# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' _publ_contact_author_name # Name of author for correspondence ; Julita Eilmes ; _publ_contact_author_address # address of author for correspondence ; Department of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Krakow, Poland ; _publ_contact_author_email jeilmes@chemia.uj.edu.pl _publ_contact_author_phone +48-12-6336377 _publ_contact_author_fax +48-12-6340515 loop_ _publ_author_name _publ_author_address 'Dariusz Pawlica' ; Department of Chemistry Jagiellonian University Ingardena 3, 30-060 Krakow Poland ; 'Marek Marszalek' ; Department of Chemistry Jagiellonian University Ingardena 3, 30-060 Krakow Poland ; 'Grzegorz Mynarczuk' ; Department of Chemistry Jagiellonian University Ingardena 3, 30-060 Krakow Poland ; 'Leslaw Sieron' ; Institute of General & Ecological Chemistry Technical University of Lodz \.Zeromskiego 116 90-924 Lodz Poland ; 'Julita Eilmes' ; Department of Chemistry Jagiellonian University Ingardena 3, 30-060 Krakow Poland ; _publ_section_title ; New unsymmetrical Schiff base Ni(II) complexes as scaffolds for dendritic and amino acid superstructure ; ###################### data_3D3 _database_code_depnum_ccdc_archive 'CCDC 255522' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [8-(3'-(3,5-dibenzyloxy-benzyloxy)-2'-hydroxyphenyl)- (5,6)-benzo-4,7-diazaocta-2,7-dien-1-onato(2-)]nickel(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H36 N2 Ni O5' _chemical_formula_sum 'C44 H36 N2 Ni O5' _chemical_formula_weight 731.46 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2878(5) _cell_length_b 14.4364(8) _cell_length_c 17.4246(10) _cell_angle_alpha 72.557(5) _cell_angle_beta 85.278(5) _cell_angle_gamma 82.046(5) _cell_volume 1730.49(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5583 _cell_measurement_theta_min 9.20 _cell_measurement_theta_max 23.08 _exptl_crystal_description prism _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.613 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7917 _exptl_absorpt_correction_T_max 0.9584 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'CX-Mo12x0.4-S Seifert Mo tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'KUMA KM4CCD diffractometer' _diffrn_measurement_device_type ? _diffrn_measurement_method \w _diffrn_detector_type CCD _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10658 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.1229 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _reflns_number_total 6121 _reflns_number_gt 3119 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis CCD' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'SHELXTL/PC XP' _computing_publication_material PLATON _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^)+(0.0120P)^2^] 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 SHELXL _refine_ls_extinction_coef 0.00087(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6121 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0524 _refine_ls_goodness_of_fit_ref 0.675 _refine_ls_restrained_S_all 0.675 _refine_ls_shift/su_max 0.105 _refine_ls_shift/su_mean 0.023 _refine_diff_density_max 0.229 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.040 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 Ni Ni 0.24011(6) 0.01781(3) 0.47993(2) 0.03578(12) Uani 1 1 d . . . O1 O 0.2475(3) 0.09643(13) 0.37434(10) 0.0404(5) Uani 1 1 d . . . O2 O 0.1928(3) -0.07545(13) 0.43399(10) 0.0390(5) Uani 1 1 d . . . O3 O 0.2047(3) 0.19174(13) 0.21285(10) 0.0414(5) Uani 1 1 d . . . O4 O 0.2639(3) -0.11753(13) 0.05446(10) 0.0515(6) Uani 1 1 d . . . O5 O 0.2379(3) 0.22049(14) -0.08701(11) 0.0569(6) Uani 1 1 d . . . N1 N 0.2994(3) 0.11252(16) 0.52297(13) 0.0344(6) Uani 1 1 d . . . N2 N 0.2190(3) -0.06102(16) 0.58647(12) 0.0339(6) Uani 1 1 d . . . C1 C 0.2881(4) 0.0826(2) 0.60892(15) 0.0362(8) Uani 1 1 d . . . C2 C 0.3210(4) 0.1392(2) 0.65717(17) 0.0485(9) Uani 1 1 d . . . H2 H 0.3766 0.1962 0.6353 0.058 Uiso 1 1 calc R . . C3 C 0.2698(4) 0.1092(2) 0.73826(17) 0.0540(10) Uani 1 1 d . . . H3 H 0.2952 0.1447 0.7720 0.065 Uiso 1 1 calc R . . C4 C 0.1817(4) 0.0273(2) 0.76867(17) 0.0488(9) Uani 1 1 d . . . H4 H 0.1373 0.0112 0.8220 0.059 Uiso 1 1 calc R . . C5 C 0.1569(4) -0.0319(2) 0.72235(15) 0.0398(8) Uani 1 1 d . . . H5 H 0.0970 -0.0875 0.7441 0.048 Uiso 1 1 calc R . . C6 C 0.2232(4) -0.00709(19) 0.64203(15) 0.0361(8) Uani 1 1 d . . . C7 C 0.2736(4) 0.1877(2) 0.34884(16) 0.0349(8) Uani 1 1 d . . . C8 C 0.2581(4) 0.2384(2) 0.26510(16) 0.0361(8) Uani 1 1 d . . . C9 C 0.2839(4) 0.3344(2) 0.23466(17) 0.0501(9) Uani 1 1 d . . . H9 H 0.2739 0.3649 0.1797 0.060 Uiso 1 1 calc R . . C10 C 0.3252(4) 0.3882(2) 0.28455(18) 0.0554(10) Uani 1 1 d . . . H10 H 0.3430 0.4537 0.2632 0.066 Uiso 1 1 calc R . . C11 C 0.3388(4) 0.3430(2) 0.36489(17) 0.0502(9) Uani 1 1 d . . . H11 H 0.3646 0.3785 0.3984 0.060 Uiso 1 1 calc R . . C12 C 0.3148(4) 0.2433(2) 0.39840(16) 0.0358(8) Uani 1 1 d . . . C13 C 0.3255(4) 0.2006(2) 0.48278(16) 0.0403(8) Uani 1 1 d . . . H13 H 0.3544 0.2404 0.5122 0.048 Uiso 1 1 calc R . . C14 C 0.1817(4) -0.1660(2) 0.47051(17) 0.0350(7) Uani 1 1 d . . . C15 C 0.1995(4) -0.2070(2) 0.55226(16) 0.0397(8) Uani 1 1 d . . . H15 H 0.2000 -0.2745 0.5721 0.048 Uiso 1 1 calc R . . C16 C 0.2171(4) -0.1568(2) 0.60824(16) 0.0336(7) Uani 1 1 d . . . C17 C 0.2428(4) -0.22107(19) 0.69355(15) 0.0442(8) Uani 1 1 d . . . H171 H 0.3238 -0.1939 0.7195 0.053 Uiso 1 1 calc R . . H172 H 0.2963 -0.2855 0.6930 0.053 Uiso 1 1 calc R . . H173 H 0.1247 -0.2247 0.7224 0.053 Uiso 1 1 calc R . . C21 C 0.1510(4) -0.22642(19) 0.41813(17) 0.0386(8) Uani 1 1 d . . . C22 C 0.0908(4) -0.3179(2) 0.44845(18) 0.0552(9) Uani 1 1 d . . . H22 H 0.0696 -0.3438 0.5037 0.066 Uiso 1 1 calc R . . C23 C 0.0619(5) -0.3712(2) 0.3970(2) 0.0673(11) Uani 1 1 d . . . H23 H 0.0241 -0.4331 0.4180 0.081 Uiso 1 1 calc R . . C24 C 0.0888(5) -0.3330(2) 0.3151(2) 0.0616(10) Uani 1 1 d . . . H24 H 0.0670 -0.3684 0.2808 0.074 Uiso 1 1 calc R . . C25 C 0.1477(4) -0.2427(2) 0.28451(18) 0.0570(10) Uani 1 1 d . . . H25 H 0.1663 -0.2166 0.2292 0.068 Uiso 1 1 calc R . . C26 C 0.1797(4) -0.1897(2) 0.33577(17) 0.0454(8) Uani 1 1 d . . . H26 H 0.2211 -0.1287 0.3143 0.055 Uiso 1 1 calc R . . C30 C 0.3233(4) 0.1057(2) 0.20701(16) 0.0510(9) Uani 1 1 d . . . H301 H 0.2951 0.0496 0.2515 0.061 Uiso 1 1 calc R . . H302 H 0.4522 0.1146 0.2090 0.061 Uiso 1 1 calc R . . C31 C 0.2902(4) 0.0890(2) 0.12775(16) 0.0396(8) Uani 1 1 d . . . C32 C 0.2872(4) -0.0049(2) 0.12475(16) 0.0444(8) Uani 1 1 d . . . H32 H 0.2994 -0.0571 0.1715 0.053 Uiso 1 1 calc R . . C33 C 0.2660(4) -0.0216(2) 0.05133(16) 0.0414(8) Uani 1 1 d . . . C34 C 0.2495(4) 0.0558(2) -0.01739(16) 0.0433(8) Uani 1 1 d . . . H34 H 0.2353 0.0450 -0.0665 0.052 Uiso 1 1 calc R . . C35 C 0.2540(4) 0.1504(2) -0.01373(17) 0.0416(8) Uani 1 1 d . . . C36 C 0.2715(4) 0.1683(2) 0.05845(16) 0.0424(8) Uani 1 1 d . . . H36 H 0.2709 0.2318 0.0609 0.051 Uiso 1 1 calc R . . C40 C 0.2367(4) -0.13592(19) -0.01920(15) 0.0426(8) Uani 1 1 d . . . H401 H 0.3314 -0.1091 -0.0590 0.051 Uiso 1 1 calc R . . H402 H 0.1168 -0.1036 -0.0391 0.051 Uiso 1 1 calc R . . C41 C 0.2455(4) -0.2428(2) -0.00791(17) 0.0416(8) Uani 1 1 d . . . C42 C 0.2692(4) -0.3120(2) 0.06438(18) 0.0558(10) Uani 1 1 d . . . H42 H 0.2782 -0.2932 0.1104 0.067 Uiso 1 1 calc R . . C43 C 0.2800(5) -0.4106(2) 0.0699(2) 0.0719(11) Uani 1 1 d . . . H43 H 0.2981 -0.4571 0.1197 0.086 Uiso 1 1 calc R . . C44 C 0.2648(5) -0.4399(3) 