# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Nagao Kobayashi' 'Takamitsu Fukuda' 'Yusuke Ogi' _publ_contact_author_name 'Nagao Kobayashi' _publ_contact_author_address ; Department of Chemistry Tohoku University Sendai 980-8578 JAPAN ; _publ_contact_author_email NAGAOK@MAIL.TAINS.TOHOKU.AC.JP _publ_requested_journal 'Chemical Communications' _publ_section_title ; Skeletal Modification of a Non-Planar Phthalocyanine Analogue under Very Mild Conditions ; data_omeibc _database_code_depnum_ccdc_archive 'CCDC 283235' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H54 N8 Ni O2' _chemical_formula_sum 'C58 H54 N8 Ni O2' _chemical_formula_weight 953.80 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.817(5) _cell_length_b 15.359(6) _cell_length_c 15.504(6) _cell_angle_alpha 73.82(2) _cell_angle_beta 75.54(2) _cell_angle_gamma 64.453(18) _cell_volume 2410.9(17) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5670 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 223.2 _exptl_crystal_description cubic _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 0.456 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.851 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 22872 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18990 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8331 _reflns_number_gt 7524 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+2.1372P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8331 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 Ni1 Ni 0.13326(3) 0.05413(2) 0.21611(2) 0.02547(11) Uani 1 1 d . . . O1 O 0.0048(2) 0.19695(16) 0.01621(15) 0.0471(5) Uani 1 1 d . . . O2 O 0.15772(16) -0.15782(13) 0.20590(12) 0.0283(4) Uani 1 1 d . . . N1 N 0.0095(2) 0.17376(15) 0.17340(15) 0.0287(5) Uani 1 1 d . . . N2 N 0.1454(2) 0.24549(17) 0.05441(17) 0.0363(6) Uani 1 1 d . . . N3 N 0.2612(2) 0.09696(15) 0.15166(15) 0.0272(5) Uani 1 1 d . . . N4 N 0.4386(2) -0.03305(16) 0.21683(15) 0.0288(5) Uani 1 1 d . . . N5 N 0.25512(19) -0.06959(15) 0.24449(15) 0.0250(5) Uani 1 1 d . . . N6 N 0.13507(19) -0.15528(15) 0.35556(14) 0.0250(5) Uani 1 1 d . . . N7 N 0.01290(19) 0.01621(15) 0.30149(15) 0.0264(5) Uani 1 1 d . . . N8 N -0.1629(2) 0.17212(16) 0.29242(15) 0.0302(5) Uani 1 1 d . . . C1 C -0.1091(2) 0.20990(18) 0.21147(19) 0.0294(6) Uani 1 1 d . . . C2 C -0.1916(3) 0.3040(2) 0.1564(2) 0.0340(6) Uani 1 1 d . . . C3 C -0.0887(3) 0.3372(2) 0.0881(2) 0.0416(7) Uani 1 1 d . . . C4 C 0.0262(3) 0.2343(2) 0.0817(2) 0.0395(7) Uani 1 1 d . . . C5 C 0.2448(3) 0.18445(19) 0.08732(19) 0.0314(6) Uani 1 1 d . . . C6 C 0.3718(3) 0.1953(2) 0.0551(2) 0.0383(7) Uani 1 1 d . . . C7 C 0.4463(3) 0.1269(2) 0.1338(2) 0.0340(6) Uani 1 1 d . . . C8 C 0.3801(2) 0.05584(19) 0.17103(18) 0.0270(6) Uani 1 1 d . . . C9 C 0.3766(2) -0.09465(18) 0.24353(17) 0.0249(5) Uani 1 1 d . . . C10 C 0.4413(2) -0.20259(19) 0.27039(18) 0.0264(6) Uani 1 1 d . . . C11 C 0.3515(2) -0.24207(18) 0.27918(18) 0.0262(6) Uani 1 1 d . . . C12 C 0.2228(2) -0.15699(18) 0.27049(18) 0.0252(6) Uani 1 1 d . . . C13 C 0.0391(2) -0.07417(18) 0.36319(17) 0.0245(5) Uani 1 1 d . . . C14 C -0.0677(2) -0.06187(19) 0.43987(18) 0.0266(6) Uani 1 1 d . . . C15 C -0.1555(2) 0.03498(19) 0.42005(18) 0.0283(6) Uani 1 1 d . . . C16 C -0.1020(2) 0.08130(19) 0.33239(18) 0.0262(6) Uani 1 1 d . . . C17 C -0.2836(3) 0.3777(2) 0.2160(2) 0.0514(9) Uani 1 1 d . . . H1 H -0.3453 0.3524 0.2549 0.077 Uiso 1 1 calc R . . H2 H -0.3270 0.4399 0.1778 0.077 Uiso 1 1 calc R . . H3 H -0.2368 0.3875 0.2533 0.077 Uiso 1 1 calc R . . C18 C -0.2713(3) 0.2771(3) 0.1115(2) 0.0522(9) Uani 1 1 d . . . H4 H -0.2155 0.2318 0.0716 0.078 Uiso 1 1 calc R . . H5 H -0.3270 0.3362 0.0765 0.078 Uiso 1 1 calc R . . H6 H -0.3218 0.2461 0.1581 0.078 Uiso 1 1 calc R . . C19 C -0.1240(4) 