# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Marius Andruh' _publ_contact_author_email marius.andruh@dnt.ro loop_ _publ_author_name 'Augustin M. Madalan' 'Narcis Avarvari' 'Marius Andruh' data_mam107 _database_code_depnum_ccdc_archive 'CCDC 293152' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H35 Cl Cu N4 O11 Pd' _chemical_formula_weight 869.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.987 _cell_length_b 36.016 _cell_length_c 8.417 _cell_angle_alpha 90.00 _cell_angle_beta 105.49 _cell_angle_gamma 90.00 _cell_volume 3501.8 _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 215 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1764 _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.677792 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type area_detector _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19313 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.1469 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7689 _reflns_number_gt 3636 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'Denzo and Scalepak' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+0.0186P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7689 _refine_ls_number_parameters 468 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1762 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1481 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6992(5) 0.25984(17) 0.4544(7) 0.0648(18) Uani 1 1 d . . . H1A H 0.6249 0.2647 0.3793 0.097 Uiso 1 1 calc R . . H1B H 0.7442 0.2822 0.4720 0.097 Uiso 1 1 calc R . . H1C H 0.6889 0.2513 0.5575 0.097 Uiso 1 1 calc R . . C2 C 0.8671(5) 0.22183(17) 0.4742(7) 0.0476(15) Uani 1 1 d . . . C3 C 0.9306(6) 0.24111(19) 0.6108(7) 0.0613(18) Uani 1 1 d . . . H3 H 0.9017 0.2628 0.6449 0.074 Uiso 1 1 calc R . . C4 C 1.0404(6) 0.2271(2) 0.6975(8) 0.075(2) Uani 1 1 d . . . H4 H 1.0826 0.2392 0.7920 0.090 Uiso 1 1 calc R . . C5 C 1.0842(5) 0.1968(2) 0.6453(8) 0.068(2) Uani 1 1 d . . . H5 H 1.1576 0.1887 0.7025 0.082 Uiso 1 1 calc R . . C6 C 1.0222(5) 0.17683(19) 0.5060(7) 0.0529(17) Uani 1 1 d . . . C7 C 0.9096(5) 0.18939(17) 0.4173(7) 0.0444(15) Uani 1 1 d . . . C8 C 1.0723(6) 0.1434(2) 0.4667(9) 0.068(2) Uani 1 1 d . . . H8 H 1.1470 0.1382 0.5299 0.082 Uiso 1 1 calc R . . C9 C 1.0922(7) 0.0869(2) 0.3244(10) 0.097(3) Uani 1 1 d . . . H9A H 1.1391 0.0935 0.2509 0.117 Uiso 1 1 calc R . . H9B H 1.1433 0.0781 0.4272 0.117 Uiso 1 1 calc R . . C10 C 1.0114(7) 0.0579(2) 0.2505(12) 0.107(3) Uani 1 1 d . . . H10A H 0.9925 0.0433 0.3367 0.128 Uiso 1 1 calc R . . H10B H 1.0473 0.0415 0.1871 0.128 Uiso 1 1 calc R . . C11 C 0.8382(7) 0.05424(19) 0.0249(10) 0.068(2) Uani 1 1 d . . . H11 H 0.8656 0.0312 0.0029 0.082 Uiso 1 1 calc R . . C12 C 0.7268(7) 0.06523(18) -0.0738(8) 0.0589(18) Uani 1 1 d . . . C13 C 0.6688(8) 0.0396(2) -0.1971(10) 0.082(2) Uani 1 1 d . . . H13 H 0.7054 0.0177 -0.2129 0.099 Uiso 1 1 calc R . . C14 C 0.5596(9) 0.0471(2) -0.2926(9) 0.087(3) Uani 1 1 d . . . H14 H 0.5226 0.0302 -0.3732 0.105 Uiso 1 1 calc R . . C15 C 0.5035(7) 0.0794(2) -0.2707(8) 0.074(2) Uani 1 1 d . . . H15 H 0.4291 0.0840 -0.3361 0.089 Uiso 1 1 calc R . . C16 C 0.5570(6) 0.1048(2) -0.1526(7) 0.0604(18) Uani 1 1 d . . . C17 C 0.6710(6) 0.09848(19) -0.0519(7) 0.0519(16) Uani 1 1 d . . . C18 C 0.3911(6) 0.1443(2) -0.1948(8) 0.085(2) Uani 1 1 d . . . H18A H 0.3706 0.1683 -0.1618 0.128 Uiso 1 1 calc R . . H18B H 0.3443 0.1257 -0.1623 0.128 Uiso 1 1 calc R . . H18C H 0.3781 0.1438 -0.3124 0.128 Uiso 1 1 calc R . . C19 C 0.7200(5) 0.16488(17) 0.6585(7) 0.0499(15) Uani 1 1 d . . . H19 H 0.6833 0.1869 0.6729 0.060 Uiso 1 1 calc R . . C20 C 0.8276(5) 0.15746(19) 0.7596(7) 0.0538(17) Uani 1 1 d . . . H20 H 0.8629 0.1740 0.8428 0.065 Uiso 1 1 calc R . . C21 C 0.8822(6) 0.1257(2) 0.7369(8) 0.0621(19) Uani 1 1 d . . . H21 H 0.9560 0.1205 0.8032 0.074 Uiso 1 1 calc R . . C22 C 0.8290(5) 0.10149(18) 0.6180(8) 0.0514(16) Uani 1 1 d . . . H22 H 0.8658 0.0795 0.6036 0.062 Uiso 1 1 calc R . . C23 C 0.7199(5) 0.10944(16) 0.5177(7) 0.0439(15) Uani 1 1 d . . . C24 C 0.6505(5) 0.08509(15) 0.3889(7) 0.0415(14) Uani 1 1 d . . . C25 C 0.6864(6) 0.05054(17) 0.3503(8) 0.0563(17) Uani 1 1 d . . . H25 H 0.7595 0.0417 0.4043 0.068 Uiso 1 1 calc R . . C26 C 0.6122(7) 0.02939(18) 0.2303(9) 0.0677(19) Uani 1 1 d . . . H26 H 0.6349 0.0061 0.2033 0.081 Uiso 1 1 calc R . . C27 C 0.5055(7) 0.04295(17) 0.1519(8) 0.0630(19) Uani 1 1 d . . . H27 H 0.4542 0.0290 0.0716 0.076 Uiso 1 1 calc R . . C28 C 0.4753(5) 0.07785(17) 0.1944(7) 0.0531(16) Uani 1 1 d . . . H28 H 0.4029 0.0873 0.1403 0.064 Uiso 1 1 calc R . . C29 C 0.1690(5) 0.16770(19) 0.0990(7) 0.071(2) Uani 1 1 d . . . H29A H 0.1771 0.1476 0.0282 0.106 Uiso 1 1 calc R . . H29B H 0.1538 0.1903 0.0361 0.106 Uiso 1 1 calc R . . H29C H 0.1058 0.1626 0.1459 0.106 Uiso 1 1 calc R . . C30 C 0.2785(5) 0.17183(18) 0.2343(7) 0.0491(16) Uani 1 1 d . . . C31 C 0.2891(5) 0.19954(18) 0.3485(8) 0.0598(17) Uani 1 1 d . . . H31 H 0.2225 0.2131 0.3451 0.072 Uiso 1 1 calc R . . C32 C 0.3881(5) 0.20973(16) 0.4689(7) 0.0498(16) Uani 1 1 d . . . C33 C 0.3862(6) 0.24173(19) 0.5781(8) 0.084(2) Uani 1 1 d . . . H33A H 0.4617 0.2451 0.6521 0.126 Uiso 1 1 calc R . . H33B H 0.3312 0.2372 0.6404 0.126 Uiso 1 1 calc R . . H33C H 0.3644 0.2637 0.5127 0.126 Uiso 1 1 calc R . . N1 N 1.0275(4) 0.11968(16) 0.3556(7) 0.0574(14) Uani 1 1 d . . . N2 N 0.9041(5) 0.07354(15) 0.1416(7) 0.0640(15) Uani 1 1 d . . . N3 N 0.6662(4) 0.14142(13) 0.5399(5) 0.0418(12) Uani 1 1 d . . . N4 N 0.5453(4) 0.09844(12) 0.3092(5) 0.0440(12) Uani 1 1 d . . . O1 O 0.7580(3) 0.23202(11) 0.3862(4) 0.0527(10) Uani 1 1 d . . . O2 O 0.8420(3) 0.17326(10) 0.2870(4) 0.0462(10) Uani 1 1 d . . . O1W O 0.5865(5) 0.17996(16) 0.1887(7) 0.0514(12) Uani 1 1 d . . . O3 O 0.5092(4) 0.13721(14) -0.1182(5) 0.0666(13) Uani 1 1 d . . . O4 O 0.7136(3) 0.12467(11) 0.0566(4) 0.0492(10) Uani 1 1 d . . . O5 O 0.3584(3) 0.14896(12) 0.2317(5) 0.0588(11) Uani 1 1 d . . . O6 O 0.4847(3) 0.19302(11) 0.4938(4) 0.0551(11) Uani 1 1 d . . . O7 O 0.2201(7) 0.0404(2) 0.9535(11) 0.209(4) Uani 1 1 d . . . O8 O 0.1459(6) 0.08849(17) 0.7882(11) 0.183(4) Uani 1 1 d . . . O9 O 0.0368(6) 0.03983(18) 0.8005(13) 0.209(4) Uani 1 1 d . . . O10 O 0.1844(11) 0.0353(3) 0.6996(12) 0.282(6) Uani 1 1 d . . . Pd1 Pd 0.87139(4) 0.122864(13) 0.20871(5) 0.04750(18) Uani 1 1 d . . . Cu2 Cu 0.51329(6) 0.149695(19) 0.37644(8) 0.0454(2) Uani 1 1 d . . . Cl3 Cl 0.14672(17) 0.05152(6) 0.8162(3) 0.0792(6) Uani 1 1 d . . . H1W H 0.649(5) 0.1860(15) 0.233(6) 0.04(2) Uiso 1 1 d . . . H2W H 0.593(8) 0.165(2) 0.139(10) 0.12(5) 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 C1 0.069(5) 0.052(4) 0.072(4) -0.009(4) 0.016(4) 0.004(4) C2 0.053(4) 0.055(4) 0.034(3) 0.001(3) 0.011(3) -0.018(4) C3 0.067(5) 0.069(5) 0.049(4) -0.007(4) 0.018(4) -0.017(4) C4 0.064(5) 0.100(6) 0.052(4) -0.006(5) -0.002(4) -0.040(5) C5 0.041(4) 0.098(6) 0.061(5) 0.005(5) 0.005(4) -0.012(4) C6 0.041(4) 0.072(5) 0.046(4) 0.004(4) 0.013(3) -0.011(4) C7 0.039(4) 0.057(4) 0.038(3) 0.004(3) 0.012(3) -0.012(3) C8 0.039(4) 0.104(7) 0.057(5) 0.019(5) 0.006(4) 0.004(4) C9 0.084(6) 0.089(6) 0.116(7) 0.024(6) 0.021(5) 0.041(6) C10 0.071(6) 0.065(5) 0.185(9) 0.008(6) 0.036(6) 0.016(5) C11 0.073(5) 0.046(4) 0.102(6) -0.007(4) 0.051(5) 0.004(4) C12 0.087(6) 0.045(4) 0.060(4) -0.010(4) 0.046(4) -0.015(4) C13 0.120(7) 0.064(5) 0.078(6) -0.011(5) 0.052(5) -0.024(6) C14 0.141(9) 0.072(6) 0.055(5) -0.023(5) 0.036(5) -0.056(6) C15 0.089(6) 0.086(6) 0.046(4) 0.001(4) 0.016(4) -0.045(5) C16 0.078(5) 0.064(5) 0.040(4) 0.002(4) 0.018(4) -0.021(5) C17 0.057(4) 0.065(5) 0.038(4) -0.004(4) 0.021(3) -0.018(4) C18 0.059(5) 0.115(7) 0.067(5) 0.008(5) -0.009(4) -0.002(5) C19 0.050(4) 0.042(4) 0.061(4) 0.004(3) 0.021(3) 0.000(3) C20 0.048(4) 0.067(5) 0.043(4) 0.002(3) 0.005(3) -0.010(4) C21 0.044(4) 0.073(5) 0.063(5) 0.020(4) 0.003(3) 0.002(4) C22 0.040(4) 0.055(4) 0.062(4) 0.011(4) 0.017(3) 0.010(3) C23 0.047(4) 0.046(4) 0.045(4) 0.012(3) 0.022(3) 0.003(3) C24 0.056(4) 0.033(3) 0.043(4) 0.004(3) 0.026(3) 0.004(3) C25 0.071(5) 0.050(4) 0.055(4) 0.014(3) 0.029(4) 0.014(4) C26 0.091(6) 0.045(4) 0.073(5) 0.002(4) 0.032(4) 0.012(4) C27 0.091(6) 0.047(4) 0.058(4) -0.016(4) 0.031(4) -0.014(4) C28 0.062(4) 0.051(4) 0.050(4) -0.002(3) 0.021(3) -0.010(4) C29 0.047(4) 0.093(5) 0.064(4) 0.012(4) 0.001(3) 0.000(4) C30 0.038(4) 0.057(4) 0.052(4) 0.012(4) 0.011(3) 0.001(3) C31 0.047(4) 0.061(5) 0.074(5) 0.008(4) 0.021(4) 0.015(4) C32 0.053(4) 0.042(4) 0.062(4) 0.002(3) 0.028(4) 0.002(3) C33 0.084(5) 0.074(5) 0.099(5) -0.028(4) 0.033(4) 0.024(4) N1 0.047(3) 0.070(4) 0.055(3) 0.013(3) 0.014(3) 0.014(3) N2 0.064(4) 0.054(4) 0.080(4) 0.005(3) 0.031(3) -0.001(3) N3 0.046(3) 0.042(3) 0.038(3) 0.004(2) 0.013(2) 0.001(3) N4 0.051(3) 0.040(3) 0.042(3) 0.000(2) 0.015(2) -0.001(3) O1 0.048(3) 0.062(3) 0.043(2) -0.010(2) 0.005(2) -0.001(2) O2 0.041(2) 0.053(3) 0.037(2) -0.003(2) -0.0014(18) 0.003(2) O1W 0.045(3) 0.051(3) 0.056(3) 0.000(3) 0.010(3) -0.002(3) O3 0.054(3) 0.082(3) 0.056(3) -0.005(3) 0.000(2) -0.004(3) O4 0.049(2) 0.055(3) 0.043(2) -0.010(2) 0.0112(19) -0.001(2) O5 0.044(3) 0.063(3) 0.064(3) -0.016(2) 0.005(2) 0.001(2) O6 0.043(2) 0.053(3) 0.067(3) -0.017(2) 0.012(2) 0.007(2) O7 0.185(8) 0.172(8) 0.193(7) 0.038(6) -0.081(6) 0.016(6) O8 0.118(5) 0.073(4) 0.345(11) 0.059(6) 0.038(6) 0.013(4) O9 0.073(5) 0.117(6) 0.423(13) 0.024(7) 0.042(6) 0.002(4) O10 0.374(15) 0.295(13) 0.210(9) 0.041(8) 0.132(10) 0.216(12) Pd1 0.0459(3) 0.0509(3) 0.0491(3) 0.0031(3) 0.0186(2) 0.0009(3) Cu2 0.0396(4) 0.0437(4) 0.0519(5) -0.0068(4) 0.0105(3) 0.0044(4) Cl3 0.0561(13) 0.0661(13) 0.1104(17) 0.0133(13) 0.0139(11) 0.0152(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.431(6) . ? C2 O1 1.370(6) . ? C2 C3 1.384(7) . ? C2 C7 1.409(8) . ? C3 C4 1.416(9) . ? C4 C5 1.336(9) . ? C5 C6 1.407(8) . ? C6 C8 1.424(9) . ? C6 C7 1.430(8) . ? C7 O2 1.312(6) . ? C8 N1 1.274(8) . ? C9 C10 1.448(9) . ? C9 N1 1.474(8) . ? C10 N2 1.478(8) . ? C11 N2 1.288(8) . ? C11 C12 1.427(9) . ? C12 C17 1.407(8) . ? C12 C13 1.423(9) . ? C13 C14 1.368(10) . ? C14 C15 1.379(10) . ? C15 C16 1.378(8) . ? C16 O3 1.365(8) . ? C16 C17 1.421(8) . ? C17 O4 1.317(6) . ? C18 O3 1.413(7) . ? C19 N3 1.336(7) . ? C19 C20 1.369(7) . ? C20 C21 1.357(8) . ? C21 C22 1.351(8) . ? C22 C23 1.384(7) . ? C23 N3 1.356(7) . ? C23 C24 1.468(8) . ? C24 N4 1.348(7) . ? C24 C25 1.383(7) . ? C25 C26 1.382(8) . ? C26 C27 1.363(9) . ? C27 C28 1.382(7) . ? C28 N4 1.324(6) . ? C29 C30 1.499(7) . ? C30 O5 1.268(6) . ? C30 C31 1.368(8) . ? C31 C32 1.388(8) . ? C32 O6 1.272(6) . ? C32 C33 1.479(8) . ? N1 Pd1 1.951(5) . ? N2 Pd1 1.936(6) . ? N3 Cu2 1.998(4) . ? N4 Cu2 1.998(4) . ? O2 Pd1 1.994(4) . ? O1W Cu2 2.279(5) . ? O4 Pd1 1.982(4) . ? O5 Cu2 1.930(4) . ? O6 Cu2 1.926(4) . ? O7 Cl3 1.313(7) . ? O8 Cl3 1.352(6) . ? O9 Cl3 1.355(7) . ? O10 Cl3 1.321(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 O1 C2 C3 123.3(6) . . ? O1 C2 C7 114.7(5) . . ? C3 C2 C7 122.1(6) . . ? C2 C3 