# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'E Bouwman' 'Joris Berding' 'Martin Lutz' 'A Spek' 'Thomas F. van Dijkman' _publ_contact_author_name 'E Bouwman' _publ_contact_author_email BOUWMAN@CHEM.LEIDENUNIV.NL _publ_section_title ; N-donor functionalized N-heterocyclic carbene nickel(II) complexes in the Kumada coupling ; # Attachment 'deposit.cif' data_s4110a _database_code_depnum_ccdc_archive 'CCDC 723717' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 N6 Ni O2, 2(C H4 O), 0.5(H2 O)' _chemical_formula_sum 'C26 H33 N6 Ni O4.50' _chemical_formula_weight 560.29 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.7321(3) _cell_length_b 8.5908(1) _cell_length_c 33.5771(6) _cell_angle_alpha 90.00 _cell_angle_beta 117.8263(8) _cell_angle_gamma 90.00 _cell_volume 5288.74(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 132761 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 41023 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 27.45 _reflns_number_total 11971 _reflns_number_gt 8536 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement HKL2000 _computing_data_reduction 'HKL2000, Sortav' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+2.2204P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11971 _refine_ls_number_parameters 684 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.012 _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 0.376460(15) 0.30319(3) 0.124812(9) 0.02024(8) Uani 1 1 d . . . N11 N 0.29848(11) 0.1004(2) 0.15921(6) 0.0282(5) Uani 1 1 d . . . C12 C 0.35296(12) 0.1326(3) 0.14907(7) 0.0237(5) Uani 1 1 d . . . N13 N 0.39331(11) 0.0022(2) 0.15912(6) 0.0271(4) Uani 1 1 d . . . C14 C 0.36506(15) -0.1122(3) 0.17527(8) 0.0345(6) Uani 1 1 d . . . H14 H 0.3838 -0.2142 0.1844 0.041 Uiso 1 1 calc R . . C15 C 0.30595(15) -0.0506(3) 0.17545(8) 0.0356(6) Uani 1 1 d . . . H15 H 0.2747 -0.1011 0.1850 0.043 Uiso 1 1 calc R . . C16 C 0.24354(15) 0.2102(3) 0.15662(9) 0.0358(6) Uani 1 1 d . . . H16A H 0.2647 0.3149 0.1638 0.054 Uiso 1 1 calc R . . H16B H 0.2264 0.1806 0.1782 0.054 Uiso 1 1 calc R . . H16C H 0.2025 0.2095 0.1261 0.054 Uiso 1 1 calc R . . C17 C 0.46046(13) -0.0067(3) 0.15519(8) 0.0292(5) Uani 1 1 d . . . H17A H 0.4481 -0.0115 0.1230 0.035 Uiso 1 1 calc R . . H17B H 0.4869 -0.1034 0.1698 0.035 Uiso 1 1 calc R . . C18 C 0.50989(13) 0.1331(3) 0.17700(7) 0.0248(5) Uani 1 1 d . . . O19 O 0.57657(9) 0.1034(2) 0.20075(6) 0.0332(4) Uani 1 1 d . . . N110 N 0.47853(10) 0.2715(2) 0.16869(6) 0.0214(4) Uani 1 1 d . . . C111 C 0.52244(12) 0.4044(3) 0.19052(7) 0.0220(5) Uani 1 1 d . . . C112 C 0.49666(13) 0.5088(3) 0.21124(7) 0.0247(5) Uani 1 1 d . . . H112 H 0.4519 0.4885 0.2117 0.030 Uiso 1 1 calc R . . C113 C 0.53566(15) 0.6426(3) 0.23134(8) 0.0319(6) Uani 1 1 d . . . H113 H 0.5177 0.7130 0.2456 0.038 Uiso 1 1 calc R . . C114 C 0.60038(15) 0.6743(3) 0.23075(8) 0.0349(6) Uani 1 1 d . . . H114 H 0.6268 0.7666 0.2443 0.042 Uiso 1 1 calc R . . C115 C 0.62657(14) 0.5707(3) 0.21022(9) 0.0346(6) Uani 1 1 d . . . H115 H 0.6712 0.5919 0.2098 0.042 Uiso 1 1 calc R . . C116 C 0.58802(13) 0.4355(3) 0.19012(8) 0.0286(5) Uani 1 1 d . . . H116 H 0.6064 0.3646 0.1762 0.034 Uiso 1 1 calc R . . N21 N 0.22963(10) 0.2237(2) 0.05043(6) 0.0233(4) Uani 1 1 d . . . C22 C 0.27985(12) 0.3217(3) 0.08005(7) 0.0215(5) Uani 1 1 d . . . N23 N 0.24809(10) 0.4634(2) 0.06942(6) 0.0233(4) Uani 1 1 d . . . C24 C 0.17921(13) 0.4557(3) 0.03256(8) 0.0290(5) Uani 1 1 d . . . H24 H 0.1467 0.5398 0.0184 0.035 Uiso 1 1 calc R . . C25 C 0.16797(13) 0.3050(3) 0.02099(8) 0.0284(5) Uani 1 1 d . . . H25 H 0.1254 0.2617 -0.0030 0.034 Uiso 1 1 calc R . . C26 C 0.23772(14) 0.0560(3) 0.04789(8) 0.0316(6) Uani 1 1 d . . . H26A H 0.2896 0.0286 0.0636 0.047 Uiso 1 1 calc R . . H26B H 0.2169 0.0244 0.0163 0.047 Uiso 1 1 calc R . . H26C H 0.2121 0.0023 0.0621 0.047 Uiso 1 1 calc R . . C27 C 0.28890(13) 0.6024(3) 0.09285(8) 0.0275(5) Uani 1 1 d . . . H27A H 0.3010 0.5970 0.1250 0.033 Uiso 1 1 calc R . . H27B H 0.2585 0.6961 0.0796 0.033 Uiso 1 1 calc R . . C28 C 0.35885(13) 0.6148(3) 0.08876(7) 0.0226(5) Uani 1 1 d . . . O29 O 0.37016(10) 0.74027(19) 0.07440(6) 0.0331(4) Uani 1 1 d . . . N210 N 0.39921(10) 0.4860(2) 0.09920(6) 0.0213(4) Uani 1 1 d . . . C211 C 0.45613(12) 0.4730(3) 0.08700(7) 0.0236(5) Uani 1 1 d . . . C212 C 0.46593(13) 0.3286(3) 0.07201(8) 0.0271(5) Uani 1 1 d . . . H212 H 0.4364 0.2434 0.0716 0.033 Uiso 1 1 calc R . . C213 C 0.51792(15) 0.3067(3) 0.05774(9) 0.0373(6) Uani 1 1 d . . . H213 H 0.5240 0.2072 0.0476 0.045 Uiso 1 1 calc R . . C214 C 0.56101(15) 0.4297(4) 0.05818(9) 0.0407(7) Uani 1 1 d . . . H214 H 0.5960 0.4158 0.0477 0.049 Uiso 1 1 calc R . . C215 C 0.55300(14) 0.5723(3) 0.07380(9) 0.0388(7) Uani 1 1 d . . . H215 H 0.5832 0.6566 0.0745 0.047 Uiso 1 1 calc R . . C216 C 0.50141(14) 0.5948(3) 0.08846(8) 0.0316(6) Uani 1 1 d . . . H216 H 0.4969 0.6937 0.0996 0.038 Uiso 1 1 calc R . . Ni2 Ni 1.105726(15) 0.07084(3) 0.375777(9) 0.01964(8) Uani 1 1 d . . . N31 N 1.18858(11) -0.1408(2) 0.34690(6) 0.0257(4) Uani 1 1 d . . . C32 C 1.13118(12) -0.1020(3) 0.35363(7) 0.0222(5) Uani 1 1 d . . . N33 N 1.08929(11) -0.2308(2) 0.34275(6) 0.0234(4) Uani 1 1 d . . . C34 C 1.12017(14) -0.3500(3) 0.32978(8) 0.0306(6) Uani 1 1 d . . . H34 H 1.1012 -0.4520 0.3209 0.037 Uiso 1 1 calc R . . C35 C 1.18218(14) -0.2935(3) 0.33221(8) 0.0313(6) Uani 1 1 d . . . H35 H 1.2155 -0.3479 0.3252 0.038 Uiso 1 1 calc R . . C36 C 1.24672(14) -0.0357(3) 0.35122(9) 0.0345(6) Uani 1 1 d . . . H36A H 1.2264 0.0682 0.3406 0.052 Uiso 1 1 calc R . . H36B H 1.2690 -0.0748 0.3331 0.052 Uiso 1 1 calc R . . H36C H 1.2838 -0.0298 0.3829 0.052 Uiso 1 1 calc R . . C37 C 1.01903(13) -0.2323(3) 0.34292(8) 0.0277(5) Uani 1 1 d . . . H37A H 1.0273 -0.2342 0.3744 0.033 Uiso 1 1 calc R . . H37B H 0.9923 -0.3282 0.3279 0.033 Uiso 1 1 calc R . . C38 C 0.97233(13) -0.0900(3) 0.31880(8) 0.0263(5) Uani 1 1 d . . . O39 O 0.90670(10) -0.1158(2) 0.29308(7) 0.0453(5) Uani 1 1 d . . . N310 N 1.00709(10) 0.0461(2) 0.32796(6) 0.0209(4) Uani 1 1 d . . . C311 C 0.96831(12) 0.1805(3) 0.30337(7) 0.0224(5) Uani 1 1 d . . . C312 C 1.00286(14) 0.2791(3) 0.28668(7) 0.0258(5) Uani 1 1 d . . . H312 H 1.0500 0.2536 0.2905 0.031 Uiso 1 1 calc R . . C313 C 0.96876(15) 0.4156(3) 0.26432(8) 0.0320(6) Uani 1 1 d . . . H313 H 0.9927 0.4821 0.2528 0.038 Uiso 1 1 calc R . . C314 C 0.90071(15) 0.4549(3) 0.25873(8) 0.0356(6) Uani 1 1 d . . . H314 H 0.8779 0.5487 0.2438 0.043 Uiso 1 1 calc R . . C315 C 0.86587(15) 0.3555(3) 0.27516(9) 0.0371(6) Uani 1 1 d . . . H315 H 0.8187 0.3812 0.2713 0.045 Uiso 1 1 calc R . . C316 C 0.89930(14) 0.2190(3) 0.29722(8) 0.0305(6) Uani 1 1 d . . . H316 H 0.8748 0.1516 0.3082 0.037 Uiso 1 1 calc R . . N41 N 1.24475(10) -0.0285(2) 0.45300(6) 0.0231(4) Uani 1 1 d . . . C42 C 1.19894(12) 0.0785(3) 0.42354(7) 0.0218(5) Uani 1 1 d . . . N43 N 1.23551(10) 0.2142(2) 0.43684(6) 0.0223(4) Uani 1 1 d . . . C44 C 1.30278(13) 0.1947(3) 0.47413(8) 0.0273(5) Uani 1 1 d . . . H44 H 1.3380 0.2731 0.4896 0.033 Uiso 1 1 calc R . . C45 C 1.30811(13) 0.0415(3) 0.48404(8) 0.0267(5) Uani 1 1 d . . . H45 H 1.3482 -0.0088 0.5080 0.032 Uiso 1 1 calc R . . C46 C 1.22841(14) -0.1939(3) 0.45371(8) 0.0310(6) Uani 1 1 d . . . H46A H 1.1758 -0.2074 0.4425 0.047 Uiso 1 1 calc R . . H46B H 1.2547 -0.2332 0.4846 0.047 Uiso 1 1 calc R . . H46C H 1.2438 -0.2519 0.4344 0.047 Uiso 1 1 calc R . . C47 C 1.20033(13) 0.3602(3) 0.41530(9) 0.0278(5) Uani 1 1 d . . . H47A H 1.1917 0.3611 0.3837 0.033 Uiso 1 1 calc R . . H47B H 1.2327 0.4487 0.4313 0.033 Uiso 1 1 calc R . . C48 C 1.12785(13) 0.3782(3) 0.41632(7) 0.0241(5) Uani 1 1 d . . . O49 O 1.11842(10) 0.50216(19) 0.43223(6) 0.0357(4) Uani 1 1 d . . . N410 N 1.08295(10) 0.2563(2) 0.40074(6) 0.0206(4) Uani 1 1 d . . . C411 C 1.01733(12) 0.2574(3) 0.40427(7) 0.0228(5) Uani 1 1 d . . . C412 C 0.99452(14) 0.1192(3) 0.41548(8) 0.0279(5) Uani 1 1 d . . . H412 H 1.0248 0.0296 0.4227 0.033 Uiso 1 1 calc R . . C413 C 0.92915(15) 0.1103(3) 0.41629(9) 0.0378(6) Uani 1 1 d . . . H413 H 0.9143 0.0146 0.4236 0.045 Uiso 1 1 calc R . . C414 C 0.88447(16) 0.2403(3) 0.40649(10) 0.0419(7) Uani 1 1 d . . . H414 H 0.8390 0.2341 0.4069 0.050 Uiso 1 1 calc R . . C415 C 0.90696(14) 0.3776(3) 0.39624(9) 0.0393(6) Uani 1 1 d . . . H415 H 0.8770 0.4674 0.3900 0.047 Uiso 1 1 calc R . . C416 C 0.97231(13) 0.3883(3) 0.39482(8) 0.0307(6) Uani 1 1 d . . . H416 H 0.9867 0.4844 0.3874 0.037 Uiso 1 1 calc R . . O5 O 0.67038(10) 0.0581(2) 0.29025(6) 0.0405(5) Uani 1 1 d . . . H5O H 0.6357 0.0869 0.2602 0.061 Uiso 1 1 d . . . C5 C 0.73565(17) 0.0792(4) 0.28827(11) 0.0507(8) Uani 1 1 d . . . H5A H 0.7458 -0.0134 0.2751 0.076 Uiso 1 1 calc R . . H5B H 0.7756 0.0954 0.3187 0.076 Uiso 1 1 calc R . . H5C H 0.7314 0.1703 0.2696 0.076 Uiso 1 1 calc R . . O6 O 0.37437(13) 0.9752(2) 0.02339(7) 0.0535(6) Uani 1 1 d . . . H6O H 0.3698 0.8982 0.0412 0.080 Uiso 1 1 d . . . C6 C 0.41278(19) 0.9232(4) 0.00158(12) 0.0539(8) Uani 1 1 d . . . H6A H 0.4223 1.0109 -0.0136 0.081 Uiso 1 1 calc R . . H6B H 0.3840 0.8442 -0.0207 0.081 Uiso 1 1 calc R . . H6C H 0.4592 0.8778 0.0236 0.081 Uiso 1 1 calc R . . O7 O 1.08113(13) 0.7347(2) 0.47305(8) 0.0586(6) Uani 1 1 d . . . H7O H 1.0862 0.6626 0.4555 0.088 Uiso 1 1 d . . . C7 C 1.01223(18) 0.7201(4) 0.47128(11) 0.0521(8) Uani 1 1 d . . . H7A H 1.0101 0.6223 0.4857 0.078 Uiso 1 1 calc R . . H7B H 0.9743 0.7200 0.4398 0.078 Uiso 1 1 calc R . . H7C H 1.0043 0.8078 0.4872 0.078 Uiso 1 1 calc R . . O8 O 0.67622(11) 0.0228(3) 0.17240(7) 0.0601(6) Uani 1 1 d . . . H8O H 0.6375 0.0391 0.1838 