# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dennis P. Arnold' _publ_contact_author_address ; Synthesis and Molecular Recognition Program, School of Physical and Chemical Sciences, Queensland University of Technology, G.P.O. Box 2434, Brisbane, 4001, Australia ; _publ_contact_author_phone 0061-7-38641804 _publ_contact_author_fax 0061-7-38642482 _publ_contact_author_email d.arnold@qut.edu.au loop_ _publ_author_name 'Louisa J. Esdaile' D.P.Arnold M.Senge _publ_section_title ; New palladium catalysed reactions of bromoporphyrins: synthesis and crystal structures of nickel(II) complexes of primary 5-aminoporphyrin, 5,5'-bis(porphyrinyl) secondary amine, and 5-hydroxyporphyrin ; # ---------------------------------------------------------------------------- _publ_contact_letter ; 05/28/06 Deposition of the following data sets for a paper to be submitted to the journal "Chemical Communications". Please send me the CCDC deposition numbers for inclusion in the manuscript. Cheers Mathias ; #============================================================================ data_ms467 _database_code_depnum_ccdc_archive 'CCDC 610308' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[(10,15,20-triphenylporphyrinato-5-yl)nickel(II)]amine ; _chemical_name_common Bis((10,15,20-triphenylporphyrinato-5-yl)nickel(ii))amine _chemical_melting_point n/d _chemical_formula_moiety 'C76 H47 N9 Ni2' _chemical_formula_sum 'C76 H47 N9 Ni2' _chemical_formula_weight 1203.65 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4790(9) _cell_length_b 14.1516(9) _cell_length_c 16.1406(11) _cell_angle_alpha 101.5380(10) _cell_angle_beta 99.8540(10) _cell_angle_gamma 95.8160(10) _cell_volume 2724.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 3073 _cell_measurement_theta_min 4.773 _cell_measurement_theta_max 44.332 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas n/d _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details 'program SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APex2' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 27815 _diffrn_reflns_av_R_equivalents 0.0790 _diffrn_reflns_av_sigmaI/netI 0.1172 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.12 _reflns_number_total 10802 _reflns_number_gt 5743 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 v1.0-27 (Bruker, 2005' _computing_cell_refinement 'SAINT v7.12 (Bruke, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXL; Platon (Spek, 2003)' _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. N-H hydrogen atom was located in difference map. ; _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^)+(0.0691P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10802 _refine_ls_number_parameters 784 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1354 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1489 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _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 0.41363(5) 0.23703(4) 0.16741(4) 0.03018(17) Uani 1 1 d . . . N21 N 0.4076(3) 0.2719(2) 0.2862(2) 0.0296(9) Uani 1 1 d . . . N22 N 0.5251(3) 0.1585(2) 0.1946(2) 0.0308(9) Uani 1 1 d . . . N23 N 0.4261(3) 0.2090(2) 0.0490(2) 0.0319(9) Uani 1 1 d . . . N24 N 0.2952(3) 0.3070(2) 0.1406(2) 0.0311(9) Uani 1 1 d . . . C1 C 0.3685(4) 0.3531(3) 0.3275(3) 0.0302(11) Uani 1 1 d . . . C2 C 0.3895(4) 0.3591(3) 0.4172(3) 0.0325(11) Uani 1 1 d . . . H2 H 0.3757 0.4104 0.4601 0.039 Uiso 1 1 calc R . . C3 C 0.4331(4) 0.2780(3) 0.4311(3) 0.0356(12) Uani 1 1 d . . . H3 H 0.4513 0.2602 0.4849 0.043 Uiso 1 1 calc R . . C4 C 0.4460(4) 0.2256(3) 0.3505(3) 0.0309(11) Uani 1 1 d . . . C5 C 0.4955(4) 0.1397(3) 0.3360(3) 0.0351(12) Uani 1 1 d . . . C6 C 0.5443(4) 0.1169(3) 0.2654(3) 0.0320(11) Uani 1 1 d . . . C7 C 0.6310(4) 0.0586(3) 0.2573(3) 0.0379(12) Uani 1 1 d . . . H7 H 0.6577 0.0196 0.2956 0.045 Uiso 1 1 calc R . . C8 C 0.6675(4) 0.0694(3) 0.1853(3) 0.0373(12) Uani 1 1 d . . . H8 H 0.7274 0.0422 0.1653 0.045 Uiso 1 1 calc R . . C9 C 0.5999(4) 0.1291(3) 0.1448(3) 0.0324(11) Uani 1 1 d . . . C10 C 0.6011(4) 0.1424(3) 0.0622(3) 0.0345(11) Uani 1 1 d . . . C11 C 0.5135(4) 0.1734(3) 0.0154(3) 0.0340(11) Uani 1 1 d . . . C12 C 0.4917(4) 0.1612(3) -0.0756(3) 0.0394(12) Uani 1 1 d . . . H12 H 0.5396 0.1400 -0.1132 0.047 Uiso 1 1 calc R . . C13 C 0.3909(4) 0.1850(3) -0.0990(3) 0.0424(13) Uani 1 1 d . . . H13 H 0.3531 0.1809 -0.1562 0.051 Uiso 1 1 calc R . . C14 C 0.3515(4) 0.2173(3) -0.0218(3) 0.0347(11) Uani 1 1 d . . . C15 C 0.2539(4) 0.2549(3) -0.0181(3) 0.0333(11) Uani 1 1 d . . . C16 C 0.2314(4) 0.3011(3) 0.0599(3) 0.0341(11) Uani 1 1 d . . . C17 C 0.1479(4) 0.3631(4) 0.0689(3) 0.0424(13) Uani 1 1 d . . . H17 H 0.0902 0.3690 0.0242 0.051 Uiso 1 1 calc R . . C18 C 0.1654(4) 0.4107(3) 0.1507(3) 0.0399(12) Uani 1 1 d . . . H18 H 0.1246 0.4590 0.1741 0.048 Uiso 1 1 calc R . . C19 C 0.2561(4) 0.3770(3) 0.1975(3) 0.0315(11) Uani 1 1 d . . . C20 C 0.2977(4) 0.4063(3) 0.2853(3) 0.0310(11) Uani 1 1 d . . . N1 N 0.5042(3) 0.0881(3) 0.4009(2) 0.0404(10) Uani 1 1 d . . . H1A H 0.4902 0.1162 0.4509 0.048 Uiso 1 1 calc R . . Ni2 Ni 0.61694(5) -0.23233(4) 0.36569(4) 0.02999(17) Uani 1 1 d . . . N25 N 0.4941(3) -0.1776(2) 0.3101(2) 0.0312(9) Uani 1 1 d . . . N26 N 0.6662(3) -0.1078(2) 0.4484(2) 0.0340(9) Uani 1 1 d . . . N27 N 0.7354(3) -0.2884(2) 0.4261(2) 0.0307(9) Uani 1 1 d . . . N28 N 0.5707(3) -0.3551(2) 0.2813(2) 0.0292(9) Uani 1 1 d . . . C21 C 0.4111(4) -0.2250(3) 0.2420(3) 0.0341(11) Uani 1 1 d . . . C22 C 0.3342(4) -0.1594(3) 0.2212(3) 0.0378(12) Uani 1 1 d . . . H22 H 0.2699 -0.1748 0.1773 0.045 Uiso 1 1 calc R . . C23 C 0.3706(4) -0.0731(3) 0.2752(3) 0.0372(12) Uani 1 1 d . . . H23 H 0.3370 -0.0156 0.2767 0.045 Uiso 1 1 calc R . . C24 C 0.4693(4) -0.0833(3) 0.3302(3) 0.0341(11) Uani 1 1 d . . . C25 C 0.5347(4) -0.0085(3) 0.3918(3) 0.0359(12) Uani 1 1 d . . . C26 C 0.6264(4) -0.0193(3) 0.4471(3) 0.0346(12) Uani 1 1 d . . . C27 C 0.6903(4) 0.0555(3) 0.5130(3) 0.0407(12) Uani 1 1 d . . . H27 H 0.6811 0.1223 0.5233 0.049 Uiso 1 1 calc R . . C28 C 0.7666(4) 0.0159(3) 0.5588(3) 0.0425(13) Uani 1 1 d . . . H28 H 0.8194 0.0488 0.6086 0.051 Uiso 1 1 calc R . . C29 C 0.7532(4) -0.0852(3) 0.5183(3) 0.0346(11) Uani 1 1 d . . . C30 C 0.8181(4) -0.1508(3) 0.5473(3) 0.0368(12) Uani 1 1 d . . . C31 C 0.8092(4) -0.2451(3) 0.5019(3) 0.0343(11) Uani 1 1 d . . . C32 C 0.8794(4) -0.3138(3) 0.5259(3) 0.0379(12) Uani 1 1 d . . . H32 H 0.9366 -0.3021 0.5753 0.046 Uiso 1 1 calc R . . C33 C 0.8501(4) -0.3964(3) 0.4669(3) 0.0365(12) Uani 1 1 d . . . H33 H 0.8824 -0.4545 0.4662 0.044 Uiso 1 1 calc R . . C34 C 0.7611(4) -0.3820(3) 0.4047(3) 0.0310(11) Uani 1 1 d . . . C35 C 0.7078(4) -0.4545(3) 0.3340(3) 0.0301(11) Uani 1 1 d . . . C36 C 0.6194(4) -0.4400(3) 0.2767(3) 0.0304(11) Uani 1 1 d . . . C37 C 0.5605(4) -0.5147(3) 0.2054(3) 0.0357(12) Uani 1 1 d . . . H37 H 0.5780 -0.5786 0.1885 0.043 Uiso 1 1 calc R . . C38 C 0.4759(4) -0.4775(3) 0.1672(3) 0.0349(11) Uani 1 1 d . . . H38 H 0.4217 -0.5105 0.1184 0.042 Uiso 1 1 calc R . . C39 C 0.4820(4) -0.3791(3) 0.2131(3) 0.0296(10) Uani 1 1 d . . . C40 C 0.4041(4) -0.3185(3) 0.1945(3) 0.0301(11) Uani 1 1 d . . . C101 C 0.6926(4) 0.1110(3) 0.0216(3) 0.0337(11) Uani 1 1 d . . . C102 C 0.6811(4) 0.0216(3) -0.0371(3) 0.0453(13) Uani 1 1 d . . . H102 H 0.6123 -0.0192 -0.0531 0.054 Uiso 1 1 calc R . . C103 C 0.7702(4) -0.0078(3) -0.0721(3) 0.0418(13) Uani 1 1 d . . . H103 H 0.7620 -0.0692 -0.1110 0.050 Uiso 1 1 calc R . . C104 C 0.8679(4) 0.0502(3) -0.0511(3) 0.0423(13) Uani 1 1 d . . . H104 H 0.9286 0.0300 -0.0749 0.051 Uiso 1 1 calc R . . C105 C 0.8786(4) 0.1398(4) 0.0057(3) 0.0510(14) Uani 1 1 d . . . H105 H 0.9467 0.1817 0.0199 0.061 Uiso 1 1 calc R . . C106 C 0.7916(4) 0.1686(3) 0.0417(3) 0.0426(13) Uani 1 1 d . . . H106 H 0.8008 0.2298 0.0811 0.051 Uiso 1 1 calc R . . C151 C 0.1747(4) 0.2528(3) -0.0988(3) 0.0360(12) Uani 1 1 d . . . C152 C 0.0764(4) 0.1959(4) -0.1155(3) 0.0444(13) Uani 1 1 d . . . H152 H 0.0603 0.1575 -0.0760 0.053 Uiso 1 1 calc R . . C153 C -0.0025(5) 0.1921(4) -0.1898(4) 0.0540(15) Uani 1 1 d . . . H153 H -0.0717 0.1527 -0.1998 0.065 Uiso 1 1 calc R . . C154 C 0.0213(5) 0.2453(4) -0.2474(3) 0.0486(14) Uani 1 1 d . . . H154 H -0.0312 0.2431 -0.2982 0.058 Uiso 1 1 calc R . . C155 C 0.1211(5) 0.3018(4) -0.2319(4) 0.0576(16) Uani 1 1 d . . . H155 H 0.1380 0.3380 -0.2728 0.069 Uiso 1 1 calc R . . C156 C 0.1979(5) 0.3072(4) -0.1579(3) 0.0512(14) Uani 1 1 d . . . H156 H 0.2663 0.3480 -0.1474 0.061 Uiso 1 1 calc R . . C201 C 0.2615(4) 0.4932(3) 0.3350(3) 0.0312(11) Uani 1 1 d . . . C202 C 0.1524(4) 0.4945(3) 0.3439(3) 0.0429(13) Uani 1 1 d . . . H202 H 0.1009 0.4370 0.3211 0.051 Uiso 1 1 calc R . . C203 C 0.1180(4) 0.5780(4) 0.3854(3) 0.0484(14) Uani 1 1 d . . . H203 H 0.0434 0.5782 0.3907 0.058 Uiso 1 1 calc R . . C204 C 0.1934(5) 0.6607(4) 0.4190(3) 0.0538(15) Uani 1 1 d . . . H204 H 0.1706 0.7185 0.4476 0.065 Uiso 1 1 calc R . . C205 C 0.3007(5) 0.6601(3) 0.4113(3) 0.0511(14) Uani 1 1 d . . . H205 H 0.3521 0.7175 0.4341 0.061 Uiso 1 1 calc R . . C206 C 0.3343(4) 0.5765(3) 0.3705(3) 0.0406(12) Uani 1 1 d . . . H206 H 0.4095 0.5766 0.3669 0.049 Uiso 1 1 calc R . . C301 C 0.8965(4) -0.1200(3) 0.6325(3) 0.0392(12) Uani 1 1 d . . . C302 C 0.9909(4) -0.0550(3) 0.6425(4) 0.0458(13) Uani 1 1 d . . . H302 H 1.0080 -0.0305 0.5950 0.055 Uiso 1 1 calc R . . C303 C 1.0607(4) -0.0260(3) 0.7233(4) 0.0471(14) Uani 1 1 d . . . H303 H 