0.3959(3) -0.0039(3) 0.0635(11) Uani 1 1 d . . . H7 H -0.1992 0.4551 0.0036 0.095 Uiso 1 1 calc R . . H8 H -0.1410 0.3566 -0.0344 0.095 Uiso 1 1 calc R . . H9 H -0.0545 0.4136 -0.0400 0.095 Uiso 1 1 calc R . . C20 C -0.0475(3) 0.3963(2) 0.1296(3) 0.0587(10) Uani 1 1 d . . . H10 H 0.0235 0.4090 0.0897 0.088 Uiso 1 1 calc R . . H11 H -0.0223 0.3591 0.1883 0.088 Uiso 1 1 calc R . . H12 H -0.1177 0.4583 0.1373 0.088 Uiso 1 1 calc R . . C21 C 0.3581(4) 0.3015(3) 0.0321(3) 0.0653(11) Uani 1 1 d . . . H13 H 0.3099 0.3368 -0.0179 0.098 Uiso 1 1 calc R . . H14 H 0.4416 0.3041 0.0149 0.098 Uiso 1 1 calc R . . H15 H 0.3142 0.3316 0.0848 0.098 Uiso 1 1 calc R . . C22 C 0.4292(3) 0.1524(3) -0.0331(2) 0.0546(9) Uani 1 1 d . . . H16 H 0.3718 0.1886 -0.0777 0.082 Uiso 1 1 calc R . . H17 H 0.4414 0.0836 -0.0194 0.082 Uiso 1 1 calc R . . H18 H 0.5102 0.1582 -0.0573 0.082 Uiso 1 1 calc R . . C23 C 0.4171(4) 0.1828(3) 0.2106(2) 0.0569(10) Uani 1 1 d . . . H19 H 0.3261 0.2169 0.2250 0.085 Uiso 1 1 calc R . . H20 H 0.4569 0.2301 0.1910 0.085 Uiso 1 1 calc R . . H21 H 0.4501 0.1364 0.2642 0.085 Uiso 1 1 calc R . . C24 C 0.5890(3) 0.0763(2) 0.1096(2) 0.0481(8) Uani 1 1 d . . . H22 H 0.6250 0.0347 0.1638 0.072 Uiso 1 1 calc R . . H23 H 0.6254 0.1255 0.0843 0.072 Uiso 1 1 calc R . . H24 H 0.6077 0.0364 0.0652 0.072 Uiso 1 1 calc R . . C25 C 0.5693(2) -0.2613(2) 0.27652(19) 0.0317(6) Uani 1 1 d . . . C26 C 0.6017(3) -0.3627(2) 0.2885(2) 0.0381(7) Uani 1 1 d . . . H25 H 0.6861 -0.4059 0.2944 0.046 Uiso 1 1 calc R . . C27 C 0.5148(3) -0.4012(2) 0.2920(2) 0.0389(7) Uani 1 1 d . . . H26 H 0.5425 -0.4697 0.2984 0.047 Uiso 1 1 calc R . . C28 C 0.3859(3) -0.34217(19) 0.28638(19) 0.0318(6) Uani 1 1 d . . . C29 C 0.6673(2) -0.2246(2) 0.2751(2) 0.0341(6) Uani 1 1 d . . . C30 C 0.6490(3) -0.1669(2) 0.3360(2) 0.0422(7) Uani 1 1 d . . . H27 H 0.5737 -0.1499 0.3777 0.051 Uiso 1 1 calc R . . C31 C 0.7424(3) -0.1345(3) 0.3352(2) 0.0518(9) Uani 1 1 d . . . H28 H 0.7299 -0.0952 0.3764 0.062 Uiso 1 1 calc R . . C32 C 0.8528(3) -0.1592(3) 0.2747(3) 0.0576(10) Uani 1 1 d . . . H29 H 0.9148 -0.1358 0.2737 0.069 Uiso 1 1 calc R . . C33 C 0.8724(3) -0.2178(3) 0.2160(2) 0.0546(9) Uani 1 1 d . . . H30 H 0.9488 -0.2357 0.1754 0.066 Uiso 1 1 calc R . . C34 C 0.7808(3) -0.2513(2) 0.2154(2) 0.0443(8) Uani 1 1 d . . . H31 H 0.7952 -0.2919 0.1750 0.053 Uiso 1 1 calc R . . C35 C 0.3015(3) -0.38753(19) 0.2784(2) 0.0342(6) Uani 1 1 d . . . C36 C 0.3482(3) -0.4538(2) 0.2195(2) 0.0467(8) Uani 1 1 d . . . H32 H 0.4308 -0.4684 0.1870 0.056 Uiso 1 1 calc R . . C37 C 0.2739(4) -0.4979(3) 0.2086(3) 0.0581(10) Uani 1 1 d . . . H33 H 0.3064 -0.5429 0.1693 0.070 Uiso 1 1 calc R . . C38 C 0.1538(4) -0.4766(3) 0.2545(3) 0.0606(10) Uani 1 1 d . . . H34 H 0.1033 -0.5062 0.2464 0.073 Uiso 1 1 calc R . . C39 C 0.1059(3) -0.4109(2) 0.3134(3) 0.0498(9) Uani 1 1 d . . . H35 H 0.0230 -0.3964 0.3451 0.060 Uiso 1 1 calc R . . C40 C 0.1794(3) -0.3667(2) 0.3255(2) 0.0375(7) Uani 1 1 d . . . H36 H 0.1467 -0.3227 0.3656 0.045 Uiso 1 1 calc R . . C41 C -0.0939(3) -0.1289(2) 0.51466(19) 0.0321(6) Uani 1 1 d . . . C42 C -0.2084(3) -0.0904(2) 0.5718(2) 0.0469(8) Uani 1 1 d . . . H37 H -0.2284 -0.1321 0.6249 0.056 Uiso 1 1 calc R . . C43 C -0.2927(3) 0.0056(2) 0.5533(2) 0.0454(8) Uani 1 1 d . . . H38 H -0.3671 0.0276 0.5948 0.055 Uiso 1 1 calc R . . C44 C -0.2712(3) 0.0715(2) 0.47529(19) 0.0323(6) Uani 1 1 d . . . C45 C -0.0186(3) -0.2366(2) 0.53414(19) 0.0356(7) Uani 1 1 d . . . C46 C 0.1027(3) -0.2777(2) 0.5555(2) 0.0427(7) Uani 1 1 d . . . H39 H 0.1419 -0.2368 0.5579 0.051 Uiso 1 1 calc R . . C47 C 0.1671(4) -0.3790(3) 0.5736(2) 0.0568(9) Uani 1 1 d . . . H40 H 0.2502 -0.4062 0.5872 0.068 Uiso 1 1 calc R . . C48 C 0.1108(4) -0.4401(3) 0.5718(3) 0.0632(11) Uani 1 1 d . . . H41 H 0.1548 -0.5088 0.5843 0.076 Uiso 