0.090 Uiso 1 1 d . . . C8 C 0.6361(2) -0.0436(6) 0.13089(13) 0.0891(15) Uani 1 1 d . . . H8A H 0.5951 0.0245 0.1123 0.134 Uiso 1 1 calc R . . H8B H 0.6176 -0.1448 0.1344 0.134 Uiso 1 1 calc R . . H8C H 0.6671 -0.0580 0.1163 0.134 Uiso 1 1 calc R . . O9 O 0.80686(14) -0.1726(3) 0.20303(9) 0.0812(9) Uani 1 1 d . . . H9A H 0.7617 -0.1177 0.2011 0.122 Uiso 1 1 d . . . H9B H 0.8412 -0.1591 0.2341 0.122 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01974(15) 0.01717(15) 0.01981(15) 0.00176(11) 0.00589(12) -0.00051(11) N11 0.0285(11) 0.0275(11) 0.0256(10) 0.0011(8) 0.0103(9) -0.0088(9) C12 0.0247(12) 0.0236(12) 0.0174(11) -0.0015(9) 0.0052(9) -0.0044(10) N13 0.0315(11) 0.0167(10) 0.0246(10) 0.0009(8) 0.0060(9) -0.0038(8) C14 0.0415(16) 0.0207(12) 0.0284(13) 0.0035(10) 0.0055(12) -0.0077(11) C15 0.0437(16) 0.0291(14) 0.0272(13) 0.0023(11) 0.0108(12) -0.0145(12) C16 0.0336(14) 0.0357(15) 0.0419(15) -0.0052(12) 0.0208(12) -0.0074(12) C17 0.0288(13) 0.0192(11) 0.0313(13) 0.0001(10) 0.0071(11) 0.0033(10) C18 0.0258(12) 0.0241(12) 0.0211(11) 0.0002(9) 0.0082(10) 0.0007(10) O19 0.0256(9) 0.0283(9) 0.0361(10) 0.0021(8) 0.0065(8) 0.0069(7) N110 0.0216(10) 0.0192(9) 0.0190(9) 0.0015(7) 0.0057(8) 0.0009(8) C111 0.0225(11) 0.0202(11) 0.0160(10) 0.0018(9) 0.0029(9) 0.0001(9) C112 0.0264(12) 0.0223(12) 0.0212(11) 0.0037(9) 0.0077(10) 0.0036(10) C113 0.0436(16) 0.0209(12) 0.0214(12) -0.0003(10) 0.0070(11) 0.0049(11) C114 0.0359(15) 0.0224(13) 0.0288(13) -0.0005(10) 0.0003(11) -0.0044(11) C115 0.0280(13) 0.0330(14) 0.0341(14) 0.0018(11) 0.0072(11) -0.0080(11) C116 0.0265(13) 0.0293(13) 0.0265(12) -0.0010(10) 0.0094(10) -0.0007(10) N21 0.0206(10) 0.0237(10) 0.0208(10) -0.0007(8) 0.0056(8) -0.0009(8) C22 0.0226(11) 0.0198(11) 0.0213(11) 0.0008(9) 0.0095(9) -0.0005(9) N23 0.0201(10) 0.0223(10) 0.0246(10) 0.0032(8) 0.0083(8) 0.0025(8) C24 0.0219(12) 0.0340(14) 0.0272(12) 0.0062(11) 0.0081(10) 0.0047(10) C25 0.0199(12) 0.0390(14) 0.0217(12) 0.0020(11) 0.0057(9) 0.0008(11) C26 0.0341(14) 0.0229(12) 0.0317(13) -0.0062(10) 0.0104(11) -0.0042(11) C27 0.0283(13) 0.0192(11) 0.0340(13) 0.0012(10) 0.0137(11) 0.0026(10) C28 0.0275(12) 0.0179(11) 0.0199(11) 0.0005(9) 0.0090(9) -0.0004(9) O29 0.0369(10) 0.0207(9) 0.0432(10) 0.0068(8) 0.0199(9) 0.0019(8) N210 0.0205(9) 0.0203(9) 0.0209(9) 0.0013(8) 0.0080(8) -0.0006(8) C211 0.0218(12) 0.0269(12) 0.0174(11) 0.0041(9) 0.0051(9) 0.0003(10) C212 0.0264(13) 0.0288(13) 0.0227(12) -0.0012(10) 0.0086(10) -0.0008(10) C213 0.0342(15) 0.0439(16) 0.0346(14) -0.0063(12) 0.0166(12) 0.0020(13) C214 0.0286(14) 0.0597(19) 0.0379(15) -0.0006(14) 0.0190(12) 0.0000(13) C215 0.0283(14) 0.0439(17) 0.0436(16) 0.0050(13) 0.0164(12) -0.0072(12) C216 0.0308(14) 0.0303(13) 0.0322(13) 0.0027(11) 0.0136(11) -0.0003(11) Ni2 0.01974(15) 0.01569(14) 0.01889(15) -0.00101(11) 0.00515(12) 0.00043(11) N31 0.0255(10) 0.0246(10) 0.0235(10) -0.0015(8) 0.0085(8) 0.0048(8) C32 0.0229(12) 0.0216(11) 0.0151(10) 0.0023(9) 0.0030(9) 0.0005(9) N33 0.0274(11) 0.0173(9) 0.0191(9) 0.0000(8) 0.0056(8) 0.0031(8) C34 0.0347(14) 0.0186(12) 0.0257(12) -0.0019(10) 0.0032(11) 0.0063(10) C35 0.0357(14) 0.0265(13) 0.0248(12) -0.0012(10) 0.0084(11) 0.0102(11) C36 0.0257(13) 0.0410(15) 0.0368(14) -0.0019(12) 0.0147(11) 0.0008(12) C37 0.0273(13) 0.0213(12) 0.0309(13) -0.0027(10) 0.0106(10) -0.0057(10) C38 0.0238(12) 0.0244(12) 0.0260(12) -0.0018(10) 0.0076(10) -0.0023(10) O39 0.0269(10) 0.0298(10) 0.0570(12) -0.0003(9) 0.0011(9) -0.0056(8) N310 0.0214(10) 0.0183(9) 0.0191(9) 0.0009(7) 0.0062(8) 0.0003(8) C311 0.0244(12) 0.0206(11) 0.0161(10) -0.0022(9) 0.0044(9) 0.0009(9) C312 0.0297(13) 0.0229(12) 0.0223(11) -0.0031(9) 0.0101(10) -0.0043(10) C313 0.0440(16) 0.0238(13) 0.0205(12) 0.0001(10) 0.0086(11) -0.0059(11) C314 0.0435(16) 0.0241(13) 0.0223(12) 0.0030(10) 0.0011(11) 0.0063(11) C315 0.0311(14) 0.0376(15) 0.0329(14) 0.0019(12) 0.0068(11) 0.0114(12) C316 0.0277(13) 0.0315(14) 0.0266(13) 0.0054(10) 0.0080(10) 0.0041(11) N41 0.0232(10) 0.0226(10) 0.0192(9) 0.0000(8) 0.0062(8) 0.0023(8) C42 0.0247(12) 0.0193(11) 0.0212(11) -0.0010(9) 0.0105(9) 0.0025(9) N43 0.0209(10) 0.0188(10) 0.0230(10) -0.0033(8) 0.0067(8) -0.0007(8) C44 0.0203(12) 0.0285(13) 0.0254(12) -0.0060(10) 0.0043(10) -0.0038(10) C45 0.0213(12) 0.0320(13) 0.0198(11) -0.0030(10) 0.0038(9) 0.0031(10) C46 0.0372(14) 0.0187(12) 0.0291(13) 0.0036(10) 0.0086(11) 0.0008(11) C47 0.0277(13) 0.0164(11) 0.0376(14) -0.0002(10) 0.0138(11) -0.0013(10) C48 0.0284(12) 0.0173(11) 0.0225(11) 0.0004(9) 0.0085(10) 0.0006(10) O49 0.0347(10) 0.0212(9) 0.0486(11) -0.0119(8) 0.0172(9) -0.0009(8) N410 0.0203(10) 0.0186(9) 0.0211(9) 0.0003(7) 0.0081(8) 0.0012(8) C411 0.0235(12) 0.0231(11) 0.0190(11) -0.0022(9) 0.0076(9) 0.0000(9) C412 0.0338(14) 0.0258(12) 0.0251(12) 0.0001(10) 0.0146(11) 0.0001(11) C413 0.0390(16) 0.0397(15) 0.0409(15) 0.0006(12) 0.0238(13) -0.0066(13) C414 0.0326(15) 0.0481(17) 0.0510(17) -0.0038(14) 0.0246(14) -0.0001(13) C415 0.0295(14) 0.0397(16) 0.0459(16) -0.0014(13) 0.0151(13) 0.0086(12) C416 0.0298(13) 0.0262(13) 0.0318(13) -0.0014(10) 0.0107(11) 0.0016(11) O5 0.0358(11) 0.0499(12) 0.0361(10) 0.0024(9) 0.0171(9) 0.0049(9) C5 0.0449(18) 0.054(2) 0.0487(18) -0.0016(15) 0.0184(15) -0.0065(15) O6 0.0922(18) 0.0276(10) 0.0683(14) 0.0113(10) 0.0606(14) 0.0121(11) C6 0.065(2) 0.0429(18) 0.073(2) 0.0056(16) 0.0488(19) 0.0068(16) O7 0.0645(15) 0.0459(13) 0.0818(16) -0.0297(12) 0.0481(14) -0.0152(11) C7 0.057(2) 0.0436(18) 0.061(2) -0.0081(15) 0.0328(17) -0.0058(15) O8 0.0385(12) 0.0925(18) 0.0479(13) -0.0084(12) 0.0190(10) -0.0019(12) C8 0.054(2) 0.137(4) 0.063(2) -0.036(3) 0.016(2) 0.005(3) O9 0.0696(17) 0.0604(16) 0.0698(16) -0.0174(13) -0.0042(13) 0.0178(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C12 1.849(2) . ? Ni1 C22 1.867(2) . ? Ni1 N210 1.9511(18) . ? Ni1 N110 1.9524(18) . ? N11 C12 1.352(3) . ? N11 C15 1.388(3) . ? N11 C16 1.450(3) . ? C12 N13 1.343(3) . ? N13 C14 1.378(3) . ? N13 C17 1.460(3) . ? C14 C15 1.337(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.526(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O19 1.258(3) . ? C18 N110 1.321(3) . ? N110 C111 1.430(3) . ? C111 C112 1.386(3) . ? C111 C116 1.392(3) . ? C112 C113 1.386(3) . ? C112 H112 0.9500 . ? C113 C114 1.378(4) . ? C113 H113 0.9500 . ? C114 C115 1.383(4) . ? C114 H114 0.9500 . ? C115 C116 1.393(3) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N21 C22 1.347(3) . ? N21 C25 1.385(3) . ? N21 C26 1.457(3) . ? C22 N23 1.350(3) . ? N23 C24 1.388(3) . ? N23 C27 1.463(3) . ? C24 C25 1.341(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.523(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O29 1.247(3) . ? C28 N210 1.332(3) . ? N210 C211 1.423(3) . ? C211 C212 1.389(3) . ? C211 C216 1.391(3) . ? C212 C213 1.381(4) . ? C212 H212 0.9500 . ? C213 C214 1.379(4) . ? C213 H213 0.9500 . ? C214 C215 1.373(4) . ? C214 H214 0.9500 . ? C215 C216 1.384(4) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? Ni2 C32 1.845(2) . ? Ni2 C42 1.849(2) . ? Ni2 N310 1.9338(18) . ? Ni2 N410 1.9582(18) . ? N31 C32 1.352(3) . ? N31 C35 1.386(3) . ? N31 C36 1.458(3) . ? C32 N33 1.347(3) . ? N33 C34 1.382(3) . ? N33 C37 1.459(3) . ? C34 C35 1.340(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.535(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 O39 1.245(3) . ? C38 N310 1.332(3) . ? N310 C311 1.428(3) . ? C311 C312 1.386(3) . ? C311 C316 1.387(3) . ? C312 C313 1.394(3) . ? C312 H312 0.9500 . ? C313 C314 1.376(4) . ? C313 H313 0.9500 . ? C314 C315 1.388(4) . ? C314 H314 0.9500 . ? C315 C316 1.387(3) . ? C315 H315 0.9500 . ? C316 H316 0.9500 . ? N41 C42 1.359(3) . ? N41 C45 1.377(3) . ? N41 C46 1.464(3) . ? C42 N43 1.348(3) . ? N43 C44 1.382(3) . ? N43 C47 1.461(3) . ? C44 C45 1.349(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.527(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 O49 1.247(3) . ? C48 N410 1.334(3) . ? N410 C411 1.420(3) . ? C411 C412 1.393(3) . ? C411 C416 1.400(3) . ? C412 C413 1.370(4) . ? C412 H412 0.9500 . ? C413 C414 1.389(4) . ? C413 H413 0.9500 . ? C414 C415 1.370(4) . ? C414 H414 0.9500 . ? C415 C416 1.381(4) . ? C415 H415 0.9500 . ? C416 H416 0.9500 . ? O5 C5 1.397(4) . ? O5 H5O 0.9586 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? O6 C6 1.384(3) . ? O6 H6O 0.9258 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O7 C7 1.407(4) . ? O7 H7O 0.8944 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? O8 C8 1.370(4) . ? O8 H8O 1.0475 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O9 H9A 1.0233 . ? O9 H9B 0.9567 . ? 