1.1248 0.0198 0.7314 0.057 Uiso 1 1 calc R . . C304 C 1.0362(4) -0.0642(4) 0.7920(4) 0.0495(14) Uani 1 1 d . . . H304 H 1.0837 -0.0440 0.8469 0.059 Uiso 1 1 calc R . . C305 C 0.9430(4) -0.1315(4) 0.7812(3) 0.0436(13) Uani 1 1 d . . . H305 H 0.9282 -0.1593 0.8277 0.052 Uiso 1 1 calc R . . C306 C 0.8723(4) -0.1574(3) 0.7022(3) 0.0391(12) Uani 1 1 d . . . H306 H 0.8066 -0.2010 0.6951 0.047 Uiso 1 1 calc R . . C351 C 0.7505(4) -0.5508(3) 0.3209(3) 0.0349(11) Uani 1 1 d . . . C352 C 0.7142(4) -0.6217(3) 0.3608(3) 0.0436(13) Uani 1 1 d . . . H352 H 0.6582 -0.6116 0.3935 0.052 Uiso 1 1 calc R . . C353 C 0.7591(5) -0.7077(4) 0.3533(4) 0.0520(15) Uani 1 1 d . . . H353 H 0.7356 -0.7558 0.3823 0.062 Uiso 1 1 calc R . . C354 C 0.8373(5) -0.7235(4) 0.3041(4) 0.0516(15) Uani 1 1 d . . . H354 H 0.8667 -0.7833 0.2982 0.062 Uiso 1 1 calc R . . C355 C 0.8732(4) -0.6551(4) 0.2638(3) 0.0478(14) Uani 1 1 d . . . H355 H 0.9277 -0.6666 0.2300 0.057 Uiso 1 1 calc R . . C356 C 0.8301(4) -0.5681(4) 0.2722(3) 0.0434(13) Uani 1 1 d . . . H356 H 0.8556 -0.5198 0.2442 0.052 Uiso 1 1 calc R . . C401 C 0.3124(4) -0.3557(3) 0.1188(3) 0.0379(12) Uani 1 1 d . . . C402 C 0.2044(4) -0.3612(3) 0.1303(4) 0.0424(13) Uani 1 1 d . . . H402 H 0.1897 -0.3432 0.1868 0.051 Uiso 1 1 calc R . . C403 C 0.1189(5) -0.3923(4) 0.0615(4) 0.0540(15) Uani 1 1 d . . . H403 H 0.0454 -0.3940 0.0702 0.065 Uiso 1 1 calc R . . C404 C 0.1392(5) -0.4212(4) -0.0202(4) 0.0550(16) Uani 1 1 d . . . H404 H 0.0794 -0.4440 -0.0676 0.066 Uiso 1 1 calc R . . C405 C 0.2463(5) -0.4174(4) -0.0341(4) 0.0508(14) Uani 1 1 d . . . H405 H 0.2601 -0.4374 -0.0906 0.061 Uiso 1 1 calc R . . C406 C 0.3336(4) -0.3837(3) 0.0364(3) 0.0399(12) Uani 1 1 d . . . H406 H 0.4072 -0.3801 0.0278 0.048 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 0.0325(4) 0.0232(3) 0.0358(4) 0.0068(3) 0.0042(3) 0.0123(3) N21 0.029(2) 0.0243(19) 0.036(2) 0.0064(17) 0.0020(18) 0.0121(16) N22 0.028(2) 0.027(2) 0.038(2) 0.0085(18) 0.0033(19) 0.0089(17) N23 0.036(2) 0.024(2) 0.038(2) 0.0098(18) 0.0099(19) 0.0110(17) N24 0.034(2) 0.027(2) 0.036(2) 0.0088(18) 0.0070(19) 0.0116(17) C1 0.031(3) 0.022(2) 0.034(3) 0.000(2) 0.001(2) 0.0112(19) C2 0.035(3) 0.028(2) 0.034(3) 0.002(2) 0.005(2) 0.014(2) C3 0.038(3) 0.032(3) 0.038(3) 0.011(2) 0.001(2) 0.016(2) C4 0.031(3) 0.030(2) 0.033(3) 0.007(2) 0.003(2) 0.015(2) C5 0.039(3) 0.031(3) 0.037(3) 0.010(2) 0.001(2) 0.016(2) C6 0.034(3) 0.028(2) 0.037(3) 0.009(2) 0.007(2) 0.014(2) C7 0.041(3) 0.037(3) 0.041(3) 0.013(2) 0.010(3) 0.020(2) C8 0.037(3) 0.029(3) 0.045(3) 0.003(2) 0.005(2) 0.017(2) C9 0.032(3) 0.023(2) 0.042(3) 0.003(2) 0.008(2) 0.008(2) C10 0.039(3) 0.021(2) 0.044(3) 0.006(2) 0.009(2) 0.010(2) C11 0.037(3) 0.025(2) 0.043(3) 0.008(2) 0.014(2) 0.007(2) C12 0.047(3) 0.034(3) 0.044(3) 0.013(2) 0.017(3) 0.015(2) C13 0.051(3) 0.040(3) 0.040(3) 0.012(2) 0.010(3) 0.016(2) C14 0.043(3) 0.024(2) 0.040(3) 0.009(2) 0.008(2) 0.013(2) C15 0.047(3) 0.021(2) 0.033(3) 0.006(2) 0.004(2) 0.011(2) C16 0.032(3) 0.030(3) 0.043(3) 0.014(2) 0.007(2) 0.008(2) C17 0.039(3) 0.049(3) 0.042(3) 0.014(3) 0.001(3) 0.021(2) C18 0.045(3) 0.038(3) 0.040(3) 0.009(2) 0.008(3) 0.022(2) C19 0.038(3) 0.023(2) 0.036(3) 0.006(2) 0.011(2) 0.011(2) C20 0.030(3) 0.023(2) 0.044(3) 0.010(2) 0.010(2) 0.010(2) N1 0.058(3) 0.033(2) 0.036(2) 0.0074(19) 0.008(2) 0.032(2) Ni2 0.0340(4) 0.0231(3) 0.0338(4) 0.0074(3) 0.0025(3) 0.0132(3) N25 0.040(2) 0.0223(19) 0.032(2) 0.0093(17) 0.0015(19) 0.0114(17) N26 0.039(2) 0.026(2) 0.038(2) 0.0079(18) 0.002(2) 0.0181(17) N27 0.032(2) 0.0241(19) 0.036(2) 0.0038(17) 0.0053(19) 0.0132(17) N28 0.031(2) 0.030(2) 0.030(2) 0.0104(17) 0.0056(18) 0.0132(17) C21 0.034(3) 0.033(3) 0.040(3) 0.017(2) 0.007(2) 0.013(2) C22 0.033(3) 0.038(3) 0.044(3) 0.011(2) 0.002(2) 0.012(2) C23 0.042(3) 0.034(3) 0.041(3) 0.015(2) 0.007(2) 0.020(2) C24 0.041(3) 0.027(2) 0.037(3) 0.012(2) 0.003(2) 0.018(2) C25 0.046(3) 0.027(3) 0.039(3) 0.012(2) 0.006(2) 0.021(2) C26 0.044(3) 0.025(2) 0.036(3) 0.007(2) 0.004(2) 0.016(2) C27 0.044(3) 0.025(2) 0.050(3) 0.006(2) 0.002(3) 0.013(2) C28 0.047(3) 0.030(3) 0.044(3) -0.001(2) -0.004(3) 0.013(2) C29 0.032(3) 0.028(2) 0.040(3) 0.000(2) 0.000(2) 0.012(2) C30 0.038(3) 0.027(3) 0.042(3) 0.003(2) 0.002(2) 0.012(2) C31 0.036(3) 0.031(3) 0.034(3) 0.006(2) 0.002(2) 0.011(2) C32 0.035(3) 0.041(3) 0.032(3) -0.002(2) -0.003(2) 0.017(2) C33 0.044(3) 0.032(3) 0.034(3) 0.007(2) 0.002(2) 0.016(2) C34 0.034(3) 0.029(2) 0.032(3) 0.008(2) 0.006(2) 0.015(2) C35 0.036(3) 0.027(2) 0.028(3) 0.004(2) 0.006(2) 0.015(2) C36 0.035(3) 0.025(2) 0.033(3) 0.007(2) 0.009(2) 0.011(2) C37 0.039(3) 0.026(2) 0.042(3) 0.004(2) 0.009(2) 0.014(2) C38 0.034(3) 0.027(2) 0.041(3) 0.006(2) 0.002(2) 0.004(2) C39 0.030(3) 0.030(2) 0.029(3) 0.007(2) 0.005(2) 0.006(2) C40 0.027(3) 0.030(2) 0.033(3) 0.010(2) 0.001(2) 0.007(2) C101 0.032(3) 0.028(3) 0.043(3) 0.012(2) 0.007(2) 0.006(2) C102 0.043(3) 0.025(3) 0.065(4) 0.002(2) 0.015(3) 0.005(2) C103 0.042(3) 0.026(3) 0.059(4) 0.003(2) 0.020(3) 0.012(2) C104 0.044(3) 0.040(3) 0.049(3) 0.009(3) 0.019(3) 0.019(3) C105 0.039(3) 0.051(3) 0.055(4) -0.003(3) 0.011(3) -0.002(3) C106 0.047(3) 0.031(3) 0.045(3) -0.002(2) 0.008(3) 0.006(2) C151 0.039(3) 0.032(3) 0.041(3) 0.009(2) 0.010(2) 0.016(2) C152 0.050(4) 0.043(3) 0.040(3) 0.010(3) 0.004(3) 0.009(3) C153 0.052(4) 0.053(3) 0.058(4) 0.013(3) 0.004(3) 0.017(3) C154 0.059(4) 0.055(3) 0.034(3) 0.011(3) 0.002(3) 0.029(3) C155 0.064(4) 0.060(4) 0.055(4) 0.028(3) 0.004(3) 0.018(3) C156 0.058(4) 0.044(3) 0.054(4) 0.018(3) 0.008(3) 0.010(3) C201 0.035(3) 0.026(2) 0.035(3) 0.007(2) 0.006(2) 0.015(2) C202 0.049(3) 0.036(3) 0.048(3) 0.012(2) 0.013(3) 0.016(2) C203 0.045(3) 0.056(4) 0.053(3) 0.016(3) 0.017(3) 0.031(3) C204 0.066(4) 0.039(3) 0.055(4) 0.003(3) 0.005(3) 0.029(3) C205 0.050(4) 0.029(3) 0.067(4) -0.003(3) 0.003(3) 0.014(2) C206 0.044(3) 0.033(3) 0.044(3) 0.003(2) 0.007(3) 0.017(2) C301 0.035(3) 0.028(3) 0.052(3) 0.003(2) 0.000(3) 0.018(2) C302 0.045(3) 0.030(3) 0.057(4) 0.003(2) -0.003(3) 0.014(2) C303 0.042(3) 0.033(3) 0.061(4) 0.005(3) -0.005(3) 0.016(2) C304 0.048(4) 0.045(3) 0.047(3) -0.003(3) -0.004(3) 0.019(3) C305 0.041(3) 0.042(3) 0.049(3) 0.008(3) 0.007(3) 0.016(3) C306 0.038(3) 0.031(3) 0.044(3) -0.002(2) 0.005(3) 0.012(2) C351 0.038(3) 0.030(3) 0.033(3) 0.003(2) -0.004(2) 0.012(2) C352 0.050(3) 0.030(3) 0.053(3) 0.008(2) 0.014(3) 0.013(2) C353 0.063(4) 0.029(3) 0.060(4) 0.005(3) 0.003(3) 0.014(3) C354 0.055(4) 0.035(3) 0.053(4) -0.008(3) -0.010(3) 0.018(3) C355 0.040(3) 0.039(3) 0.054(4) -0.012(3) 0.001(3) 0.015(2) C356 0.042(3) 0.042(3) 0.044(3) 0.004(2) 0.007(3) 0.013(2) C401 0.041(3) 0.028(3) 0.047(3) 0.013(2) 0.005(3) 0.010(2) C402 0.036(3) 0.034(3) 0.056(3) 0.013(3) -0.001(3) 0.008(2) C403 0.040(3) 0.049(3) 0.072(4) 0.025(3) -0.004(3) 0.004(3) C404 0.043(4) 0.047(3) 0.066(4) 0.021(3) -0.019(3) 0.001(3) C405 0.060(4) 0.040(3) 0.048(3) 0.011(3) -0.005(3) 0.014(3) C406 0.037(3) 0.037(3) 0.044(3) 0.011(2) -0.004(3) 0.010(2) _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 N24 1.898(3) . ? Ni1 N21 1.898(4) . ? Ni1 N23 1.909(4) . ? Ni1 N22 1.914(3) . ? N21 C4 1.380(5) . ? N21 C1 1.386(5) . ? N22 C9 1.375(5) . ? N22 C6 1.383(5) . ? N23 C14 1.378(5) . ? N23 C11 1.393(5) . ? N24 C16 1.388(5) . ? N24 C19 1.397(5) . ? C1 C20 1.395(5) . ? C1 C2 1.409(6) . ? C2 C3 1.360(5) . ? C2 H2 0.9500 . ? C3 C4 1.406(6) . ? C3 H3 0.9500 . ? C4 C5 1.415(6) . ? C5 C6 1.381(6) . ? C5 N1 1.387(5) . ? C6 C7 1.432(6) . ? C7 C8 1.349(6) . ? C7 H7 0.9500 . ? C8 C9 1.424(6) . ? C8 H8 0.9500 . ? C9 C10 1.386(6) . ? C10 C11 1.380(6) . ? C10 C101 1.474(6) . ? C11 C12 1.419(6) . ? C12 C13 1.346(6) . ? C12 H12 0.9500 . ? C13 C14 1.425(6) . ? C13 H13 0.9500 . ? C14 C15 1.384(6) . ? C15 C16 1.385(6) . ? C15 C151 1.487(6) . ? C16 C17 1.437(6) . ? C17 C18 1.326(6) . ? C17 H17 0.9500 . ? C18 C19 1.428(6) . ? C18 H18 0.9500 . ? C19 C20 1.386(6) . ? C20 C201 1.484(6) . ? N1 C25 1.443(5) . ? N1 H1A 0.8800 . ? Ni2 N28 1.946(4) . ? Ni2 N25 1.951(3) . ? Ni2 N27 1.955(3) . ? Ni2 N26 1.956(4) . ? N25 C21 1.380(6) . ? N25 C24 1.387(5) . ? N26 C29 1.385(5) . ? N26 C26 1.396(5) . ? N27 C34 1.385(5) . ? N27 C31 1.385(6) . ? N28 C39 1.382(5) . ? N28 C36 1.395(5) . ? C21 C40 1.376(6) . ? C21 C22 1.446(6) . ? C22 C23 1.335(6) . ? C22 H22 0.9500 . ? C23 C24 1.429(6) . ? C23 H23 0.9500 . ? C24 C25 1.379(6) . ? C25 C26 1.368(6) . ? C26 C27 1.405(6) . ? C27 C28 1.341(6) . ? C27 H27 0.9500 . ? C28 C29 1.429(6) . ? C28 H28 0.9500 . ? C29 C30 1.392(6) . ? C30 C31 1.372(6) . ? C30 C301 1.501(6) . ? C31 C32 1.439(6) . ? C32 C33 1.325(6) . ? C32 H32 0.9500 . ? C33 C34 1.423(6) . ? C33 H33 0.9500 . ? C34 C35 1.389(6) . ? C35 C36 1.374(6) . ? C35 C351 1.502(6) . ? C36 C37 1.431(6) . ? C37 C38 1.339(6) . ? C37 H37 0.9500 . ? C38 C39 1.429(6) . ? C38 H38 0.9500 . ? C39 C40 1.394(6) . ? C40 C401 1.491(6) . ? C101 C106 1.359(6) . ? C101 C102 1.398(6) . ? C102 C103 1.394(6) . ? C102 H102 0.9500 . ? C103 C104 1.349(7) . ? C103 H103 0.9500 . ? C104 C105 1.387(7) . ? C104 H104 0.9500 . ? C105 C106 1.376(7) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C151 C152 1.351(6) . ? C151 C156 1.389(6) . ? C152 C153 1.404(7) . ? C152 H152 0.9500 . ? C153 C154 1.360(7) . ? C153 H153 0.9500 . ? C154 C155 1.365(7) . ? C154 H154 0.9500 . ? C155 C156 1.381(7) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? C201 C206 1.371(6) . ? C201 C202 1.394(6) . ? C202 C203 1.384(6) . ? C202 H202 0.9500 . ? C203 C204 1.378(7) . ? C203 H203 0.9500 . ? C204 C205 1.366(7) . ? C204 H204 0.9500 . ? C205 C206 1.375(6) . ? C205 H205 0.9500 . ? C206 H206 0.9500 . ? C301 C302 1.384(7) . ? C301 C306 1.400(6) . ? C302 C303 1.397(7) . ? C302 H302 0.9500 . ? C303 C304 1.392(7) . ? C303 H303 0.9500 . ? C304 C305 1.389(7) . ? C304 H304 0.9500 . ? C305 C306 1.378(6) . ? C305 H305 0.9500 . ? C306 H306 0.9500 . ? C351 C352 1.377(6) . ? C351 C356 1.379(6) . ? C352 C353 1.383(6) . ? C352 H352 0.9500 . ? C353 C354 1.368(7) . ? C353 H353 0.9500 . ? C354 C355 1.351(7) . ? C354 H354 0.9500 . ? C355 C356 1.385(6) . ? C355 H355 0.9500 . ? C356 H356 0.9500 . ? C401 C402 1.388(6) . ? C401 C406 1.388(7) . ? C402 C403 1.367(7) . ? C402 H402 0.9500 . ? C403 C404 1.374(8) . ? C403 H403 0.9500 . ? C404 C405 1.391(7) . ? C404 H404 0.9500 . ? C405 C406 1.401(7) . ? C405 H405 0.9500 . ? C406 H406 0.9500 . ? 