# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Albert Escuer' _publ_contact_author_email albert.escuer@qi.ub.es loop_ _publ_author_name 'Jordi Esteban' 'Merce Font-Bardia' 'Albert Escuer' # Attachment '- joom73a.cif' data_joom73a _database_code_depnum_ccdc_archive 'CCDC 859276' #TrackingRef '- joom73a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H54 N24 Ni3 O2, C H4 O' _chemical_formula_sum 'C37 H58 N24 Ni3 O3' _chemical_formula_weight 1063.20 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.183(5) _cell_length_b 12.582(4) _cell_length_c 16.689(5) _cell_angle_alpha 93.84(2) _cell_angle_beta 91.81(2) _cell_angle_gamma 107.65(2) _cell_volume 2428.7(15) _cell_formula_units_Z 2 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 1824 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.214 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(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 'MAR345 with image plate detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20649 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 32.26 _reflns_number_total 12039 _reflns_number_gt 8888 _reflns_threshold_expression >2sigma(I) _computing_data_collection MARXDS _computing_cell_refinement AUTOMAR _computing_data_reduction MARSCALE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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. 21 of atomic sites that are flagged as handled with Uiso or Uij restraints. 2 of atomic sites that are flagged as distance restrained. Regarding the crystal refinement parameter, for the structural resolution, it has been considered only reflections that have a value max of theta = 25\% (ACTA 50). Reflections between 25\% and 32\% have not been taken into account due to the poor quality of the reflections over this value. The poor quality of reflections could be due to the fact that the crystal does not diffract very well and to the kind of detector (image plate with spindle axis only) that was used. Other attempts of crystallization were done, but no single crystals of better quality were obtained. ; _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^)+(0.0698P)^2^+0.4960P] 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 12039 _refine_ls_number_parameters 598 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1423 _refine_ls_wR_factor_gt 0.1318 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.56139(3) 0.58155(3) 0.17889(2) 0.03658(10) Uani 1 1 d U . . Ni2 Ni 0.61352(3) 0.86480(3) 0.25508(2) 0.03063(9) Uani 1 1 d . . . Ni3 Ni 0.90888(3) 0.96756(3) 0.32435(2) 0.03352(10) Uani 1 1 d . . . O1 O 0.48274(19) 0.62747(17) 0.27802(13) 0.0390(5) Uani 1 1 d . . . O2 O 0.83876(17) 1.04012(17) 0.23766(12) 0.0350(4) Uani 1 1 d . . . N3 N 0.4922(2) 0.73372(19) 0.29727(15) 0.0334(5) Uani 1 1 d . . . N6 N 0.7272(2) 1.00233(19) 0.21494(14) 0.0308(5) Uani 1 1 d . . . N7 N 0.9376(3) 0.8544(2) 0.23560(16) 0.0435(6) Uani 1 1 d . . . H7A H 0.9764 0.8137 0.2598 0.052 Uiso 1 1 calc R . . H7B H 0.8683 0.8069 0.2182 0.052 Uiso 1 1 calc R . . N8 N 1.0647(2) 1.1027(3) 0.30546(19) 0.0477(7) Uani 1 1 d . . . N9 N 0.8685(2) 1.0654(2) 0.41962(16) 0.0417(6) Uani 1 1 d . . . H9A H 0.7943 1.0328 0.4301 0.050 Uiso 1 1 calc R . . H9B H 0.9117 1.0617 0.4635 0.050 Uiso 1 1 calc R . . N10 N 0.4301(2) 0.5930(2) 0.09823(18) 0.0459(6) Uani 1 1 d . . . H10A H 0.4447 0.6656 0.0891 0.055 Uiso 1 1 calc R . . H10B H 0.4361 0.5562 0.0513 0.055 Uiso 1 1 calc R . . N11 N 0.4615(3) 0.4104(2) 0.1999(2) 0.0519(6) Uani 1 1 d U . . N12 N 0.7007(3) 0.5792(3) 0.25516(19) 0.0513(7) Uani 1 1 d . . . H12A H 0.7577 0.5764 0.2229 0.062 Uiso 1 1 calc R . . H12B H 0.7246 0.6465 0.2832 0.062 Uiso 1 1 calc R . . N13 N 0.6554(2) 0.7558(2) 0.16816(15) 0.0358(5) Uani 1 1 d . . . N14 N 0.6808(2) 0.7896(2) 0.10333(16) 0.0398(6) Uani 1 1 d . . . N15 N 0.7072(4) 0.8226(3) 0.0415(2) 0.0657(9) Uani 1 1 d . . . N16 N 0.7414(2) 0.8451(2) 0.33612(15) 0.0362(5) Uani 1 1 d . . . N17 N 0.7130(2) 0.8012(2) 0.39668(15) 0.0347(5) Uani 1 1 d U . . N18 N 0.6844(3) 0.7579(3) 0.45458(18) 0.0535(7) Uani 1 1 d U . . N19 N 0.9827(3) 0.8905(2) 0.41414(18) 0.0463(6) Uani 1 1 d . . . N20 N 0.9609(2) 0.7923(2) 0.40443(16) 0.0422(6) Uani 1 1 d . . . N21 N 0.9393(3) 0.6948(3) 0.3946(2) 0.0574(8) Uani 1 1 d . . . N22 N 0.6420(3) 0.5361(2) 0.07616(18) 0.0479(7) Uani 1 1 d . . . N23 N 0.7445(3) 0.5780(2) 0.07500(18) 0.0447(6) Uani 1 1 d . . . N24 N 0.8447(3) 0.6151(3) 0.0730(2) 0.0626(9) Uani 1 1 d . . . N1 N 0.3907(3) 0.5935(3) 0.4371(2) 0.0637(9) Uani 1 1 d U . . C1 C 0.3119(4) 0.5131(3) 0.4781(2) 0.0600(10) Uani 1 1 d . . . H1 H 0.3365 0.4617 0.5054 0.072 Uiso 1 1 calc R . . C2 C 0.1973(4) 0.5100(3) 0.4779(2) 0.0557(9) Uani 1 1 d . . . H2 H 0.1448 0.4573 0.5056 0.067 Uiso 1 1 calc R . . C3 C 0.1618(3) 0.5865(3) 0.4361(2) 0.0538(9) Uani 1 1 d U . . H3 H 0.0848 0.5844 0.4358 0.065 Uiso 1 1 calc R . . C4 C 0.2376(2) 0.6647(2) 0.39538(17) 0.0345(6) Uani 1 1 d U . . H4 H 0.2123 0.7149 0.3672 0.041 Uiso 1 1 calc R . . C5 C 0.3501(3) 0.6687(3) 0.39640(18) 0.0385(6) Uani 1 1 d U . . C6 C 0.4290(3) 0.7564(2) 0.35363(17) 0.0331(6) Uani 1 1 d . . . N2 N 0.5388(2) 0.9472(2) 0.34135(15) 0.0348(5) Uani 1 1 d . . . C7 C 0.4446(3) 0.8758(2) 0.37301(18) 0.0346(6) Uani 1 1 d . . . C8 C 0.3723(3) 0.9170(3) 0.4203(2) 0.0415(7) Uani 1 1 d . . . H8 H 0.3093 0.8681 0.4424 0.050 Uiso 1 1 calc R . . C9 C 0.3951(3) 1.0317(3) 0.4343(2) 0.0470(8) Uani 1 1 d . . . H9 H 0.3471 1.0602 0.4656 0.056 Uiso 1 1 calc R . . C10 C 0.4891(3) 1.1033(3) 0.4015(2) 0.0466(7) Uani 1 1 d U . . H10 H 0.5051 1.1804 0.4107 0.056 Uiso 1 1 calc R . . C11 C 0.5594(3) 1.0597(3) 0.35496(19) 0.0407(6) Uani 1 1 d U . . H11 H 0.6221 1.1082 0.3324 0.049 Uiso 1 1 calc R . . N4 N 0.5110(2) 0.9110(2) 0.17187(14) 0.0323(5) Uani 1 1 d . . . C12 C 0.3946(3) 0.8607(3) 0.15473(19) 0.0409(7) Uani 1 1 d . . . H12 H 0.3576 0.7944 0.1773 0.049 Uiso 1 1 calc R . . C13 C 0.3320(3) 0.9065(3) 0.1050(2) 0.0452(7) Uani 1 1 d . . . H13 H 0.2540 0.8702 0.0928 0.054 Uiso 1 1 calc R . . C14 C 0.3859(3) 1.0071(3) 0.0730(2) 0.0471(8) Uani 1 1 d . . . H14 H 0.3437 1.0394 0.0404 0.056 Uiso 1 1 calc R . . C15 C 0.5034(3) 1.0594(3) 0.0900(2) 0.0426(7) Uani 1 1 d . . . H15 H 0.5404 1.1266 0.0686 0.051 Uiso 1 1 calc R . . C16 C 0.5649(3) 1.0097(2) 0.13942(17) 0.0323(6) Uani 1 1 d . . . C17 C 0.6893(3) 1.0531(2) 0.15940(17) 0.0335(6) Uani 1 1 d . . . N5 N 0.8614(3) 1.1315(3) 0.0794(2) 0.0578(8) Uani 1 1 d U . . C18 C 0.7675(3) 1.1450(3) 0.11899(19) 0.0396(6) Uani 1 1 d U . . C19 C 0.7446(3) 1.2445(3) 0.1232(2) 0.0515(8) Uani 1 1 d U . . H19 H 0.6814 1.2532 0.1495 0.062 Uiso 1 1 calc R . . C20 C 0.8173(5) 1.3309(4) 0.0875(3) 0.0838(15) Uani 1 1 d U . . H20 H 0.8017 1.3989 0.0895 0.101 Uiso 1 1 calc R . . C21 C 0.9127(4) 1.3224(4) 0.0487(3) 0.0713(12) Uani 1 1 d . . . H21 H 0.9613 1.3838 0.0261 0.086 Uiso 1 1 calc R . . C22 C 0.9347(3) 1.2209(3) 0.0442(2) 0.0538(9) Uani 1 1 d . . . H22 H 0.9980 1.2126 0.0178 0.065 Uiso 1 1 calc R . . C23 C 0.9995(4) 0.8952(4) 0.1641(2) 0.0585(10) Uani 1 1 d . . . H23A H 0.9505 0.9227 0.1295 0.070 Uiso 1 1 calc R . . H23B H 1.0162 0.8335 0.1343 0.070 Uiso 1 1 calc R . . C24 C 1.1094(4) 0.9864(4) 0.1856(3) 0.0725(12) Uani 1 1 d . . . H24A H 1.1531 0.9995 0.1377 0.087 Uiso 1 1 calc R . . H24B H 1.1539 0.9598 0.2244 0.087 Uiso 1 1 calc R . . C25 C 1.1000(4) 1.0968(4) 0.2199(3) 0.0619(10) Uani 1 1 d . . . H25A H 1.0447 1.1170 0.1859 0.074 Uiso 1 1 calc R . . H25B H 1.1742 1.1530 0.2166 0.074 Uiso 1 1 calc R . . C26 C 1.0469(3) 1.2145(3) 0.3157(2) 0.0532(8) Uani 1 1 d U . . H26A H 0.9911 1.2182 0.2740 0.064 Uiso 1 1 calc R . . H26B H 1.1191 1.2707 0.3069 0.064 Uiso 1 1 calc R . . C27 C 1.0057(4) 1.2454(4) 0.3963(3) 0.0644(11) Uani 1 1 d U . . H27A H 1.0550 1.2318 0.4387 0.077 Uiso 1 1 calc R . . H27B H 1.0148 1.3249 0.4004 0.077 Uiso 1 1 calc R . . C28 C 0.8833(4) 1.1833(3) 0.4103(2) 0.0547(9) Uani 1 1 d . . . H28A H 0.8600 1.2166 0.4584 0.066 Uiso 1 1 calc R . . H28B H 0.8340 1.1896 0.3653 0.066 Uiso 1 1 calc R . . C29 C 1.1587(4) 1.0984(4) 0.3601(3) 0.0777(14) Uani 1 1 d . . . H29A H 1.1695 1.0259 0.3530 0.117 Uiso 1 1 calc R . . H29B H 1.1401 1.1117 0.4146 0.117 Uiso 1 1 calc R . . H29C H 1.2283 1.1547 0.3487 0.117 Uiso 1 1 calc R . . C30 C 0.3089(4) 0.5511(4) 0.1201(3) 0.0655(11) Uani 1 1 d . . . H30A H 0.2588 0.5640 0.0780 0.079 Uiso 1 1 calc R . . H30B H 0.2987 0.5914 0.1695 0.079 Uiso 1 1 calc R . . C31 C 0.2764(4) 0.4265(4) 0.1315(3) 0.0689(11) Uani 1 1 d U . . H31A H 0.1938 0.3975 0.1368 0.083 Uiso 1 1 calc R . . H31B H 0.2954 0.3877 0.0843 0.083 Uiso 1 1 calc R . . C32 C 0.3373(4) 0.4045(4) 0.2034(3) 0.0663(10) Uani 1 1 d U . . H32A H 0.2953 0.3303 0.2180 0.080 Uiso 1 1 calc R . . H32B H 0.3316 0.4571 0.2471 0.080 Uiso 1 1 calc R . . C33 C 0.4934(5) 0.3770(4) 0.2751(3) 0.0777(12) Uani 1 1 d U . . H33A H 0.4465 0.3006 0.2805 0.093 Uiso 1 1 calc R . . H33B H 0.4755 0.4239 0.3181 0.093 Uiso 1 1 calc R . . C34 C 0.6262(5) 0.3840(4) 0.2868(3) 0.0813(10) Uani 1 1 d DU . . H34A H 0.6358 0.3372 0.3287 0.098 Uiso 1 1 calc R . . H34B H 0.6520 0.3571 0.2372 0.098 Uiso 1 1 calc R . . C35 C 0.6968(5) 0.5028(4) 0.3094(3) 0.0813(10) Uani 1 1 d D . . H35A H 0.6679 0.5277 