# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Shiuh-Tzung Liu' _publ_contact_author_email stliu@ntu.edu.tw _publ_author_name 'Shiuh-Tzung Liu' data_ic13495 _database_code_depnum_ccdc_archive 'CCDC 850847' #TrackingRef '- Complex 1-ic13495-revised-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H24 Cl4 N8 O Pd3' _chemical_formula_weight 1045.63 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 15.4308(5) _cell_length_b 16.6886(6) _cell_length_c 14.3795(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.631(3) _cell_angle_gamma 90.00 _cell_volume 3690.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10863 _cell_measurement_theta_min 2.9081 _cell_measurement_theta_max 30.1746 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.882 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 1.778 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82644 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Oxford Diffraction Gemini A' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28632 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7989 _reflns_number_gt 5354 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.1000P)^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 7989 _refine_ls_number_parameters 497 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1563 _refine_ls_wR_factor_gt 0.1492 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.006 _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 0.26002(3) 0.74703(3) 0.53560(4) 0.02586(14) Uani 1 1 d . . . Pd2 Pd 0.16739(3) 0.76824(3) 0.38437(4) 0.02515(15) Uani 1 1 d . . . Pd3 Pd 0.10984(3) 0.73216(3) 0.59010(4) 0.02440(14) Uani 1 1 d . . . Cl1 Cl 0.12599(12) 0.63858(9) 0.35098(13) 0.0381(4) Uani 1 1 d . . . Cl2 Cl 0.08178(10) 0.86458(9) 0.61749(13) 0.0325(4) Uani 1 1 d . . . N1 N 0.3307(4) 0.7629(3) 0.6758(4) 0.0346(14) Uani 1 1 d . . . N2 N 0.2647(3) 0.8680(3) 0.5475(4) 0.0282(12) Uani 1 1 d . . . N3 N 0.1923(3) 0.8860(3) 0.4021(4) 0.0264(12) Uani 1 1 d . . . N4 N 0.1144(3) 0.8121(3) 0.2563(4) 0.0292(12) Uani 1 1 d . . . N5 N 0.3815(4) 0.7282(3) 0.4706(4) 0.0354(14) Uani 1 1 d . . . N6 N 0.2622(4) 0.6263(3) 0.5233(4) 0.0314(13) Uani 1 1 d . . . N7 N 0.1273(4) 0.6128(3) 0.5796(4) 0.0280(12) Uani 1 1 d . . . N8 N -0.0089(3) 0.6921(3) 0.6311(4) 0.0275(12) Uani 1 1 d . . . C1 C 0.3615(5) 0.7089(5) 0.7366(6) 0.0439(19) Uani 1 1 d . . . H1A H 0.3571 0.6539 0.7199 0.053 Uiso 1 1 calc R . . C2 C 0.3999(6) 0.7288(6) 0.8240(6) 0.054(2) Uani 1 1 d . . . H2A H 0.4209 0.6883 0.8665 0.065 Uiso 1 1 calc R . . C3 C 0.4069(6) 0.8061(6) 0.8470(6) 0.059(2) Uani 1 1 d . . . H3A H 0.4326 0.8213 0.9067 0.071 Uiso 1 1 calc R . . C4 C 0.3765(5) 0.8636(5) 0.7840(6) 0.051(2) Uani 1 1 d . . . H4A H 0.3820 0.9189 0.7993 0.061 Uiso 1 1 calc R . . C5 C 0.3382(4) 0.8403(4) 0.6988(5) 0.0340(16) Uani 1 1 d . . . C6 C 0.3030(4) 0.8986(4) 0.6270(5) 0.0338(16) Uani 1 1 d . . . C7 C 0.3113(5) 0.9815(4) 0.6414(5) 0.0390(17) Uani 1 1 d . . . H7A H 0.3382 1.0013 0.6986 0.047 Uiso 1 1 calc R . . C8 C 0.2812(5) 1.0328(4) 0.5743(6) 0.0426(19) Uani 1 1 d . . . H8A H 0.2873 1.0889 0.5840 0.051 Uiso 1 1 calc R . . C9 C 0.2407(4) 1.0040(4) 0.4899(5) 0.0328(16) Uani 1 1 d . . . C10 C 0.2071(5) 1.0522(4) 0.4166(6) 0.0404(18) Uani 1 1 d . . . H10A H 0.2109 1.1089 0.4216 0.048 Uiso 1 1 calc R . . C11 C 0.1691(5) 1.0182(4) 0.3382(6) 0.0408(18) Uani 1 1 d . . . H11A H 0.1477 1.0507 0.2872 0.049 Uiso 1 1 calc R . . C12 C 0.1614(4) 0.9326(4) 0.3327(5) 0.0301(15) Uani 1 1 d . . . C13 C 0.2327(4) 0.9191(4) 0.4799(5) 0.0271(14) Uani 1 1 d . . . C14 C 0.1203(4) 0.8927(4) 0.2492(5) 0.0310(15) Uani 1 1 d . . . C15 C 0.0907(5) 0.9303(4) 0.1686(5) 0.0388(17) Uani 1 1 d . . . H15A H 0.0957 0.9869 0.1640 0.047 Uiso 1 1 calc R . . C16 C 0.0542(5) 0.8880(5) 0.0946(6) 0.0425(18) Uani 