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 N24 Ni1 N21 90.09(15) . . ? N24 Ni1 N23 89.97(15) . . ? N21 Ni1 N23 176.46(16) . . ? N24 Ni1 N22 175.70(15) . . ? N21 Ni1 N22 89.37(15) . . ? N23 Ni1 N22 90.83(15) . . ? C4 N21 C1 105.2(3) . . ? C4 N21 Ni1 127.8(3) . . ? C1 N21 Ni1 126.9(3) . . ? C9 N22 C6 106.3(3) . . ? C9 N22 Ni1 126.1(3) . . ? C6 N22 Ni1 127.6(3) . . ? C14 N23 C11 104.8(4) . . ? C14 N23 Ni1 128.4(3) . . ? C11 N23 Ni1 126.8(3) . . ? C16 N24 C19 105.7(3) . . ? C16 N24 Ni1 127.1(3) . . ? C19 N24 Ni1 127.2(3) . . ? N21 C1 C20 124.0(4) . . ? N21 C1 C2 109.6(3) . . ? C20 C1 C2 124.9(4) . . ? C3 C2 C1 107.6(4) . . ? C3 C2 H2 126.2 . . ? C1 C2 H2 126.2 . . ? C2 C3 C4 106.9(4) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? N21 C4 C3 110.5(4) . . ? N21 C4 C5 123.7(4) . . ? C3 C4 C5 125.8(4) . . ? C6 C5 N1 122.6(4) . . ? C6 C5 C4 120.2(4) . . ? N1 C5 C4 116.7(4) . . ? C5 C6 N22 123.6(4) . . ? C5 C6 C7 126.9(4) . . ? N22 C6 C7 109.1(4) . . ? C8 C7 C6 107.4(4) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 107.5(4) . . ? C7 C8 H8 126.2 . . ? C9 C8 H8 126.2 . . ? N22 C9 C10 126.1(4) . . ? N22 C9 C8 109.7(4) . . ? C10 C9 C8 123.6(4) . . ? C11 C10 C9 121.2(4) . . ? C11 C10 C101 120.6(4) . . ? C9 C10 C101 117.8(4) . . ? C10 C11 N23 124.8(4) . . ? C10 C11 C12 124.7(4) . . ? N23 C11 C12 110.0(4) . . ? C13 C12 C11 107.5(4) . . ? C13 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? C12 C13 C14 107.1(4) . . ? C12 C13 H13 126.4 . . ? C14 C13 H13 126.4 . . ? N23 C14 C15 124.7(4) . . ? N23 C14 C13 110.4(4) . . ? C15 C14 C13 124.8(4) . . ? C14 C15 C16 120.9(4) . . ? C14 C15 C151 120.3(4) . . ? C16 C15 C151 118.7(4) . . ? C15 C16 N24 125.6(4) . . ? C15 C16 C17 124.8(4) . . ? N24 C16 C17 109.0(4) . . ? C18 C17 C16 107.9(4) . . ? C18 C17 H17 126.1 . . ? C16 C17 H17 126.1 . . ? C17 C18 C19 108.4(4) . . ? C17 C18 H18 125.8 . . ? C19 C18 H18 125.8 . . ? C20 C19 N24 124.9(4) . . ? C20 C19 C18 126.2(4) . . ? N24 C19 C18 108.9(4) . . ? C19 C20 C1 121.1(4) . . ? C19 C20 C201 118.8(4) . . ? C1 C20 C201 120.1(4) . . ? C5 N1 C25 124.3(4) . . ? C5 N1 H1A 117.9 . . ? C25 N1 H1A 117.9 . . ? N28 Ni2 N25 90.16(14) . . ? N28 Ni2 N27 90.38(14) . . ? N25 Ni2 N27 176.88(15) . . ? N28 Ni2 N26 178.34(16) . . ? N25 Ni2 N26 89.94(14) . . ? N27 Ni2 N26 89.62(14) . . ? C21 N25 C24 104.4(3) . . ? C21 N25 Ni2 127.3(3) . . ? C24 N25 Ni2 128.2(3) . . ? C29 N26 C26 103.9(3) . . ? C29 N26 Ni2 128.2(3) . . ? C26 N26 Ni2 127.8(3) . . ? C34 N27 C31 104.5(3) . . ? C34 N27 Ni2 127.6(3) . . ? C31 N27 Ni2 127.9(3) . . ? C39 N28 C36 103.9(3) . . ? C39 N28 Ni2 128.4(3) . . ? C36 N28 Ni2 127.6(3) . . ? C40 C21 N25 126.5(4) . . ? C40 C21 C22 123.0(4) . . ? N25 C21 C22 110.2(4) . . ? C23 C22 C21 107.2(4) . . ? C23 C22 H22 126.4 . . ? C21 C22 H22 126.4 . . ? C22 C23 C24 107.2(4) . . ? C22 C23 H23 126.4 . . ? C24 C23 H23 126.4 . . ? C25 C24 N25 124.3(4) . . ? C25 C24 C23 124.7(4) . . ? N25 C24 C23 110.8(4) . . ? C26 C25 C24 124.7(4) . . ? C26 C25 N1 116.7(4) . . ? C24 C25 N1 118.6(4) . . ? C25 C26 N26 124.2(4) . . ? C25 C26 C27 125.1(4) . . ? N26 C26 C27 110.6(4) . . ? C28 C27 C26 108.1(4) . . ? C28 C27 H27 125.9 . . ? C26 C27 H27 125.9 . . ? C27 C28 C29 106.7(4) . . ? C27 C28 H28 126.6 . . ? C29 C28 H28 126.6 . . ? N26 C29 C30 125.6(4) . . ? N26 C29 C28 110.6(4) . . ? C30 C29 C28 123.8(4) . . ? C31 C30 C29 121.8(4) . . ? C31 C30 C301 118.5(4) . . ? C29 C30 C301 119.7(4) . . ? C30 C31 N27 126.5(4) . . ? C30 C31 C32 123.9(4) . . ? N27 C31 C32 109.6(4) . . ? C33 C32 C31 107.9(4) . . ? C33 C32 H32 126.0 . . ? C31 C32 H32 126.0 . . ? C32 C33 C34 107.3(4) . . ? C32 C33 H33 126.4 . . ? C34 C33 H33 126.4 . . ? N27 C34 C35 126.1(4) . . ? N27 C34 C33 110.7(4) . . ? C35 C34 C33 123.2(4) . . ? C36 C35 C34 122.2(4) . . ? C36 C35 C351 120.0(4) . . ? C34 C35 C351 117.8(4) . . ? C35 C36 N28 126.1(4) . . ? C35 C36 C37 123.1(4) . . ? N28 C36 C37 110.6(4) . . ? C38 C37 C36 107.0(4) . . ? C38 C37 H37 126.5 . . ? C36 C37 H37 126.5 . . ? C37 C38 C39 107.5(4) . . ? C37 C38 H38 126.2 . . ? C39 C38 H38 126.2 . . ? N28 C39 C40 125.1(4) . . ? N28 C39 C38 110.9(4) . . ? C40 C39 C38 123.9(4) . . ? C21 C40 C39 122.2(4) . . ? C21 C40 C401 119.3(4) . . ? C39 C40 C401 118.5(4) . . ? C106 C101 C102 118.3(5) . . ? C106 C101 C10 120.2(4) . . ? C102 C101 C10 121.5(4) . . ? C103 C102 C101 120.3(5) . . ? C103 C102 H102 119.9 . . ? C101 C102 H102 119.9 . . ? C104 C103 C102 120.6(5) . . ? C104 C103 H103 119.7 . . ? C102 C103 H103 119.7 . . ? C103 C104 C105 119.1(5) . . ? C103 C104 H104 120.5 . . ? C105 C104 H104 120.5 . . ? C106 C105 C104 120.7(5) . . ? C106 C105 H105 119.7 . . ? C104 C105 H105 119.7 . . ? C101 C106 C105 121.1(5) . . ? C101 C106 H106 119.5 . . ? C105 C106 H106 119.5 . . ? C152 C151 C156 118.5(5) . . ? C152 C151 C15 119.0(4) . . ? C156 C151 C15 122.5(4) . . ? C151 C152 C153 121.6(5) . . ? C151 C152 H152 119.2 . . ? C153 C152 H152 119.2 . . ? C154 C153 C152 119.3(5) . . ? C154 C153 H153 120.3 . . ? C152 C153 H153 120.3 . . ? C153 C154 C155 119.6(5) . . ? C153 C154 H154 120.2 . . ? C155 C154 H154 120.2 . . ? C154 C155 C156 121.1(5) . . ? C154 C155 H155 119.4 . . ? C156 C155 H155 119.4 . . ? C155 C156 C151 119.8(5) . . ? C155 C156 H156 120.1 . . ? C151 C156 H156 120.1 . . ? C206 C201 C202 117.9(4) . . ? C206 C201 C20 120.5(4) . . ? C202 C201 C20 121.6(4) . . ? C203 C202 C201 121.1(5) . . ? C203 C202 H202 119.4 . . ? C201 C202 H202 119.4 . . ? C202 C203 C204 119.1(5) . . ? C202 C203 H203 120.4 . . ? C204 C203 H203 120.4 . . ? C205 C204 C203 120.3(5) . . ? C205 C204 H204 119.9 . . ? C203 C204 H204 119.9 . . ? C204 C205 C206 120.2(5) . . ? C204 C205 H205 119.9 . . ? C206 C205 H205 119.9 . . ? C201 C206 C205 121.4(5) . . ? C201 C206 H206 119.3 . . ? C205 C206 H206 119.3 . . ? C302 C301 C306 120.3(5) . . ? C302 C301 C30 120.7(5) . . ? C306 C301 C30 119.0(4) . . ? C301 C302 C303 119.2(5) . . ? C301 C302 H302 120.4 . . ? C303 C302 H302 120.4 . . ? C304 C303 C302 119.9(5) . . ? C304 C303 H303 120.0 . . ? C302 C303 H303 120.0 . . ? C305 C304 C303 120.7(5) . . ? C305 C304 H304 119.6 . . ? C303 C304 H304 119.6 . . ? C306 C305 C304 119.2(5) . . ? C306 C305 H305 120.4 . . ? C304 C305 H305 120.4 . . ? C305 C306 C301 120.6(5) . . ? C305 C306 H306 119.7 . . ? C301 C306 H306 119.7 . . ? C352 C351 C356 118.8(4) . . ? C352 C351 C35 120.2(4) . . ? C356 C351 C35 120.9(4) . . ? C351 C352 C353 120.0(5) . . ? C351 C352 H352 120.0 . . ? C353 C352 H352 120.0 . . ? C354 C353 C352 120.0(5) . . ? C354 C353 H353 120.0 . . ? C352 C353 H353 120.0 . . ? C355 C354 C353 120.8(5) . . ? C355 C354 H354 119.6 . . ? C353 C354 H354 119.6 . . ? C354 C355 C356 119.6(5) . . ? C354 C355 H355 120.2 . . ? C356 C355 H355 120.2 . . ? C351 C356 C355 120.7(5) . . ? C351 C356 H356 119.6 . . ? C355 C356 H356 119.6 . . ? C402 C401 C406 119.4(5) . . ? C402 C401 C40 119.9(5) . . ? C406 C401 C40 120.7(4) . . ? C403 C402 C401 120.9(5) . . ? C403 C402 H402 119.6 . . ? C401 C402 H402 119.6 . . ? C402 C403 C404 120.1(5) . . ? C402 C403 H403 119.9 . . ? C404 C403 H403 119.9 . . ? C403 C404 C405 120.6(5) . . ? C403 C404 H404 119.7 . . ? C405 C404 H404 119.7 . . ? C404 C405 C406 119.1(5) . . ? C404 C405 H405 120.4 . . ? C406 C405 H405 120.4 . . ? C401 C406 C405 119.9(5) . . ? C401 C406 H406 120.1 . . ? C405 C406 H406 120.1 . . ? 