 0.8451 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.66 _diffrn_reflns_number 13707 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.01 _reflns_number_total 8430 _reflns_number_gt 7254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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^)+(0.1247P)^2^+11.9811P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8430 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1827 _refine_ls_wR_factor_gt 0.1761 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Gd1 Gd 0.27336(4) -0.00159(2) 1.00329(2) 0.00974(13) Uani 1 1 d . . . Pd1 Pd 0.52397(6) 0.53292(4) 0.59677(4) 0.01325(15) Uani 1 1 d . . . Pd2 Pd 0.00387(6) 0.56681(4) 0.88414(4) 0.01489(16) Uani 1 1 d . . . Cl1 Cl 0.7478(2) 0.46594(15) 0.68019(13) 0.0219(4) Uani 1 1 d . . . Cl2 Cl 0.6285(2) 0.65285(15) 0.49053(13) 0.0209(4) Uani 1 1 d . . . Cl3 Cl 0.2388(2) 0.47598(16) 0.87683(16) 0.0246(4) Uani 1 1 d . . . Cl4 Cl 0.1036(2) 0.70256(15) 0.86444(15) 0.0237(4) Uani 1 1 d . . . O1 O 0.4156(6) 0.1032(4) 0.9072(4) 0.0158(11) Uani 1 1 d . . . O2 O 0.6290(6) 0.1496(4) 0.8664(4) 0.0177(11) Uani 1 1 d . . . O3 O -0.0345(8) 0.8068(6) 0.2921(5) 0.043(2) Uani 1 1 d . . . O4 O 0.2078(7) 0.8203(5) 0.2927(4) 0.0310(15) Uani 1 1 d . . . O5 O 0.0978(6) 0.1571(4) 0.9483(4) 0.0180(11) Uani 1 1 d . . . O6 O -0.1173(6) 0.1130(4) 0.9800(4) 0.0178(11) Uani 1 1 d . . . O7 O -0.3462(6) 0.9156(4) 0.9131(4) 0.0183(11) Uani 1 1 d . . . O8 O -0.5747(6) 0.8863(4) 0.9442(4) 0.0158(11) Uani 1 1 d . . . O9 O 0.1772(6) 0.0277(4) 0.8511(4) 0.0222(12) Uani 1 1 d . . . O10 O 0.1179(6) -0.0076(4) 1.1363(4) 0.0166(11) Uani 1 1 d . . . N1 N 0.4163(7) 0.4283(5) 0.6794(4) 0.0139(12) Uani 1 1 d . . . N2 N 0.3165(7) 0.5889(5) 0.5365(4) 0.0152(12) Uani 1 1 d . . . N3 N -0.1017(7) 0.4552(5) 0.8977(4) 0.0146(12) Uani 1 1 d . . . N4 N -0.2082(7) 0.6382(5) 0.8899(5) 0.0165(13) Uani 1 1 d . . . C1 C 0.4859(8) 0.3381(6) 0.7438(5) 0.0156(15) Uani 1 1 d . . . H1 H 0.5907 0.3243 0.7569 0.019 Uiso 1 1 calc R . . C2 C 0.4062(8) 0.2662(5) 0.7904(5) 0.0151(15) Uani 1 1 d . . . C3 C 0.2510(8) 0.2891(5) 0.7753(5) 0.0153(14) Uani 1 1 d . . . H3 H 0.1941 0.2423 0.8103 0.018 Uiso 1 1 calc R . . C4 C 0.1798(9) 0.3813(6) 0.7086(5) 0.0175(15) Uani 1 1 d . . . H4 H 0.0744 0.3981 0.6961 0.021 Uiso 1 1 calc R . . C5 C 0.2687(9) 0.4479(6) 0.6607(5) 0.0150(14) Uani 1 1 d . . . C6 C 0.2079(9) 0.5421(6) 0.5804(5) 0.0167(15) Uani 1 1 d . . . C7 C 0.0594(9) 0.5746(6) 0.5494(5) 0.0188(15) Uani 1 1 d . . . H7 H -0.0143 0.5420 0.5836 0.023 Uiso 1 1 calc R . . C8 C 0.0201(8) 0.6554(6) 0.4677(6) 0.0212(17) Uani 1 1 d . . . H8 H -0.0814 0.6795 0.4448 0.025 Uiso 1 1 calc R . . C9 C 0.1310(9) 0.7009(6) 0.4194(6) 0.0205(16) Uani 1 1 d . . . C10 C 0.2764(9) 0.6673(6) 0.4573(5) 0.0164(15) Uani 1 1 d . . . H10 H 0.3509 0.7012 0.4259 0.020 Uiso 1 1 calc R . . C11 C 0.4894(8) 0.1667(5) 0.8588(5) 