# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_jwjh111128 _database_code_depnum_ccdc_archive 'CCDC 898396' #TrackingRef '13550_web_deposit_cif_file_0_RUPPERTRomain_1346083023.jwjh111128.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C104 H84 I2 N12 Ni2 O2 Pd' _chemical_formula_sum 'C104 H84 I2 N12 Ni2 O2 Pd' _chemical_formula_weight 2011.45 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' Ni Ni 0.3393 1.1124 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc ' 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 16.311(3) _cell_length_b 26.899(5) _cell_length_c 13.696(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.885(4) _cell_angle_gamma 90.00 _cell_volume 5651.1(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4893 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 24.39 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 1.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6720 _exptl_absorpt_correction_T_max 0.9480 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator triumph _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39341 _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_sigmaI/netI 0.1272 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.83 _reflns_number_total 13185 _reflns_number_gt 6059 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.1487P)^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 13185 _refine_ls_number_parameters 542 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1655 _refine_ls_R_factor_gt 0.0887 _refine_ls_wR_factor_ref 0.2684 _refine_ls_wR_factor_gt 0.2348 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.959 _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 0.6210(6) 0.3659(3) 0.3528(6) 0.040(2) Uani 1 1 d . . . C2 C 0.5430(7) 0.3869(3) 0.3574(7) 0.059(3) Uani 1 1 d . . . H2 H 0.5049 0.3720 0.3882 0.071 Uiso 1 1 calc R . . C3 C 0.5316(7) 0.4321(3) 0.3105(7) 0.052(2) Uani 1 1 d . . . H3 H 0.4829 0.4537 0.2966 0.062 Uiso 1 1 calc R . . C4 C 0.6103(7) 0.4399(3) 0.2865(7) 0.047(2) Uani 1 1 d . . . C5 C 0.6332(6) 0.4852(3) 0.2527(6) 0.038(2) Uani 1 1 d . . . C6 C 0.7162(6) 0.4952(3) 0.2574(6) 0.0388(19) Uani 1 1 d . . . C7 C 0.7455(6) 0.5459(3) 0.2507(7) 0.048(2) Uani 1 1 d . . . H7 H 0.7105 0.5750 0.2334 0.057 Uiso 1 1 calc R . . C8 C 0.8314(7) 0.5429(3) 0.2740(8) 0.055(3) Uani 1 1 d . . . H8 H 0.8701 0.5700 0.2796 0.066 Uiso 1 1 calc R . . C9 C 0.8551(6) 0.4913(3) 0.2890(6) 0.043(2) Uani 1 1 d . . . C10 C 0.9379(6) 0.4743(3) 0.3031(7) 0.047(2) Uani 1 1 d . . . C11 C 0.9496(7) 0.4235(4) 0.2882(8) 0.060(2) Uani 1 1 d . . . C12 C 1.0251(7) 0.4022(4) 0.2727(8) 0.060(2) Uani 1 1 d . . . H12 H 1.0776 0.4190 0.2777 0.072 Uiso 1 1 calc R . . C13 C 1.0076(7) 0.3556(3) 0.2506(7) 0.053(2) Uani 1 1 d . . . H13 H 1.0449 0.3325 0.2338 0.064 Uiso 1 1 calc R . . C14 C 0.9210(6) 0.3441(3) 0.2555(6) 0.041(2) Uani 1 1 d . . . C15 C 0.8905(6) 0.2969(3) 0.2524(7) 0.045(2) Uani 1 1 d . . . C16 C 0.8206(5) 0.2867(3) 0.2895(7) 0.0395(19) Uani 1 1 d . . . C17 C 0.7949(7) 0.2380(3) 0.3109(7) 0.054(2) Uani 1 1 d . . . H17 H 0.8167 0.2073 0.2959 0.064 Uiso 1 1 calc R . . C18 C 0.7350(6) 0.2441(3) 0.3558(7) 0.045(2) Uani 1 