1 1 d . . . H16A H 0.0324 0.9144 0.0390 0.051 Uiso 1 1 calc R . . C17 C 0.0496(4) 0.8066(5) 0.1025(5) 0.0393(17) Uani 1 1 d . . . H17A H 0.0253 0.7754 0.0516 0.047 Uiso 1 1 calc R . . C18 C 0.0803(5) 0.7702(4) 0.1842(5) 0.0356(16) Uani 1 1 d . . . H18A H 0.0769 0.7135 0.1891 0.043 Uiso 1 1 calc R . . C19 C 0.4389(5) 0.7821(5) 0.4458(6) 0.0454(19) Uani 1 1 d . . . H19A H 0.4287 0.8371 0.4577 0.054 Uiso 1 1 calc R . . C20 C 0.5124(6) 0.7609(6) 0.4039(8) 0.061(3) Uani 1 1 d . . . H20A H 0.5521 0.8008 0.3866 0.073 Uiso 1 1 calc R . . C21 C 0.5273(6) 0.6830(6) 0.3874(8) 0.073(3) Uani 1 1 d . . . H21A H 0.5775 0.6670 0.3580 0.088 Uiso 1 1 calc R . . C22 C 0.4700(5) 0.6280(5) 0.4134(7) 0.062(3) Uani 1 1 d . . . H22A H 0.4802 0.5727 0.4030 0.074 Uiso 1 1 calc R . . C23 C 0.3969(5) 0.6516(5) 0.4549(6) 0.0434(19) Uani 1 1 d . . . C24 C 0.3318(5) 0.5940(4) 0.4868(5) 0.0378(17) Uani 1 1 d . . . C25 C 0.3418(5) 0.5105(4) 0.4791(6) 0.0445(19) Uani 1 1 d . . . H25A H 0.3918 0.4890 0.4538 0.053 Uiso 1 1 calc R . . C26 C 0.2797(5) 0.4606(4) 0.5080(6) 0.0428(19) Uani 1 1 d . . . H26A H 0.2867 0.4042 0.5040 0.051 Uiso 1 1 calc R . . C27 C 0.2053(5) 0.4926(4) 0.5438(5) 0.0337(16) Uani 1 1 d . . . C28 C 0.1378(5) 0.4458(4) 0.5724(5) 0.0379(17) Uani 1 1 d . . . H28A H 0.1413 0.3890 0.5703 0.046 Uiso 1 1 calc R . . C29 C 0.0661(5) 0.4824(4) 0.6035(5) 0.0384(17) Uani 1 1 d . . . H29A H 0.0197 0.4510 0.6233 0.046 Uiso 1 1 calc R . . C30 C 0.0612(4) 0.5681(4) 0.6062(5) 0.0299(15) Uani 1 1 d . . . C31 C 0.1991(4) 0.5766(4) 0.5504(5) 0.0287(14) Uani 1 1 d . . . C32 C -0.0151(4) 0.6109(4) 0.6329(5) 0.0304(15) Uani 1 1 d . . . C33 C -0.0904(5) 0.5738(4) 0.6576(5) 0.0373(17) Uani 1 1 d . . . H33A H -0.0943 0.5170 0.6582 0.045 Uiso 1 1 calc R . . C34 C -0.1587(5) 0.6191(5) 0.6810(5) 0.0401(18) Uani 1 1 d . . . H34A H -0.2098 0.5942 0.6995 0.048 Uiso 1 1 calc R . . C35 C -0.1530(5) 0.7017(5) 0.6775(5) 0.0389(17) Uani 1 1 d . . . H35A H -0.2009 0.7342 0.6914 0.047 Uiso 1 1 calc R . . C36 C -0.0757(4) 0.7367(4) 0.6534(5) 0.0323(15) Uani 1 1 d . . . H36A H -0.0707 0.7935 0.6529 0.039 Uiso 1 1 calc R . . Cl3 Cl 0.25060(15) 0.75224(11) 0.03749(18) 0.0554(6) Uani 1 1 d . . . Cl5 Cl 0.3212(6) 0.5085(5) 0.7391(6) 0.044(2) Uani 0.22 1 d PU A 1 Cl7 Cl 0.2883(5) 0.6581(6) 0.2234(6) 0.049(2) Uani 0.22 1 d PU B 1 Cl4 Cl 0.5138(4) 0.4458(3) 0.3316(6) 0.0655(19) Uani 0.33 1 d PU C -1 Cl6 Cl 0.5157(6) 1.0003(6) 0.5315(7) 0.052(3) Uani 0.22 1 d PU D -1 O1 O 0.3320(7) 0.8347(7) 0.2469(8) 0.071(3) Uiso 0.60 1 d P E 1 O1' O 0.5000 0.9337(13) 0.2500 0.060(6) Uiso 0.40 2 d SP F 2 O1" O 0.5580(15) 0.9461(18) 0.1795(15) 0.057(8) Uiso 0.20 1 d PD G 3 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 0.0335(3) 0.0177(2) 0.0265(3) 0.0008(2) 0.0032(2) 0.00174(18) Pd2 0.0360(3) 0.0145(2) 0.0249(3) 0.0013(2) 0.0029(2) -0.00158(18) Pd3 0.0343(3) 0.0147(2) 0.0244(3) -0.0006(2) 0.0037(2) -0.00122(18) Cl1 0.0635(11) 0.0179(7) 0.0322(10) 0.0008(7) 0.0005(8) -0.0080(7) Cl2 0.0392(8) 0.0166(7) 0.0425(11) -0.0061(7) 0.0074(7) -0.0012(6) N1 0.043(3) 0.032(3) 0.030(3) 0.001(3) 0.005(3) 0.005(2) N2 0.030(3) 0.020(3) 0.035(3) -0.002(3) 0.004(2) -0.001(2) N3 0.032(3) 0.014(2) 0.033(3) -0.001(2) 0.002(2) -0.001(2) N4 0.034(3) 0.027(3) 0.027(3) 0.003(3) 0.008(2) -0.002(2) N5 0.036(3) 0.034(3) 0.037(4) 0.003(3) 0.007(3) 0.005(2) N6 0.049(3) 0.017(2) 0.028(3) 0.000(2) 0.003(3) 0.007(2) N7 0.049(3) 0.014(2) 0.021(3) 0.004(2) -0.001(2) 0.000(2) N8 0.039(3) 0.022(3) 0.021(3) -0.001(2) 0.000(2) -0.005(2) C1 0.049(4) 0.046(4) 0.036(5) 0.001(4) 0.001(4) 0.011(4) C2 0.063(5) 0.065(6) 0.034(5) 0.001(4) 0.001(4) 0.021(4) C3 0.070(6) 0.071(6) 0.035(5) -0.008(5) -0.010(4) 0.017(5) C4 0.057(5) 0.047(5) 0.046(5) -0.010(4) -0.006(4) -0.001(4) C5 0.035(3) 0.034(4) 0.033(4) -0.005(3) 