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 N24 Ni1 N21 C4 157.9(4) . . . . ? N22 Ni1 N21 C4 -17.8(4) . . . . ? N24 Ni1 N21 C1 -25.9(4) . . . . ? N22 Ni1 N21 C1 158.3(4) . . . . ? N21 Ni1 N22 C9 -158.4(4) . . . . ? N23 Ni1 N22 C9 18.0(4) . . . . ? N21 Ni1 N22 C6 24.3(4) . . . . ? N23 Ni1 N22 C6 -159.2(4) . . . . ? N24 Ni1 N23 C14 -15.4(4) . . . . ? N22 Ni1 N23 C14 160.4(4) . . . . ? N24 Ni1 N23 C11 165.9(4) . . . . ? N22 Ni1 N23 C11 -18.3(4) . . . . ? N21 Ni1 N24 C16 -165.2(4) . . . . ? N23 Ni1 N24 C16 18.3(4) . . . . ? N21 Ni1 N24 C19 16.7(4) . . . . ? N23 Ni1 N24 C19 -159.7(4) . . . . ? C4 N21 C1 C20 -162.8(4) . . . . ? Ni1 N21 C1 C20 20.4(6) . . . . ? C4 N21 C1 C2 3.6(5) . . . . ? Ni1 N21 C1 C2 -173.3(3) . . . . ? N21 C1 C2 C3 -4.9(5) . . . . ? C20 C1 C2 C3 161.3(4) . . . . ? C1 C2 C3 C4 4.1(5) . . . . ? C1 N21 C4 C3 -1.1(5) . . . . ? Ni1 N21 C4 C3 175.8(3) . . . . ? C1 N21 C4 C5 -178.6(4) . . . . ? Ni1 N21 C4 C5 -1.8(7) . . . . ? C2 C3 C4 N21 -1.9(5) . . . . ? C2 C3 C4 C5 175.6(5) . . . . ? N21 C4 C5 C6 24.0(7) . . . . ? C3 C4 C5 C6 -153.2(5) . . . . ? N21 C4 C5 N1 -163.9(4) . . . . ? C3 C4 C5 N1 18.9(7) . . . . ? N1 C5 C6 N22 171.1(4) . . . . ? C4 C5 C6 N22 -17.2(7) . . . . ? N1 C5 C6 C7 -17.5(8) . . . . ? C4 C5 C6 C7 154.1(5) . . . . ? C9 N22 C6 C5 171.1(4) . . . . ? Ni1 N22 C6 C5 -11.2(7) . . . . ? C9 N22 C6 C7 -1.6(5) . . . . ? Ni1 N22 C6 C7 176.1(3) . . . . ? C5 C6 C7 C8 -169.0(5) . . . . ? N22 C6 C7 C8 3.4(5) . . . . ? C6 C7 C8 C9 -3.7(5) . . . . ? C6 N22 C9 C10 170.6(4) . . . . ? Ni1 N22 C9 C10 -7.1(6) . . . . ? C6 N22 C9 C8 -0.7(5) . . . . ? Ni1 N22 C9 C8 -178.4(3) . . . . ? C7 C8 C9 N22 2.8(5) . . . . ? C7 C8 C9 C10 -168.7(4) . . . . ? N22 C9 C10 C11 -11.1(7) . . . . ? C8 C9 C10 C11 159.0(4) . . . . ? N22 C9 C10 C101 176.2(4) . . . . ? C8 C9 C10 C101 -13.7(7) . . . . ? C9 C10 C11 N23 10.9(7) . . . . ? C101 C10 C11 N23 -176.6(4) . . . . ? C9 C10 C11 C12 -159.9(4) . . . . ? C101 C10 C11 C12 12.6(7) . . . . ? C14 N23 C11 C10 -171.4(4) . . . . ? Ni1 N23 C11 C10 7.5(6) . . . . ? C14 N23 C11 C12 0.5(5) . . . . ? Ni1 N23 C11 C12 179.4(3) . . . . ? C10 C11 C12 C13 169.6(4) . . . . ? N23 C11 C12 C13 -2.3(5) . . . . ? C11 C12 C13 C14 3.0(5) . . . . ? C11 N23 C14 C15 -176.6(4) . . . . ? Ni1 N23 C14 C15 4.6(6) . . . . ? C11 N23 C14 C13 1.4(5) . . . . ? Ni1 N23 C14 C13 -177.5(3) . . . . ? C12 C13 C14 N23 -2.8(5) . . . . ? C12 C13 C14 C15 175.1(4) . . . . ? N23 C14 C15 C16 9.8(7) . . . . ? C13 C14 C15 C16 -167.8(4) . . . . ? N23 C14 C15 C151 -174.8(4) . . . . ? C13 C14 C15 C151 7.6(7) . . . . ? C14 C15 C16 N24 -6.4(7) . . . . ? C151 C15 C16 N24 178.1(4) . . . . ? C14 C15 C16 C17 163.5(4) . . . . ? C151 C15 C16 C17 -12.0(7) . . . . ? C19 N24 C16 C15 167.1(4) . . . . ? Ni1 N24 C16 C15 -11.2(6) . . . . ? C19 N24 C16 C17 -4.1(5) . . . . ? Ni1 N24 C16 C17 177.5(3) . . . . ? C15 C16 C17 C18 -166.6(5) . . . . ? N24 C16 C17 C18 4.7(5) . . . . ? C16 C17 C18 C19 -3.3(6) . . . . ? C16 N24 C19 C20 -179.4(4) . . . . ? Ni1 N24 C19 C20 -1.1(6) . . . . ? C16 N24 C19 C18 2.1(5) . . . . ? Ni1 N24 C19 C18 -179.5(3) . . . . ? C17 C18 C19 C20 -177.6(5) . . . . ? C17 C18 C19 N24 0.8(6) . . . . ? N24 C19 C20 C1 -13.5(7) . . . . ? C18 C19 C20 C1 164.7(5) . . . . ? N24 C19 C20 C201 169.3(4) . . . . ? C18 C19 C20 C201 -12.5(7) . . . . ? N21 C1 C20 C19 3.7(7) . . . . ? C2 C1 C20 C19 -160.6(4) . . . . ? N21 C1 C20 C201 -179.1(4) . . . . ? C2 C1 C20 C201 16.6(7) . . . . ? C6 C5 N1 C25 -19.1(7) . . . . ? C4 C5 N1 C25 169.0(4) . . . . ? N28 Ni2 N25 C21 4.5(4) . . . . ? N26 Ni2 N25 C21 -177.1(4) . . . . ? N28 Ni2 N25 C24 -176.3(4) . . . . ? N26 Ni2 N25 C24 2.0(4) . . . . ? N25 Ni2 N26 C29 176.5(4) . . . . ? N27 Ni2 N26 C29 -0.4(4) . . . . ? N25 Ni2 N26 C26 -8.3(4) . . . . ? N27 Ni2 N26 C26 174.8(4) . . . . ? N28 Ni2 N27 C34 0.2(4) . . . . ? N26 Ni2 N27 C34 -178.1(4) . . . . ? N28 Ni2 N27 C31 -176.7(4) . . . . ? N26 Ni2 N27 C31 5.0(4) . . . . ? N25 Ni2 N28 C39 -0.1(4) . . . . ? N27 Ni2 N28 C39 176.8(4) . . . . ? N25 Ni2 N28 C36 -179.1(4) . . . . ? N27 Ni2 N28 C36 -2.2(4) . . . . ? C24 N25 C21 C40 174.2(5) . . . . ? Ni2 N25 C21 C40 -6.5(7) . . . . ? C24 N25 C21 C22 -0.8(5) . . . . ? Ni2 N25 C21 C22 178.5(3) . . . . ? C40 C21 C22 C23 -174.5(4) . . . . ? N25 C21 C22 C23 0.7(5) . . . . ? C21 C22 C23 C24 -0.3(5) . . . . ? C21 N25 C24 C25 -176.0(4) . . . . ? Ni2 N25 C24 C25 4.7(7) . . . . ? C21 N25 C24 C23 0.7(5) . . . . ? Ni2 N25 C24 C23 -178.6(3) . . . . ? C22 C23 C24 C25 176.4(5) . . . . ? C22 C23 C24 N25 -0.2(6) . . . . ? N25 C24 C25 C26 -7.1(8) . . . . ? C23 C24 C25 C26 176.8(5) . . . . ? N25 C24 C25 N1 174.5(4) . . . . ? C23 C24 C25 N1 -1.6(7) . . . . ? C5 N1 C25 C26 120.9(5) . . . . ? C5 N1 C25 C24 -60.6(6) . . . . ? C24 C25 C26 N26 0.2(8) . . . . ? N1 C25 C26 N26 178.6(4) . . . . ? C24 C25 C26 C27 -176.5(5) . . . . ? N1 C25 C26 C27 1.9(7) . . . . ? C29 N26 C26 C25 -175.3(5) . . . . ? Ni2 N26 C26 C25 8.7(7) . . . . ? C29 N26 C26 C27 1.9(5) . . . . ? Ni2 N26 C26 C27 -174.2(3) . . . . ? C25 C26 C27 C28 174.2(5) . . . . ? N26 C26 C27 C28 -2.9(6) . . . . ? C26 C27 C28 C29 2.6(6) . . . . ? C26 N26 C29 C30 178.4(5) . . . . ? Ni2 N26 C29 C30 -5.6(7) . . . . ? C26 N26 C29 C28 -0.3(5) . . . . ? Ni2 N26 C29 C28 175.8(3) . . . . ? C27 C28 C29 N26 -1.5(6) . . . . ? C27 C28 C29 C30 179.9(5) . . . . ? N26 C29 C30 C31 7.8(8) . . . . ? C28 C29 C30 C31 -173.7(5) . . . . ? N26 C29 C30 C301 -169.3(4) . . . . ? C28 C29 C30 C301 9.1(8) . . . . ? C29 C30 C31 N27 -2.8(8) . . . . ? C301 C30 C31 N27 174.4(4) . . . . ? C29 C30 C31 C32 175.5(5) . . . . ? C301 C30 C31 C32 -7.4(7) . . . . ? C34 N27 C31 C30 178.3(5) . . . . ? Ni2 N27 C31 C30 -4.3(7) . . . . ? C34 N27 C31 C32 -0.2(5) . . . . ? Ni2 N27 C31 C32 177.3(3) . . . . ? C30 C31 C32 C33 -178.3(5) . . . . ? N27 C31 C32 C33 0.2(6) . . . . ? C31 C32 C33 C34 -0.1(6) . . . . ? C31 N27 C34 C35 178.7(4) . . . . ? Ni2 N27 C34 C35 1.3(7) . . . . ? C31 N27 C34 C33 0.1(5) . . . . ? Ni2 N27 C34 C33 -177.4(3) . . . . ? C32 C33 C34 N27 0.0(6) . . . . ? C32 C33 C34 C35 -178.7(4) . . . . ? N27 C34 C35 C36 -1.0(7) . . . . ? C33 C34 C35 C36 177.4(4) . . . . ? N27 C34 C35 C351 178.4(4) . . . . ? C33 C34 C35 C351 -3.1(7) . . . . ? C34 C35 C36 N28 -1.2(7) . . . . ? C351 C35 C36 N28 179.4(4) . . . . ? C34 C35 C36 C37 -177.4(4) . . . . ? C351 C35 C36 C37 3.2(7) . . . . ? C39 N28 C36 C35 -176.2(4) . . . . ? Ni2 N28 C36 C35 3.1(7) . . . . ? C39 N28 C36 C37 0.4(5) . . . . ? Ni2 N28 C36 C37 179.6(3) . . . . ? C35 C36 C37 C38 175.9(4) . . . . ? N28 C36 C37 C38 -0.8(5) . . . . ? C36 C37 C38 C39 0.9(5) . . . . ? C36 N28 C39 C40 176.0(4) . . . . ? Ni2 N28 C39 C40 -3.2(6) . . . . ? C36 N28 C39 C38 0.1(5) . . . . ? Ni2 N28 C39 C38 -179.1(3) . . . . ? C37 C38 C39 N28 -0.7(5) . . . . ? C37 C38 C39 C40 -176.6(4) . . . . ? N25 C21 C40 C39 2.5(7) . . . . ? C22 C21 C40 C39 176.9(4) . . . . ? N25 C21 C40 C401 -175.6(4) . . . . ? C22 C21 C40 C401 -1.2(7) . . . . ? N28 C39 C40 C21 2.5(7) . . . . ? C38 C39 C40 C21 177.9(4) . . . . ? N28 C39 C40 C401 -179.4(4) . . . . ? C38 C39 C40 C401 -4.0(7) . . . . ? C11 C10 C101 C106 106.9(5) . . . . ? C9 C10 C101 C106 -80.3(6) . . . . ? C11 C10 C101 C102 -74.0(6) . . . . ? C9 C10 C101 C102 98.8(5) . . . . ? C106 C101 C102 C103 1.5(7) . . . . ? C10 C101 C102 C103 -177.7(4) . . . . ? C101 C102 C103 C104 -1.2(7) . . . . ? C102 C103 C104 C105 -0.2(8) . . . . ? C103 C104 C105 C106 1.3(8) . . . . ? C102 C101 C106 C105 -0.4(7) . . . . ? C10 C101 C106 C105 178.8(4) . . . . ? C104 C105 C106 C101 -1.0(8) . . . . ? C14 C15 C151 C152 113.2(5) . . . . ? C16 C15 C151 C152 -71.3(6) . . . . ? C14 C15 C151 C156 -66.9(6) . . . . ? C16 C15 C151 C156 108.6(5) . . . . ? C156 C151 C152 C153 -1.0(7) . . . . ? C15 C151 C152 C153 178.9(4) . . . . ? C151 C152 C153 C154 1.4(8) . . . . ? C152 C153 C154 C155 -0.3(8) . . . . ? C153 C154 C155 C156 -1.1(8) . . . . ? C154 C155 C156 C151 1.5(8) . . . . ? C152 C151 C156 C155 -0.4(7) . . . . ? C15 C151 C156 C155 179.7(5) . . . . ? C19 C20 C201 C206 -112.8(5) . . . . ? C1 C20 C201 C206 70.0(6) . . . . ? C19 C20 C201 C202 64.3(6) . . . . ? C1 C20 C201 C202 -112.9(5) . . . . ? C206 C201 C202 C203 1.6(7) . . . . ? C20 C201 C202 C203 -175.6(4) . . . . ? C201 C202 C203 C204 -0.5(7) . . . . ? C202 C203 C204 C205 0.0(8) . . . . ? C203 C204 C205 C206 -0.5(8) . . . . ? C202 C201 C206 C205 -2.1(7) . . . . ? C20 C201 C206 C205 175.1(4) . . . . ? C204 C205 C206 C201 1.6(8) . . . . ? C31 C30 C301 C302 111.0(5) . . . . ? C29 C30 C301 C302 -71.8(6) . . . . ? C31 C30 C301 C306 -69.5(6) . . . . ? C29 C30 C301 C306 107.7(5) . . . . ? C306 C301 C302 C303 -1.1(7) . . . . ? C30 C301 C302 C303 178.4(4) . . . . ? C301 C302 C303 C304 1.5(7) . . . . ? C302 C303 C304 C305 0.3(7) . . . . ? C303 C304 C305 C306 -2.5(7) . . . . ? C304 C305 C306 C301 3.0(7) . . . . ? C302 C301 C306 C305 -1.2(7) . . . . ? C30 C301 C306 C305 179.3(4) . . . . ? C36 C35 C351 C352 -93.7(6) . . . . ? C34 C35 C351 C352 86.8(6) . . . . ? C36 C35 C351 C356 89.4(6) . . . . ? C34 C35 C351 C356 -90.1(6) . . . . ? C356 C351 C352 C353 1.4(7) . . . . ? C35 C351 C352 C353 -175.6(4) . . . . ? C351 C352 C353 C354 -1.9(8) . . . . ? C352 C353 C354 C355 1.3(8) . . . . ? C353 C354 C355 C356 -0.2(8) . . . . ? C352 C351 C356 C355 -0.3(7) . . . . ? C35 C351 C356 C355 176.7(4) . . . . ? C354 C355 C356 C351 -0.4(7) . . . . ? C21 C40 C401 C402 -60.8(6) . . . . ? C39 C40 C401 C402 121.0(5) . . . . ? C21 C40 C401 C406 118.3(5) . . . . ? C39 C40 C401 C406 -59.8(6) . . . . ? C406 C401 C402 C403 -1.1(7) . . . . ? C40 C401 C402 C403 178.0(4) . . . . ? C401 C402 C403 C404 1.8(7) . . . . ? C402 C403 C404 C405 -1.2(7) . . . . ? C403 C404 C405 C406 0.0(7) . . . . ? C402 C401 C406 C405 -0.1(6) . . . . ? C40 C401 C406 C405 -179.2(4) . . . . ? C404 C405 C406 C401 0.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.676 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.082 #===END data_ms496 _database_code_depnum_ccdc_archive 'CCDC 610309' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (5-Hydroxy-10,15,20-triphenylporphyrinato)nickel(II) ; _chemical_name_common (5-Hydroxy-10,15,20-triphenylporphyrinato)nickel(ii) _chemical_melting_point n/d _chemical_formula_moiety 'C38 H24 N4 Ni O' _chemical_formula_sum 'C38 H24 N4 Ni O' _chemical_formula_weight 611.32 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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6815(19) _cell_length_b 12.028(2) _cell_length_c 12.986(3) _cell_angle_alpha 69.02(3) _cell_angle_beta 77.92(3) _cell_angle_gamma 85.14(3) _cell_volume 1380.