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 C12 Ni1 C22 91.02(10) . . ? C12 Ni1 N210 178.57(9) . . ? C22 Ni1 N210 88.05(9) . . ? C12 Ni1 N110 88.44(9) . . ? C22 Ni1 N110 175.52(9) . . ? N210 Ni1 N110 92.57(8) . . ? C12 N11 C15 109.7(2) . . ? C12 N11 C16 125.2(2) . . ? C15 N11 C16 124.9(2) . . ? N13 C12 N11 105.2(2) . . ? N13 C12 Ni1 120.67(18) . . ? N11 C12 Ni1 134.11(18) . . ? C12 N13 C14 111.4(2) . . ? C12 N13 C17 121.97(19) . . ? C14 N13 C17 126.6(2) . . ? C15 C14 N13 106.2(2) . . ? C15 C14 H14 126.9 . . ? N13 C14 H14 126.9 . . ? C14 C15 N11 107.6(2) . . ? C14 C15 H15 126.2 . . ? N11 C15 H15 126.2 . . ? N11 C16 H16A 109.5 . . ? N11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N13 C17 C18 111.72(19) . . ? N13 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N13 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? O19 C18 N110 127.1(2) . . ? O19 C18 C17 116.0(2) . . ? N110 C18 C17 116.9(2) . . ? C18 N110 C111 118.51(19) . . ? C18 N110 Ni1 122.55(15) . . ? C111 N110 Ni1 118.81(14) . . ? C112 C111 C116 119.2(2) . . ? C112 C111 N110 118.1(2) . . ? C116 C111 N110 122.6(2) . . ? C113 C112 C111 120.5(2) . . ? C113 C112 H112 119.8 . . ? C111 C112 H112 119.8 . . ? C114 C113 C112 120.5(2) . . ? C114 C113 H113 119.7 . . ? C112 C113 H113 119.7 . . ? C113 C114 C115 119.4(2) . . ? C113 C114 H114 120.3 . . ? C115 C114 H114 120.3 . . ? C114 C115 C116 120.6(2) . . ? C114 C115 H115 119.7 . . ? C116 C115 H115 119.7 . . ? C111 C116 C115 119.8(2) . . ? C111 C116 H116 120.1 . . ? C115 C116 H116 120.1 . . ? C22 N21 C25 110.48(19) . . ? C22 N21 C26 126.18(19) . . ? C25 N21 C26 123.3(2) . . ? N21 C22 N23 104.74(19) . . ? N21 C22 Ni1 135.25(17) . . ? N23 C22 Ni1 119.81(16) . . ? C22 N23 C24 111.40(19) . . ? C22 N23 C27 120.37(18) . . ? C24 N23 C27 127.91(19) . . ? C25 C24 N23 105.8(2) . . ? C25 C24 H24 127.1 . . ? N23 C24 H24 127.1 . . ? C24 C25 N21 107.6(2) . . ? C24 C25 H25 126.2 . . ? N21 C25 H25 126.2 . . ? N21 C26 H26A 109.5 . . ? N21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N23 C27 C28 110.16(19) . . ? N23 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? N23 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? O29 C28 N210 127.7(2) . . ? O29 C28 C27 117.0(2) . . ? N210 C28 C27 115.22(19) . . ? C28 N210 C211 119.53(19) . . ? C28 N210 Ni1 122.22(16) . . ? C211 N210 Ni1 117.88(15) . . ? C212 C211 C216 118.3(2) . . ? C212 C211 N210 117.1(2) . . ? C216 C211 N210 124.6(2) . . ? C213 C212 C211 121.1(2) . . ? C213 C212 H212 119.4 . . ? C211 C212 H212 119.4 . . ? C214 C213 C212 119.9(3) . . ? C214 C213 H213 120.0 . . ? C212 C213 H213 120.0 . . ? C215 C214 C213 119.6(3) . . ? C215 C214 H214 120.2 . . ? C213 C214 H214 120.2 . . ? C214 C215 C216 120.8(3) . . ? C214 C215 H215 119.6 . . ? C216 C215 H215 119.6 . . ? C215 C216 C211 120.3(2) . . ? C215 C216 H216 119.9 . . ? C211 C216 H216 119.9 . . ? C32 Ni2 C42 89.92(9) . . ? C32 Ni2 N310 88.14(9) . . ? C42 Ni2 N310 175.05(9) . . ? C32 Ni2 N410 177.65(9) . . ? C42 Ni2 N410 87.87(8) . . ? N310 Ni2 N410 94.12(8) . . ? C32 N31 C35 110.3(2) . . ? C32 N31 C36 125.6(2) . . ? C35 N31 C36 124.0(2) . . ? N33 C32 N31 104.98(19) . . ? N33 C32 Ni2 120.04(17) . . ? N31 C32 Ni2 134.86(18) . . ? C32 N33 C34 111.1(2) . . ? C32 N33 C37 121.65(19) . . ? C34 N33 C37 127.2(2) . . ? C35 C34 N33 106.5(2) . . ? C35 C34 H34 126.7 . . ? N33 C34 H34 126.7 . . ? C34 C35 N31 107.1(2) . . ? C34 C35 H35 126.5 . . ? N31 C35 H35 126.5 . . ? N31 C36 H36A 109.5 . . ? N31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N33 C37 C38 112.06(19) . . ? N33 C37 H37A 109.2 . . ? C38 C37 H37A 109.2 . . ? N33 C37 H37B 109.2 . . ? C38 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? O39 C38 N310 127.9(2) . . ? O39 C38 C37 116.1(2) . . ? N310 C38 C37 115.9(2) . . ? C38 N310 C311 118.56(18) . . ? C38 N310 Ni2 122.44(15) . . ? C311 N310 Ni2 118.88(14) . . ? C312 C311 C316 119.1(2) . . ? C312 C311 N310 118.0(2) . . ? C316 C311 N310 122.8(2) . . ? C311 C312 C313 120.3(2) . . ? C311 C312 H312 119.9 . . ? C313 C312 H312 119.9 . . ? C314 C313 C312 120.7(2) . . ? C314 C313 H313 119.7 . . ? C312 C313 H313 119.7 . . ? C313 C314 C315 119.0(2) . . ? C313 C314 H314 120.5 . . ? C315 C314 H314 120.5 . . ? C316 C315 C314 120.6(3) . . ? C316 C315 H315 119.7 . . ? C314 C315 H315 119.7 . . ? C315 C316 C311 120.3(2) . . ? C315 C316 H316 119.9 . . ? C311 C316 H316 119.9 . . ? C42 N41 C45 110.55(19) . . ? C42 N41 C46 125.45(19) . . ? C45 N41 C46 123.92(19) . . ? N43 C42 N41 104.47(19) . . ? N43 C42 Ni2 121.11(16) . . ? N41 C42 Ni2 134.39(17) . . ? C42 N43 C44 111.63(19) . . ? C42 N43 C47 120.31(19) . . ? C44 N43 C47 127.73(19) . . ? C45 C44 N43 105.9(2) . . ? C45 C44 H44 127.1 . . ? N43 C44 H44 127.1 . . ? C44 C45 N41 107.5(2) . . ? C44 C45 H45 126.3 . . ? N41 C45 H45 126.3 . . ? N41 C46 H46A 109.5 . . ? N41 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N41 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N43 C47 C48 110.16(19) . . ? N43 C47 H47A 109.6 . . ? C48 C47 H47A 109.6 . . ? N43 C47 H47B 109.6 . . ? C48 C47 H47B 109.6 . . ? H47A C47 H47B 108.1 . . ? O49 C48 N410 128.1(2) . . ? O49 C48 C47 116.6(2) . . ? N410 C48 C47 115.20(19) . . ? C48 N410 C411 118.85(19) . . ? C48 N410 Ni2 122.86(16) . . ? C411 N410 Ni2 118.22(14) . . ? C412 C411 C416 118.1(2) . . ? C412 C411 N410 118.5(2) . . ? C416 C411 N410 123.3(2) . . ? C413 C412 C411 121.1(2) . . ? C413 C412 H412 119.5 . . ? C411 C412 H412 119.5 . . ? C412 C413 C414 120.5(3) . . ? C412 C413 H413 119.8 . . ? C414 C413 H413 119.8 . . ? C415 C414 C413 119.0(3) . . ? C415 C414 H414 120.5 . . ? C413 C414 H414 120.5 . . ? C414 C415 C416 121.3(3) . . ? C414 C415 H415 119.3 . . ? C416 C415 H415 119.3 . . ? C415 C416 C411 120.0(2) . . ? C415 C416 H416 120.0 . . ? C411 C416 H416 120.0 . . ? C5 O5 H5O 100.6 . . ? O5 C5 H5A 109.5 . . ? O5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O5 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 O6 H6O 111.7 . . ? O6 C6 H6A 109.5 . . ? O6 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O6 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C7 O7 H7O 109.9 . . ? O7 C7 H7A 109.5 . . ? O7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C8 O8 H8O 102.9 . . ? O8 C8 H8A 109.5 . . ? O8 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O8 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? H9A O9 H9B 101.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 N11 C12 N13 -0.1(2) . . . . ? C16 N11 C12 N13 175.8(2) . . . . ? C15 N11 C12 Ni1 177.68(18) . . . . ? C16 N11 C12 Ni1 -6.4(4) . . . . ? C22 Ni1 C12 N13 131.73(19) . . . . ? N110 Ni1 C12 N13 -43.82(18) . . . . ? C22 Ni1 C12 N11 -45.7(2) . . . . ? N110 Ni1 C12 N11 138.7(2) . . . . ? N11 C12 N13 C14 0.3(3) . . . . ? Ni1 C12 N13 C14 -177.86(16) . . . . ? N11 C12 N13 C17 -176.46(19) . . . . ? Ni1 C12 N13 C17 5.4(3) . . . . ? C12 N13 C14 C15 -0.4(3) . . . . ? C17 N13 C14 C15 176.2(2) . . . . ? N13 C14 C15 N11 0.3(3) . . . . ? C12 N11 C15 C14 -0.2(3) . . . . ? C16 N11 C15 C14 -176.1(2) . . . . ? C12 N13 C17 C18 47.6(3) . . . . ? C14 N13 C17 C18 -128.6(2) . . . . ? N13 C17 C18 O19 136.2(2) . . . . ? N13 C17 C18 N110 -44.4(3) . . . . ? O19 C18 N110 C111 -4.1(4) . . . . ? C17 C18 N110 C111 176.6(2) . . . . ? O19 C18 N110 Ni1 171.67(19) . . . . ? C17 C18 N110 Ni1 -7.6(3) . . . . ? C12 Ni1 N110 C18 45.85(19) . . . . ? N210 Ni1 N110 C18 -135.16(19) . . . . ? C12 Ni1 N110 C111 -138.42(17) . . . . ? N210 Ni1 N110 C111 40.57(17) . . . . ? C18 N110 C111 C112 -132.0(2) . . . . ? Ni1 N110 C111 C112 52.1(2) . . . . ? C18 N110 C111 C116 50.7(3) . . . . ? Ni1 N110 C111 C116 -125.2(2) . . . . ? C116 C111 C112 C113 0.0(3) . . . . ? N110 C111 C112 C113 -177.4(2) . . . . ? C111 C112 C113 C114 0.4(3) . . . . ? C112 C113 C114 C115 -0.5(4) . . . . ? C113 C114 C115 C116 0.2(4) . . . . ? C112 C111 C116 C115 -0.3(3) . . . . ? N110 C111 C116 C115 177.0(2) . . . . ? C114 C115 C116 C111 0.2(4) . . . . ? C25 N21 C22 N23 1.5(3) . . . . ? C26 N21 C22 N23 180.0(2) . . . . ? C25 N21 C22 Ni1 -173.16(19) . . . . ? C26 N21 C22 Ni1 5.3(4) . . . . ? C12 Ni1 C22 N21 -49.8(2) . . . . ? N210 Ni1 C22 N21 131.3(2) . . . . ? C12 Ni1 C22 N23 136.16(19) . . . . ? N210 Ni1 C22 N23 -42.76(18) . . . . ? N21 C22 N23 C24 -1.7(3) . . . . ? Ni1 C22 N23 C24 173.91(16) . . . . ? N21 C22 N23 C27 -175.79(19) . . . . ? Ni1 C22 N23 C27 -0.1(3) . . . . ? C22 N23 C24 C25 1.4(3) . . . . ? C27 N23 C24 C25 174.8(2) . . . . ? N23 C24 C25 N21 -0.4(3) . . . . ? C22 N21 C25 C24 -0.7(3) . . . . ? C26 N21 C25 C24 -179.3(2) . . . . ? C22 N23 C27 C28 55.8(3) . . . . ? C24 N23 C27 C28 -117.1(2) . . . . ? N23 C27 C28 O29 127.3(2) . . . . ? N23 C27 C28 N210 -49.7(3) . . . . ? O29 C28 N210 C211 -10.8(3) . . . . ? C27 C28 N210 C211 165.86(19) . . . . ? O29 C28 N210 Ni1 176.20(18) . . . . ? C27 C28 N210 Ni1 -7.1(3) . . . . ? C22 Ni1 N210 C28 47.56(18) . . . . ? N110 Ni1 N210 C28 -136.88(17) . . . . ? C22 Ni1 N210 C211 -125.53(16) . . . . ? N110 Ni1 N210 C211 50.03(16) . . . . ? C28 N210 C211 C212 -141.1(2) . . . . ? Ni1 N210 C211 C212 32.2(2) . . . . ? C28 N210 C211 C216 37.9(3) . . . . ? Ni1 N210 C211 C216 -148.78(19) . . . . ? C216 C211 C212 C213 -1.7(3) . . . . ? N210 C211 C212 C213 177.4(2) . . . . ? C211 C212 C213 C214 -0.1(4) . . . . ? C212 C213 C214 C215 1.5(4) . . . . ? C213 C214 C215 C216 -1.0(4) . . . . ? C214 C215 C216 C211 -0.8(4) . . . . ? C212 C211 C216 C215 2.2(3) . . . . ? N210 C211 C216 C215 -176.8(2) . . . . ? C35 N31 C32 N33 -0.4(2) . . . . ? C36 N31 C32 N33 175.6(2) . . . . ? C35 N31 C32 Ni2 175.40(18) . . . . ? C36 N31 C32 Ni2 -8.6(4) . . . . ? C42 Ni2 C32 N33 129.08(18) . . . . ? N310 Ni2 C32 N33 -46.37(17) . . . . ? C42 Ni2 C32 N31 -46.2(2) . . . . ? N310 Ni2 C32 N31 138.3(2) . . . . ? N31 C32 N33 C34 0.6(2) . . . . ? Ni2 C32 N33 C34 -175.92(15) . . . . ? N31 C32 N33 C37 -176.09(19) . . . . ? Ni2 C32 N33 C37 7.3(3) . . . . ? C32 N33 C34 C35 -0.6(3) . . . . ? C37 N33 C34 C35 175.9(2) . . . . ? N33 C34 C35 N31 0.4(3) . . . . ? C32 N31 C35 C34 0.0(3) . . . . ? C36 N31 C35 C34 -176.0(2) . . . . ? C32 N33 C37 C38 46.8(3) . . . . ? C34 N33 C37 C38 -129.4(2) . . . . ? N33 C37 C38 O39 136.5(2) . . . . ? N33 C37 C38 N310 -43.5(3) . . . . ? O39 C38 N310 C311 -5.9(4) . . . . ? C37 C38 N310 C311 174.1(2) . . . . ? O39 C38 N310 Ni2 170.1(2) . . . . ? C37 C38 N310 Ni2 -10.0(3) . . . . ? C32 Ni2 N310 C38 48.72(19) . . . . ? N410 Ni2 N310 C38 -131.90(19) . . . . ? C32 Ni2 N310 C311 -135.36(17) . . . . ? N410 Ni2 N310 C311 44.03(17) . . . . ? C38 N310 C311 C312 -134.7(2) . . . . ? Ni2 N310 C311 C312 49.3(2) . . . . ? C38 N310 C311 