0.0120(13) Uani 1 1 d . . . C12 C 0.0926(9) 0.7819(6) 0.3280(6) 0.0214(17) Uani 1 1 d . . . C13 C -0.0375(8) 0.3598(6) 0.9123(5) 0.0158(15) Uani 1 1 d . . . H13 H 0.0687 0.3410 0.9120 0.019 Uiso 1 1 calc R . . C14 C -0.1187(8) 0.2860(5) 0.9280(5) 0.0118(13) Uani 1 1 d . . . C15 C -0.2744(9) 0.3154(6) 0.9239(5) 0.0171(15) Uani 1 1 d . . . H15 H -0.3334 0.2673 0.9324 0.020 Uiso 1 1 calc R . . C16 C -0.3430(9) 0.4154(6) 0.9074(5) 0.0179(15) Uani 1 1 d . . . H16 H -0.4493 0.4369 0.9037 0.022 Uiso 1 1 calc R . . C17 C -0.2542(8) 0.4830(6) 0.8964(5) 0.0160(15) Uani 1 1 d . . . C18 C -0.3113(9) 0.5866(6) 0.8888(5) 0.0168(15) Uani 1 1 d . . . C19 C -0.4653(9) 0.6289(6) 0.8879(6) 0.0198(16) Uani 1 1 d . . . H19 H -0.5373 0.5935 0.8832 0.024 Uiso 1 1 calc R . . C20 C -0.5123(9) 0.7227(6) 0.8939(6) 0.0175(15) Uani 1 1 d . . . H20 H -0.6159 0.7521 0.8935 0.021 Uiso 1 1 calc R . . C21 C -0.4014(9) 0.7727(5) 0.9006(5) 0.0154(14) Uani 1 1 d . . . C22 C -0.2549(9) 0.7317(6) 0.8960(6) 0.0207(16) Uani 1 1 d . . . H22 H -0.1818 0.7680 0.8969 0.025 Uiso 1 1 calc R . . C23 C -0.0430(8) 0.1755(5) 0.9546(5) 0.0142(14) Uani 1 1 d . . . C24 C -0.4450(9) 0.8665(6) 0.9199(5) 0.0142(14) 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 Gd1 0.00878(19) 0.00608(18) 0.0132(2) -0.00170(14) 0.00096(12) -0.00324(12) Pd1 0.0105(3) 0.0126(3) 0.0139(3) -0.0007(2) 0.0010(2) -0.0056(2) Pd2 0.0120(3) 0.0138(3) 0.0211(3) -0.0079(2) 0.0023(2) -0.0056(2) Cl1 0.0122(8) 0.0263(10) 0.0215(9) -0.0016(8) -0.0029(7) -0.0070(7) Cl2 0.0176(9) 0.0210(9) 0.0207(9) -0.0011(7) 0.0047(7) -0.0114(7) Cl3 0.0127(8) 0.0256(10) 0.0392(12) -0.0165(9) 0.0035(8) -0.0054(7) Cl4 0.0205(9) 0.0238(9) 0.0347(11) -0.0152(9) 0.0068(8) -0.0144(8) O1 0.020(3) 0.010(2) 0.012(2) 0.002(2) 0.006(2) -0.007(2) O2 0.019(3) 0.014(3) 0.015(3) 0.002(2) -0.001(2) -0.008(2) O3 0.036(4) 0.039(4) 0.036(4) 0.011(3) -0.015(3) -0.017(3) O4 0.023(3) 0.035(4) 0.022(3) 0.005(3) 0.000(2) -0.012(3) O5 0.009(2) 0.014(2) 0.024(3) -0.002(2) -0.001(2) 0.0015(19) O6 0.017(3) 0.012(2) 0.026(3) -0.007(2) -0.002(2) -0.008(2) O7 0.011(2) 0.021(3) 0.033(3) -0.020(3) 0.002(2) -0.007(2) O8 0.011(2) 0.014(2) 0.025(3) -0.011(2) 0.003(2) -0.0009(19) O9 0.018(3) 0.021(3) 0.021(3) -0.003(2) -0.002(2) 0.000(2) O10 0.019(3) 0.016(3) 0.014(3) -0.004(2) 0.004(2) -0.006(2) N1 0.016(3) 0.011(3) 0.014(3) -0.002(2) 0.002(2) -0.007(2) N2 0.016(3) 0.013(3) 0.015(3) -0.004(2) 0.003(2) -0.005(2) N3 0.017(3) 0.013(3) 0.017(3) -0.009(3) 0.003(2) -0.005(2) N4 0.014(3) 0.015(3) 0.020(3) -0.008(3) 0.003(2) -0.002(2) C1 0.008(3) 0.014(3) 0.020(4) -0.001(3) -0.003(3) -0.002(3) C2 0.019(4) 0.015(4) 0.010(3) -0.002(3) 0.001(3) -0.007(3) C3 0.016(4) 0.011(3) 0.014(4) -0.001(3) 0.005(3) -0.002(3) C4 0.013(3) 0.015(4) 0.017(4) 0.003(3) 0.001(3) -0.005(3) C5 0.017(4) 0.015(3) 0.013(3) -0.005(3) 0.005(3) -0.004(3) C6 0.016(4) 0.014(3) 0.013(3) 0.002(3) 0.002(3) -0.004(3) C7 