1 d . . . H18 H 0.7079 0.2186 0.3821 0.054 Uiso 1 1 calc R . . C19 C 0.7191(6) 0.2964(3) 0.3568(6) 0.040(2) Uani 1 1 d . . . C20 C 0.6489(6) 0.3167(3) 0.3798(7) 0.043(2) Uani 1 1 d . . . C21 C 0.5171(6) 0.5376(3) 0.1320(6) 0.039(2) Uani 1 1 d . . . C22 C 0.5643(7) 0.5613(3) 0.3025(7) 0.056(3) Uani 1 1 d . . . C23 C 0.6053(8) 0.5633(4) 0.4068(7) 0.067(3) Uani 1 1 d . . . H23 H 0.6458 0.5385 0.4430 0.081 Uiso 1 1 calc R . . C24 C 0.5843(10) 0.6043(4) 0.4588(8) 0.088(4) Uani 1 1 d . . . H24 H 0.6124 0.6088 0.5313 0.106 Uiso 1 1 calc R . . C25 C 0.5210(10) 0.6381(4) 0.4004(9) 0.089(4) Uani 1 1 d . . . H25 H 0.5048 0.6643 0.4367 0.107 Uiso 1 1 calc R . . C26 C 0.4811(7) 0.6362(3) 0.2958(8) 0.058(3) Uani 1 1 d . . . H26 H 0.4405 0.6607 0.2587 0.070 Uiso 1 1 calc R . . C27 C 0.5036(6) 0.5958(3) 0.2463(7) 0.046(2) Uani 1 1 d . . . C28 C 0.4083(7) 0.6035(4) 0.0616(8) 0.0713(18) Uani 1 1 d D . . H28A H 0.4073 0.5905 -0.0065 0.086 Uiso 1 1 calc R . . H28B H 0.4198 0.6397 0.0632 0.086 Uiso 1 1 calc R . . C29 C 0.3175(7) 0.5940(4) 0.0746(8) 0.0713(18) Uani 1 1 d D . . H29A H 0.3094 0.5579 0.0814 0.086 Uiso 1 1 calc R . . H29B H 0.3164 0.6104 0.1389 0.086 Uiso 1 1 calc R . . C30 C 0.2448(8) 0.6135(4) -0.0155(8) 0.0713(18) Uani 1 1 d . . . H30A H 0.2475 0.5995 -0.0811 0.086 Uiso 1 1 calc R . . H30B H 0.2482 0.6502 -0.0188 0.086 Uiso 1 1 calc R . . C31 C 0.1590(9) 0.5977(8) 0.0009(11) 0.139(8) Uani 1 1 d . . . H31A H 0.1354 0.5681 -0.0408 0.209 Uiso 1 1 calc R . . H31B H 0.1165 0.6248 -0.0205 0.209 Uiso 1 1 calc R . . H31C H 0.1708 0.5902 0.0745 0.209 Uiso 1 1 calc R . . C32 C 1.0106(6) 0.5091(3) 0.3190(7) 0.045(2) Uani 1 1 d . . . C33 C 1.0186(8) 0.5381(4) 0.2406(9) 0.074(3) Uani 1 1 d . . . H33 H 0.9779 0.5345 0.1724 0.088 Uiso 1 1 calc R . . C34 C 1.0867(9) 0.5736(4) 0.2594(11) 0.079(4) Uani 1 1 d . . . H34 H 1.0910 0.5935 0.2041 0.095 Uiso 1 1 calc R . . C35 C 1.1447(8) 0.5790(3) 0.3548(10) 0.068(3) Uani 1 1 d . . . C36 C 1.1391(9) 0.5481(5) 0.4315(9) 0.082(4) Uani 1 1 d . . . H36 H 1.1822 0.5505 0.4986 0.099 Uiso 1 1 calc R . . C37 C 1.0733(8) 0.5137(3) 0.4149(8) 0.064(3) Uani 1 1 d . . . H37 H 1.0714 0.4930 0.4704 0.077 Uiso 1 1 calc R . . C38 C 1.2166(9) 0.6182(5) 0.3750(12) 0.101(5) Uani 1 1 d . . . H38A H 1.2514 0.6115 0.3305 0.152 Uiso 1 1 calc R . . H38B H 1.2542 0.6168 0.4480 0.152 Uiso 1 1 calc R . . H38C H 1.1903 0.6512 0.3594 0.152 Uiso 1 1 calc R . . C39 C 0.9332(6) 0.2547(3) 0.2192(7) 0.042(2) Uani 1 1 d . . . C40 C 0.9943(8) 0.2252(4) 0.2867(8) 0.067(3) Uani 1 1 d . . . H40 H 1.0093 0.2307 0.3592 0.081 Uiso 1 1 calc R . . C41 C 1.0344(8) 0.1879(4) 0.2528(8) 0.071(3) Uani 1 1 d . . . H41 H 1.0752 0.1672 0.3022 0.086 Uiso 1 1 calc R . . C42 C 1.0169(7) 0.1793(3) 0.1471(8) 0.054(2) Uani 1 1 d . . . C43 C 0.9559(7) 0.2082(4) 0.0785(7) 0.056(2) Uani 1 1 d . . . H43 H 0.9416 0.2029 0.0060 0.067 Uiso 1 1 calc R . . C44 C 0.9152(6) 0.2451(3) 0.1136(7) 0.053(2) Uani 1 1 d . . . H44 H 0.8730 0.2649 0.0642 0.064 Uiso 1 1 calc R . . C45 C 1.0450(10) 0.1322(5) 0.0160(10) 0.107(5) Uani 1 1 d . . . H45A H 0.9840 0.1220 -0.0158 0.161 Uiso 1 1 calc R . . H45B H 1.0832 0.1053 0.0091 0.161 Uiso 1 1 calc R . . H45C H 1.0555 