0.3583 0.098 Uiso 1 1 calc R . . H35B H 0.7753 0.5037 0.3221 0.098 Uiso 1 1 calc R . . C36 C 0.4677(5) 0.3320(4) 0.1315(3) 0.0887(17) Uani 1 1 d U . . H36A H 0.4453 0.3575 0.0824 0.133 Uiso 1 1 calc R . . H36B H 0.4165 0.2589 0.1387 0.133 Uiso 1 1 calc R . . H36C H 0.5452 0.3288 0.1289 0.133 Uiso 1 1 calc R . . C1W C 0.0656(5) 0.6204(5) 0.2186(4) 0.0930(17) Uani 1 1 d . . . H1W H 0.1101 0.5694 0.2127 0.112 Uiso 1 1 calc R . . H1WA H 0.0308 0.6259 0.1672 0.112 Uiso 1 1 calc R . . H1WB H 0.0063 0.5935 0.2554 0.112 Uiso 1 1 calc R . . O1W O 0.1407(3) 0.7304(3) 0.2495(2) 0.0860(10) Uani 1 1 d . . . H1WO H 0.2081 0.7339 0.2430 0.129 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 0.0359(2) 0.03288(19) 0.0394(2) 0.00056(16) 0.00249(16) 0.00859(15) Ni2 0.03036(18) 0.02877(17) 0.03187(18) 0.00253(14) 0.00109(14) 0.00776(14) Ni3 0.03278(19) 0.03273(18) 0.03357(19) 0.00282(15) -0.00006(15) 0.00798(15) O1 0.0420(12) 0.0327(10) 0.0411(11) 0.0005(9) 0.0043(9) 0.0101(9) O2 0.0314(10) 0.0349(10) 0.0365(10) 0.0062(9) -0.0014(8) 0.0064(8) N3 0.0354(12) 0.0286(11) 0.0349(12) 0.0007(10) -0.0004(10) 0.0083(9) N6 0.0304(11) 0.0311(11) 0.0322(11) 0.0015(10) 0.0021(9) 0.0115(9) N7 0.0499(16) 0.0415(14) 0.0412(14) 0.0050(12) 0.0040(12) 0.0168(12) N8 0.0387(14) 0.0467(15) 0.0529(16) 0.0077(14) 0.0000(12) 0.0055(12) N9 0.0459(15) 0.0398(13) 0.0373(13) 0.0003(12) 0.0007(11) 0.0107(12) N10 0.0425(15) 0.0464(15) 0.0479(15) -0.0016(13) 0.0015(12) 0.0132(12) N11 0.0508(14) 0.0380(11) 0.0615(16) 0.0047(12) 0.0079(14) 0.0050(11) N12 0.0511(17) 0.0452(15) 0.0571(18) -0.0017(14) -0.0068(14) 0.0160(13) N13 0.0379(13) 0.0345(12) 0.0348(12) -0.0004(10) 0.0020(10) 0.0114(10) N14 0.0459(15) 0.0366(13) 0.0384(13) 0.0010(11) 0.0005(11) 0.0153(11) N15 0.095(3) 0.062(2) 0.0474(17) 0.0110(16) 0.0091(18) 0.034(2) N16 0.0346(13) 0.0361(12) 0.0357(12) 0.0033(11) 0.0019(10) 0.0076(10) N17 0.0344(12) 0.0326(12) 0.0363(11) 0.0008(9) -0.0002(10) 0.0098(10) N18 0.0554(18) 0.0595(19) 0.0460(14) 0.0137(13) 0.0068(13) 0.0156(15) N19 0.0474(16) 0.0441(15) 0.0462(15) 0.0030(13) -0.0063(12) 0.0133(13) N20 0.0432(14) 0.0439(14) 0.0387(13) 0.0039(12) -0.0010(11) 0.0124(12) N21 0.067(2) 0.0501(17) 0.0562(18) 0.0060(15) 0.0004(16) 0.0192(16) N22 0.0417(15) 0.0461(15) 0.0517(16) -0.0059(14) 0.0036(13) 0.0092(12) N23 0.0449(16) 0.0421(14) 0.0483(15) 0.0020(13) 0.0036(12) 0.0154(12) N24 0.0511(19) 0.065(2) 0.068(2) 0.0071(18) 0.0045(16) 0.0121(16) N1 0.072(2) 0.060(2) 0.065(2) 0.0176(16) 0.0051(17) 0.0261(17) C1 0.074(3) 0.051(2) 0.054(2) 0.0124(18) 0.0036(19) 0.0158(19) C2 0.062(2) 0.050(2) 0.051(2) 0.0065(17) 0.0087(17) 0.0087(18) C3 0.0463(19) 0.0480(19) 0.062(2) 0.0112(16) 0.0124(16) 0.0046(15) C4 0.0308(13) 0.0362(14) 0.0364(14) 0.0050(11) 0.0018(11) 0.0097(11) C5 0.0385(15) 0.0387(14) 0.0358(14) 0.0016(12) 0.0039(12) 0.0080(12) C6 0.0336(14) 0.0329(13) 0.0329(13) 0.0048(12) 0.0031(11) 0.0097(11) N2 0.0363(13) 0.0321(12) 0.0348(12) 0.0013(10) 0.0014(10) 0.0091(10) C7 0.0322(14) 0.0355(14) 0.0354(14) 0.0038(12) 0.0044(11) 0.0087(11) C8 0.0422(16) 0.0397(15) 0.0432(16) 0.0017(14) 0.0045(13) 0.0133(13) C9 0.0495(19) 0.0451(17) 0.0483(18) 0.0009(15) 0.0041(15) 0.0179(15) C10 0.0526(19) 0.0405(16) 0.0478(18) 0.0000(15) 0.0038(14) 0.0164(14) C11 0.0449(17) 0.0355(14) 0.0416(16) 0.0047(13) 0.0044(13) 0.0118(12) N4 0.0315(12) 0.0321(11) 0.0335(11) 0.0021(10) 0.0006(9) 0.0101(9) C12 0.0403(16) 0.0420(16) 0.0386(15) 0.0021(14) -0.0006(13) 0.0102(13) C13 0.0429(17) 0.0480(18) 0.0458(17) 0.0028(15) 0.0017(14) 0.0158(14) C14 0.0433(18) 0.0537(19) 0.0476(18) 0.0057(16) -0.0008(14) 0.0199(15) C15 0.0442(17) 0.0440(16) 0.0431(16) 0.0033(14) 0.0027(14) 0.0185(14) C16 0.0355(14) 0.0341(13) 0.0301(12) 0.0025(11) 0.0052(11) 0.0146(11) C17 0.0364(14) 0.0323(13) 0.0328(13) 0.0047(11) 0.0029(11) 0.0115(11) N5 0.0529(17) 0.068(2) 0.0533(18) 0.0072(16) 0.0087(14) 0.0196(16) C18 0.0414(15) 0.0369(14) 0.0386(15) 0.0062(13) -0.0001(11) 0.0085(12) C19 0.054(2) 0.0424(17) 0.062(2) 0.0090(15) 0.0096(17) 0.0204(15) C20 0.093(4) 0.057(2) 0.102(4) 0.028(2) 0.026(3) 0.017(2) C21 0.072(3) 0.060(2) 0.075(3) 0.021(2) 0.011(2) 0.006(2) C22 0.0449(19) 0.062(2) 0.051(2) 0.0107(18) 0.0042(16) 0.0089(17) C23 0.064(2) 0.060(2) 0.054(2) 0.0058(19) 0.0130(19) 0.021(2) C24 0.067(3) 0.069(3) 0.082(3) 0.009(2) 0.018(2) 0.020(2) C25 0.055(2) 0.059(2) 0.067(3) 0.007(2) 0.0097(19) 0.0093(19) C26 0.050(2) 0.0470(19) 0.0555(18) 0.0077(16) 0.0024(16) 0.0039(16) C27 0.074(3) 0.051(2) 0.056(2) 0.0005(19) 0.0037(19) 0.003(2) C28 0.063(2) 0.0488(19) 0.053(2) 0.0009(17) 0.0038(18) 0.0188(18) C29 0.056(3) 0.082(3) 0.087(3) 0.025(3) -0.011(2) 0.006(2) C30 0.053(2) 0.072(3) 0.069(3) -0.005(2) 0.003(2) 0.017(2) C31 0.052(2) 0.072(3) 0.074(3) 0.001(2) 0.0057(19) 0.007(2) C32 0.0542(17) 0.062(2) 0.080(3) 0.008(2) 0.0113(19) 0.0113(19) C33 0.090(2) 0.067(3) 0.075(3) 0.021(2) 0.003(2) 0.019(3) C34 0.086(2) 0.068(2) 0.081(2) 0.0160(19) -0.0098(19) 0.0094(18) C35 0.086(2) 0.068(2) 0.081(2) 0.0160(19) -0.0098(19) 0.0094(18) C36 0.106(4) 0.064(3) 0.088(3) -0.016(2) 0.015(3) 0.017(3) C1W 0.079(4) 0.121(5) 0.086(4) 0.004(4) 0.002(3) 0.044(4) O1W 0.077(2) 0.097(3) 0.084(2) 0.016(2) -0.0012(19) 0.025(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 O1 2.073(2) . ? Ni1 N12 2.098(3) . ? Ni1 N10 2.103(3) . ? Ni1 N22 2.132(3) . ? Ni1 N13 2.166(3) . ? Ni1 N11 2.186(3) . ? Ni2 N6 2.030(2) . ? Ni2 N3 2.035(3) . ? Ni2 N4 2.065(2) . ? Ni2 N2 2.105(3) . ? Ni2 N13 2.110(3) . ? Ni2 N16 2.113(3) . ? Ni3 O2 2.056(2) . ? Ni3 N7 2.097(3) . ? Ni3 N9 2.107(3) . ? Ni3 N19 2.152(3) . ? Ni3 N16 2.176(3) . ? Ni3 N8 2.178(3) . ? O1 N3 1.323(3) . ? O2 N6 1.330(3) . ? N3 C6 1.305(4) . ? N6 C17 1.308(4) . ? N7 C23 1.470(5) . ? N7 H7A 0.9000 . ? N7 H7B 0.9000 . ? N8 C29 1.457(5) . ? N8 C26 1.488(5) . ? N8 C25 1.508(5) . ? N9 C28 1.459(5) . ? N9 H9A 0.9000 . ? N9 H9B 0.9000 . ? N10 C30 1.475(5) . ? N10 H10A 0.9000 . ? N10 H10B 0.9000 . ? N11 C33 1.429(6) . ? N11 C36 1.477(5) . ? N11 C32 1.496(5) . ? N12 C35 1.355(5) . ? N12 H12A 0.9000 . ? N12 H12B 0.9000 . ? N13 N14 1.204(4) . ? N14 N15 1.157(4) . ? N16 N17 1.195(3) . ? N17 N18 1.152(4) . ? N19 N20 1.181(4) . ? N20 N21 1.173(4) . ? N22 N23 1.200(4) . ? N23 N24 1.170(4) . ? N1 C5 1.396(5) . ? N1 C1 1.399(5) . ? C1 C2 1.384(6) . ? C1 H1 0.9300 . ? C2 C3 1.388(6) . ? C2 H2 0.9300 . ? C3 C4 1.364(4) . ? C3 H3 0.9300 . ? C4 C5 1.355(4) . ? C4 H4 0.9300 . ? C5 C6 1.468(4) . ? C6 C7 1.468(4) . ? N2 C11 1.362(4) . ? N2 C7 1.371(4) . ? C7 C8 1.391(4) . ? C8 C9 1.386(5) . ? C8 H8 0.9300 . ? C9 C10 1.380(5) . ? C9 H9 0.9300 . ? C10 C11 1.381(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? N4 C16 1.372(4) . ? N4 C12 1.378(4) . ? C12 C13 1.376(5) . ? C12 H12 0.9300 . ? C13 C14 1.387(5) . ? C13 H13 0.9300 . ? C14 C15 1.393(5) . ? C14 H14 0.9300 . ? C15 C16 1.395(4) . ? C15 H15 0.9300 . ? C16 C17 1.466(4) . ? C17 C18 1.475(4) . ? N5 C22 1.385(5) . ? N5 C18 1.387(5) . ? C18 C19 1.361(5) . ? C19 C20 1.362(6) . ? C19 H19 0.9300 . ? C20 C21 1.377(7) . ? C20 H20 0.9300 . ? C21 C22 1.380(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.491(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.505(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.518(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.493(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.523(6) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.477(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.599(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.497(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C1W O1W 1.457(7) . ? C1W H1W 0.9600 . ? C1W H1WA 0.9600 . ? C1W H1WB 0.9600 . ? O1W H1WO 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 N12 89.20(11) . . ? O1 Ni1 N10 92.75(10) . . ? N12 Ni1 N10 175.90(12) . . ? O1 Ni1 N22 179.25(11) . . ? N12 Ni1 N22 91.26(13) . . ? N10 Ni1 N22 86.75(12) . . ? O1 Ni1 N13 89.89(9) . . ? N12 Ni1 N13 86.12(11) . . ? N10 Ni1 N13 90.28(11) . . ? N22 Ni1 N13 89.55(11) . . ? O1 Ni1 N11 85.08(11) . . ? N12 Ni1 N11 93.02(13) . . ? N10 Ni1 N11 90.74(12) . . ? N22 Ni1 N11 95.49(12) . . ? N13 Ni1 N11 174.91(11) . . ? N6 Ni2 N3 175.95(10) . . ? N6 Ni2 N4 78.45(10) . . ? N3 Ni2 N4 99.23(10) . . ? N6 Ni2 N2 97.96(10) . . ? N3 Ni2 N2 78.47(10) . . ? N4 Ni2 N2 85.38(10) . . ? N6 Ni2 N13 92.77(10) . . ? N3 Ni2 N13 90.61(10) . . ? N4 Ni2 N13 91.78(10) . . ? N2 Ni2 N13 168.10(10) . . ? N6 Ni2 N16 91.13(10) . . ? N3 Ni2 N16 91.11(10) . . ? N4 Ni2 N16 169.51(10) . . ? N2 Ni2 N16 95.03(10) . . ? N13 Ni2 N16 89.87(10) . . ? O2 Ni3 N7 89.92(10) . . ? O2 Ni3 N9 93.42(10) . . ? N7 Ni3 N9 173.52(11) . . ? O2 Ni3 N19 179.42(10) . . ? N7 Ni3 N19 89.50(12) . . ? N9 Ni3 N19 87.16(11) . . ? O2 Ni3 N16 90.42(9) . . ? N7 Ni3 N16 86.97(11) . . ? N9 Ni3 N16 87.45(11) . . ? N19 Ni3 N16 89.59(11) . . ? O2 Ni3 N8 82.78(10) . . ? N7 Ni3 N8 95.27(12) . . ? N9 Ni3 N8 90.66(12) . . ? N19 Ni3 N8 97.24(12) . . ? N16 Ni3 N8 172.82(11) . . ? N3 O1 Ni1 120.80(17) . . ? N6 O2 Ni3 121.61(16) . . ? C6 N3 O1 118.0(2) . . ? C6 N3 Ni2 117.5(2) . . ? O1 N3 Ni2 124.06(19) . . ? C17 N6 O2 117.9(2) . . ? C17 N6 Ni2 117.5(2) . . ? O2 N6 Ni2 124.47(17) . . ? C23 N7 Ni3 120.3(2) . . ? C23 N7 H7A 107.2 . . ? Ni3 