# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dong Wen' _publ_contact_author_address ; guangzhou guangzhou Guangdong China 510006 ; _publ_contact_author_email dw320@yahoo.com.cn loop_ _publ_author_name 'Jiao-Min Lin' 'Wen-Bin Chen' 'Xue-Mei Lin' 'An-Hui Lin' 'Chang-Yan Ma' ; Dong Wen ; 'Chang-En Tian' # Attachment '- Ni.cif' data_d _database_code_depnum_ccdc_archive 'CCDC 758557' #TrackingRef '- Ni.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H68 N32 Ni2 O10' _chemical_formula_weight 1562.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.5467(3) _cell_length_b 24.5577(5) _cell_length_c 22.8190(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.1530(10) _cell_angle_gamma 90.00 _cell_volume 7392.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9990 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 27.490 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.244 _exptl_crystal_size_mid 0.192 _exptl_crystal_size_min 0.127 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3248 _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 30696 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.49 _reflns_number_total 14957 _reflns_number_gt 12110 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(8) _refine_ls_number_reflns 14957 _refine_ls_number_parameters 1082 _refine_ls_number_restraints 164 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 1.002 _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 0.05322(3) 0.168662(14) 0.101273(18) 0.04629(10) Uani 1 1 d . . . Ni2 Ni 0.53620(3) 0.006056(14) 0.091085(18) 0.04533(10) Uani 1 1 d . . . N11 N 0.1248(3) 0.90587(15) 0.31757(18) 0.0842(10) Uani 1 1 d U . . N12 N 0.0533(3) 0.93333(16) 0.33445(19) 0.0867(11) Uani 1 1 d U . . N13 N -0.0263(3) 0.90307(17) 0.3285(2) 0.0947(11) Uani 1 1 d U . . N14 N -0.0070(3) 0.85480(17) 0.3072(2) 0.0950(12) Uani 1 1 d U . . N15 N 0.1440(3) 0.81190(18) 0.2911(2) 0.0970(12) Uani 1 1 d . . . N16 N 0.1461(3) 0.79623(15) 0.2391(2) 0.0912(11) Uani 1 1 d . . . N17 N 0.0527(4) 0.86978(17) 0.1792(2) 0.1112(15) Uani 1 1 d U . . N18 N 0.0222(3) 0.87552(16) 0.11792(18) 0.0976(12) Uani 1 1 d U . . N19 N 0.0441(6) 0.83392(17) 0.0938(3) 0.1153(15) Uani 1 1 d U . . N20 N 0.0899(5) 0.79908(19) 0.1356(2) 0.1290(18) Uani 1 1 d U . . N21 N -0.0503(2) 0.17089(10) 0.15632(12) 0.0480(6) Uani 1 1 d . . . N22 N -0.0455(2) 0.22973(12) 0.05966(11) 0.0554(7) Uani 1 1 d . . . N23 N 0.1587(2) 0.17970(13) 0.04794(12) 0.0567(7) Uani 1 1 d . . . N24 N 0.1491(2) 0.22691(11) 0.15090(11) 0.0507(6) Uani 1 1 d . . . N25 N 0.12741(19) 0.10045(11) 0.14458(11) 0.0475(6) Uani 1 1 d . . . N26 N -0.0252(2) 0.10550(12) 0.04966(11) 0.0537(7) Uani 1 1 d . . . N27 N 0.59475(18) -0.05183(11) 0.04085(11) 0.0468(6) Uani 1 1 d . . . N28 N 0.68584(19) 0.00022(11) 0.14130(12) 0.0482(6) Uani 1 1 d . . . N29 N 0.5064(2) 0.07148(12) 0.14298(12) 0.0533(6) Uani 1 1 d . . . N30 N 0.5672(2) 0.07231(11) 0.04077(12) 0.0525(6) Uani 1 1 d . . . N31 N 0.4818(2) -0.05366(11) 0.14104(11) 0.0520(6) Uani 1 1 d . . . N32 N 0.3855(2) -0.00159(11) 0.04300(12) 0.0502(6) Uani 1 1 d . . . C3 C 0.0867(3) 0.85838(17) 0.30159(19) 0.0705(9) Uani 1 1 d U . . C4 C 0.0939(3) 0.82420(15) 0.1862(2) 0.0664(9) Uani 1 1 d U . . C5 C -0.0453(3) 0.14338(14) 0.20727(14) 0.0525(7) Uani 1 1 d . . . H5 H 0.0071 0.1184 0.2192 0.063 Uiso 