C316 48.1(3) . . . . ? Ni2 N310 C311 C316 -128.0(2) . . . . ? C316 C311 C312 C313 0.4(3) . . . . ? N310 C311 C312 C313 -176.9(2) . . . . ? C311 C312 C313 C314 0.4(3) . . . . ? C312 C313 C314 C315 -0.9(4) . . . . ? C313 C314 C315 C316 0.5(4) . . . . ? C314 C315 C316 C311 0.4(4) . . . . ? C312 C311 C316 C315 -0.8(4) . . . . ? N310 C311 C316 C315 176.4(2) . . . . ? C45 N41 C42 N43 0.5(2) . . . . ? C46 N41 C42 N43 177.4(2) . . . . ? C45 N41 C42 Ni2 -177.21(19) . . . . ? C46 N41 C42 Ni2 -0.4(4) . . . . ? C32 Ni2 C42 N43 135.23(19) . . . . ? N410 Ni2 C42 N43 -43.98(19) . . . . ? C32 Ni2 C42 N41 -47.4(2) . . . . ? N410 Ni2 C42 N41 133.4(2) . . . . ? N41 C42 N43 C44 -0.5(3) . . . . ? Ni2 C42 N43 C44 177.55(16) . . . . ? N41 C42 N43 C47 -174.47(19) . . . . ? Ni2 C42 N43 C47 3.6(3) . . . . ? C42 N43 C44 C45 0.4(3) . . . . ? C47 N43 C44 C45 173.7(2) . . . . ? N43 C44 C45 N41 0.0(3) . . . . ? C42 N41 C45 C44 -0.3(3) . . . . ? C46 N41 C45 C44 -177.2(2) . . . . ? C42 N43 C47 C48 53.1(3) . . . . ? C44 N43 C47 C48 -119.7(2) . . . . ? N43 C47 C48 O49 127.3(2) . . . . ? N43 C47 C48 N410 -51.4(3) . . . . ? O49 C48 N410 C411 -4.2(4) . . . . ? C47 C48 N410 C411 174.31(19) . . . . ? O49 C48 N410 Ni2 178.90(19) . . . . ? C47 C48 N410 Ni2 -2.6(3) . . . . ? C42 Ni2 N410 C48 44.04(18) . . . . ? N310 Ni2 N410 C48 -140.49(18) . . . . ? C42 Ni2 N410 C411 -132.88(17) . . . . ? N310 Ni2 N410 C411 42.59(16) . . . . ? C48 N410 C411 C412 -140.6(2) . . . . ? Ni2 N410 C411 C412 36.4(3) . . . . ? C48 N410 C411 C416 42.8(3) . . . . ? Ni2 N410 C411 C416 -140.15(19) . . . . ? C416 C411 C412 C413 1.4(3) . . . . ? N410 C411 C412 C413 -175.4(2) . . . . ? C411 C412 C413 C414 -0.9(4) . . . . ? C412 C413 C414 C415 -0.4(4) . . . . ? C413 C414 C415 C416 1.0(4) . . . . ? C414 C415 C416 C411 -0.5(4) . . . . ? C412 C411 C416 C415 -0.7(4) . . . . ? N410 C411 C416 C415 175.9(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5O O19 0.96 1.80 2.740(2) 168 . O6 H6O O29 0.93 1.75 2.675(2) 173 . O7 H7O O49 0.89 1.86 2.731(3) 166 . O8 H8O O19 1.05 1.70 2.737(3) 169 . O9 H9A O8 1.02 1.98 2.934(3) 154 . O9 H9B O39 0.96 1.84 2.797(3) 175 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.904 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.068 #===END data_s4111a _database_code_depnum_ccdc_archive 'CCDC 723718' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H36 N6 Ni O2' _chemical_formula_sum 'C44 H36 N6 Ni O2' _chemical_formula_weight 739.50 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3697(2) _cell_length_b 16.9361(4) _cell_length_c 24.0007(6) _cell_angle_alpha 90.00 _cell_angle_beta 115.0097(13) _cell_angle_gamma 90.00 _cell_volume 4188.20(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 142439 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 0.504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 33596 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.27 _reflns_number_total 7579 _reflns_number_gt 4857 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement HKL2000 _computing_data_reduction 'HKL2000, Sortav' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0909P)^2^+0.8668P] 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 7579 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1601 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.53848(4) 0.39056(2) 0.19934(2) 0.04265(18) Uani 1 1 d . . . N11 N 0.4018(3) 0.45767(15) 0.27015(13) 0.0421(7) Uani 1 1 d . . . C12 C 0.4856(4) 0.40805(19) 0.26143(17) 0.0471(10) Uani 1 1 d . . . N13 N 0.5425(3) 0.36586(18) 0.31419(13) 0.0498(8) Uani 1 1 d . . . C14 C 0.4982(4) 0.3894(2) 0.35727(16) 0.0464(9) Uani 1 1 d . . . C15 C 0.4068(4) 0.4479(2) 0.32894(17) 0.0477(9) Uani 1 1 d . . . C16 C 0.3156(3) 0.51176(19) 0.22373(17) 0.0475(9) Uani 1 1 d . . . H16A H 0.3420 0.5144 0.1894 0.057 Uiso 1 1 calc R . . H16B H 0.3261 0.5652 0.2419 0.057 Uiso 1 1 calc R . . C17 C 0.6238(4) 0.2970(2) 0.31727(17) 0.0548(10) Uani 1 1 d . . . H17A H 0.6406 0.2666 0.3551 0.066 Uiso 1 1 calc R . . H17B H 0.7083 0.3152 0.3194 0.066 Uiso 1 1 calc R . . C18 C 0.5593(4) 0.2444(2) 0.26217(17) 0.0512(10) Uani 1 1 d . . . O19 O 0.5620(3) 0.17132(15) 0.27144(12) 0.0617(7) Uani 1 1 d . . . N110 N 0.5036(3) 0.28089(16) 0.20735(13) 0.0455(7) Uani 1 1 d . . . C111 C 0.4313(4) 0.2370(2) 0.15381(17) 0.0493(9) Uani 1 1 d . . . C112 C 0.4689(4) 0.1645(2) 0.13950(18) 0.0560(10) Uani 1 1 d . . . H112 H 0.5483 0.1416 0.1673 0.067 Uiso 1 1 calc R . . C113 C 0.3948(4) 0.1257(2) 0.08658(19) 0.0592(11) Uani 1 1 d . . . H113 H 0.4223 0.0758 0.0784 0.071 Uiso 1 1 calc R . . C114 C 0.2835(5) 0.1570(3) 0.0459(2) 0.0801(15) Uani 1 1 d . . . H114 H 0.2324 0.1291 0.0092 0.096 Uiso 1 1 calc R . . C115 C 0.2425(5) 0.2301(3) 0.0572(2) 0.1001(19) Uani 1 1 d . . . H115 H 0.1640 0.2528 0.0282 0.120 Uiso 1 1 calc R . . C116 C 0.3178(4) 0.2695(3) 0.1114(2) 0.0700(13) Uani 1 1 d . . . H116 H 0.2906 0.3197 0.1194 0.084 Uiso 1 1 calc R . . C117 C 0.1739(3) 0.4890(2) 0.19824(16) 0.0437(9) Uani 1 1 d . . . C118 C 0.1345(4) 0.4107(2) 0.18682(17) 0.0510(10) Uani 1 1 d . . . H118 H 0.1975 0.3699 0.1971 0.061 Uiso 1 1 calc R . . C119 C 0.0022(4) 0.3917(3) 0.1602(2) 0.0656(12) Uani 1 1 d . . . H119 H -0.0243 0.3381 0.1525 0.079 Uiso 1 1 calc R . . C120 C -0.0885(5) 0.4501(3) 0.1452(2) 0.0832(15) Uani 1 1 d . . . H120 H -0.1783 0.4374 0.1265 0.100 Uiso 1 1 calc R . . C121 C -0.0489(5) 0.5283(3) 0.1574(2) 0.0814(14) Uani 1 1 d . . . H121 H -0.1120 0.5691 0.1475 0.098 Uiso 1 1 calc R . . C122 C 0.0810(4) 0.5472(2) 0.18379(18) 0.0572(10) Uani 1 1 d . . . H122 H 0.1069 0.6008 0.1921 0.069 Uiso 1 1 calc R . . C123 C 0.3412(4) 0.4844(2) 0.3590(2) 0.0610(11) Uani 1 1 d . . . H123 H 0.2770 0.5234 0.3392 0.073 Uiso 1 1 calc R . . C124 C 0.3726(5) 0.4620(3) 0.4182(2) 0.0697(13) Uani 1 1 d . . . H124 H 0.3289 0.4858 0.4400 0.084 Uiso 1 1 calc R . . C125 C 0.4685(5) 0.4044(3) 0.4480(2) 0.0686(13) Uani 1 1 d . . . H125 H 0.4902 0.3915 0.4897 0.082 Uiso 1 1 calc R . . C126 C 0.5303(4) 0.3669(3) 0.41787(19) 0.0617(11) Uani 1 1 d . . . H126 H 0.5929 0.3269 0.4373 0.074 Uiso 1 1 calc R . . N21 N 0.6549(3) 0.55086(16) 0.23681(13) 0.0444(7) Uani 1 1 d . . . C22 C 0.5808(3) 0.4964(2) 0.19399(16) 0.0432(8) Uani 1 1 d . . . N23 N 0.5525(3) 0.52879(15) 0.13868(12) 0.0397(7) Uani 1 1 d . . . C24 C 0.6127(3) 0.60194(18) 0.14391(17) 0.0435(9) Uani 1 1 d . . . C25 C 0.6768(3) 0.61650(19) 0.20714(17) 0.0447(9) Uani 1 1 d . . . C26 C 0.7062(4) 0.5426(2) 0.30305(16) 0.0492(9) Uani 1 1 d . . . H26A H 0.6379 0.5204 0.3138 0.059 Uiso 1 1 calc R . . H26B H 0.7292 0.5955 0.3222 0.059 Uiso 1 1 calc R . . C27 C 0.4849(3) 0.48258(19) 0.08272(16) 0.0461(9) Uani 1 1 d . . . H27A H 0.4743 0.5148 0.0465 0.055 Uiso 1 1 calc R . . H27B H 0.3975 0.4681 0.0789 0.055 Uiso 1 1 calc R . . C28 C 0.5611(3) 0.4077(2) 0.08418(16) 0.0421(8) Uani 1 1 d . . . O29 O 0.5829(3) 0.39361(14) 0.03876(12) 0.0529(7) Uani 1 1 d . . . N210 N 0.5997(3) 0.36667(16) 0.13650(12) 0.0404(7) Uani 1 1 d . . . C211 C 0.6873(3) 0.3020(2) 0.14608(17) 0.0445(9) Uani 1 1 d . . . C212 C 0.6800(4) 0.2485(2) 0.1008(2) 0.0588(11) Uani 1 1 d . . . H212 H 0.6137 0.2542 0.0603 0.071 Uiso 1 1 calc R . . C213 C 0.7677(5) 0.1875(2) 0.1139(2) 0.0680(12) Uani 1 1 d . . . H213 H 0.7624 0.1521 0.0822 0.082 Uiso 1 1 calc R . . C214 C 0.8625(5) 0.1772(3) 0.1723(3) 0.0770(14) Uani 1 1 d . . . H214 H 0.9222 0.1348 0.1810 0.092 Uiso 1 1 calc R . . C215 C 0.8713(4) 0.2289(2) 0.2189(2) 0.0655(12) Uani 1 1 d . . . H215 H 0.9372 0.2226 0.2594 0.079 Uiso 1 1 calc R . . C216 C 0.7817(4) 0.2902(2) 0.20494(19) 0.0537(10) Uani 1 1 d . . . H216 H 0.7856 0.3248 0.2368 0.064 Uiso 1 1 calc R . . C217 C 0.8231(4) 0.4906(3) 0.32898(18) 0.0641(12) Uani 1 1 d . . . C218 C 0.9003(4) 0.4732(2) 0.29984(19) 0.0567(10) Uani 1 1 d . . . H218 H 0.8794 0.4959 0.2606 0.068 Uiso 1 1 calc R . . C219 C 1.0072(4) 0.4244(3) 0.3246(2) 0.0846(15) Uani 1 1 d . . . H219 H 1.0600 0.4153 0.3033 0.101 Uiso 1 1 calc R . . C220 C 1.0358(6) 0.3894(4) 0.3802(3) 0.1007(19) Uani 1 1 d . . . H220 H 1.1076 0.3544 0.3974 0.121 Uiso 1 1 calc R . . C221 C 0.9599(6) 0.4050(5) 0.4114(3) 0.125(3) Uani 1 1 d . . . H221 H 0.9799 0.3808 0.4501 0.149 Uiso 1 1 calc R . . C222 C 0.8538(5) 0.4564(4) 0.3859(2) 0.1005(19) Uani 1 1 d . . . H222 H 0.8027 0.4678 0.4077 0.121 Uiso 1 1 calc R . . C223 C 0.7489(4) 0.6846(2) 0.22967(19) 0.0576(11) Uani 1 1 d . . . H223 H 0.7922 0.6948 0.2725 0.069 Uiso 1 1 calc R . . C224 C 0.7550(4) 0.7368(2) 0.1871(2) 0.0622(12) Uani 1 1 d . . . H224 H 0.8035 0.7841 0.2008 0.075 Uiso 1 1 calc R . . C225 C 0.6910(4) 0.7217(2) 0.1235(2) 0.0574(11) Uani 1 1 d . . . H225 H 0.6983 0.7590 0.0956 0.069 Uiso 1 1 calc R . . C226 C 0.6176(4) 0.6540(2) 0.10039(18) 0.0531(10) Uani 1 1 d . . . H226 H 0.5735 0.6440 0.0575 0.064 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 0.0420(3) 0.0323(3) 0.0441(3) 0.00444(19) 0.0090(2) -0.00009(19) N11 0.0324(16) 0.0302(14) 0.0530(19) -0.0003(13) 0.0078(13) 0.0000(12) C12 0.042(2) 0.0329(19) 0.053(2) 0.0028(16) 0.0064(17) -0.0066(16) N13 0.055(2) 0.0417(17) 0.0425(18) 0.0044(14) 0.0104(15) 0.0025(15) C14 0.047(2) 0.047(2) 0.038(2) -0.0031(17) 0.0111(17) -0.0099(18) C15 0.050(2) 0.043(2) 0.044(2) -0.0064(17) 0.0143(18) -0.0126(17) C16 0.041(2) 0.0286(17) 0.064(2) -0.0011(16) 0.0131(18) -0.0053(15) C17 0.064(3) 0.050(2) 0.044(2) 0.0125(18) 0.0158(19) 0.0127(19) C18 0.050(2) 0.046(2) 0.059(2) 0.0169(19) 0.0240(19) 0.0168(18) O19 0.079(2) 0.0396(15) 0.0678(18) 0.0156(13) 0.0326(15) 0.0146(13) N110 0.0481(18) 0.0344(15) 0.0462(17) 0.0034(14) 0.0123(14) 0.0011(13) C111 0.048(2) 