0.013(3) 0.024(4) 0.018(4) -0.006(3) 0.004(3) -0.007(3) C8 0.007(3) 0.020(4) 0.032(5) -0.005(3) -0.007(3) -0.002(3) C9 0.021(4) 0.021(4) 0.020(4) -0.008(3) 0.001(3) -0.006(3) C10 0.018(4) 0.012(3) 0.016(4) -0.002(3) 0.002(3) -0.003(3) C11 0.014(3) 0.005(3) 0.017(3) -0.004(3) -0.002(3) -0.001(2) C12 0.014(4) 0.022(4) 0.024(4) -0.004(3) -0.006(3) -0.003(3) C13 0.010(3) 0.015(3) 0.022(4) -0.006(3) -0.003(3) -0.003(3) C14 0.012(3) 0.008(3) 0.012(3) -0.001(3) 0.001(3) -0.001(3) C15 0.014(3) 0.019(4) 0.020(4) -0.009(3) 0.005(3) -0.006(3) C16 0.014(3) 0.014(3) 0.022(4) -0.004(3) 0.001(3) 0.001(3) C17 0.014(3) 0.015(3) 0.017(4) -0.005(3) 0.001(3) -0.003(3) C18 0.027(4) 0.012(3) 0.014(4) -0.006(3) 0.005(3) -0.008(3) C19 0.016(4) 0.024(4) 0.025(4) -0.013(3) 0.003(3) -0.009(3) C20 0.013(3) 0.019(4) 0.026(4) -0.014(3) 0.000(3) -0.003(3) C21 0.020(4) 0.012(3) 0.017(4) -0.007(3) 0.004(3) -0.006(3) C22 0.020(4) 0.016(4) 0.028(4) -0.010(3) 0.000(3) -0.005(3) C23 0.017(4) 0.014(3) 0.011(3) -0.006(3) 0.002(3) 0.001(3) C24 0.021(4) 0.014(3) 0.008(3) -0.002(3) 0.003(3) -0.008(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 Gd1 O1 2.319(5) . ? Gd1 O6 2.342(5) 2_557 ? Gd1 O5 2.375(5) . ? Gd1 O2 2.382(5) 2_657 ? Gd1 O7 2.382(5) 2_567 ? Gd1 O8 2.387(5) 1_645 ? Gd1 O9 2.490(6) . ? Gd1 O10 2.522(5) . ? Pd1 N2 2.012(6) . ? Pd1 N1 2.028(6) . ? Pd1 Cl1 2.2927(18) . ? Pd1 Cl2 2.2930(19) . ? Pd2 N4 2.010(6) . ? Pd2 N3 2.026(6) . ? Pd2 Cl4 2.2881(19) . ? Pd2 Cl3 2.292(2) . ? O1 C11 1.271(9) . ? O2 C11 1.248(9) . ? O2 Gd1 2.382(5) 2_657 ? O3 C12 1.233(10) . ? O4 C12 1.315(10) . ? O5 C23 1.265(9) . ? O6 C23 1.202(10) . ? O6 Gd1 2.342(5) 2_557 ? O7 C24 1.256(9) . ? O7 Gd1 2.382(5) 2_567 ? O8 C24 1.246(9) . ? O8 Gd1 2.387(5) 1_465 ? N1 C5 1.338(10) . ? N1 C1 1.359(9) . ? N2 C10 1.342(10) . ? N2 C6 1.357(10) . ? N3 C13 1.326(10) . ? N3 C17 1.363(10) . ? N4 C18 1.343(10) . ? N4 C22 1.390(10) . ? C1 C2 1.379(10) . ? C2 C3 1.393(10) . ? C2 C11 1.500(9) . ? C3 C4 1.396(10) . ? C4 C5 1.394(10) . ? C5 C6 1.491(10) . ? C6 C7 1.379(11) . ? C7 C8 1.383(11) . ? C8 C9 1.389(12) . ? C9 C10 1.387(11) . ? C9 C12 1.485(11) . ? C13 C14 1.390(10) . ? C14 C15 1.390(10) . ? C14 C23 1.512(9) . ? C15 C16 1.389(11) . ? C16 C17 1.377(11) . ? C17 C18 1.457(10) . ? C18 C19 1.407(11) . ? C19 C20 1.393(11) . ? C20 C21 1.411(10) . ? C21 C22 1.356(11) . ? C21 C24 1.501(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd1 O6 146.6(2) . 2_557 ? O1 Gd1 O5 78.33(19) . . ? O6 Gd1 O5 101.27(19) 2_557 . ? O1 Gd1 O2 124.93(19) . 2_657 ? O6 Gd1 O2 73.82(19) 2_557 2_657 ? O5 Gd1 O2 144.9(2) . 2_657 ? O1 Gd1 O7 75.4(2) . 2_567 ? O6 Gd1 O7 137.6(2) 2_557 2_567 ? O5 Gd1 O7 76.99(19) . 2_567 ? O2 Gd1 O7 83.9(2) 2_657 2_567 ? O1 Gd1 O8 79.02(19) . 1_645 ? O6 Gd1 O8 79.86(19) 2_557 1_645 ? O5 Gd1 O8 138.1(2) . 