0.1620 -0.0192 0.161 Uiso 1 1 calc R . . C46 C 0.6029(6) 0.2855(3) 0.4313(7) 0.041(2) Uani 1 1 d . . . C47 C 0.6428(6) 0.2671(3) 0.5299(7) 0.047(2) Uani 1 1 d . . . H47 H 0.7020 0.2755 0.5659 0.057 Uiso 1 1 calc R . . C48 C 0.5989(8) 0.2364(3) 0.5791(7) 0.060(3) Uani 1 1 d . . . H48 H 0.6289 0.2257 0.6483 0.072 Uiso 1 1 calc R . . C49 C 0.5165(7) 0.2215(3) 0.5321(8) 0.052(2) Uani 1 1 d . . . C50 C 0.4743(7) 0.2398(4) 0.4303(9) 0.064(3) Uani 1 1 d . . . H50 H 0.4153 0.2308 0.3946 0.077 Uiso 1 1 calc R . . C51 C 0.5172(6) 0.2707(4) 0.3808(7) 0.052(2) Uani 1 1 d . . . H51 H 0.4874 0.2816 0.3119 0.063 Uiso 1 1 calc R . . C52 C 0.4672(8) 0.1899(4) 0.5819(9) 0.081(4) Uani 1 1 d . . . H52A H 0.5018 0.1604 0.6122 0.121 Uiso 1 1 calc R . . H52B H 0.4120 0.1796 0.5298 0.121 Uiso 1 1 calc R . . H52C H 0.4553 0.2089 0.6367 0.121 Uiso 1 1 calc R . . N1 N 0.6625(4) 0.3995(2) 0.3084(5) 0.0324(14) Uani 1 1 d . . . N2 N 0.7830(4) 0.4637(2) 0.2777(5) 0.0360(15) Uani 1 1 d . . . N3 N 0.8884(4) 0.3858(2) 0.2797(5) 0.0368(16) Uani 1 1 d . . . N4 N 0.7716(4) 0.3222(2) 0.3153(5) 0.0364(15) Uani 1 1 d . . . N5 N 0.5700(5) 0.5253(2) 0.2294(5) 0.0397(17) Uani 1 1 d . . . N6 N 0.4760(5) 0.5797(2) 0.1426(5) 0.0388(16) Uani 1 1 d . . . O1 O 1.0629(5) 0.1429(3) 0.1240(6) 0.077(2) Uani 1 1 d . . . Ni1 Ni 0.77594(7) 0.39278(3) 0.29522(8) 0.0379(3) Uani 1 1 d . . . Pd1 Pd 0.5000 0.5000 0.0000 0.0345(2) Uani 1 2 d S . . I1 I 0.37441(5) 0.45060(2) 0.03121(5) 0.0571(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 0.057(6) 0.033(4) 0.037(5) -0.001(3) 0.023(4) 0.009(4) C2 0.095(8) 0.047(5) 0.058(6) 0.029(5) 0.056(6) 0.015(5) C3 0.082(7) 0.031(4) 0.060(6) 0.006(4) 0.046(6) 0.013(4) C4 0.082(7) 0.016(3) 0.061(6) 0.005(3) 0.049(5) 0.006(4) C5 0.064(6) 0.015(3) 0.036(4) -0.002(3) 0.020(4) 0.008(3) C6 0.048(5) 0.021(4) 0.046(5) 0.007(3) 0.015(4) 0.001(4) C7 0.055(6) 0.028(4) 0.053(6) 0.011(4) 0.008(5) 0.001(4) C8 0.065(7) 0.027(4) 0.069(7) 0.007(4) 0.018(5) -0.002(4) C9 0.049(6) 0.038(5) 0.040(5) -0.003(4) 0.011(4) 0.003(4) C10 0.071(7) 0.024(4) 0.047(5) -0.008(4) 0.021(5) -0.019(4) C11 0.085(5) 0.049(4) 0.067(5) -0.005(3) 0.055(4) -0.017(4) C12 0.085(5) 0.049(4) 0.067(5) -0.005(3) 0.055(4) -0.017(4) C13 0.071(7) 0.038(5) 0.064(6) 0.003(4) 0.040(5) -0.001(4) C14 0.056(6) 0.032(4) 0.032(4) -0.004(3) 0.011(4) 0.001(4) C15 0.057(6) 0.033(4) 0.042(5) 0.003(4) 0.013(4) 0.005(4) C16 0.041(5) 0.032(4) 0.047(5) -0.005(4) 0.018(4) -0.003(4) C17 0.081(7) 0.032(4) 0.050(6) -0.011(4) 0.026(5) -0.001(5) C18 0.066(6) 0.019(4) 0.056(5) 0.005(4) 0.029(5) 0.003(4) C19 0.059(6) 0.019(3) 0.043(5) 0.000(3) 0.019(4) 0.002(4) C20 0.057(6) 0.030(4) 0.042(5) 0.002(4) 0.018(4) -0.011(4) C21 0.064(6) 0.020(4) 0.043(5) 0.009(3) 0.029(4) 0.004(4) C22 0.092(8) 0.043(5) 0.048(5) 0.006(4) 0.043(6) 0.024(5) C23 0.103(9) 0.055(6) 0.041(6) -0.010(4) 0.021(6) 0.032(6) C24 0.144(12) 0.081(8) 0.041(6) -0.017(6) 0.033(7) 0.028(8) C25 0.169(14) 0.044(6) 0.074(8) -0.002(5) 0.066(9) 0.038(7) C26 0.090(8) 0.033(5) 0.063(7) -0.002(4) 0.041(6) 0.012(5) C27 0.072(6) 0.030(4) 0.048(5) -0.004(4) 0.038(5) 0.004(4) C28 0.096(5) 0.063(4) 0.056(4) 0.001(3) 0.029(4) 0.025(4) C29 0.096(5) 0.063(4) 