0.0045(2) 0.0844(13) Uani 1 1 d . . . H44 H 0.2741 -0.5061 0.0085 0.101 Uiso 1 1 calc R . . C45 C 0.2356(7) -0.3709(3) -0.0677(2) 0.1149(17) Uani 1 1 d . . . H45 H 0.2209 -0.3898 -0.1132 0.138 Uiso 1 1 calc R . . C46 C 0.2278(6) -0.2735(3) -0.0737(2) 0.0925(14) Uani 1 1 d . . . H46 H 0.2102 -0.2273 -0.1236 0.111 Uiso 1 1 calc R . . C50 C 0.2444(4) 0.3195(2) -0.08975(17) 0.0522(9) Uani 1 1 d . . . H501 H 0.3502 0.3243 -0.0614 0.063 Uiso 1 1 calc R . . H502 H 0.1326 0.3439 -0.0642 0.063 Uiso 1 1 calc R . . C51 C 0.2607(4) 0.3787(2) -0.17689(18) 0.0434(8) Uani 1 1 d . . . C52 C 0.3881(5) 0.3463(2) -0.22887(19) 0.0543(9) Uani 1 1 d . . . H52 H 0.4631 0.2873 -0.2100 0.065 Uiso 1 1 calc R . . C53 C 0.4060(5) 0.4006(2) -0.30904(19) 0.0616(10) Uani 1 1 d . . . H53 H 0.4924 0.3783 -0.3438 0.074 Uiso 1 1 calc R . . C54 C 0.2942(5) 0.4880(3) -0.3365(2) 0.0636(11) Uani 1 1 d . . . H54 H 0.3038 0.5246 -0.3903 0.076 Uiso 1 1 calc R . . C55 C 0.1706(5) 0.5204(2) -0.2853(2) 0.0649(11) Uani 1 1 d . . . H55 H 0.0971 0.5799 -0.3040 0.078 Uiso 1 1 calc R . . C56 C 0.1519(4) 0.4662(2) -0.20545(19) 0.0539(9) Uani 1 1 d . . . H56 H 0.0654 0.4890 -0.1710 0.065 Uiso 1 1 calc R . . 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 Ni 0.0469(3) 0.0336(2) 0.0286(2) -0.01006(16) -0.00299(18) -0.00796(19) O1 0.0655(16) 0.0319(11) 0.0258(11) -0.0075(9) 0.0001(10) -0.0161(11) O2 0.0564(15) 0.0319(11) 0.0325(12) -0.0115(9) -0.0073(10) -0.0098(11) O3 0.0502(15) 0.0423(12) 0.0330(11) -0.0128(10) -0.0071(10) -0.0023(11) O4 0.0842(18) 0.0402(13) 0.0308(12) -0.0081(10) -0.0048(11) -0.0137(12) O5 0.101(2) 0.0385(13) 0.0309(12) -0.0037(10) -0.0132(12) -0.0154(12) N1 0.0406(17) 0.0319(14) 0.0335(14) -0.0113(12) -0.0018(12) -0.0097(12) N2 0.0429(18) 0.0349(14) 0.0262(14) -0.0103(12) -0.0085(12) -0.0051(12) C1 0.040(2) 0.0457(19) 0.0257(17) -0.0143(15) -0.0062(15) -0.0042(16) C2 0.062(3) 0.048(2) 0.041(2) -0.0169(16) -0.0067(17) -0.0151(18) C3 0.078(3) 0.058(2) 0.036(2) -0.0226(17) -0.0159(19) -0.011(2) C4 0.060(3) 0.057(2) 0.0303(18) -0.0153(16) -0.0053(17) -0.0007(19) C5 0.048(2) 0.0423(18) 0.0298(17) -0.0106(15) -0.0023(15) -0.0067(16) C6 0.047(2) 0.0369(18) 0.0265(17) -0.0102(14) -0.0074(15) -0.0055(16) C7 0.037(2) 0.0367(18) 0.0315(17) -0.0101(15) -0.0004(15) -0.0067(15) C8 0.043(2) 0.0356(18) 0.0291(17) -0.0080(14) -0.0033(15) -0.0053(15) C9 0.069(3) 0.0370(19) 0.0386(19) -0.0025(15) -0.0067(17) -0.0044(17) C10 0.082(3) 0.0331(19) 0.051(2) -0.0082(17) -0.0096(19) -0.0125(18) C11 0.071(3) 0.0391(19) 0.044(2) -0.0144(16) -0.0085(18) -0.0130(18) C12 0.044(2) 0.0371(18) 0.0303(17) -0.0133(14) -0.0004(15) -0.0106(15) C13 0.050(2) 0.0389(19) 0.0378(19) -0.0187(16) -0.0030(16) -0.0092(17) C14 0.034(2) 0.0348(18) 0.0388(18) -0.0143(15) -0.0040(15) -0.0036(15) C15 0.052(2) 0.0327(18) 0.0338(18) -0.0067(15) -0.0082(16) -0.0064(16) C16 0.038(2) 0.0344(18) 0.0280(17) -0.0083(14) -0.0016(15) -0.0051(15) C17 0.056(2) 0.0380(18) 0.0377(19) -0.0097(15) -0.0061(17) -0.0020(16) C21 0.048(2) 0.0315(17) 0.0396(18) -0.0128(15) -0.0106(16) -0.0043(15) C22 0.079(3) 0.048(2) 0.0437(19) -0.0152(17) -0.0089(18) -0.0180(19) C23 0.098(3) 0.044(2) 0.069(3) -0.0175(19) -0.016(2) -0.026(2) C24 0.078(3) 0.053(2) 0.068(3) -0.037(2) -0.017(2) -0.006(2) C25 0.080(3) 0.053(2) 0.046(2) -0.0245(18) -0.0078(19) -0.008(2) C26 0.058(2) 0.0383(18) 0.043(2) -0.0161(16) -0.0059(17) -0.0065(16) C30 0.069(3) 0.049(2) 0.0371(19) -0.0184(16) -0.0099(17) 0.0037(18) C31 0.047(2) 0.0458(19) 0.0286(17) -0.0144(15) -0.0039(15) -0.0062(16) C32 0.055(2) 0.046(2) 0.0299(17) -0.0074(15) 0.0020(16) -0.0085(17) C33 0.053(2) 0.0403(19) 0.0328(18) -0.0112(16) -0.0020(17) -0.0093(17) C34 0.059(2) 0.046(2) 0.0283(17) -0.0132(16) -0.0034(16) -0.0111(18) C35 0.052(2) 0.0409(19) 0.0310(18) -0.0059(15) -0.0048(16) -0.0096(16) C36 0.059(2) 0.0378(18) 0.0328(18) -0.0098(15) -0.0073(16) -0.0107(16) C40 0.054(2) 0.046(2) 0.0301(18) -0.0124(15) -0.0012(16) -0.0112(17) C41 0.047(2) 0.0408(19) 0.0378(19) -0.0121(16) -0.0016(16) -0.0058(16) C42 0.074(3) 0.049(2) 0.047(2) -0.0160(18) -0.0048(19) -0.0115(19) C43 0.091(3) 0.051(2) 0.066(3) -0.004(2) -0.006(2) -0.008(2) C44 0.113(4) 0.047(2) 0.098(3) -0.031(2) -0.002(3) -0.006(2) C45 0.223(6) 0.064(3) 0.070(3) -0.035(2) -0.017(3) -0.021(3) C46 0.182(4) 0.052(2) 0.049(2) -0.020(2) -0.016(3) -0.015(3) C50 0.064(3) 0.045(2) 0.048(2) -0.0130(17) -0.0032(18) -0.0105(18) C51 0.046(2) 0.0407(19) 0.046(2) -0.0092(17) -0.0089(18) -0.0138(17) C52 0.059(3) 0.047(2) 0.052(2) -0.0066(18) -0.0081(19) -0.0019(18) C53 0.068(3) 0.065(2) 0.051(2) -0.0123(19) 0.001(2) -0.016(2) C54 0.073(3) 0.060(3) 0.053(2) 0.003(2) -0.014(2) -0.028(2) C55 0.080(3) 0.034(2) 0.072(3) 0.003(2) -0.016(2) -0.012(2) C56 0.062(3) 0.038(2) 0.062(2) -0.0128(18) -0.0087(19) -0.0086(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O1 1.8507(17) . ? Ni O2 1.8420(17) . ? Ni N1 1.858(2) . ? Ni N2 1.871(2) . ? O1 C7 1.294(3) . ? O2 C14 1.281(3) . ? O3 C8 1.391(3) . ? O3 C30 1.438(3) . ? O4 C33 1.371(3) . ? O4 C40 1.421(3) . ? O5 C35 1.373(3) . ? O5 C50 1.423(3) . ? N1 C13 1.286(3) . ? N1 C1 1.428(3) . ? N2 C16 1.322(3) . ? N2 C6 1.417(3) . ? C1 C6 1.382(3) . ? C1 C2 1.390(3) . ? C2 C3 1.384(3) . ? C2 H2 0.9300 . ? C3 C4 1.368(3) . ? C3 H3 0.9300 . ? C4 C5 1.377(3) . ? C4 H4 0.9300 . ? C5 C6 1.399(3) . ? C5 H5 0.9300 . ? C7 C12 1.417(3) . ? C7 C8 1.429(3) . ? C8 C9 1.361(3) . ? C9 C10 1.401(3) . ? C9 H9 0.9300 . ? C10 C11 1.361(3) . ? C10 H10 0.9300 . ? C11 C12 1.411(3) . ? C11 H11 0.9300 . ? C12 C13 1.418(3) . ? C13 H13 0.9300 . ? C14 C15 1.379(3) . ? C14 C21 1.487(3) . ? C15 C16 1.401(3) . ? C15 H15 0.9300 . ? C16 C17 1.509(3) . ? C17 H171 0.9600 . ? C17 H172 0.9600 . ? C17 H173 0.9600 . ? C21 C26 1.382(3) . ? C21 C22 1.385(3) . ? C22 C23 1.390(3) . ? C22 H22 0.9300 . ? C23 C24 1.374(4) . ? C23 H23 0.9300 . ? C24 C25 1.367(4) . ? C24 H24 0.9300 . ? C25 C26 1.389(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C30 C31 1.514(3) . ? C30 H301 0.9700 . ? C30 H302 0.9700 . ? C31 C32 1.376(3) . ? C31 C36 1.393(3) . ? C32 C33 1.396(3) . ? C32 H32 0.9300 . ? C33 C34 1.372(3) . ? C34 C35 1.392(3) . ? C34 H34 0.9300 . ? C35 C36 1.377(3) . ? C36 H36 0.9300 . ? C40 C41 1.489(3) . ? C40 H401 0.9700 . ? C40 H402 0.9700 . ? C41 C42 1.359(3) . ? C41 C46 1.368(4) . ? C42 C43 1.389(4) . ? C42 H42 0.9300 . ? C43 C44 1.347(4) . ? C43 H43 0.9300 . ? C44 C45 1.362(4) . ? C44 H44 0.9300 . ? C45 C46 1.371(4) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C50 C51 1.507(3) . ? C50 H501 0.9700 . ? C50 H502 0.9700 . ? C51 C56 1.372(4) . ? C51 C52 1.377(4) . ? C52 C53 1.387(4) . ? C52 H52 0.9300 . ? C53 C54 1.379(4) . ? C53 H53 0.9300 . ? C54 C55 1.352(4) . ? C54 H54 0.9300 . ? C55 C56 1.382(4) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? 