1 1 calc R . . C49 C -0.0102(4) -0.3998(3) 0.5515(3) 0.0660(11) Uani 1 1 d . . . H42 H -0.0494 -0.4412 0.5506 0.079 Uiso 1 1 calc R . . C50 C -0.0749(3) -0.2993(2) 0.5326(2) 0.0512(9) Uani 1 1 d . . . H43 H -0.1576 -0.2727 0.5185 0.061 Uiso 1 1 calc R . . C51 C -0.3731(3) 0.1723(2) 0.45544(19) 0.0338(6) Uani 1 1 d . . . C52 C -0.4603(3) 0.1897(3) 0.4020(3) 0.0580(10) Uani 1 1 d . . . H44 H -0.4524 0.1394 0.3747 0.070 Uiso 1 1 calc R . . C53 C -0.5587(3) 0.2797(3) 0.3879(3) 0.0649(11) Uani 1 1 d . . . H45 H -0.6173 0.2901 0.3510 0.078 Uiso 1 1 calc R . . C54 C -0.5731(3) 0.3543(3) 0.4264(2) 0.0541(9) Uani 1 1 d . . . H46 H -0.6409 0.4158 0.4165 0.065 Uiso 1 1 calc R . . C55 C -0.4864(3) 0.3378(2) 0.4801(2) 0.0536(9) Uani 1 1 d . . . H47 H -0.4946 0.3885 0.5069 0.064 Uiso 1 1 calc R . . C56 C -0.3871(3) 0.2469(2) 0.4953(2) 0.0415(7) Uani 1 1 d . . . H48 H -0.3291 0.2362 0.5328 0.050 Uiso 1 1 calc R . . C57 C 0.0911(3) 0.1004(2) 0.0071(3) 0.0585(10) Uani 1 1 d . . . H49 H 0.1772 0.0971 -0.0041 0.088 Uiso 1 1 calc R . . H50 H 0.0758 0.0833 -0.0434 0.088 Uiso 1 1 calc R . . H51 H 0.0795 0.0545 0.0625 0.088 Uiso 1 1 calc R . . C58 C 0.2293(3) -0.1701(2) 0.1182(2) 0.0398(7) Uani 1 1 d . . . H52 H 0.2614 -0.1183 0.0935 0.060 Uiso 1 1 calc R . . H53 H 0.1755 -0.1669 0.0784 0.060 Uiso 1 1 calc R . . H54 H 0.2999 -0.2336 0.1232 0.060 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 Ni1 0.02008(19) 0.02171(18) 0.0311(2) -0.00301(14) -0.00044(14) -0.00802(14) O1 0.0460(13) 0.0485(13) 0.0422(13) -0.0091(10) -0.0071(10) -0.0138(11) O2 0.0243(9) 0.0325(10) 0.0285(10) -0.0082(8) -0.0031(8) -0.0105(8) N1 0.0250(12) 0.0221(11) 0.0341(13) -0.0018(9) -0.0021(10) -0.0081(9) N2 0.0310(13) 0.0310(13) 0.0414(15) -0.0007(11) -0.0006(11) -0.0134(11) N3 0.0236(12) 0.0243(11) 0.0324(13) -0.0047(9) -0.0003(9) -0.0107(9) N4 0.0234(12) 0.0313(12) 0.0320(13) -0.0058(10) -0.0022(9) -0.0121(10) N5 0.0207(11) 0.0234(11) 0.0292(12) -0.0032(9) -0.0009(9) -0.0098(9) N6 0.0229(11) 0.0250(11) 0.0269(12) -0.0042(9) -0.0008(9) -0.0112(9) N7 0.0202(11) 0.0239(11) 0.0322(13) -0.0055(9) -0.0004(9) -0.0080(9) N8 0.0256(12) 0.0280(12) 0.0314(13) -0.0065(10) 0.0014(10) -0.0080(10) C1 0.0256(14) 0.0226(13) 0.0378(16) -0.0077(12) -0.0050(12) -0.0060(11) C2 0.0262(14) 0.0276(14) 0.0372(17) -0.0044(12) -0.0031(12) -0.0025(12) C3 0.0425(18) 0.0259(15) 0.0468(19) -0.0012(13) -0.0039(14) -0.0097(13) C4 0.0402(17) 0.0407(17) 0.0370(17) -0.0009(14) -0.0051(13) -0.0196(14) C5 0.0311(15) 0.0257(14) 0.0349(16) -0.0064(12) 0.0026(12) -0.0126(12) C6 0.0338(16) 0.0343(16) 0.0438(18) -0.0018(13) 0.0018(13) -0.0181(13) C7 0.0340(16) 0.0393(16) 0.0343(16) -0.0071(13) -0.0005(12) -0.0217(13) C8 0.0275(14) 0.0307(14) 0.0259(14) -0.0085(11) 0.0014(11) -0.0151(12) C9 0.0207(13) 0.0281(13) 0.0240(14) -0.0061(11) -0.0005(10) -0.0086(11) C10 0.0220(13) 0.0267(13) 0.0268(14) -0.0065(11) -0.0010(11) -0.0067(11) C11 0.0227(13) 0.0258(13) 0.0258(14) -0.0059(11) -0.0017(11) -0.0061(11) C12 0.0220(13) 0.0226(13) 0.0287(14) -0.0058(11) -0.0011(11) -0.0077(11) C13 0.0244(13) 0.0242(13) 0.0265(14) -0.0060(11) -0.0022(11) -0.0110(11) C14 0.0237(13) 0.0298(14) 0.0280(15) -0.0081(11) -0.0023(11) -0.0114(11) C15 0.0245(14) 0.0319(14) 0.0295(15) -0.0115(12) -0.0011(11) -0.0103(12) C16 0.0245(14) 0.0274(13) 0.0295(15) -0.0069(11) -0.0028(11) -0.0125(11) C17 0.0397(18) 0.0342(17) 0.059(2) -0.0105(16) 0.0020(16) 0.0009(14) C18 0.0388(18) 0.056(2) 0.058(2) -0.0088(17) -0.0140(16) -0.0130(16) C19 0.061(2) 0.044(2) 0.060(2) 0.0083(18) -0.0089(19) -0.0087(18) C20 0.053(2) 0.0293(17) 0.088(3) -0.0133(17) 0.0012(19) -0.0155(16) C21 0.060(2) 0.046(2) 0.093(3) 0.008(2) -0.015(2) -0.0346(19) C22 0.0419(19) 0.084(3) 0.0343(19) -0.0073(17) 0.0012(15) -0.0279(19) C23 0.075(3) 0.073(2) 0.045(2) -0.0233(18) 