0.056(4) 0.001(3) 0.029(4) 0.025(4) C30 0.096(5) 0.063(4) 0.056(4) 0.001(3) 0.029(4) 0.025(4) C31 0.077(10) 0.27(3) 0.073(10) 0.001(12) 0.026(8) -0.012(13) C32 0.067(6) 0.024(4) 0.052(6) 0.003(4) 0.032(5) -0.001(4) C33 0.088(9) 0.070(7) 0.061(7) 0.005(6) 0.023(6) -0.010(6) C34 0.104(10) 0.053(6) 0.093(9) 0.017(6) 0.052(8) -0.024(7) C35 0.096(9) 0.031(5) 0.081(8) -0.009(5) 0.035(7) -0.011(5) C36 0.115(10) 0.082(8) 0.048(6) -0.016(6) 0.026(7) -0.041(8) C37 0.105(9) 0.042(5) 0.049(6) 0.007(4) 0.032(6) -0.020(5) C38 0.108(11) 0.075(8) 0.119(11) -0.008(8) 0.036(9) -0.057(8) C39 0.048(5) 0.038(4) 0.046(5) -0.005(4) 0.025(4) 0.006(4) C40 0.108(9) 0.047(6) 0.041(5) -0.004(4) 0.016(6) 0.024(6) C41 0.088(8) 0.071(7) 0.041(6) -0.008(5) 0.003(5) 0.035(6) C42 0.073(7) 0.039(5) 0.059(6) -0.001(4) 0.033(5) 0.014(5) C43 0.068(7) 0.060(6) 0.041(5) -0.004(4) 0.020(5) 0.012(5) C44 0.047(6) 0.053(6) 0.056(6) 0.008(5) 0.013(5) 0.023(4) C45 0.166(14) 0.083(9) 0.083(9) 0.002(7) 0.057(9) 0.070(10) C46 0.055(6) 0.023(4) 0.050(5) 0.002(3) 0.026(4) -0.004(4) C47 0.046(5) 0.035(4) 0.060(6) 0.000(4) 0.017(5) -0.009(4) C48 0.105(9) 0.033(5) 0.043(5) 0.012(4) 0.027(6) -0.011(5) C49 0.063(7) 0.037(5) 0.065(6) -0.002(4) 0.033(5) -0.005(4) C50 0.065(7) 0.049(6) 0.083(8) 0.007(5) 0.032(6) -0.009(5) C51 0.046(6) 0.064(6) 0.044(5) 0.001(4) 0.012(4) 0.000(5) C52 0.108(10) 0.064(7) 0.084(8) 0.008(6) 0.050(8) -0.035(7) N1 0.031(4) 0.030(3) 0.039(4) 0.004(3) 0.015(3) 0.006(3) N2 0.046(4) 0.027(3) 0.036(4) 0.002(3) 0.015(3) 0.006(3) N3 0.050(4) 0.023(3) 0.046(4) 0.003(3) 0.029(3) 0.004(3) N4 0.047(4) 0.022(3) 0.045(4) -0.004(3) 0.021(3) 0.003(3) N5 0.059(5) 0.022(3) 0.045(4) 0.002(3) 0.027(4) 0.014(3) N6 0.063(5) 0.022(3) 0.040(4) 0.007(3) 0.028(4) 0.012(3) O1 0.109(6) 0.051(4) 0.077(5) -0.011(4) 0.041(5) 0.035(4) Ni1 0.0556(7) 0.0237(5) 0.0412(6) 0.0010(4) 0.0251(5) 0.0039(5) Pd1 0.0533(6) 0.0176(4) 0.0409(5) 0.0014(3) 0.0267(4) 0.0044(4) I1 0.0749(5) 0.0422(3) 0.0669(4) 0.0021(3) 0.0407(4) -0.0082(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.387(10) . ? C1 C20 1.406(11) . ? C1 C2 1.414(12) . ? C2 C3 1.357(11) . ? C2 H2 0.9500 . ? C3 C4 1.446(12) . ? C3 H3 0.9500 . ? C4 N1 1.350(10) . ? C4 C5 1.398(10) . ? C5 C6 1.361(12) . ? C5 N5 1.452(10) . ? C6 N2 1.332(10) . ? C6 C7 1.458(11) . ? C7 C8 1.330(13) . ? C7 H7 0.9500 . ? C8 C9 1.435(11) . ? C8 H8 0.9500 . ? C9 N2 1.355(11) . ? C9 C10 1.377(13) . ? C10 C11 1.404(12) . ? C10 C32 1.467(12) . ? C11 N3 1.399(11) . ? C11 C12 1.438(14) . ? C12 C13 1.299(12) . ? C12 H12 0.9500 . ? C13 C14 1.470(12) . ? C13 H13 0.9500 . ? C14 N3 1.331(10) . ? C14 C15 1.359(11) . ? C15 C16 1.423(12) . ? C15 C39 1.481(11) . ? C16 N4 1.367(10) . ? C16 C17 1.435(12) . ? C17 C18 1.330(12) . ? C17 H17 0.9500 . ? C18 C19 1.433(10) . ? C18 H18 0.9500 . ? C19 N4 1.368(10) . ? C19 C20 1.398(12) . ? C20 C46 1.459(11) . ? C21 N6 1.348(9) . ? C21 N5 1.359(10) . ? C21 Pd1 2.007(8) . ? C22 C23 1.357(13) . ? C22 C27 1.384(13) . ? C22 N5 1.419(10) . ? C23 C24 1.417(13) . ? C23 H23 0.9500 . ? C24 C25 1.405(16) . ? C24 H24 0.9500 . ? C25 C26 1.358(15) . ? C25 H25 0.9500 . ? C26 C27 1.393(11) . ? C26 H26 0.9500 . ? C27 N6 1.406(10) . ? C28 