1_645 ? O2 Gd1 O8 76.31(19) 2_657 1_645 ? O7 Gd1 O8 129.55(18) 2_567 1_645 ? O1 Gd1 O9 76.4(2) . . ? O6 Gd1 O9 71.8(2) 2_557 . ? O5 Gd1 O9 72.6(2) . . ? O2 Gd1 O9 133.80(19) 2_657 . ? O7 Gd1 O9 141.9(2) 2_567 . ? O8 Gd1 O9 68.05(19) 1_645 . ? O1 Gd1 O10 137.67(18) . . ? O6 Gd1 O10 72.31(19) 2_557 . ? O5 Gd1 O10 76.72(19) . . ? O2 Gd1 O10 68.59(19) 2_657 . ? O7 Gd1 O10 66.00(18) 2_567 . ? O8 Gd1 O10 139.86(18) 1_645 . ? O9 Gd1 O10 126.21(19) . . ? N2 Pd1 N1 79.7(3) . . ? N2 Pd1 Cl1 173.64(19) . . ? N1 Pd1 Cl1 95.69(19) . . ? N2 Pd1 Cl2 95.00(19) . . ? N1 Pd1 Cl2 173.62(19) . . ? Cl1 Pd1 Cl2 89.90(7) . . ? N4 Pd2 N3 80.5(3) . . ? N4 Pd2 Cl4 94.8(2) . . ? N3 Pd2 Cl4 175.05(19) . . ? N4 Pd2 Cl3 175.7(2) . . ? N3 Pd2 Cl3 95.26(19) . . ? Cl4 Pd2 Cl3 89.34(7) . . ? C11 O1 Gd1 174.1(5) . . ? C11 O2 Gd1 111.1(5) . 2_657 ? C23 O5 Gd1 128.7(5) . . ? C23 O6 Gd1 167.8(5) . 2_557 ? C24 O7 Gd1 134.8(5) . 2_567 ? C24 O8 Gd1 140.2(5) . 1_465 ? C5 N1 C1 119.8(6) . . ? C5 N1 Pd1 115.4(5) . . ? C1 N1 Pd1 124.5(5) . . ? C10 N2 C6 117.5(7) . . ? C10 N2 Pd1 126.1(5) . . ? C6 N2 Pd1 116.4(5) . . ? C13 N3 C17 118.9(6) . . ? C13 N3 Pd2 126.7(5) . . ? C17 N3 Pd2 114.3(5) . . ? C18 N4 C22 119.0(7) . . ? C18 N4 Pd2 114.2(5) . . ? C22 N4 Pd2 126.8(5) . . ? N1 C1 C2 120.8(7) . . ? C1 C2 C3 119.5(7) . . ? C1 C2 C11 118.6(7) . . ? C3 C2 C11 121.8(7) . . ? C2 C3 C4 119.5(7) . . ? C5 C4 C3 117.7(7) . . ? N1 C5 C4 122.4(7) . . ? N1 C5 C6 115.3(7) . . ? C4 C5 C6 122.1(7) . . ? N2 C6 C7 123.1(7) . . ? N2 C6 C5 112.7(6) . . ? C7 C6 C5 124.0(7) . . ? C6 C7 C8 118.6(7) . . ? C7 C8 C9 119.1(7) . . ? C10 C9 C8 118.7(7) . . ? C10 C9 C12 121.7(7) . . ? C8 C9 C12 119.7(7) . . ? N2 C10 C9 122.8(7) . . ? O2 C11 O1 122.4(6) . . ? O2 C11 C2 118.5(6) . . ? O1 C11 C2 119.1(6) . . ? O3 C12 O4 126.2(8) . . ? O3 C12 C9 121.4(8) . . ? O4 C12 C9 112.4(7) . . ? N3 C13 C14 122.9(7) . . ? C13 C14 C15 118.0(6) . . ? C13 C14 C23 122.0(6) . . ? C15 C14 C23 119.8(7) . . ? C16 C15 C14 119.6(7) . . ? C17 C16 C15 118.8(7) . . ? N3 C17 C16 121.8(7) . . ? N3 C17 C18 114.0(7) . . ? C16 C17 C18 124.0(7) . . ? N4 C18 C19 120.8(7) . . ? N4 C18 C17 116.3(7) . . ? C19 C18 C17 122.6(7) . . ? C20 C19 C18 120.1(7) . . ? C19 C20 C21 118.0(7) . . ? C22 C21 C20 119.7(7) . . ? C22 C21 C24 120.2(7) . . ? C20 C21 C24 119.9(7) . . ? C21 C22 N4 122.1(7) . . ? O6 C23 O5 125.3(7) . . ? O6 C23 C14 119.4(7) . . ? O5 C23 C14 115.3(7) . . ? O8 C24 O7 126.2(7) . . ? O8 C24 C21 116.5(7) . . ? O7 C24 C21 117.2(7) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.048 0.000 0.500 608.3 92.5 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 8.452 _refine_diff_density_min -1.894 _refine_diff_density_rms 0.326 data_mo_11130a _database_code_depnum_ccdc_archive 'CCDC 913616' #TrackingRef 'Complex-4 Pd-Tb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H17 Cl4 N4 O10 Pd2 Tb' _chemical_formula_weight 1034.94 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' Tb Tb -0.1723 4.1537 '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 9.1570(7) _cell_length_b 14.7179(11) _cell_length_c 16.2237(13) _cell_angle_alpha 66.9190(10) _cell_angle_beta 87.9440(10) _cell_angle_gamma 77.0270(10) _cell_volume 1956.