C4 118.6(7) . . ? C5 C4 C3 120.9(7) . . ? C4 C5 C6 121.7(7) . . ? C5 C6 C8 117.7(6) . . ? C5 C6 C7 119.2(6) . . ? C8 C6 C7 123.0(6) . . ? O2 C7 C2 116.9(5) . . ? O2 C7 C6 125.6(6) . . ? C2 C7 C6 117.4(6) . . ? N1 C8 C6 128.0(6) . . ? C10 C9 N1 109.4(7) . . ? C9 C10 N2 111.3(6) . . ? N2 C11 C12 125.6(6) . . ? C17 C12 C13 119.4(7) . . ? C17 C12 C11 124.3(6) . . ? C13 C12 C11 116.3(7) . . ? C14 C13 C12 120.3(8) . . ? C13 C14 C15 120.8(7) . . ? C16 C15 C14 120.5(8) . . ? O3 C16 C15 125.5(7) . . ? O3 C16 C17 113.7(6) . . ? C15 C16 C17 120.8(7) . . ? O4 C17 C12 126.2(6) . . ? O4 C17 C16 115.5(6) . . ? C12 C17 C16 118.2(6) . . ? N3 C19 C20 121.9(6) . . ? C21 C20 C19 119.1(6) . . ? C22 C21 C20 119.9(6) . . ? C21 C22 C23 120.0(6) . . ? N3 C23 C22 119.9(6) . . ? N3 C23 C24 114.4(5) . . ? C22 C23 C24 125.7(6) . . ? N4 C24 C25 120.8(6) . . ? N4 C24 C23 115.1(5) . . ? C25 C24 C23 124.1(6) . . ? C26 C25 C24 119.1(6) . . ? C27 C26 C25 119.6(6) . . ? C26 C27 C28 118.5(6) . . ? N4 C28 C27 122.6(6) . . ? O5 C30 C31 123.9(5) . . ? O5 C30 C29 115.8(6) . . ? C31 C30 C29 120.3(6) . . ? C30 C31 C32 127.3(6) . . ? O6 C32 C31 124.0(5) . . ? O6 C32 C33 115.5(6) . . ? C31 C32 C33 120.5(6) . . ? C8 N1 C9 121.9(6) . . ? C8 N1 Pd1 124.8(5) . . ? C9 N1 Pd1 113.3(5) . . ? C11 N2 C10 121.5(6) . . ? C11 N2 Pd1 126.0(5) . . ? C10 N2 Pd1 112.3(5) . . ? C19 N3 C23 119.2(5) . . ? C19 N3 Cu2 126.3(4) . . ? C23 N3 Cu2 114.4(4) . . ? C28 N4 C24 119.3(5) . . ? C28 N4 Cu2 126.3(4) . . ? C24 N4 Cu2 114.4(4) . . ? C2 O1 C1 118.2(4) . . ? C7 O2 Pd1 123.7(4) . . ? C16 O3 C18 118.9(6) . . ? C17 O4 Pd1 123.4(4) . . ? C30 O5 Cu2 125.7(4) . . ? C32 O6 Cu2 125.3(4) . . ? N2 Pd1 N1 84.0(3) . . ? N2 Pd1 O4 94.3(2) . . ? N1 Pd1 O4 178.3(2) . . ? N2 Pd1 O2 177.7(2) . . ? N1 Pd1 O2 93.9(2) . . ? O4 Pd1 O2 87.76(15) . . ? O6 Cu2 O5 93.56(17) . . ? O6 Cu2 N4 165.45(17) . . ? O5 Cu2 N4 91.93(19) . . ? O6 Cu2 N3 91.36(18) . . ? O5 Cu2 N3 169.55(18) . . ? N4 Cu2 N3 81.2(2) . . ? O6 Cu2 O1W 97.0(2) . . ? O5 Cu2 O1W 93.01(19) . . ? N4 Cu2 O1W 96.1(2) . . ? N3 Cu2 O1W 95.54(18) . . ? O7 Cl3 O10 103.8(6) . . ? O7 Cl3 O8 115.1(5) . . ? O10 Cl3 O8 107.1(6) . . ? O7 Cl3 O9 113.3(6) . . ? O10 Cl3 O9 107.8(7) . . ? O8 Cl3 O9 109.1(4) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.515 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.092 # Attachment 'Crystal2.cif' data_mam104 _database_code_depnum_ccdc_archive 'CCDC 293153' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H33 Cl Cu N4 O11 Pd' _chemical_formula_weight 891.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.543 _cell_length_b 35.525 _cell_length_c 8.437 _cell_angle_alpha 90.00 _cell_angle_beta 105.64 _cell_angle_gamma 90.00 _cell_volume 3620.2 _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 220 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1804 _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.770271 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type area_detector _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 19439 _diffrn_reflns_av_R_equivalents 0.1241 _diffrn_reflns_av_sigmaI/netI 0.2289 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7912 _reflns_number_gt 2946 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'Denzo and Scalepak' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^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 7912 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2402 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1501 _refine_ls_wR_factor_gt 0.1094 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.000 _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 C1 C 0.2814(6) 0.26150(17) 0.5073(7) 0.066(2) Uani 1 1 d . . . H1A H 0.3536 0.2662 0.5795 0.099 Uiso 1 1 calc R . . H1B H 0.2382 0.2842 0.4941 0.099 Uiso 1 1 calc R . . H1C H 0.2883 0.2534 0.4020 0.099 Uiso 1 1 calc R . . C2 C 0.1236(7) 0.2220(2) 0.4923(8) 0.053(2) Uani 1 1 d . . . C3 C 0.0603(8) 0.2411(2) 0.3603(9) 0.068(2) Uani 1 1 d . . . H3 H 0.0871 0.2629 0.3229 0.081 Uiso 1 1 calc R . . C4 C -0.0430(9) 0.2280(3) 0.2834(10) 0.094(3) Uani 1 1 d . . . H4 H -0.0867 0.2408 0.1929 0.113 Uiso 1 1 calc R . . C5 C -0.0833(7) 0.1957(3) 0.3395(11) 0.089(3) Uani 1 1 d . . . H5 H -0.1538 0.1873 0.2845 0.107 Uiso 1 1 calc R . . C6 C -0.0215(7) 0.1752(3) 0.4768(9) 0.065(2) Uani 1 1 d . . . C7 C 0.0857(7) 0.18885(19) 0.5562(8) 0.0481(18) Uani 1 1 d . . . C8 C -0.0665(7) 0.1413(3) 0.5226(11) 0.077(2) Uani 1 1 d . . . H8 H -0.1382 0.1351 0.4632 0.093 Uiso 1 1 calc R . . C9 C -0.0802(9) 0.0872(3) 0.6770(12) 0.119(4) Uani 1 1 d . . . H9A H -0.1240 0.0956 0.7491 0.143 Uiso 1 1 calc R . . H9B H -0.1301 0.0772 0.5774 0.143 Uiso 1 1 calc R . . C10 C -0.0055(9) 0.0588(3) 0.7560(15) 0.125(4) Uani 1 1 d . . . H10A H 0.0083 0.0420 0.6730 0.151 Uiso 1 1 calc R . . H10B H -0.0397 0.0442 0.8260 0.151 Uiso 1 1 calc R . . C11 C 0.1729(11) 0.0556(2) 0.9724(13) 0.089(3) Uani 1 1 d . . . H11 H 0.1498 0.0321 0.9994 0.107 Uiso 1 1 calc R . . C12 C 0.2815(10) 0.0672(2) 1.0623(10) 0.070(2) Uani 1 1 d . . . C13 C 0.3429(10) 0.0423(2) 1.1872(12) 0.090(3) Uani 1 1 d . . . H13 H 0.3114 0.0198 1.2088 0.108 Uiso 1 1 calc R . . C14 C 0.4472(11) 0.0515(3) 1.2741(12) 0.106(4) Uani 1 1 d . . . H14 H 0.4861 0.0352 1.3556 0.127 Uiso 1 1 calc R . . C15 C 0.4964(8) 0.0840(3) 1.2451(9) 0.081(3) Uani 1 1 d . . . H15 H 0.5683 0.0897 1.3051 0.098 Uiso 1 1 calc R . . C16 C 0.4386(9) 0.1081(2) 1.1265(9) 0.068(2) Uani 1 1 d . . . C17 C 0.3301(8) 0.1011(2) 1.0313(10) 0.060(2) Uani 