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 O2 Ni O1 83.59(8) . . ? O2 Ni N1 176.98(10) . . ? O1 Ni N1 94.80(9) . . ? O2 Ni N2 95.60(8) . . ? O1 Ni N2 176.99(10) . . ? N1 Ni N2 86.13(9) . . ? C7 O1 Ni 127.40(17) . . ? C14 O2 Ni 126.37(17) . . ? C8 O3 C30 116.1(2) . . ? C33 O4 C40 116.5(2) . . ? C35 O5 C50 118.1(2) . . ? C13 N1 C1 121.2(2) . . ? C13 N1 Ni 125.67(19) . . ? C1 N1 Ni 112.61(17) . . ? C16 N2 C6 123.4(2) . . ? C16 N2 Ni 124.65(18) . . ? C6 N2 Ni 111.72(17) . . ? C6 C1 C2 121.0(3) . . ? C6 C1 N1 113.5(2) . . ? C2 C1 N1 125.2(3) . . ? C3 C2 C1 118.8(3) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 121.7(3) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C4 C5 C6 118.9(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.6 . . ? C1 C6 C5 118.7(3) . . ? C1 C6 N2 114.0(2) . . ? C5 C6 N2 127.1(2) . . ? O1 C7 C12 124.7(3) . . ? O1 C7 C8 119.1(2) . . ? C12 C7 C8 116.2(2) . . ? C9 C8 O3 117.9(2) . . ? C9 C8 C7 121.8(3) . . ? O3 C8 C7 120.2(2) . . ? C8 C9 C10 121.2(3) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 118.9(3) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 121.5(3) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C7 120.4(3) . . ? C11 C12 C13 119.1(3) . . ? C7 C12 C13 120.4(2) . . ? N1 C13 C12 126.8(3) . . ? N1 C13 H13 116.6 . . ? C12 C13 H13 116.6 . . ? O2 C14 C15 123.7(3) . . ? O2 C14 C21 115.3(2) . . ? C15 C14 C21 121.0(2) . . ? C14 C15 C16 126.2(3) . . ? C14 C15 H15 116.9 . . ? C16 C15 H15 116.9 . . ? N2 C16 C15 121.9(2) . . ? N2 C16 C17 123.2(2) . . ? C15 C16 C17 114.8(2) . . ? C16 C17 H171 109.5 . . ? C16 C17 H172 109.5 . . ? H171 C17 H172 109.5 . . ? C16 C17 H173 109.5 . . ? H171 C17 H173 109.5 . . ? H172 C17 H173 109.5 . . ? C26 C21 C22 118.3(3) . . ? C26 C21 C14 119.1(2) . . ? C22 C21 C14 122.6(3) . . ? C21 C22 C23 120.4(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 120.5(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 119.6(3) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.2(3) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 121.0(3) . . ? C21 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? O3 C30 C31 107.9(2) . . ? O3 C30 H301 110.1 . . ? C31 C30 H301 110.1 . . ? O3 C30 H302 110.1 . . ? C31 C30 H302 110.1 . . ? H301 C30 H302 108.4 . . ? C32 C31 C36 121.0(2) . . ? C32 C31 C30 119.2(3) . . ? C36 C31 C30 119.7(2) . . ? C31 C32 C33 119.8(3) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? O4 C33 C34 124.8(2) . . ? O4 C33 C32 115.6(2) . . ? C34 C33 C32 119.6(3) . . ? C33 C34 C35 120.1(3) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? O5 C35 C36 125.2(3) . . ? O5 C35 C34 113.8(2) . . ? C36 C35 C34 121.0(3) . . ? C35 C36 C31 118.5(3) . . ? C35 C36 H36 120.8 . . ? C31 C36 H36 120.8 . . ? O4 C40 C41 110.8(2) . . ? O4 C40 H401 109.5 . . ? C41 C40 H401 109.5 . . ? O4 C40 H402 109.5 . . ? C41 C40 H402 109.5 . . ? H401 C40 H402 108.1 . . ? C42 C41 C46 117.9(3) . . ? C42 C41 C40 123.6(3) . . ? C46 C41 C40 118.4(3) . . ? C41 C42 C43 120.4(3) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C44 C43 C42 121.1(3) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 118.8(3) . . ? C43 C44 H44 120.6 . . ? C45 C44 H44 120.6 . . ? C44 C45 C46 120.3(4) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C41 C46 C45 121.5(3) . . ? C41 C46 H46 119.3 . . ? C45 C46 H46 119.3 . . ? O5 C50 C51 107.9(2) . . ? O5 C50 H501 110.1 . . ? C51 C50 H501 110.1 . . ? O5 C50 H502 110.1 . . ? C51 C50 H502 110.1 . . ? H501 C50 H502 108.4 . . ? C56 C51 C52 118.9(3) . . ? C56 C51 C50 120.8(3) . . ? C52 C51 C50 120.2(3) . . ? C51 C52 C53 120.8(3) . . ? C51 C52 H52 119.6 . . ? C53 C52 H52 119.6 . . ? C54 C53 C52 119.2(3) . . ? C54 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C55 C54 C53 120.0(3) . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C54 C55 C56 120.9(3) . . ? C54 C55 H55 119.6 . . ? C56 C55 H55 119.6 . . ? C51 C56 C55 120.1(3) . . ? C51 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? ####################### data_6 _database_code_depnum_ccdc_archive 'CCDC 255523' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [8-(3'-Ac-(D,L)-alanyloxy)-2'-hydroxyphenyl)-(5,6)-benzo -4,7-diazaocta-2,7-dien-1-onato(2-)]nickel(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H25 N3 Ni O5' _chemical_formula_sum 'C28 H25 N3 Ni O5' _chemical_formula_weight 542.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.2759(3) _cell_length_b 8.43810(10) _cell_length_c 25.9355(3) _cell_angle_alpha 90 _cell_angle_beta 96.4760(10) _cell_angle_gamma 90 _cell_volume 5061.34(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7182 _cell_measurement_theta_min 3.82 _cell_measurement_theta_max 65.61 _exptl_crystal_description ? _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 1.475 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_probe ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w _diffrn_detector_type CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_measured_fraction_theta_max 0.902 _diffrn_measured_fraction_theta_full 0.902 _diffrn_reflns_number 10263 _diffrn_reflns_av_R_equivalents 0.0089 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 65.06 _diffrn_reflns_theta_full 65.06 _reflns_number_total 3895 _reflns_number_gt 3611 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+2.1850P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3895 _refine_ls_number_parameters 365 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.218 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.038 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 Ni Ni 0.071654(12) 0.76269(4) -0.002356(11) 0.04919(14) Uani 1 1 d . . . O1 O 0.13194(5) 0.83989(18) 0.04309(5) 0.0550(3) Uani 1 1 d . . . O2 O 0.02944(6) 0.79711(19) 0.05247(5) 0.0584(4) Uani 1 1 d . . . O3 O 0.19771(5) 0.99506(15) 0.11776(5) 0.0508(3) Uani 1 1 d . . . O4 O 0.23516(7) 0.75481(16) 0.13926(6) 0.0620(4) Uani 1 1 d . . . O5 O 0.27893(7) 1.01581(17) 0.22649(6) 0.0655(4) Uani 1 1 d . . . N1 N 0.11508(7) 0.74259(18) -0.05748(6) 0.0484(4) Uani 1 1 d . . . N2 N 0.01020(7) 0.6835(2) -0.04778(6) 0.0531(4) Uani 1 1 d . . . N3 N 0.21182(7) 0.8370(2) 0.24233(6) 0.0551(4) Uani 1 1 d . . . H30 H 0.2063(10) 0.745(2) 0.2563(8) 0.051(6) Uiso 1 1 d . . . C1 C 0.08711(8) 0.6519(2) -0.09888(7) 0.0523(4) Uani 1 1 d . . . C2 C 0.11222(10) 0.5989(3) -0.14194(8) 0.0611(5) Uani 1 1 d . . . H2 H 0.1501 0.6261 -0.1461 0.079(7) Uiso 1 1 calc R . . C3 C 0.08049(11) 0.5059(3) -0.17835(9) 0.0733(6) Uani 1 1 d . . . H3 H 0.0964 0.4736 -0.2079 0.081(8) Uiso 1 1 calc R . . C4 C 0.02509(11) 0.4607(3) -0.17101(9) 0.0755(6) Uani 1 1 d . . . H4A H 0.0045 0.3947 -0.1952 0.088(8) Uiso 1 1 calc R . . C5 C -0.00016(10) 0.5118(3) -0.12840(9) 0.0679(6) Uani 1 1 d . . . H5 H -0.0372 0.4778 -0.1235 0.072(7) Uiso 1 1 calc R . . C6 C 0.02964(8) 0.6144(2) -0.09269(7) 0.0544(5) Uani 1 1 d . . . C7 C 0.17919(7) 0.9018(2) 0.03002(7) 0.0468(4) Uani 1 1 d . . . C8 C 0.21636(8) 0.9829(2) 0.06789(7) 0.0487(4) Uani 1 1 d . . . C9 C 0.26577(8) 1.0556(3) 0.05786(8) 0.0580(5) Uani 1 1 d . . . H9 H 0.2881 1.1107 0.0840 0.064(6) Uiso 1 1 calc R . . C10 C 0.28308(9) 1.0475(3) 0.00804(8) 0.0629(5) Uani 1 1 d . . . H10 H 0.3172 1.0962 0.0009 0.094(8) Uiso 1 1 calc R . . C11 C 0.24982(8) 0.9680(2) -0.02987(7) 0.0549(5) Uani 1 1 d . . . H11 H 0.2617 0.9620 -0.0629 0.065(6) Uiso 1 1 calc R . . C12 C 0.19756(7) 0.8945(2) -0.02036(7) 0.0474(4) Uani 1 1 d . . . C13 C 0.16555(8) 0.8083(2) -0.06070(7) 0.0495(4) Uani 1 1 d . . . H13 H 0.1815 0.7974 -0.0918 0.050(5) Uiso 1 1 calc R . . C14 C -0.02624(8) 0.8132(3) 0.04757(8) 0.0551(5) Uani 1 1 d . . . C15 C -0.06174(9) 0.7798(3) 0.00287(9) 0.0630(6) Uani 1 1 d . . . H15 H -0.1008 0.8025 0.0031 0.076(7) Uiso 1 1 calc R . . C16 C -0.04523(9) 0.7154(3) -0.04276(9) 0.0606(5) Uani 1 1 d . . . C17 C -0.09355(10) 0.6920(4) -0.08566(10) 0.0870(8) Uani 1 1 d . . . H17A H -0.0800 0.7164 -0.1184 0.079(8) Uiso 1 1 calc R . . H17B H -0.1252 0.7608 -0.0802 0.109(11) Uiso 1 1 calc R . . H17C H -0.1063 0.5838 -0.0858 0.094(9) Uiso 1 1 calc R . . C21 C -0.04960(9) 0.8764(3) 0.09438(8) 0.0582(5) Uani 1 1 d . . . C22 C -0.10560(10) 0.8442(3) 0.10495(10) 0.0764(7) Uani 