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4051 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 28.17 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 3.017 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6439 _exptl_absorpt_correction_T_max 0.8166 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.87 _diffrn_reflns_number 13850 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.01 _reflns_number_total 8422 _reflns_number_gt 6554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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^)+(0.1186P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8422 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1896 _refine_ls_wR_factor_gt 0.1723 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.004 _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 Tb1 Tb 0.27241(4) -0.00140(3) 1.00314(3) 0.00881(14) Uani 1 1 d . . . Pd1 Pd 0.52463(7) 0.53279(5) 0.59707(5) 0.01222(17) Uani 1 1 d . . . Pd2 Pd 0.00359(7) 0.56707(5) 0.88448(5) 0.01381(18) Uani 1 1 d . . . Cl1 Cl 0.7479(2) 0.46587(18) 0.68073(16) 0.0199(5) Uani 1 1 d . . . Cl2 Cl 0.6295(3) 0.65251(17) 0.49077(16) 0.0207(5) Uani 1 1 d . . . Cl3 Cl 0.2384(2) 0.47618(18) 0.87646(19) 0.0234(5) Uani 1 1 d . . . Cl4 Cl 0.1025(3) 0.70336(18) 0.86465(18) 0.0229(5) Uani 1 1 d . . . O1 O 0.4110(6) 0.1031(4) 0.9064(4) 0.0130(13) Uani 1 1 d . . . O2 O 0.6244(7) 0.1488(5) 0.8665(4) 0.0157(13) Uani 1 1 d . . . O3 O -0.0285(8) 0.8066(6) 0.2914(6) 0.041(2) Uani 1 1 d . . . O4 O 0.2084(8) 0.8201(5) 0.2912(5) 0.0260(16) Uani 1 1 d . . . O5 O 0.0972(6) 0.1560(5) 0.9499(4) 0.0153(13) Uani 1 1 d . . . O6 O -0.1189(7) 0.1114(5) 0.9794(5) 0.0197(15) Uani 1 1 d . . . O7 O -0.3486(7) 0.9152(4) 0.9158(4) 0.0131(13) Uani 1 1 d . . . O8 O -0.5748(7) 0.8872(4) 0.9451(4) 0.0146(13) Uani 1 1 d . . . O9 O 0.1787(7) 0.0287(5) 0.8506(5) 0.0202(14) Uani 1 1 d . . . O10 O 0.1183(7) -0.0063(4) 1.1350(4) 0.0130(12) Uiso 1 1 d . . . N1 N 0.4179(8) 0.4274(5) 0.6801(5) 0.0114(14) Uani 1 1 d . . . N2 N 0.3173(8) 0.5893(5) 0.5357(5) 0.0103(14) Uani 1 1 d . . . N3 N -0.1035(8) 0.4549(5) 0.8987(5) 0.0143(15) Uani 1 1 d . . . N4 N -0.2086(9) 0.6395(6) 0.8904(5) 0.0182(17) Uani 1 1 d . . . C1 C 0.4833(10) 0.3385(7) 0.7428(6) 0.0155(18) Uani 1 1 d . . . H1 H 0.5885 0.3241 0.7553 0.019 Uiso 1 1 calc R . . C2 C 0.4058(9) 0.2657(6) 0.7906(6) 0.0097(16) Uani 1 1 d . . . C3 C 0.2494(10) 0.2907(7) 0.7733(7) 0.0165(19) Uani 1 1 d . . . H3 H 0.1914 0.2438 0.8065 0.020 Uiso 1 1 calc R . . C4 C 0.1809(10) 0.3817(7) 0.7092(6) 0.0147(18) Uani 1 1 d . . . H4 H 0.0750 0.3995 0.6982 0.018 Uiso 1 1 calc R . . C5 C 0.2684(10) 0.4483(7) 0.6599(6) 0.0140(18) Uani 1 1 d . . . C6 