0.003(3) 0.000(3) C6 0.035(3) 0.031(4) 0.035(4) -0.005(3) 0.003(3) -0.003(3) C7 0.052(4) 0.031(4) 0.032(4) -0.010(3) -0.003(3) -0.003(3) C8 0.050(4) 0.020(3) 0.059(6) -0.008(4) 0.008(4) -0.012(3) C9 0.042(4) 0.021(3) 0.037(4) -0.002(3) 0.012(3) -0.005(3) C10 0.051(4) 0.015(3) 0.056(5) 0.000(3) 0.005(4) -0.003(3) C11 0.052(4) 0.025(3) 0.044(5) 0.008(4) 0.003(4) 0.004(3) C12 0.037(4) 0.017(3) 0.037(4) 0.007(3) 0.007(3) 0.002(3) C13 0.032(3) 0.016(3) 0.035(4) 0.002(3) 0.010(3) -0.001(2) C14 0.036(3) 0.023(3) 0.035(4) 0.002(3) 0.007(3) 0.001(3) C15 0.050(4) 0.025(3) 0.041(5) 0.010(3) 0.004(4) 0.000(3) C16 0.042(4) 0.045(4) 0.038(5) 0.017(4) -0.003(3) 0.005(3) C17 0.039(4) 0.048(4) 0.031(4) 0.005(4) 0.001(3) -0.006(3) C18 0.046(4) 0.033(4) 0.029(4) -0.002(3) 0.003(3) -0.007(3) C19 0.043(4) 0.039(4) 0.054(5) 0.005(4) 0.005(4) 0.000(3) C20 0.041(4) 0.066(6) 0.076(7) 0.011(5) 0.013(4) 0.003(4) C21 0.053(5) 0.064(6) 0.107(9) 0.011(6) 0.035(5) 0.020(5) C22 0.056(5) 0.046(5) 0.087(8) 0.010(5) 0.030(5) 0.021(4) C23 0.046(4) 0.036(4) 0.049(5) 0.001(4) 0.008(4) 0.012(3) C24 0.047(4) 0.034(4) 0.032(4) 0.004(3) 0.001(3) 0.013(3) C25 0.061(5) 0.030(4) 0.043(5) -0.004(4) 0.006(4) 0.021(3) C26 0.066(5) 0.020(3) 0.042(5) -0.002(3) 0.003(4) 0.007(3) C27 0.054(4) 0.022(3) 0.024(4) 0.000(3) 0.000(3) 0.006(3) C28 0.068(5) 0.013(3) 0.032(4) -0.004(3) 0.000(4) -0.002(3) C29 0.059(5) 0.025(3) 0.031(4) 0.002(3) 0.002(3) -0.005(3) C30 0.046(4) 0.021(3) 0.022(4) 0.001(3) 0.000(3) -0.003(3) C31 0.045(4) 0.018(3) 0.023(4) 0.001(3) 0.002(3) 0.002(3) C32 0.050(4) 0.020(3) 0.022(4) 0.002(3) 0.002(3) -0.007(3) C33 0.059(5) 0.027(3) 0.026(4) -0.004(3) 0.006(3) -0.013(3) C34 0.046(4) 0.049(4) 0.026(4) -0.002(4) 0.007(3) -0.017(3) C35 0.042(4) 0.043(4) 0.032(4) -0.004(4) 0.006(3) -0.005(3) C36 0.034(3) 0.030(4) 0.032(4) 0.003(3) 0.002(3) -0.005(3) Cl3 0.0701(14) 0.0300(9) 0.0681(16) 0.0033(10) 0.0177(11) 0.0053(9) Cl5 0.061(4) 0.038(4) 0.032(4) -0.011(3) -0.009(3) 0.019(3) Cl7 0.041(4) 0.065(5) 0.042(4) -0.005(4) 0.013(3) -0.008(4) Cl4 0.035(3) 0.029(3) 0.133(6) -0.039(3) 0.012(3) 0.003(2) Cl6 0.054(5) 0.033(3) 0.073(6) 0.008(5) 0.035(5) 0.009(4) _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 N6 2.023(5) . ? Pd1 N2 2.027(5) . ? Pd1 N5 2.184(6) . ? Pd1 N1 2.229(6) . ? Pd1 Pd3 2.5179(7) . ? Pd1 Pd2 2.5288(7) . ? Pd2 N3 2.015(5) . ? Pd2 N4 2.086(5) . ? Pd2 Cl1 2.2958(16) . ? Pd2 Pd3 3.2136(7) . ? Pd3 N7 2.017(5) . ? Pd3 N8 2.080(5) . ? Pd3 Cl2 2.2922(15) . ? N1 C1 1.318(9) . ? N1 C5 1.336(9) . ? N2 C6 1.344(9) . ? N2 C13 1.357(8) . ? N3 C12 1.323(8) . ? N3 C13 1.353(8) . ? N4 C18 1.325(9) . ? N4 C14 1.353(8) . ? N5 C23 1.324(9) . ? N5 C19 1.330(10) . ? N6 C24 1.346(9) . ? N6 C31 1.360(8) . ? N7 C30 1.344(8) . ? N7 C31 1.358(8) . ? N8 C36 1.332(9) . ? N8 C32 1.360(8) . ? C1 C2 1.385(11) . ? C2 C3 1.334(13) . ? C3 C4 1.376(12) . ? C4 C5 1.373(10) . ? C5 C6 1.490(10) . ? C6 C7 1.402(9) . ? C7 C8 1.346(11) . ? C8 C9 1.403(11) . ? C9 C10 1.393(10) . ? C9 C13 1.428(8) . ? C10 C11 1.353(11) . ? C11 C12 1.435(9) . ? C12 C14 1.471(10) . ? C14 C15 1.364(10) . ? C15 C16 1.361(11) . ? C16 C17 1.365(10) . ? C17 C18 1.373(10) . ? C19 C20 1.373(12) . ? C20 C21 1.345(12) . ? C21 C22 1.348(12) . ? C22 C23 1.376(11) . ? C23 C24 1.488(11) . ? C24 C25 1.408(9) . ? C25 C26 1.360(11) . ? C26 C27 1.402(11) . ? C27 C28 1.390(10) . ? C27 C31 1.409(8) . ? C28 C29 1.369(10) . ? C29 C30 1.434(9) . ? C30 C32 1.454(10) . ? C32 C33 1.388(9) . ? C33 C34 1.361(10) . ? C34 C35 1.383(10) . ? C35 C36 1.397(9) . ? 