1 1 d . . . C18 C 0.5968(8) 0.1477(2) 1.1582(8) 0.092(3) Uani 1 1 d . . . H18A H 0.6158 0.1716 1.1210 0.138 Uiso 1 1 calc R . . H18B H 0.6396 0.1283 1.1250 0.138 Uiso 1 1 calc R . . H18C H 0.6124 0.1478 1.2760 0.138 Uiso 1 1 calc R . . C19 C 0.2719(6) 0.16453(19) 1.3202(8) 0.0517(19) Uani 1 1 d . . . H19 H 0.3013 0.1875 1.3000 0.062 Uiso 1 1 calc R . . C20 C 0.1680(7) 0.1543(2) 1.2259(8) 0.064(2) Uani 1 1 d . . . H20 H 0.1286 0.1701 1.1428 0.077 Uiso 1 1 calc R . . C21 C 0.1239(6) 0.1212(2) 1.2548(8) 0.061(2) Uani 1 1 d . . . H21 H 0.0536 0.1144 1.1918 0.073 Uiso 1 1 calc R . . C22 C 0.1826(6) 0.0969(2) 1.3787(8) 0.0474(18) Uani 1 1 d . . . C23 C 0.2850(6) 0.10877(19) 1.4677(7) 0.0467(18) Uani 1 1 d . . . C24 C 0.3519(6) 0.08556(18) 1.5949(7) 0.0452(17) Uani 1 1 d . . . C25 C 0.3154(6) 0.05037(18) 1.6299(8) 0.0481(18) Uani 1 1 d . . . C26 C 0.3868(7) 0.02929(17) 1.7534(8) 0.056(2) Uani 1 1 d . . . H26 H 0.3661 0.0055 1.7801 0.067 Uiso 1 1 calc R . . C27 C 0.4858(7) 0.04369(19) 1.8333(8) 0.063(2) Uani 1 1 d . . . H27 H 0.5332 0.0299 1.9168 0.075 Uiso 1 1 calc R . . C28 C 0.5182(6) 0.07930(18) 1.7923(8) 0.0498(18) Uani 1 1 d . . . H28 H 0.5872 0.0886 1.8492 0.060 Uiso 1 1 calc R . . C29 C 0.1453(6) 0.0606(2) 1.4160(9) 0.067(2) Uani 1 1 d . . . H29 H 0.0758 0.0521 1.3568 0.080 Uiso 1 1 calc R . . C30 C 0.2082(7) 0.03857(19) 1.5345(9) 0.062(2) Uani 1 1 d . . . H30 H 0.1815 0.0152 1.5548 0.075 Uiso 1 1 calc R . . C31 C 0.8128(6) 0.1710(2) 1.8588(8) 0.077(2) Uani 1 1 d . . . H31A H 0.8075 0.1514 1.9349 0.116 Uiso 1 1 calc R . . H31B H 0.8292 0.1945 1.9165 0.116 Uiso 1 1 calc R . . H31C H 0.8708 0.1650 1.8084 0.116 Uiso 1 1 calc R . . C32 C 0.7041(6) 0.1742(2) 1.7273(8) 0.0531(19) Uani 1 1 d . . . C33 C 0.6926(7) 0.20116(19) 1.6040(9) 0.062(2) Uani 1 1 d . . . H33 H 0.7564 0.2138 1.5979 0.075 Uiso 1 1 calc R . . C34 C 0.5953(8) 0.21086(19) 1.4903(9) 0.056(2) Uani 1 1 d . . . C35 C 0.5943(7) 0.24258(19) 1.3741(9) 0.090(3) Uani 1 1 d . . . H35A H 0.5210 0.2456 1.3029 0.136 Uiso 1 1 calc R . . H35B H 0.6448 0.2372 1.3093 0.136 Uiso 1 1 calc R . . H35C H 0.6167 0.2654 1.4354 0.136 Uiso 1 1 calc R . . N1 N -0.0185(6) 0.1188(2) 0.6362(8) 0.081(2) Uani 1 1 d . . . N2 N 0.1034(7) 0.07385(17) 0.8584(10) 0.079(2) Uani 1 1 d . . . N3 N 0.3313(4) 0.14250(15) 1.4390(6) 0.0455(14) Uani 1 1 d . . . N4 N 0.4538(5) 0.10009(13) 1.6752(6) 0.0429(14) Uani 1 1 d . . . O1 O 0.2278(4) 0.23283(12) 0.5763(5) 0.0594(13) Uani 1 1 d . . . O2 O 0.1554(4) 0.17331(11) 0.6838(5) 0.0565(13) Uani 1 1 d . . . O1W O 0.3982(3) 0.18204(10) 1.7800(4) 0.0495(12) Uani 1 1 d . . . O3 O 0.4826(5) 0.14058(16) 1.0884(5) 0.0759(16) Uani 1 1 d . . . O4 O 0.2842(4) 0.12643(12) 0.9216(5) 0.0620(13) Uani 1 1 d . . . O5 O 0.6267(4) 0.15295(12) 1.7430(5) 0.0606(13) Uani 1 1 d . . . O6 O 0.5024(4) 0.19552(12) 1.4774(5) 0.0604(13) Uani 1 1 d . . . O7 O 0.9142(16) 0.0387(6) 2.102(3) 0.155(6) Uani 0.60 1 d P . . O7A O 0.785(3) 0.0496(7) 1.970(2) 0.144(10) Uani 0.40 1 d P . . O8 O 0.842(3) 0.0487(9) 2.307(2) 0.232(13) Uani 0.60 1 d P . . O8A O 0.8927(19) 0.0282(5) 2.220(4) 0.096(7) Uani 0.40 1 d P . . O9 O 0.8508(6) 0.09350(17) 2.1509(10) 0.176(3) Uani 1 1 d . . . O10 O 0.7298(16) 0.0430(5) 2.061(3) 0.146(8) Uani 0.60 1 d P . . O10A O 0.734(3) 0.0554(7) 2.214(6) 0.165(14) Uani 0.40 1 d P . . Cu1 Cu 0.47870(7) 0.15224(2) 1.60168(9) 0.0512(3) Uani 1 1 d . . . Cl1 Cl 0.8245(2) 0.05646(6) 2.1449(4) 0.0799(7) Uani 1 1 d . . . Pd1 Pd 0.13167(5) 0.123337(14) 0.77581(6) 0.0602(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 C1 0.083(6) 0.055(5) 0.059(4) 0.008(4) 0.016(4) -0.008(4) C2 0.063(6) 0.056(5) 0.035(4) -0.001(4) 0.006(4) 0.018(5) C3 0.073(7) 0.074(5) 0.054(5) 0.010(4) 0.013(5) 0.023(5) C4 0.088(9) 0.112(8) 0.071(6) 0.010(6) -0.001(6) 0.038(7) C5 0.045(6) 0.136(9) 0.079(7) -0.020(6) 0.005(5) 0.008(6) C6 0.047(6) 0.101(7) 0.045(5) -0.009(5) 0.011(4) 0.008(6) C7 0.053(6) 0.052(5) 0.041(4) 0.001(4) 0.015(4) 0.016(4) C8 0.059(7) 0.096(7) 0.079(6) -0.021(5) 0.021(5) -0.018(6) C9 0.126(11) 0.097(8) 0.142(9) -0.006(7) 0.049(8) -0.033(8) C10 0.099(10) 0.076(7) 0.224(12) -0.002(8) 0.084(9) -0.027(7) C11 0.140(11) 0.050(6) 0.109(7) 0.031(6) 0.085(7) 0.027(7) C12 0.106(8) 0.054(6) 0.069(5) 0.007(5) 0.055(6) 0.026(6) C13 0.153(11) 0.053(5) 0.098(7) 0.023(6) 0.090(7) 0.045(7) C14 0.148(12) 0.110(9) 0.072(7) 0.033(6) 0.050(7) 0.066(9) C15 0.113(9) 0.078(6) 0.062(5) 0.004(5) 0.039(6) 0.036(6) C16 0.104(9) 0.062(6) 0.047(5) 0.011(5) 0.035(5) 0.034(6) C17 0.089(8) 0.047(5) 0.059(5) 0.012(4) 0.045(5) 0.021(5) C18 0.098(9) 0.094(7) 0.069(5) -0.007(5) -0.004(6) 0.009(6) C19 0.054(6) 0.060(5) 0.041(4) 0.000(4) 0.011(4) 0.014(4) C20 0.076(7) 0.069(6) 0.042(4) 0.000(4) 0.005(5) 0.023(5) C21 0.043(5) 0.083(6) 0.055(5) -0.031(5) 0.012(4) 0.005(5) C22 0.041(5) 0.057(5) 0.039(4) -0.005(4) 0.004(4) 0.004(4) C23 0.050(6) 0.052(4) 0.037(4) -0.004(4) 0.011(4) 0.005(4) C24 0.051(5) 0.045(4) 0.040(4) -0.014(4) 0.014(4) 0.003(4) C25 0.062(6) 0.041(4) 0.048(4) -0.011(4) 0.028(4) -0.009(4) C26 0.080(7) 0.029(4) 0.064(5) 0.010(4) 0.027(5) 0.001(4) C27 0.080(7) 0.045(5) 0.060(5) 0.005(4) 0.013(5) 0.005(4) C28 0.051(5) 0.044(4) 0.055(4) -0.007(4) 0.015(4) -0.001(4) C29 0.046(6) 0.084(6) 0.069(5) -0.021(5) 0.015(4) -0.016(5) C30 0.071(7) 0.051(5) 0.072(5) -0.009(4) 0.032(5) -0.019(5) C31 0.052(6) 0.092(6) 0.080(5) 0.004(5) 0.002(5) -0.003(5) C32 0.046(6) 0.052(5) 0.061(5) -0.014(4) 0.015(4) -0.001(4) C33 0.068(7) 0.058(5) 0.065(5) 0.000(4) 0.025(5) -0.019(4) C34 0.071(7) 