0.0063(18) -0.050(2) C24 0.0349(17) 0.056(2) 0.054(2) 0.0016(16) -0.0045(15) -0.0271(16) C25 0.0231(14) 0.0343(15) 0.0325(16) -0.0077(12) -0.0029(11) -0.0064(12) C26 0.0249(15) 0.0353(16) 0.0451(18) -0.0088(13) -0.0089(13) -0.0009(13) C27 0.0358(16) 0.0246(14) 0.0481(19) -0.0094(13) -0.0097(14) -0.0010(12) C28 0.0281(15) 0.0273(14) 0.0340(16) -0.0062(12) -0.0050(12) -0.0051(12) C29 0.0211(14) 0.0377(16) 0.0371(17) -0.0019(13) -0.0089(12) -0.0066(12) C30 0.0313(16) 0.0478(18) 0.0464(19) -0.0119(15) -0.0107(14) -0.0102(14) C31 0.0419(19) 0.066(2) 0.056(2) -0.0150(18) -0.0143(16) -0.0231(17) C32 0.039(2) 0.080(3) 0.066(3) -0.007(2) -0.0150(17) -0.0341(19) C33 0.0281(17) 0.078(3) 0.050(2) -0.0006(19) -0.0036(15) -0.0213(17) C34 0.0299(16) 0.055(2) 0.0398(18) -0.0097(15) -0.0038(13) -0.0098(15) C35 0.0387(16) 0.0220(13) 0.0409(17) -0.0027(12) -0.0126(13) -0.0094(12) C36 0.0484(19) 0.0357(17) 0.053(2) -0.0133(15) -0.0120(16) -0.0084(15) C37 0.077(3) 0.045(2) 0.063(2) -0.0172(18) -0.021(2) -0.0239(19) C38 0.079(3) 0.046(2) 0.076(3) -0.0020(19) -0.034(2) -0.035(2) C39 0.048(2) 0.0410(18) 0.064(2) 0.0035(16) -0.0155(17) -0.0256(16) C40 0.0398(17) 0.0263(14) 0.0438(18) -0.0031(13) -0.0071(14) -0.0124(13) C41 0.0306(15) 0.0361(15) 0.0279(15) -0.0049(12) 0.0009(12) -0.0149(13) C42 0.0431(19) 0.0514(19) 0.0307(17) 0.0030(14) 0.0063(14) -0.0171(16) C43 0.0351(17) 0.053(2) 0.0322(17) -0.0083(15) 0.0081(13) -0.0093(15) C44 0.0281(15) 0.0392(16) 0.0275(15) -0.0108(12) 0.0003(11) -0.0109(13) C45 0.0401(17) 0.0376(16) 0.0251(15) 0.0008(12) -0.0013(12) -0.0175(14) C46 0.0437(18) 0.0420(18) 0.0404(19) -0.0060(14) -0.0101(14) -0.0140(15) C47 0.057(2) 0.050(2) 0.051(2) 0.0002(17) -0.0213(18) -0.0090(18) C48 0.084(3) 0.0324(18) 0.062(3) 0.0111(17) -0.021(2) -0.0187(19) C49 0.084(3) 0.043(2) 0.077(3) 0.0098(19) -0.023(2) -0.038(2) C50 0.049(2) 0.049(2) 0.056(2) 0.0074(16) -0.0100(16) -0.0289(17) C51 0.0252(14) 0.0427(16) 0.0289(15) -0.0135(13) 0.0064(11) -0.0108(13) C52 0.048(2) 0.055(2) 0.070(3) -0.0313(19) -0.0233(18) 0.0004(17) C53 0.049(2) 0.065(2) 0.075(3) -0.024(2) -0.030(2) 0.0008(19) C54 0.0403(19) 0.0422(19) 0.054(2) -0.0083(16) -0.0023(16) 0.0045(15) C55 0.063(2) 0.0404(18) 0.049(2) -0.0181(16) 0.0002(17) -0.0112(17) C56 0.0416(18) 0.0441(18) 0.0374(18) -0.0092(14) -0.0020(14) -0.0165(15) C57 0.061(2) 0.0390(18) 0.054(2) -0.0154(16) -0.0094(18) 0.0043(17) C58 0.0355(16) 0.0479(18) 0.0321(17) -0.0124(14) -0.0021(13) -0.0114(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 Ni1 N5 1.835(2) . ? Ni1 N1 1.855(2) . ? Ni1 N3 1.858(2) . ? Ni1 N7 1.860(2) . ? O1 C57 1.414(4) . ? O1 C4 1.414(4) . ? O2 C12 1.413(3) . ? O2 C58 1.425(3) . ? N1 C1 1.311(3) . ? N1 C4 1.485(4) . ? N2 C5 1.266(4) . ? N2 C4 1.437(4) . ? N3 C8 1.343(3) . ? N3 C5 1.401(3) . ? N4 C8 1.318(3) . ? N4 C9 1.353(3) . ? N5 C9 1.314(3) . ? N5 C12 1.474(3) . ? N6 C13 1.284(3) . ? N6 C12 1.459(3) . ? N7 C16 1.358(3) . ? N7 C13 1.405(3) . ? N8 C16 1.313(3) . ? N8 C1 1.353(4) . ? C1 C2 1.510(4) . ? C2 C17 1.529(4) . ? C2 C18 1.539(4) . ? C2 C3 1.566(4) . ? C3 C19 1.509(5) . ? C3 C20 1.530(5) . ? C3 C4 1.587(4) . ? C5 C6 1.524(4) . ? C6 C21 1.514(4) . ? C6 C7 1.547(4) . ? C6 C22 1.555(4) . ? C7 C8 1.516(4) . ? C7 C24 1.518(4) . ? C7 C23 1.544(4) . ? C9 C10 1.479(4) . ? C10 C11 1.396(4) . ? C10 C25 1.399(4) . ? C11 C28 1.389(4) . ? C11 C12 1.526(3) . ? C13 C14 1.488(4) . ? C14 C41 1.389(4) . ? C14 C15 1.399(4) . ? C15 C44 1.393(4) . ? C15 C16 1.474(4) . ? C17 H1 0.9700 . ? C17 H2 0.9700 . ? C17 H3 0.9700 . ? C18 H4 0.9700 . ? C18 H5 0.9700 . ? C18 H6 0.9700 . ? C19 H7 0.9700 . ? C19 H8 0.9700 . ? C19 H9 0.9700 . ? C20 H10 0.9700 . ? C20 H11 0.9700 . ? C20 H12 0.9700 . ? C21 H13 0.9700 . ? C21 H14 0.9700 . ? C21 H15 0.9700 . ? C22 H16 0.9700 . ? C22 H17 0.9700 . ? C22 H18 0.9700 . ? C23 