N7 H7A 107.2 . . ? C23 N7 H7B 107.2 . . ? Ni3 N7 H7B 107.2 . . ? H7A N7 H7B 106.9 . . ? C29 N8 C26 110.1(3) . . ? C29 N8 C25 109.5(3) . . ? C26 N8 C25 103.0(3) . . ? C29 N8 Ni3 110.0(3) . . ? C26 N8 Ni3 112.2(2) . . ? C25 N8 Ni3 111.7(2) . . ? C28 N9 Ni3 118.9(2) . . ? C28 N9 H9A 107.6 . . ? Ni3 N9 H9A 107.6 . . ? C28 N9 H9B 107.6 . . ? Ni3 N9 H9B 107.6 . . ? H9A N9 H9B 107.0 . . ? C30 N10 Ni1 119.1(3) . . ? C30 N10 H10A 107.6 . . ? Ni1 N10 H10A 107.6 . . ? C30 N10 H10B 107.6 . . ? Ni1 N10 H10B 107.6 . . ? H10A N10 H10B 107.0 . . ? C33 N11 C36 112.4(4) . . ? C33 N11 C32 106.3(4) . . ? C36 N11 C32 106.1(3) . . ? C33 N11 Ni1 112.7(3) . . ? C36 N11 Ni1 110.5(3) . . ? C32 N11 Ni1 108.5(2) . . ? C35 N12 Ni1 125.0(3) . . ? C35 N12 H12A 106.1 . . ? Ni1 N12 H12A 106.1 . . ? C35 N12 H12B 106.1 . . ? Ni1 N12 H12B 106.1 . . ? H12A N12 H12B 106.3 . . ? N14 N13 Ni2 117.7(2) . . ? N14 N13 Ni1 120.7(2) . . ? Ni2 N13 Ni1 112.86(12) . . ? N15 N14 N13 178.9(4) . . ? N17 N16 Ni2 119.2(2) . . ? N17 N16 Ni3 123.4(2) . . ? Ni2 N16 Ni3 112.18(12) . . ? N18 N17 N16 179.2(4) . . ? N20 N19 Ni3 115.8(2) . . ? N21 N20 N19 179.8(4) . . ? N23 N22 Ni1 116.6(2) . . ? N24 N23 N22 177.6(4) . . ? C5 N1 C1 118.2(4) . . ? C2 C1 N1 120.1(4) . . ? C2 C1 H1 120.0 . . ? N1 C1 H1 120.0 . . ? C1 C2 C3 119.2(4) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 121.2(4) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.5(3) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 N1 121.8(3) . . ? C4 C5 C6 117.5(3) . . ? N1 C5 C6 120.7(3) . . ? N3 C6 C7 115.4(3) . . ? N3 C6 C5 122.3(3) . . ? C7 C6 C5 122.3(3) . . ? C11 N2 C7 119.2(3) . . ? C11 N2 Ni2 126.9(2) . . ? C7 N2 Ni2 112.49(19) . . ? N2 C7 C8 120.7(3) . . ? N2 C7 C6 114.9(3) . . ? C8 C7 C6 124.3(3) . . ? C9 C8 C7 119.3(3) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 119.4(3) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? N2 C11 C10 121.5(3) . . ? N2 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C16 N4 C12 119.1(3) . . ? C16 N4 Ni2 114.01(19) . . ? C12 N4 Ni2 126.4(2) . . ? C13 C12 N4 121.3(3) . . ? C13 C12 H12 119.3 . . ? N4 C12 H12 119.3 . . ? C12 C13 C14 119.7(3) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 119.8(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 119.1(3) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? N4 C16 C15 121.0(3) . . ? N4 C16 C17 114.2(2) . . ? C15 C16 C17 124.9(3) . . ? N6 C17 C16 114.9(3) . . ? N6 C17 C18 121.9(3) . . ? C16 C17 C18 123.1(3) . . ? C22 N5 C18 119.9(3) . . ? C19 C18 N5 121.2(3) . . ? C19 C18 C17 117.1(3) . . ? N5 C18 C17 121.7(3) . . ? C18 C19 C20 117.8(4) . . ? C18 C19 H19 121.1 . . ? C20 C19 H19 121.1 . . ? C19 C20 C21 123.2(5) . . ? C19 C20 H20 118.4 . . ? C21 C20 H20 118.4 . . ? C20 C21 C22 118.5(4) . . ? C20 C21 H21 120.8 . . ? C22 C21 H21 120.8 . . ? C21 C22 N5 119.3(4) . . ? C21 C22 H22 120.3 . . ? N5 C22 H22 120.3 . . ? N7 C23 C24 111.9(4) . . ? N7 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? N7 C23 H23B 109.2 . . ? C24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 C24 C25 117.1(4) . . ? C23 C24 H24A 108.0 . . ? C25 C24 H24A 108.0 . . ? C23 C24 H24B 108.0 . . ? C25 C24 H24B 108.0 . . ? H24A C24 H24B 107.3 . . ? C24 C25 N8 117.0(4) . . ? C24 C25 H25A 108.0 . . ? N8 C25 H25A 108.0 . . ? C24 C25 H25B 108.1 . . ? N8 C25 H25B 108.0 . . ? H25A C25 H25B 107.3 . . ? N8 C26 C27 116.4(3) . . ? N8 C26 H26A 108.2 . . ? C27 C26 H26A 108.2 . . ? N8 C26 H26B 108.2 . . ? C27 C26 H26B 108.2 . . ? H26A C26 H26B 107.3 . . ? C28 C27 C26 114.7(3) . . ? C28 C27 H27A 108.6 . . ? C26 C27 H27A 108.6 . . ? C28 C27 H27B 108.6 . . ? C26 C27 H27B 108.6 . . ? H27A C27 H27B 107.6 . . ? N9 C28 C27 111.3(3) . . ? N9 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? N9 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? N8 C29 H29A 109.5 . . ? N8 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N8 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N10 C30 C31 110.2(4) . . ? N10 C30 H30A 109.6 . . ? C31 C30 H30A 109.6 . . ? N10 C30 H30B 109.6 . . ? C31 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C32 C31 C30 111.6(4) . . ? C32 C31 H31A 109.3 . . ? C30 C31 H31A 109.3 . . ? C32 C31 H31B 109.3 . . ? C30 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? C31 C32 N11 119.3(4) . . ? C31 C32 H32A 107.5 . . ? N11 C32 H32A 107.5 . . ? C31 C32 H32B 107.5 . . ? N11 C32 H32B 107.5 . . ? H32A C32 H32B 107.0 . . ? N11 C33 C34 114.9(4) . . ? N11 C33 H33A 108.5 . . ? C34 C33 H33A 108.5 . . ? N11 C33 H33B 108.5 . . ? C34 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C35 C34 C33 109.4(5) . . ? C35 C34 H34A 109.8 . . ? C33 C34 H34A 109.8 . . ? C35 C34 H34B 109.8 . . ? C33 C34 H34B 109.8 . . ? H34A C34 H34B 108.3 . . ? N12 C35 C34 118.1(4) . . ? N12 C35 H35A 107.8 . . ? C34 C35 H35A 107.8 . . ? N12 C35 H35B 107.8 . . ? C34 C35 H35B 107.8 . . ? H35A C35 H35B 107.1 . . ? N11 C36 H36A 109.5 . . ? N11 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N11 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O1W C1W H1W 109.5 . . ? O1W C1W H1WA 109.5 . . ? H1W C1W H1WA 109.5 . . ? O1W C1W H1WB 109.5 . . ? H1W C1W H1WB 109.5 . . ? H1WA C1W H1WB 109.5 . . ? C1W O1W H1WO 109.5 . . ? _diffrn_measured_fraction_theta_max 0.693 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.984 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.088 # Attachment '- af09tf1na.cif' data_af09tf1na _database_code_depnum_ccdc_archive 'CCDC 859277' #TrackingRef '- af09tf1na.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H156 N57 Ni9 O6, 2(N O3), C2 H3 N, N3' _chemical_formula_sum 'C110 H159 N63 Ni9 O12' _chemical_formula_weight 3084.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 17.8824(3) _cell_length_b 17.8824(3) _cell_length_c 72.9661(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 20207.1(6) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9846 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 36.4 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9648 _exptl_absorpt_coefficient_mu 1.310 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 X8 KappaAPEXII' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69558 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 91 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 26.45 _reflns_number_total 4621 _reflns_number_gt 3954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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. 14 of atomic sites that are flagged as handled with Uiso or Uij restraints. 2 of atomic sites that are flagged as distance restrained. ; _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^)+(0.0412P)^2^+28.1880P] 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 4621 _refine_ls_number_parameters 298 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.002 _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 0.326232(18) 0.3333 0.0833 0.02210(9) Uani 1 2 d SU . . Ni2 Ni 0.515097(16) 0.473769(16) 0.058577(3) 0.02900(9) Uani 1 1 d U . . O1 O 0.39613(9) 0.42003(9) 0.046804(18) 0.0311(3) Uani 1 1 d . . . N1 N 0.20175(10) 0.24427(10) 0.07584(2) 0.0242(3) Uani 1 1 d . . . N2 N 0.32868(10) 0.35803(10) 0.05590(2) 0.0255(3) Uani 1 1 d U . . N3 N 0.51566(11) 0.35902(11) 0.05638(2) 0.0321(4) Uani 1 1 d . . . H3A H 0.5688 0.3694 0.0594 0.039 Uiso 1 1 calc R . . H3B H 0.4789 0.3224 0.0648 0.039 Uiso 1 1 calc R . . N4 N 0.56972(14) 0.51553(14) 0.03236(3) 0.0433(4) Uani 1 1 d U . . H4N H 0.631(2) 0.540(2) 0.0342(4) 0.076(10) Uiso 1 1 d . . . N5 N 0.51334(14) 0.58961(13) 0.06233(3) 0.0489(5) Uani 1 1 d U . . H5A H 0.4660 0.5837 0.0566 0.059 Uiso 1 1 calc R . . H5B H 0.5064 0.5949 0.0744 0.059 Uiso 1 1 calc R . . N6 N 0.36037(10) 0.23592(10) 0.08116(2) 0.0275(3) Uani 1 1 d . . . N7 N 0.32560(10) 0.18389(11) 0.06899(2) 0.0268(3) Uani 1 1 d . . . N8 N 0.29152(12) 0.13414(12) 0.05748(3) 0.0377(4) Uani 1 1 d . . . N9 N 0.64313(13) 0.53117(15) 0.06836(3) 0.0544(6) Uani 1 1 d U . . N10 N 0.6667 0.54269(13) 0.0833 0.0310(5) Uani 1 2 d SU . . C1 C 0.13926(12) 0.18675(12) 0.08676(3) 0.0287(4) Uani 1 1 d . . . H1 H 0.1518 0.1841 0.0990 0.034 Uiso 1 1 calc R . . C2 C 0.05634(13) 0.13096(14) 0.08043(3) 0.0340(4) Uani 1 1 d . . . H2 H 0.0143 0.0912 0.0883 0.041 Uiso 1 1 calc R . . C3 C 0.03761(14) 0.13561(14) 0.06240(3) 0.0363(5) Uani 1 1 d . . . H3 H -0.0179 0.1001 0.0579 0.044 Uiso 1 1 calc R . . C4 C 0.10240(13) 0.19395(14) 0.05092(3) 0.0325(4) Uani 1 1 d . . . H4 H 0.0909 0.1975 0.0386 0.039 Uiso 1 1 calc R . . C5 C 0.18491(12) 0.24715(12) 0.05795(3) 0.0256(4) Uani 1 1 d . . . C6 C 0.25767(12) 0.31043(12) 0.04682(2) 0.0256(4) Uani 1 1 d . . . C7 C 0.24793(13) 0.31912(15) 0.02683(3) 0.0337(4) Uani 1 1 d . . . C8 C 0.22615(17) 0.24895(19) 0.01549(3) 0.0544(6) Uani 1 1 d U . . H8 H 0.2213 0.1984 0.0202 0.065 Uiso 1 1 calc R . . C9 C 0.2113(2) 0.2555(2) -0.00339(4) 0.0752(9) Uani 1 1 d U . . H9 H 0.1968 0.2094 -0.0113 0.090 Uiso 1 1 calc R . . C10 C 0.2189(2) 0.3321(3) -0.00988(4) 0.0780(9) Uani 1 1 d U . . H10 H 0.2051 0.3352 -0.0220 0.094 Uiso 1 1 calc R . . C11 C 0.2458(2) 0.4024(2) 0.00104(4) 0.0682(8) Uani 1 1 d U . . H11 H 0.2549 0.4544 -0.0038 0.082 Uiso 1 1 calc R . . C12 C 0.25937(17) 0.39581(18) 