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 N6 Pd1 N2 177.0(2) . . ? N6 Pd1 N5 78.4(2) . . ? N2 Pd1 N5 98.8(2) . . ? N6 Pd1 N1 100.8(2) . . ? N2 Pd1 N1 78.1(2) . . ? N5 Pd1 N1 91.7(2) . . ? N6 Pd1 Pd3 87.20(16) . . ? N2 Pd1 Pd3 95.70(14) . . ? N5 Pd1 Pd3 164.26(16) . . ? N1 Pd1 Pd3 97.23(15) . . ? N6 Pd1 Pd2 94.37(16) . . ? N2 Pd1 Pd2 86.98(16) . . ? N5 Pd1 Pd2 95.58(17) . . ? N1 Pd1 Pd2 164.22(15) . . ? Pd3 Pd1 Pd2 79.10(2) . . ? N3 Pd2 N4 80.0(2) . . ? N3 Pd2 Cl1 173.11(16) . . ? N4 Pd2 Cl1 93.64(15) . . ? N3 Pd2 Pd1 86.51(16) . . ? N4 Pd2 Pd1 164.19(15) . . ? Cl1 Pd2 Pd1 100.16(5) . . ? N3 Pd2 Pd3 97.51(16) . . ? N4 Pd2 Pd3 139.52(15) . . ? Cl1 Pd2 Pd3 85.58(5) . . ? Pd1 Pd2 Pd3 50.299(17) . . ? N7 Pd3 N8 80.2(2) . . ? N7 Pd3 Cl2 173.26(17) . . ? N8 Pd3 Cl2 94.48(15) . . ? N7 Pd3 Pd1 86.67(16) . . ? N8 Pd3 Pd1 166.89(15) . . ? Cl2 Pd3 Pd1 98.62(4) . . ? N7 Pd3 Pd2 93.87(16) . . ? N8 Pd3 Pd2 129.51(15) . . ? Cl2 Pd3 Pd2 92.73(5) . . ? Pd1 Pd3 Pd2 50.600(17) . . ? C1 N1 C5 118.5(7) . . ? C1 N1 Pd1 130.0(5) . . ? C5 N1 Pd1 111.4(5) . . ? C6 N2 C13 118.7(6) . . ? C6 N2 Pd1 117.4(4) . . ? C13 N2 Pd1 123.8(4) . . ? C12 N3 C13 119.9(5) . . ? C12 N3 Pd2 115.1(4) . . ? C13 N3 Pd2 124.9(4) . . ? C18 N4 C14 119.4(6) . . ? C18 N4 Pd2 127.5(5) . . ? C14 N4 Pd2 113.1(4) . . ? C23 N5 C19 118.3(7) . . ? C23 N5 Pd1 112.6(5) . . ? C19 N5 Pd1 129.1(5) . . ? C24 N6 C31 118.7(6) . . ? C24 N6 Pd1 116.9(5) . . ? C31 N6 Pd1 124.4(4) . . ? C30 N7 C31 119.8(5) . . ? C30 N7 Pd3 114.7(4) . . ? C31 N7 Pd3 125.5(4) . . ? C36 N8 C32 119.8(6) . . ? C36 N8 Pd3 127.3(4) . . ? C32 N8 Pd3 113.0(4) . . ? N1 C1 C2 122.9(8) . . ? C3 C2 C1 118.5(8) . . ? C2 C3 C4 119.7(8) . . ? C5 C4 C3 119.3(8) . . ? N1 C5 C4 121.2(7) . . ? N1 C5 C6 116.1(6) . . ? C4 C5 C6 122.7(7) . . ? N2 C6 C7 122.0(7) . . ? N2 C6 C5 116.8(6) . . ? C7 C6 C5 121.2(6) . . ? C8 C7 C6 119.9(7) . . ? C7 C8 C9 120.4(6) . . ? C10 C9 C8 124.6(6) . . ? C10 C9 C13 118.2(7) . . ? C8 C9 C13 117.2(6) . . ? C11 C10 C9 119.9(6) . . ? C10 C11 C12 119.5(7) . . ? N3 C12 C11 121.3(6) . . ? N3 C12 C14 117.1(5) . . ? C11 C12 C14 121.6(6) . . ? N3 C13 N2 117.0(5) . . ? N3 C13 C9 121.2(6) . . ? N2 C13 C9 121.8(6) . . ? N4 C14 C15 120.1(6) . . ? N4 C14 C12 114.5(6) . . ? C15 C14 C12 125.3(6) . . ? C16 C15 C14 121.0(7) . . ? C15 C16 C17 118.2(7) . . ? C16 C17 C18 119.6(7) . . ? N4 C18 C17 121.6(7) . . ? N5 C19 C20 122.4(8) . . ? C21 C20 C19 119.0(9) . . ? C20 C21 C22 119.0(8) . . ? C21 C22 C23 120.3(8) . . ? N5 C23 C22 121.0(8) . . ? N5 C23 C24 115.8(6) . . ? C22 C23 C24 123.1(7) . . ? N6 C24 C25 121.5(7) . . ? N6 C24 C23 116.2(6) . . ? C25 C24 C23 122.3(7) . . ? C26 C25 C24 119.9(7) . . ? C25 C26 C27 119.8(6) . . ? C28 C27 C26 123.4(6) . . ? C28 C27 C31 118.9(6) . . ? C26 C27 C31 117.8(6) . . ? C29 C28 C27 119.3(6) . . ? C28 C29 C30 120.0(7) . . ? N7 C30 C29 120.2(6) . . ? N7 C30 C32 116.9(6) . . ? C29 C30 C32 122.8(6) . . ? N7 C31 N6 115.9(5) . . ? N7 C31 C27 121.7(6) . . ? N6 C31 C27 122.3(6) . . ? N8 C32 C33 120.7(6) . . ? N8 C32 C30 115.1(6) . . ? C33 C32 C30 124.2(6) . . ? C34 C33 C32 119.7(6) . . ? C33 C34 C35 119.6(7) . . ? C34 C35 C36 118.9(7) . . ? N8 C36 C35 121.3(6) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 2.176 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.156 # Attachment '- ic14012-platon-revised.cif' data_ic14012 _database_code_depnum_ccdc_archive 'CCDC 850848' #TrackingRef '- ic14012-platon-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H40 Cl6 Co N8 O3 Pd3' _chemical_formula_weight 1283.64 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.4036(3) _cell_length_b 18.7413(2) _cell_length_c 23.7872(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8650.