C 0.2110(11) 0.5405(7) 0.5806(6) 0.0162(19) Uani 1 1 d . . . C7 C 0.0578(10) 0.5770(7) 0.5485(6) 0.0168(19) Uani 1 1 d . . . H7 H -0.0168 0.5455 0.5826 0.020 Uiso 1 1 calc R . . C8 C 0.0191(11) 0.6571(7) 0.4685(7) 0.019(2) Uani 1 1 d . . . H8 H -0.0829 0.6828 0.4465 0.023 Uiso 1 1 calc R . . C9 C 0.1324(11) 0.7016(7) 0.4187(7) 0.020(2) Uani 1 1 d . . . C10 C 0.2756(10) 0.6683(6) 0.4546(7) 0.0162(19) Uani 1 1 d . . . H10 H 0.3501 0.7014 0.4219 0.019 Uiso 1 1 calc R . . C11 C 0.4874(10) 0.1672(6) 0.8577(6) 0.0104(16) Uani 1 1 d . . . C12 C 0.0920(12) 0.7804(7) 0.3280(6) 0.020(2) Uani 1 1 d . . . C13 C -0.0356(9) 0.3587(6) 0.9142(6) 0.0107(16) Uiso 1 1 d . . . H13 H 0.0708 0.3396 0.9154 0.013 Uiso 1 1 calc R . . C14 C -0.1201(9) 0.2855(6) 0.9286(5) 0.0077(15) Uani 1 1 d . . . C15 C -0.2749(10) 0.3155(7) 0.9230(7) 0.019(2) Uani 1 1 d . . . H15 H -0.3346 0.2683 0.9294 0.022 Uiso 1 1 calc R . . C16 C -0.3416(10) 0.4151(7) 0.9078(7) 0.0178(19) Uani 1 1 d . . . H16 H -0.4479 0.4361 0.9054 0.021 Uiso 1 1 calc R . . C17 C -0.2556(10) 0.4834(7) 0.8963(7) 0.0166(19) Uani 1 1 d . . . C18 C -0.3124(11) 0.5892(7) 0.8879(6) 0.0148(18) Uani 1 1 d . . . C19 C -0.4689(10) 0.6287(7) 0.8895(6) 0.0169(19) Uani 1 1 d . . . H19 H -0.5400 0.5912 0.8882 0.020 Uiso 1 1 calc R . . C20 C -0.5145(11) 0.7226(7) 0.8931(7) 0.021(2) Uani 1 1 d . . . H20 H -0.6180 0.7538 0.8900 0.025 Uiso 1 1 calc R . . C21 C -0.4000(10) 0.7722(6) 0.9016(6) 0.0111(17) Uani 1 1 d . . . C22 C -0.2526(11) 0.7307(7) 0.8958(6) 0.0169(19) Uani 1 1 d . . . H22 H -0.1790 0.7672 0.8956 0.020 Uiso 1 1 calc R . . C23 C -0.0412(9) 0.1758(6) 0.9552(6) 0.0097(16) Uani 1 1 d . . . C24 C -0.4427(10) 0.8690(7) 0.9202(6) 0.0153(18) 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 Tb1 0.0089(2) 0.0037(2) 0.0123(2) -0.00163(16) 0.00075(15) -0.00118(14) Pd1 0.0107(3) 0.0097(3) 0.0125(4) -0.0001(3) 0.0009(3) -0.0030(2) Pd2 0.0106(3) 0.0115(3) 0.0205(4) -0.0071(3) 0.0024(3) -0.0034(2) Cl1 0.0123(10) 0.0237(11) 0.0178(11) -0.0010(9) -0.0034(8) -0.0054(8) Cl2 0.0171(11) 0.0191(11) 0.0210(12) -0.0006(9) 0.0054(9) -0.0087(9) Cl3 0.0121(10) 0.0204(11) 0.0398(15) -0.0148(11) 0.0066(10) -0.0035(8) Cl4 0.0211(11) 0.0206(11) 0.0333(14) -0.0144(10) 0.0027(10) -0.0101(9) O1 0.008(3) 0.012(3) 0.016(3) -0.001(2) 0.007(2) -0.005(2) O2 0.010(3) 0.012(3) 0.019(3) -0.002(3) -0.003(3) 0.005(2) O3 0.015(4) 0.036(4) 0.042(5) 0.022(4) -0.004(3) -0.015(3) O4 0.023(4) 0.028(4) 0.014(4) 0.008(3) -0.004(3) -0.011(3) O5 0.007(3) 0.013(3) 0.020(3) -0.003(3) 0.007(2) 0.001(2) O6 0.019(3) 0.008(3) 0.030(4) -0.002(3) -0.001(3) -0.008(2) O7 0.016(3) 0.015(3) 0.015(3) -0.011(3) 0.001(3) -0.006(2) O8 0.013(3) 0.011(3) 0.021(3) -0.010(3) 0.005(3) 0.002(2) O9 0.015(3) 0.020(3) 0.022(4) -0.007(3) 0.002(3) 0.003(3) N1 0.013(3) 0.007(3) 0.010(4) 0.001(3) -0.002(3) -0.003(3) N2 0.011(3) 0.009(3) 0.008(4) -0.001(3) 0.001(3) -0.002(3) N3 