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 3868 _cell_measurement_theta_min 4.925 _cell_measurement_theta_max 50.575 _exptl_crystal_description parallelpiped _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas n/d _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8077 _exptl_absorpt_correction_T_max 0.9853 _exptl_absorpt_process_details 'program SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APex2' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15377 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.51 _reflns_number_total 5050 _reflns_number_gt 3718 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 v1.0-27 (Bruker, 2005' _computing_cell_refinement 'SAINT v7.12 (Bruke, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL _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. Residual electron density was located close to the nickel center. ; _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^)+(0.1112P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5050 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1690 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Ni Ni 0.23241(5) 0.03880(4) 0.48261(4) 0.02013(19) Uani 1 1 d . . . N21 N 0.1093(3) -0.0623(3) 0.6201(2) 0.0199(7) Uani 1 1 d . . . N22 N 0.1179(3) 0.1796(3) 0.4885(3) 0.0216(7) Uani 1 1 d . . . N23 N 0.3491(3) 0.1378(3) 0.3407(3) 0.0210(7) Uani 1 1 d . . . N24 N 0.3522(3) -0.1000(3) 0.4818(3) 0.0217(7) Uani 1 1 d . . . C1 C 0.1252(4) -0.1813(3) 0.6814(3) 0.0207(8) Uani 1 1 d . . . C2 C 0.0042(4) -0.2241(3) 0.7717(3) 0.0231(8) Uani 1 1 d . . . H2 H -0.0090 -0.3026 0.8250 0.028 Uiso 1 1 calc R . . C3 C -0.0856(4) -0.1311(3) 0.7653(3) 0.0232(8) Uani 1 1 d . . . H3 H -0.1748 -0.1317 0.8129 0.028 Uiso 1 1 calc R . . C4 C -0.0208(4) -0.0309(3) 0.6731(3) 0.0203(8) Uani 1 1 d . . . C5 C -0.0716(4) 0.0843(3) 0.6507(3) 0.0229(8) Uani 1 1 d . . . C6 C -0.0021(4) 0.1837(3) 0.5686(3) 0.0236(8) Uani 1 1 d . . . C7 C -0.0460(5) 0.3038(4) 0.5541(4) 0.0324(10) Uani 1 1 d . . . H7 H -0.1238 0.3295 0.5985 0.039 Uiso 1 1 calc R . . C8 C 0.0460(5) 0.3744(4) 0.4640(3) 0.0320(10) Uani 1 1 d . . . H8 H 0.0450 0.4590 0.4344 0.038 Uiso 1 1 calc R . . C9 C 0.1442(4) 0.2977(3) 0.4224(3) 0.0263(9) Uani 1 1 d . . . C10 C 0.2471(4) 0.3382(3) 0.3221(3) 0.0239(9) Uani 1 1 d . . . C11 C 0.3370(4) 0.2598(3) 0.2825(3) 0.0230(8) Uani 1 1 d . . . C12 C 0.4283(4) 0.2925(4) 0.1730(3) 0.0259(9) Uani 1 1 d . . . H12 H 0.4378 0.3700 0.1175 0.031 Uiso 1 1 calc R . . C13 C 0.4973(4) 0.1937(3) 0.1636(3) 0.0252(9) Uani 1 1 d . . . H13 H 0.5638 0.1880 0.1005 0.030 Uiso 1 1 calc R . . C14 C 0.4505(4) 0.0977(3) 0.2685(3) 0.0225(8) Uani 1 1 d . . . C15 C 0.5094(4) -0.0164(3) 0.2946(3) 0.0227(8) Uani 1 1 d . . . C16 C 0.4674(4) -0.1058(3) 0.3985(3) 0.0214(8) Uani 1 1 d . . . C17 C 0.5353(4) -0.2213(4) 0.4331(3) 0.0263(9) Uani 1 1 d . . . H17 H 0.6154 -0.2476 0.3912 0.032 Uiso 1 1 calc R . . C18 C 0.4637(4) -0.2849(4) 0.5362(3) 0.0273(9) Uani 1 1 d . . . H18 H 0.4860 -0.3636 0.5808 0.033 Uiso 1 1 calc R . . C19 C 0.3473(4) -0.2123(3) 0.5665(3) 0.0235(8) Uani 1 1 d . . . C20 C 0.2412(4) -0.2530(3) 0.6614(3) 0.0231(8) Uani 1 1 d . . . O1 O -0.1959(3) 0.0977(2) 0.7207(2) 0.0296(7) Uani 1 1 d . . . H1 H -0.2258 0.1680 0.6962 0.036 Uiso 1 1 calc R . . C101 C 0.2504(4) 0.4691(4) 0.2524(3) 0.0255(9) Uani 1 1 d . . . C102 C 0.1317(4) 0.5287(4) 0.2128(3) 0.0281(9) Uani 1 1 d . . . H102 H 0.0479 0.4850 0.2282 0.034 Uiso 1 1 calc R . . C103 C 0.1321(4) 0.6495(4) 0.1517(4) 0.0315(10) Uani 1 1 d . . . H103 H 0.0490 0.6873 0.1267 0.038 Uiso 1 1 calc R . . C104 C 0.2532(5) 0.7159(4) 0.1266(4) 0.0324(10) Uani 1 1 d . . . H104 H 0.2535 0.7989 0.0850 0.039 Uiso 1 1 calc R . . C105 C 0.3724(5) 0.6592(4) 0.1632(4) 0.0356(10) Uani 1 1 d . . . H105 H 0.4559 0.7036 0.1467 0.043 Uiso 1 1 calc R . . C106 C 0.3724(4) 0.5365(4) 0.2247(4) 0.0321(10) Uani 1 1 d . . . H106 H 0.4565 0.4987 0.2479 0.038 Uiso 1 1 calc R . . C151 C 0.6236(4) -0.0431(3) 0.2079(3) 0.0230(8) Uani 1 1 d . . . C152 C 0.5924(4) -0.0581(3) 0.1138(3) 0.0265(9) Uani 1 1 d . . . H152 H 0.4969 -0.0527 0.1048 0.032 Uiso 1 1 calc R . . C153 C 0.6978(4) -0.0809(4) 0.0328(3) 0.0283(9) Uani 1 1 d . . . H153 H 0.6736 -0.0895 -0.0311 0.034 Uiso 1 1 calc R . . C154 C 0.8368(4) -0.0912(4) 0.0443(3) 0.0280(9) Uani 1 1 d . . . H154 H 0.9089 -0.1059 -0.0116 0.034 Uiso 1 1 calc R . . C155 C 0.8695(4) -0.0798(4) 0.1385(3) 0.0301(9) Uani 1 1 d . . . H155 H 0.9647 -0.0887 0.1485 0.036 Uiso 1 1 calc R . . C156 C 0.7637(4) -0.0553(4) 0.2197(4) 0.0289(9) Uani 1 1 d . . . H156 H 0.7884 -0.0468 0.2835 0.035 Uiso 1 1 calc R . . C201 C 0.2461(4) -0.3772(4) 0.7447(3) 0.0249(9) Uani 1 1 d . . . C202 C 0.2481(4) -0.4785(4) 0.7143(3) 0.0268(9) Uani 1 1 d . . . H202 H 0.2488 -0.4693 0.6384 0.032 Uiso 1 1 calc R . . C203 C 0.2489(4) -0.5922(4) 0.7948(4) 0.0327(10) Uani 1 1 d . . . H203 H 0.2519 -0.6599 0.7730 0.039 Uiso 1 1 calc R . . C204 C 0.2455(4) -0.6076(4) 0.9060(4) 0.0353(10) Uani 1 1 d . . . H204 H 0.2454 -0.6855 0.9602 0.042 Uiso 1 1 calc R . . C205 C 0.2421(4) -0.5089(4) 0.9385(4) 0.0328(10) Uani 1 1 d . . . H205 H 0.2393 -0.5191 1.0149 0.039 Uiso 1 1 calc R . . C206 C 0.2427(4) -0.3947(4) 0.8580(3) 0.0276(9) Uani 1 1 d . . . H206 H 0.2409 -0.3275 0.8803 0.033 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 0.0159(3) 0.0212(3) 0.0242(3) -0.0078(2) -0.0045(2) -0.00464(19) N21 0.0163(16) 0.0228(17) 0.0231(17) -0.0091(14) -0.0051(13) -0.0041(13) N22 0.0224(17) 0.0219(17) 0.0206(16) -0.0065(13) -0.0043(13) -0.0041(13) N23 0.0143(16) 0.0241(17) 0.0266(17) -0.0099(14) -0.0049(13) -0.0040(13) N24 0.0178(16) 0.0205(16) 0.0270(17) -0.0069(14) -0.0059(14) -0.0035(13) C1 0.0198(19) 0.023(2) 0.0213(19) -0.0085(16) -0.0060(16) -0.0047(16) C2 0.022(2) 0.022(2) 0.025(2) -0.0060(17) -0.0062(16) -0.0063(16) C3 0.0175(19) 0.029(2) 0.025(2) -0.0109(17) -0.0045(16) -0.0065(16) C4 0.0163(19) 0.026(2) 0.0223(19) -0.0103(16) -0.0069(15) -0.0042(15) C5 0.0192(19) 0.028(2) 0.025(2) -0.0113(17) -0.0078(16) -0.0019(16) C6 0.024(2) 0.023(2) 0.025(2) -0.0093(17) -0.0046(17) -0.0015(16) C7 0.035(2) 0.026(2) 0.034(2) -0.0128(19) 0.001(2) 0.0013(18) C8 0.038(2) 0.024(2) 0.034(2) -0.0111(18) -0.0004(19) -0.0067(18) C9 0.029(2) 0.025(2) 0.027(2) -0.0105(17) -0.0060(18) -0.0042(17) C10 0.020(2) 0.026(2) 0.029(2) -0.0101(17) -0.0101(17) -0.0054(16) C11 0.0174(19) 0.025(2) 0.028(2) -0.0072(17) -0.0087(16) -0.0068(16) C12 0.021(2) 0.027(2) 0.027(2) -0.0048(17) -0.0049(17) -0.0066(17) C13 0.021(2) 0.029(2) 0.027(2) -0.0103(18) -0.0052(17) -0.0070(16) C14 0.0136(18) 0.029(2) 0.026(2) -0.0083(17) -0.0045(16) -0.0072(15) C15 0.0185(19) 0.028(2) 0.025(2) -0.0102(17) -0.0078(16) -0.0070(16) C16 0.0184(19) 0.023(2) 0.026(2) -0.0099(17) -0.0075(16) -0.0041(15) C17 0.018(2) 0.030(2) 0.031(2) -0.0114(18) -0.0031(17) -0.0018(16) C18 0.022(2) 0.029(2) 0.030(2) -0.0083(18) -0.0078(18) -0.0015(17) C19 0.024(2) 0.022(2) 0.026(2) -0.0080(17) -0.0080(17) -0.0013(16) C20 0.0182(19) 0.028(2) 0.025(2) -0.0098(17) -0.0044(16) -0.0053(16) O1 0.0235(15) 0.0296(16) 0.0332(16) -0.0097(13) -0.0009(12) -0.0032(12) C101 0.020(2) 0.028(2) 0.028(2) -0.0102(18) -0.0037(17) -0.0047(16) C102 0.021(2) 0.030(2) 0.035(2) -0.0131(18) -0.0046(17) -0.0030(17) C103 0.025(2) 0.033(2) 0.036(2) -0.012(2) -0.0068(19) 0.0027(18) C104 0.034(2) 0.022(2) 0.035(2) -0.0047(18) -0.0013(19) -0.0027(18) C105 0.025(2) 0.032(2) 0.043(3) -0.005(2) -0.003(2) -0.0129(18) C106 0.022(2) 0.029(2) 0.043(3) -0.0068(19) -0.0108(19) -0.0066(17) C151 0.027(2) 0.0171(19) 0.024(2) -0.0040(16) -0.0060(17) -0.0057(16) C152 0.021(2) 0.029(2) 0.031(2) -0.0103(18) -0.0093(17) 0.0000(17) C153 0.033(2) 0.030(2) 0.028(2) -0.0129(18) -0.0135(19) 0.0028(18) C154 0.021(2) 0.032(2) 0.030(2) -0.0113(18) 0.0004(17) -0.0044(17) C155 0.018(2) 0.036(2) 0.038(2) -0.013(2) -0.0034(18) -0.0082(17) C156 0.021(2) 0.037(2) 0.035(2) -0.0176(19) -0.0064(18) -0.0077(17) C201 0.0127(18) 0.029(2) 0.031(2) -0.0092(18) -0.0012(16) -0.0010(16) C202 0.019(2) 0.029(2) 0.031(2) -0.0088(18) -0.0029(17) -0.0037(17) C203 0.024(2) 0.028(2) 0.045(3) -0.015(2) -0.001(2) -0.0026(18) C204 0.026(2) 0.028(2) 0.041(3) 0.000(2) -0.0034(19) -0.0020(18) C205 0.023(2) 0.039(3) 0.029(2) -0.004(2) -0.0039(18) 0.0004(18) C206 0.0168(19) 0.032(2) 0.035(2) -0.0124(19) -0.0052(17) -0.0030(16) _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 N24 1.953(3) . ? Ni N22 1.960(3) . ? Ni N23 1.968(3) . ? Ni N21 1.972(3) . ? N21 C1 1.380(5) . ? N21 C4 1.395(5) . ? N22 C9 1.384(5) . ? N22 C6 1.398(5) . ? N23 C14 1.391(5) . ? N23 C11 1.397(5) . ? N24 C16 1.398(5) . ? N24 C19 1.400(5) . ? C1 C20 1.396(5) . ? C1 C2 1.451(5) . ? C2 C3 1.346(5) . ? C2 H2 0.9500 . ? C3 C4 1.436(5) . ? C3 H3 0.9500 . ? C4 C5 1.378(5) . ? C5 O1 1.384(5) . ? C5 C6 1.394(5) . ? C6 C7 1.428(5) . ? C7 C8 1.366(6) . ? C7 H7 0.9500 . ? C8 C9 1.429(6) . ? C8 H8 0.9500 . ? C9 C10 1.417(6) . ? C10 C11 1.390(6) . ? C10 C101 1.509(5) . ? C11 C12 1.446(5) . ? C12 C13 1.344(6) . ? C12 H12 0.9500 . ? C13 C14 1.448(5) . ? C13 H13 0.9500 . ? C14 C15 1.392(5) . ? C15 C16 1.395(5) . ? C15 C151 1.508(6) . ? C16 C17 1.444(5) . ? C17 C18 1.352(6) . ? C17 H17 0.9500 . ? C18 C19 1.443(6) . ? C18 H18 0.9500 . ? C19 C20 1.391(5) . ? C20 C201 1.502(5) . ? O1 H1 0.8400 . ? C101 C102 1.395(6) . ? C101 C106 1.399(6) . ? C102 C103 1.383(6) . ? C102 H102 0.9500 . ? C103 C104 1.390(6) . ? C103 H103 0.9500 . ? C104 C105 1.373(6) . ? C104 H104 0.9500 . ? C105 C106 1.405(6) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C151 C156 1.386(5) . ? C151 C152 1.392(5) . ? C152 C153 1.391(6) . ? C152 H152 0.9500 . ? C153 C154 1.375(6) . ? C153 H153 0.9500 . ? C154 C155 1.381(6) . ? C154 H154 0.9500 . ? C155 C156 1.402(6) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? C201 C206 1.403(6) . ? C201 C202 1.405(6) . ? C202 C203 1.393(6) . ? C202 H202 0.9500 . ? C203 C204 1.382(6) . ? C203 H203 0.9500 . ? C204 C205 1.390(6) . ? C204 H204 0.9500 . ? C205 C206 1.397(6) . ? C205 H205 0.9500 . ? C206 H206 0.9500 . ? 