0.038(2) 0.059(2) 0.0028(17) 0.0194(19) -0.0022(17) C112 0.067(3) 0.038(2) 0.060(2) -0.0012(18) 0.023(2) 0.0005(18) C113 0.064(3) 0.053(2) 0.060(3) -0.006(2) 0.026(2) -0.001(2) C114 0.063(3) 0.074(3) 0.082(3) -0.039(3) 0.010(3) -0.013(2) C115 0.059(3) 0.111(4) 0.085(4) -0.035(3) -0.013(3) 0.022(3) C116 0.047(2) 0.060(3) 0.078(3) -0.022(2) 0.002(2) 0.009(2) C117 0.043(2) 0.0368(18) 0.046(2) -0.0018(16) 0.0135(17) -0.0039(16) C118 0.053(2) 0.047(2) 0.051(2) -0.0030(17) 0.0198(19) -0.0106(17) C119 0.062(3) 0.066(3) 0.061(3) -0.001(2) 0.018(2) -0.023(2) C120 0.045(3) 0.110(4) 0.078(3) 0.012(3) 0.011(2) -0.022(3) C121 0.053(3) 0.090(4) 0.096(4) 0.014(3) 0.026(3) 0.018(3) C122 0.053(2) 0.051(2) 0.062(2) -0.0001(19) 0.018(2) 0.0059(19) C123 0.066(3) 0.051(2) 0.063(3) -0.013(2) 0.026(2) -0.010(2) C124 0.088(3) 0.064(3) 0.065(3) -0.024(2) 0.040(3) -0.024(3) C125 0.088(3) 0.066(3) 0.053(3) -0.017(2) 0.031(3) -0.026(3) C126 0.067(3) 0.056(2) 0.051(2) -0.001(2) 0.014(2) -0.019(2) N21 0.0365(16) 0.0399(16) 0.0471(17) -0.0033(13) 0.0082(13) -0.0012(13) C22 0.0369(19) 0.0362(18) 0.050(2) -0.0022(17) 0.0115(16) -0.0014(15) N23 0.0380(16) 0.0305(14) 0.0393(16) 0.0004(12) 0.0054(13) -0.0024(12) C24 0.0344(19) 0.0273(17) 0.056(2) -0.0006(16) 0.0063(16) -0.0002(14) C25 0.0372(19) 0.0354(19) 0.055(2) 0.0060(16) 0.0128(17) 0.0016(15) C26 0.044(2) 0.053(2) 0.046(2) -0.0064(17) 0.0146(17) -0.0050(17) C27 0.044(2) 0.0377(19) 0.044(2) 0.0036(16) 0.0067(16) -0.0011(16) C28 0.040(2) 0.043(2) 0.033(2) -0.0035(16) 0.0054(16) -0.0066(15) O29 0.0584(17) 0.0467(15) 0.0455(15) 0.0052(12) 0.0141(13) 0.0050(12) N210 0.0370(16) 0.0340(14) 0.0394(16) 0.0048(13) 0.0057(13) 0.0002(12) C211 0.0353(19) 0.0358(19) 0.055(2) 0.0075(17) 0.0118(17) -0.0006(15) C212 0.057(3) 0.043(2) 0.069(3) 0.003(2) 0.021(2) 0.0057(19) C213 0.074(3) 0.041(2) 0.095(3) -0.002(2) 0.041(3) 0.005(2) C214 0.060(3) 0.046(3) 0.125(4) 0.027(3) 0.038(3) 0.018(2) C215 0.046(2) 0.047(2) 0.088(3) 0.023(2) 0.013(2) 0.0040(19) C216 0.042(2) 0.040(2) 0.068(3) 0.0078(19) 0.0131(19) -0.0033(17) C217 0.043(2) 0.089(3) 0.048(2) 0.006(2) 0.0074(19) 0.001(2) C218 0.048(2) 0.061(2) 0.053(2) 0.004(2) 0.015(2) -0.001(2) C219 0.046(3) 0.124(4) 0.069(3) -0.001(3) 0.010(2) 0.011(3) C220 0.068(4) 0.134(5) 0.076(4) 0.023(3) 0.007(3) 0.030(3) C221 0.074(4) 0.194(7) 0.089(4) 0.061(4) 0.018(3) 0.039(4) C222 0.061(3) 0.174(6) 0.051(3) 0.023(3) 0.009(2) 0.020(3) C223 0.046(2) 0.049(2) 0.060(2) -0.006(2) 0.0051(19) -0.0061(18) C224 0.046(2) 0.038(2) 0.089(3) -0.001(2) 0.016(2) -0.0066(17) C225 0.048(2) 0.040(2) 0.073(3) 0.0144(19) 0.015(2) 0.0000(17) C226 0.049(2) 0.034(2) 0.062(2) 0.0112(18) 0.0097(19) 0.0034(17) _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 C12 1.852(4) . ? Ni1 C22 1.875(3) . ? Ni1 N110 1.926(3) . ? Ni1 N210 1.952(3) . ? N11 C12 1.351(5) . ? N11 C15 1.398(5) . ? N11 C16 1.455(4) . ? C12 N13 1.357(4) . ? N13 C14 1.387(5) . ? N13 C17 1.470(5) . ? C14 C15 1.387(5) . ? C14 C126 1.395(5) . ? C15 C123 1.382(5) . ? C16 C117 1.511(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.504(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O19 1.256(4) . ? C18 N110 1.345(4) . ? N110 C111 1.409(4) . ? C111 C116 1.376(5) . ? C111 C112 1.390(5) . ? C112 C113 1.361(5) . ? C112 H112 0.9500 . ? C113 C114 1.338(6) . ? C113 H113 0.9500 . ? C114 C115 1.389(7) . ? C114 H114 0.9500 . ? C115 C116 1.390(6) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C117 C122 1.377(5) . ? C117 C118 1.390(5) . ? C118 C119 1.400(6) . ? C118 H118 0.9500 . ? C119 C120 1.364(7) . ? C119 H119 0.9500 . ? C120 C121 1.390(7) . ? C120 H120 0.9500 . ? C121 C122 1.376(6) . ? C121 H121 0.9500 . ? C122 H122 0.9500 . ? C123 C124 1.366(6) . ? C123 H123 0.9500 . ? C124 C125 1.412(7) . ? C124 H124 0.9500 . ? C125 C126 1.359(6) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? N21 C22 1.372(4) . ? N21 C25 1.398(4) . ? N21 C26 1.450(4) . ? C22 N23 1.343(4) . ? N23 C24 1.395(4) . ? N23 C27 1.461(4) . ? C24 C226 1.385(5) . ? C24 C25 1.400(5) . ? C25 C223 1.386(5) . ? C26 C217 1.493(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.527(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O29 1.239(4) . ? C28 N210 1.337(4) . ? N210 C211 1.432(4) . ? C211 C216 1.380(5) . ? C211 C212 1.390(5) . ? C212 C213 1.377(6) . ? C212 H212 0.9500 . ? C213 C214 1.371(6) . ? C213 H213 0.9500 . ? C214 C215 1.389(6) . ? C214 H214 0.9500 . ? C215 C216 1.392(5) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C217 C218 1.366(6) . ? C217 C222 1.386(6) . ? C218 C219 1.379(6) . ? C218 H218 0.9500 . ? C219 C220 1.369(7) . ? C219 H219 0.9500 . ? C220 C221 1.386(8) . ? C220 H220 0.9500 . ? C221 C222 1.402(8) . ? C221 H221 0.9500 . ? C222 H222 0.9500 . ? C223 C224 1.375(6) . ? C223 H223 0.9500 . ? C224 C225 1.407(6) . ? C224 H224 0.9500 . ? C225 C226 1.389(5) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Ni1 C22 94.71(15) . . ? C12 Ni1 N110 85.60(14) . . ? C22 Ni1 N110 177.27(14) . . ? C12 Ni1 N210 176.65(13) . . ? C22 Ni1 N210 87.69(14) . . ? N110 Ni1 N210 91.89(12) . . ? C12 N11 C15 110.6(3) . . ? C12 N11 C16 124.3(3) . . ? C15 N11 C16 125.0(3) . . ? N11 C12 N13 105.8(3) . . ? N11 C12 Ni1 135.6(3) . . ? N13 C12 Ni1 118.6(3) . . ? C12 N13 C14 111.3(3) . . ? C12 N13 C17 120.4(3) . . ? C14 N13 C17 127.6(3) . . ? N13 C14 C15 105.8(3) . . ? N13 C14 C126 132.9(4) . . ? C15 C14 C126 121.2(4) . . ? C123 C15 C14 121.4(4) . . ? C123 C15 N11 132.3(4) . . ? C14 C15 N11 106.4(3) . . ? N11 C16 C117 114.1(3) . . ? N11 C16 H16A 108.7 . . ? C117 C16 H16A 108.7 . . ? N11 C16 H16B 108.7 . . ? C117 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? N13 C17 C18 111.3(3) . . ? N13 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? N13 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? O19 C18 N110 126.3(4) . . ? O19 C18 C17 117.5(3) . . ? N110 C18 C17 116.2(3) . . ? C18 N110 C111 120.1(3) . . ? C18 N110 Ni1 120.6(2) . . ? C111 N110 Ni1 118.9(2) . . ? C116 C111 C112 117.5(4) . . ? C116 C111 N110 117.8(3) . . ? C112 C111 N110 124.7(3) . . ? C113 C112 C111 121.6(4) . . ? C113 C112 H112 119.2 . . ? C111 C112 H112 119.2 . . ? C114 C113 C112 120.8(4) . . ? C114 C113 H113 119.6 . . ? C112 C113 H113 119.6 . . ? C113 C114 C115 120.1(4) . . ? C113 C114 H114 119.9 . . ? C115 C114 H114 119.9 . . ? C114 C115 C116 119.1(4) . . ? C114 C115 H115 120.5 . . ? C116 C115 H115 120.5 . . ? C111 C116 C115 120.9(4) . . ? C111 C116 H116 119.5 . . ? C115 C116 H116 119.5 . . ? C122 C117 C118 118.9(3) . . ? C122 C117 C16 119.5(3) . . ? C118 C117 C16 121.5(3) . . ? C117 C118 C119 120.3(4) . . ? C117 C118 H118 119.9 . . ? C119 C118 H118 119.9 . . ? C120 C119 C118 120.1(4) . . ? C120 C119 H119 120.0 . . ? C118 C119 H119 120.0 . . ? C119 C120 C121 119.6(4) . . ? C119 C120 H120 120.2 . . ? C121 C120 H120 120.2 . . ? C122 C121 C120 120.5(4) . . ? C122 C121 H121 119.8 . . ? C120 C121 H121 119.8 . . ? C121 C122 C117 120.7(4) . . ? C121 C122 H122 119.7 . . ? C117 C122 H122 119.7 . . ? C124 C123 C15 117.2(4) . . ? C124 C123 H123 121.4 . . ? C15 C123 H123 121.4 . . ? C123 C124 C125 121.6(4) . . ? C123 C124 H124 119.2 . . ? C125 C124 H124 119.2 . . ? C126 C125 C124 121.1(4) . . ? C126 C125 H125 119.4 . . ? C124 C125 H125 119.4 . . ? C125 C126 C14 117.4(4) . . ? C125 C126 H126 121.3 . . ? C14 C126 H126 121.3 . . ? C22 N21 C25 109.7(3) . . ? C22 N21 C26 126.2(3) . . ? C25 N21 C26 124.0(3) . . ? N23 C22 N21 106.3(3) . . ? N23 C22 Ni1 119.8(2) . . ? N21 C22 Ni1 133.2(3) . . ? C22 N23 C24 111.7(3) . . ? C22 N23 C27 120.2(3) . . ? C24 N23 C27 127.3(3) . . ? C226 C24 N23 132.2(3) . . ? C226 C24 C25 122.5(3) . . ? N23 C24 C25 105.3(3) . . ? C223 C25 N21 131.8(3) . . ? C223 C25 C24 121.4(3) . . ? N21 C25 C24 106.8(3) . . ? N21 C26 C217 112.9(3) . . ? N21 C26 H26A 109.0 . . ? C217 C26 H26A 109.0 . . ? N21 C26 H26B 109.0 . . ? C217 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? N23 C27 C28 110.5(3) . . ? N23 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? N23 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? O29 C28 N210 128.1(3) . . ? O29 C28 C27 117.5(3) . . ? N210 C28 C27 114.3(3) . . ? C28 N210 C211 118.6(3) . . ? C28 N210 Ni1 122.3(2) . . ? C211 N210 Ni1 119.0(2) . . ? C216 C211 C212 118.0(3) . . ? C216 C211 N210 117.5(3) . . ? C212 C211 N210 124.4(3) . . ? C213 C212 C211 120.8(4) . . ? C213 C212 H212 119.6 . . ? C211 C212 H212 119.6 . . ? C214 C213 C212 120.6(4) . . ? C214 C213 H213 119.7 . . ? C212 C213 H213 119.7 . . ? C213 C214 C215 120.1(4) . . ? C213 C214 H214 120.0 . . ? C215 C214 H214 120.0 . . ? C214 C215 C216 118.6(4) . . ? C214 C215 H215 120.7 . . ? C216 C215 H215 120.7 . . ? C211 C216 C215 121.8(4) . . ? C211 C216 H216 119.1 . . ? C215 C216 H216 119.1 . . ? C218 C217 C222 117.8(4) . . ? C218 C217 C26 124.4(4) . . ? C222 C217 C26 117.8(4) . . ? C217 C218 C219 123.3(4) . . ? C217 C218 H218 118.3 . . ? C219 C218 H218 118.3 . . ? C220 C219 C218 118.8(5) . . ? C220 C219 H219 120.6 . . ? C218 C219 H219 120.6 . . ? C219 C220 C221 119.9(5) . . ? C219 C220 H220 120.0 . . ? C221 C220 H220 120.0 . . ? C220 C221 C222 120.0(5) . . ? C220 C221 H221 120.0 . . ? C222 C221 H221 120.0 . . ? C217 C222 C221 120.1(5) . . ? C217 C222 H222 119.9 . . ? C221 C222 H222 119.9 . . ? C224 C223 C25 116.9(4) . . ? C224 C223 H223 121.6 . . ? C25 C223 H223 121.6 . . ? C223 C224 C225 121.6(4) . . ? C223 C224 H224 119.2 . . ? C225 C224 H224 119.2 . . ? C226 C225 C224 122.1(4) . . ? C226 C225 H225 119.0 . . ? C224 C225 H225 119.0 . . ? C24 C226 C225 115.6(4) . . ? C24 C226 H226 122.2 . . ? C225 C226 H226 122.