0.01931(3) 0.0504(6) Uani 1 1 d U . . H12 H 0.2766 0.4436 0.0269 0.060 Uiso 1 1 calc R . . C13 C 0.49254(15) 0.31424(15) 0.03843(3) 0.0400(5) Uani 1 1 d . . . H13A H 0.4332 0.2970 0.0354 0.048 Uiso 1 1 calc R . . H13B H 0.4974 0.2627 0.0391 0.048 Uiso 1 1 calc R . . C14 C 0.55351(18) 0.37509(17) 0.02335(3) 0.0519(6) Uani 1 1 d . . . H14A H 0.6127 0.3983 0.0274 0.062 Uiso 1 1 calc R . . H14B H 0.5459 0.3413 0.0124 0.062 Uiso 1 1 calc R . . C15 C 0.54016(18) 0.44868(18) 0.01846(3) 0.0536(7) Uani 1 1 d . . . H15A H 0.5704 0.4742 0.0071 0.064 Uiso 1 1 calc R . . H15B H 0.4791 0.4265 0.0163 0.064 Uiso 1 1 calc R . . C16 C 0.5718(2) 0.5968(2) 0.02603(4) 0.0674(8) Uani 1 1 d U . . H16A H 0.5970 0.6113 0.0139 0.081 Uiso 1 1 calc R . . H16B H 0.5130 0.5857 0.0251 0.081 Uiso 1 1 calc R . . C17 C 0.6219(2) 0.6730(2) 0.03843(5) 0.0752(9) Uani 1 1 d . . . H17A H 0.6788 0.6798 0.0401 0.090 Uiso 1 1 calc R . . H17B H 0.6297 0.7239 0.0320 0.090 Uiso 1 1 calc R . . C18 C 0.5888(3) 0.6729(2) 0.05598(5) 0.0889(12) Uani 1 1 d U . . H18A H 0.5721 0.7168 0.0562 0.107 Uiso 1 1 calc R . . H18B H 0.6352 0.6900 0.0648 0.107 Uiso 1 1 calc R . . N11 N 0.6667 0.3333 0.06585(5) 0.0502(9) Uani 1 3 d SD . . N12 N 0.6667 0.3333 0.0833 0.0337(10) Uani 1 6 d SD . . N13 N 0.0000 0.0000 0.12268(10) 0.113(2) Uani 1 3 d S . . O12 O 0.0824(2) 0.0528(2) 0.12253(4) 0.1198(11) Uani 1 1 d . . . N14 N 0.0000 0.0000 -0.01624(11) 0.120(3) Uani 0.50 3 d SP . . C19 C 0.0000 0.0000 0.0000 0.116(5) Uani 1 6 d S . . C20 C 0.0000 0.0000 -0.01624(11) 0.120(3) Uani 0.50 3 d SP . . 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 0.02220(13) 0.02555(18) 0.01966(16) -0.00046(12) -0.00023(6) 0.01278(9) Ni2 0.02608(14) 0.03238(15) 0.02761(14) -0.00087(10) 0.00218(10) 0.01393(11) O1 0.0276(7) 0.0361(8) 0.0284(7) 0.0035(6) 0.0026(5) 0.0152(6) N1 0.0246(8) 0.0260(8) 0.0237(7) -0.0009(6) 0.0001(6) 0.0139(7) N2 0.0264(8) 0.0295(8) 0.0227(6) 0.0008(6) 0.0011(6) 0.0155(7) N3 0.0297(9) 0.0373(10) 0.0313(9) -0.0025(7) -0.0001(7) 0.0184(8) N4 0.0420(11) 0.0538(12) 0.0360(9) 0.0060(8) 0.0088(8) 0.0255(10) N5 0.0558(12) 0.0393(9) 0.0518(12) 0.0011(9) 0.0129(10) 0.0239(9) N6 0.0288(8) 0.0309(9) 0.0253(8) -0.0029(7) -0.0024(6) 0.0170(7) N7 0.0267(8) 0.0301(8) 0.0265(8) -0.0001(7) 0.0002(7) 0.0163(7) N8 0.0364(10) 0.0417(10) 0.0338(9) -0.0065(8) -0.0021(8) 0.0186(9) N9 0.0330(9) 0.0681(14) 0.0471(10) -0.0084(10) -0.0032(8) 0.0140(10) N10 0.0221(11) 0.0272(9) 0.0420(10) 0.0019(5) 0.0038(9) 0.0110(6) C1 0.0288(10) 0.0290(10) 0.0298(10) 0.0002(8) 0.0014(8) 0.0155(8) C2 0.0310(11) 0.0306(11) 0.0398(11) 0.0004(9) 0.0028(9) 0.0149(9) C3 0.0300(11) 0.0362(11) 0.0432(12) -0.0036(9) -0.0039(9) 0.0170(9) C4 0.0307(10) 0.0348(11) 0.0331(10) -0.0026(9) -0.0045(8) 0.0173(9) C5 0.0256(9) 0.0286(10) 0.0266(9) -0.0013(7) -0.0019(7) 0.0167(8) C6 0.0266(10) 0.0297(10) 0.0238(9) -0.0013(7) -0.0013(7) 0.0165(8) C7 0.0308(11) 0.0457(12) 0.0273(10) 0.0010(9) -0.0010(8) 0.0212(10) C8 0.0505(15) 0.0559(16) 0.0461(12) -0.0065(12) 0.0014(11) 0.0186(13) C9 0.073(2) 0.083(2) 0.0470(12) -0.0096(14) -0.0001(14) 0.0218(18) C10 0.067(2) 0.107(2) 0.0502(17) 0.0060(17) -0.0093(15) 0.036(2) C11 0.071(2) 0.093(2) 0.0494(13) 0.0132(16) 0.0006(14) 0.0481(19) C12 0.0554(15) 0.0628(16) 0.0432(11) 0.0073(12) 0.0054(11) 0.0372(14) C13 0.0422(13) 0.0402(12) 0.0365(11) -0.0060(9) 0.0024(9) 0.0198(11) C14 0.0520(15) 0.0579(16) 0.0442(13) -0.0050(11) 0.0087(11) 0.0261(13) C15 0.0524(15) 0.0604(17) 0.0417(13) 0.0007(12) 0.0067(11) 0.0234(14) C16 0.082(2) 0.0674(18) 0.0578(17) 0.0120(14) 0.0014(15) 0.0406(17) C17 0.094(2) 0.0601(19) 0.071(2) 0.0093(16) 0.0185(18) 0.0375(18) C18 0.091(2) 0.0568(18) 0.085(2) 0.0042(17) 0.035(2) 0.0110(15) N11 0.0445(13) 0.0445(13) 0.062(2) 0.000 0.000 0.0223(6) N12 0.0244(13) 0.0244(13) 0.052(3) 0.000 0.000 0.0122(7) N13 0.120(3) 0.120(3) 0.098(5) 0.000 0.000 0.0601(17) O12 0.100(2) 0.119(2) 0.106(2) 0.0021(18) 0.0061(18) 0.0282(19) N14 0.124(4) 0.124(4) 0.112(6) 0.000 0.000 0.062(2) C19 0.075(5) 0.075(5) 0.198(16) 0.000 0.000 0.037(2) C20 0.124(4) 0.124(4) 0.112(6) 0.000 0.000 0.062(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 N2 2.0451(15) 18_554 ? Ni1 N2 2.0453(15) . ? Ni1 N1 2.0604(15) 18_554 ? Ni1 N1 2.0605(15) . ? Ni1 N6 2.1204(16) . ? Ni1 N6 2.1204(16) 18_554 ? Ni2 O1 2.0355(14) . ? Ni2 N3 2.0632(17) . ? Ni2 N5 2.105(2) . ? Ni2 N4 2.1075(19) . ? Ni2 N9 2.111(2) . ? Ni2 N6 2.1714(16) 18_554 ? O1 N2 1.337(2) . ? N1 C1 1.339(2) . ? N1 C5 1.346(2) . ? N2 C6 1.302(2) . ? N3 C13 1.482(3) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C15 1.451(3) . ? N4 C16 1.508(4) . ? N4 H4N 0.96(3) . ? N5 C18 1.499(4) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N6 N7 1.209(2) . ? N6 Ni2 2.1715(16) 18_554 ? N7 N8 1.152(2) . ? N9 N10 1.152(2) . ? N10 N9 1.152(2) 17_654 ? C1 C2 1.389(3) . ? C1 H1 0.9300 . ? C2 C3 1.371(3) . ? C2 H2 0.9300 . ? C3 C4 1.387(3) . ? C3 H3 0.9300 . ? C4 C5 1.393(3) . ? C4 H4 0.9300 . ? C5 C6 1.470(3) . ? C6 C7 1.486(3) . ? C7 C8 1.386(3) . ? C7 C12 1.394(3) . ? C8 C9 1.419(4) . ? C8 H8 0.9300 . ? C9 C10 1.390(5) . ? C9 H9 0.9300 . ? C10 C11 1.357(5) . ? C10 H10 0.9300 . ? C11 C12 1.370(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.548(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.493(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.502(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.411(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? N11 N12 1.275(4) . ? N12 N11 1.275(4) 16_544 ? N13 O12 1.293(3) . ? N13 O12 1.293(3) 3 ? N13 O12 1.293(3) 2 ? N14 C19 1.185(8) . ? C19 C20 1.185(8) 19 ? C19 N14 1.185(8) 19 ? 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 N2 Ni1 N2 170.07(9) 18_554 . ? N2 Ni1 N1 78.79(6) 18_554 18_554 ? N2 Ni1 N1 94.26(6) . 18_554 ? N2 Ni1 N1 94.27(6) 18_554 . ? N2 Ni1 N1 78.78(6) . . ? N1 Ni1 N1 92.12(9) 18_554 . ? N2 Ni1 N6 90.04(6) 18_554 . ? N2 Ni1 N6 96.91(6) . . ? N1 Ni1 N6 168.81(6) 18_554 . ? N1 Ni1 N6 89.35(6) . . ? N2 Ni1 N6 96.91(6) 18_554 18_554 ? N2 Ni1 N6 90.04(6) . 18_554 ? N1 Ni1 N6 89.36(6) 18_554 18_554 ? N1 Ni1 N6 168.80(6) . 18_554 ? N6 Ni1 N6 91.35(9) . 18_554 ? O1 Ni2 N3 91.23(6) . . ? O1 Ni2 N5 89.60(7) . . ? N3 Ni2 N5 176.94(7) . . ? O1 Ni2 N4 88.52(7) . . ? N3 Ni2 N4 92.87(7) . . ? N5 Ni2 N4 90.09(8) . . ? O1 Ni2 N9 174.79(7) . . ? N3 Ni2 N9 88.07(8) . . ? N5 Ni2 N9 91.36(9) . . ? N4 Ni2 N9 86.37(8) . . ? O1 Ni2 N6 91.03(6) . 18_554 ? N3 Ni2 N6 87.36(6) . 18_554 ? N5 Ni2 N6 89.68(7) . 18_554 ? N4 Ni2 N6 179.49(7) . 18_554 ? N9 Ni2 N6 94.09(7) . 18_554 ? N2 O1 Ni2 118.59(10) . . ? C1 N1 C5 119.34(16) . . ? C1 N1 Ni1 126.87(13) . . ? C5 N1 Ni1 113.80(12) . . ? C6 N2 O1 118.02(15) . . ? C6 N2 Ni1 116.65(13) . . ? O1 N2 Ni1 125.31(11) . . ? C13 N3 Ni2 117.85(13) . . ? C13 N3 H3A 107.8 . . ? Ni2 N3 H3A 107.8 . . ? C13 N3 H3B 107.8 . . ? Ni2 N3 H3B 107.8 . . ? H3A N3 H3B 107.2 . . ? C15 N4 C16 113.8(2) . . ? C15 N4 Ni2 115.42(16) . . ? C16 N4 Ni2 113.77(16) . . ? C15 N4 H4N 109.8(19) . . ? C16 N4 H4N 96.9(19) . . ? Ni2 N4 H4N 105.0(19) . . ? C18 N5 Ni2 119.3(2) . . ? C18 N5 H5A 107.5 . . ? Ni2 N5 H5A 107.5 . . ? C18 N5 H5B 107.5 . . ? Ni2 N5 H5B 107.5 . . ? H5A N5 H5B 107.0 . . ? N7 N6 Ni1 116.02(12) . . ? N7 N6 Ni2 119.87(13) . 18_554 ? Ni1 N6 Ni2 110.89(7) . 18_554 ? N8 N7 N6 179.2(2) . . ? N10 N9 Ni2 128.19(15) . . ? N9 N10 N9 179.6(3) 17_654 . ? N1 C1 C2 122.36(18) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.8(2) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 119.2(2) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.52(19) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 120.75(17) . . ? N1 C5 C6 115.88(16) . . ? C4 C5 C6 123.35(17) . . ? N2 C6 C5 114.85(16) . . ? N2 C6 C7 123.93(17) . . ? C5 C6 C7 121.19(17) . . ? C8 C7 C12 119.5(2) . . ? C8 C7 C6 119.1(2) . . ? C12 C7 C6 121.5(2) . . ? C7 C8 C9 119.0(3) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C10 C9 C8 118.8(3) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C11 C10 C9 121.8(3) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C10 C11 C12 119.2(3) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C11 C12 C7 121.5(3) . . ? C11 C12 H12 119.3 . . ? C7 C12 H12 119.3 . . ? N3 C13 C14 109.89(19) . . ? N3 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? N3 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C15 C14 C13 115.0(2) . . ? C15 C14 H14A 108.5 . . ? C13 C14 H14A 108.5 . . ? C15 C14 H14B 108.5 . . ? C13 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? N4 C15 C14 114.0(2) . . ? N4 C15 H15A 108.8 . . ? C14 C15 H15A 108.8 . . ? N4 C15 H15B 108.8 . . ? C14 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17 C16 N4 113.9(3) . . ? C17 C16 H16A 108.8 . . ? N4 C16 H16A 108.8 . . ? C17 C16 H16B 108.8 . . ? N4 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C18 C17 C16 119.1(3) . . ? C18 C17 H17A 107.5 . . ? C16 C17 H17A 107.5 . . ? C18 C17 H17B 107.5 . . ? C16 C17 H17B 107.5 . . ? H17A C17 H17B 107.0 . . ? C17 C18 N5 116.7(3) . . ? C17 C18 H18A 108.1 . . ? N5 C18 H18A 108.1 . . ? C17 C18 H18B 108.1 . . ? N5 C18 H18B 108.1 . . ? H18A C18 H18B 107.3 . . ? N11 N12 N11 180.0 16_544 . ? O12 N13 O12 119.994(18) . 3 ? O12 N13 O12 119.994(18) . 