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 N24 Ni N22 177.04(12) . . ? N24 Ni N23 90.80(13) . . ? N22 Ni N23 89.49(13) . . ? N24 Ni N21 89.22(13) . . ? N22 Ni N21 90.64(13) . . ? N23 Ni N21 176.97(12) . . ? C1 N21 C4 103.9(3) . . ? C1 N21 Ni 128.8(3) . . ? C4 N21 Ni 127.1(3) . . ? C9 N22 C6 104.4(3) . . ? C9 N22 Ni 128.3(3) . . ? C6 N22 Ni 127.0(3) . . ? C14 N23 C11 104.4(3) . . ? C14 N23 Ni 126.7(3) . . ? C11 N23 Ni 128.5(3) . . ? C16 N24 C19 105.2(3) . . ? C16 N24 Ni 126.9(3) . . ? C19 N24 Ni 127.8(3) . . ? N21 C1 C20 125.5(3) . . ? N21 C1 C2 111.1(3) . . ? C20 C1 C2 123.4(3) . . ? C3 C2 C1 106.8(3) . . ? C3 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? C2 C3 C4 107.0(3) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? C5 C4 N21 124.5(3) . . ? C5 C4 C3 123.7(4) . . ? N21 C4 C3 111.2(3) . . ? C4 C5 O1 115.4(3) . . ? C4 C5 C6 124.2(4) . . ? O1 C5 C6 120.3(3) . . ? C5 C6 N22 124.9(3) . . ? C5 C6 C7 124.2(4) . . ? N22 C6 C7 110.9(3) . . ? C8 C7 C6 106.5(4) . . ? C8 C7 H7 126.8 . . ? C6 C7 H7 126.8 . . ? C7 C8 C9 107.4(4) . . ? C7 C8 H8 126.3 . . ? C9 C8 H8 126.3 . . ? N22 C9 C10 125.3(4) . . ? N22 C9 C8 110.8(3) . . ? C10 C9 C8 123.8(4) . . ? C11 C10 C9 121.8(4) . . ? C11 C10 C101 119.4(4) . . ? C9 C10 C101 118.6(4) . . ? C10 C11 N23 125.2(4) . . ? C10 C11 C12 124.6(4) . . ? N23 C11 C12 110.1(3) . . ? C13 C12 C11 107.9(4) . . ? C13 C12 H12 126.1 . . ? C11 C12 H12 126.1 . . ? C12 C13 C14 106.6(4) . . ? C12 C13 H13 126.7 . . ? C14 C13 H13 126.7 . . ? N23 C14 C15 125.5(3) . . ? N23 C14 C13 111.0(3) . . ? C15 C14 C13 123.3(4) . . ? C14 C15 C16 122.2(4) . . ? C14 C15 C151 118.5(3) . . ? C16 C15 C151 119.2(3) . . ? C15 C16 N24 126.0(3) . . ? C15 C16 C17 123.9(4) . . ? N24 C16 C17 110.0(3) . . ? C18 C17 C16 107.2(4) . . ? C18 C17 H17 126.4 . . ? C16 C17 H17 126.4 . . ? C17 C18 C19 107.9(4) . . ? C17 C18 H18 126.1 . . ? C19 C18 H18 126.1 . . ? C20 C19 N24 126.1(3) . . ? C20 C19 C18 124.1(4) . . ? N24 C19 C18 109.6(3) . . ? C19 C20 C1 121.4(4) . . ? C19 C20 C201 121.0(3) . . ? C1 C20 C201 117.6(3) . . ? C5 O1 H1 109.5 . . ? C102 C101 C106 116.9(4) . . ? C102 C101 C10 121.4(3) . . ? C106 C101 C10 121.7(4) . . ? C103 C102 C101 122.0(4) . . ? C103 C102 H102 119.0 . . ? C101 C102 H102 119.0 . . ? C102 C103 C104 120.6(4) . . ? C102 C103 H103 119.7 . . ? C104 C103 H103 119.7 . . ? C105 C104 C103 118.7(4) . . ? C105 C104 H104 120.6 . . ? C103 C104 H104 120.6 . . ? C104 C105 C106 120.8(4) . . ? C104 C105 H105 119.6 . . ? C106 C105 H105 119.6 . . ? C101 C106 C105 121.0(4) . . ? C101 C106 H106 119.5 . . ? C105 C106 H106 119.5 . . ? C156 C151 C152 117.5(4) . . ? C156 C151 C15 121.1(3) . . ? C152 C151 C15 121.4(3) . . ? C153 C152 C151 121.5(4) . . ? C153 C152 H152 119.3 . . ? C151 C152 H152 119.3 . . ? C154 C153 C152 120.7(4) . . ? C154 C153 H153 119.6 . . ? C152 C153 H153 119.6 . . ? C153 C154 C155 118.6(4) . . ? C153 C154 H154 120.7 . . ? C155 C154 H154 120.7 . . ? C154 C155 C156 120.8(4) . . ? C154 C155 H155 119.6 . . ? C156 C155 H155 119.6 . . ? C151 C156 C155 120.9(4) . . ? C151 C156 H156 119.6 . . ? C155 C156 H156 119.6 . . ? C206 C201 C202 118.0(4) . . ? C206 C201 C20 119.8(4) . . ? C202 C201 C20 122.2(4) . . ? C203 C202 C201 120.4(4) . . ? C203 C202 H202 119.8 . . ? C201 C202 H202 119.8 . . ? C204 C203 C202 120.8(4) . . ? C204 C203 H203 119.6 . . ? C202 C203 H203 119.6 . . ? C203 C204 C205 120.0(4) . . ? C203 C204 H204 120.0 . . ? C205 C204 H204 120.0 . . ? C204 C205 C206 119.5(4) . . ? C204 C205 H205 120.3 . . ? C206 C205 H205 120.3 . . ? C205 C206 C201 121.4(4) . . ? C205 C206 H206 119.3 . . ? C201 C206 H206 119.3 . . ? 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 N24 Ni N21 C1 2.9(3) . . . . ? N22 Ni N21 C1 -174.1(3) . . . . ? N24 Ni N21 C4 -172.1(3) . . . . ? N22 Ni N21 C4 10.9(3) . . . . ? N23 Ni N22 C9 -10.3(3) . . . . ? N21 Ni N22 C9 172.7(3) . . . . ? N23 Ni N22 C6 176.7(3) . . . . ? N21 Ni N22 C6 -0.3(3) . . . . ? N24 Ni N23 C14 13.0(3) . . . . ? N22 Ni N23 C14 -170.0(3) . . . . ? N24 Ni N23 C11 -176.4(3) . . . . ? N22 Ni N23 C11 0.7(3) . . . . ? N23 Ni N24 C16 -2.9(3) . . . . ? N21 Ni N24 C16 174.1(3) . . . . ? N23 Ni N24 C19 172.9(3) . . . . ? N21 Ni N24 C19 -10.2(3) . . . . ? C4 N21 C1 C20 -179.2(3) . . . . ? Ni N21 C1 C20 4.9(5) . . . . ? C4 N21 C1 C2 0.8(4) . . . . ? Ni N21 C1 C2 -175.1(2) . . . . ? N21 C1 C2 C3 0.0(4) . . . . ? C20 C1 C2 C3 179.9(3) . . . . ? C1 C2 C3 C4 -0.7(4) . . . . ? C1 N21 C4 C5 170.2(3) . . . . ? Ni N21 C4 C5 -13.8(5) . . . . ? C1 N21 C4 C3 -1.2(4) . . . . ? Ni N21 C4 C3 174.8(2) . . . . ? C2 C3 C4 C5 -170.2(3) . . . . ? C2 C3 C4 N21 1.2(4) . . . . ? N21 C4 C5 O1 -173.4(3) . . . . ? C3 C4 C5 O1 -3.0(5) . . . . ? N21 C4 C5 C6 2.8(6) . . . . ? C3 C4 C5 C6 173.2(4) . . . . ? C4 C5 C6 N22 8.9(6) . . . . ? O1 C5 C6 N22 -175.1(3) . . . . ? C4 C5 C6 C7 -172.3(4) . . . . ? O1 C5 C6 C7 3.8(6) . . . . ? C9 N22 C6 C5 176.9(4) . . . . ? Ni N22 C6 C5 -8.8(5) . . . . ? C9 N22 C6 C7 -2.1(4) . . . . ? Ni N22 C6 C7 172.2(3) . . . . ? C5 C6 C7 C8 -178.3(4) . . . . ? N22 C6 C7 C8 0.7(5) . . . . ? C6 C7 C8 C9 1.0(5) . . . . ? C6 N22 C9 C10 -172.9(4) . . . . ? Ni N22 C9 C10 12.9(6) . . . . ? C6 N22 C9 C8 2.7(4) . . . . ? Ni N22 C9 C8 -171.5(3) . . . . ? C7 C8 C9 N22 -2.4(5) . . . . ? C7 C8 C9 C10 173.3(4) . . . . ? N22 C9 C10 C11 -2.4(6) . . . . ? C8 C9 C10 C11 -177.5(4) . . . . ? N22 C9 C10 C101 172.6(3) . . . . ? C8 C9 C10 C101 -2.4(6) . . . . ? C9 C10 C11 N23 -8.0(6) . . . . ? C101 C10 C11 N23 177.0(3) . . . . ? C9 C10 C11 C12 169.8(4) . . . . ? C101 C10 C11 C12 -5.2(6) . . . . ? C14 N23 C11 C10 -180.0(3) . . . . ? Ni N23 C11 C10 7.8(5) . . . . ? C14 N23 C11 C12 2.0(4) . . . . ? Ni N23 C11 C12 -170.3(3) . . . . ? C10 C11 C12 C13 -179.0(4) . . . . ? N23 C11 C12 C13 -0.9(4) . . . . ? C11 C12 C13 C14 -0.6(4) . . . . ? C11 N23 C14 C15 172.8(3) . . . . ? Ni N23 C14 C15 -14.8(5) . . . . ? C11 N23 C14 C13 -2.3(4) . . . . ? Ni N23 C14 C13 170.1(2) . . . . ? C12 C13 C14 N23 1.9(4) . . . . ? C12 C13 C14 C15 -173.4(3) . . . . ? N23 C14 C15 C16 2.1(6) . . . . ? C13 C14 C15 C16 176.7(3) . . . . ? N23 C14 C15 C151 -177.1(3) . . . . ? C13 C14 C15 C151 -2.6(5) . . . . ? C14 C15 C16 N24 9.3(6) . . . . ? C151 C15 C16 N24 -171.5(3) . . . . ? C14 C15 C16 C17 -173.5(3) . . . . ? C151 C15 C16 C17 5.7(5) . . . . ? C19 N24 C16 C15 176.4(3) . . . . ? Ni N24 C16 C15 -7.1(5) . . . . ? C19 N24 C16 C17 -1.1(4) . . . . ? Ni N24 C16 C17 175.4(2) . . . . ? C15 C16 C17 C18 -178.0(4) . . . . ? N24 C16 C17 C18 -0.5(4) . . . . ? C16 C17 C18 C19 1.8(4) . . . . ? C16 N24 C19 C20 -172.7(4) . . . . ? Ni N24 C19 C20 10.9(5) . . . . ? C16 N24 C19 C18 2.2(4) . . . . ? Ni N24 C19 C18 -174.2(2) . . . . ? C17 C18 C19 C20 172.4(4) . . . . ? C17 C18 C19 N24 -2.6(4) . . . . ? N24 C19 C20 C1 -0.6(6) . . . . ? C18 C19 C20 C1 -174.8(4) . . . . ? N24 C19 C20 C201 178.1(3) . . . . ? C18 C19 C20 C201 3.9(6) . . . . ? N21 C1 C20 C19 -7.5(6) . . . . ? C2 C1 C20 C19 172.6(4) . . . . ? N21 C1 C20 C201 173.8(3) . . . . ? C2 C1 C20 C201 -6.1(5) . . . . ? C11 C10 C101 C102 119.0(4) . . . . ? C9 C10 C101 C102 -56.2(5) . . . . ? C11 C10 C101 C106 -61.2(5) . . . . ? C9 C10 C101 C106 123.6(4) . . . . ? C106 C101 C102 C103 -1.9(6) . . . . ? C10 C101 C102 C103 178.0(4) . . . . ? C101 C102 C103 C104 0.7(6) . . . . ? C102 C103 C104 C105 0.3(6) . . . . ? C103 C104 C105 C106 0.0(7) . . . . ? C102 C101 C106 C105 2.2(6) . . . . ? C10 C101 C106 C105 -177.7(4) . . . . ? C104 C105 C106 C101 -1.3(7) . . . . ? C14 C15 C151 C156 106.3(4) . . . . ? C16 C15 C151 C156 -73.0(5) . . . . ? C14 C15 C151 C152 -74.6(5) . . . . ? C16 C15 C151 C152 106.1(4) . . . . ? C156 C151 C152 C153 -1.9(6) . . . . ? C15 C151 C152 C153 179.0(4) . . . . ? C151 C152 C153 C154 1.0(6) . . . . ? C152 C153 C154 C155 0.7(6) . . . . ? C153 C154 C155 C156 -1.6(6) . . . . ? C152 C151 C156 C155 1.0(6) . . . . ? C15 C151 C156 C155 -179.8(4) . . . . ? C154 C155 C156 C151 0.7(6) . . . . ? C19 C20 C201 C206 123.1(4) . . . . ? C1 C20 C201 C206 -58.2(5) . . . . ? C19 C20 C201 C202 -59.6(5) . . . . ? C1 C20 C201 C202 119.1(4) . . . . ? C206 C201 C202 C203 -1.0(6) . . . . ? C20 C201 C202 C203 -178.3(4) . . . . ? C201 C202 C203 C204 1.1(6) . . . . ? C202 C203 C204 C205 -0.4(6) . . . . ? C203 C204 C205 C206 -0.2(6) . . . . ? C204 C205 C206 C201 0.3(6) . . . . ? C202 C201 C206 C205 0.3(6) . . . . ? C20 C201 C206 C205 177.7(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C156 H156 N21 0.95 2.49 3.364(5) 153.4 2_656 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.624 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.147 #===END data_ms498 _database_code_depnum_ccdc_archive 'CCDC 610310' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (5-Amino-10,15,20-triphenylporphyrinato)nickel(II) ; _chemical_name_common (5-Amino-10,15,20-triphenylporphyrinato)nickel(ii) _chemical_melting_point n/d _chemical_formula_moiety 'C38 H25 N5 Ni' _chemical_formula_sum 'C38 H25 N5 Ni' _chemical_formula_weight 610.34 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.4778(2) _cell_length_b 19.0155(6) _cell_length_c 