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 N11 C12 N13 0.9(4) . . . . ? C16 N11 C12 N13 -177.2(3) . . . . ? C15 N11 C12 Ni1 -176.2(3) . . . . ? C16 N11 C12 Ni1 5.7(5) . . . . ? C22 Ni1 C12 N11 52.5(4) . . . . ? N110 Ni1 C12 N11 -130.2(4) . . . . ? C22 Ni1 C12 N13 -124.3(3) . . . . ? N110 Ni1 C12 N13 53.0(3) . . . . ? N11 C12 N13 C14 -1.5(4) . . . . ? Ni1 C12 N13 C14 176.2(2) . . . . ? N11 C12 N13 C17 169.9(3) . . . . ? Ni1 C12 N13 C17 -12.4(4) . . . . ? C12 N13 C14 C15 1.5(4) . . . . ? C17 N13 C14 C15 -169.1(3) . . . . ? C12 N13 C14 C126 -177.0(4) . . . . ? C17 N13 C14 C126 12.3(6) . . . . ? N13 C14 C15 C123 179.3(3) . . . . ? C126 C14 C15 C123 -1.9(5) . . . . ? N13 C14 C15 N11 -0.9(4) . . . . ? C126 C14 C15 N11 177.9(3) . . . . ? C12 N11 C15 C123 179.8(4) . . . . ? C16 N11 C15 C123 -2.1(6) . . . . ? C12 N11 C15 C14 0.0(4) . . . . ? C16 N11 C15 C14 178.1(3) . . . . ? C12 N11 C16 C117 109.3(4) . . . . ? C15 N11 C16 C117 -68.5(4) . . . . ? C12 N13 C17 C18 -46.3(5) . . . . ? C14 N13 C17 C18 123.7(4) . . . . ? N13 C17 C18 O19 -135.7(4) . . . . ? N13 C17 C18 N110 44.2(5) . . . . ? O19 C18 N110 C111 5.3(6) . . . . ? C17 C18 N110 C111 -174.5(3) . . . . ? O19 C18 N110 Ni1 -167.2(3) . . . . ? C17 C18 N110 Ni1 13.0(5) . . . . ? C12 Ni1 N110 C18 -54.7(3) . . . . ? N210 Ni1 N110 C18 123.1(3) . . . . ? C12 Ni1 N110 C111 132.7(3) . . . . ? N210 Ni1 N110 C111 -49.5(3) . . . . ? C18 N110 C111 C116 139.2(4) . . . . ? Ni1 N110 C111 C116 -48.2(5) . . . . ? C18 N110 C111 C112 -43.5(6) . . . . ? Ni1 N110 C111 C112 129.1(3) . . . . ? C116 C111 C112 C113 -2.0(6) . . . . ? N110 C111 C112 C113 -179.4(4) . . . . ? C111 C112 C113 C114 1.1(7) . . . . ? C112 C113 C114 C115 0.3(8) . . . . ? C113 C114 C115 C116 -0.7(9) . . . . ? C112 C111 C116 C115 1.6(7) . . . . ? N110 C111 C116 C115 179.1(5) . . . . ? C114 C115 C116 C111 -0.3(9) . . . . ? N11 C16 C117 C122 143.5(4) . . . . ? N11 C16 C117 C118 -38.9(5) . . . . ? C122 C117 C118 C119 1.0(6) . . . . ? C16 C117 C118 C119 -176.6(4) . . . . ? C117 C118 C119 C120 0.1(6) . . . . ? C118 C119 C120 C121 -1.0(7) . . . . ? C119 C120 C121 C122 0.8(8) . . . . ? C120 C121 C122 C117 0.3(7) . . . . ? C118 C117 C122 C121 -1.2(6) . . . . ? C16 C117 C122 C121 176.5(4) . . . . ? C14 C15 C123 C124 1.7(5) . . . . ? N11 C15 C123 C124 -178.0(4) . . . . ? C15 C123 C124 C125 0.3(6) . . . . ? C123 C124 C125 C126 -2.3(6) . . . . ? C124 C125 C126 C14 2.0(6) . . . . ? N13 C14 C126 C125 178.4(4) . . . . ? C15 C14 C126 C125 0.0(5) . . . . ? C25 N21 C22 N23 -2.4(4) . . . . ? C26 N21 C22 N23 178.7(3) . . . . ? C25 N21 C22 Ni1 167.7(3) . . . . ? C26 N21 C22 Ni1 -11.2(6) . . . . ? C12 Ni1 C22 N23 -140.3(3) . . . . ? N210 Ni1 C22 N23 42.0(3) . . . . ? C12 Ni1 C22 N21 50.6(4) . . . . ? N210 Ni1 C22 N21 -127.1(4) . . . . ? N21 C22 N23 C24 3.4(4) . . . . ? Ni1 C22 N23 C24 -168.3(2) . . . . ? N21 C22 N23 C27 173.9(3) . . . . ? Ni1 C22 N23 C27 2.2(4) . . . . ? C22 N23 C24 C226 176.0(4) . . . . ? C27 N23 C24 C226 6.3(6) . . . . ? C22 N23 C24 C25 -3.1(4) . . . . ? C27 N23 C24 C25 -172.7(3) . . . . ? C22 N21 C25 C223 -177.1(4) . . . . ? C26 N21 C25 C223 1.8(6) . . . . ? C22 N21 C25 C24 0.6(4) . . . . ? C26 N21 C25 C24 179.5(3) . . . . ? C226 C24 C25 C223 0.2(6) . . . . ? N23 C24 C25 C223 179.4(3) . . . . ? C226 C24 C25 N21 -177.8(3) . . . . ? N23 C24 C25 N21 1.4(4) . . . . ? C22 N21 C26 C217 77.8(4) . . . . ? C25 N21 C26 C217 -100.9(4) . . . . ? C22 N23 C27 C28 -57.5(4) . . . . ? C24 N23 C27 C28 111.3(4) . . . . ? N23 C27 C28 O29 -129.4(3) . . . . ? N23 C27 C28 N210 48.5(4) . . . . ? O29 C28 N210 C211 6.5(5) . . . . ? C27 C28 N210 C211 -171.1(3) . . . . ? O29 C28 N210 Ni1 -172.4(3) . . . . ? C27 C28 N210 Ni1 10.0(4) . . . . ? C22 Ni1 N210 C28 -49.5(3) . . . . ? N110 Ni1 N210 C28 133.2(3) . . . . ? C22 Ni1 N210 C211 131.7(3) . . . . ? N110 Ni1 N210 C211 -45.6(2) . . . . ? C28 N210 C211 C216 142.8(3) . . . . ? Ni1 N210 C211 C216 -38.3(4) . . . . ? C28 N210 C211 C212 -40.2(5) . . . . ? Ni1 N210 C211 C212 138.7(3) . . . . ? C216 C211 C212 C213 -2.5(6) . . . . ? N210 C211 C212 C213 -179.5(4) . . . . ? C211 C212 C213 C214 1.3(7) . . . . ? C212 C213 C214 C215 -0.3(7) . . . . ? C213 C214 C215 C216 0.6(6) . . . . ? C212 C211 C216 C215 2.7(6) . . . . ? N210 C211 C216 C215 180.0(3) . . . . ? C214 C215 C216 C211 -1.8(6) . . . . ? N21 C26 C217 C218 20.4(6) . . . . ? N21 C26 C217 C222 -158.2(4) . . . . ? C222 C217 C218 C219 -0.8(7) . . . . ? C26 C217 C218 C219 -179.4(4) . . . . ? C217 C218 C219 C220 2.1(8) . . . . ? C218 C219 C220 C221 -1.8(9) . . . . ? C219 C220 C221 C222 0.2(11) . . . . ? C218 C217 C222 C221 -0.8(8) . . . . ? C26 C217 C222 C221 177.8(5) . . . . ? C220 C221 C222 C217 1.1(10) . . . . ? N21 C25 C223 C224 177.0(4) . . . . ? C24 C25 C223 C224 -0.3(6) . . . . ? C25 C223 C224 C225 0.0(6) . . . . ? C223 C224 C225 C226 0.6(6) . . . . ? N23 C24 C226 C225 -178.6(4) . . . . ? C25 C24 C226 C225 0.3(5) . . . . ? C224 C225 C226 C24 -0.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.27 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.027 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.061 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.000 -0.000 0.500 440 99 ' ' 2 -0.000 0.500 -0.000 440 100 ' ' _platon_squeeze_details ; ; #===END data_s4144a _database_code_depnum_ccdc_archive 'CCDC 723719' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H34 N8 Ni' _chemical_formula_sum 'C44 H34 N8 Ni' _chemical_formula_weight 733.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5841(1) _cell_length_b 13.4533(2) _cell_length_c 15.7310(2) _cell_angle_alpha 109.7758(8) _cell_angle_beta 103.2347(6) _cell_angle_gamma 95.7404(5) _cell_volume 2393.36(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 55881 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 44462 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10861 _reflns_number_gt 7719 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement HKL2000 _computing_data_reduction 'HKL2000, Sortav, Squeeze' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^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 10861 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 0.0000 0.0000 0.0000 0.04160(10) Uani 1 2 d S . . N11 N 0.07704(12) 0.18095(13) -0.05449(10) 0.0462(4) Uani 1 1 d . . . C12 C 0.08547(13) 0.12968(15) 0.00666(11) 0.0451(4) Uani 1 1 d . . . N13 N 0.16504(12) 0.19580(14) 0.08537(10) 0.0521(4) Uani 1 1 d . . . C14 C 0.20576(15) 0.28923(17) 0.07503(15) 0.0579(5) Uani 1 1 d . . . C15 C 0.14953(16) 0.28023(18) -0.01361(15) 0.0581(5) Uani 1 1 d . . . C16 C -0.00344(15) 0.14471(16) -0.14725(11) 0.0497(4) Uani 1 1 d . . . H16A H -0.0186 0.0651 -0.1752 0.060 Uiso 1 1 calc R . . H16B H 0.0293 0.1717 -0.1887 0.060 Uiso 1 1 calc R . . C17 C 0.18767(15) 0.17290(19) 0.17153(13) 0.0597(5) Uani 1 1 d . . . H17A H 0.2365 0.2362 0.2247 0.072 Uiso 1 1 calc R . . H17B H 0.2262 0.1111 0.1637 0.072 Uiso 1 1 calc R . . C18 C 0.08028(15) 0.14724(17) 0.19192(12) 0.0538(5) Uani 1 1 d . . . N19 N 0.06410(13) 0.18863(16) 0.27571(10) 0.0658(5) Uani 1 1 d . . . N110 N -0.00925(11) 0.08001(13) 0.12128(9) 0.0453(4) Uani 1 1 d . . . C111 C -0.09297(14) 0.07971(16) 0.16414(11) 0.0460(4) Uani 1 1 d . . . C112 C -0.20448(16) 0.02830(17) 0.12976(14) 0.0535(5) Uani 1 1 d . . . H112 H -0.2364 -0.0157 0.0652 0.064 Uiso 1 1 calc R . . C113 C -0.26682(18) 0.04402(19) 0.19361(16) 0.0642(5) Uani 1 1 d . . . H113 H -0.3428 0.0092 0.1724 0.077 Uiso 1 1 calc R . . C114 C -0.2209(2) 0.1096(2) 0.28814(15) 0.0684(6) Uani 1 1 d . . . H114 H -0.2660 0.1185 0.3300 0.082 Uiso 1 1 calc R . . C115 C -0.11174(19) 0.1615(2) 0.32181(14) 0.0677(6) Uani 1 1 d . . . H115 H -0.0811 0.2072 0.3861 0.081 Uiso 1 1 calc R . . C116 C -0.04753(16) 0.14538(18) 0.25961(12) 0.0575(5) Uani 1 1 d . . . C117 C -0.11162(15) 0.18283(15) -0.14340(11) 0.0475(4) Uani 1 1 d . . . C118 C -0.17337(17) 0.15872(18) -0.08847(14) 0.0580(5) Uani 1 1 d . . . H118 H -0.1461 0.1200 -0.0503 0.070 Uiso 1 1 calc R . . C119 C -0.27469(17) 0.1904(2) -0.08856(15) 0.0674(6) Uani 1 1 d . . . H119 H -0.3159 0.1752 -0.0494 0.081 Uiso 1 1 calc R . . C120 C -0.31573(18) 0.24432(19) -0.14577(15) 0.0693(6) Uani 1 1 d . . . H120 H -0.3859 0.2649 -0.1470 0.083 Uiso 1 1 calc R . . C121 C -0.25494(19) 0.26810(18) -0.20085(14) 0.0667(6) Uani 1 1 d . . . H121 H -0.2832 0.3051 -0.2403 0.080 Uiso 1 1 calc R . . C122 C -0.15256(17) 0.23840(16) -0.19917(12) 0.0546(5) Uani 1 1 d . . . H122 H -0.1102 0.2563 -0.2366 0.066 Uiso 1 1 calc R . . C123 C 0.1673(2) 0.3621(2) -0.0473(2) 0.0763(7) Uani 1 1 d . . . H123 H 0.1279 0.3553 -0.1088 0.092 Uiso 1 1 calc R . . C124 C 0.2433(3) 0.4515(2) 0.0115(3) 0.0976(9) Uani 1 1 d . . . H124 H 0.2580 0.5084 -0.0096 0.117 Uiso 1 1 calc R . . C125 C 0.2996(2) 0.4625(2) 0.1005(3) 0.0968(9) Uani 1 1 d . . . H125 H 0.3512 0.5274 0.1393 0.116 Uiso 1 1 calc R . . C126 C 0.28459(17) 0.3825(2) 0.13686(19) 0.0801(8) Uani 1 1 d . . . H126 H 0.3244 0.3903 0.1986 0.096 Uiso 1 1 calc R . . Ni2 Ni 0.5000 0.0000 0.5000 0.03143(8) Uani 1 2 d S . . N21 N 0.26201(10) 0.01922(10) 0.44271(8) 0.0335(3) Uani 1 1 d . . . C22 C 0.34176(12) -0.03260(12) 0.47032(10) 0.0335(3) Uani 1 1 d . . . N23 N 0.28805(10) -0.12665(10) 0.46706(8) 0.0343(3) Uani 1 1 d . . . C24 C 0.17318(12) -0.13497(13) 0.43940(10) 0.0365(4) Uani 1 1 d . . . C25 C 0.15695(12) -0.04119(13) 0.42391(10) 0.0344(3) Uani 1 1 d . . . C26 C 0.28044(13) 0.12369(13) 0.43349(11) 0.0376(4) Uani 1 1 d . . . H26A H 0.3134 0.1799 0.4971 0.045 Uiso 1 1 calc R . . H26B H 0.2075 0.1389 0.4069 0.045 Uiso 1 1 calc R . . C27 C 0.34818(14) -0.21018(14) 0.48113(12) 