0.042(5) 0.059(5) -0.008(4) 0.028(5) -0.009(5) C35 0.110(8) 0.068(5) 0.099(6) 0.031(5) 0.038(6) -0.017(5) N1 0.097(7) 0.074(5) 0.077(5) 0.000(4) 0.034(4) -0.023(5) N2 0.096(7) 0.048(4) 0.110(5) 0.001(4) 0.058(5) -0.010(4) N3 0.052(4) 0.048(3) 0.035(3) -0.005(3) 0.009(3) 0.010(3) N4 0.053(4) 0.029(3) 0.042(3) -0.001(3) 0.005(3) 0.004(3) O1 0.072(4) 0.058(3) 0.044(3) 0.016(2) 0.009(3) 0.001(3) O2 0.067(4) 0.052(3) 0.047(3) 0.004(2) 0.010(3) -0.004(3) O1W 0.063(3) 0.040(2) 0.047(2) -0.004(2) 0.016(2) 0.000(2) O3 0.085(5) 0.079(4) 0.057(3) 0.008(3) 0.008(3) 0.015(4) O4 0.080(4) 0.051(3) 0.057(3) 0.013(2) 0.023(3) 0.009(3) O5 0.053(4) 0.053(3) 0.071(3) 0.014(2) 0.010(3) -0.001(3) O6 0.069(4) 0.049(3) 0.066(3) 0.018(2) 0.022(3) -0.001(3) O7 0.132(15) 0.158(15) 0.171(16) -0.067(13) 0.035(15) 0.005(12) O7A 0.15(3) 0.19(2) 0.067(13) 0.003(12) 0.004(14) 0.007(18) O8 0.30(3) 0.29(3) 0.095(13) 0.002(14) 0.030(17) -0.13(3) O8A 0.096(18) 0.058(10) 0.103(17) 0.009(12) -0.026(16) 0.023(9) O9 0.143(7) 0.070(5) 0.299(10) 0.026(5) 0.030(6) -0.032(4) O10 0.077(14) 0.138(13) 0.19(2) 0.013(15) -0.032(15) -0.054(11) O10A 0.13(2) 0.126(19) 0.28(5) 0.03(3) 0.13(3) 0.015(19) Cu1 0.0563(7) 0.0414(5) 0.0545(5) 0.0052(4) 0.0122(5) -0.0021(4) Cl1 0.062(2) 0.0625(16) 0.103(2) 0.0094(14) 0.0010(19) -0.0049(14) Pd1 0.0810(6) 0.0493(3) 0.0600(4) -0.0036(3) 0.0359(3) -0.0018(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 C1 O1 1.428(7) . ? C2 C3 1.362(8) . ? C2 O1 1.362(8) . ? C2 C7 1.430(8) . ? C3 C4 1.364(11) . ? C4 C5 1.387(11) . ? C5 C6 1.411(10) . ? C6 C7 1.415(9) . ? C6 C8 1.427(10) . ? C7 O2 1.312(7) . ? C8 N1 1.269(9) . ? C9 C10 1.415(11) . ? C9 N1 1.458(10) . ? C10 N2 1.504(10) . ? C11 N2 1.286(10) . ? C11 C12 1.429(11) . ? C12 C17 1.407(10) . ? C12 C13 1.431(11) . ? C13 C14 1.355(12) . ? C14 C15 1.362(12) . ? C15 C16 1.368(10) . ? C16 O3 1.354(9) . ? C16 C17 1.403(10) . ? C17 O4 1.308(8) . ? C18 O3 1.416(8) . ? C19 N3 1.330(7) . ? C19 C20 1.380(9) . ? C20 C21 1.349(9) . ? C21 C22 1.402(9) . ? C22 C23 1.369(8) . ? C22 C29 1.434(9) . ? C23 N3 1.380(8) . ? C23 C24 1.432(8) . ? C24 N4 1.375(7) . ? C24 C25 1.390(8) . ? C25 C26 1.395(8) . ? C25 C30 1.431(9) . ? C26 C27 1.344(9) . ? C27 C28 1.401(8) . ? C28 N4 1.320(7) . ? C29 C30 1.346(8) . ? C31 C32 1.512(8) . ? C32 O5 1.265(7) . ? C32 C33 1.393(9) . ? C33 C34 1.377(9) . ? C34 O6 1.265(8) . ? C34 C35 1.491(8) . ? N1 Pd1 1.940(7) . ? N2 Pd1 1.958(6) . ? N3 Cu1 2.014(5) . ? N4 Cu1 2.005(5) . ? O2 Pd1 1.992(4) . ? O1W Cu1 2.285(4) . ? O4 Pd1 1.979(5) . ? O5 Cu1 1.917(5) . ? O6 Cu1 1.928(4) . ? O7 O8A 1.16(2) . ? O7 Cl1 1.421(18) . ? O7 O7A 1.75(3) . ? O7A O10 1.18(2) . ? O7A Cl1 1.446(19) . ? O8 O8A 1.31(3) . ? O8 Cl1 1.356(18) . ? O8 O10A 1.40(4) . ? O8A Cl1 1.361(17) . ? O9 Cl1 1.354(6) . ? O10 Cl1 1.299(15) . ? O10 O10A 1.35(4) . ? O10A Cl1 1.41(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C2 O1 123.4(7) . . ? C3 C2 C7 122.6(8) . . ? O1 C2 C7 114.0(6) . . ? C2 C3 C4 119.2(8) . . ? C3 C4 C5 120.4(8) . . ? C4 C5 C6 122.5(8) . . ? C5 C6 C7 117.0(8) . . ? C5 C6 C8 119.2(9) . . ? C7 C6 C8 123.7(7) . . ? O2 C7 C6 125.6(7) . . ? O2 C7 C2 116.1(7) . . ? C6 C7 C2 118.3(7) . . ? N1 C8 C6 126.5(8) . . ? C10 C9 N1 109.5(9) . . ? C9 C10 N2 113.7(8) . . ? N2 C11 C12 127.5(9) . . ? C17 C12 C11 123.1(8) . . ? C17 C12 C13 119.5(10) . . ? C11 C12 C13 117.4(9) . . ? C14 C13 C12 119.9(10) . . ? C13 C14 C15 121.7(10) . . ? C14 C15 C16 119.1(10) . . ? O3 C16 C15 122.5(10) . . ? O3 C16 C17 114.2(7) . . ? C15 C16 C17 123.2(9) . . ? O4 C17 C16 117.2(7) . . ? O4 C17 C12 126.2(9) . . ? C16 C17 C12 116.6(8) . . ? N3 C19 C20 121.9(7) . . ? C21 C20 C19 119.7(7) . . ? C20 C21 C22 120.9(7) . . ? C23 C22 C21 116.4(7) . . ? C23 C22 C29 118.1(6) . . ? C21 C22 C29 125.4(7) . . ? C22 C23 N3 123.3(6) . . ? C22 C23 C24 120.4(7) . . ? N3 C23 C24 116.3(6) . . ? N4 C24 C25 123.3(6) . . ? N4 C24 C23 115.6(6) . . ? C25 C24 C23 121.1(7) . . ? C24 C25 C26 117.3(7) . . ? C24 C25 C30 117.2(7) . . ? C26 C25 C30 125.4(7) . . ? C27 C26 C25 119.4(6) . . ? C26 C27 C28 120.7(7) . . ? N4 C28 C27 122.0(7) . . ? C30 C29 C22 121.6(7) . . ? C29 C30 C25 121.4(7) . . ? O5 C32 C33 124.1(7) . . ? O5 C32 C31 116.3(7) . . ? C33 C32 C31 119.4(7) . . ? C34 C33 C32 125.9(7) . . ? O6 C34 C33 125.1(7) . . ? O6 C34 C35 115.2(7) . . ? C33 C34 C35 119.7(7) . . ? C8 N1 C9 119.3(8) . . ? C8 N1 Pd1 126.3(6) . . ? C9 N1 Pd1 114.2(6) . . ? C11 N2 C10 125.3(9) . . ? C11 N2 Pd1 124.6(7) . . ? C10 N2 Pd1 109.7(6) . . ? C19 N3 C23 117.8(6) . . ? C19 N3 Cu1 129.6(5) . . ? C23 N3 Cu1 112.4(4) . . ? C28 N4 C24 117.3(5) . . ? C28 N4 Cu1 129.3(5) . . ? C24 N4 Cu1 113.3(4) . . ? C2 O1 C1 118.7(5) . . ? C7 O2 Pd1 123.9(4) . . ? C16 O3 C18 118.9(7) . . ? C17 O4 Pd1 124.7(5) . . ? C32 O5 Cu1 125.8(4) . . ? C34 O6 Cu1 124.8(5) . . ? O8A O7 Cl1 62.6(14) . . ? O8A O7 O7A 103(2) . . ? Cl1 O7 O7A 53.1(11) . . ? O10 O7A Cl1 58.1(11) . . ? O10 O7A O7 98.4(17) . . ? Cl1 O7A O7 51.8(9) . . ? O8A O8 Cl1 61.2(11) . . ? O8A O8 O10A 109(3) . . ? Cl1 O8 O10A 61.6(16) . . ? O7 O8A O8 124(2) . . ? O7 O8A Cl1 68.0(14) . . ? O8 O8A Cl1 60.9(13) . . ? O7A O10 Cl1 71.0(16) . . ? O7A O10 O10A 133(3) . . ? Cl1 O10 O10A 64.4(16) . . ? O10 O10A O8 105(3) . . ? O10 O10A Cl1 56.1(16) . . ? O8 O10A Cl1 57.8(17) . . ? O5 Cu1 O6 93.6(2) . . ? O5 Cu1 N4 91.4(2) . . ? O6 Cu1 N4 164.72(18) . . ? O5 Cu1 N3 169.61(19) . . ? O6 Cu1 N3 90.8(2) . . ? N4 Cu1 N3 82.0(2) . . ? O5 Cu1 O1W 96.31(17) . . ? O6 Cu1 O1W 98.56(16) . . ? N4 Cu1 O1W 95.21(17) . . ? N3 Cu1 O1W 