N6 1.424(12) . ? C28 C29 1.573(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.486(14) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.551(17) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C37 1.369(14) . ? C32 C33 1.370(13) . ? C33 C34 1.419(15) . ? C33 H33 0.9500 . ? C34 C35 1.335(16) . ? C34 H34 0.9500 . ? C35 C36 1.365(15) . ? C35 C38 1.530(14) . ? C36 C37 1.378(15) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.360(13) . ? C39 C44 1.399(12) . ? C40 C41 1.364(13) . ? C40 H40 0.9500 . ? C41 C42 1.395(13) . ? C41 H41 0.9500 . ? C42 O1 1.335(10) . ? C42 C43 1.358(13) . ? C43 C44 1.368(12) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 O1 1.437(13) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.376(12) . ? C46 C51 1.390(12) . ? C47 C48 1.407(12) . ? C47 H47 0.9500 . ? C48 C49 1.339(14) . ? C48 H48 0.9500 . ? C49 C50 1.417(14) . ? C49 C52 1.485(13) . ? C50 C51 1.401(13) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? N1 Ni1 1.928(6) . ? N2 Ni1 1.931(6) . ? N3 Ni1 1.926(6) . ? N4 Ni1 1.922(6) . ? Pd1 C21 2.007(8) 3_665 ? Pd1 I1 2.5962(7) 3_665 ? Pd1 I1 2.5962(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C20 124.4(7) . . ? N1 C1 C2 109.9(7) . . ? C20 C1 C2 125.5(8) . . ? C3 C2 C1 108.5(8) . . ? C3 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? C2 C3 C4 104.4(8) . . ? C2 C3 H3 127.8 . . ? C4 C3 H3 127.8 . . ? N1 C4 C5 123.8(8) . . ? N1 C4 C3 112.0(7) . . ? C5 C4 C3 124.0(8) . . ? C6 C5 C4 122.1(8) . . ? C6 C5 N5 118.9(7) . . ? C4 C5 N5 118.1(8) . . ? N2 C6 C5 127.8(7) . . ? N2 C6 C7 110.3(8) . . ? C5 C6 C7 121.6(7) . . ? C8 C7 C6 105.6(8) . . ? C8 C7 H7 127.2 . . ? C6 C7 H7 127.2 . . ? C7 C8 C9 107.6(8) . . ? C7 C8 H8 126.2 . . ? C9 C8 H8 126.2 . . ? N2 C9 C10 127.3(8) . . ? N2 C9 C8 109.5(8) . . ? C10 C9 C8 123.0(8) . . ? C9 C10 C11 118.6(8) . . ? C9 C10 C32 120.9(8) . . ? C11 C10 C32 120.0(9) . . ? N3 C11 C10 126.1(9) . . ? N3 C11 C12 108.8(8) . . ? C10 C11 C12 125.1(9) . . ? C13 C12 C11 106.7(9) . . ? C13 C12 H12 126.7 . . ? C11 C12 H12 126.7 . . ? C12 C13 C14 109.3(9) . . ? C12 C13 H13 125.3 . . ? C14 C13 H13 125.3 . . ? N3 C14 C15 128.5(8) . . ? N3 C14 C13 107.8(7) . . ? C15 C14 C13 122.8(8) . . ? C14 C15 C16 119.8(8) . . ? C14 C15 C39 121.4(8) . . ? C16 C15 C39 118.6(7) . . ? N4 C16 C15 124.6(7) . . ? N4 C16 C17 110.3(7) . . ? C15 C16 C17 125.0(8) . . ? C18 C17 C16 107.2(8) . . ? C18 C17 H17 126.4 . . ? C16 C17 H17 126.4 . . ? C17 C18 C19 106.7(8) . . ? C17 C18 H18 126.6 . . ? C19 C18 H18 126.6 . . ? N4 C19 C20 124.9(7) . . ? N4 C19 C18 110.7(7) . . ? C20 C19 C18 123.5(8) . . ? C19 C20 C1 121.7(7) . . ? C19 C20 C46 118.6(7) . . ? C1 C20 C46 119.7(8) . . ? N6 C21 N5 105.7(7) . . ? N6 C21 Pd1 126.7(6) . . ? N5 C21 Pd1 127.5(5) . . ? C23 C22 C27 124.3(8) . . ? C23 C22 N5 130.0(8) . . ? C27 C22 N5 105.7(8) . . ? C22 C23 C24 116.2(10) . . ? C22 C23 H23 121.9 . . ? C24 C23 H23 121.9 . . ? C25 C24 C23 118.4(10) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? C26 C25 C24 124.8(9) . . ? C26 C25 H25 117.6 . . ? C24 C25 H25 117.6 . . ? C25 C26 C27 115.6(9) . . ? C25 C26 H26 122.2 . . ? C27 C26 H26 122.2 . . ? C22 C27 C26 120.6(9) . . ? C22 C27 N6 