H19 0.9700 . ? C23 H20 0.9700 . ? C23 H21 0.9700 . ? C24 H22 0.9700 . ? C24 H23 0.9700 . ? C24 H24 0.9700 . ? C25 C26 1.402(4) . ? C25 C29 1.485(4) . ? C26 C27 1.373(4) . ? C26 H25 0.9400 . ? C27 C28 1.408(4) . ? C27 H26 0.9400 . ? C28 C35 1.485(4) . ? C29 C30 1.386(4) . ? C29 C34 1.393(4) . ? C30 C31 1.390(4) . ? C30 H27 0.9400 . ? C31 C32 1.374(5) . ? C31 H28 0.9400 . ? C32 C33 1.366(5) . ? C32 H29 0.9400 . ? C33 C34 1.387(5) . ? C33 H30 0.9400 . ? C34 H31 0.9400 . ? C35 C40 1.386(4) . ? C35 C36 1.399(4) . ? C36 C37 1.383(5) . ? C36 H32 0.9400 . ? C37 C38 1.361(5) . ? C37 H33 0.9400 . ? C38 C39 1.391(5) . ? C38 H34 0.9400 . ? C39 C40 1.382(4) . ? C39 H35 0.9400 . ? C40 H36 0.9400 . ? C41 C42 1.403(4) . ? C41 C45 1.485(4) . ? C42 C43 1.375(4) . ? C42 H37 0.9400 . ? C43 C44 1.391(4) . ? C43 H38 0.9400 . ? C44 C51 1.501(4) . ? C45 C46 1.380(4) . ? C45 C50 1.394(4) . ? C46 C47 1.385(5) . ? C46 H39 0.9400 . ? C47 C48 1.373(5) . ? C47 H40 0.9400 . ? C48 C49 1.371(5) . ? C48 H41 0.9400 . ? C49 C50 1.377(5) . ? C49 H42 0.9400 . ? C50 H43 0.9400 . ? C51 C52 1.373(4) . ? C51 C56 1.380(4) . ? C52 C53 1.373(5) . ? C52 H44 0.9400 . ? C53 C54 1.365(5) . ? C53 H45 0.9400 . ? C54 C55 1.375(5) . ? C54 H46 0.9400 . ? C55 C56 1.386(4) . ? C55 H47 0.9400 . ? C56 H48 0.9400 . ? C57 H49 0.9700 . ? C57 H50 0.9700 . ? C57 H51 0.9700 . ? C58 H52 0.9700 . ? C58 H53 0.9700 . ? C58 H54 0.9700 . ? 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 N5 Ni1 N1 172.08(10) . . ? N5 Ni1 N3 88.77(10) . . ? N1 Ni1 N3 91.26(10) . . ? N5 Ni1 N7 90.13(10) . . ? N1 Ni1 N7 91.48(10) . . ? N3 Ni1 N7 167.93(10) . . ? C57 O1 C4 114.8(3) . . ? C12 O2 C58 115.8(2) . . ? C1 N1 C4 109.6(2) . . ? C1 N1 Ni1 126.13(19) . . ? C4 N1 Ni1 123.43(18) . . ? C5 N2 C4 122.8(2) . . ? C8 N3 C5 109.6(2) . . ? C8 N3 Ni1 123.82(18) . . ? C5 N3 Ni1 125.83(18) . . ? C8 N4 C9 117.6(2) . . ? C9 N5 C12 111.1(2) . . ? C9 N5 Ni1 128.16(18) . . ? C12 N5 Ni1 120.74(16) . . ? C13 N6 C12 117.0(2) . . ? C16 N7 C13 108.6(2) . . ? C16 N7 Ni1 123.20(17) . . ? C13 N7 Ni1 125.10(17) . . ? C16 N8 C1 119.4(2) . . ? N1 C1 N8 127.3(2) . . ? N1 C1 C2 114.4(2) . . ? N8 C1 C2 118.3(2) . . ? C1 C2 C17 111.9(3) . . ? C1 C2 C18 107.3(2) . . ? C17 C2 C18 107.5(3) . . ? C1 C2 C3 101.0(2) . . ? C17 C2 C3 114.8(2) . . ? C18 C2 C3 114.1(3) . . ? C19 C3 C20 108.1(3) . . ? C19 C3 C2 116.4(3) . . ? C20 C3 C2 110.7(3) . . ? C19 C3 C4 112.3(3) . . ? C20 C3 C4 107.8(3) . . ? C2 C3 C4 101.2(2) . . ? O1 C4 N2 110.2(2) . . ? O1 C4 N1 109.9(2) . . ? N2 C4 N1 115.5(2) . . ? O1 C4 C3 106.2(2) . . ? N2 C4 C3 111.2(2) . . ? N1 C4 C3 103.2(2) . . ? N2 C5 N3 128.4(2) . . ? N2 C5 C6 122.2(2) . . ? N3 C5 C6 109.3(2) . . ? C21 C6 C5 112.8(3) . . ? C21 C6 C7 117.0(3) . . ? C5 C6 C7 101.5(2) . . ? C21 C6 C22 108.2(3) . . ? C5 C6 C22 105.8(2) . . ? C7 C6 C22 110.8(3) . . ? C8 C7 C24 113.4(2) . . ? C8 C7 C23 105.2(2) . . ? C24 C7 C23 109.2(3) . . ? C8 C7 C6 101.0(2) . . ? C24 C7 C6 116.8(2) . . ? C23 C7 C6 110.4(3) . . ? N4 C8 N3 128.1(2) . . ? N4 C8 C7 120.7(2) . . ? N3 C8 C7 111.2(2) . . ? N5 C9 N4 126.1(2) . . ? N5 C9 C10 110.6(2) . . ? N4 C9 C10 123.2(2) . . ? C11 C10 C25 122.5(2) . . ? C11 C10 C9 106.7(2) . . ? C25 C10 C9 130.4(2) . . ? C28 C11 C10 121.8(2) . . ? C28 C11 C12 130.0(2) . . ? C10 C11 C12 108.0(2) . . ? O2 C12 N6 104.96(19) . . ? O2 C12 N5 111.0(2) . . ? N6 C12 N5 110.9(2) . . ? O2 C12 C11 114.8(2) . . ? N6 C12 C11 112.3(2) . . ? N5 C12 C11 103.0(2) . . ? N6 C13 N7 127.5(2) . . ? N6 C13 C14 124.5(2) . . ? N7 C13 C14 108.0(2) . . ? C41 C14 C15 121.4(2) . . ? C41 C14 C13 131.6(2) . . ? C15 C14 C13 106.7(2) . . ? C44 C15 C14 122.6(3) . . ? C44 C15 C16 130.7(3) . . ? C14 C15 C16 106.5(2) . . ? N8 C16 N7 127.5(2) . . ? N8 C16 C15 122.3(2) . . ? N7 C16 C15 110.1(2) . . ? C2 C17 H1 109.5 . . ? C2 C17 H2 109.5 . . ? H1 C17 