92.32(16) . . ? O10 Cl1 O9 123.8(8) . . ? O10 Cl1 O8 110.6(14) . . ? O9 Cl1 O8 100.8(12) . . ? O10 Cl1 O8A 110.5(11) . . ? O9 Cl1 O8A 125.7(9) . . ? O8 Cl1 O8A 57.9(13) . . ? O10 Cl1 O10A 59.5(16) . . ? O9 Cl1 O10A 103.1(13) . . ? O8 Cl1 O10A 60.6(15) . . ? O8A Cl1 O10A 105.3(17) . . ? O10 Cl1 O7 111.6(14) . . ? O9 Cl1 O7 103.9(9) . . ? O8 Cl1 O7 104.1(17) . . ? O8A Cl1 O7 49.4(10) . . ? O10A Cl1 O7 151.1(14) . . ? O10 Cl1 O7A 50.8(11) . . ? O9 Cl1 O7A 102.5(12) . . ? O8 Cl1 O7A 156.2(16) . . ? O8A Cl1 O7A 110.6(16) . . ? O10A Cl1 O7A 109(2) . . ? O7 Cl1 O7A 75.1(14) . . ? N1 Pd1 N2 84.4(3) . . ? N1 Pd1 O4 178.2(3) . . ? N2 Pd1 O4 93.8(3) . . ? N1 Pd1 O2 93.4(3) . . ? N2 Pd1 O2 177.7(3) . . ? O4 Pd1 O2 88.37(18) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.441 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.085 # Attachment 'Crystal3.cif' data_mam33 _database_code_depnum_ccdc_archive 'CCDC 293154' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H35 Cl Cu N4 Ni O11' _chemical_formula_weight 845.37 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' Cu Cu 0.3201 1.2651 '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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6386(12) _cell_length_b 35.110(2) _cell_length_c 8.4367(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.723(10) _cell_angle_gamma 90.00 _cell_volume 3585.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 24.95 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 1.259 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8675 _exptl_absorpt_correction_T_max 0.8793 _exptl_absorpt_process_details wingx _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type STOE-IPDS _diffrn_measurement_method 'Oscillation, Phi. incr. = 0.7' _diffrn_detector_area_resol_mean 6.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27115 _diffrn_reflns_av_R_equivalents 0.1016 _diffrn_reflns_av_sigmaI/netI 0.1276 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.97 _reflns_number_total 6751 _reflns_number_gt 2594 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0163P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6751 _refine_ls_number_parameters 513 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1360 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0721 _refine_ls_wR_factor_gt 0.0545 _refine_ls_goodness_of_fit_ref 0.757 _refine_ls_restrained_S_all 0.757 _refine_ls_shift/su_max 0.000 _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 C1 C 0.7129(4) -0.26024(13) 0.9935(6) 0.0839(16) Uani 1 1 d . . . H1A H 0.6394 -0.2644 0.9227 0.126 Uiso 1 1 calc R . . H1B H 0.7094 -0.2520 1.1005 0.126 Uiso 1 1 calc R . . H1C H 0.7542 -0.2835 1.0048 0.126 Uiso 1 1 calc R . . C2 C 0.8716(4) -0.22162(13) 1.0074(6) 0.0663(13) Uani 1 1 d . . . C3 C 0.9358(5) -0.24156(14) 1.1377(7) 0.0802(15) Uani 1 1 d . . . H3 H 0.9084 -0.2637 1.1718 0.096 Uiso 1 1 calc R . . C4 C 1.0428(5) -0.22927(19) 1.2216(8) 0.101(2) Uani 1 1 d . . . H4 H 1.0857 -0.2427 1.3125 0.121 Uiso 1 1 calc R . . C5 C 1.0828(4) -0.1974(2) 1.1677(8) 0.0989(19) Uani 1 1 d . . . H5 H 1.1542 -0.1893 1.2215 0.119 Uiso 1 1 calc R . . C6 C 1.0187(4) -0.17647(17) 1.0327(7) 0.0793(15) Uani 1 1 d . . . C7 C 0.9113(4) -0.18816(13) 0.9480(6) 0.0623(12) Uani 1 1 d . . . C8 C 1.0637(4) -0.14260(19) 0.9839(8) 0.0913(19) Uani 1 1 d . . . H8 H 1.1362 -0.1364 1.0409 0.110 Uiso 1 1 calc R . . C9 C 1.0747(6) -0.0873(2) 0.8275(11) 0.144(3) Uani 1 1 d . . . H9A H 1.1248 -0.0772 0.9286 0.173 Uiso 1 1 calc R . . H9B H 1.1182 -0.0957 0.7564 0.173 Uiso 1 1 calc R . . C10 C 1.0034(6) -0.05965(18) 0.7504(12) 0.146(3) Uani 1 1 d . . . H10A H 1.0349 -0.0458 0.6752 0.175 Uiso 1 1 calc R . . H10B H 0.9928 -0.0418 0.8321 0.175 Uiso 1 1 calc R . . C11 C 0.8242(7) -0.05732(15) 0.5372(9) 0.094(2) Uani 1 1 d . . . H11 H 0.8483 -0.0340 0.5086 0.113 Uiso 1 1 calc R . . C12 C 0.7175(5) -0.06818(15) 0.4477(8) 0.0815(16) Uani 1 1 d . . . C13 C 0.6557(6) -0.04376(16) 0.3217(8) 0.096(2) Uani 1 1 d . . . H13 H 0.6867 -0.0211 0.2996 0.115 Uiso 1 1 calc R . . C14 C 0.5528(6) -0.05316(17) 0.2340(9) 0.104(2) Uani 1 1 d . . . H14 H 0.5129 -0.0371 0.1504 0.124 Uiso 1 1 calc R . . C15 C 0.5054(5) -0.08691(16) 0.2674(7) 0.0917(18) Uani 1 1 d . . . H15 H 0.4339 -0.0932 0.2059 0.110 Uiso 1 1 calc R . . C16 C 0.5632(5) -0.11106(14) 0.3906(7) 0.0752(15) Uani 1 1 d . . . C17 C 0.6735(5) -0.10282(13) 0.4844(7) 0.0704(14) Uani 1 1 d . . . C18 C 0.4077(4) -0.15143(17) 0.3698(7) 0.0998(18) Uani 1 1 d . . . H18A H 0.3903 -0.1758 0.4080 0.150 Uiso 1 1 calc R . . H18B H 0.3874 -0.1514 0.2511 0.150 Uiso 1 1 calc R . . H18C H 0.3674 -0.1319 0.4070 0.150 Uiso 1 1 calc R . . C19 C 0.4846(4) -0.07774(12) 0.7196(6) 0.0588(12) Uani 1 1 d . . . H19 H 0.4149 -0.0869 0.6631 0.071 Uiso 1 1 calc R . . C20 C 0.5161(4) -0.04214(12) 0.6770(6) 0.0673(13) Uani 1 1 d . . . H20 H 0.4681 -0.0279 0.5938 0.081 Uiso 1 1 calc R . . C21 C 0.6173(4) -0.02839(13) 0.7575(7) 0.0709(14) Uani 1 1 d . . . H21 H 0.6394 -0.0047 0.7296 0.085 Uiso 1 1 calc R . . C22 C 0.6884(4) -0.04995(13) 0.8826(6) 0.0617(13) Uani 1 1 d . . . C23 C 0.6500(4) -0.08559(11) 0.9189(6) 0.0516(11) Uani 1 1 d . . . C24 C 0.7170(4) -0.10886(12) 1.0454(6) 0.0534(11) Uani 1 1 d . . . C25 C 0.8228(4) -0.09684(14) 1.1379(6) 0.0642(13) Uani 1 1 d . . . C26 C 0.8829(4) -0.12145(15) 1.2596(7) 0.0720(14) Uani 1 1 d . . . H26 H 0.9545 -0.1152 1.3209 0.086 Uiso 1 1 calc R . . C27 C 0.8368(4) -0.15481(16) 1.2890(6) 0.0758(14) Uani 1 1 d . . . H27 H 0.8757 -0.1710 