2 ? O12 N13 O12 119.994(18) 3 2 ? C20 C19 N14 180.0 19 . ? N14 C19 N14 180.0 19 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.599 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.050 # Attachment '- af31fua1na.cif' data_af31fua1na _database_code_depnum_ccdc_archive 'CCDC 859278' #TrackingRef '- af31fua1na.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H156 N57 Ni9 O6, Br3, H2 O' _chemical_formula_sum 'C108 H156 Br3 N57 Ni9 O7' _chemical_formula_weight 3133.02 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 18.0774(8) _cell_length_b 18.0774(8) _cell_length_c 72.889(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 20628.2(18) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1830 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 22.41 _exptl_crystal_description Plate _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9696 _exptl_absorpt_coefficient_mu 2.147 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.74 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4716 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 91 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.42 _reflns_number_total 4698 _reflns_number_gt 3535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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. 1 of atomic sites that are flagged as handled with Uiso or Uij restraints. 7 of atomic sites that are flagged as distance restrained. ; _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^)+(0.0898P)^2^+98.7314P] 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 4698 _refine_ls_number_parameters 277 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1676 _refine_ls_wR_factor_gt 0.1466 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _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 0.3333 0.32542(4) 0.4167 0.0316(2) Uani 1 2 d S . . Ni2 Ni 0.47030(4) 0.51287(3) 0.441373(7) 0.03995(19) Uani 1 1 d . . . Br1 Br 0.3333 0.6667 0.4167 0.0595(3) Uani 1 6 d S . . Br2 Br 0.6570(3) 0.4139(3) 0.46422(9) 0.0829(16) Uani 0.17 1 d P . . Br2' Br 0.6666(12) 0.3993(8) 0.45782(15) 0.229(8) Uani 0.17 1 d P . . O1 O 0.2525(2) 0.31392(19) 0.37981(4) 0.0451(7) Uani 1 1 d . . . N1 N 0.4230(2) 0.2910(2) 0.40952(5) 0.0371(7) Uani 1 1 d . . . N2 N 0.3124(2) 0.3060(2) 0.38917(5) 0.0366(8) Uani 1 1 d . . . N3 N 0.3574(2) 0.5147(2) 0.44264(4) 0.0393(8) Uani 1 1 d D . . H3A H 0.3685 0.5668 0.4390 0.047 Uiso 1 1 calc R . . H3B H 0.3217 0.4771 0.4343 0.047 Uiso 1 1 calc R . . N4 N 0.5081(3) 0.5655(3) 0.46777(6) 0.0674(12) Uani 1 1 d . . . H4A H 0.5232 0.6209 0.4657 0.081 Uiso 1 1 calc R . . N5 N 0.5860(3) 0.5113(3) 0.43870(6) 0.0673(13) Uani 1 1 d D . . H5A H 0.5763 0.4622 0.4440 0.081 Uiso 1 1 calc R . . H5B H 0.5919 0.5055 0.4266 0.081 Uiso 1 1 calc R . . N6 N 0.4299(2) 0.4557(2) 0.41455(4) 0.0344(7) Uani 1 1 d . . . N7 N 0.4829(2) 0.4737(2) 0.40249(4) 0.0323(7) Uani 1 1 d . . . N8 N 0.5326(2) 0.4898(2) 0.39112(5) 0.0433(9) Uani 1 1 d . . . N9 N 0.5304(3) 0.6412(3) 0.43171(7) 0.0664(12) Uani 1 1 d . . . N10 N 0.5454(3) 0.6667 0.4167 0.0534(14) Uani 1 2 d S . . C1 C 0.4779(3) 0.2846(3) 0.42039(6) 0.0444(10) Uani 1 1 d . . . H1 H 0.4793 0.2986 0.4327 0.053 Uiso 1 1 calc R . . C2 C 0.5332(3) 0.2584(3) 0.41443(7) 0.0514(11) Uani 1 1 d . . . H2 H 0.5720 0.2564 0.4225 0.062 Uiso 1 1 calc R . . C3 C 0.5305(3) 0.2359(3) 0.39686(8) 0.0587(13) Uani 1 1 d . . . H3 H 0.5655 0.2153 0.3927 0.070 Uiso 1 1 calc R . . C4 C 0.4739(3) 0.2437(3) 0.38458(7) 0.0491(11) Uani 1 1 d . . . H4 H 0.4728 0.2310 0.3722 0.059 Uiso 1 1 calc R . . C5 C 0.4200(3) 0.2709(3) 0.39169(6) 0.0405(9) Uani 1 1 d . . . C6 C 0.3582(3) 0.2819(3) 0.38020(6) 0.0404(9) Uani 1 1 d . . . C7 C 0.3469(3) 0.2617(2) 0.36038(4) 0.0629(14) Uani 1 1 d G . . C8 C 0.2708(3) 0.1937(2) 0.35391(5) 0.093(2) Uani 1 1 d G . . H8 H 0.2257 0.1629 0.3619 0.111 Uiso 1 1 calc R . . C9 C 0.2622(3) 0.1720(3) 0.33543(6) 0.104(3) Uani 1 1 d G . . H9 H 0.2114 0.1265 0.3311 0.125 Uiso 1 1 calc R . . C10 C 0.3297(4) 0.2181(4) 0.32342(4) 0.105(3) Uani 1 1 d G . . H10 H 0.3239 0.2036 0.3111 0.127 Uiso 1 1 calc R . . C11 C 0.4057(3) 0.2861(4) 0.32989(5) 0.102(3) Uani 1 1 d G . . H11 H 0.4509 0.3169 0.3218 0.123 Uiso 1 1 calc R . . C12 C 0.4143(2) 0.3078(3) 0.34836(6) 0.0838(19) Uani 1 1 d G . . H12 H 0.4652 0.3533 0.3527 0.101 Uiso 1 1 calc R . . C13 C 0.3122(4) 0.4963(4) 0.45970(7) 0.0648(14) Uani 1 1 d D . . H13A H 0.2905 0.4369 0.4628 0.078 Uiso 1 1 calc R . . H13B H 0.2637 0.5051 0.4583 0.078 Uiso 1 1 calc R . . C14 C 0.3683(4) 0.5521(4) 0.47500(7) 0.0749(17) Uani 1 1 d D . . H14A H 0.3326 0.5420 0.4857 0.090 Uiso 1 1 calc R . . H14B H 0.3907 0.6111 0.4714 0.090 Uiso 1 1 calc R . . C15 C 0.4427(5) 0.5418(5) 0.48076(8) 0.0801(19) Uani 1 1 d . . . H15A H 0.4674 0.5754 0.4918 0.096 Uiso 1 1 calc R . . H15B H 0.4211 0.4823 0.4840 0.096 Uiso 1 1 calc R . . C16 C 0.5946(4) 0.5751(5) 0.47376(8) 0.087(2) Uani 1 1 d D . . H16A H 0.6097 0.6038 0.4856 0.105 Uiso 1 1 calc R . . H16B H 0.5865 0.5184 0.4756 0.105 Uiso 1 1 calc R . . C17 C 0.6677(4) 0.6220(5) 0.46119(10) 0.1069(19) Uani 1 1 d D . . H17A H 0.6684 0.6735 0.4572 0.128 Uiso 1 1 calc R . . H17B H 0.7200 0.6395 0.4680 0.128 Uiso 1 1 calc R . . C18 C 0.6679(4) 0.5744(5) 0.44488(9) 0.1069(19) Uani 1 1 d D . . H18A H 0.6965 0.6147 0.4350 0.128 Uiso 1 1 calc R . . H18B H 0.7011 0.5470 0.4476 0.128 Uiso 1 1 calc R . . O1W O 0.6667 0.3333 0.3528(4) 0.169(11) Uani 0.50 3 d SP . . 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 0.0360(4) 0.0320(3) 0.0282(4) -0.00049(14) -0.0010(3) 0.0180(2) Ni2 0.0438(3) 0.0405(3) 0.0356(3) -0.0053(2) -0.0056(2) 0.0211(3) Br1 0.0557(5) 0.0557(5) 0.0671(8) 0.000 0.000 0.0278(2) Br2 0.097(3) 0.047(2) 0.101(4) -0.013(2) -0.044(3) 0.033(2) Br2' 0.48(2) 0.158(9) 0.120(7) -0.032(6) -0.063(9) 0.212(12) O1 0.0579(19) 0.0424(16) 0.0387(16) -0.0046(13) -0.0084(14) 0.0280(15) N1 0.0402(19) 0.0325(17) 0.0384(18) 0.0003(14) 0.0018(15) 0.0181(15) N2 0.0437(19) 0.0326(17) 0.0328(18) -0.0008(14) -0.0010(15) 0.0185(15) N3 0.046(2) 0.0334(17) 0.0385(19) 0.0011(14) 0.0013(15) 0.0202(16) N4 0.075(3) 0.077(3) 0.053(3) -0.020(2) -0.017(2) 0.040(3) N5 0.060(3) 0.087(3) 0.057(3) -0.021(2) -0.014(2) 0.039(3) N6 0.0379(18) 0.0336(17) 0.0324(17) -0.0011(13) -0.0003(14) 0.0184(15) N7 0.0363(18) 0.0310(17) 0.0310(17) -0.0015(13) -0.0040(15) 0.0178(14) N8 0.047(2) 0.046(2) 0.040(2) 0.0017(16) 0.0030(17) 0.0251(18) N9 0.067(3) 0.054(3) 0.059(3) -0.001(2) -0.001(2) 0.016(2) N10 0.053(3) 0.042(3) 0.061(4) -0.011(3) -0.0053(14) 0.0208(15) C1 0.045(2) 0.042(2) 0.045(3) 0.0020(19) 0.0018(19) 0.022(2) C2 0.048(3) 0.048(3) 0.062(3) 0.004(2) 0.002(2) 0.027(2) C3 0.056(3) 0.051(3) 0.072(4) 0.005(2) 0.011(3) 0.029(3) C4 0.055(3) 0.044(2) 0.048(3) -0.004(2) 0.007(2) 0.025(2) C5 0.047(2) 0.032(2) 0.042(2) 0.0001(17) 0.0050(18) 0.0185(19) C6 0.049(2) 0.032(2) 0.036(2) 0.0005(16) 0.0043(18) 0.0175(19) C7 0.099(4) 0.060(3) 0.045(3) -0.008(2) -0.003(3) 0.051(3) C8 0.148(7) 0.061(4) 0.059(4) -0.011(3) -0.017(4) 0.044(4) C9 0.154(8) 0.088(5) 0.070(5) -0.016(4) -0.022(5) 0.060(6) C10 0.142(8) 0.137(8) 0.065(4) -0.019(5) 0.005(5) 0.091(7) C11 0.113(6) 0.145(8) 0.075(5) 0.027(5) 0.023(4) 0.085(6) C12 0.097(5) 0.113(5) 0.056(4) 0.016(3) 0.021(3) 0.063(4) C13 0.064(3) 0.065(3) 0.059(3) -0.005(3) 0.013(3) 0.028(3) C14 0.072(4) 0.077(4) 0.062(4) -0.018(3) 0.008(3) 0.027(3) C15 0.093(5) 0.081(4) 0.051(3) -0.010(3) -0.007(3) 0.032(4) C16 0.082(5) 0.099(5) 0.060(4) -0.004(3) -0.016(3) 0.029(4) C17 0.072(3) 0.142(5) 0.093(4) -0.037(4) -0.018(3) 0.043(3) C18 0.072(3) 0.142(5) 0.093(4) -0.037(4) -0.018(3) 0.043(3) O1W 0.163(16) 0.163(16) 0.18(3) 0.000 0.000 0.081(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 2.037(3) . ? Ni1 N2 2.038(3) 12 ? Ni1 N1 2.072(3) . ? Ni1 N1 2.072(3) 12 ? Ni1 N6 2.122(3) . ? Ni1 N6 2.123(3) 12 ? Ni2 O1 2.051(3) 12 ? Ni2 N3 2.059(4) . ? Ni2 N4 2.103(4) . ? Ni2 N5 2.115(5) . ? Ni2 N9 2.130(5) . ? Ni2 N6 2.161(3) . ? O1 N2 1.346(4) . ? O1 Ni2 2.051(3) 12 ? N1 C1 1.320(5) . ? N1 C5 1.343(5) . ? N2 C6 1.290(5) . ? N3 C13 1.433(5) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C15 1.404(8) . ? N4 C16 1.547(8) . ? N4 H4A 0.9100 . ? N5 C18 1.417(6) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N6 N7 1.219(5) . ? N7 N8 1.147(5) . ? N9 N10 1.167(5) . ? N10 N9 1.167(5) 11_565 ? C1 C2 1.373(6) . ? C1 H1 0.9300 . ? C2 C3 1.338(7) . ? C2 H2 0.9300 . ? C3 C4 1.419(7) . ? C3 H3 0.9300 . ? C4 C5 1.392(6) . ? C4 H4 0.9300 . ? C5 C6 1.487(6) . ? C6 C7 1.479(5) . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C8 H8 0.9300 . ? C9 C10 1.3900 . ? C9 H9 0.9300 . ? C10 C11 1.3900 . ? C10 H10 0.9300 . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.506(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.506(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.478(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.470(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 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 N2 Ni1 N2 170.94(19) . 12 ? N2 Ni1 N1 78.87(14) . . ? N2 Ni1 N1 94.81(14) 12 . ? N2 Ni1 N1 94.81(14) . 12 ? N2 Ni1 N1 78.87(14) 12 12 ? N1 Ni1 N1 92.48(19) . 