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25750 _cell_measurement_theta_min 3.1345 _cell_measurement_theta_max 30.1862 _exptl_crystal_description plate _exptl_crystal_colour dark_brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.971 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5064 _exptl_absorpt_coefficient_mu 2.011 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88748 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Oxford Diffraction Gemini A' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53323 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9916 _reflns_number_gt 7634 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0452P)^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 9916 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.064242(10) 0.752448(9) 0.386283(8) 0.01524(5) Uani 1 1 d . . . Pd2 Pd 0.151659(11) 0.737347(10) 0.463695(8) 0.01782(5) Uani 1 1 d . . . Pd3 Pd -0.015510(11) 0.727836(10) 0.468146(8) 0.01871(6) Uani 1 1 d . . . Cl1 Cl 0.16117(4) 0.61552(3) 0.46246(3) 0.02686(15) Uani 1 1 d . . . Cl2 Cl -0.02537(4) 0.84156(3) 0.50308(3) 0.03675(19) Uani 1 1 d . . . N1 N -0.01319(11) 0.79342(11) 0.32644(9) 0.0204(5) Uani 1 1 d . . . N2 N 0.06818(11) 0.85892(11) 0.40123(9) 0.0189(5) Uani 1 1 d . . . N3 N 0.15259(11) 0.84446(11) 0.46879(9) 0.0195(5) Uani 1 1 d . . . N4 N 0.22802(12) 0.75041(12) 0.52392(9) 0.0233(5) Uani 1 1 d . . . N5 N 0.14013(11) 0.74311(11) 0.31813(9) 0.0191(5) Uani 1 1 d . . . N6 N 0.05930(10) 0.64704(10) 0.36822(8) 0.0157(4) Uani 1 1 d . . . N7 N -0.01870(11) 0.62637(10) 0.44020(9) 0.0165(4) Uani 1 1 d . . . N8 N -0.08373(12) 0.68382(12) 0.52659(9) 0.0229(5) Uani 1 1 d . . . C1 C -0.04979(15) 0.75846(14) 0.28825(12) 0.0262(6) Uani 1 1 d . . . H1A H -0.0418 0.7088 0.2833 0.031 Uiso 1 1 calc R . . C2 C -0.09902(16) 0.79142(16) 0.25539(13) 0.0343(7) Uani 1 1 d . . . H2A H -0.1239 0.7651 0.2279 0.041 Uiso 1 1 calc R . . C3 C -0.11159(16) 0.86299(16) 0.26299(13) 0.0363(7) Uani 1 1 d . . . H3A H -0.1466 0.8864 0.2420 0.044 Uiso 1 1 calc R . . C4 C -0.07229(15) 0.90067(16) 0.30186(13) 0.0325(7) Uani 1 1 d . . . H4A H -0.0795 0.9503 0.3075 0.039 Uiso 1 1 calc R . . C5 C -0.02242(14) 0.86429(14) 0.33217(11) 0.0234(6) Uani 1 1 d . . . C6 C 0.02486(15) 0.90030(14) 0.37170(12) 0.0254(6) Uani 1 1 d . . . C7 C 0.02525(18) 0.97492(15) 0.37806(15) 0.0402(8) Uani 1 1 d . . . H7A H -0.0054 1.0033 0.3564 0.048 Uiso 1 1 calc R . . C8 C 0.06866(17) 1.00648(15) 0.41454(15) 0.0402(8) Uani 1 1 d . . . H8A H 0.0689 1.0569 0.4185 0.048 Uiso 1 1 calc R . . C9 C 0.11370(16) 0.96421(14) 0.44681(13) 0.0312(7) Uani 1 1 d . . . C10 C 0.11176(14) 0.88971(13) 0.43875(11) 0.0210(6) Uani 1 1 d . . . C11 C 0.15910(18) 0.99101(15) 0.48752(14) 0.0377(8) Uani 1 1 d . . . H11A H 0.1612 1.0409 0.4944 0.045 Uiso 1 1 calc R . . C12 C 0.20009(17) 0.94584(15) 0.51705(13) 0.0360(7) Uani 1 1 d . . . H12A H 0.2313 0.9639 0.5443 0.043 Uiso 1 1 calc R . . C13 C 0.19594(15) 0.87186(14) 0.50684(11) 0.0255(6) Uani 1 1 d . . . C14 C 0.23918(14) 0.81996(14) 0.53761(11) 0.0235(6) Uani 1 1 d . . . C15 C 0.28767(15) 0.83866(16) 0.57718(11) 0.0282(6) Uani 1 1 d . . . H15A H 0.2944 0.8873 0.5870 0.034 Uiso 1 1 calc R . . C16 C 0.32663(15) 0.78535(16) 0.60252(12) 0.0300(7) Uani 1 1 d . . . H16A H 0.3613 0.7973 0.6291 0.036 Uiso 1 1 calc R . . C17 C 0.31461(16) 0.71510(16) 0.58869(12) 0.0326(7) Uani 1 1 d . . . H17A H 0.3404 0.6779 0.6058 0.039 Uiso 1 1 calc R . . C18 C 0.26427(15) 0.69973(16) 0.54932(12) 0.0295(7) Uani 1 1 d . . . H18A H 0.2553 0.6513 0.5402 0.035 Uiso 1 1 calc R . . C19 C 0.17759(14) 0.79434(14) 0.29414(11) 0.0241(6) Uani 1 1 d . . . H19A H 0.1738 0.8418 0.3079 0.029 Uiso 1 1 calc R . . C20 C 0.22189(15) 0.78076(15) 0.24980(12) 0.0301(7) Uani 1 1 d . . . H20A H 0.2469 0.8184 0.2326 0.036 Uiso 1 1 calc R . . C21 C 0.22888(16) 0.71171(16) 0.23121(13) 0.0337(7) Uani 1 1 d . . . H21A H 0.2603 0.7007 0.2018 0.040 Uiso 1 1 calc R . . C22 C 0.18947(15) 0.65805(15) 0.25590(11) 0.0282(6) Uani 1 1 d . . . H22A H 0.1934 0.6101 0.2434 0.034 Uiso 1 1 calc R . . C23 C 0.14444(14) 0.67554(13) 0.29890(11) 0.0199(5) Uani 1 1 d . . . C24 C 0.09884(13) 0.62331(13) 0.32606(10) 0.0184(5) Uani 1 1 d . . . C25 C 0.09622(15) 0.55151(14) 0.30834(11) 0.0236(6) Uani 1 1 d . . . H25A H 0.1252 0.5358 0.2786 0.028 Uiso 1 1 calc R . . C26 C 0.05256(14) 0.50484(13) 0.33357(12) 0.0228(6) Uani 1 1 d . . . H26A H 0.0496 0.4569 0.3208 0.027 Uiso 1 1 calc R . . C27 C 0.01188(14) 0.52826(13) 0.37879(11) 0.0195(5) Uani 1 1 d . . . C28 C 0.01715(13) 0.60047(12) 0.39547(10) 0.0167(5) Uani 1 1 d . . . C29 C -0.03426(15) 0.48414(13) 0.40820(11) 0.0233(6) Uani 1 1 d . . . H29A H -0.0404 0.4358 0.3972 0.028 Uiso 1 1 calc R . . C30 C -0.07017(14) 0.51110(14) 0.45262(11) 0.0232(6) Uani 1 1 d . . . H30A H -0.1014 0.4816 0.4728 0.028 Uiso 1 1 calc R . . C31 C -0.06097(13) 0.58228(14) 0.46851(10) 0.0194(5) Uani 1 1 d . . . C32 C -0.09700(14) 0.61403(14) 0.51715(11) 0.0205(5) Uani 1 1 d . . . C33 C -0.14192(15) 0.57615(15) 0.55120(11) 0.0270(6) Uani 1 1 d . . . H33A H -0.1507 0.5271 0.5442 0.032 Uiso 1 1 calc R . . C34 C -0.17366(16) 0.61061(16) 0.59541(12) 0.0322(7) Uani 1 1 d . . . H34A H -0.2042 0.5854 0.6195 0.039 Uiso 1 1 calc R . . C35 C -0.16062(16) 0.68169(17) 0.60428(12) 0.0341(7) Uani 1 1 d . . . H35A H -0.1828 0.7066 0.6340 0.041 Uiso 1 1 calc R . . C36 C -0.11470(16) 0.71643(15) 0.56938(12) 0.0305(7) Uani 1 1 d . . . H36A H -0.1049 0.7653 0.5762 0.037 Uiso 1 1 calc R . . Co1 Co -0.168105(19) 0.479450(18) 0.288425(15) 0.02324(9) Uani 1 1 d . . . Cl3 Cl -0.12576(4) 0.59269(4) 0.29232(3) 0.04008(19) Uani 1 1 d . . . Cl4 Cl -0.23048(5) 0.45615(5) 0.36684(4) 0.0527(2) Uani 1 1 d . . . Cl5 Cl -0.23759(4) 0.47210(4) 0.21140(3) 0.03811(19) Uani 1 1 d . . . Cl6 Cl -0.07926(4) 0.40203(5) 0.27926(4) 0.0462(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01913(11) 0.01196(8) 0.01462(9) -0.00040(7) -0.00049(8) -0.00023(7) Pd2 0.02289(12) 0.01391(9) 0.01665(10) 0.00008(7) -0.00344(8) -0.00107(7) Pd3 0.02402(12) 0.01498(9) 0.01713(10) -0.00284(7) 0.00359(8) -0.00149(8) Cl1 0.0348(4) 0.0150(3) 0.0308(4) 0.0034(3) -0.0093(3) -0.0011(3) Cl2 0.0514(5) 0.0201(3) 0.0387(4) -0.0115(3) 0.0197(4) -0.0046(3) N1 0.0210(12) 0.0187(10) 0.0214(11) 0.0040(9) -0.0020(10) -0.0009(9) N2 0.0226(12) 0.0134(9) 0.0208(11) -0.0019(8) -0.0007(9) -0.0003(9) N3 0.0224(12) 0.0168(10) 0.0194(11) -0.0028(8) -0.0023(9) -0.0017(9) N4 0.0280(13) 0.0214(10) 0.0204(11) 0.0016(9) -0.0055(10) -0.0046(10) N5 0.0176(12) 0.0205(10) 0.0192(11) 0.0012(9) -0.0012(9) -0.0010(9) N6 0.0179(12) 0.0145(9) 0.0148(10) -0.0015(8) -0.0008(9) -0.0002(8) N7 0.0184(11) 0.0139(9) 0.0173(10) -0.0013(8) -0.0006(9) -0.0007(8) N8 0.0271(13) 0.0243(11) 0.0174(11) -0.0009(9) 0.0042(10) -0.0012(10) C1 0.0259(16) 0.0257(14) 0.0270(15) 0.0036(12) -0.0031(12) -0.0070(11) C2 0.0319(18) 0.0366(16) 0.0344(17) 0.0106(14) -0.0107(14) -0.0125(13) C3 0.0300(18) 0.0378(16) 0.0413(18) 0.0204(14) -0.0112(15) -0.0068(13) C4 0.0318(18) 0.0261(14) 0.0396(18) 0.0117(13) -0.0069(14) 0.0003(12) C5 0.0222(15) 0.0223(13) 0.0257(14) 0.0063(11) -0.0014(12) 0.0005(11) C6 0.0298(17) 0.0176(12) 0.0289(15) 0.0012(11) 0.0000(13) 0.0015(11) C7 0.045(2) 0.0186(13) 0.057(2) 0.0013(14) -0.0172(17) 0.0062(13) C8 0.052(2) 0.0151(13) 0.054(2) -0.0076(14) -0.0103(17) 0.0055(13) C9 0.0412(19) 0.0179(12) 0.0345(16) -0.0050(12) -0.0044(14) 0.0006(12) C10 0.0261(16) 0.0171(11) 0.0199(13) -0.0025(10) -0.0017(11) 0.0004(11) C11 0.053(2) 0.0175(13) 0.0425(18) -0.0094(13) -0.0124(16) -0.0027(13) C12 0.049(2) 0.0238(14) 0.0349(17) -0.0092(13) -0.0121(15) -0.0070(14) C13 0.0321(17) 0.0245(13) 0.0201(13) -0.0035(11) -0.0016(12) -0.0043(12) C14 0.0236(15) 0.0259(13) 0.0210(13) -0.0015(11) -0.0002(11) -0.0051(11) C15 0.0295(17) 0.0361(15) 0.0190(13) -0.0026(12) -0.0007(12) -0.0102(13) C16 0.0256(16) 0.0443(17) 0.0200(14) 0.0001(12) -0.0014(12) -0.0042(13) C17 0.0309(18) 