1 1 d . . . H22 H -0.1294 0.7810 0.0822 0.143(15) Uiso 1 1 calc R . . C23 C -0.12626(13) 0.9041(4) 0.14830(12) 0.0946(9) Uani 1 1 d . . . H23 H -0.1637 0.8804 0.1551 0.120(11) Uiso 1 1 calc R . . C24 C -0.09218(16) 0.9980(4) 0.18148(12) 0.0963(10) Uani 1 1 d . . . H24 H -0.1066 1.0398 0.2106 0.124(11) Uiso 1 1 calc R . . C25 C -0.03575(14) 1.0324(4) 0.17222(11) 0.0880(8) Uani 1 1 d . . . H25 H -0.0123 1.0956 0.1952 0.062(6) Uiso 1 1 calc R . . C26 C -0.01506(11) 0.9711(3) 0.12840(9) 0.0686(6) Uani 1 1 d . . . H26 H 0.0225 0.9940 0.1218 0.064(6) Uiso 1 1 calc R . . C30 C 0.20679(8) 0.8671(2) 0.14868(7) 0.0476(4) Uani 1 1 d . . . C31 C 0.17465(8) 0.8830(2) 0.19599(7) 0.0522(4) Uani 1 1 d . . . H31 H 0.1629 0.9937 0.1994 0.056(5) Uiso 1 1 calc R . . C32 C 0.12110(10) 0.7791(3) 0.18875(10) 0.0698(6) Uani 1 1 d . . . H32A H 0.1324 0.6699 0.1876 0.084(8) Uiso 1 1 calc R . . H32B H 0.0983 0.8066 0.1568 0.083(8) Uiso 1 1 calc R . . H32C H 0.0987 0.7952 0.2172 0.116(11) Uiso 1 1 calc R . . C33 C 0.26298(9) 0.9090(2) 0.25378(8) 0.0573(5) Uani 1 1 d . . . C34 C 0.29850(14) 0.8552(3) 0.30234(10) 0.0859(8) Uani 1 1 d . . . H34A H 0.3371 0.8325 0.2949 0.116(12) Uiso 1 1 calc R . . H34B H 0.2816 0.7613 0.3152 0.093(9) Uiso 1 1 calc R . . H34C H 0.2995 0.9373 0.3281 0.137(13) Uiso 1 1 calc R . . 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 Ni 0.0348(2) 0.0663(2) 0.0462(2) 0.00671(13) 0.00317(14) -0.00161(12) O1 0.0375(7) 0.0814(10) 0.0467(7) 0.0029(6) 0.0069(5) -0.0057(6) O2 0.0355(8) 0.0856(10) 0.0547(8) 0.0080(7) 0.0075(6) -0.0025(6) O3 0.0496(8) 0.0581(8) 0.0446(7) 0.0006(6) 0.0048(5) 0.0034(5) O4 0.0695(10) 0.0621(9) 0.0565(8) 0.0017(6) 0.0157(7) 0.0154(7) O5 0.0708(10) 0.0570(8) 0.0668(9) -0.0001(7) -0.0004(7) -0.0082(7) N1 0.0403(9) 0.0580(9) 0.0460(8) 0.0046(7) 0.0013(7) 0.0016(6) N2 0.0397(9) 0.0650(10) 0.0534(9) 0.0111(8) -0.0002(7) -0.0025(7) N3 0.0622(11) 0.0558(10) 0.0469(9) 0.0030(8) 0.0044(7) -0.0027(8) C1 0.0487(11) 0.0563(11) 0.0500(10) 0.0053(9) -0.0025(8) 0.0013(8) C2 0.0583(13) 0.0694(13) 0.0548(11) -0.0012(10) 0.0030(9) 0.0028(10) C3 0.0841(18) 0.0751(15) 0.0591(13) -0.0087(11) 0.0013(12) 0.0030(12) C4 0.0809(17) 0.0749(15) 0.0670(14) -0.0092(12) -0.0081(12) -0.0129(12) C5 0.0610(14) 0.0698(14) 0.0694(14) 0.0036(11) -0.0082(11) -0.0126(10) C6 0.0500(11) 0.0588(11) 0.0525(10) 0.0104(9) -0.0021(8) -0.0012(8) C7 0.0372(9) 0.0561(10) 0.0466(9) 0.0065(8) 0.0028(7) 0.0039(7) C8 0.0451(10) 0.0553(11) 0.0454(9) 0.0047(8) 0.0040(8) 0.0035(8) C9 0.0504(12) 0.0638(12) 0.0588(11) 0.0016(10) 0.0019(9) -0.0095(9) C10 0.0510(13) 0.0728(14) 0.0662(13) 0.0066(11) 0.0112(10) -0.0162(10) C11 0.0478(11) 0.0665(12) 0.0515(11) 0.0084(9) 0.0110(8) -0.0034(9) C12 0.0383(10) 0.0575(11) 0.0465(9) 0.0070(8) 0.0047(7) 0.0027(7) C13 0.0418(10) 0.0620(11) 0.0454(10) 0.0066(9) 0.0073(8) 0.0045(8) C14 0.0397(11) 0.0641(12) 0.0624(12) 0.0167(10) 0.0098(9) -0.0005(8) C15 0.0339(11) 0.0831(15) 0.0718(15) 0.0151(11) 0.0048(10) -0.0003(9) C16 0.0412(12) 0.0753(14) 0.0634(13) 0.0147(10) -0.0022(9) -0.0059(9) C17 0.0481(14) 0.131(3) 0.0782(17) 0.0017(16) -0.0105(12) 0.0006(15) C21 0.0468(11) 0.0672(13) 0.0620(12) 0.0185(10) 0.0119(9) 0.0056(9) C22 0.0538(14) 0.0972(18) 0.0823(16) 0.0232(14) 0.0259(12) 0.0042(12) C23 0.0755(19) 0.123(3) 0.092(2) 0.0287(19) 0.0384(16) 0.0181(17) C24 0.109(2) 0.106(2) 0.0825(19) 0.0249(17) 0.0490(18) 0.0368(18) C25 0.107(2) 0.0882(18) 0.0701(15) 0.0028(14) 0.0140(15) 0.0131(16) C26 0.0630(15) 0.0740(15) 0.0706(14) 0.0137(12) 0.0153(11) 0.0089(11) C30 0.0417(10) 0.0534(11) 0.0471(10) -0.0013(8) 0.0020(8) -0.0010(8) C31 0.0504(11) 0.0559(11) 0.0509(10) 0.0006(9) 0.0083(8) 0.0044(8) C32 0.0513(13) 0.0812(16) 0.0767(16) 0.0040(12) 0.0066(12) -0.0037(10) C33 0.0687(13) 0.0506(11) 0.0506(10) -0.0053(9) -0.0018(10) 0.0017(9) C34 0.099(2) 0.0764(17) 0.0739(16) 0.0064(14) -0.0261(14) -0.0100(14) _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 Ni O2 1.8404(14) . ? Ni O1 1.8465(13) . ? Ni N1 1.8494(16) . ? Ni N2 1.8708(16) . ? O1 C7 1.297(2) . ? O2 C14 1.295(2) . ? O3 C30 1.348(2) . ? O3 C8 1.414(2) . ? O4 C30 1.195(2) . ? O5 C33 1.229(2) . ? N1 C13 1.310(2) . ? N1 C1 1.416(2) . ? N2 C16 1.339(3) . ? N2 C6 1.421(3) . ? N3 C33 1.340(3) . ? N3 C31 1.452(2) . ? N3 H30 0.87(2) . ? C1 C2 1.391(3) . ? C1 C6 1.401(3) . ? C2 C3 1.377(3) . ? C2 H2 0.9300 . ? C3 C4 1.378(4) . ? C3 H3 0.9300 . ? C4 C5 1.378(3) . ? C4 H4A 0.9300 . ? C5 C6 1.394(3) . ? C5 H5 0.9300 . ? C7 C8 1.411(3) . ? C7 C12 1.421(2) . ? C8 C9 1.354(3) . ? C9 C10 1.398(3) . ? C9 H9 0.9300 . ? C10 C11 1.358(3) . ? C10 H10 0.9300 . ? C11 C12 1.412(3) . ? C11 H11 0.9300 . ? C12 C13 1.415(3) . ? C13 H13 0.9300 . ? C14 C15 1.375(3) . ? C14 C21 1.485(3) . ? C15 C16 1.395(3) . ? C15 H15 0.9300 . ? C16 C17 1.503(3) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C21 C26 1.380(3) . ? C21 C22 1.389(3) . ? C22 C23 1.369(4) . ? C22 H22 0.9300 . ? C23 C24 1.358(5) . ? C23 H23 0.9300 . ? C24 C25 1.392(4) . ? C24 H24 0.9300 . ? C25 C26 1.384(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C30 C31 1.513(2) . ? C31 C32 1.518(3) . ? C31 H31 0.9800 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.497(3) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? 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 O2 Ni O1 83.38(6) . . ? O2 Ni N1 176.15(7) . . ? O1 Ni N1 94.79(6) . . ? O2 Ni N2 96.08(7) . . ? O1 Ni N2 179.37(6) . . ? N1 Ni N2 85.76(7) . . ? C7 O1 Ni 125.52(11) . . ? C14 O2 Ni 123.80(13) . . ? C30 O3 C8 116.26(14) . . ? C13 N1 C1 121.28(17) . . ? C13 N1 Ni 125.64(14) . . ? C1 N1 Ni 113.03(13) . . ? C16 N2 C6 124.16(17) . . ? C16 N2 Ni 122.95(15) . . ? C6 N2 Ni 111.79(12) . . ? C33 N3 C31 119.59(18) . . ? C33 N3 H30 118.7(15) . . ? C31 N3 H30 118.7(14) . . ? C2 C1 C6 120.82(19) . . ? C2 C1 N1 125.70(18) . . ? C6 C1 N1 113.47(17) . . ? C3 C2 C1 119.5(2) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 120.1(2) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.9(2) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 120.1(2) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 118.3(2) . . ? C5 C6 N2 128.23(19) . . ? C1 C6 N2 113.42(17) . . ? O1 C7 C8 119.01(16) . . ? O1 C7 C12 125.10(16) . . ? C8 C7 C12 115.89(17) . . ? C9 C8 C7 123.61(17) . . ? C9 C8 O3 119.85(17) . . ? C7 C8 O3 116.41(16) . . ? C8 C9 C10 119.65(19) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 119.56(18) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 121.51(18) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C11 C12 C13 119.28(16) . . ? C11 C12 C7 119.73(17) . . ? C13 C12 C7 120.93(16) . . ? N1 C13 C12 124.85(17) . . ? N1 C13 H13 117.6 . . ? C12 C13 H13 117.6 . . ? O2 C14 C15 124.1(2) . . ? O2 C14 C21 114.34(18) . . ? C15 C14 C21 121.50(18) . . ? C14 C15 C16 126.7(2) . . ? C14 C15 H15 116.6 . . ? C16 C15 H15 116.6 . . ? N2 C16 C15 121.4(2) . . ? N2 C16 C17 123.4(2) . . ? C15 C16 C17 115.1(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C26 C21 C22 118.7(2) . . ? C26 C21 C14 119.36(19) . . ? C22 C21 C14 122.0(2) . . ? C23 C22 C21 121.0(3) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C24 C23 C22 120.1(3) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.5(3) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 119.1(3) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C21 C26 C25 120.7(2) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? O4 C30 O3 124.51(17) . . ? O4 C30 C31 124.83(17) . . ? O3 C30 C31 110.64(15) . . ? N3 C31 C30 110.14(15) . . ? N3 C31 C32 110.62(17) . . ? C30 C31 C32 108.80(17) . . ? N3 C31 H31 109.1 . . ? C30 C31 H31 109.1 . . ? C32 C31 H31 109.