12 ? N2 Ni1 N6 95.64(13) . . ? N2 Ni1 N6 90.68(13) 12 . ? N1 Ni1 N6 88.98(13) . . ? N1 Ni1 N6 169.53(13) 12 . ? N2 Ni1 N6 90.69(13) . 12 ? N2 Ni1 N6 95.64(13) 12 12 ? N1 Ni1 N6 169.54(13) . 12 ? N1 Ni1 N6 88.98(13) 12 12 ? N6 Ni1 N6 91.45(18) . 12 ? O1 Ni2 N3 91.08(13) 12 . ? O1 Ni2 N4 87.43(17) 12 . ? N3 Ni2 N4 92.99(16) . . ? O1 Ni2 N5 90.22(17) 12 . ? N3 Ni2 N5 177.29(16) . . ? N4 Ni2 N5 89.45(18) . . ? O1 Ni2 N9 173.70(15) 12 . ? N3 Ni2 N9 88.15(17) . . ? N4 Ni2 N9 86.4(2) . . ? N5 Ni2 N9 90.8(2) . . ? O1 Ni2 N6 91.13(12) 12 . ? N3 Ni2 N6 87.01(13) . . ? N4 Ni2 N6 178.56(17) . . ? N5 Ni2 N6 90.58(14) . . ? N9 Ni2 N6 95.07(16) . . ? N2 O1 Ni2 118.9(2) . 12 ? C1 N1 C5 119.2(4) . . ? C1 N1 Ni1 127.7(3) . . ? C5 N1 Ni1 113.1(3) . . ? C6 N2 O1 117.7(3) . . ? C6 N2 Ni1 117.5(3) . . ? O1 N2 Ni1 124.8(2) . . ? C13 N3 Ni2 119.4(3) . . ? C13 N3 H3A 107.5 . . ? Ni2 N3 H3A 107.5 . . ? C13 N3 H3B 107.5 . . ? Ni2 N3 H3B 107.5 . . ? H3A N3 H3B 107.0 . . ? C15 N4 C16 119.6(5) . . ? C15 N4 Ni2 116.4(4) . . ? C16 N4 Ni2 113.0(3) . . ? C15 N4 H4A 101.2 . . ? C16 N4 H4A 101.2 . . ? Ni2 N4 H4A 101.2 . . ? C18 N5 Ni2 127.1(4) . . ? C18 N5 H5A 105.5 . . ? Ni2 N5 H5A 105.5 . . ? C18 N5 H5B 105.5 . . ? Ni2 N5 H5B 105.5 . . ? H5A N5 H5B 106.1 . . ? N7 N6 Ni1 116.7(3) . . ? N7 N6 Ni2 119.5(3) . . ? Ni1 N6 Ni2 111.04(14) . . ? N8 N7 N6 179.3(4) . . ? N10 N9 Ni2 129.2(3) . . ? N9 N10 N9 176.0(8) 11_565 . ? N1 C1 C2 123.3(4) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 119.1(5) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.5(5) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 117.9(4) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? N1 C5 C4 121.0(4) . . ? N1 C5 C6 116.1(4) . . ? C4 C5 C6 122.9(4) . . ? N2 C6 C7 123.1(4) . . ? N2 C6 C5 114.3(4) . . ? C7 C6 C5 122.5(4) . . ? C8 C7 C12 120.0 . . ? C8 C7 C6 120.2(3) . . ? C12 C7 C6 119.7(3) . . ? C7 C8 C9 120.0 . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.0 . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? N3 C13 C14 111.8(4) . . ? N3 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? N3 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C13 C14 C15 117.9(5) . . ? C13 C14 H14A 107.8 . . ? C15 C14 H14A 107.8 . . ? C13 C14 H14B 107.8 . . ? C15 C14 H14B 107.8 . . ? H14A C14 H14B 107.2 . . ? N4 C15 C14 116.2(5) . . ? N4 C15 H15A 108.2 . . ? C14 C15 H15A 108.2 . . ? N4 C15 H15B 108.2 . . ? C14 C15 H15B 108.2 . . ? H15A C15 H15B 107.4 . . ? C17 C16 N4 116.9(6) . . ? C17 C16 H16A 108.1 . . ? N4 C16 H16A 108.1 . . ? C17 C16 H16B 108.1 . . ? N4 C16 H16B 108.1 . . ? H16A C16 H16B 107.3 . . ? C18 C17 C16 115.4(6) . . ? C18 C17 H17A 108.4 . . ? C16 C17 H17A 108.4 . . ? C18 C17 H17B 108.4 . . ? C16 C17 H17B 108.4 . . ? H17A C17 H17B 107.5 . . ? N5 C18 C17 114.9(5) . . ? N5 C18 H18A 108.5 . . ? C17 C18 H18A 108.5 . . ? N5 C18 H18B 108.5 . . ? C17 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.546 _refine_diff_density_min -2.092 _refine_diff_density_rms 0.090 data_af03fua2na _database_code_depnum_ccdc_archive 'CCDC 876039' #TrackingRef '- af03fua2na.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C108 H156 N57 Ni9 O6), Cl4, 2(N3), (H2 O)' _chemical_formula_sum 'C216 H314 Cl4 N120 Ni18 O13' _chemical_formula_weight 5998.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 18.0085(9) _cell_length_b 18.0085(9) _cell_length_c 73.205(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 20560(2) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1962 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.25 _exptl_crystal_description Plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9378 _exptl_absorpt_coefficient_mu 1.319 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6814 _exptl_absorpt_correction_T_max 0.9100 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4756 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 90 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 26.60 _reflns_number_total 4756 _reflns_number_gt 3058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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. 11 of atomic sites that are flagged as handled with Uiso or Uij restraints. ; _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^)+(0.0693P)^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 4756 _refine_ls_number_parameters 298 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1265 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.32648(3) 0.3333 0.0833 0.04244(17) Uani 1 2 d S . . Ni2 Ni 0.51428(3) 0.47105(3) 0.058743(6) 0.05092(16) Uani 1 1 d . . . Cl1 Cl 0.3641(10) 0.5999(9) 0.04264(13) 0.137(4) Uani 0.17 1 d P . . Cl1' Cl 0.4113(6) 0.6609(12) 0.04046(17) 0.193(9) Uani 0.17 1 d P . . O1 O 0.39559(14) 0.41554(15) 0.04680(3) 0.0557(6) Uani 1 1 d . . . N1 N 0.20286(16) 0.24443(17) 0.07610(4) 0.0476(6) Uani 1 1 d . . . N2 N 0.32884(16) 0.35666(18) 0.05594(4) 0.0471(6) Uani 1 1 d . . . N3 N 0.5133(2) 0.58655(19) 0.06214(5) 0.0828(10) Uani 1 1 d . . . H3A H 0.4670 0.5812 0.0562 0.099 Uiso 1 1 calc R . . H3B H 0.5057 0.5922 0.0741 0.099 Uiso 1 1 calc R . . N4 N 0.5679(2) 0.5110(2) 0.03245(4) 0.0724(8) Uani 1 1 d U . . H4 H 0.6239 0.5263 0.0340 0.087 Uiso 1 1 calc R . . N5 N 0.51546(15) 0.35754(17) 0.05686(3) 0.0494(6) Uani 1 1 d . . . H5A H 0.5682 0.3682 0.0600 0.059 Uiso 1 1 calc R . . H5B H 0.4787 0.3213 0.0653 0.059 Uiso 1 1 calc R . . N6 N 0.36055(16) 0.23695(16) 0.08122(3) 0.0450(6) Uani 1 1 d . . . N7 N 0.32586(16) 0.18452(17) 0.06924(4) 0.0445(6) Uani 1 1 d . . . N8 N 0.29154(17) 0.13511(19) 0.05779(4) 0.0567(7) Uani 1 1 d . . . N9 N 0.6411(2) 0.5289(2) 0.06851(5) 0.0842(11) Uani 1 1 d U . . N10 N 0.6667 0.5419(2) 0.0833 0.0545(10) Uani 1 2 d SU . . N11 N 0.6667 0.3333 0.0833 0.0368(13) Uani 1 6 d S . . N12 N 0.6667 0.3333 0.06707(9) 0.0679(15) Uani 1 3 d S . . C1 C 0.1412(2) 0.1880(2) 0.08709(5) 0.0554(8) Uani 1 1 d . . . H1 H 0.1545 0.1855 0.0993 0.066 Uiso 1 1 calc R . . C2 C 0.0586(2) 0.1331(2) 0.08112(5) 0.0630(10) Uani 1 1 d . . . H2 H 0.0170 0.0943 0.0891 0.076 Uiso 1 1 calc R . . C3 C 0.0395(2) 0.1375(3) 0.06280(6) 0.0678(10) Uani 1 1 d . . . H3 H -0.0156 0.1021 0.0583 0.081 Uiso 1 1 calc R . . C4 C 0.1032(2) 0.1947(2) 0.05146(5) 0.0610(9) Uani 1 1 d . . . H4A H 0.0913 0.1979 0.0392 0.073 Uiso 1 1 calc R . . C5 C 0.1852(2) 0.2477(2) 0.05815(5) 0.0494(8) Uani 1 1 d . . . C6 C 0.2578(2) 0.3096(2) 0.04700(4) 0.0493(8) Uani 1 1 d . . . C7 C 0.2470(2) 0.3165(3) 0.02707(5) 0.0683(10) Uani 1 1 d U . . C8 C 0.2542(4) 0.3906(4) 0.01993(6) 0.127(2) Uani 1 1 d U . . H8 H 0.2688 0.4378 0.0274 0.152 Uiso 1 1 calc R . . C9 C 0.2391(5) 0.3934(6) 0.00143(9) 0.181(4) Uani 1 1 d U . . H9 H 0.2430 0.4428 -0.0035 0.218 Uiso 1 1 calc R . . C10 C 0.2188(5) 0.3250(9) -0.00981(9) 0.193(4) Uani 1 1 d U . . H10 H 0.2081 0.3273 -0.0222 0.231 Uiso 1 1 calc R . . C11 C 0.2147(4) 0.2568(6) -0.00275(8) 0.172(4) Uani 1 1 d U . . H11 H 0.2012 0.2101 -0.0103 0.206 Uiso 1 1 calc R . . C12 C 0.2302(3) 0.2514(4) 0.01586(6) 0.1040(16) Uani 1 1 d . . . H12 H 0.2287 0.2025 0.0204 0.125 Uiso 1 1 calc R . . C13 C 0.5888(4) 0.6674(3) 0.05594(8) 0.148(3) Uani 1 1 d . . . H13A H 0.5751 0.7130 0.0568 0.177 Uiso 1 1 calc R . . H13B H 0.6358 0.6814 0.0643 0.177 Uiso 1 1 calc R . . C14 C 0.6168(5) 0.6666(3) 0.03816(9) 0.137(3) Uani 1 1 d . . . H14A H 0.6754 0.6781 0.0391 0.165 Uiso 1 1 calc R . . H14B H 0.6193 0.7151 0.0318 0.165 Uiso 1 1 calc R . . C15 C 0.5721(4) 0.5930(4) 0.02614(7) 0.1154(18) Uani 1 1 d U . . H15A H 0.5999 0.6081 0.0143 0.138 Uiso 1 1 calc R . . H15B H 0.5140 0.5819 0.0245 0.138 Uiso 1 1 calc R . . C16 C 0.5383(3) 0.4447(3) 0.01877(5) 0.0873(12) Uani 1 1 d U . . H16A H 0.5686 0.4694 0.0074 0.105 Uiso 1 1 calc R . . H16B H 0.4778 0.4231 0.0166 0.105 Uiso 1 1 calc R . . C17 C 0.5513(3) 0.3698(3) 0.02418(5) 0.0820(11) Uani 1 1 d U . . H17A H 0.5422 0.3346 0.0134 0.098 Uiso 1 1 calc R . . H17B H 0.6104 0.3928 0.0279 0.098 Uiso 1 1 calc R . . C18 C 0.4939(2) 0.3128(2) 0.03928(5) 0.0651(10) Uani 1 1 d . . . H18A H 0.4347 0.2942 0.0363 0.078 Uiso 1 1 calc R . . H18B H 0.4998 0.2622 0.0402 0.078 Uiso 1 1 calc R . . O1W O 0.0000 0.0000 0.0096(8) 0.32(4) Uani 0.25 3 d SP . . 