0.0396(17) 0.0272(15) 0.0055(13) -0.0087(13) 0.0013(14) C18 0.0321(17) 0.0283(14) 0.0281(15) 0.0012(12) -0.0076(13) -0.0008(13) C19 0.0224(15) 0.0228(13) 0.0270(14) 0.0045(11) -0.0025(12) -0.0004(11) C20 0.0271(17) 0.0322(15) 0.0310(15) 0.0066(13) 0.0065(13) -0.0024(12) C21 0.0335(18) 0.0381(16) 0.0294(16) -0.0012(13) 0.0112(14) -0.0035(13) C22 0.0313(17) 0.0283(14) 0.0249(14) -0.0061(12) 0.0068(13) 0.0019(12) C23 0.0201(15) 0.0196(12) 0.0200(13) -0.0003(10) -0.0010(11) 0.0004(10) C24 0.0200(14) 0.0193(12) 0.0157(12) -0.0011(10) -0.0013(11) 0.0018(10) C25 0.0262(16) 0.0223(13) 0.0223(14) -0.0059(11) 0.0034(12) 0.0017(11) C26 0.0261(16) 0.0161(12) 0.0263(14) -0.0077(11) 0.0005(12) -0.0013(10) C27 0.0216(14) 0.0176(11) 0.0192(13) -0.0026(10) -0.0026(11) -0.0004(10) C28 0.0200(14) 0.0150(11) 0.0151(12) 0.0001(9) -0.0041(10) -0.0015(10) C29 0.0317(16) 0.0145(12) 0.0238(14) -0.0001(10) -0.0046(12) -0.0043(11) C30 0.0251(16) 0.0216(13) 0.0231(14) 0.0023(11) 0.0016(12) -0.0044(11) C31 0.0205(15) 0.0202(12) 0.0177(13) 0.0031(10) -0.0018(11) -0.0015(10) C32 0.0226(15) 0.0223(12) 0.0167(13) 0.0037(10) -0.0017(11) 0.0004(11) C33 0.0315(17) 0.0258(13) 0.0237(14) 0.0051(11) 0.0025(12) 0.0005(12) C34 0.0351(18) 0.0371(16) 0.0244(15) 0.0093(13) 0.0084(13) -0.0013(13) C35 0.0404(19) 0.0394(17) 0.0225(15) -0.0037(13) 0.0113(13) -0.0001(14) C36 0.0383(18) 0.0295(14) 0.0237(14) -0.0057(12) 0.0089(13) -0.0006(13) Co1 0.0253(2) 0.02089(18) 0.02357(19) -0.00340(14) -0.00025(16) -0.00084(15) Cl3 0.0473(5) 0.0243(3) 0.0487(5) -0.0006(3) -0.0105(4) -0.0100(3) Cl4 0.0722(7) 0.0428(5) 0.0431(5) -0.0053(4) 0.0299(5) -0.0060(4) Cl5 0.0447(5) 0.0269(3) 0.0428(4) -0.0041(3) -0.0206(4) 0.0022(3) Cl6 0.0301(5) 0.0509(5) 0.0577(5) -0.0303(4) -0.0115(4) 0.0128(4) _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 N6 2.024(2) . ? Pd1 N2 2.028(2) . ? Pd1 N5 2.197(2) . ? Pd1 N1 2.208(2) . ? Pd1 Pd2 2.5195(3) . ? Pd1 Pd3 2.5297(3) . ? Pd2 N3 2.011(2) . ? Pd2 N4 2.076(2) . ? Pd2 Cl1 2.2908(6) . ? Pd2 Pd3 3.2503(3) . ? Pd3 N7 2.0154(19) . ? Pd3 N8 2.089(2) . ? Pd3 Cl2 2.2955(7) . ? N1 C1 1.326(3) . ? N1 C5 1.347(3) . ? N2 C6 1.342(3) . ? N2 C10 1.358(3) . ? N3 C13 1.338(3) . ? N3 C10 1.363(3) . ? N4 C18 1.327(4) . ? N4 C14 1.361(3) . ? N5 C19 1.332(3) . ? N5 C23 1.349(3) . ? N6 C24 1.339(3) . ? N6 C28 1.360(3) . ? N7 C31 1.345(3) . ? N7 C28 1.361(3) . ? N8 C36 1.331(3) . ? N8 C32 1.352(3) . ? C1 C2 1.380(4) . ? C2 C3 1.375(4) . ? C3 C4 1.391(4) . ? C4 C5 1.386(4) . ? C5 C6 1.477(4) . ? C6 C7 1.407(4) . ? C7 C8 1.346(4) . ? C8 C9 1.407(4) . ? C9 C11 1.402(4) . ? C9 C10 1.410(3) . ? C11 C12 1.357(4) . ? C12 C13 1.410(4) . ? C13 C14 1.479(4) . ? C14 C15 1.376(4) . ? C15 C16 1.390(4) . ? C16 C17 1.377(4) . ? C17 C18 1.384(4) . ? C19 C20 1.384(4) . ? C20 C21 1.374(4) . ? C21 C22 1.393(4) . ? C22 C23 1.385(4) . ? C23 C24 1.469(4) . ? C24 C25 1.411(3) . ? C25 C26 1.358(4) . ? C26 C27 1.405(4) . ? C27 C29 1.405(4) . ? C27 C28 1.414(3) . ? C29 C30 1.363(4) . ? C30 C31 1.398(4) . ? C31 C32 1.477(4) . ? C32 C33 1.386(4) . ? C33 C34 1.379(4) . ? C34 C35 1.372(4) . ? C35 C36 1.381(4) . ? Co1 Cl6 2.2638(9) . ? Co1 Cl4 2.2660(9) . ? Co1 Cl3 2.2776(8) . ? Co1 Cl5 2.2791(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Pd1 N2 177.76(8) . . ? N6 Pd1 N5 78.31(8) . . ? N2 Pd1 N5 100.51(8) . . ? N6 Pd1 N1 99.81(8) . . ? N2 Pd1 N1 78.26(8) . . ? N5 Pd1 N1 90.46(8) . . ? N6 Pd1 Pd2 94.44(6) . . ? N2 Pd1 Pd2 87.54(6) . . ? N5 Pd1 Pd2 94.54(6) . . ? N1 Pd1 Pd2 165.59(6) . . ? N6 Pd1 Pd3 87.51(6) . . ? N2 Pd1 Pd3 93.87(6) . . ? N5 Pd1 Pd3 164.47(5) . . ? N1 Pd1 Pd3 98.25(6) . . ? Pd2 Pd1 Pd3 80.139(9) . . ? N3 Pd2 N4 80.46(9) . . ? N3 Pd2 Cl1 174.19(6) . . ? N4 Pd2 Cl1 93.95(6) . . ? N3 Pd2 Pd1 86.44(6) . . ? N4 Pd2 Pd1 166.37(6) . . ? Cl1 Pd2 Pd1 99.022(18) . . ? N3 