106.1(7) . . ? C26 C27 N6 133.3(9) . . ? N6 C28 C29 110.5(8) . . ? N6 C28 H28A 109.6 . . ? C29 C28 H28A 109.6 . . ? N6 C28 H28B 109.6 . . ? C29 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C30 C29 C28 111.4(9) . . ? C30 C29 H29A 109.3 . . ? C28 C29 H29A 109.3 . . ? C30 C29 H29B 109.3 . . ? C28 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? C29 C30 C31 106.7(10) . . ? C29 C30 H30A 110.4 . . ? C31 C30 H30A 110.4 . . ? C29 C30 H30B 110.4 . . ? C31 C30 H30B 110.4 . . ? H30A C30 H30B 108.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 117.5(9) . . ? C37 C32 C10 120.1(8) . . ? C33 C32 C10 122.4(9) . . ? C32 C33 C34 121.3(11) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C35 C34 C33 120.1(10) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 118.4(10) . . ? C34 C35 C38 119.7(11) . . ? C36 C35 C38 121.8(12) . . ? C35 C36 C37 122.3(11) . . ? C35 C36 H36 118.8 . . ? C37 C36 H36 118.8 . . ? C32 C37 C36 120.3(9) . . ? C32 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 116.2(8) . . ? C40 C39 C15 123.4(8) . . ? C44 C39 C15 120.3(8) . . ? C39 C40 C41 121.6(9) . . ? C39 C40 H40 119.2 . . ? C41 C40 H40 119.2 . . ? C40 C41 C42 121.5(9) . . ? C40 C41 H41 119.3 . . ? C42 C41 H41 119.3 . . ? O1 C42 C43 126.4(9) . . ? O1 C42 C41 115.7(9) . . ? C43 C42 C41 117.8(8) . . ? C42 C43 C44 120.0(9) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C43 C44 C39 122.9(8) . . ? C43 C44 H44 118.6 . . ? C39 C44 H44 118.6 . . ? O1 C45 H45A 109.5 . . ? O1 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O1 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 C51 116.4(8) . . ? C47 C46 C20 122.2(8) . . ? C51 C46 C20 121.3(8) . . ? C46 C47 C48 122.2(9) . . ? C46 C47 H47 118.9 . . ? C48 C47 H47 118.9 . . ? C49 C48 C47 122.4(9) . . ? C49 C48 H48 118.8 . . ? C47 C48 H48 118.8 . . ? C48 C49 C50 116.3(9) . . ? C48 C49 C52 124.1(10) . . ? C50 C49 C52 119.5(10) . . ? C51 C50 C49 121.7(10) . . ? C51 C50 H50 119.1 . . ? C49 C50 H50 119.1 . . ? C46 C51 C50 120.9(9) . . ? C46 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C4 N1 C1 104.9(6) . . ? C4 N1 Ni1 127.3(5) . . ? C1 N1 Ni1 127.4(5) . . ? C6 N2 C9 106.9(7) . . ? C6 N2 Ni1 125.1(6) . . ? C9 N2 Ni1 127.9(6) . . ? C14 N3 C11 107.3(7) . . ? C14 N3 Ni1 125.8(6) . . ? C11 N3 Ni1 126.8(6) . . ? C16 N4 C19 104.9(6) . . ? C16 N4 Ni1 126.9(5) . . ? C19 N4 Ni1 128.2(5) . . ? C21 N5 C22 110.8(6) . . ? C21 N5 C5 124.2(6) . . ? C22 N5 C5 124.4(7) . . ? C21 N6 C27 111.6(7) . . ? C21 N6 C28 125.2(7) . . ? C27 N6 C28 123.0(7) . . ? C42 O1 C45 117.2(8) . . ? N4 Ni1 N3 90.1(3) . . ? N4 Ni1 N1 89.7(3) . . ? N3 Ni1 N1 179.1(3) . . ? N4 Ni1 N2 178.6(3) . . ? N3 Ni1 N2 89.0(3) . . ? N1 Ni1 N2 91.1(3) . . ? C21 Pd1 C21 180.0(3) . 3_665 ? C21 Pd1 I1 90.8(2) . 