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 0.0428(2) 0.0541(3) 0.0342(3) -0.0026(2) -0.00129(12) 0.02705(17) Ni2 0.0490(3) 0.0610(3) 0.0426(3) 0.00190(19) 0.00564(18) 0.0273(2) Cl1 0.205(11) 0.204(12) 0.095(6) 0.078(7) 0.048(7) 0.173(11) Cl1' 0.062(5) 0.30(2) 0.138(9) 0.122(12) -0.022(5) 0.028(7) O1 0.0538(13) 0.0758(16) 0.0431(13) 0.0083(11) 0.0036(10) 0.0366(12) N1 0.0453(14) 0.0581(16) 0.0458(16) -0.0082(13) -0.0031(12) 0.0308(13) N2 0.0492(15) 0.0605(16) 0.0406(16) 0.0001(13) -0.0013(12) 0.0341(14) N3 0.113(3) 0.061(2) 0.079(2) 0.0162(17) 0.042(2) 0.047(2) N4 0.074(2) 0.094(2) 0.0526(19) 0.0086(17) 0.0142(16) 0.0448(19) N5 0.0387(13) 0.0647(17) 0.0459(16) -0.0013(13) 0.0003(11) 0.0267(13) N6 0.0491(14) 0.0526(15) 0.0394(15) -0.0052(13) -0.0039(12) 0.0299(13) N7 0.0447(14) 0.0517(15) 0.0413(16) 0.0002(14) -0.0016(13) 0.0273(13) N8 0.0527(17) 0.0651(18) 0.0491(18) -0.0098(14) -0.0031(13) 0.0270(14) N9 0.0509(19) 0.098(3) 0.065(2) -0.0094(19) 0.0039(16) 0.0085(17) N10 0.041(2) 0.0551(17) 0.063(2) 0.0055(9) 0.0109(18) 0.0203(11) N11 0.0280(19) 0.0280(19) 0.054(4) 0.000 0.000 0.0140(10) N12 0.057(2) 0.057(2) 0.091(4) 0.000 0.000 0.0283(10) C1 0.053(2) 0.061(2) 0.054(2) -0.0035(17) -0.0020(17) 0.0307(18) C2 0.047(2) 0.063(2) 0.074(3) -0.0063(19) 0.0032(18) 0.0227(17) C3 0.048(2) 0.073(2) 0.084(3) -0.019(2) -0.013(2) 0.0309(19) C4 0.058(2) 0.079(2) 0.059(2) -0.0111(19) -0.0142(18) 0.045(2) C5 0.0515(19) 0.059(2) 0.049(2) -0.0110(16) -0.0083(15) 0.0367(17) C6 0.057(2) 0.069(2) 0.0386(18) -0.0090(15) -0.0100(15) 0.0442(18) C7 0.059(2) 0.124(3) 0.037(2) -0.004(2) -0.0091(16) 0.058(2) C8 0.191(6) 0.221(6) 0.065(3) 0.046(4) 0.032(3) 0.174(6) C9 0.224(9) 0.371(12) 0.071(4) 0.087(5) 0.036(4) 0.240(9) C10 0.125(6) 0.387(11) 0.040(4) 0.032(5) -0.011(4) 0.108(8) C11 0.121(5) 0.234(8) 0.041(4) -0.038(4) -0.005(3) 0.000(5) C12 0.108(4) 0.124(4) 0.049(3) -0.025(3) -0.013(2) 0.035(3) C13 0.188(6) 0.084(4) 0.118(5) 0.021(3) 0.093(5) 0.027(4) C14 0.209(7) 0.074(3) 0.123(5) 0.026(3) 0.065(5) 0.067(4) C15 0.165(5) 0.107(4) 0.069(3) 0.030(3) 0.005(3) 0.064(4) C16 0.084(3) 0.111(3) 0.050(2) 0.005(2) 0.011(2) 0.036(3) C17 0.075(3) 0.094(3) 0.063(3) -0.018(2) 0.019(2) 0.031(2) C18 0.063(2) 0.075(2) 0.052(2) -0.0088(19) 0.0099(18) 0.031(2) O1W 0.30(4) 0.30(4) 0.36(11) 0.000 0.000 0.15(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 N2 2.044(3) 18_554 ? Ni1 N2 2.045(3) . ? Ni1 N1 2.058(3) 18_554 ? Ni1 N1 2.058(3) . ? Ni1 N6 2.116(2) . ? Ni1 N6 2.116(2) 18_554 ? Ni2 O1 2.048(2) . ? Ni2 N5 2.060(3) . ? Ni2 N3 2.104(3) . ? Ni2 N9 2.105(3) . ? Ni2 N4 2.112(3) . ? Ni2 N6 2.161(2) 18_554 ? Cl1 Cl1' 1.011(15) . ? Cl1 Cl1' 1.975(19) 3_565 ? Cl1' Cl1 1.975(19) 2_665 ? O1 N2 1.320(3) . ? N1 C1 1.335(4) . ? N1 C5 1.360(4) . ? N2 C6 1.304(4) . ? N3 C13 1.482(6) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C16 1.440(5) . ? N4 C15 1.514(6) . ? N4 H4 0.9100 . ? N5 C18 1.464(4) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N6 N7 1.209(3) . ? N6 Ni2 2.162(2) 18_554 ? N7 N8 1.152(4) . ? N9 N10 1.156(3) . ? N10 N9 1.156(3) 17_654 ? N11 N12 1.190(6) 16_544 ? N11 N12 1.190(6) . ? C1 C2 1.383(5) . ? C1 H1 0.9300 . ? C2 C3 1.397(5) . ? C2 H2 0.9300 . ? C3 C4 1.373(5) . ? C3 H3 0.9300 . ? C4 C5 1.387(5) . ? C4 H4A 0.9300 . ? C5 C6 1.470(5) . ? C6 C7 1.485(5) . ? C7 C12 1.336(6) . ? C7 C8 1.377(7) . ? C8 C9 1.387(7) . ? C8 H8 0.9300 . ? C9 C10 1.370(13) . ? C9 H9 0.9300 . ? C10 C11 1.301(13) . ? C10 H10 0.9300 . ? C11 C12 1.403(7) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.399(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.452(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.533(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.510(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? O1W O1W 1.41(12) 19 ? 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 N2 Ni1 N2 170.60(14) 18_554 . ? N2 Ni1 N1 79.11(11) 18_554 18_554 ? N2 Ni1 N1 94.33(10) . 18_554 ? N2 Ni1 N1 94.33(10) 18_554 . ? N2 Ni1 N1 79.10(11) . . ? N1 Ni1 N1 92.30(14) 18_554 . ? N2 Ni1 N6 90.14(10) 18_554 . ? N2 Ni1 N6 96.44(10) . . ? N1 Ni1 N6 169.22(10) 18_554 . ? N1 Ni1 N6 89.29(10) . . ? N2 Ni1 N6 96.45(10) 18_554 18_554 ? N2 Ni1 N6 90.14(10) . 18_554 ? N1 Ni1 N6 89.29(10) 18_554 18_554 ? N1 Ni1 N6 169.21(10) . 18_554 ? N6 Ni1 N6 91.14(14) . 18_554 ? O1 Ni2 N5 90.75(9) . . ? O1 Ni2 N3 90.59(13) . . ? N5 Ni2 N3 177.06(12) . . ? O1 Ni2 N9 174.54(11) . . ? N5 Ni2 N9 88.13(12) . . ? N3 Ni2 N9 90.78(15) . . ? O1 Ni2 N4 88.00(11) . . ? N5 Ni2 N4 92.69(12) . . ? N3 Ni2 N4 89.98(13) . . ? N9 Ni2 N4 86.72(13) . . ? O1 Ni2 N6 90.89(9) . 18_554 ? N5 Ni2 N6 87.65(10) . 18_554 ? N3 Ni2 N6 89.71(11) . 18_554 ? N9 Ni2 N6 94.40(11) . 18_554 ? N4 Ni2 N6 178.84(11) . 18_554 ? Cl1' Cl1 Cl1' 111.4(11) . 3_565 ? Cl1 Cl1' Cl1 125.9(14) . 2_665 ? N2 O1 Ni2 118.98(17) . . ? C1 N1 C5 119.4(3) . . ? C1 N1 Ni1 127.0(2) . . ? C5 N1 Ni1 113.6(2) . . ? C6 N2 O1 118.1(3) . . ? C6 N2 Ni1 116.5(2) . . ? O1 N2 Ni1 125.40(19) . . ? C13 N3 Ni2 118.6(3) . . ? C13 N3 H3A 107.7 . . ? Ni2 N3 H3A 107.7 . . ? C13 N3 H3B 107.7 . . ? Ni2 N3 H3B 107.7 . . ? H3A N3 H3B 107.1 . . ? C16 N4 C15 114.4(4) . . ? C16 N4 Ni2 115.8(3) . . ? C15 N4 Ni2 113.7(3) . . ? C16 N4 H4 103.6 . . ? C15 N4 H4 103.6 . . ? Ni2 N4 H4 103.6 . . ? C18 N5 Ni2 118.3(2) . . ? C18 N5 H5A 107.7 . . ? Ni2 N5 H5A 107.7 . . ? C18 N5 H5B 107.7 . . ? Ni2 N5 H5B 107.7 . . ? H5A N5 H5B 107.1 . . ? N7 N6 Ni1 116.44(19) . . ? N7 N6 Ni2 119.5(2) . 18_554 ? Ni1 N6 Ni2 111.09(11) . 18_554 ? N8 N7 N6 178.5(3) . . ? N10 N9 Ni2 130.0(2) . . ? N9 N10 N9 179.6(6) 17_654 . ? N12 N11 N12 180.0 16_544 . ? N1 C1 C2 122.8(3) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 118.1(3) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C4 C3 C2 119.1(3) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 120.4(3) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? N1 C5 C4 120.2(3) . . ? N1 C5 C6 115.5(3) . . ? C4 C5 C6 124.3(3) . . ? N2 C6 C5 115.2(3) . . ? N2 C6 C7 124.5(3) . . ? C5 C6 C7 120.3(3) . . ? C12 C7 C8 119.1(4) . . ? C12 C7 C6 120.8(4) . . ? C8 C7 C6 120.1(4) . . ? C7 C8 C9 118.7(6) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 121.5(7) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C11 C10 C9 118.3(6) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C10 C11 C12 122.1(8) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C7 C12 C11 120.2(6) . . ? C7 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C14 C13 N3 115.6(5) . . ? C14 C13 H13A 108.4 . . ? N3 C13 H13A 108.4 . . ? C14 C13 H13B 108.4 . . ? N3 C13 H13B 108.4 . . ? H13A C13 H13B 107.4 . . ? C13 C14 C15 122.4(5) . . ? C13 C14 H14A 106.7 . . ? C15 C14 H14A 106.7 . . ? C13 C14 H14B 106.7 . . ? C15 C14 H14B 106.7 . . ? H14A C14 H14B 106.6 . . ? C14 C15 N4 116.1(5) . . ? C14 C15 H15A 108.3 . . ? N4 C15 H15A 108.3 . . ? C14 C15 H15B 108.3 . . ? N4 C15 H15B 108.3 . . ? H15A C15 H15B 107.4 . . ? N4 C16 C17 113.2(4) . . ? N4 C16 H16A 108.9 . . ? C17 C16 H16A 108.9 . . ? N4 C16 H16B 108.9 . . ? C17 C16 H16B 108.9 . . ? H16A C16 H16B 107.8 . . ? C18 C17 C16 115.7(3) . . ? C18 C17 H17A 108.4 . . ? C16 C17 H17A 108.4 . . ? C18 C17 H17B 108.4 . . ? C16 C17 H17B 108.4 . . ? H17A C17 H17B 107.4 . . ? N5 C18 C17 111.5(3) . . ? N5 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? N5 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.60 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.625 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.060 # Attachment '- af06fua1na.cif' data_af06fua1na _database_code_depnum_ccdc_archive 'CCDC 876040' #TrackingRef '- af06fua1na.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H156 N57 Ni9 O6, 2(H2 O), 3(I)' _chemical_formula_sum 'C108 H160 I3 N57 Ni9 O8' _chemical_formula_weight 3294.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 17.9113(12) _cell_length_b 17.9113(12) _cell_length_c 72.574(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 20164(2) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1995 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 24.34 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10092 _exptl_absorpt_coefficient_mu 1.995 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.71 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4598 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 90 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 26.38 _reflns_number_total 4598 _reflns_number_gt 3332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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. 4 of atomic sites that are flagged as handled with Uiso or Uij restraints. 2 of atomic sites that are flagged as distance restrained. ; _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^)+(0.1108P)^2^+83.3892P] 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 4598 _refine_ls_number_parameters 280 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1883 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.062 _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 0.32550(4) 0.3333 0.0833 0.0245(2) Uani 1 2 d S . . Ni2 Ni 0.51404(4) 0.47526(4) 0.058528(9) 0.0314(2) Uani 1 1 d . . . I1 I 0.6667 0.3333 0.0833 0.0836(5) Uani 1 6 d S . . I2 I 0.0000 0.0000 0.127771(13) 0.0716(3) Uani 1 3 d S . . O1 O 0.3950(2) 0.4210(2) 0.04667(5) 0.0330(8) Uani 1 1 d . . . N1 N 0.2009(2) 0.2440(2) 0.07568(5) 0.0282(8) Uani 1 1 d . . . N2 N 0.3282(2) 0.3590(3) 0.05551(6) 0.0283(9) Uani 1 1 d . . . N3 N 0.5142(3) 0.3607(3) 0.05631(6) 0.0347(10) Uani 1 1 d . . . H3A H 0.5667 0.3706 0.0597 0.042 Uiso 1 1 calc R . . H3B H 0.4762 0.3237 0.0645 0.042 Uiso 1 1 calc R . . N4 N 0.5677(3) 0.5165(3) 0.03216(7) 0.0486(11) Uani 1 1 d U . . H4O H 0.6240 0.5321 0.0340 0.058 Uiso 1 1 calc R . . N5 N 0.5089(4) 0.5892(3) 0.06163(8) 0.0539(13) Uani 1 1 d . . . H5A H 0.4581 0.5782 0.0568 0.065 Uiso 1 1 calc R . . H5B H 0.5053 0.5959 0.0738 0.065 Uiso 1 1 calc R . . N6 N 0.3589(3) 0.2352(3) 0.08126(5) 0.0298(9) Uani 1 1 d . . . N7 N 0.3236(3) 0.1826(3) 0.06908(6) 0.0304(9) Uani 1 1 d . . . N8 N 0.2889(3) 0.1322(3) 0.05743(7) 0.0422(11) Uani 1 1 d . . . N9 N 0.6413(3) 0.5351(4) 0.06835(8) 0.0538(13) Uani 1 1 d . . . N10 N 0.6667 0.5476(3) 0.0833 0.0362(14) Uani 1 2 d S . . C1 C 0.1389(3) 0.1858(3) 0.08650(7) 0.0311(10) Uani 1 