H2 109.5 . . ? C2 C17 H3 109.5 . . ? H1 C17 H3 109.5 . . ? H2 C17 H3 109.5 . . ? C2 C18 H4 109.5 . . ? C2 C18 H5 109.5 . . ? H4 C18 H5 109.5 . . ? C2 C18 H6 109.5 . . ? H4 C18 H6 109.5 . . ? H5 C18 H6 109.5 . . ? C3 C19 H7 109.5 . . ? C3 C19 H8 109.5 . . ? H7 C19 H8 109.5 . . ? C3 C19 H9 109.5 . . ? H7 C19 H9 109.5 . . ? H8 C19 H9 109.5 . . ? C3 C20 H10 109.5 . . ? C3 C20 H11 109.5 . . ? H10 C20 H11 109.5 . . ? C3 C20 H12 109.5 . . ? H10 C20 H12 109.5 . . ? H11 C20 H12 109.5 . . ? C6 C21 H13 109.5 . . ? C6 C21 H14 109.5 . . ? H13 C21 H14 109.5 . . ? C6 C21 H15 109.5 . . ? H13 C21 H15 109.5 . . ? H14 C21 H15 109.5 . . ? C6 C22 H16 109.5 . . ? C6 C22 H17 109.5 . . ? H16 C22 H17 109.5 . . ? C6 C22 H18 109.5 . . ? H16 C22 H18 109.5 . . ? H17 C22 H18 109.5 . . ? C7 C23 H19 109.5 . . ? C7 C23 H20 109.5 . . ? H19 C23 H20 109.5 . . ? C7 C23 H21 109.5 . . ? H19 C23 H21 109.5 . . ? H20 C23 H21 109.5 . . ? C7 C24 H22 109.5 . . ? C7 C24 H23 109.5 . . ? H22 C24 H23 109.5 . . ? C7 C24 H24 109.5 . . ? H22 C24 H24 109.5 . . ? H23 C24 H24 109.5 . . ? C10 C25 C26 115.0(3) . . ? C10 C25 C29 125.2(2) . . ? C26 C25 C29 119.7(2) . . ? C27 C26 C25 122.4(3) . . ? C27 C26 H25 118.8 . . ? C25 C26 H25 118.8 . . ? C26 C27 C28 122.6(3) . . ? C26 C27 H26 118.7 . . ? C28 C27 H26 118.7 . . ? C11 C28 C27 115.4(3) . . ? C11 C28 C35 125.0(2) . . ? C27 C28 C35 119.2(2) . . ? C30 C29 C34 119.3(3) . . ? C30 C29 C25 120.2(3) . . ? C34 C29 C25 120.4(3) . . ? C29 C30 C31 119.7(3) . . ? C29 C30 H27 120.1 . . ? C31 C30 H27 120.1 . . ? C32 C31 C30 120.6(3) . . ? C32 C31 H28 119.7 . . ? C30 C31 H28 119.7 . . ? C33 C32 C31 119.9(3) . . ? C33 C32 H29 120.1 . . ? C31 C32 H29 120.1 . . ? C32 C33 C34 120.7(3) . . ? C32 C33 H30 119.6 . . ? C34 C33 H30 119.6 . . ? C33 C34 C29 119.8(3) . . ? C33 C34 H31 120.1 . . ? C29 C34 H31 120.1 . . ? C40 C35 C36 118.9(3) . . ? C40 C35 C28 123.4(3) . . ? C36 C35 C28 117.7(3) . . ? C37 C36 C35 120.5(3) . . ? C37 C36 H32 119.8 . . ? C35 C36 H32 119.8 . . ? C38 C37 C36 120.3(3) . . ? C38 C37 H33 119.9 . . ? C36 C37 H33 119.9 . . ? C37 C38 C39 120.0(3) . . ? C37 C38 H34 120.0 . . ? C39 C38 H34 120.0 . . ? C40 C39 C38 120.4(3) . . ? C40 C39 H35 119.8 . . ? C38 C39 H35 119.8 . . ? C39 C40 C35 120.0(3) . . ? C39 C40 H36 120.0 . . ? C35 C40 H36 120.0 . . ? C14 C41 C42 115.4(3) . . ? C14 C41 C45 126.1(2) . . ? C42 C41 C45 118.2(3) . . ? C43 C42 C41 122.8(3) . . ? C43 C42 H37 118.6 . . ? C41 C42 H37 118.6 . . ? C42 C43 C44 122.1(3) . . ? C42 C43 H38 118.9 . . ? C44 C43 H38 118.9 . . ? C43 C44 C15 115.4(3) . . ? C43 C44 C51 119.0(2) . . ? C15 C44 C51 125.5(3) . . ? C46 C45 C50 118.4(3) . . ? C46 C45 C41 123.5(3) . . ? C50 C45 C41 118.1(3) . . ? C45 C46 C47 120.4(3) . . ? C45 C46 H39 119.8 . . ? C47 C46 H39 119.8 . . ? C48 C47 C46 120.7(3) . . ? C48 C47 H40 119.6 . . ? C46 C47 H40 119.6 . . ? C49 C48 C47 119.2(3) . . ? C49 C48 H41 120.4 . . ? C47 C48 H41 120.4 . . ? C48 C49 C50 120.7(3) . . ? C48 C49 H42 119.7 . . ? C50 C49 H42 119.7 . . ? C49 C50 C45 120.5(3) . . ? C49 C50 H43 119.7 . . ? C45 C50 H43 119.7 . . ? C52 C51 C56 118.6(3) . . ? C52 C51 C44 120.0(3) . . ? C56 C51 C44 121.3(3) . . ? C53 C52 C51 120.7(3) . . ? C53 C52 H44 119.6 . . ? C51 C52 H44 119.6 . . ? C54 C53 C52 121.2(3) . . ? C54 C53 H45 119.4 . . ? C52 C53 H45 119.4 . . ? C53 C54 C55 118.6(3) . . ? C53 C54 H46 120.7 . . ? C55 C54 H46 120.7 . . ? C54 C55 C56 120.6(3) . . ? C54 C55 H47 119.7 . . ? C56 C55 H47 119.7 . . ? C51 C56 C55 120.2(3) . . ? C51 C56 H48 119.9 . . ? C55 C56 H48 119.9 . . ? O1 C57 H49 109.5 . . ? O1 C57 H50 109.5 . . ? H49 C57 H50 109.5 . . ? O1 C57 H51 109.5 . . ? H49 C57 H51 109.5 . . ? H50 C57 H51 109.5 . . ? O2 C58 H52 109.5 . . ? O2 C58 H53 109.5 . . ? H52 C58 H53 109.5 . . ? O2 C58 H54 109.5 . . ? H52 C58 H54 109.5 . . ? H53 C58 H54 109.5 . . ? 