1.3727 0.091 Uiso 1 1 calc R . . C28 C 0.7302(4) -0.16442(13) 1.1915(6) 0.0676(14) Uani 1 1 d . . . H28 H 0.6999 -0.1874 1.2121 0.081 Uiso 1 1 calc R . . C29 C 0.7961(4) -0.03819(15) 0.9799(7) 0.0785(15) Uani 1 1 d . . . H29 H 0.8224 -0.0145 0.9602 0.094 Uiso 1 1 calc R . . C30 C 0.8596(4) -0.06024(15) 1.0976(8) 0.0789(15) Uani 1 1 d . . . H30 H 0.9298 -0.0518 1.1555 0.095 Uiso 1 1 calc R . . C31 C 0.4048(4) -0.24222(13) 1.1396(7) 0.0951(18) Uani 1 1 d . . . H31A H 0.4777 -0.2454 1.2139 0.143 Uiso 1 1 calc R . . H31B H 0.3823 -0.2654 1.0787 0.143 Uiso 1 1 calc R . . H31C H 0.3542 -0.2363 1.2018 0.143 Uiso 1 1 calc R . . C32 C 0.4054(5) -0.21019(12) 1.0208(6) 0.0650(13) Uani 1 1 d . . . C33 C 0.3078(4) -0.20025(13) 0.9038(7) 0.0694(13) Uani 1 1 d . . . H33 H 0.2440 -0.2130 0.9074 0.083 Uiso 1 1 calc R . . C34 C 0.2973(4) -0.17279(13) 0.7810(6) 0.0633(13) Uani 1 1 d . . . C35 C 0.1894(4) -0.16959(15) 0.6470(7) 0.0966(19) Uani 1 1 d . . . H35A H 0.1947 -0.1498 0.5712 0.145 Uiso 1 1 calc R . . H35B H 0.1315 -0.1636 0.6956 0.145 Uiso 1 1 calc R . . H35C H 0.1732 -0.1933 0.5887 0.145 Uiso 1 1 calc R . . Cu1 Cu 0.52262(4) -0.151391(14) 0.91288(8) 0.05951(17) Uani 1 1 d . . . N1 N 1.0115(4) -0.12001(13) 0.8671(6) 0.0855(14) Uani 1 1 d . . . N2 N 0.8939(4) -0.07574(12) 0.6555(7) 0.0885(14) Uani 1 1 d . . . N3 N 0.5488(3) -0.09914(9) 0.8362(5) 0.0547(9) Uani 1 1 d . . . N4 N 0.6713(3) -0.14253(10) 1.0729(5) 0.0550(10) Uani 1 1 d . . . Ni1 Ni 0.86919(5) -0.123113(17) 0.73587(9) 0.0689(2) Uani 1 1 d . . . O1 O 0.7662(3) -0.23150(8) 0.9228(4) 0.0695(9) Uani 1 1 d . . . O2 O 0.8442(2) -0.16983(8) 0.8237(4) 0.0674(9) Uani 1 1 d . . . O1W O 0.5978(3) -0.18267(9) 0.7375(5) 0.0642(9) Uani 1 1 d . . . O3 O 0.7254(2) -0.12686(8) 0.6005(4) 0.0700(9) Uani 1 1 d . . . O4 O 0.5238(3) -0.14441(10) 0.4345(5) 0.0836(10) Uani 1 1 d . . . O5 O 0.4984(2) -0.19440(8) 1.0370(4) 0.0685(9) Uani 1 1 d . . . O6 O 0.3750(2) -0.15123(9) 0.7686(4) 0.0716(9) Uani 1 1 d . . . O7 O 1.2556(12) -0.0423(5) 1.490(3) 0.190(9) Uani 0.50 1 d P . . O8 O 1.1507(4) -0.09428(13) 1.3493(9) 0.191(3) Uani 1 1 d . . . O9 O 1.1304(11) -0.0322(4) 1.238(2) 0.142(7) Uani 0.50 1 d P . . O10 O 1.0903(12) -0.0348(5) 1.359(4) 0.231(14) Uani 0.50 1 d P . . O11 O 1.153(4) -0.0491(6) 1.498(4) 0.358(19) Uani 0.50 1 d P . . O13 O 1.2919(8) -0.0523(4) 1.392(3) 0.142(7) Uani 0.50 1 d P . . O14 O 1.215(3) -0.0579(6) 1.219(3) 0.276(11) Uani 0.50 1 d P . . Cl1 Cl 1.18042(13) -0.05694(4) 1.3610(3) 0.0926(5) Uani 1 1 d . . . H1W H 0.678(5) -0.1951(16) 0.789(8) 0.14(2) Uiso 1 1 d . . . H2W H 0.612(4) -0.1677(15) 0.668(8) 0.11(2) 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 C1 0.118(4) 0.064(3) 0.067(4) 0.009(3) 0.024(3) -0.005(3) C2 0.076(4) 0.072(3) 0.051(4) 0.003(3) 0.017(3) 0.020(3) C3 0.087(4) 0.084(3) 0.067(4) 0.009(3) 0.017(3) 0.027(3) C4 0.102(5) 0.116(5) 0.077(5) 0.011(4) 0.014(4) 0.037(4) C5 0.065(4) 0.142(6) 0.079(5) 0.003(4) 0.006(3) 0.018(4) C6 0.069(4) 0.097(4) 0.076(5) -0.010(3) 0.029(3) 0.005(3) C7 0.070(3) 0.072(3) 0.049(4) -0.002(3) 0.022(3) 0.012(3) C8 0.060(4) 0.124(5) 0.086(5) -0.030(4) 0.015(3) -0.003(4) C9 0.139(7) 0.114(6) 0.178(9) 0.002(5) 0.046(6) -0.035(5) C10 0.106(5) 0.091(5) 0.260(11) 0.012(6) 0.083(6) -0.029(4) C11 0.141(6) 0.058(3) 0.111(6) 0.012(4) 0.080(5) 0.013(4) C12 0.105(5) 0.067(4) 0.088(5) 0.005(3) 0.053(4) 0.014(3) C13 0.147(6) 0.069(4) 0.097(6) 0.020(4) 0.074(5) 0.034(4) C14 0.161(7) 0.076(4) 0.092(6) 0.026(4) 0.066(5) 0.051(4) C15 0.127(5) 0.091(4) 0.065(4) 0.012(3) 0.041(3) 0.048(4) C16 0.095(4) 0.073(3) 0.060(4) 0.003(3) 0.025(3) 0.027(3) C17 0.096(4) 0.059(3) 0.073(4) 0.005(3) 0.051(3) 0.019(3) C18 0.103(4) 0.108(4) 0.076(5) -0.007(4) 0.008(3) 0.011(4) C19 0.065(3) 0.052(3) 0.059(4) 0.000(2) 0.018(3) 0.003(2) C20 0.082(4) 0.052(3) 0.069(4) 0.004(2) 0.024(3) 0.007(2) C21 0.086(4) 0.055(3) 0.081(4) 0.002(3) 0.040(3) -0.001(3) C22 0.068(3) 0.058(3) 0.067(4) -0.009(3) 0.033(3) -0.004(3) C23 0.057(3) 0.052(3) 0.050(3) -0.006(2) 0.023(2) 0.001(2) C24 0.056(3) 0.059(3) 0.049(3) -0.011(2) 0.020(2) 0.004(2) C25 0.060(3) 0.076(3) 0.056(4) -0.016(3) 0.015(3) 0.005(3) C26 0.058(3) 0.090(4) 0.063(4) -0.014(3) 0.010(3) 0.007(3) C27 0.078(4) 0.087(4) 0.060(4) 0.003(3) 0.017(3) 0.020(3) C28 0.075(3) 0.069(3) 0.058(4) -0.002(3) 0.018(3) 0.002(3) C29 0.082(4) 0.073(3) 0.088(5) -0.012(3) 0.035(3) -0.016(3) C30 0.063(3) 0.082(4) 0.094(5) -0.022(3) 0.025(3) -0.018(3) C31 0.105(4) 0.072(3) 0.112(5) 0.028(3) 0.039(3) -0.003(3) C32 0.090(4) 0.048(3) 0.066(4) 0.001(2) 0.036(3) -0.005(3) C33 0.073(3) 0.069(3) 0.073(4) 0.000(3) 0.031(3) -0.007(3) C34 0.059(3) 0.066(3) 0.066(4) -0.013(3) 0.020(3) 0.002(2) C35 0.064(3) 0.105(4) 0.113(6) 0.004(4) 0.011(3) -0.008(3) Cu1 0.0620(3) 0.0541(3) 0.0613(4) 0.0050(3) 0.0158(3) -0.0017(3) N1 0.081(3) 0.087(3) 0.094(4) -0.014(3) 0.033(3) -0.021(3) N2 0.100(4) 0.070(3) 0.113(5) 0.000(3) 0.060(3) -0.010(3) N3 0.053(2) 0.055(2) 0.056(3) 0.0003(19) 0.0148(19) 0.0022(18) N4 0.068(2) 0.052(2) 0.046(3) 0.0031(18) 0.017(2) 0.0045(18) Ni1 0.0826(5) 0.0629(3) 0.0712(5) -0.0035(3) 0.0382(4) 0.0005(3) O1 0.078(2) 0.070(2) 0.058(2) 0.0112(17) 0.0156(19) 0.0044(17) O2 0.075(2) 0.0642(18) 0.062(3) 0.0058(17) 0.0184(18) 0.0001(16) O1W 0.072(2) 0.0586(18) 0.061(3) 0.0039(17) 0.0176(19) 0.0061(16) O3 0.077(2) 0.0705(19) 0.065(3) 0.0111(18) 0.0233(18) 0.0123(17) O4 0.092(3) 0.084(2) 0.070(3) 0.010(2) 0.015(2) 0.012(2) O5 0.069(2) 0.0608(18) 0.077(3) 0.0136(16) 0.0228(17) -0.0054(16) O6 0.0556(19) 0.0709(19) 