0.012(4) 0.011(4) 0.024(4) -0.009(3) 0.005(3) -0.006(3) N4 0.020(4) 0.019(4) 0.015(4) -0.008(3) 0.001(3) 0.000(3) C1 0.016(4) 0.013(4) 0.017(5) -0.006(4) -0.008(4) 0.000(3) C2 0.007(4) 0.009(4) 0.007(4) 0.001(3) -0.002(3) 0.003(3) C3 0.012(4) 0.012(4) 0.022(5) -0.002(4) 0.011(4) -0.004(3) C4 0.013(4) 0.015(4) 0.019(5) -0.008(4) -0.003(4) -0.007(3) C5 0.017(4) 0.014(4) 0.008(4) -0.001(3) -0.001(3) -0.005(3) C6 0.023(5) 0.010(4) 0.007(4) 0.003(3) -0.001(4) 0.003(3) C7 0.009(4) 0.026(5) 0.013(5) -0.004(4) 0.005(3) -0.006(4) C8 0.018(5) 0.009(4) 0.024(5) 0.002(4) -0.005(4) -0.004(3) C9 0.022(5) 0.015(4) 0.017(5) -0.003(4) 0.009(4) -0.002(4) C10 0.015(4) 0.011(4) 0.024(5) -0.007(4) 0.005(4) -0.005(3) C11 0.019(4) 0.002(3) 0.009(4) 0.000(3) -0.001(3) -0.002(3) C12 0.031(5) 0.017(5) 0.010(5) 0.000(4) -0.008(4) -0.005(4) C14 0.007(4) 0.008(4) 0.008(4) -0.004(3) -0.001(3) 0.002(3) C15 0.017(4) 0.019(5) 0.024(5) -0.012(4) 0.007(4) -0.006(4) C16 0.011(4) 0.014(4) 0.027(5) -0.009(4) 0.007(4) 0.003(3) C17 0.015(4) 0.010(4) 0.024(5) -0.009(4) 0.001(4) 0.003(3) C18 0.025(5) 0.011(4) 0.010(4) -0.003(3) 0.004(4) -0.009(4) C19 0.015(4) 0.018(5) 0.019(5) -0.007(4) 0.003(4) -0.008(4) C20 0.019(5) 0.018(5) 0.030(6) -0.013(4) -0.001(4) -0.004(4) C21 0.015(4) 0.008(4) 0.013(4) -0.006(3) 0.000(3) -0.004(3) C22 0.022(5) 0.010(4) 0.019(5) -0.008(4) -0.006(4) 0.001(3) C23 0.013(4) 0.011(4) 0.007(4) -0.004(3) 0.000(3) -0.004(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 Tb1 O1 2.298(6) . ? Tb1 O6 2.305(6) 2_557 ? Tb1 O5 2.356(6) . ? Tb1 O7 2.366(6) 2_567 ? Tb1 O8 2.370(6) 1_645 ? Tb1 O2 2.387(6) 2_657 ? Tb1 O9 2.486(7) . ? Tb1 O10 2.506(6) . ? Pd1 N2 2.016(7) . ? Pd1 N1 2.031(7) . ? Pd1 Cl1 2.289(2) . ? Pd1 Cl2 2.293(2) . ? Pd2 N4 2.015(8) . ? Pd2 N3 2.037(7) . ? Pd2 Cl4 2.288(2) . ? Pd2 Cl3 2.292(2) . ? O1 C11 1.294(10) . ? O2 C11 1.224(11) . ? O2 Tb1 2.387(6) 2_657 ? O3 C12 1.181(12) . ? O4 C12 1.340(12) . ? O5 C23 1.243(10) . ? O6 C23 1.245(10) . ? O6 Tb1 2.305(6) 2_557 ? O7 C24 1.197(11) . ? O7 Tb1 2.366(6) 2_567 ? O8 C24 1.266(11) . ? O8 Tb1 2.370(6) 1_465 ? N1 C1 1.324(11) . ? N1 C5 1.356(11) . ? N2 C6 1.359(12) . ? N2 C10 1.366(12) . ? N3 C13 1.339(11) . ? N3 C17 1.359(11) . ? N4 C18 1.340(12) . ? N4 C22 1.349(11) . ? C1 C2 1.379(12) . ? C2 C3 1.406(11) . ? C2 C11 1.477(11) . ? C3 C4 1.359(13) . ? C4 C5 1.391(12) . ? C5 C6 1.461(12) . ? C6 C7 1.422(12) . ? C7 C8 1.358(13) . ? C8 C9 1.411(13) . ? C9 C10 1.357(13) . ? C9 C12 1.468(13) . ? C13 C14 1.406(11) . ? C14 C15 1.382(12) . ? C14 C23 1.505(11) . ? C15 C16 1.381(12) . ? C16 C17 1.366(13) . ? C17 C18 1.479(12) . ? C18 C19 1.423(13) . ? C19 C20 1.374(13) . ? C20 C21 1.443(12) . ? C21 C22 1.368(12) . ? C21 C24 1.533(12) . ? 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 O1 Tb1 O6 146.3(3) . 2_557 ? O1 Tb1 O5 78.3(2) . . ? O6 Tb1 O5 101.2(2) 2_557 . ? O1 Tb1 O7 75.0(2) . 