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 N3 Ni1 N1 C1 -157.8(2) . . . . ? N7 Ni1 N1 C1 10.5(2) . . . . ? N3 Ni1 N1 C4 33.5(2) . . . . ? N7 Ni1 N1 C4 -158.3(2) . . . . ? N5 Ni1 N3 C8 -27.9(2) . . . . ? N1 Ni1 N3 C8 160.0(2) . . . . ? N7 Ni1 N3 C8 56.9(5) . . . . ? N5 Ni1 N3 C5 163.4(2) . . . . ? N1 Ni1 N3 C5 -8.7(2) . . . . ? N7 Ni1 N3 C5 -111.8(4) . . . . ? N3 Ni1 N5 C9 20.6(2) . . . . ? N7 Ni1 N5 C9 -147.4(2) . . . . ? N3 Ni1 N5 C12 -157.9(2) . . . . ? N7 Ni1 N5 C12 34.1(2) . . . . ? N5 Ni1 N7 C16 165.1(2) . . . . ? N1 Ni1 N7 C16 -22.6(2) . . . . ? N3 Ni1 N7 C16 80.4(5) . . . . ? N5 Ni1 N7 C13 7.2(2) . . . . ? N1 Ni1 N7 C13 179.4(2) . . . . ? N3 Ni1 N7 C13 -77.5(5) . . . . ? C4 N1 C1 N8 175.8(3) . . . . ? Ni1 N1 C1 N8 5.8(4) . . . . ? C4 N1 C1 C2 -3.9(3) . . . . ? Ni1 N1 C1 C2 -173.95(18) . . . . ? C16 N8 C1 N1 -14.1(4) . . . . ? C16 N8 C1 C2 165.7(2) . . . . ? N1 C1 C2 C17 -139.6(3) . . . . ? N8 C1 C2 C17 40.6(4) . . . . ? N1 C1 C2 C18 102.7(3) . . . . ? N8 C1 C2 C18 -77.1(3) . . . . ? N1 C1 C2 C3 -17.0(3) . . . . ? N8 C1 C2 C3 163.2(2) . . . . ? C1 C2 C3 C19 150.5(3) . . . . ? C17 C2 C3 C19 -89.0(4) . . . . ? C18 C2 C3 C19 35.8(4) . . . . ? C1 C2 C3 C20 -85.6(3) . . . . ? C17 C2 C3 C20 35.0(4) . . . . ? C18 C2 C3 C20 159.7(3) . . . . ? C1 C2 C3 C4 28.4(3) . . . . ? C17 C2 C3 C4 149.0(3) . . . . ? C18 C2 C3 C4 -86.2(3) . . . . ? C57 O1 C4 N2 65.4(3) . . . . ? C57 O1 C4 N1 -63.1(3) . . . . ? C57 O1 C4 C3 -174.0(3) . . . . ? C5 N2 C4 O1 -101.3(3) . . . . ? C5 N2 C4 N1 24.0(4) . . . . ? C5 N2 C4 C3 141.2(3) . . . . ? C1 N1 C4 O1 -90.0(3) . . . . ? Ni1 N1 C4 O1 80.4(3) . . . . ? C1 N1 C4 N2 144.5(3) . . . . ? Ni1 N1 C4 N2 -45.1(3) . . . . ? C1 N1 C4 C3 22.9(3) . . . . ? Ni1 N1 C4 C3 -166.71(18) . . . . ? C19 C3 C4 O1 -40.8(3) . . . . ? C20 C3 C4 O1 -159.7(3) . . . . ? C2 C3 C4 O1 84.0(3) . . . . ? C19 C3 C4 N2 79.1(3) . . . . ? C20 C3 C4 N2 -39.8(3) . . . . ? C2 C3 C4 N2 -156.0(2) . . . . ? C19 C3 C4 N1 -156.4(3) . . . . ? C20 C3 C4 N1 84.7(3) . . . . ? C2 C3 C4 N1 -31.5(3) . . . . ? C4 N2 C5 N3 1.6(5) . . . . ? C4 N2 C5 C6 177.6(3) . . . . ? C8 N3 C5 N2 -177.4(3) . . . . ? Ni1 N3 C5 N2 -7.4(4) . . . . ? C8 N3 C5 C6 6.2(3) . . . . ? Ni1 N3 C5 C6 176.21(18) . . . . ? N2 C5 C6 C21 36.3(4) . . . . ? N3 C5 C6 C21 -147.0(3) . . . . ? N2 C5 C6 C7 162.4(3) . . . . ? N3 C5 C6 C7 -20.9(3) . . . . ? N2 C5 C6 C22 -81.8(3) . . . . ? N3 C5 C6 C22 94.9(3) . . . . ? C21 C6 C7 C8 148.9(3) . . . . ? C5 C6 C7 C8 25.7(3) . . . . ? C22 C6 C7 C8 -86.4(3) . . . . ? C21 C6 C7 C24 -87.6(4) . . . . ? C5 C6 C7 C24 149.2(3) . . . . ? C22 C6 C7 C24 37.2(3) . . . . ? C21 C6 C7 C23 38.0(4) . . . . ? C5 C6 C7 C23 -85.3(3) . . . . ? C22 C6 C7 C23 162.7(3) . . . . ? C9 N4 C8 N3 4.8(4) . . . . ? C9 N4 C8 C7 -176.2(2) . . . . ? C5 N3 C8 N4 -168.6(3) . . . . ? Ni1 N3 C8 N4 21.1(4) . . . . ? C5 N3 C8 C7 12.3(3) . . . . ? Ni1 N3 C8 C7 -157.96(18) . . . . ? C24 C7 C8 N4 30.2(4) . . . . ? C23 C7 C8 N4 -89.0(3) . . . . ? C6 C7 C8 N4 156.1(2) . . . . ? C24 C7 C8 N3 -150.6(3) . . . . ? C23 C7 C8 N3 90.1(3) . . . . ? C6 C7 C8 N3 -24.8(3) . . . . ? C12 N5 C9 N4 175.3(2) . . . . ? Ni1 N5 C9 N4 -3.3(4) . . . . ? C12 N5 C9 C10 -0.9(3) . . . . ? Ni1 N5 C9 C10 -179.51(17) . . . . ? C8 N4 C9 N5 -14.4(4) . . . . ? C8 N4 C9 C10 161.4(2) . . . . ? N5 C9 C10 C11 5.7(3) . . . . ? N4 C9 C10 C11 -170.7(2) . . . . ? N5 C9 C10 C25 178.2(3) . . . . ? N4 C9 C10 C25 1.8(4) . . . . ? C25 C10 C11 C28 -6.0(4) . . . . ? C9 C10 C11 C28 167.2(2) . . . . ? C25 C10 C11 C12 179.0(2) . . . . ? C9 C10 C11 C12 -7.8(3) . . . . ? C58 O2 C12 N6 -173.5(2) . . . . ? C58 O2 C12 N5 66.6(3) . . . . ? C58 O2 C12 C11 -49.7(3) . . . . ? C13 N6 C12 O2 -73.0(3) . . . . ? C13 N6 C12 N5 46.9(3) . . . . ? C13 N6 C12 C11 161.5(2) . . . . ? C9 N5 C12 O2 -127.1(2) . . . . ? Ni1 N5 C12 O2 51.6(3) . . . . ? C9 