3_665 ? C21 Pd1 I1 89.2(2) 3_665 3_665 ? C21 Pd1 I1 89.2(2) . . ? C21 Pd1 I1 90.8(2) 3_665 . ? I1 Pd1 I1 180.00(3) 3_665 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 3.9(11) . . . . ? C20 C1 C2 C3 -170.5(9) . . . . ? C1 C2 C3 C4 -5.6(11) . . . . ? C2 C3 C4 N1 5.9(11) . . . . ? C2 C3 C4 C5 -169.2(9) . . . . ? N1 C4 C5 C6 -12.5(14) . . . . ? C3 C4 C5 C6 162.0(9) . . . . ? N1 C4 C5 N5 178.5(8) . . . . ? C3 C4 C5 N5 -7.0(13) . . . . ? C4 C5 C6 N2 10.9(14) . . . . ? N5 C5 C6 N2 179.8(8) . . . . ? C4 C5 C6 C7 -162.2(8) . . . . ? N5 C5 C6 C7 6.7(12) . . . . ? N2 C6 C7 C8 -3.7(10) . . . . ? C5 C6 C7 C8 170.6(8) . . . . ? C6 C7 C8 C9 3.2(10) . . . . ? C7 C8 C9 N2 -1.8(11) . . . . ? C7 C8 C9 C10 172.8(9) . . . . ? N2 C9 C10 C11 11.2(14) . . . . ? C8 C9 C10 C11 -162.4(9) . . . . ? N2 C9 C10 C32 -177.2(8) . . . . ? C8 C9 C10 C32 9.3(13) . . . . ? C9 C10 C11 N3 -13.2(14) . . . . ? C32 C10 C11 N3 175.1(9) . . . . ? C9 C10 C11 C12 162.6(10) . . . . ? C32 C10 C11 C12 -9.1(15) . . . . ? N3 C11 C12 C13 3.3(12) . . . . ? C10 C11 C12 C13 -173.1(10) . . . . ? C11 C12 C13 C14 -2.6(11) . . . . ? C12 C13 C14 N3 1.0(11) . . . . ? C12 C13 C14 C15 -169.3(9) . . . . ? N3 C14 C15 C16 -7.8(14) . . . . ? C13 C14 C15 C16 160.2(8) . . . . ? N3 C14 C15 C39 177.3(8) . . . . ? C13 C14 C15 C39 -14.6(13) . . . . ? C14 C15 C16 N4 10.0(14) . . . . ? C39 C15 C16 N4 -174.9(8) . . . . ? C14 C15 C16 C17 -166.1(9) . . . . ? C39 C15 C16 C17 8.9(14) . . . . ? N4 C16 C17 C18 -4.1(11) . . . . ? C15 C16 C17 C18 172.5(9) . . . . ? C16 C17 C18 C19 3.5(11) . . . . ? C17 C18 C19 N4 -1.9(11) . . . . ? C17 C18 C19 C20 167.6(8) . . . . ? N4 C19 C20 C1 5.9(13) . . . . ? C18 C19 C20 C1 -162.1(8) . . . . ? N4 C19 C20 C46 -175.3(8) . . . . ? C18 C19 C20 C46 16.7(13) . . . . ? N1 C1 C20 C19 -4.5(13) . . . . ? C2 C1 C20 C19 169.1(9) . . . . ? N1 C1 C20 C46 176.7(8) . . . . ? C2 C1 C20 C46 -9.7(14) . . . . ? C27 C22 C23 C24 -1.3(18) . . . . ? N5 C22 C23 C24 -179.0(11) . . . . ? C22 C23 C24 C25 2.8(19) . . . . ? C23 C24 C25 C26 -4(2) . . . . ? C24 C25 C26 C27 3.0(19) . . . . ? C23 C22 C27 C26 0.6(16) . . . . ? N5 C22 C27 C26 178.8(8) . . . . ? C23 C22 C27 N6 -178.7(10) . . . . ? N5 C22 C27 N6 -0.6(10) . . . . ? C25 C26 C27 C22 -1.4(15) . . . . ? C25 C26 C27 N6 177.8(10) . . . . ? N6 C28 C29 C30 -173.4(8) . . . . ? C28 C29 C30 C31 174.7(11) . . . . ? C9 C10 C32 C37 107.6(11) . . . . ? C11 C10 C32 C37 -80.9(12) . . . . ? C9 C10 C32 C33 -72.1(12) . . . . ? C11 C10 C32 C33 99.4(12) . . . . ? C37 C32 C33 C34 -3.4(16) . . . . ? C10 C32 C33 C34 176.2(10) . . . . ? C32 C33 C34 C35 0.3(19) . . . . ? C33 C34 C35 C36 3.1(19) . . . . ? C33 C34 C35 C38 -178.6(12) . . . . ? C34 C35 C36 C37 -4(2) . . . . ? C38 C35 C36 C37 178.2(12) . . . . ? C33 C32 C37 C36 3.0(16) . . . . ? C10 C32 C37 C36 -176.6(10) . . . . ? C35 C36 C37 C32 0.4(19) . . . . ? C14 C15 C39 C40 95.0(12) . . . . ? C16 C15 C39 C40 -79.9(12) . . . . ? C14 C15 C39 C44 -81.3(12) . . . . ? C16 C15 C39 C44 103.7(10) . . . . ? C44 C39 C40 C41 -1.0(16) . . . . ? C15 C39 C40 C41 -177.5(11) . . . . ? C39 C40 C41 C42 2.2(19) . . . . ? C40 C41 C42 O1 177.4(11) . . . . ? C40 C41 C42 C43 -2.3(18) . . . . ? O1 C42 C43 C44 -178.4(10) . . . . ? C41 C42 C43 C44 1.3(16) . . . . ? C42 C43 C44 C39 -0.2(16) . . . . ? C40 C39 C44 C43 0.0(15) . . . . ? C15 C39 C44 C43 176.6(9) . . . . ? C19 C20 C46 C47 64.1(11) . . . . ? C1 C20 C46 C47 -117.1(10) . . . . ? C19 C20 C46 C51 -112.6(10) . . . . ? C1 C20 C46 C51 66.2(11) . . . . ? C51 C46 C47 C48 -2.2(13) . . . . ? C20 C46 C47 C48 -179.0(8) . . . . ? C46 C47 C48 C49 2.4(15) . . . . ? C47 C48 C49 C50 -1.9(14) . . . . ? C47 C48 C49 C52 -178.7(9) . . . . ? C48 C49 C50 C51 1.5(14) . . . . ? C52 C49 C50 C51 178.4(10) . . . . ? C47 C46 C51 C50 1.8(13) . . . . ? C20 C46 C51 C50 178.6(8) . . . . ? C49 C50 C51 C46 -1.5(15) . . . . ? C5 C4 N1 C1 171.6(8) . . . . ? C3 C4 N1 C1 -3.5(10) . . . . ? C5 C4 N1 Ni1 -2.2(13) . . . . ? C3 C4 N1 Ni1 -177.2(6) . . . . ? C20 C1 N1 C4 174.4(8) . . . . ? C2 C1 N1 C4 -0.2(10) . . . . ? C20 C1 N1 Ni1 -11.9(12) . . . . ? C2 C1 N1 Ni1 173.6(6) . . . . ? C5 C6 N2 C9 -171.3(8) . . . . ? C7 C6 N2 C9 2.5(9) . . . . ? C5 C6 N2 Ni1 5.4(12) . . . . ? C7 C6 N2 Ni1 179.2(6) . . . . ? C10 C9 N2 C6 -174.8(8) . . . . ? C8 C9 N2 C6 -0.5(10) . . . . ? C10 C9 N2 Ni1 8.7(13) . . . . ? C8 C9 N2 Ni1 -177.0(6) . . . . ? C15 C14 N3 C11 170.7(9) . . . . ? C13 C14 N3 C11 1.2(10) . . . . ? C15 C14 N3 Ni1 -11.2(13) . . . . ? C13 C14 N3 Ni1 179.4(5) . . . . ? C10 C11 N3 C14 173.7(9) . . . . ? C12 C11 N3 C14 -2.7(10) . . . . ? C10 C11 N3 Ni1 -4.5(14) . . . . ? C12 C11 N3 Ni1 179.1(6) . . . . ? C15 C16 N4 C19 -173.8(8) . . . . ? C17 C16 N4 C19 2.8(9) . . . . ? C15 C16 N4 Ni1 6.8(12) . . . . ? C17 C16 N4 Ni1 -176.6(6) . . . . ? C20 C19 N4 C16 -169.9(8) . . . . ? C18 C19 N4 C16 -0.6(9) . . . . ? C20 C19 N4 Ni1 9.5(12) . . . . ? C18 C19 N4 Ni1 178.7(6) . . . . ? N6 C21 N5 C22 -2.0(9) . . . . ? Pd1 C21 N5 C22 180.0(6) . . . . ? N6 C21 N5 C5 -173.3(7) . . . . ? Pd1 C21 N5 C5 8.6(12) . . . . ? C23 C22 N5 C21 179.6(11) . . . . ? C27 C22 N5 C21 1.6(10) . . . . ? C23 C22 N5 C5 -9.1(16) . . . . ? C27 C22 N5 C5 172.9(8) . . . . ? C6 C5 N5 C21 91.2(10) . . . . ? C4 C5 N5 C21 -99.4(9) . . . . ? C6 C5 N5 C22 -79.0(10) . . . . ? C4 C5 N5 C22 90.4(10) . . . . ? N5 C21 N6 C27 1.6(9) . . . . ? Pd1 C21 N6 C27 179.7(6) . . . . ? N5 C21 N6 C28 -174.0(8) . . . . ? Pd1 C21 N6 C28 4.1(12) . . . . ? C22 C27 N6 C21 -0.6(10) . . . . ? C26 C27 N6 C21 -179.9(10) . . . . ? C22 C27 N6 C28 175.1(8) . . . . ? C26 C27 N6 C28 -4.2(15) . . . . ? C29 C28 N6 C21 104.9(10) . . . . ? C29 C28 N6 C27 -70.3(11) . . . . ? C43 C42 O1 C45 -1.8(17) . . . . ? C41 C42 O1 C45 178.5(11) . . . . ? C16 N4 Ni1 N3 -18.1(7) . . . . ? C19 N4 Ni1 N3 162.7(7) . . . . ? C16 N4 Ni1 N1 161.0(7) . . . . ? C19 N4 Ni1 N1 -18.2(7) . . . . ? C14 N3 Ni1 N4 20.1(7) . . . . ? C11 N3 Ni1 N4 -162.1(8) . . . . ? C14 N3 Ni1 N2 -161.0(7) . . . . ? C11 N3 Ni1 N2 16.9(8) . . . . ? C4 N1 Ni1 N4 -168.4(7) . . . . ? C1 N1 Ni1 N4 19.3(7) . . . . ? C4 N1 Ni1 N2 12.7(7) . . . . ? C1 N1 Ni1 N2 -159.7(7) . . . . ? C6 N2 Ni1 N3 164.9(7) . . . . ? C9 N2 Ni1 N3 -19.1(7) . . . . ? C6 N2 Ni1 N1 -14.1(7) . . . . ? C9 N2 Ni1 N1 161.8(7) . . . . ? N6 C21 Pd1 I1 92.0(7) . . . 3_665 ? N5 C21 Pd1 I1 -90.3(7) . . . 3_665 ? N6 C21 Pd1 I1 -88.0(7) . . . . ? N5 C21 Pd1 I1 89.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.83 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.549 _refine_diff_density_min -0.960 _refine_diff_density_rms 0.160 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.498 0.002 -0.009 1733.8 176.8 _platon_squeeze_details ; The residual electron density was assigned to two molecules of the ethanol solvent [177/4= 44 e per asymmetric unit; two molecules of C2H6O1 would give 52 e]. ;