0.0412(4) Uani 1 1 d . . . H27A H 0.2948 -0.2782 0.4624 0.049 Uiso 1 1 calc R . . H27B H 0.3888 -0.1880 0.5485 0.049 Uiso 1 1 calc R . . C28 C 0.42815(13) -0.22709(13) 0.42337(11) 0.0379(4) Uani 1 1 d . . . N29 N 0.44170(12) -0.32345(11) 0.37177(11) 0.0479(4) Uani 1 1 d . . . N210 N 0.48998(10) -0.14218(10) 0.41908(9) 0.0348(3) Uani 1 1 d . . . C211 C 0.54760(13) -0.18703(14) 0.35554(11) 0.0401(4) Uani 1 1 d . . . C212 C 0.62135(14) -0.14049(16) 0.31876(12) 0.0475(4) Uani 1 1 d . . . H212 H 0.6408 -0.0647 0.3370 0.057 Uiso 1 1 calc R . . C213 C 0.66440(16) -0.21077(19) 0.25446(14) 0.0658(6) Uani 1 1 d . . . H213 H 0.7139 -0.1821 0.2274 0.079 Uiso 1 1 calc R . . C214 C 0.63777(19) -0.3216(2) 0.22821(17) 0.0794(7) Uani 1 1 d . . . H214 H 0.6706 -0.3666 0.1848 0.095 Uiso 1 1 calc R . . C215 C 0.56530(18) -0.36759(18) 0.26339(17) 0.0727(7) Uani 1 1 d . . . H215 H 0.5469 -0.4436 0.2446 0.087 Uiso 1 1 calc R . . C216 C 0.51916(15) -0.29934(14) 0.32786(13) 0.0505(5) Uani 1 1 d . . . C217 C 0.35500(13) 0.13206(14) 0.37264(11) 0.0390(4) Uani 1 1 d . . . C218 C 0.37665(14) 0.04388(16) 0.30719(12) 0.0447(4) Uani 1 1 d . . . H218 H 0.3445 -0.0268 0.2993 0.054 Uiso 1 1 calc R . . C219 C 0.44547(16) 0.05822(19) 0.25272(14) 0.0576(5) Uani 1 1 d . . . H219 H 0.4608 -0.0026 0.2082 0.069 Uiso 1 1 calc R . . C220 C 0.49113(16) 0.1598(2) 0.26314(16) 0.0635(6) Uani 1 1 d . . . H220 H 0.5386 0.1692 0.2262 0.076 Uiso 1 1 calc R . . C221 C 0.46867(15) 0.24844(19) 0.32682(16) 0.0588(5) Uani 1 1 d . . . H221 H 0.4989 0.3189 0.3328 0.071 Uiso 1 1 calc R . . C222 C 0.40159(14) 0.23422(16) 0.38233(13) 0.0472(4) Uani 1 1 d . . . H222 H 0.3876 0.2954 0.4274 0.057 Uiso 1 1 calc R . . C223 C 0.05057(13) -0.02236(15) 0.39424(11) 0.0423(4) Uani 1 1 d . . . H223 H 0.0389 0.0417 0.3837 0.051 Uiso 1 1 calc R . . C224 C -0.03719(14) -0.10173(17) 0.38094(11) 0.0499(5) Uani 1 1 d . . . H224 H -0.1111 -0.0920 0.3606 0.060 Uiso 1 1 calc R . . C225 C -0.02042(14) -0.19520(17) 0.39649(12) 0.0509(5) Uani 1 1 d . . . H225 H -0.0831 -0.2476 0.3865 0.061 Uiso 1 1 calc R . . C226 C 0.08476(14) -0.21392(15) 0.42596(11) 0.0450(4) Uani 1 1 d . . . H226 H 0.0961 -0.2780 0.4366 0.054 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 0.02720(16) 0.0698(2) 0.02889(15) 0.01718(14) 0.00790(12) 0.01855(14) N11 0.0365(8) 0.0662(10) 0.0408(8) 0.0192(7) 0.0172(6) 0.0195(7) C12 0.0286(8) 0.0698(12) 0.0348(9) 0.0127(8) 0.0110(7) 0.0198(8) N13 0.0281(7) 0.0815(12) 0.0387(8) 0.0112(8) 0.0073(6) 0.0195(8) C14 0.0336(10) 0.0657(13) 0.0653(13) 0.0080(10) 0.0199(9) 0.0152(9) C15 0.0392(10) 0.0697(14) 0.0645(13) 0.0157(11) 0.0240(10) 0.0179(10) C16 0.0515(11) 0.0719(12) 0.0337(9) 0.0202(8) 0.0190(8) 0.0294(9) C17 0.0310(9) 0.0957(15) 0.0407(10) 0.0133(10) 0.0024(8) 0.0213(10) C18 0.0376(10) 0.0900(14) 0.0307(9) 0.0165(9) 0.0050(7) 0.0305(10) N19 0.0424(9) 0.1169(15) 0.0314(8) 0.0164(8) 0.0064(7) 0.0351(9) N110 0.0333(7) 0.0719(10) 0.0326(7) 0.0184(7) 0.0092(6) 0.0225(7) C111 0.0396(9) 0.0713(12) 0.0366(9) 0.0243(8) 0.0144(7) 0.0298(9) C112 0.0463(11) 0.0741(13) 0.0506(11) 0.0245(9) 0.0241(9) 0.0296(10) C113 0.0528(12) 0.0860(15) 0.0676(14) 0.0298(12) 0.0344(10) 0.0290(11) C114 0.0718(15) 0.0995(17) 0.0636(14) 0.0401(12) 0.0466(12) 0.0484(13) C115 0.0679(15) 0.1113(18) 0.0400(10) 0.0322(11) 0.0256(10) 0.0492(13) C116 0.0511(11) 0.0942(15) 0.0374(10) 0.0283(10) 0.0140(8) 0.0414(11) C117 0.0454(10) 0.0636(12) 0.0311(8) 0.0119(8) 0.0092(7) 0.0253(9) C118 0.0486(11) 0.0868(14) 0.0477(10) 0.0283(10) 0.0175(9) 0.0323(10) C119 0.0435(11) 0.1019(17) 0.0538(12) 0.0177(12) 0.0194(9) 0.0277(11) C120 0.0485(12) 0.0891(15) 0.0495(12) 0.0028(11) 0.0005(10) 0.0359(11) C121 0.0720(14) 0.0743(14) 0.0462(11) 0.0157(10) 0.0015(11) 0.0406(12) C122 0.0637(12) 0.0617(12) 0.0344(9) 0.0120(8) 0.0090(8) 0.0266(10) C123 0.0701(16) 0.0779(16) 0.0944(17) 0.0313(14) 0.0470(14) 0.0212(13) C124 0.081(2) 0.082(2) 0.125(3) 0.0223(18) 0.0437(19) 0.0172(16) C125 0.0707(18) 0.0586(16) 0.146(3) 0.0127(18) 0.041(2) 0.0106(13) C126 0.0375(11) 0.0884(18) 0.0841(16) -0.0038(14) 0.0110(11) 0.0210(12) Ni2 0.02262(14) 0.03784(16) 0.03172(15) 0.01151(12) 0.00435(11) 0.00936(11) N21 0.0263(6) 0.0440(7) 0.0305(6) 0.0143(6) 0.0062(5) 0.0116(6) C22 0.0278(8) 0.0402(9) 0.0288(8) 0.0104(6) 0.0039(6) 0.0090(7) N23 0.0286(7) 0.0408(8) 0.0323(7) 0.0147(6) 0.0047(5) 0.0071(6) C24 0.0284(8) 0.0511(10) 0.0261(7) 0.0108(7) 0.0063(6) 0.0070(7) C25 0.0241(7) 0.0516(10) 0.0237(7) 0.0094(7) 0.0064(6) 0.0077(7) C26 0.0309(8) 0.0462(9) 0.0399(9) 0.0192(7) 0.0087(7) 0.0171(7) C27 0.0366(9) 0.0435(9) 0.0434(9) 0.0201(8) 0.0061(7) 0.0060(7) C28 0.0312(8) 0.0401(9) 0.0399(9) 0.0166(7) 0.0015(7) 0.0096(7) N29 0.0441(8) 0.0388(8) 0.0549(9) 0.0135(7) 0.0072(7) 0.0124(7) N210 0.0267(6) 0.0381(7) 0.0340(7) 0.0086(6) 0.0039(5) 0.0091(6) C211 0.0289(8) 0.0501(10) 0.0354(8) 0.0097(7) 0.0040(7) 0.0154(7) C212 0.0315(9) 0.0625(11) 0.0385(9) 0.0081(8) 0.0066(7) 0.0116(8) C213 0.0376(10) 0.0877(17) 0.0520(11) -0.0006(11) 0.0154(9) 0.0116(10) C214 0.0558(14) 0.0825(17) 0.0745(15) -0.0103(12) 0.0269(12) 0.0232(12) C215 0.0540(13) 0.0562(13) 0.0831(15) -0.0064(11) 0.0186(12) 0.0194(10) C216 0.0424(10) 0.0442(10) 0.0520(10) 0.0061(8) 0.0027(8) 0.0184(8) C217 0.0270(8) 0.0535(10) 0.0401(9) 0.0229(8) 0.0049(7) 0.0151(7) C218 0.0344(9) 0.0629(11) 0.0417(9) 0.0229(8) 0.0107(7) 0.0186(8) C219 0.0486(11) 0.0923(16) 0.0534(11) 0.0396(11) 0.0266(9) 0.0343(11) C220 0.0383(10) 0.1134(19) 0.0700(14) 0.0642(14) 0.0222(10) 0.0284(12) C221 0.0363(10) 0.0822(15) 0.0753(14) 0.0553(12) 0.0080(10) 0.0141(10) C222 0.0362(9) 0.0598(11) 0.0524(10) 0.0327(9) 0.0052(8) 0.0145(8) C223 0.0279(8) 0.0660(11) 0.0326(8) 0.0160(8) 0.0089(7) 0.0147(8) C224 0.0264(8) 0.0827(14) 0.0330(9) 0.0139(9) 0.0063(7) 0.0089(9) C225 0.0327(9) 0.0725(13) 0.0391(9) 0.0129(9) 0.0122(7) -0.0041(9) C226 0.0392(9) 0.0555(11) 0.0355(9) 0.0133(8) 0.0107(7) 0.0003(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 N110 1.8840(13) . ? Ni1 N110 1.8840(13) 2 ? Ni1 C12 1.9133(19) 2 ? Ni1 C12 1.9133(19) . ? N11 C12 1.352(2) . ? N11 C15 1.392(3) . ? N11 C16 1.461(2) . ? C12 N13 1.355(2) . ? N13 C14 1.384(3) . ? N13 C17 1.462(3) . ? C14 C15 1.370(3) . ? C14 C126 1.410(3) . ? C15 C123 1.394(3) . ? C16 C117 1.509(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.493(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N19 1.318(2) . ? C18 N110 1.366(2) . ? N19 C116 1.396(3) . ? N110 C111 1.375(2) . ? C111 C112 1.395(3) . ? C111 C116 1.404(3) . ? C112 C113 1.385(3) . ? C112 H112 0.9500 . ? C113 C114 1.393(3) . ? C113 H113 0.9500 . ? C114 C115 1.371(3) . ? C114 H114 0.9500 . ? C115 C116 1.382(3) . ? C115 H115 0.9500 . ? C117 C118 1.379(3) . ? C117 C122 1.381(3) . ? C118 C119 1.384(3) . ? C118 H118 0.9500 . ? C119 C120 1.381(3) . ? C119 H119 0.9500 . ? C120 C121 1.371(3) . ? C120 H120 0.9500 . ? C121 C122 1.384(3) . ? C121 H121 0.9500 . ? C122 H122 0.9500 . ? C123 C124 1.352(4) . ? C123 H123 0.9500 . ? C124 C125 1.367(4) . ? C124 H124 0.9500 . ? C125 C126 1.394(4) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? Ni2 N210 1.8776(13) 2_656 ? Ni2 N210 1.8776(12) . ? Ni2 C22 1.9070(15) . ? Ni2 C22 1.9070(15) 2_656 ? N21 C22 1.3518(19) . ? N21 C25 1.3926(19) . ? N21 C26 1.462(2) . ? C22 N23 1.353(2) . ? N23 C24 1.3921(19) . ? N23 C27 1.465(2) . ? C24 C226 1.384(2) . ? C24 C25 1.389(2) . ? C25 C223 1.391(2) . ? C26 C217 1.508(2) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.488(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 N29 1.328(2) . ? C28 N210 1.347(2) . ? N29 C216 1.389(3) . ? N210 C211 1.379(2) . ? C211 C212 1.401(3) . ? C211 C216 1.406(2) . ? C212 C213 1.385(3) . ? C212 H212 0.9500 . ? C213 C214 1.388(3) . ? C213 H213 0.9500 . ? C214 C215 1.368(4) . ? C214 H214 0.9500 . ? C215 C216 1.398(3) . ? C215 H215 0.9500 . ? C217 C218 1.381(2) . ? C217 C222 1.383(2) . ? C218 C219 1.393(3) . ? C218 H218 0.9500 . ? C219 C220 1.369(3) . ? C219 H219 0.9500 . ? C220 C221 1.376(3) . ? C220 H220 0.9500 . ? C221 C222 1.389(3) . ? C221 H221 0.9500 . ? C222 H222 0.9500 . ? C223 C224 1.382(3) . ? C223 H223 0.9500 . ? C224 C225 1.387(3) . ? C224 H224 0.9500 . ? C225 C226 1.377(3) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N110 Ni1 N110 180.0 . 2 ? N110 Ni1 C12 93.59(7) . 