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O5 C33 N3 121.57(19) . . ? O5 C33 C34 122.2(2) . . ? N3 C33 C34 116.2(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? ################### data_5 _database_code_depnum_ccdc_archive 'CCDC 255524' _audit_creation_method SHELXL-97 _chemical_name_systematic ;[8-(3'-Boc-(L)-phenylalanyloxy-2'-hydroxyphenyl)-(5,6) -benzo-3-methyl-1-phenyl-4,7-diazaocta-2,7-dien-1 -onato(2-)]nickel(II) dihydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H35 N3 Ni O6, 2(H2 O)' _chemical_formula_sum 'C37 H39 N3 Ni O8' _chemical_formula_weight 712.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M P21 _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 21.8152(3) _cell_length_b 7.57810(10) _cell_length_c 22.9560(4) _cell_angle_alpha 90 _cell_angle_beta 114.2092(7) _cell_angle_gamma 90 _cell_volume 3461.28(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9776 _cell_measurement_theta_min 3.64 _cell_measurement_theta_max 64.81 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 1.278 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_probe ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w _diffrn_detector_type CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measured_fraction_theta_full 0.976 _diffrn_reflns_theta_full 65.83 _diffrn_reflns_number 29857 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 65.83 _reflns_number_total 10952 _reflns_number_gt 8527 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+0.1116P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 10952 _refine_ls_number_parameters 891 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.351 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.038 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 Ni Ni 0.87274(3) 0.71981(8) 0.88595(3) 0.06288(19) Uani 1 1 d . . . O1 O 0.78956(12) 0.6236(4) 0.87084(11) 0.0645(7) Uani 1 1 d . . . O2 O 0.87163(12) 0.7844(4) 0.96308(11) 0.0707(8) Uani 1 1 d . . . O3 O 0.67627(11) 0.4863(4) 0.87191(11) 0.0616(7) Uani 1 1 d . . . O4 O 0.75244(13) 0.2751(4) 0.92155(12) 0.0725(7) Uani 1 1 d . . . O5 O 0.60265(14) 0.1995(4) 0.93148(16) 0.0880(9) Uani 1 1 d . . . O6 O 0.52580(12) 0.4098(4) 0.92455(13) 0.0749(8) Uani 1 1 d . . . O7 O 0.6286(3) 0.8444(6) 0.9577(3) 0.185(2) Uani 1 1 d . . . H71 H 0.6575 0.8665 0.9445 0.222 Uiso 1 1 d . . . H72 H 0.6001 0.9202 0.9415 0.222 Uiso 1 1 d . . . O8 O 0.71820(14) 0.8986(5) 0.90367(14) 0.0844(9) Uani 1 1 d . . . H81 H 0.7394 0.9883 0.9189 0.101 Uiso 1 1 d . . . H82 H 0.7457 0.8212 0.9067 0.101 Uiso 1 1 d . . . N1 N 0.86863(14) 0.6709(4) 0.80668(15) 0.0605(8) Uani 1 1 d . . . N2 N 0.96011(15) 0.7987(5) 0.90619(15) 0.0669(8) Uani 1 1 d . . . N3 N 0.63307(15) 0.4775(5) 0.96671(14) 0.0615(8) Uani 1 1 d . . . H30 H 0.6201 0.5779 0.9750 0.074 Uiso 1 1 calc R . . C1 C 0.92479(19) 0.7428(6) 0.7963(2) 0.0678(11) Uani 1 1 d . . . C2 C 0.9299(2) 0.7499(7) 0.7380(2) 0.0841(14) Uani 1 1 d . . . H2 H 0.8975 0.6968 0.7020 0.101 Uiso 1 1 calc R . . C3 C 0.9836(2) 0.8364(9) 0.7340(2) 0.0984(17) Uani 1 1 d . . . H3 H 0.9889 0.8373 0.6958 0.118 Uiso 1 1 calc R . . C4 C 1.0294(3) 0.9214(9) 0.7868(3) 0.1062(18) Uani 1 1 d . . . H4 H 1.0644 0.9843 0.7833 0.127 Uiso 1 1 calc R . . C5 C 1.0246(2) 0.9152(7) 0.8453(3) 0.0905(15) Uani 1 1 d . . . H5 H 1.0553 0.9763 0.8802 0.109 Uiso 1 1 calc R . . C6 C 0.97316(19) 0.8162(6) 0.8516(2) 0.0711(11) Uani 1 1 d . . . C7 C 0.74843(18) 0.5468(6) 0.81845(17) 0.0590(10) Uani 1 1 d . . . C8 C 0.68844(17) 0.4697(6) 0.81733(17) 0.0582(9) Uani 1 1 d . . . C9 C 0.64178(18) 0.3906(6) 0.76408(18) 0.0662(11) Uani 1 1 d . . . H9 H 0.6033 0.3414 0.7654 0.079 Uiso 1 1 calc R . . C10 C 0.6515(2) 0.3833(6) 0.70744(19) 0.0699(11) Uani 1 1 d . . . H10 H 0.6195 0.3317 0.6708 0.084 Uiso 1 1 calc R . . C11 C 0.7088(2) 0.4534(6) 0.70729(19) 0.0680(11) Uani 1 1 d . . . H11 H 0.7153 0.4487 0.6697 0.082 Uiso 1 1 calc R . . C12 C 0.75913(18) 0.5332(5) 0.76181(18) 0.0611(10) Uani 1 1 d . . . C13 C 0.8193(2) 0.5998(6) 0.75885(19) 0.0637(11) Uani 1 1 d . . . H13 H 0.8232 0.5915 0.7201 0.076 Uiso 1 1 calc R . . C14 C 0.9235(2) 0.8225(6) 1.0150(2) 0.0707(11) Uani 1 1 d . . . C15 C 0.9877(2) 0.8256(7) 1.0179(2) 0.0747(11) Uani 1 1 d . . . H15 H 1.0226 0.8359 1.0583 0.090 Uiso 1 1 calc R . . C16 C 1.0057(2) 0.8147(7) 0.9658(2) 0.0749(11) Uani 1 1 d . . . C17 C 1.08095(19) 0.8165(8) 0.9838(2) 0.0952(15) Uani 1 1 d . . . H17A H 1.0900 0.7627 0.9503 0.114 Uiso 1 1 calc R . . H17B H 1.1035 0.7517 1.0228 0.114 Uiso 1 1 calc R . . H17C H 1.0968 0.9361 0.9897 0.114 Uiso 1 1 calc R . . C21 C 0.9084(2) 0.8658(6) 1.0708(2) 0.0728(11) Uani 1 1 d . . . C22 C 0.9583(3) 0.8883(9) 1.1324(2) 0.1019(18) Uani 1 1 d . . . H22 H 1.0032 0.8733 1.1397 0.122 Uiso 1 1 calc R . . C23 C 0.9423(3) 0.9314(9) 1.1815(2) 0.1102(19) Uani 1 1 d . . . H23 H 0.9763 0.9448 1.2222 0.132 Uiso 1 1 calc R . . C24 C 0.8764(3) 0.9558(8) 1.1721(2) 0.1085(18) Uani 1 1 d . . . H24 H 0.8658 0.9891 1.2059 0.130 Uiso 1 1 calc R . . C25 C 0.8274(3) 0.9310(8) 1.1133(2) 0.1125(19) Uani 1 1 d . . . H25 H 0.7826 0.9442 1.1066 0.135 Uiso 1 1 calc R . . C26 C 0.8435(2) 0.8858(8) 1.0628(2) 0.0931(15) Uani 1 1 d . . . H26 H 0.8091 0.8688 1.0225 0.112 Uiso 1 1 calc R . . C30 C 0.71439(19) 0.3882(6) 0.92291(19) 0.0589(9) Uani 1 1 d . . . C31 C 0.70424(17) 0.4465(5) 0.98158(17) 0.0633(10) Uani 1 1 d . . . H31 H 0.7269 0.5607 0.9944 0.076 Uiso 1 1 calc R . . C32 C 0.5884(2) 0.3482(6) 0.9400(2) 0.0653(10) Uani 1 1 d . . . C33 C 0.4676(2) 0.2872(7) 0.89888(18) 0.0768(12) Uani 1 1 d . . . C34 C 0.4722(2) 0.1526(8) 0.9488(2) 0.1061(17) Uani 1 1 d . . . H34A H 0.5037 0.0623 0.9502 0.127 Uiso 1 1 calc R . . H34B H 0.4288 0.1007 0.9381 0.127 Uiso 1 1 calc R . . H34C H 0.4871 0.2091 0.9897 0.127 Uiso 1 1 calc R . . C35 C 0.4087(2) 0.4082(8) 0.8858(2) 0.1120(19) Uani 1 1 d . . . H35A H 0.4139 0.4674 0.9246 0.134 Uiso 1 1 calc R . . H35B H 0.3679 0.3404 0.8703 0.134 Uiso 1 1 calc R . . H35C H 0.4066 0.4939 0.8543 0.134 Uiso 1 1 calc R . . C36 C 0.4637(2) 0.2057(8) 0.83726(19) 0.0983(14) Uani 1 1 d . . . H36A H 0.4614 0.2975 0.8076 0.118 Uiso 1 1 calc R . . H36B H 0.4243 0.1331 0.8193 0.118 Uiso 1 1 calc R . . H36C H 0.5029 0.1349 0.8458 0.118 Uiso 1 1 calc R . . C40 C 0.73874(19) 0.3208(6) 1.03715(17) 0.0780(11) Uani 1 1 d . . . H40A H 0.7176 0.2057 1.0260 0.094 Uiso 1 1 calc R . . H40B H 0.7854 0.3077 1.0439 0.094 Uiso 1 1 calc R . . C41 C 0.7360(2) 0.3813(7) 1.09872(19) 0.0785(12) Uani 1 1 d . . . C42 C 0.7784(2) 0.5031(10) 1.1361(2) 0.1105(18) Uani 1 1 d . . . H42 H 0.8115 0.5493 1.1249 0.133 Uiso 1 1 calc R . . C43 C 0.7734(3) 0.5615(12) 1.1915(3) 0.137(3) Uani 1 1 d . . . H43 H 0.8017 0.6503 1.2159 0.164 Uiso 1 1 calc R . . C44 C 0.7278(3) 0.4898(10) 1.2095(2) 0.1145(19) Uani 1 1 d . . . H44 H 0.7271 0.5228 1.2482 0.137 Uiso 1 1 calc R . . C45 C 0.6841(3) 0.3734(10) 1.1733(3) 0.1095(18) Uani 1 1 d . . . H45 H 0.6508 0.3305 1.1850 0.131 Uiso 1 1 calc R . . C46 C 0.6878(2) 0.3142(8) 1.1167(2) 0.0962(14) Uani 1 1 d . . . H46 H 0.6576 0.2297 1.0914 0.115 Uiso 1 1 calc R . . Ni' Ni 0.62800(3) 0.81175(8) 0.61805(3) 0.06210(18) Uani 1 1 d . . . O1' O 0.70895(12) 0.9171(4) 0.63205(11) 0.0644(7) Uani 1 1 d . . . O2' O 0.63104(12) 0.7393(4) 0.54295(11) 0.0688(7) Uani 1 1 d . . . O3' O 0.82349(12) 1.0632(4) 0.63062(12) 0.0652(7) Uani 1 1 d . . . O4' O 0.75170(15) 1.2849(5) 0.58652(14) 0.0892(9) Uani 1 1 d . . . O5' O 0.92307(16) 1.3559(5) 0.5644(2) 0.1155(12) Uani 1 1 d . . . O6' O 0.98470(12) 1.1090(4) 0.58066(13) 0.0770(8) Uani 1 1 d . . . O7' O 0.8781(3) 0.7086(7) 0.5583(3) 0.189(2) Uani 1 1 d . . . H71' H 0.8482 0.6716 0.5677 0.227 Uiso 1 1 d . . . H72' H 0.9039 0.6246 0.5648 0.227 Uiso 1 1 d . . . O8' O 0.78447(18) 0.6512(6) 0.60379(17) 0.1082(12) Uani 1 1 d . . . H81' H 0.7828 0.5450 0.5958 0.130 Uiso 1 1 d . . . H82' H 0.7489 0.6710 0.6072 0.130 Uiso 1 1 d . . . N1' N 0.63150(15) 0.8646(5) 0.69800(15) 0.0628(9) Uani 1 1 d . . . N2' N 0.54191(15) 0.7238(5) 0.59895(15) 0.0674(9) Uani 1 1 d . . . N3' N 0.87514(16) 1.0889(5) 0.54303(15) 0.0649(9) Uani 1 1 d . . . H30' H 0.8810 0.9776 0.5400 0.078 Uiso 1 1 calc R . . C1' C 0.57595(19) 0.7937(6) 0.7080(2) 0.0677(10) Uani 1 1 d . . . C2' C 0.5704(2) 0.7932(8) 0.7666(2) 0.0809(13) Uani 1 1 d . . . H2' H 0.6014 0.8531 0.8016 0.097 Uiso 1 1 calc R . . C3' C 0.5177(2) 0.7018(8) 0.7714(3) 0.0976(16) Uani 1 1 d . . . H3' H 0.5129 0.6992 0.8098 0.117 Uiso 1 1 calc R . . C4' C 0.4732(3) 0.6161(8) 0.7196(3) 0.1014(18) Uani 1 1 d . . . H4' H 0.4382 0.5543 0.7234 0.122 Uiso 1 1 calc R . . C5' C 0.4774(2) 0.6166(7) 0.6618(3) 0.0901(15) Uani 1 1 d . . . H5' H 0.4465 0.5533 0.6277 0.108 Uiso 1 1 calc R . . C6' C 0.52831(19) 0.7125(6) 0.6544(2) 0.0714(11) Uani 1 1 d . . . C7' C 0.75108(18) 0.9935(5) 0.68456(17) 0.0592(9) Uani 1 1 d . . . C8' C 0.81031(18) 1.0741(6) 0.68627(17) 0.0600(10) Uani 1 1 d . . . C9' C 0.8582(2) 1.1458(6) 0.73960(18) 0.0699(11) Uani 1 1 d . . . H9' H 0.8974 1.1917 0.7388 0.084 Uiso 1 1 calc R . . C10' C 0.8479(2) 1.1497(6) 0.79590(19) 0.0720(12) Uani 1 1 d . . . H10' H 0.8803 1.1983 0.8329 0.086 Uiso 1 1 calc R . . C11' C 0.7904(2) 1.0825(6) 0.79643(18) 0.0649(10) Uani 1 1 d . . . H11' H 0.7835 1.0877 0.8338 0.078 Uiso 1 1 calc R . . C12' C 0.74133(18) 1.0054(6) 0.74170(16) 0.0583(10) Uani 1 1 d . . . C13' C 0.68171(19) 0.9379(6) 0.74453(18) 0.0633(10) Uani 1 1 d . . . H13' H 0.6783 0.9473 0.7835 0.076 Uiso 1 1 calc R . . C14' C 0.5797(2) 0.6905(6) 0.49193(19) 0.0671(11) Uani 1 1 d . . . C15' C 0.5155(2) 0.6813(6) 0.4884(2) 0.0771(12) Uani 1 1 d . . . H15' H 0.4814 0.6613 0.4482 0.093 Uiso 1 1 calc R . . C16' C 0.4961(2) 0.6985(6) 0.5383(2) 0.0750(12) Uani 1 1 d . . . C17' C 0.4219(2) 0.6857(8) 0.5210(2) 0.0958(15) Uani 1 1 d . . . H17D H 0.4100 0.5648 0.5234 0.115 Uiso 1 1 calc R . . H17E H 0.3975 0.7289 0.4784 0.115 Uiso 1 1 calc R . . H17F H 0.4108 0.7552 0.5503 0.115 Uiso 1 1 calc R . . C21' C 0.5956(2) 0.6375(6) 0.4375(2) 0.0709(11) Uani 1 1 d . . . C22' C 0.5471(3) 0.6426(8) 0.3745(2) 0.0897(15) Uani 1 1 d . . . H22' H 0.5044 0.6873 0.3655 0.108 Uiso 1 1 calc R . . C23' C 0.5629(3) 0.5808(10) 0.3255(3) 0.117(2) Uani 1 1 d . . . H23' H 0.5305 0.5852 0.2837 0.140 Uiso 1 1 calc R . . C24' C 0.6245(4) 0.5141(9) 0.3367(3) 0.120(2) Uani 1 1 d . . . H24' H 0.6339 0.4729 0.3031 0.144 Uiso 1 1 calc R . . C25' C 0.6725(3) 0.5081(8) 0.3979(3) 0.1142(18) Uani 1 1 d . . . H25' H 0.7147 0.4616 0.4061 0.137 Uiso 1 1 calc R . . C26' C 0.6584(2) 0.5716(7) 0.4484(2) 0.0905(14) Uani 1 1 d . . . H26' H 0.6918 0.5693 0.4898 0.109 Uiso 1 1 calc R . . C30' C 0.79157(19) 1.1807(6) 0.58395(19) 0.0637(10) Uani 1 1 d . . . C31' C 0.80805(16) 1.1575(6) 0.52635(16) 0.0622(9) Uani 1 1 d . . . H31' H 0.8062 1.2746 0.5076 0.075 Uiso 1 1 calc R . . C32' C 0.92790(19) 1.1978(7) 0.56311(19) 0.0680(10) Uani 1 1 d . . . C33' C 1.0497(2) 1.1987(9) 0.6013(2) 0.0906(15) Uani 1 1 d . . . C36' C 1.0634(3) 1.3020(11) 0.6619(2) 0.126(2) Uani 1 1 d . . . H36D H 1.0320 1.3978 0.6526 0.151 Uiso 1 1 calc R . . H36E H 1.1083 1.3480 0.6783 0.151 Uiso 1 1 calc R . . H36F H 1.0585 1.2257 0.6931 0.151 Uiso 1 1 calc R . . C35' C 1.0971(2) 1.0428(11) 0.6137(3) 0.143(3) Uani 1 1 d . . . H35D H 1.0929 0.9678 0.6456 0.171 Uiso 1 1 calc R . . H35E H 1.1425 1.0847 0.6285 0.171 Uiso 1 1 calc R . . H35F H 1.0858 0.9772 0.5749 0.171 Uiso 1 1 calc R . . C34' C 1.0506(2) 1.3116(11) 0.5477(2) 0.131(2) Uani 1 1 d . . . H34D H 1.0364 1.2426 0.5094 0.157 Uiso 1 1 calc R . . H34E H 1.0953 1.3545 0.5586 0.157 Uiso 1 1 calc R . . H34F H 1.0206 1.4096 0.5411 0.157 Uiso 1 1 calc R . . C40' C 0.75427(18) 1.0460(6) 0.47667(17) 0.0764(11) Uani 1 1 d . . . H40C H 0.7592 0.9256 0.4923 0.092 Uiso 1 1 calc R . . H40D H 0.7108 1.0881 0.4728 0.092 Uiso 1 1 calc R . . C41' C 0.75421(19) 1.0436(6) 0.41101(18) 0.0722(10) Uani 1 1 d . . . C42' C 0.7111(3) 0.9321(8) 0.3665(2) 0.1021(16) Uani 1 1 d . . . H42' H 0.6829 0.8600 0.3772 0.123 Uiso 1 1 calc R . . C43' C 0.7089(3) 0.9247(10) 0.3044(3) 0.1190(19) Uani 1 1 d . . . H43' H 0.6784 0.8497 0.2744 0.143 Uiso 1 1 calc R . . C44' C 0.7491(3) 1.0215(10) 0.2882(2) 0.1067(18) Uani 1 1 d . . . H44' H 0.7482 1.0113 0.2475 0.128 Uiso 1 1 calc R . . C45' C 0.7923(3) 1.1375(9) 0.3308(2) 0.1060(17) Uani 1 1 d . . . H45' H 0.8198 1.2093 0.3190 0.127 Uiso 1 1 calc R . . C46' C 0.7945(2) 1.1470(7) 0.3931(2) 0.0879(13) Uani 1 1 d . . . H46' H 0.8241 1.2253 0.4225 0.106 Uiso 1 1 calc R . . 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 Ni 0.0572(4) 0.0615(4) 0.0696(4) 0.0020(3) 0.0257(3) 0.0038(3) O1 0.0599(15) 0.0735(19) 0.0610(15) -0.0087(14) 0.0256(13) -0.0027(14) O2 0.0615(14) 0.081(2) 0.0652(15) -0.0031(15) 0.0211(13) 0.0004(15) O3 0.0558(14) 0.0728(18) 0.0606(15) 0.0018(14) 0.0284(13) 0.0080(14) O4 0.0678(15) 0.0733(19) 0.0811(17) 0.0046(14) 0.0352(14) 0.0129(15) O5 0.0745(17) 0.0605(19) 0.128(2) -0.0047(16) 0.0401(17) 0.0071(15) O6 0.0593(15) 0.079(2) 0.0855(18) -0.0061(16) 0.0288(14) 0.0034(15) O7 0.247(5) 0.077(3) 0.343(7) 0.039(4) 0.234(6) 0.022(3) O8 0.0783(18) 0.079(2) 0.093(2) -0.0073(17) 0.0324(16) 0.0095(16) N1 0.0495(16) 0.051(2) 0.074(2) 0.0039(16) 0.0176(16) 0.0086(15) N2 0.0643(18) 0.057(2) 0.080(2) 0.0027(19) 0.0307(18) 0.0070(17) N3 0.0620(18) 0.0595(19) 0.0716(19) -0.0015(15) 0.0361(16) 0.0044(15) C1 0.062(2) 0.067(3) 0.081(3) 0.016(2) 0.035(2) 0.013(2) C2 0.078(3) 0.088(4) 0.098(3) 0.015(3) 0.048(3) 0.013(3) C3 0.086(3) 0.118(5) 0.106(4) 0.023(4) 0.054(3) 0.005(4) C4 0.086(4) 0.115(5) 0.130(5) 0.020(4) 0.058(4) -0.004(4) C5 0.070(3) 0.085(4) 0.119(4) 0.009(3) 0.041(3) -0.013(3) C6 0.061(2) 0.059(3) 0.092(3) 0.008(2) 0.031(2) 0.009(2) C7 0.060(2) 0.060(2) 0.062(2) 0.009(2) 0.029(2) 0.013(2) C8 0.052(2) 0.058(2) 0.062(2) 0.0035(19) 0.0203(19) 0.0099(19) C9 0.056(2) 0.064(3) 0.079(3) 0.005(2) 0.029(2) 0.006(2) C10 0.066(3) 0.068(3) 0.067(3) -0.009(2) 0.019(2) 0.001(2) C11 0.079(3) 0.067(3) 0.065(2) 0.004(2) 0.035(2) 0.015(2) C12 0.063(2) 0.055(2) 0.062(2) 0.003(2) 0.022(2) 0.011(2) C13 0.074(3) 0.056(2) 0.075(3) 0.011(2) 0.045(2) 0.014(2) C14 0.075(3) 0.054(2) 0.077(3) 0.000(2) 0.024(2) 0.003(2) C15 0.067(2) 0.069(3) 0.073(3) -0.006(2) 0.013(2) 0.007(2) C16 0.066(2) 0.059(3) 0.092(3) -0.001(2) 0.024(2) 0.003(2) C17 0.058(2) 0.098(4) 0.110(3) -0.014(3) 0.015(2) 0.002(3) C21 0.090(3) 0.056(2) 0.072(3) 0.0026(19) 0.033(2) 0.001(2) C22 0.100(4) 0.115(5) 0.077(3) -0.013(3) 0.023(3) -0.034(4) C23 0.142(5) 0.118(5) 0.067(3) -0.012(3) 0.039(4) -0.033(4) C24 0.157(5) 0.097(4) 0.083(3) -0.003(3) 0.060(4) -0.001(4) C25 0.113(4) 0.139(5) 0.085(3) 0.012(3) 0.039(3) 0.030(4) C26 0.094(3) 0.114(4) 0.064(2) 0.006(3) 0.025(2) 0.016(3) C30 0.051(2) 0.053(2) 0.075(2) -0.0001(18) 0.0280(19) -0.0048(18) C31 0.058(2) 0.065(3) 0.070(2) -0.0006(18) 0.0298(19) -0.0005(18) C32 0.063(2) 0.063(3) 0.076(2) 0.004(2) 0.035(2) 