0.084(3) 0.0127(19) 0.0133(17) -0.0088(18) O7 0.078(9) 0.241(15) 0.186(17) -0.094(13) -0.067(10) 0.015(9) O8 0.174(5) 0.091(3) 0.286(8) 0.019(4) 0.032(5) -0.048(3) O9 0.092(9) 0.117(9) 0.181(15) 0.099(11) -0.020(8) -0.005(6) O10 0.073(8) 0.154(13) 0.40(4) -0.142(18) -0.038(13) 0.033(8) O11 0.63(5) 0.29(2) 0.33(4) 0.04(2) 0.42(4) 0.05(3) O13 0.037(5) 0.131(9) 0.25(2) 0.049(11) 0.034(8) -0.008(5) O14 0.48(4) 0.213(18) 0.20(2) 0.007(17) 0.21(2) -0.04(2) Cl1 0.0701(10) 0.0756(9) 0.1196(17) 0.0170(10) 0.0071(10) -0.0066(8) _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 C1 O1 1.435(5) . ? C2 C3 1.358(6) . ? C2 O1 1.362(5) . ? C2 C7 1.424(6) . ? C3 C4 1.402(7) . ? C4 C5 1.360(8) . ? C5 C6 1.401(7) . ? C6 C7 1.400(6) . ? C6 C8 1.429(8) . ? C7 O2 1.312(5) . ? C8 N1 1.289(7) . ? C9 C10 1.356(8) . ? C9 N1 1.492(7) . ? C10 N2 1.495(7) . ? C11 N2 1.298(7) . ? C11 C12 1.395(7) . ? C12 C17 1.409(7) . ? C12 C13 1.413(8) . ? C13 C14 1.339(7) . ? C14 C15 1.393(8) . ? C15 C16 1.377(7) . ? C16 O4 1.365(6) . ? C16 C17 1.420(7) . ? C17 O3 1.316(5) . ? C18 O4 1.433(5) . ? C19 N3 1.316(5) . ? C19 C20 1.390(6) . ? C20 C21 1.353(6) . ? C21 C22 1.396(6) . ? C22 C23 1.407(6) . ? C22 C29 1.433(6) . ? C23 N3 1.355(5) . ? C23 C24 1.415(6) . ? C24 N4 1.365(5) . ? C24 C25 1.405(6) . ? C25 C26 1.389(7) . ? C25 C30 1.440(7) . ? C26 C27 1.362(7) . ? C27 C28 1.403(6) . ? C28 N4 1.311(5) . ? C29 C30 1.330(7) . ? C31 C32 1.508(6) . ? C32 O5 1.272(5) . ? C32 C33 1.384(6) . ? C33 C34 1.393(7) . ? C34 O6 1.268(5) . ? C34 C35 1.504(6) . ? Cu1 O5 1.912(3) . ? Cu1 O6 1.912(3) . ? Cu1 N4 1.998(4) . ? Cu1 N3 2.004(3) . ? Cu1 O1W 2.261(3) . ? N1 Ni1 1.824(5) . ? N2 Ni1 1.856(4) . ? Ni1 O3 1.851(3) . ? Ni1 O2 1.864(3) . ? O7 O13 1.116(18) . ? O7 Cl1 1.326(12) . ? O7 O11 1.34(3) . ? O8 Cl1 1.359(4) . ? O9 O10 1.27(3) . ? O9 Cl1 1.363(10) . ? O9 O14 1.44(2) . ? O10 O11 1.31(3) . ? O10 Cl1 1.375(14) . ? O11 Cl1 1.331(16) . ? O13 Cl1 1.367(9) . ? O13 O14 1.51(3) . ? O14 Cl1 1.390(18) . ? 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 C3 C2 O1 124.0(5) . . ? C3 C2 C7 121.4(5) . . ? O1 C2 C7 114.6(4) . . ? C2 C3 C4 121.0(5) . . ? C5 C4 C3 118.8(6) . . ? C4 C5 C6 121.3(6) . . ? C7 C6 C5 120.7(6) . . ? C7 C6 C8 120.3(5) . . ? C5 C6 C8 119.0(6) . . ? O2 C7 C6 124.9(5) . . ? O2 C7 C2 118.3(4) . . ? C6 C7 C2 116.8(5) . . ? N1 C8 C6 125.0(5) . . ? C10 C9 N1 109.5(6) . . ? C9 C10 N2 111.8(6) . . ? N2 C11 C12 128.1(5) . . ? C11 C12 C17 119.9(5) . . ? C11 C12 C13 118.7(6) . . ? C17 C12 C13 121.4(6) . . ? C14 C13 C12 120.3(6) . . ? C13 C14 C15 120.2(6) . . ? C16 C15 C14 120.7(6) . . ? O4 C16 C15 125.3(6) . . ? O4 C16 C17 113.6(4) . . ? C15 C16 C17 121.2(5) . . ? O3 C17 C12 125.0(5) . . ? O3 C17 C16 118.9(4) . . ? C12 C17 C16 116.1(5) . . ? N3 C19 C20 123.1(4) . . ? C21 C20 C19 119.4(4) . . ? C20 C21 C22 119.7(4) . . ? C21 C22 C23 117.4(4) . . ? C21 C22 C29 125.1(5) . . ? C23 C22 C29 117.5(5) . . ? N3 C23 C22 122.2(4) . . ? N3 C23 C24 117.2(4) . . ? C22 C23 C24 120.6(4) . . ? N4 C24 C25 123.2(4) . . ? N4 C24 C23 116.0(4) . . ? C25 C24 C23 120.8(4) . . ? C26 C25 C24 117.0(5) . . ? C26 C25 C30 125.8(5) . . ? C24 C25 C30 117.2(4) . . ? C27 C26 C25 119.8(5) . . ? C26 C27 C28 119.3(5) . . ? N4 C28 C27 123.0(5) . . ? C30 C29 C22 121.9(5) . . ? C29 C30 C25 122.0(5) . . ? O5 C32 C33 125.0(4) . . ? O5 C32 C31 115.8(5) . . ? C33 C32 C31 119.3(4) . . ? C32 C33 C34 125.4(4) . . ? O6 C34 C33 124.3(4) . . ? O6 C34 C35 116.7(5) . . ? C33 C34 C35 118.9(5) . . ? O5 Cu1 O6 94.06(13) . . ? O5 Cu1 N4 91.16(14) . . ? O6 Cu1 N4 170.28(14) . . ? O5 Cu1 N3 165.28(15) . . ? O6 Cu1 N3 90.76(14) . . ? N4 Cu1 N3 82.24(15) . . ? O5 Cu1 O1W 97.96(14) . . ? O6 Cu1 O1W 95.84(14) . . ? N4 Cu1 O1W 91.55(13) . . ? N3 Cu1 O1W 95.36(14) . . ? C8 N1 C9 117.2(5) . . ? C8 N1 Ni1 128.7(4) . . ? C9 N1 Ni1 114.1(5) . . ? C11 N2 C10 122.8(5) . . ? C11 N2 Ni1 125.4(4) . . ? C10 N2 Ni1 111.7(4) . . ? C19 N3 C23 118.2(4) . . ? C19 N3 Cu1 129.8(3) . . ? C23 N3 Cu1 112.0(3) . . ? C28 N4 C24 117.6(4) . . ? C28 N4 Cu1 129.9(3) . . ? C24 N4 Cu1 112.4(3) . . ? N1 Ni1 O3 179.05(19) . . ? N1 Ni1 N2 85.9(2) . . ? O3 Ni1 N2 94.4(2) . . ? N1 Ni1 O2 93.52(19) . . ? O3 Ni1 O2 86.24(14) . . ? N2 Ni1 O2 177.90(19) . . ? C2 O1 C1 117.8(4) . . ? C7 O2 Ni1 127.2(3) . . ? C17 O3 Ni1 127.2(3) . . ? C16 O4 C18 117.3(4) . . ? C32 O5 Cu1 125.0(3) . . ? C34 O6 Cu1 125.6(3) . . ? O13 O7 Cl1 67.5(11) . . ? O13 O7 O11 126.4(18) . . ? Cl1 O7 O11 59.8(13) . . ? O10 O9 Cl1 62.9(9) . . ? O10 O9 O14 121.7(14) . . ? Cl1 O9 O14 59.4(9) . . ? O9 O10 O11 118.2(19) . . ? O9 O10 Cl1 61.9(10) . . ? O11 O10 Cl1 59.3(10) . . ? O10 O11 Cl1 62.7(13) . . ? O10 O11 O7 103.3(16) . . ? Cl1 O11 O7 59.5(8) . . ? O7 O13 Cl1 63.6(8) . . ? O7 O13 O14 118.1(16) . . ? Cl1 O13 O14 57.4(10) . . ? Cl1 O14 O9 57.5(10) . . ? Cl1 O14 O13 56.0(9) . . ? O9 O14 O13 96.0(14) . . ? O7 Cl1 O11 60.6(14) . . ? O7 Cl1 O8 123.4(9) . . ? O11 Cl1 O8 97.3(10) . . ? O7 Cl1 O9 116.6(12) . . ? O11 Cl1 O9 110.6(14) . . ? O8 Cl1 O9 120.0(7) . . ? O7 Cl1 O13 48.9(8) . . ? O11 Cl1 O13 109.0(17) . . ? O8 Cl1 O13 112.1(6) . . ? O9 Cl1 O13 107.2(8) . . ? O7 Cl1 O10 100.8(9) . . ? O11 Cl1 O10 58.0(13) . . ? O8 Cl1 O10 109.6(9) . . ? O9 Cl1 O10 55.2(11) . . ? O13 Cl1 O10 137.7(11) . . ? O7 Cl1 O14 113.0(12) . . ? O11 Cl1 O14 169.1(12) . . ? O8 Cl1 O14 93.6(8) . . ? O9 Cl1 O14 63.1(10) . . ? O13 Cl1 O14 66.6(12) . . ? O10 Cl1 O14 117.8(14) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.242 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.049