22.2824(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2744.72(15) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 512 _cell_measurement_theta_min 6.575 _cell_measurement_theta_max 44.394 _exptl_crystal_description parallelpiped _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas n/d _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details 'Program SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APex2' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31404 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6313 _reflns_number_gt 5423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 v1.0-27 (Bruker, 2005' _computing_cell_refinement 'SAINT v7.12 (Bruke, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL _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. Friedel pairs were not merged. ; _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^)+(0.0404P)^2^+0.1901P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(11) _refine_ls_number_reflns 6303 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0800 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 Ni Ni 0.80063(5) 0.909169(16) 0.030610(13) 0.01797(8) Uani 1 1 d . . . N21 N 0.6073(3) 0.87883(10) -0.03086(9) 0.0205(4) Uani 1 1 d . . . N22 N 0.6458(3) 0.85764(10) 0.09039(8) 0.0203(4) Uani 1 1 d . . . N23 N 0.9934(3) 0.93956(10) 0.09177(8) 0.0191(4) Uani 1 1 d . . . N24 N 0.9609(3) 0.95820(10) -0.02983(9) 0.0193(4) Uani 1 1 d . . . C1 C 0.6363(4) 0.87937(13) -0.09243(10) 0.0200(5) Uani 1 1 d . . . C2 C 0.4683(4) 0.84567(14) -0.12176(11) 0.0238(6) Uani 1 1 d . . . H2 H 0.4557 0.8374 -0.1636 0.029 Uiso 1 1 calc R . . C3 C 0.3298(4) 0.82758(13) -0.07899(11) 0.0245(5) Uani 1 1 d . . . H3 H 0.1993 0.8060 -0.0852 0.029 Uiso 1 1 calc R . . C4 C 0.4174(4) 0.84718(12) -0.02300(11) 0.0203(5) Uani 1 1 d . . . C5 C 0.3372(4) 0.82525(11) 0.03165(11) 0.0207(5) Uani 1 1 d . . . C6 C 0.4558(4) 0.82575(13) 0.08417(11) 0.0219(5) Uani 1 1 d . . . C7 C 0.3989(4) 0.78947(13) 0.13721(11) 0.0263(6) Uani 1 1 d . . . H7 H 0.2766 0.7629 0.1434 0.032 Uiso 1 1 calc R . . C8 C 0.5527(4) 0.80005(13) 0.17742(11) 0.0248(6) Uani 1 1 d . . . H8 H 0.5586 0.7823 0.2172 0.030 Uiso 1 1 calc R . . C9 C 0.7036(4) 0.84275(12) 0.14885(10) 0.0213(5) Uani 1 1 d . . . C10 C 0.8812(4) 0.86758(12) 0.17740(10) 0.0202(5) Uani 1 1 d . . . C11 C 1.0155(4) 0.91322(14) 0.15012(10) 0.0207(5) Uani 1 1 d . . . C12 C 1.1905(4) 0.94472(12) 0.17870(10) 0.0235(5) Uani 1 1 d . . . H12 H 1.2404 0.9345 0.2178 0.028 Uiso 1 1 calc R . . C13 C 1.2714(4) 0.99150(13) 0.14000(10) 0.0228(5) Uani 1 1 d . . . H13 H 1.3869 1.0212 0.1470 0.027 Uiso 1 1 calc R . . C14 C 1.1495(4) 0.98799(12) 0.08587(10) 0.0193(5) Uani 1 1 d . . . C15 C 1.1970(4) 1.02548(12) 0.03423(10) 0.0206(5) Uani 1 1 d . . . C16 C 1.1122(4) 1.00777(12) -0.02102(10) 0.0197(5) Uani 1 1 d . . . C17 C 1.1837(4) 1.03515(13) -0.07735(10) 0.0237(5) Uani 1 1 d . . . H17 H 1.2823 1.0716 -0.0830 0.028 Uiso 1 1 calc R . . C18 C 1.0847(4) 0.99949(13) -0.12052(11) 0.0244(6) Uani 1 1 d . . . H18 H 1.1044 1.0046 -0.1625 0.029 Uiso 1 1 calc R . . C19 C 0.9441(4) 0.95248(13) -0.09181(10) 0.0198(5) Uani 1 1 d . . . C20 C 0.7994(4) 0.91239(13) -0.12210(9) 0.0205(4) Uani 1 1 d . . . N1 N 0.1459(3) 0.79562(11) 0.03266(10) 0.0266(5) Uani 1 1 d . . . H1A H 0.0758 0.7907 -0.0009 0.032 Uiso 1 1 calc R . . H1B H 0.0924 0.7814 0.0669 0.032 Uiso 1 1 calc R . . C101 C 0.9111(4) 0.84909(13) 0.24241(10) 0.0209(5) Uani 1 1 d . . . C102 C 1.0380(5) 0.79493(15) 0.26077(12) 0.0358(7) Uani 1 1 d . . . H102 H 1.1083 0.7674 0.2317 0.043 Uiso 1 1 calc R . . C103 C 1.0642(5) 0.78018(16) 0.32169(12) 0.0373(7) Uani 1 1 d . . . H103 H 1.1534 0.7431 0.3338 0.045 Uiso 1 1 calc R . . C104 C 0.9620(4) 0.81883(14) 0.36381(11) 0.0261(6) Uani 1 1 d . . . H104 H 0.9796 0.8086 0.4052 0.031 Uiso 1 1 calc R . . C105 C 0.8341(5) 0.87230(15) 0.34639(11) 0.0335(7) Uani 1 1 d . . . H105 H 0.7631 0.8993 0.3757 0.040 Uiso 1 1 calc R . . C106 C 0.8079(5) 0.88716(14) 0.28589(11) 0.0322(6) Uani 1 1 d . . . H106 H 0.7177 0.9241 0.2742 0.039 Uiso 1 1 calc R . . C151 C 1.3521(3) 1.08350(12) 0.03728(9) 0.0201(5) Uani 1 1 d . . . C152 C 1.3004(4) 1.14758(12) 0.06390(10) 0.0233(5) Uani 1 1 d . . . H152 H 1.1679 1.1532 0.0815 0.028 Uiso 1 1 calc R . . C153 C 1.4386(4) 1.20291(13) 0.06512(11) 0.0266(6) Uani 1 1 d . . . H153 H 1.3996 1.2464 0.0828 0.032 Uiso 1 1 calc R . . C154 C 1.6344(4) 1.19509(13) 0.04060(10) 0.0260(6) Uani 1 1 d . . . H154 H 1.7294 1.2331 0.0414 0.031 Uiso 1 1 calc R . . C155 C 1.6901(4) 1.13130(13) 0.01496(9) 0.0241(5) Uani 1 1 d . . . H155 H 1.8244 1.1255 -0.0015 0.029 Uiso 1 1 calc R . . C156 C 1.5506(4) 1.07617(13) 0.01330(10) 0.0217(5) Uani 1 1 d . . . H156 H 1.5902 1.0328 -0.0044 0.026 Uiso 1 1 calc R . . C201 C 0.8121(4) 0.90644(13) -0.18875(9) 0.0216(5) Uani 1 1 d . . . C202 C 0.9827(4) 0.87462(14) -0.21467(10) 0.0236(5) Uani 1 1 d . . . H202 H 1.0921 0.8584 -0.1898 0.028 Uiso 1 1 calc R . . C203 C 0.9962(4) 0.86605(14) -0.27660(11) 0.0262(6) Uani 1 1 d . . . H203 H 1.1138 0.8440 -0.2938 0.031 Uiso 1 1 calc R . . C204 C 0.8386(5) 0.88960(13) -0.31296(11) 0.0282(6) Uani 1 1 d . . . H204 H 0.8473 0.8838 -0.3552 0.034 Uiso 1 1 calc R . . C205 C 0.6693(5) 0.92140(14) -0.28802(11) 0.0302(6) Uani 1 1 d . . . H205 H 0.5608 0.9375 -0.3132 0.036 Uiso 1 1 calc R . . C206 C 0.6541(4) 0.93048(13) -0.22627(11) 0.0267(6) Uani 1 1 d . . . H206 H 0.5365 0.9530 -0.2096 0.032 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 0.01899(14) 0.02042(14) 0.01449(13) -0.00042(13) 0.00028(13) -0.00112(14) N21 0.0202(10) 0.0217(9) 0.0194(9) 0.0009(9) -0.0007(10) -0.0020(8) N22 0.0218(11) 0.0228(10) 0.0161(9) -0.0017(8) 0.0006(8) -0.0005(9) N23 0.0234(11) 0.0204(10) 0.0135(9) 0.0007(8) 0.0009(8) 0.0000(9) N24 0.0218(10) 0.0211(10) 0.0149(9) 0.0003(9) 0.0002(9) -0.0010(8) C1 0.0186(12) 0.0229(12) 0.0184(11) -0.0023(10) -0.0025(9) 0.0020(10) C2 0.0221(13) 0.0289(14) 0.0204(12) 0.0001(11) -0.0046(10) 0.0005(11) C3 0.0211(14) 0.0296(13) 0.0227(12) 0.0004(10) -0.0020(11) -0.0012(11) C4 0.0160(12) 0.0211(11) 0.0239(13) 0.0009(10) -0.0024(10) 0.0014(10) C5 0.0194(12) 0.0183(11) 0.0245(11) -0.0027(10) 0.0022(12) 0.0007(9) C6 0.0233(13) 0.0201(12) 0.0222(12) -0.0023(10) 0.0039(11) 0.0007(10) C7 0.0277(15) 0.0258(14) 0.0253(13) -0.0009(11) 0.0047(11) -0.0061(12) C8 0.0288(14) 0.0260(13) 0.0196(12) 0.0017(10) 0.0031(11) -0.0048(11) C9 0.0249(12) 0.0206(11) 0.0185(11) 0.0005(9) 0.0024(11) 0.0012(12) C10 0.0252(13) 0.0206(12) 0.0149(11) -0.0007(10) 0.0024(10) 0.0030(11) C11 0.0230(12) 0.0225(12) 0.0166(11) -0.0021(11) 0.0002(9) 0.0014(12) C12 0.0261(13) 0.0276(13) 0.0169(11) 0.0000(9) -0.0022(12) -0.0002(12) C13 0.0261(14) 0.0227(12) 0.0196(11) -0.0028(9) -0.0006(10) -0.0039(11) C14 0.0197(13) 0.0200(11) 0.0183(11) -0.0024(9) 0.0021(10) 0.0005(10) C15 0.0216(11) 0.0219(11) 0.0183(10) -0.0022(10) 0.0020(13) -0.0012(11) C16 0.0217(12) 0.0203(11) 0.0173(12) -0.0001(9) 0.0022(10) 0.0024(10) C17 0.0264(14) 0.0247(12) 0.0199(11) 0.0031(10) -0.0009(12) -0.0037(12) C18 0.0293(15) 0.0269(13) 0.0170(12) 0.0037(10) 0.0001(11) -0.0010(12) C19 0.0200(12) 0.0226(12) 0.0169(11) 0.0008(10) -0.0009(10) 0.0017(10) C20 0.0220(11) 0.0227(11) 0.0166(10) 0.0004(10) -0.0014(10) 0.0005(13) N1 0.0236(11) 0.0317(11) 0.0245(10) -0.0019(10) 0.0024(10) -0.0066(9) C101 0.0235(13) 0.0224(12) 0.0170(11) -0.0010(10) 0.0018(10) -0.0042(11) C102 0.0453(18) 0.0404(17) 0.0215(13) 0.0008(12) 0.0076(12) 0.0176(15) C103 0.050(2) 0.0393(17) 0.0225(13) 0.0073(12) 0.0034(13) 0.0196(15) C104 0.0317(15) 0.0303(14) 0.0163(12) 0.0031(11) 0.0007(11) -0.0031(12) C105 0.048(2) 0.0329(14) 0.0197(12) -0.0039(11) 0.0048(13) 0.0103(14) C106 0.0442(17) 0.0306(14) 0.0219(12) 0.0007(10) 0.0010(14) 0.0136(14) C151 0.0226(12) 0.0240(12) 0.0136(10) 0.0023(10) -0.0037(9) -0.0015(10) C152 0.0236(12) 0.0275(12) 0.0188(11) 0.0006(9) -0.0009(11) 0.0043(12) C153 0.0352(16) 0.0205(13) 0.0240(13) -0.0006(10) -0.0029(11) 0.0022(12) C154 0.0309(14) 0.0288(13) 0.0183(12) 0.0073(10) -0.0055(10) -0.0088(11) C155 0.0236(13) 0.0347(13) 0.0140(10) 0.0032(9) -0.0005(11) -0.0015(12) C156 0.0250(13) 0.0230(13) 0.0171(11) 0.0006(9) -0.0005(9) 0.0013(10) C201 0.0258(12) 0.0223(11) 0.0168(10) 0.0013(10) -0.0015(10) -0.0029(13) C202 0.0227(14) 0.0291(14) 0.0189(12) 0.0021(11) -0.0018(10) -0.0021(11) C203 0.0304(15) 0.0300(14) 0.0182(12) -0.0008(11) 0.0037(11) -0.0010(12) C204 0.0382(17) 0.0302(14) 0.0160(11) -0.0011(10) 0.0002(11) -0.0069(12) C205 0.0358(16) 0.0327(15) 0.0221(12) 0.0044(11) -0.0097(12) 0.0000(13) C206 0.0235(14) 0.0291(13) 0.0275(13) 0.0007(10) -0.0042(11) 0.0044(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N22 1.9342(19) . ? Ni N23 1.937(2) . ? Ni N24 1.939(2) . ? Ni N21 1.944(2) . ? N21 C4 1.381(3) . ? N21 C1 1.385(3) . ? N22 C6 1.379(3) . ? N22 C9 1.385(3) . ? N23 C14 1.374(3) . ? N23 C11 1.401(3) . ? N24 C16 1.374(3) . ? N24 C19 1.390(3) . ? C1 C20 1.396(3) . ? C1 C2 1.422(3) . ? C2 C3 1.353(3) . ? C2 H2 0.9500 . ? C3 C4 1.420(3) . ? C3 H3 0.9500 . ? C4 C5 1.388(3) . ? C5 N1 1.361(3) . ? C5 C6 1.400(3) . ? C6 C7 1.417(3) . ? C7 C8 1.355(4) . ? C7 H7 0.9500 . ? C8 C9 1.421(4) . ? C8 H8 0.9500 . ? C9 C10 1.397(4) . ? C10 C11 1.371(3) . ? C10 C101 1.503(3) . ? C11 C12 1.432(3) . ? C12 C13 1.345(3) . ? C12 H12 0.9500 . ? C13 C14 1.443(3) . ? C13 H13 0.9500 . ? C14 C15 1.388(3) . ? C15 C16 1.390(3) . ? C15 C151 1.494(3) . ? C16 C17 1.436(3) . ? C17 C18 1.340(3) . ? C17 H17 0.9500 . ? C18 C19 1.427(3) . ? C18 H18 0.9500 . ? C19 C20 1.384(3) . ? C20 C201 1.492(3) . ? N1 H1A 0.8800 . ? N1 H1B 0.8800 . ? C101 C102 1.380(4) . ? C101 C106 1.382(3) . ? C102 C103 1.396(4) . ? C102 H102 0.9500 . ? C103 C104 1.364(4) . ? C103 H103 0.9500 . ? C104 C105 1.368(4) . ? C104 H104 0.9500 . ? C105 C106 1.388(3) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C151 C152 1.396(3) . ? C151 C156 1.400(3) . ? C152 C153 1.382(4) . ? C152 H152 0.9500 . ? C153 C154 1.389(4) . ? C153 H153 0.9500 . ? C154 C155 1.389(4) . ? C154 H154 0.9500 . ? C155 C156 1.385(3) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? C201 C202 1.386(3) . ? C201 C206 1.398(3) . ? C202 C203 1.392(3) . ? C202 H202 0.9500 . ? C203 C204 1.378(4) . ? C203 H203 0.9500 . ? C204 C205 1.370(4) . ? C204 H204 0.9500 . ? C205 C206 1.390(3) . ? C205 H205 0.9500 . ? C206 H206 0.9500 . ? 