1 d . . . H1 H 0.1515 0.1826 0.0988 0.037 Uiso 1 1 calc R . . C2 C 0.0576(3) 0.1308(3) 0.08018(8) 0.0356(11) Uani 1 1 d . . . H2 H 0.0161 0.0907 0.0881 0.043 Uiso 1 1 calc R . . C3 C 0.0373(3) 0.1350(3) 0.06197(8) 0.0385(12) Uani 1 1 d . . . H3 H -0.0181 0.0990 0.0575 0.046 Uiso 1 1 calc R . . C4 C 0.1034(3) 0.1959(4) 0.05018(8) 0.0355(11) Uani 1 1 d . . . H4 H 0.0924 0.2005 0.0378 0.043 Uiso 1 1 calc R . . C5 C 0.1847(3) 0.2482(3) 0.05759(7) 0.0292(10) Uani 1 1 d . . . C6 C 0.2576(3) 0.3120(3) 0.04655(6) 0.0285(10) Uani 1 1 d . . . C7 C 0.2472(3) 0.3211(4) 0.02658(7) 0.0359(11) Uani 1 1 d . . . C8 C 0.2250(4) 0.2533(4) 0.01510(8) 0.0520(15) Uani 1 1 d . . . H8 H 0.2194 0.2019 0.0195 0.062 Uiso 1 1 calc R . . C9 C 0.2102(5) 0.2631(6) -0.00453(11) 0.075(2) Uani 1 1 d U . . H9 H 0.1949 0.2175 -0.0127 0.090 Uiso 1 1 calc R . . C10 C 0.2185(5) 0.3358(6) -0.01048(11) 0.076(2) Uani 1 1 d U . . H10 H 0.2052 0.3398 -0.0227 0.091 Uiso 1 1 calc R . . C11 C 0.2465(5) 0.4072(5) 0.00095(10) 0.0643(19) Uani 1 1 d . . . H11 H 0.2562 0.4594 -0.0039 0.077 Uiso 1 1 calc R . . C12 C 0.2601(4) 0.4008(4) 0.01938(8) 0.0483(14) Uani 1 1 d . . . H12 H 0.2775 0.4481 0.0271 0.058 Uiso 1 1 calc R . . C13 C 0.4941(4) 0.3174(4) 0.03842(8) 0.0479(14) Uani 1 1 d . . . H13A H 0.4354 0.3006 0.0350 0.058 Uiso 1 1 calc R . . H13B H 0.4983 0.2656 0.0393 0.058 Uiso 1 1 calc R . . C14 C 0.5556(4) 0.3761(4) 0.02363(9) 0.0555(16) Uani 1 1 d . . . H14A H 0.5484 0.3425 0.0126 0.067 Uiso 1 1 calc R . . H14B H 0.6144 0.3991 0.0279 0.067 Uiso 1 1 calc R . . C15 C 0.5412(4) 0.4506(4) 0.01879(9) 0.0560(17) Uani 1 1 d . . . H15A H 0.5716 0.4764 0.0074 0.067 Uiso 1 1 calc R . . H15B H 0.4802 0.4274 0.0165 0.067 Uiso 1 1 calc R . . C16 C 0.5740(6) 0.5992(5) 0.02582(11) 0.078(2) Uani 1 1 d U . . H16A H 0.5162 0.5901 0.0244 0.094 Uiso 1 1 calc R . . H16B H 0.6016 0.6140 0.0138 0.094 Uiso 1 1 calc R . . C18 C 0.5736(6) 0.6745(5) 0.05455(11) 0.082(2) Uani 1 1 d D . . H18A H 0.5443 0.7058 0.0512 0.098 Uiso 1 1 calc R . . H18B H 0.6133 0.7062 0.0645 0.098 Uiso 1 1 calc R . . C17 C 0.6234(6) 0.6740(5) 0.03873(11) 0.080(2) Uani 1 1 d D . . H17A H 0.6738 0.6724 0.0431 0.096 Uiso 1 1 calc R . . H17B H 0.6435 0.7273 0.0319 0.096 Uiso 1 1 calc R . . O1W O 0.0000 0.0000 0.0050(7) 0.195(18) Uani 1 3 d S . . 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 0.0257(3) 0.0278(4) 0.0207(4) 0.0005(3) 0.00024(16) 0.0139(2) Ni2 0.0290(4) 0.0363(4) 0.0267(4) 0.0012(3) 0.0018(2) 0.0148(3) I1 0.0799(6) 0.0799(6) 0.0909(11) 0.000 0.000 0.0400(3) I2 0.0798(4) 0.0798(4) 0.0553(5) 0.000 0.000 0.0399(2) O1 0.0319(18) 0.0381(19) 0.0284(18) 0.0045(14) 0.0017(14) 0.0171(15) N1 0.031(2) 0.029(2) 0.026(2) 0.0001(16) 0.0004(16) 0.0158(17) N2 0.029(2) 0.030(2) 0.029(2) 0.0030(16) 0.0016(16) 0.0171(18) N3 0.032(2) 0.043(2) 0.029(2) -0.0013(18) 0.0004(17) 0.0181(19) N4 0.044(3) 0.065(3) 0.036(3) 0.005(2) 0.005(2) 0.027(3) N5 0.057(3) 0.050(3) 0.051(3) 0.003(2) 0.013(2) 0.024(3) N6 0.035(2) 0.035(2) 0.023(2) 0.0001(17) -0.0013(17) 0.0201(19) N7 0.031(2) 0.035(2) 0.028(2) 0.0021(19) 0.0009(18) 0.0193(18) N8 0.042(3) 0.048(3) 0.036(3) -0.006(2) -0.005(2) 0.022(2) N9 0.040(3) 0.063(3) 0.046(3) 0.002(3) -0.003(2) 0.016(2) N10 0.030(3) 0.035(3) 0.042(4) 0.0016(14) 0.003(3) 0.0148(16) C1 0.034(3) 0.030(2) 0.032(3) 0.000(2) -0.001(2) 0.017(2) C2 0.032(3) 0.032(3) 0.042(3) 0.000(2) 0.000(2) 0.015(2) C3 0.033(3) 0.036(3) 0.046(3) 0.001(2) -0.002(2) 0.016(2) C4 0.036(3) 0.041(3) 0.033(3) -0.001(2) -0.004(2) 0.022(2) C5 0.030(2) 0.030(2) 0.030(3) -0.0014(19) -0.0023(19) 0.017(2) C6 0.033(3) 0.031(2) 0.025(2) -0.0017(19) -0.0009(19) 0.019(2) C7 0.032(3) 0.051(3) 0.028(3) 0.001(2) -0.003(2) 0.024(2) C8 0.047(3) 0.057(4) 0.043(4) -0.006(3) -0.004(3) 0.020(3) C9 0.069(5) 0.082(5) 0.058(5) -0.010(4) -0.002(4) 0.027(4) C10 0.062(4) 0.101(5) 0.053(4) 0.008(4) -0.007(4) 0.033(5) C11 0.064(4) 0.077(5) 0.055(4) 0.008(4) 0.000(3) 0.038(4) C12 0.054(4) 0.058(4) 0.039(3) 0.005(3) 0.003(3) 0.033(3) C13 0.051(3) 0.052(3) 0.037(3) -0.006(3) 0.002(3) 0.023(3) C14 0.055(4) 0.065(4) 0.048(4) -0.001(3) 0.012(3) 0.031(3) C15 0.051(4) 0.067(4) 0.038(4) 0.004(3) 0.007(3) 0.021(3) C16 0.094(6) 0.075(5) 0.065(5) 0.016(4) -0.001(4) 0.042(5) C18 0.086(6) 0.068(5) 0.076(6) 0.015(4) 0.018(5) 0.027(4) C17 0.104(7) 0.061(5) 0.066(5) 0.013(4) 0.019(5) 0.035(5) O1W 0.195(10) 0.195(10) 0.19(6) 0.000 0.000 0.098(5) _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 N2 2.066(4) 17_554 ? Ni1 N2 2.066(4) . ? Ni1 N1 2.069(4) 17_554 ? Ni1 N1 2.069(4) . ? Ni1 N6 2.126(4) . ? Ni1 N6 2.126(4) 17_554 ? Ni2 O1 2.040(3) . ? Ni2 N3 2.059(4) . ? Ni2 N9 2.100(5) . ? Ni2 N5 2.100(5) . ? Ni2 N4 2.103(5) . ? Ni2 N6 2.159(4) 17_554 ? O1 N2 1.322(5) . ? N1 C1 1.334(6) . ? N1 C5 1.354(6) . ? N2 C6 1.291(6) . ? N3 C13 1.462(7) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C15 1.414(8) . ? N4 C16 1.501(9) . ? N4 H4O 0.9100 . ? N5 C18 1.474(9) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N6 N7 1.215(6) . ? N6 Ni2 2.159(4) 17_554 ? N7 N8 1.164(6) . ? N9 N10 1.156(6) . ? N10 N9 1.156(6) 18_654 ? C1 C2 1.366(7) . ? C1 H1 0.9300 . ? C2 C3 1.383(8) . ? C2 H2 0.9300 . ? C3 C4 1.426(8) . ? C3 H3 0.9300 . ? C4 C5 1.386(7) . ? C4 H4 0.9300 . ? C5 C6 1.470(7) . ? C6 C7 1.480(7) . ? C7 C8 1.359(8) . ? C7 C12 1.426(8) . ? C8 C9 1.476(10) . ? C8 H8 0.9300 . ? C9 C10 1.308(11) . ? C9 H9 0.9300 . ? C10 C11 1.392(11) . ? C10 H10 0.9300 . ? C11 C12 1.374(9) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.521(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.521(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.507(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C18 C17 1.458(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? O1W O1W 0.73(10) 19 ? 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 N2 Ni1 N2 169.9(2) 17_554 . ? N2 Ni1 N1 78.81(15) 17_554 17_554 ? N2 Ni1 N1 94.16(15) . 17_554 ? N2 Ni1 N1 94.16(15) 17_554 . ? N2 Ni1 N1 78.80(15) . . ? N1 Ni1 N1 92.3(2) 17_554 . ? N2 Ni1 N6 89.54(15) 17_554 . ? N2 Ni1 N6 97.47(15) . . ? N1 Ni1 N6 168.34(15) 17_554 . ? N1 Ni1 N6 89.01(15) . . ? N2 Ni1 N6 97.48(15) 17_554 17_554 ? N2 Ni1 N6 89.54(15) . 17_554 ? N1 Ni1 N6 89.01(15) 17_554 17_554 ? N1 Ni1 N6 168.33(15) . 17_554 ? N6 Ni1 N6 92.0(2) . 17_554 ? O1 Ni2 N3 90.85(15) . . ? O1 Ni2 N9 174.79(18) . . ? N3 Ni2 N9 89.6(2) . . ? O1 Ni2 N5 87.95(19) . . ? N3 Ni2 N5 177.32(19) . . ? N9 Ni2 N5 91.8(2) . . ? O1 Ni2 N4 88.22(17) . . ? N3 Ni2 N4 92.88(19) . . ? N9 Ni2 N4 86.6(2) . . ? N5 Ni2 N4 89.5(2) . . ? O1 Ni2 N6 90.92(14) . 17_554 ? N3 Ni2 N6 86.84(16) . 17_554 ? N9 Ni2 N6 94.28(19) . 17_554 ? N5 Ni2 N6 90.78(18) . 17_554 ? N4 Ni2 N6 179.10(19) . 17_554 ? N2 O1 Ni2 119.1(3) . . ? C1 N1 C5 119.8(4) . . ? C1 N1 Ni1 126.9(3) . . ? C5 N1 Ni1 113.3(3) . . ? C6 N2 O1 118.9(4) . . ? C6 N2 Ni1 116.1(3) . . ? O1 N2 Ni1 124.9(3) . . ? C13 N3 Ni2 118.4(4) . . ? C13 N3 H3A 107.7 . . ? Ni2 N3 H3A 107.7 . . ? C13 N3 H3B 107.7 . . ? Ni2 N3 H3B 107.7 . . ? H3A N3 H3B 107.1 . . ? C15 N4 C16 116.2(6) . . ? C15 N4 Ni2 115.3(4) . . ? C16 N4 Ni2 114.9(4) . . ? C15 N4 H4O 102.5 . . ? C16 N4 H4O 102.5 . . ? Ni2 N4 H4O 102.5 . . ? C18 N5 Ni2 125.2(5) . . ? C18 N5 H5A 106.0 . . ? Ni2 N5 H5A 106.0 . . ? C18 N5 H5B 106.0 . . ? Ni2 N5 H5B 106.0 . . ? H5A N5 H5B 106.3 . . ? N7 N6 Ni1 116.1(3) . . ? N7 N6 Ni2 119.0(3) . 17_554 ? Ni1 N6 Ni2 111.34(17) . 17_554 ? N8 N7 N6 179.3(5) . . ? N10 N9 Ni2 129.7(4) . . ? N9 N10 N9 179.7(8) 18_654 . ? N1 C1 C2 122.4(5) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 119.7(5) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 118.4(5) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 118.3(5) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? N1 C5 C4 121.4(5) . . ? N1 C5 C6 116.1(4) . . ? C4 C5 C6 122.5(5) . . ? N2 C6 C5 115.6(4) . . ? N2 C6 C7 123.9(4) . . ? C5 C6 C7 120.5(4) . . ? C8 C7 C12 119.9(5) . . ? C8 C7 C6 119.9(5) . . ? C12 C7 C6 120.2(5) . . ? C7 C8 C9 118.3(7) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? C10 C9 C8 120.0(8) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 121.8(8) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C12 C11 C10 120.1(7) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C7 119.6(6) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? N3 C13 C14 111.0(5) . . ? N3 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? N3 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C13 C14 C15 112.8(5) . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N4 C15 C14 116.1(6) . . ? N4 C15 H15A 108.3 . . ? C14 C15 H15A 108.3 . . ? N4 C15 H15B 108.3 . . ? C14 C15 H15B 108.3 . . ? H15A C15 H15B 107.4 . . ? N4 C16 C17 114.0(7) . . ? N4 C16 H16A 108.7 . . ? C17 C16 H16A 108.7 . . ? N4 C16 H16B 108.7 . . ? C17 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C17 C18 N5 115.7(7) . . ? C17 C18 H18A 108.3 . . ? N5 C18 H18A 108.3 . . ? C17 C18 H18B 108.3 . . ? N5 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? C18 C17 C16 113.9(8) . . ? C18 C17 H17A 108.8 . . ? C16 C17 H17A 108.8 . . ? C18 C17 H17B 108.8 . . ? C16 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.153 _refine_diff_density_min -2.239 _refine_diff_density_rms 0.132