Pd2 Pd3 93.54(6) . . ? N4 Pd2 Pd3 134.14(7) . . ? Cl1 Pd2 Pd3 91.498(19) . . ? Pd1 Pd2 Pd3 50.067(7) . . ? N7 Pd3 N8 80.06(9) . . ? N7 Pd3 Cl2 173.15(6) . . ? N8 Pd3 Cl2 94.18(6) . . ? N7 Pd3 Pd1 86.39(6) . . ? N8 Pd3 Pd1 166.35(6) . . ? Cl2 Pd3 Pd1 99.23(2) . . ? N7 Pd3 Pd2 94.11(6) . . ? N8 Pd3 Pd2 132.50(6) . . ? Cl2 Pd3 Pd2 92.53(2) . . ? Pd1 Pd3 Pd2 49.793(6) . . ? C1 N1 C5 119.0(2) . . ? C1 N1 Pd1 129.36(18) . . ? C5 N1 Pd1 111.60(17) . . ? C6 N2 C10 119.2(2) . . ? C6 N2 Pd1 116.95(17) . . ? C10 N2 Pd1 123.82(17) . . ? C13 N3 C10 118.8(2) . . ? C13 N3 Pd2 115.44(17) . . ? C10 N3 Pd2 125.75(17) . . ? C18 N4 C14 119.5(2) . . ? C18 N4 Pd2 127.44(19) . . ? C14 N4 Pd2 113.06(18) . . ? C19 N5 C23 119.8(2) . . ? C19 N5 Pd1 128.62(18) . . ? C23 N5 Pd1 111.49(16) . . ? C24 N6 C28 119.2(2) . . ? C24 N6 Pd1 117.14(16) . . ? C28 N6 Pd1 123.61(16) . . ? C31 N7 C28 119.0(2) . . ? C31 N7 Pd3 115.68(17) . . ? C28 N7 Pd3 125.36(16) . . ? C36 N8 C32 119.0(2) . . ? C36 N8 Pd3 127.86(19) . . ? C32 N8 Pd3 113.08(17) . . ? N1 C1 C2 122.5(3) . . ? C3 C2 C1 119.0(3) . . ? C2 C3 C4 119.0(3) . . ? C5 C4 C3 118.6(3) . . ? N1 C5 C4 121.7(3) . . ? N1 C5 C6 115.6(2) . . ? C4 C5 C6 122.7(3) . . ? N2 C6 C7 121.0(3) . . ? N2 C6 C5 117.3(2) . . ? C7 C6 C5 121.7(3) . . ? C8 C7 C6 120.6(3) . . ? C7 C8 C9 119.5(3) . . ? C11 C9 C8 124.4(3) . . ? C11 C9 C10 117.7(3) . . ? C8 C9 C10 117.8(3) . . ? N2 C10 N3 116.2(2) . . ? N2 C10 C9 121.8(2) . . ? N3 C10 C9 122.0(2) . . ? C12 C11 C9 120.1(3) . . ? C11 C12 C13 119.4(3) . . ? N3 C13 C12 122.0(3) . . ? N3 C13 C14 116.0(2) . . ? C12 C13 C14 122.0(2) . . ? N4 C14 C15 121.1(3) . . ? N4 C14 C13 114.9(2) . . ? C15 C14 C13 124.0(3) . . ? C14 C15 C16 119.0(3) . . ? C17 C16 C15 119.4(3) . . ? C16 C17 C18 118.7(3) . . ? N4 C18 C17 122.2(3) . . ? N5 C19 C20 122.2(3) . . ? C21 C20 C19 118.7(3) . . ? C20 C21 C22 119.3(3) . . ? C23 C22 C21 119.1(3) . . ? N5 C23 C22 120.8(2) . . ? N5 C23 C24 116.0(2) . . ? C22 C23 C24 123.2(2) . . ? N6 C24 C25 121.3(2) . . ? N6 C24 C23 117.0(2) . . ? C25 C24 C23 121.7(2) . . ? C26 C25 C24 120.3(2) . . ? C25 C26 C27 119.2(2) . . ? C26 C27 C29 123.8(2) . . ? C26 C27 C28 118.2(2) . . ? C29 C27 C28 118.0(2) . . ? N6 C28 N7 116.8(2) . . ? N6 C28 C27 121.6(2) . . ? N7 C28 C27 121.6(2) . . ? C30 C29 C27 119.6(2) . . ? C29 C30 C31 119.9(2) . . ? N7 C31 C30 121.9(2) . . ? N7 C31 C32 115.7(2) . . ? C30 C31 C32 122.4(2) . . ? N8 C32 C33 121.2(2) . . ? N8 C32 C31 115.5(2) . . ? C33 C32 C31 123.3(2) . . ? C34 C33 C32 119.1(3) . . ? C35 C34 C33 119.3(3) . . ? C34 C35 C36 119.0(3) . . ? N8 C36 C35 122.3(3) . . ? Cl6 Co1 Cl4 111.25(4) . . ? Cl6 Co1 Cl3 109.05(4) . . ? Cl4 Co1 Cl3 109.80(3) . . ? Cl6 Co1 Cl5 109.53(3) . . ? Cl4 Co1 Cl5 109.52(4) . . ? Cl3 Co1 Cl5 107.60(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.717 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.086 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.495 0.176 0.138 176 33 ' ' 2 0.995 0.176 0.362 176 33 ' ' 3 0.495 0.324 0.638 176 33 ' ' 4 0.995 0.324 0.862 176 33 ' ' 5 0.005 0.676 0.138 176 33 ' ' 6 0.505 0.676 0.362 176 33 ' ' 7 0.005 0.824 0.638 176 33 ' ' 8 0.505 0.824 0.862 176 33 ' ' _platon_squeeze_details ; PLATON/SQUEEZE was used to treat two Ethanol and one Methanol molecules in the asymmetric unit. These were removed from the model, but included in the empirical formula. PLATON / Squeeze results (Spek, 2009): Total Potential Solvent Area Vol 1430.7 Ang^3 per Unit Cell Vol 8650.2 Ang^3 [16.5%] Total Potential Solvent Accessible Void Vol: 1430.7 Ang^3 Electron Count / Cell = 267 - To be included in D(calc), F000 & Mol.Wght. Correction - Since two Ethanol and one Methanol with electron count = 70 were removed, then 70 electron will be added into F000. The empirical formula is correct. ;