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 N22 Ni N23 90.05(8) . . ? N22 Ni N24 178.21(9) . . ? N23 Ni N24 90.01(8) . . ? N22 Ni N21 90.05(8) . . ? N23 Ni N21 179.89(9) . . ? N24 Ni N21 89.90(8) . . ? C4 N21 C1 104.5(2) . . ? C4 N21 Ni 127.88(17) . . ? C1 N21 Ni 127.49(16) . . ? C6 N22 C9 104.2(2) . . ? C6 N22 Ni 128.06(16) . . ? C9 N22 Ni 127.68(17) . . ? C14 N23 C11 104.67(19) . . ? C14 N23 Ni 127.39(15) . . ? C11 N23 Ni 127.77(16) . . ? C16 N24 C19 104.56(19) . . ? C16 N24 Ni 127.77(16) . . ? C19 N24 Ni 127.64(16) . . ? N21 C1 C20 125.1(2) . . ? N21 C1 C2 110.4(2) . . ? C20 C1 C2 124.4(2) . . ? C3 C2 C1 107.3(2) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? C2 C3 C4 106.7(2) . . ? C2 C3 H3 126.7 . . ? C4 C3 H3 126.7 . . ? N21 C4 C5 125.2(2) . . ? N21 C4 C3 111.0(2) . . ? C5 C4 C3 122.8(2) . . ? N1 C5 C4 118.7(2) . . ? N1 C5 C6 119.2(2) . . ? C4 C5 C6 121.7(2) . . ? N22 C6 C5 125.2(2) . . ? N22 C6 C7 111.2(2) . . ? C5 C6 C7 123.4(2) . . ? C8 C7 C6 106.7(2) . . ? C8 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? C7 C8 C9 107.1(2) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N22 C9 C10 125.6(2) . . ? N22 C9 C8 110.6(2) . . ? C10 C9 C8 123.7(2) . . ? C11 C10 C9 122.3(2) . . ? C11 C10 C101 119.6(2) . . ? C9 C10 C101 117.8(2) . . ? C10 C11 N23 125.0(2) . . ? C10 C11 C12 124.8(2) . . ? N23 C11 C12 110.1(2) . . ? C13 C12 C11 107.5(2) . . ? C13 C12 H12 126.3 . . ? C11 C12 H12 126.3 . . ? C12 C13 C14 107.0(2) . . ? C12 C13 H13 126.5 . . ? C14 C13 H13 126.5 . . ? N23 C14 C15 125.9(2) . . ? N23 C14 C13 110.7(2) . . ? C15 C14 C13 123.2(2) . . ? C14 C15 C16 121.5(2) . . ? C14 C15 C151 119.4(2) . . ? C16 C15 C151 119.0(2) . . ? N24 C16 C15 125.1(2) . . ? N24 C16 C17 110.7(2) . . ? C15 C16 C17 124.0(2) . . ? C18 C17 C16 106.8(2) . . ? C18 C17 H17 126.6 . . ? C16 C17 H17 126.6 . . ? C17 C18 C19 107.5(2) . . ? C17 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? C20 C19 N24 125.5(2) . . ? C20 C19 C18 123.9(2) . . ? N24 C19 C18 110.3(2) . . ? C19 C20 C1 122.0(2) . . ? C19 C20 C201 119.4(2) . . ? C1 C20 C201 118.6(2) . . ? C5 N1 H1A 120.0 . . ? C5 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C102 C101 C106 118.1(2) . . ? C102 C101 C10 122.5(2) . . ? C106 C101 C10 119.4(2) . . ? C101 C102 C103 120.7(3) . . ? C101 C102 H102 119.6 . . ? C103 C102 H102 119.6 . . ? C104 C103 C102 120.1(3) . . ? C104 C103 H103 119.9 . . ? C102 C103 H103 119.9 . . ? C103 C104 C105 120.0(2) . . ? C103 C104 H104 120.0 . . ? C105 C104 H104 120.0 . . ? C104 C105 C106 120.1(3) . . ? C104 C105 H105 120.0 . . ? C106 C105 H105 120.0 . . ? C101 C106 C105 121.0(3) . . ? C101 C106 H106 119.5 . . ? C105 C106 H106 119.5 . . ? C152 C151 C156 118.0(2) . . ? C152 C151 C15 120.2(2) . . ? C156 C151 C15 121.8(2) . . ? C153 C152 C151 121.2(3) . . ? C153 C152 H152 119.4 . . ? C151 C152 H152 119.4 . . ? C152 C153 C154 120.2(2) . . ? C152 C153 H153 119.9 . . ? C154 C153 H153 119.9 . . ? C153 C154 C155 119.5(2) . . ? C153 C154 H154 120.2 . . ? C155 C154 H154 120.2 . . ? C156 C155 C154 120.2(2) . . ? C156 C155 H155 119.9 . . ? C154 C155 H155 119.9 . . ? C155 C156 C151 120.9(2) . . ? C155 C156 H156 119.5 . . ? C151 C156 H156 119.5 . . ? C202 C201 C206 118.5(2) . . ? C202 C201 C20 119.5(2) . . ? C206 C201 C20 122.0(2) . . ? C201 C202 C203 120.9(2) . . ? C201 C202 H202 119.5 . . ? C203 C202 H202 119.5 . . ? C204 C203 C202 119.9(2) . . ? C204 C203 H203 120.1 . . ? C202 C203 H203 120.1 . . ? C205 C204 C203 119.9(2) . . ? C205 C204 H204 120.1 . . ? C203 C204 H204 120.1 . . ? C204 C205 C206 120.8(2) . . ? C204 C205 H205 119.6 . . ? C206 C205 H205 119.6 . . ? C205 C206 C201 120.0(2) . . ? C205 C206 H206 120.0 . . ? C201 C206 H206 120.0 . . ? 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 N22 Ni N21 C4 12.4(2) . . . . ? N24 Ni N21 C4 -169.4(2) . . . . ? N22 Ni N21 C1 -162.3(2) . . . . ? N24 Ni N21 C1 15.9(2) . . . . ? N23 Ni N22 C6 170.6(2) . . . . ? N21 Ni N22 C6 -9.3(2) . . . . ? N23 Ni N22 C9 -11.3(2) . . . . ? N21 Ni N22 C9 168.7(2) . . . . ? N22 Ni N23 C14 -171.9(2) . . . . ? N24 Ni N23 C14 9.9(2) . . . . ? N22 Ni N23 C11 13.7(2) . . . . ? N24 Ni N23 C11 -164.5(2) . . . . ? N23 Ni N24 C16 -14.5(2) . . . . ? N21 Ni N24 C16 165.5(2) . . . . ? N23 Ni N24 C19 167.5(2) . . . . ? N21 Ni N24 C19 -12.5(2) . . . . ? C4 N21 C1 C20 173.6(2) . . . . ? Ni N21 C1 C20 -10.7(4) . . . . ? C4 N21 C1 C2 -2.3(3) . . . . ? Ni N21 C1 C2 173.40(16) . . . . ? N21 C1 C2 C3 3.3(3) . . . . ? C20 C1 C2 C3 -172.7(2) . . . . ? C1 C2 C3 C4 -2.7(3) . . . . ? C1 N21 C4 C5 169.5(2) . . . . ? Ni N21 C4 C5 -6.2(3) . . . . ? C1 N21 C4 C3 0.6(3) . . . . ? Ni N21 C4 C3 -175.11(16) . . . . ? C2 C3 C4 N21 1.4(3) . . . . ? C2 C3 C4 C5 -167.8(2) . . . . ? N21 C4 C5 N1 179.1(2) . . . . ? C3 C4 C5 N1 -13.2(3) . . . . ? N21 C4 C5 C6 -8.0(4) . . . . ? C3 C4 C5 C6 159.7(2) . . . . ? C9 N22 C6 C5 -178.6(2) . . . . ? Ni N22 C6 C5 -0.2(3) . . . . ? C9 N22 C6 C7 -2.0(3) . . . . ? Ni N22 C6 C7 176.43(17) . . . . ? N1 C5 C6 N22 -175.8(2) . . . . ? C4 C5 C6 N22 11.3(4) . . . . ? N1 C5 C6 C7 7.9(4) . . . . ? C4 C5 C6 C7 -164.9(2) . . . . ? N22 C6 C7 C8 1.3(3) . . . . ? C5 C6 C7 C8 178.0(2) . . . . ? C6 C7 C8 C9 -0.1(3) . . . . ? C6 N22 C9 C10 -176.1(2) . . . . ? Ni N22 C9 C10 5.5(3) . . . . ? C6 N22 C9 C8 1.9(3) . . . . ? Ni N22 C9 C8 -176.48(17) . . . . ? C7 C8 C9 N22 -1.2(3) . . . . ? C7 C8 C9 C10 176.8(2) . . . . ? N22 C9 C10 C11 3.0(4) . . . . ? C8 C9 C10 C11 -174.7(2) . . . . ? N22 C9 C10 C101 176.4(2) . . . . ? C8 C9 C10 C101 -1.3(4) . . . . ? C9 C10 C11 N23 -0.5(4) . . . . ? C101 C10 C11 N23 -173.8(2) . . . . ? C9 C10 C11 C12 174.8(2) . . . . ? C101 C10 C11 C12 1.5(4) . . . . ? C14 N23 C11 C10 174.1(2) . . . . ? Ni N23 C11 C10 -10.5(4) . . . . ? C14 N23 C11 C12 -1.8(3) . . . . ? Ni N23 C11 C12 173.64(17) . . . . ? C10 C11 C12 C13 -173.7(2) . . . . ? N23 C11 C12 C13 2.2(3) . . . . ? C11 C12 C13 C14 -1.6(3) . . . . ? C11 N23 C14 C15 176.4(2) . . . . ? Ni N23 C14 C15 0.9(3) . . . . ? C11 N23 C14 C13 0.8(3) . . . . ? Ni N23 C14 C13 -174.65(16) . . . . ? C12 C13 C14 N23 0.5(3) . . . . ? C12 C13 C14 C15 -175.2(2) . . . . ? N23 C14 C15 C16 -12.2(4) . . . . ? C13 C14 C15 C16 162.9(2) . . . . ? N23 C14 C15 C151 171.5(2) . . . . ? C13 C14 C15 C151 -13.5(3) . . . . ? C19 N24 C16 C15 -172.9(2) . . . . ? Ni N24 C16 C15 8.7(3) . . . . ? C19 N24 C16 C17 2.5(3) . . . . ? Ni N24 C16 C17 -175.91(16) . . . . ? C14 C15 C16 N24 7.2(4) . . . . ? C151 C15 C16 N24 -176.5(2) . . . . ? C14 C15 C16 C17 -167.6(2) . . . . ? C151 C15 C16 C17 8.8(4) . . . . ? N24 C16 C17 C18 -3.5(3) . . . . ? C15 C16 C17 C18 172.0(2) . . . . ? C16 C17 C18 C19 2.9(3) . . . . ? C16 N24 C19 C20 -174.8(2) . . . . ? Ni N24 C19 C20 3.5(4) . . . . ? C16 N24 C19 C18 -0.7(3) . . . . ? Ni N24 C19 C18 177.71(16) . . . . ? C17 C18 C19 C20 172.8(2) . . . . ? C17 C18 C19 N24 -1.5(3) . . . . ? N24 C19 C20 C1 7.9(4) . . . . ? C18 C19 C20 C1 -165.5(2) . . . . ? N24 C19 C20 C201 -174.6(2) . . . . ? C18 C19 C20 C201 11.9(4) . . . . ? N21 C1 C20 C19 -4.2(4) . . . . ? C2 C1 C20 C19 171.1(2) . . . . ? N21 C1 C20 C201 178.3(2) . . . . ? C2 C1 C20 C201 -6.3(4) . . . . ? C11 C10 C101 C102 -86.9(3) . . . . ? C9 C10 C101 C102 99.5(3) . . . . ? C11 C10 C101 C106 93.3(3) . . . . ? C9 C10 C101 C106 -80.2(3) . . . . ? C106 C101 C102 C103 -1.3(4) . . . . ? C10 C101 C102 C103 179.0(3) . . . . ? C101 C102 C103 C104 0.8(5) . . . . ? C102 C103 C104 C105 -0.2(5) . . . . ? C103 C104 C105 C106 0.1(5) . . . . ? C102 C101 C106 C105 1.2(4) . . . . ? C10 C101 C106 C105 -179.0(3) . . . . ? C104 C105 C106 C101 -0.7(5) . . . . ? C14 C15 C151 C152 -74.3(3) . . . . ? C16 C15 C151 C152 109.2(3) . . . . ? C14 C15 C151 C156 106.5(3) . . . . ? C16 C15 C151 C156 -69.9(3) . . . . ? C156 C151 C152 C153 1.8(3) . . . . ? C15 C151 C152 C153 -177.4(2) . . . . ? C151 C152 C153 C154 -1.2(4) . . . . ? C152 C153 C154 C155 -0.1(4) . . . . ? C153 C154 C155 C156 0.7(3) . . . . ? C154 C155 C156 C151 -0.1(3) . . . . ? C152 C151 C156 C155 -1.2(3) . . . . ? C15 C151 C156 C155 178.0(2) . . . . ? C19 C20 C201 C202 63.6(3) . . . . ? C1 C20 C201 C202 -118.9(3) . . . . ? C19 C20 C201 C206 -118.0(3) . . . . ? C1 C20 C201 C206 59.5(3) . . . . ? C206 C201 C202 C203 -0.7(4) . . . . ? C20 C201 C202 C203 177.8(2) . . . . ? C201 C202 C203 C204 0.2(4) . . . . ? C202 C203 C204 C205 0.0(4) . . . . ? C203 C204 C205 C206 0.1(4) . . . . ? C204 C205 C206 C201 -0.6(4) . . . . ? C202 C201 C206 C205 0.8(4) . . . . ? C20 C201 C206 C205 -177.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.388 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.055 #===END