0.009(2) C33 0.064(2) 0.093(3) 0.068(2) 0.003(2) 0.022(2) -0.003(2) C34 0.094(3) 0.131(5) 0.096(3) 0.018(3) 0.040(3) -0.023(3) C35 0.066(3) 0.134(5) 0.119(4) -0.023(4) 0.021(3) 0.006(3) C36 0.107(3) 0.105(4) 0.080(3) -0.007(3) 0.036(3) -0.009(3) C40 0.071(2) 0.086(3) 0.077(2) 0.010(2) 0.031(2) 0.018(2) C41 0.064(2) 0.102(3) 0.068(2) 0.018(2) 0.026(2) 0.016(2) C42 0.086(3) 0.165(6) 0.073(3) -0.006(4) 0.024(3) -0.026(4) C43 0.127(5) 0.191(8) 0.082(4) -0.024(4) 0.032(3) -0.048(5) C44 0.148(5) 0.126(5) 0.073(3) 0.001(3) 0.049(4) 0.012(5) C45 0.119(4) 0.125(5) 0.103(4) 0.023(4) 0.066(4) 0.015(4) C46 0.103(3) 0.105(4) 0.087(3) 0.007(3) 0.045(3) -0.008(3) Ni' 0.0584(4) 0.0607(4) 0.0661(4) 0.0020(3) 0.0244(3) 0.0044(3) O1' 0.0647(15) 0.0736(18) 0.0547(14) -0.0020(14) 0.0244(13) 0.0019(15) O2' 0.0669(15) 0.072(2) 0.0637(15) -0.0041(14) 0.0229(13) -0.0009(14) O3' 0.0659(16) 0.0673(18) 0.0665(16) 0.0031(14) 0.0314(14) 0.0090(14) O4' 0.106(2) 0.085(2) 0.091(2) 0.0170(17) 0.0552(18) 0.035(2) O5' 0.079(2) 0.071(2) 0.183(4) -0.007(2) 0.040(2) 0.0001(17) O6' 0.0544(15) 0.086(2) 0.0857(19) -0.0002(16) 0.0241(14) 0.0036(14) O7' 0.261(6) 0.093(3) 0.312(6) 0.042(4) 0.218(5) 0.055(4) O8' 0.113(3) 0.105(3) 0.116(3) -0.012(2) 0.056(2) 0.000(2) N1' 0.0613(18) 0.062(2) 0.069(2) 0.0126(17) 0.0307(17) 0.0077(17) N2' 0.0638(19) 0.057(2) 0.084(2) 0.0016(18) 0.0322(18) 0.0038(17) N3' 0.0618(19) 0.063(2) 0.073(2) -0.0028(16) 0.0306(17) 0.0065(16) C1' 0.061(2) 0.060(3) 0.089(3) 0.011(2) 0.037(2) 0.010(2) C2' 0.075(3) 0.090(3) 0.089(3) 0.015(3) 0.045(2) 0.012(3) C3' 0.097(3) 0.103(4) 0.112(4) 0.030(4) 0.063(3) 0.013(4) C4' 0.084(3) 0.092(4) 0.151(5) 0.026(4) 0.071(4) 0.002(3) C5' 0.075(3) 0.080(3) 0.126(4) 0.009(3) 0.051(3) 0.004(3) C6' 0.067(2) 0.062(3) 0.092(3) 0.008(3) 0.039(2) 0.007(2) C7' 0.059(2) 0.053(2) 0.065(2) 0.001(2) 0.024(2) 0.011(2) C8' 0.060(2) 0.065(3) 0.057(2) -0.0033(19) 0.025(2) 0.008(2) C9' 0.063(2) 0.071(3) 0.069(2) -0.004(2) 0.020(2) 0.003(2) C10' 0.072(3) 0.074(3) 0.060(3) -0.001(2) 0.016(2) 0.009(2) C11' 0.074(3) 0.060(3) 0.059(2) 0.0000(19) 0.027(2) 0.008(2) C12' 0.063(2) 0.057(2) 0.056(2) 0.0059(19) 0.025(2) 0.009(2) C13' 0.068(3) 0.061(3) 0.063(2) 0.003(2) 0.028(2) 0.011(2) C14' 0.071(3) 0.051(2) 0.066(2) -0.0005(19) 0.015(2) 0.000(2) C15' 0.068(3) 0.067(3) 0.086(3) -0.005(2) 0.021(2) 0.001(2) C16' 0.063(2) 0.054(3) 0.100(3) -0.012(2) 0.025(2) -0.002(2) C17' 0.065(3) 0.091(4) 0.126(4) -0.018(3) 0.034(3) -0.001(3) C21' 0.078(3) 0.060(2) 0.069(2) -0.0014(19) 0.025(2) -0.011(2) C22' 0.096(3) 0.093(4) 0.067(3) -0.005(2) 0.020(3) -0.021(3) C23' 0.127(5) 0.137(6) 0.072(3) -0.017(3) 0.028(4) -0.063(5) C24' 0.173(6) 0.118(5) 0.088(4) -0.032(3) 0.072(4) -0.059(5) C25' 0.150(5) 0.114(4) 0.105(4) -0.004(3) 0.079(4) 0.015(4) C26' 0.104(3) 0.092(4) 0.078(3) 0.000(2) 0.041(3) 0.010(3) C30' 0.062(2) 0.061(3) 0.069(2) -0.001(2) 0.028(2) 0.005(2) C31' 0.056(2) 0.068(3) 0.064(2) 0.0006(18) 0.0269(18) -0.0006(18) C32' 0.061(2) 0.069(3) 0.075(3) 0.000(2) 0.028(2) 0.002(2) C33' 0.059(2) 0.123(4) 0.085(3) 0.001(3) 0.025(2) -0.012(3) C36' 0.107(4) 0.166(6) 0.088(3) -0.031(4) 0.023(3) -0.033(4) C35' 0.073(3) 0.167(7) 0.172(6) -0.006(5) 0.035(4) 0.028(4) C34' 0.100(4) 0.181(7) 0.115(4) 0.026(4) 0.046(3) -0.035(4) C40' 0.060(2) 0.096(3) 0.070(2) -0.005(2) 0.025(2) -0.005(2) C41' 0.064(2) 0.081(3) 0.069(2) 0.007(2) 0.025(2) 0.003(2) C42' 0.098(3) 0.114(4) 0.084(3) -0.013(3) 0.027(3) -0.016(3) C43' 0.119(4) 0.130(5) 0.085(4) -0.017(3) 0.019(3) -0.025(4) C44' 0.109(4) 0.118(5) 0.074(3) -0.005(3) 0.018(3) -0.007(4) C45' 0.107(4) 0.124(5) 0.090(3) 0.012(3) 0.043(3) -0.007(4) C46' 0.091(3) 0.094(3) 0.078(3) -0.004(2) 0.034(2) -0.009(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 Ni N1 1.823(3) . ? Ni O2 1.847(2) . ? Ni O1 1.852(2) . ? Ni N2 1.865(3) . ? O1 C7 1.306(4) . ? O2 C14 1.295(4) . ? O3 C30 1.348(5) . ? O3 C8 1.389(4) . ? O4 C30 1.202(4) . ? O5 C32 1.206(5) . ? O6 C32 1.346(4) . ? O6 C33 1.486(5) . ? O7 H71 0.8225 . ? O7 H72 0.8153 . ? O8 H81 0.8164 . ? O8 H82 0.8218 . ? N1 C13 1.298(5) . ? N1 C1 1.447(5) . ? N2 C16 1.327(5) . ? N2 C6 1.401(5) . ? N3 C32 1.340(5) . ? N3 C31 1.465(4) . ? N3 H30 0.8600 . ? C1 C2 1.390(5) . ? C1 C6 1.391(6) . ? C2 C3 1.378(6) . ? C2 H2 0.9300 . ? C3 C4 1.374(7) . ? C3 H3 0.9300 . ? C4 C5 1.390(7) . ? C4 H4 0.9300 . ? C5 C6 1.406(6) . ? C5 H5 0.9300 . ? C7 C12 1.416(5) . ? C7 C8 1.424(5) . ? C8 C9 1.367(5) . ? C9 C10 1.402(5) . ? C9 H9 0.9300 . ? C10 C11 1.360(6) . ? C10 H10 0.9300 . ? C11 C12 1.418(5) . ? C11 H11 0.9300 . ? C12 C13 1.433(5) . ? C13 H13 0.9300 . ? C14 C15 1.375(6) . ? C14 C21 1.486(6) . ? C15 C16 1.405(5) . ? C15 H15 0.9300 . ? C16 C17 1.520(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C21 C26 1.360(6) . ? C21 C22 1.396(6) . ? C22 C23 1.350(7) . ? C22 H22 0.9300 . ? C23 C24 1.376(7) . ? C23 H23 0.9300 . ? C24 C25 1.348(7) . ? C24 H24 0.9300 . ? C25 C26 1.385(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C30 C31 1.518(5) . ? C31 C40 1.521(5) . ? C31 H31 0.9800 . ? C33 C34 1.505(6) . ? C33 C35 1.506(6) . ? C33 C36 1.513(6) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C40 C41 1.510(5) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.339(7) . ? C41 C46 1.375(6) . ? C42 C43 1.391(7) . ? C42 H42 0.9300 . ? C43 C44 1.339(8) . ? C43 H43 0.9300 . ? C44 C45 1.315(8) . ? C44 H44 0.9300 . ? C45 C46 1.408(7) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? Ni' O2' 1.836(2) . ? Ni' O1' 1.842(3) . ? Ni' N1' 1.849(3) . ? Ni' N2' 1.868(3) . ? O1' C7' 1.313(4) . ? O2' C14' 1.299(4) . ? O3' C30' 1.346(5) . ? O3' C8' 1.422(4) . ? O4' C30' 1.194(5) . ? O5' C32' 1.204(6) . ? O6' C32' 1.320(5) . ? O6' C33' 1.465(5) . ? O7' H71' 0.8172 . ? O7' H72' 0.8214 . ? O8' H81' 0.8236 . ? O8' H82' 0.8252 . ? N1' C13' 1.300(5) . ? N1' C1' 1.428(5) . ? N2' C16' 1.354(5) . ? N2' C6' 1.422(5) . ? N3' C32' 1.335(5) . ? N3' C31' 1.449(4) . ? N3' H30' 0.8600 . ? C1' C6' 1.387(6) . ? C1' C2' 1.400(5) . ? C2' C3' 1.384(6) . ? C2' H2' 0.9300 . ? C3' C4' 1.354(7) . ? C3' H3' 0.9300 . ? C4' C5' 1.365(7) . ? C4' H4' 0.9300 . ? C5' C6' 1.396(6) . ? C5' H5' 0.9300 . ? C7' C8' 1.415(5) . ? C7' C12' 1.415(5) . ? C8' C9' 1.356(5) . ? C9' C10' 1.401(5) . ? C9' H9' 0.9300 . ? C10' C11' 1.358(5) . ? C10' H10' 0.9300 . ? C11' C12' 1.401(5) . ? C11' H11' 0.9300 . ? C12' C13' 1.423(5) . ? C13' H13' 0.9300 . ? C14' C15' 1.371(5) . ? C14' C21' 1.482(5) . ? C15' C16' 1.379(5) . ? C15' H15' 0.9300 . ? C16' C17' 1.504(5) . ? C17' H17D 0.9600 . ? C17' H17E 0.9600 . ? C17' H17F 0.9600 . ? C21' C26' 1.382(6) . ? C21' C22' 1.401(5) . ? C22' C23' 1.387(7) . ? C22' H22' 0.9300 . ? C23' C24' 1.357(8) . ? C23' H23' 0.9300 . ? C24' C25' 1.365(7) . ? C24' H24' 0.9300 . ? C25' C26' 1.400(6) . ? C25' H25' 0.9300 . ? C26' H26' 0.9300 . ? C30' C31' 1.516(5) . ? C31' C40' 1.514(5) . ? C31' H31' 0.9800 . ? C33' C34' 1.505(7) . ? C33' C36' 1.514(7) . ? C33' C35' 1.518(8) . ? C36' H36D 0.9600 . ? C36' H36E 0.9600 . ? C36' H36F 0.9600 . ? C35' H35D 0.9600 . ? C35' H35E 0.9600 . ? C35' H35F 0.9600 . ? C34' H34D 0.9600 . ? C34' H34E 0.9600 . ? C34' H34F 0.9600 . ? C40' C41' 1.507(5) . ? C40' H40C 0.9700 . ? C40' H40D 0.9700 . ? C41' C46' 1.360(6) . ? C41' C42' 1.362(6) . ? C42' C43' 1.408(7) . ? C42' H42' 0.9300 . ? C43' C44' 1.308(8) . ? C43' H43' 0.9300 . ? C44' C45' 1.364(8) . ? C44' H44' 0.9300 . ? C45' C46' 1.414(6) . ? C45' H45' 0.9300 . ? C46' H46' 0.9300 . ? 