N5 C12 N6 116.7(2) . . . . ? Ni1 N5 C12 N6 -64.7(3) . . . . ? C9 N5 C12 C11 -3.7(3) . . . . ? Ni1 N5 C12 C11 174.98(16) . . . . ? C28 C11 C12 O2 -46.5(4) . . . . ? C10 C11 C12 O2 127.9(2) . . . . ? C28 C11 C12 N6 73.3(4) . . . . ? C10 C11 C12 N6 -112.2(2) . . . . ? C28 C11 C12 N5 -167.3(3) . . . . ? C10 C11 C12 N5 7.2(3) . . . . ? C12 N6 C13 N7 -5.0(4) . . . . ? C12 N6 C13 C14 172.5(2) . . . . ? C16 N7 C13 N6 176.0(2) . . . . ? Ni1 N7 C13 N6 -23.4(4) . . . . ? C16 N7 C13 C14 -1.9(3) . . . . ? Ni1 N7 C13 C14 158.76(17) . . . . ? N6 C13 C14 C41 -3.2(5) . . . . ? N7 C13 C14 C41 174.7(3) . . . . ? N6 C13 C14 C15 -176.5(2) . . . . ? N7 C13 C14 C15 1.4(3) . . . . ? C41 C14 C15 C44 2.7(4) . . . . ? C13 C14 C15 C44 176.9(2) . . . . ? C41 C14 C15 C16 -174.5(2) . . . . ? C13 C14 C15 C16 -0.4(3) . . . . ? C1 N8 C16 N7 -1.0(4) . . . . ? C1 N8 C16 C15 -179.2(2) . . . . ? C13 N7 C16 N8 -176.7(3) . . . . ? Ni1 N7 C16 N8 22.2(4) . . . . ? C13 N7 C16 C15 1.7(3) . . . . ? Ni1 N7 C16 C15 -159.42(17) . . . . ? C44 C15 C16 N8 0.8(4) . . . . ? C14 C15 C16 N8 177.7(2) . . . . ? C44 C15 C16 N7 -177.7(3) . . . . ? C14 C15 C16 N7 -0.8(3) . . . . ? C11 C10 C25 C26 2.4(4) . . . . ? C9 C10 C25 C26 -169.0(3) . . . . ? C11 C10 C25 C29 -174.9(3) . . . . ? C9 C10 C25 C29 13.7(5) . . . . ? C10 C25 C26 C27 1.3(4) . . . . ? C29 C25 C26 C27 178.8(3) . . . . ? C25 C26 C27 C28 -1.8(5) . . . . ? C10 C11 C28 C27 5.2(4) . . . . ? C12 C11 C28 C27 179.0(3) . . . . ? C10 C11 C28 C35 -167.8(3) . . . . ? C12 C11 C28 C35 6.0(5) . . . . ? C26 C27 C28 C11 -1.5(4) . . . . ? C26 C27 C28 C35 172.0(3) . . . . ? C10 C25 C29 C30 54.3(4) . . . . ? C26 C25 C29 C30 -122.9(3) . . . . ? C10 C25 C29 C34 -128.6(3) . . . . ? C26 C25 C29 C34 54.2(4) . . . . ? C34 C29 C30 C31 1.7(5) . . . . ? C25 C29 C30 C31 178.8(3) . . . . ? C29 C30 C31 C32 -0.2(5) . . . . ? C30 C31 C32 C33 -1.3(6) . . . . ? C31 C32 C33 C34 1.2(6) . . . . ? C32 C33 C34 C29 0.3(5) . . . . ? C30 C29 C34 C33 -1.8(5) . . . . ? C25 C29 C34 C33 -178.9(3) . . . . ? C11 C28 C35 C40 -49.3(4) . . . . ? C27 C28 C35 C40 137.9(3) . . . . ? C11 C28 C35 C36 130.0(3) . . . . ? C27 C28 C35 C36 -42.8(4) . . . . ? C40 C35 C36 C37 -0.2(5) . . . . ? C28 C35 C36 C37 -179.5(3) . . . . ? C35 C36 C37 C38 0.7(5) . . . . ? C36 C37 C38 C39 -0.7(6) . . . . ? C37 C38 C39 C40 0.2(5) . . . . ? C38 C39 C40 C35 0.3(5) . . . . ? C36 C35 C40 C39 -0.3(4) . . . . ? C28 C35 C40 C39 179.0(3) . . . . ? C15 C14 C41 C42 -4.9(4) . . . . ? C13 C14 C41 C42 -177.4(3) . . . . ? C15 C14 C41 C45 169.2(3) . . . . ? C13 C14 C41 C45 -3.2(5) . . . . ? C14 C41 C42 C43 3.1(5) . . . . ? C45 C41 C42 C43 -171.6(3) . . . . ? C41 C42 C43 C44 1.3(5) . . . . ? C42 C43 C44 C15 -3.6(5) . . . . ? C42 C43 C44 C51 174.3(3) . . . . ? C14 C15 C44 C43 1.7(4) . . . . ? C16 C15 C44 C43 178.2(3) . . . . ? C14 C15 C44 C51 -176.0(3) . . . . ? C16 C15 C44 C51 0.5(5) . . . . ? C14 C41 C45 C46 67.5(4) . . . . ? C42 C41 C45 C46 -118.5(3) . . . . ? C14 C41 C45 C50 -113.9(3) . . . . ? C42 C41 C45 C50 60.1(4) . . . . ? C50 C45 C46 C47 1.0(5) . . . . ? C41 C45 C46 C47 179.5(3) . . . . ? C45 C46 C47 C48 -0.9(5) . . . . ? C46 C47 C48 C49 0.2(6) . . . . ? C47 C48 C49 C50 0.4(6) . . . . ? C48 C49 C50 C45 -0.4(6) . . . . ? C46 C45 C50 C49 -0.3(5) . . . . ? C41 C45 C50 C49 -179.0(3) . . . . ? C43 C44 C51 C52 -92.6(4) . . . . ? C15 C44 C51 C52 85.0(4) . . . . ? C43 C44 C51 C56 82.7(4) . . . . ? C15 C44 C51 C56 -99.7(3) . . . . ? C56 C51 C52 C53 0.5(5) . . . . ? C44 C51 C52 C53 175.8(3) . . . . ? C51 C52 C53 C54 -0.1(6) . . . . ? C52 C53 C54 C55 0.0(6) . . . . ? C53 C54 C55 C56 -0.5(6) . . . . ? C52 C51 C56 C55 -0.9(5) . . . . ? C44 C51 C56 C55 -176.2(3) . . . . ? C54 C55 C56 C51 0.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.670 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.053 #===END