2_567 ? O6 Tb1 O7 138.3(2) 2_557 2_567 ? O5 Tb1 O7 76.9(2) . 2_567 ? O1 Tb1 O8 78.7(2) . 1_645 ? O6 Tb1 O8 80.4(2) 2_557 1_645 ? O5 Tb1 O8 138.8(2) . 1_645 ? O7 Tb1 O8 128.3(2) 2_567 1_645 ? O1 Tb1 O2 124.4(2) . 2_657 ? O6 Tb1 O2 74.8(2) 2_557 2_657 ? O5 Tb1 O2 144.7(2) . 2_657 ? O7 Tb1 O2 83.4(2) 2_567 2_657 ? O8 Tb1 O2 75.9(2) 1_645 2_657 ? O1 Tb1 O9 75.0(2) . . ? O6 Tb1 O9 72.8(2) 2_557 . ? O5 Tb1 O9 73.1(2) . . ? O7 Tb1 O9 141.0(2) 2_567 . ? O8 Tb1 O9 68.2(2) 1_645 . ? O2 Tb1 O9 134.7(2) 2_657 . ? O1 Tb1 O10 137.6(2) . . ? O6 Tb1 O10 72.3(2) 2_557 . ? O5 Tb1 O10 76.0(2) . . ? O7 Tb1 O10 66.8(2) 2_567 . ? O8 Tb1 O10 140.2(2) 1_645 . ? O2 Tb1 O10 69.4(2) 2_657 . ? O9 Tb1 O10 126.9(2) . . ? N2 Pd1 N1 80.3(3) . . ? N2 Pd1 Cl1 173.9(2) . . ? N1 Pd1 Cl1 95.3(2) . . ? N2 Pd1 Cl2 94.7(2) . . ? N1 Pd1 Cl2 173.8(2) . . ? Cl1 Pd1 Cl2 89.92(8) . . ? N4 Pd2 N3 80.6(3) . . ? N4 Pd2 Cl4 94.3(2) . . ? N3 Pd2 Cl4 174.7(2) . . ? N4 Pd2 Cl3 176.0(2) . . ? N3 Pd2 Cl3 95.5(2) . . ? Cl4 Pd2 Cl3 89.58(9) . . ? C11 O1 Tb1 173.7(6) . . ? C11 O2 Tb1 113.4(5) . 2_657 ? C23 O5 Tb1 130.1(5) . . ? C23 O6 Tb1 169.6(6) . 2_557 ? C24 O7 Tb1 137.2(6) . 2_567 ? C24 O8 Tb1 139.5(6) . 1_465 ? C1 N1 C5 119.3(8) . . ? C1 N1 Pd1 125.9(6) . . ? C5 N1 Pd1 114.4(6) . . ? C6 N2 C10 118.1(7) . . ? C6 N2 Pd1 114.9(6) . . ? C10 N2 Pd1 126.9(6) . . ? C13 N3 C17 120.3(7) . . ? C13 N3 Pd2 125.2(6) . . ? C17 N3 Pd2 114.3(6) . . ? C18 N4 C22 119.3(8) . . ? C18 N4 Pd2 114.2(6) . . ? C22 N4 Pd2 126.6(7) . . ? N1 C1 C2 123.0(8) . . ? C1 C2 C3 117.2(7) . . ? C1 C2 C11 119.8(7) . . ? C3 C2 C11 122.9(8) . . ? C4 C3 C2 120.3(8) . . ? C3 C4 C5 118.9(8) . . ? N1 C5 C4 121.0(8) . . ? N1 C5 C6 115.3(8) . . ? C4 C5 C6 123.6(8) . . ? N2 C6 C7 120.9(8) . . ? N2 C6 C5 114.7(8) . . ? C7 C6 C5 124.4(9) . . ? C8 C7 C6 119.5(8) . . ? C7 C8 C9 119.1(9) . . ? C10 C9 C8 119.3(9) . . ? C10 C9 C12 122.1(9) . . ? C8 C9 C12 118.6(9) . . ? C9 C10 N2 122.8(8) . . ? O2 C11 O1 121.9(7) . . ? O2 C11 C2 119.4(7) . . ? O1 C11 C2 118.7(7) . . ? O3 C12 O4 123.6(9) . . ? O3 C12 C9 124.5(10) . . ? O4 C12 C9 111.9(8) . . ? N3 C13 C14 120.7(7) . . ? C15 C14 C13 118.8(7) . . ? C15 C14 C23 121.4(7) . . ? C13 C14 C23 119.8(7) . . ? C14 C15 C16 119.1(9) . . ? C17 C16 C15 120.4(8) . . ? N3 C17 C16 120.6(8) . . ? N3 C17 C18 113.7(8) . . ? C16 C17 C18 125.5(8) . . ? N4 C18 C19 122.6(8) . . ? N4 C18 C17 116.3(8) . . ? C19 C18 C17 120.6(8) . . ? C20 C19 C18 118.4(8) . . ? C19 C20 C21 117.9(9) . . ? C22 C21 C20 119.7(8) . . ? C22 C21 C24 120.0(8) . . ? C20 C21 C24 120.3(8) . . ? N4 C22 C21 121.9(9) . . ? O5 C23 O6 124.4(8) . . ? O5 C23 C14 117.5(7) . . ? O6 C23 C14 118.0(7) . . ? O7 C24 O8 126.7(9) . . ? O7 C24 C21 118.6(8) . . ? O8 C24 C21 114.5(8) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.047 0.000 0.500 608.5 102.6 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 6.538 _refine_diff_density_min -1.499 _refine_diff_density_rms 0.391