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 Ni O2 175.13(14) . . ? N1 Ni O1 95.14(12) . . ? O2 Ni O1 83.51(11) . . ? N1 Ni N2 86.61(14) . . ? O2 Ni N2 95.16(13) . . ? O1 Ni N2 174.61(15) . . ? C7 O1 Ni 126.8(2) . . ? C14 O2 Ni 126.2(2) . . ? C30 O3 C8 117.1(3) . . ? C32 O6 C33 119.8(4) . . ? H71 O7 H72 104.2 . . ? H81 O8 H82 107.0 . . ? C13 N1 C1 118.8(3) . . ? C13 N1 Ni 127.8(3) . . ? C1 N1 Ni 112.9(3) . . ? C16 N2 C6 125.0(3) . . ? C16 N2 Ni 122.9(3) . . ? C6 N2 Ni 111.7(3) . . ? C32 N3 C31 119.5(4) . . ? C32 N3 H30 120.3 . . ? C31 N3 H30 120.3 . . ? C2 C1 C6 122.2(4) . . ? C2 C1 N1 125.5(4) . . ? C6 C1 N1 112.2(3) . . ? C3 C2 C1 119.2(5) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C4 C3 C2 119.7(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 121.3(5) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C6 119.8(5) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 N2 114.9(4) . . ? C1 C6 C5 117.3(4) . . ? N2 C6 C5 127.3(4) . . ? O1 C7 C12 124.6(3) . . ? O1 C7 C8 118.6(3) . . ? C12 C7 C8 116.8(4) . . ? C9 C8 O3 119.9(3) . . ? C9 C8 C7 122.5(3) . . ? O3 C8 C7 117.5(3) . . ? C8 C9 C10 120.4(4) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 118.4(4) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C10 C11 C12 123.0(4) . . ? C10 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C7 C12 C11 118.8(4) . . ? C7 C12 C13 121.1(4) . . ? C11 C12 C13 120.0(4) . . ? N1 C13 C12 124.3(4) . . ? N1 C13 H13 117.8 . . ? C12 C13 H13 117.8 . . ? O2 C14 C15 122.5(4) . . ? O2 C14 C21 115.1(4) . . ? C15 C14 C21 122.4(4) . . ? C14 C15 C16 126.2(4) . . ? C14 C15 H15 116.9 . . ? C16 C15 H15 116.9 . . ? N2 C16 C15 122.1(3) . . ? N2 C16 C17 123.4(4) . . ? C15 C16 C17 114.5(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C26 C21 C22 117.4(4) . . ? C26 C21 C14 119.7(4) . . ? C22 C21 C14 122.9(4) . . ? C23 C22 C21 120.9(5) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 120.8(5) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 119.2(5) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 120.2(5) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 121.4(5) . . ? C21 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? O4 C30 O3 123.9(4) . . ? O4 C30 C31 125.8(4) . . ? O3 C30 C31 110.3(3) . . ? N3 C31 C30 111.5(3) . . ? N3 C31 C40 114.1(3) . . ? C30 C31 C40 111.1(3) . . ? N3 C31 H31 106.6 . . ? C30 C31 H31 106.6 . . ? C40 C31 H31 106.6 . . ? O5 C32 N3 124.8(4) . . ? O5 C32 O6 125.6(4) . . ? N3 C32 O6 109.7(4) . . ? O6 C33 C34 110.0(3) . . ? O6 C33 C35 102.6(4) . . ? C34 C33 C35 110.4(4) . . ? O6 C33 C36 109.7(3) . . ? C34 C33 C36 113.3(5) . . ? C35 C33 C36 110.2(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C41 C40 C31 113.5(3) . . ? C41 C40 H40A 108.9 . . ? C31 C40 H40A 108.9 . . ? C41 C40 H40B 108.9 . . ? C31 C40 H40B 108.9 . . ? H40A C40 H40B 107.7 . . ? C42 C41 C46 118.3(4) . . ? C42 C41 C40 121.8(4) . . ? C46 C41 C40 119.8(5) . . ? C41 C42 C43 120.9(5) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C44 C43 C42 119.9(6) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C45 C44 C43 121.0(6) . . ? C45 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? C44 C45 C46 119.7(5) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C41 C46 C45 120.0(5) . . ? C41 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? O2' Ni' O1' 83.82(11) . . ? O2' Ni' N1' 173.65(14) . . ? O1' Ni' N1' 94.96(13) . . ? O2' Ni' N2' 95.33(13) . . ? O1' Ni' N2' 174.45(15) . . ? N1' Ni' N2' 86.49(14) . . ? C7' O1' Ni' 127.7(2) . . ? C14' O2' Ni' 125.5(2) . . ? C30' O3' C8' 116.6(3) . . ? C32' O6' C33' 121.6(4) . . ? H71' O7' H72' 104.3 . . ? H81' O8' H82' 104.0 . . ? C13' N1' C1' 120.9(3) . . ? C13' N1' Ni' 125.9(3) . . ? C1' N1' Ni' 112.7(3) . . ? C16' N2' C6' 125.1(3) . . ? C16' N2' Ni' 122.6(3) . . ? C6' N2' Ni' 111.7(3) . . ? C32' N3' C31' 120.3(4) . . ? C32' N3' H30' 119.9 . . ? C31' N3' H30' 119.9 . . ? C6' C1' C2' 121.5(4) . . ? C6' C1' N1' 113.6(3) . . ? C2' C1' N1' 124.7(4) . . ? C3' C2' C1' 118.7(5) . . ? C3' C2' H2' 120.7 . . ? C1' C2' H2' 120.7 . . ? C4' C3' C2' 119.4(5) . . ? C4' C3' H3' 120.3 . . ? C2' C3' H3' 120.3 . . ? C3' C4' C5' 122.8(5) . . ? C3' C4' H4' 118.6 . . ? C5' C4' H4' 118.6 . . ? C4' C5' C6' 119.6(5) . . ? C4' C5' H5' 120.2 . . ? C6' C5' H5' 120.2 . . ? C1' C6' C5' 117.8(4) . . ? C1' C6' N2' 114.3(3) . . ? C5' C6' N2' 127.6(4) . . ? O1' C7' C8' 120.2(3) . . ? O1' C7' C12' 124.3(4) . . ? C8' C7' C12' 115.4(3) . . ? C9' C8' C7' 123.7(3) . . ? C9' C8' O3' 118.0(3) . . ? C7' C8' O3' 118.0(3) . . ? C8' C9' C10' 119.0(4) . . ? C8' C9' H9' 120.5 . . ? C10' C9' H9' 120.5 . . ? C11' C10' C9' 120.0(4) . . ? C11' C10' H10' 120.0 . . ? C9' C10' H10' 120.0 . . ? C10' C11' C12' 121.1(4) . . ? C10' C11' H11' 119.4 . . ? C12' C11' H11' 119.4 . . ? C11' C12' C7' 120.5(4) . . ? C11' C12' C13' 119.0(3) . . ? C7' C12' C13' 120.5(4) . . ? N1' C13' C12' 126.4(4) . . ? N1' C13' H13' 116.8 . . ? C12' C13' H13' 116.8 . . ? O2' C14' C15' 123.4(4) . . ? O2' C14' C21' 115.0(3) . . ? C15' C14' C21' 121.5(4) . . ? C14' C15' C16' 126.8(4) . . ? C14' C15' H15' 116.6 . . ? C16' C15' H15' 116.6 . . ? N2' C16' C15' 121.3(3) . . ? N2' C16' C17' 122.7(4) . . ? C15' C16' C17' 116.0(4) . . ? C16' C17' H17D 109.5 . . ? C16' C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? C16' C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? C26' C21' C22' 118.0(4) . . ? C26' C21' C14' 120.3(4) . . ? C22' C21' C14' 121.7(4) . . ? C23' C22' C21' 119.7(5) . . ? C23' C22' H22' 120.2 . . ? C21' C22' H22' 120.2 . . ? C24' C23' C22' 121.9(5) . . ? C24' C23' H23' 119.1 . . ? C22' C23' H23' 119.1 . . ? C23' C24' C25' 119.3(6) . . ? C23' C24' H24' 120.3 . . ? C25' C24' H24' 120.3 . . ? C24' C25' C26' 120.3(6) . . ? C24' C25' H25' 119.9 . . ? C26' C25' H25' 119.9 . . ? C21' C26' C25' 120.9(5) . . ? C21' C26' H26' 119.6 . . ? C25' C26' H26' 119.6 . . ? O4' C30' O3' 123.2(4) . . ? O4' C30' C31' 123.9(4) . . ? O3' C30' C31' 112.8(3) . . ? N3' C31' C40' 112.7(3) . . ? N3' C31' C30' 112.7(3) . . ? C40' C31' C30' 109.5(3) . . ? N3' C31' H31' 107.2 . . ? C40' C31' H31' 107.2 . . ? C30' C31' H31' 107.2 . . ? O5' C32' O6' 125.5(4) . . ? O5' C32' N3' 123.5(4) . . ? O6' C32' N3' 111.0(4) . . ? O6' C33' C34' 109.5(4) . . ? O6' C33' C36' 109.8(4) . . ? C34' C33' C36' 113.1(6) . . ? O6' C33' C35' 101.2(5) . . ? C34' C33' C35' 111.1(5) . . ? C36' C33' C35' 111.6(5) . . ? C33' C36' H36D 109.5 . . ? C33' C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C33' C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? C33' C35' H35D 109.5 . . ? C33' C35' H35E 109.5 . . ? H35D C35' H35E 109.5 . . ? C33' C35' H35F 109.5 . . ? H35D C35' H35F 109.5 . . ? H35E C35' H35F 109.5 . . ? C33' C34' H34D 109.5 . . ? C33' C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? C33' C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C41' C40' C31' 116.3(3) . . ? C41' C40' H40C 108.2 . . ? C31' C40' H40C 108.2 . . ? C41' C40' H40D 108.2 . . ? C31' C40' H40D 108.2 . . ? H40C C40' H40D 107.4 . . ? C46' C41' C42' 117.6(4) . . ? C46' C41' C40' 124.0(4) . . ? C42' C41' C40' 118.4(4) . . ? C41' C42' C43' 120.8(5) . . ? C41' C42' H42' 119.6 . . ? C43' C42' H42' 119.6 . . ? C44' C43' C42' 121.1(6) . . ? C44' C43' H43' 119.5 . . ? C42' C43' H43' 119.5 . . ? C43' C44' C45' 120.3(5) . . ? C43' C44' H44' 119.9 . . ? C45' C44' H44' 119.9 . . ? C44' C45' C46' 119.1(5) . . ? C44' C45' H45' 120.5 . . ? C46' C45' H45' 120.5 . . ? C41' C46' C45' 121.2(5) . . ? C41' C46' H46' 119.4 . . ? C45' C46' H46' 119.4 . . ? #EOF