2 ? N110 Ni1 C12 86.41(7) 2 2 ? N110 Ni1 C12 86.41(7) . . ? N110 Ni1 C12 93.59(7) 2 . ? C12 Ni1 C12 180.0 2 . ? C12 N11 C15 110.47(15) . . ? C12 N11 C16 126.04(16) . . ? C15 N11 C16 123.23(16) . . ? N11 C12 N13 105.58(16) . . ? N11 C12 Ni1 131.53(13) . . ? N13 C12 Ni1 122.60(13) . . ? C12 N13 C14 111.02(16) . . ? C12 N13 C17 121.15(17) . . ? C14 N13 C17 127.20(16) . . ? C15 C14 N13 106.25(17) . . ? C15 C14 C126 121.3(2) . . ? N13 C14 C126 132.4(2) . . ? C14 C15 N11 106.66(19) . . ? C14 C15 C123 122.0(2) . . ? N11 C15 C123 131.3(2) . . ? N11 C16 C117 112.63(13) . . ? N11 C16 H16A 109.1 . . ? C117 C16 H16A 109.1 . . ? N11 C16 H16B 109.1 . . ? C117 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N13 C17 C18 109.11(14) . . ? N13 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? N13 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? N19 C18 N110 116.16(17) . . ? N19 C18 C17 123.64(17) . . ? N110 C18 C17 120.17(15) . . ? C18 N19 C116 102.99(15) . . ? C18 N110 C111 104.07(14) . . ? C18 N110 Ni1 122.99(11) . . ? C111 N110 Ni1 132.59(12) . . ? N110 C111 C112 132.13(16) . . ? N110 C111 C116 107.31(16) . . ? C112 C111 C116 120.57(16) . . ? C113 C112 C111 117.30(19) . . ? C113 C112 H112 121.4 . . ? C111 C112 H112 121.4 . . ? C112 C113 C114 121.6(2) . . ? C112 C113 H113 119.2 . . ? C114 C113 H113 119.2 . . ? C115 C114 C113 121.16(18) . . ? C115 C114 H114 119.4 . . ? C113 C114 H114 119.4 . . ? C114 C115 C116 118.1(2) . . ? C114 C115 H115 120.9 . . ? C116 C115 H115 120.9 . . ? C115 C116 N19 129.34(19) . . ? C115 C116 C111 121.2(2) . . ? N19 C116 C111 109.45(16) . . ? C118 C117 C122 119.14(17) . . ? C118 C117 C16 121.15(16) . . ? C122 C117 C16 119.64(17) . . ? C117 C118 C119 120.54(19) . . ? C117 C118 H118 119.7 . . ? C119 C118 H118 119.7 . . ? C120 C119 C118 119.8(2) . . ? C120 C119 H119 120.1 . . ? C118 C119 H119 120.1 . . ? C121 C120 C119 119.87(19) . . ? C121 C120 H120 120.1 . . ? C119 C120 H120 120.1 . . ? C120 C121 C122 120.2(2) . . ? C120 C121 H121 119.9 . . ? C122 C121 H121 119.9 . . ? C117 C122 C121 120.4(2) . . ? C117 C122 H122 119.8 . . ? C121 C122 H122 119.8 . . ? C124 C123 C15 117.0(3) . . ? C124 C123 H123 121.5 . . ? C15 C123 H123 121.5 . . ? C123 C124 C125 122.0(3) . . ? C123 C124 H124 119.0 . . ? C125 C124 H124 119.0 . . ? C124 C125 C126 122.9(3) . . ? C124 C125 H125 118.6 . . ? C126 C125 H125 118.6 . . ? C125 C126 C14 114.9(3) . . ? C125 C126 H126 122.6 . . ? C14 C126 H126 122.6 . . ? N210 Ni2 N210 180.0 2_656 . ? N210 Ni2 C22 93.41(6) 2_656 . ? N210 Ni2 C22 86.59(6) . . ? N210 Ni2 C22 86.59(6) 2_656 2_656 ? N210 Ni2 C22 93.41(6) . 2_656 ? C22 Ni2 C22 180.0 . 2_656 ? C22 N21 C25 110.20(13) . . ? C22 N21 C26 126.13(13) . . ? C25 N21 C26 123.66(12) . . ? N21 C22 N23 106.33(13) . . ? N21 C22 Ni2 132.17(12) . . ? N23 C22 Ni2 121.30(11) . . ? C22 N23 C24 111.11(13) . . ? C22 N23 C27 121.56(13) . . ? C24 N23 C27 126.97(13) . . ? C226 C24 C25 121.76(15) . . ? C226 C24 N23 132.77(16) . . ? C25 C24 N23 105.46(13) . . ? C24 C25 C223 121.31(15) . . ? C24 C25 N21 106.87(13) . . ? C223 C25 N21 131.81(16) . . ? N21 C26 C217 114.75(13) . . ? N21 C26 H26A 108.6 . . ? C217 C26 H26A 108.6 . . ? N21 C26 H26B 108.6 . . ? C217 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? N23 C27 C28 109.40(13) . . ? N23 C27 H27A 109.8 . . ? C28 C27 H27A 109.8 . . ? N23 C27 H27B 109.8 . . ? C28 C27 H27B 109.8 . . ? H27A C27 H27B 108.2 . . ? N29 C28 N210 115.88(15) . . ? N29 C28 C27 123.81(15) . . ? N210 C28 C27 120.28(14) . . ? C28 N29 C216 103.21(14) . . ? C28 N210 C211 104.61(13) . . ? C28 N210 Ni2 122.57(11) . . ? C211 N210 Ni2 132.29(11) . . ? N210 C211 C212 131.76(16) . . ? N210 C211 C216 106.98(15) . . ? C212 C211 C216 121.26(16) . . ? C213 C212 C211 116.51(19) . . ? C213 C212 H212 121.7 . . ? C211 C212 H212 121.7 . . ? C212 C213 C214 122.3(2) . . ? C212 C213 H213 118.9 . . ? C214 C213 H213 118.9 . . ? C215 C214 C213 121.5(2) . . ? C215 C214 H214 119.3 . . ? C213 C214 H214 119.3 . . ? C214 C215 C216 118.0(2) . . ? C214 C215 H215 121.0 . . ? C216 C215 H215 121.0 . . ? N29 C216 C215 130.22(19) . . ? N29 C216 C211 109.26(15) . . ? C215 C216 C211 120.5(2) . . ? C218 C217 C222 119.04(16) . . ? C218 C217 C26 123.58(16) . . ? C222 C217 C26 117.37(15) . . ? C217 C218 C219 120.19(19) . . ? C217 C218 H218 119.9 . . ? C219 C218 H218 119.9 . . ? C220 C219 C218 120.1(2) . . ? C220 C219 H219 119.9 . . ? C218 C219 H219 119.9 . . ? C219 C220 C221 120.32(18) . . ? C219 C220 H220 119.8 . . ? C221 C220 H220 119.8 . . ? C220 C221 C222 119.6(2) . . ? C220 C221 H221 120.2 . . ? C222 C221 H221 120.2 . . ? C217 C222 C221 120.72(19) . . ? C217 C222 H222 119.6 . . ? C221 C222 H222 119.6 . . ? C224 C223 C25 116.49(17) . . ? C224 C223 H223 121.8 . . ? C25 C223 H223 121.8 . . ? C223 C224 C225 121.92(16) . . ? C223 C224 H224 119.0 . . ? C225 C224 H224 119.0 . . ? C226 C225 C224 121.69(16) . . ? C226 C225 H225 119.2 . . ? C224 C225 H225 119.2 . . ? C225 C226 C24 116.83(17) . . ? C225 C226 H226 121.6 . . ? C24 C226 H226 121.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 N11 C12 N13 -1.26(18) . . . . ? C16 N11 C12 N13 -175.54(14) . . . . ? C15 N11 C12 Ni1 172.51(13) . . . . ? C16 N11 C12 Ni1 -1.8(2) . . . . ? N110 Ni1 C12 N11 -130.68(16) . . . . ? N110 Ni1 C12 N11 49.32(16) 2 . . . ? N110 Ni1 C12 N13 42.19(14) . . . . ? N110 Ni1 C12 N13 -137.81(14) 2 . . . ? N11 C12 N13 C14 0.94(18) . . . . ? Ni1 C12 N13 C14 -173.52(12) . . . . ? N11 C12 N13 C17 172.50(15) . . . . ? Ni1 C12 N13 C17 -2.0(2) . . . . ? C12 N13 C14 C15 -0.3(2) . . . . ? C17 N13 C14 C15 -171.19(16) . . . . ? C12 N13 C14 C126 177.3(2) . . . . ? C17 N13 C14 C126 6.4(3) . . . . ? N13 C14 C15 N11 -0.49(19) . . . . ? C126 C14 C15 N11 -178.43(17) . . . . ? N13 C14 C15 C123 178.15(18) . . . . ? C126 C14 C15 C123 0.2(3) . . . . ? C12 N11 C15 C14 1.11(19) . . . . ? C16 N11 C15 C14 175.59(15) . . . . ? C12 N11 C15 C123 -177.4(2) . . . . ? C16 N11 C15 C123 -2.9(3) . . . . ? C12 N11 C16 C117 87.4(2) . . . . ? C15 N11 C16 C117 -86.2(2) . . . . ? C12 N13 C17 C18 -48.1(2) . . . . ? C14 N13 C17 C18 122.04(19) . . . . ? N13 C17 C18 N19 -133.6(2) . . . . ? N13 C17 C18 N110 44.4(3) . . . . ? N110 C18 N19 C116 -0.4(2) . . . . ? C17 C18 N19 C116 177.69(19) . . . . ? N19 C18 N110 C111 1.2(2) . . . . ? C17 C18 N110 C111 -176.93(18) . . . . ? N19 C18 N110 Ni1 -172.71(14) . . . . ? C17 C18 N110 Ni1 9.2(3) . . . . ? C12 Ni1 N110 C18 134.55(15) 2 . . . ? C12 Ni1 N110 C18 -45.45(15) . . . . ? C12 Ni1 N110 C111 -37.42(17) 2 . . . ? C12 Ni1 N110 C111 142.58(17) . . . . ? C18 N110 C111 C112 178.9(2) . . . . ? Ni1 N110 C111 C112 -8.0(3) . . . . ? C18 N110 C111 C116 -1.5(2) . . . . ? Ni1 N110 C111 C116 171.58(13) . . . . ? N110 C111 C112 C113 178.88(19) . . . . ? C116 C111 C112 C113 -0.7(3) . . . . ? C111 C112 C113 C114 0.9(3) . . . . ? C112 C113 C114 C115 0.1(4) . . . . ? C113 C114 C115 C116 -1.2(3) . . . . ? C114 C115 C116 N19 179.6(2) . . . . ? C114 C115 C116 C111 1.4(3) . . . . ? C18 N19 C116 C115 -179.0(2) . . . . ? C18 N19 C116 C111 -0.6(2) . . . . ? N110 C111 C116 C115 179.90(19) . . . . ? C112 C111 C116 C115 -0.4(3) . . . . ? N110 C111 C116 N19 1.4(2) . . . . ? C112 C111 C116 N19 -178.97(18) . . . . ? N11 C16 C117 C118 -57.1(3) . . . . ? N11 C16 C117 C122 126.04(18) . . . . ? C122 C117 C118 C119 -0.5(3) . . . . ? C16 C117 C118 C119 -177.35(19) . . . . ? C117 C118 C119 C120 1.6(3) . . . . ? C118 C119 C120 C121 -1.3(3) . . . . ? C119 C120 C121 C122 -0.1(3) . . . . ? C118 C117 C122 C121 -0.9(3) . . . . ? C16 C117 C122 C121 175.99(18) . . . . ? C120 C121 C122 C117 1.2(3) . . . . ? C14 C15 C123 C124 0.1(3) . . . . ? N11 C15 C123 C124 178.4(2) . . . . ? C15 C123 C124 C125 -0.7(4) . . . . ? C123 C124 C125 C126 1.0(4) . . . . ? C124 C125 C126 C14 -0.6(4) . . . . ? C15 C14 C126 C125 0.0(3) . . . . ? N13 C14 C126 C125 -177.3(2) . . . . ? C25 N21 C22 N23 1.40(16) . . . . ? C26 N21 C22 N23 -178.81(13) . . . . ? C25 N21 C22 Ni2 176.28(11) . . . . ? C26 N21 C22 Ni2 -3.9(2) . . . . ? N210 Ni2 C22 N21 49.29(15) 2_656 . . . ? N210 Ni2 C22 N21 -130.71(15) . . . . ? N210 Ni2 C22 N23 -136.46(12) 2_656 . . . ? N210 Ni2 C22 N23 43.54(12) . . . . ? N21 C22 N23 C24 -1.39(16) . . . . ? Ni2 C22 N23 C24 -176.95(10) . . . . ? N21 C22 N23 C27 172.23(13) . . . . ? Ni2 C22 N23 C27 -3.33(19) . . . . ? C22 N23 C24 C226 -179.95(16) . . . . ? C27 N23 C24 C226 6.9(3) . . . . ? C22 N23 C24 C25 0.84(16) . . . . ? C27 N23 C24 C25 -172.35(14) . . . . ? C226 C24 C25 C223 0.1(2) . . . . ? N23 C24 C25 C223 179.44(13) . . . . ? C226 C24 C25 N21 -179.28(14) . . . . ? N23 C24 C25 N21 0.04(15) . . . . ? C22 N21 C25 C24 -0.90(16) . . . . ? C26 N21 C25 C24 179.31(13) . . . . ? C22 N21 C25 C223 179.78(15) . . . . ? C26 N21 C25 C223 0.0(2) . . . . ? C22 N21 C26 C217 53.5(2) . . . . ? C25 N21 C26 C217 -126.73(15) . . . . ? C22 N23 C27 C28 -46.89(19) . . . . ? C24 N23 C27 C28 125.65(15) . . . . ? N23 C27 C28 N29 -135.32(15) . . . . ? N23 C27 C28 N210 42.83(19) . . . . ? N210 C28 N29 C216 -1.03(18) . . . . ? C27 C28 N29 C216 177.20(15) . . . . ? N29 C28 N210 C211 2.24(18) . . . . ? C27 C28 N210 C211 -176.06(14) . . . . ? N29 C28 N210 Ni2 -170.37(11) . . . . ? C27 C28 N210 Ni2 11.33(19) . . . . ? C22 Ni2 N210 C28 -47.76(12) . . . . ? C22 Ni2 N210 C28 132.24(12) 2_656 . . . ? C22 Ni2 N210 C211 141.92(14) . . . . ? C22 Ni2 N210 C211 -38.08(14) 2_656 . . . ? C28 N210 C211 C212 176.99(17) . . . . ? Ni2 N210 C211 C212 -11.4(3) . . . . ? C28 N210 C211 C216 -2.41(16) . . . . ? Ni2 N210 C211 C216 169.16(11) . . . . ? N210 C211 C212 C213 -179.51(17) . . . . ? C216 C211 C212 C213 -0.2(2) . . . . ? C211 C212 C213 C214 -0.9(3) . . . . ? C212 C213 C214 C215 1.3(4) . . . . ? C213 C214 C215 C216 -0.7(4) . . . . ? C28 N29 C216 C215 -178.8(2) . . . . ? C28 N29 C216 C211 -0.62(18) . . . . ? C214 C215 C216 N29 177.6(2) . . . . ? C214 C215 C216 C211 -0.4(3) . . . . ? N210 C211 C216 N29 1.95(18) . . . . ? C212 C211 C216 N29 -177.53(15) . . . . ? N210 C211 C216 C215 -179.70(17) . . . . ? C212 C211 C216 C215 0.8(3) . . . . ? N21 C26 C217 C218 19.8(2) . . . . ? N21 C26 C217 C222 -161.72(13) . . . . ? C222 C217 C218 C219 0.7(2) . . . . ? C26 C217 C218 C219 179.20(15) . . . . ? C217 C218 C219 C220 -0.6(3) . . . . ? C218 C219 C220 C221 -0.6(3) . . . . ? C219 C220 C221 C222 1.7(3) . . . . ? C218 C217 C222 C221 0.4(2) . . . . ? C26 C217 C222 C221 -178.19(15) . . . . ? C220 C221 C222 C217 -1.6(3) . . . . ? C24 C25 C223 C224 -0.2(2) . . . . ? N21 C25 C223 C224 179.07(15) . . . . ? C25 C223 C224 C225 0.1(2) . . . . ? C223 C224 C225 C226 -0.1(3) . . . . ? C224 C225 C226 C24 0.0(2) . . . . ? C25 C24 C226 C225 0.0(2) . . . . ? N23 C24 C226 C225 -179.15(16) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.325 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.041 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.011 0.000 -0.014 852 367 ' ' _platon_squeeze_details ; ; #===END