1 1 calc R . . C6 C -0.1132(3) 0.14986(15) 0.24304(15) 0.0607(9) Uani 1 1 d . . . H6 H -0.1061 0.1301 0.2785 0.073 Uiso 1 1 calc R . . C7 C -0.1916(3) 0.18594(18) 0.22567(17) 0.0720(10) Uani 1 1 d . . . H7 H -0.2392 0.1909 0.2488 0.086 Uiso 1 1 calc R . . C8 C -0.1978(3) 0.21456(16) 0.17324(17) 0.0676(9) Uani 1 1 d . . . H8 H -0.2504 0.2393 0.1606 0.081 Uiso 1 1 calc R . . C9 C -0.1267(2) 0.20695(13) 0.13908(14) 0.0495(7) Uani 1 1 d . . . C10 C -0.1257(3) 0.23816(13) 0.08398(14) 0.0523(7) Uani 1 1 d . . . C11 C -0.2024(3) 0.27425(16) 0.05849(17) 0.0728(11) Uani 1 1 d . . . H11 H -0.2584 0.2785 0.0753 0.087 Uiso 1 1 calc R . . C12 C -0.1953(4) 0.30360(18) 0.00845(19) 0.0823(13) Uani 1 1 d . . . H12 H -0.2458 0.3281 -0.0090 0.099 Uiso 1 1 calc R . . C13 C -0.1110(4) 0.29583(18) -0.01533(18) 0.0835(13) Uani 1 1 d . . . H13 H -0.1032 0.3157 -0.0487 0.100 Uiso 1 1 calc R . . C14 C -0.0385(3) 0.25817(16) 0.01108(15) 0.0684(10) Uani 1 1 d . . . H14 H 0.0171 0.2525 -0.0057 0.082 Uiso 1 1 calc R . . C15 C 0.1585(4) 0.15539(19) -0.00453(18) 0.0787(12) Uani 1 1 d . . . H15 H 0.1091 0.1295 -0.0194 0.094 Uiso 1 1 calc R . . C16 C 0.2295(5) 0.1678(2) -0.0371(2) 0.0934(17) Uani 1 1 d . . . H16 H 0.2269 0.1510 -0.0740 0.112 Uiso 1 1 calc R . . C17 C 0.3017(4) 0.2039(2) -0.0156(2) 0.0966(15) Uani 1 1 d . . . H17 H 0.3509 0.2117 -0.0369 0.116 Uiso 1 1 calc R . . C18 C 0.3040(4) 0.2295(2) 0.0378(2) 0.0859(13) Uani 1 1 d . . . H18 H 0.3538 0.2551 0.0529 0.103 Uiso 1 1 calc R . . C19 C 0.2307(3) 0.21665(16) 0.06919(15) 0.0602(8) Uani 1 1 d . . . C20 C 0.2260(2) 0.24300(14) 0.12661(14) 0.0535(7) Uani 1 1 d . . . C21 C 0.2912(3) 0.2829(2) 0.1539(2) 0.0827(12) Uani 1 1 d . . . H21 H 0.3435 0.2941 0.1365 0.099 Uiso 1 1 calc R . . C22 C 0.2805(4) 0.3069(2) 0.2070(2) 0.0863(13) Uani 1 1 d . . . H22 H 0.3252 0.3338 0.2256 0.104 Uiso 1 1 calc R . . C23 C 0.2029(4) 0.29011(17) 0.23110(17) 0.0756(11) Uani 1 1 d . . . H23 H 0.1930 0.3054 0.2666 0.091 Uiso 1 1 calc R . . C24 C 0.1392(3) 0.25005(15) 0.20223(15) 0.0624(9) Uani 1 1 d . . . H24 H 0.0866 0.2385 0.2193 0.075 Uiso 1 1 calc R . . C25 C 0.2029(3) 0.10006(16) 0.19417(15) 0.0612(9) Uani 1 1 d . . . H25 H 0.2337 0.1329 0.2080 0.073 Uiso 1 1 calc R . . C26 C 0.2367(3) 0.05363(18) 0.22531(17) 0.0709(10) Uani 1 1 d . . . H26 H 0.2890 0.0549 0.2597 0.085 Uiso 1 1 calc R . . C27 C 0.1921(3) 0.00558(18) 0.20497(18) 0.0737(11) Uani 1 1 d . . . H27 H 0.2139 -0.0265 0.2256 0.088 Uiso 1 1 calc R . . C28 C 0.1156(3) 0.00410(16) 0.15448(18) 0.0686(10) Uani 1 1 d . . . H28 H 0.0845 -0.0287 0.1406 0.082 Uiso 1 1 calc R . . C29 C 0.0849(2) 0.05277(14) 0.12398(13) 0.0489(7) Uani 1 1 d . . . C30 C 0.0036(2) 0.05503(14) 0.06886(13) 0.0513(7) Uani 1 1 d . . . C31 C -0.0397(3) 0.00924(16) 0.03853(17) 0.0644(9) Uani 1 1 d . . . H31 H -0.0193 -0.0253 0.0532 0.077 Uiso 1 1 calc R . . C32 C -0.1137(3) 0.01511(19) -0.01391(18) 0.0760(11) Uani 1 1 d . . . H32 H -0.1423 -0.0153 -0.0356 0.091 Uiso 1 1 calc R . . C33 C -0.1439(3) 0.0657(2) -0.03316(17) 0.0774(11) Uani 1 1 d . . . H33 H -0.1947 0.0704 -0.0678 0.093 Uiso 1 1 calc R . . C34 C -0.0990(3) 0.11090(17) -0.00106(16) 0.0695(10) Uani 1 1 d . . . H34 H -0.1202 0.1456 -0.0148 0.083 Uiso 1 1 calc R . . C35 C 0.5471(3) -0.07533(14) -0.01042(14) 0.0579(8) Uani 1 1 d . . . H35 H 0.4793 -0.0667 -0.0258 0.070 Uiso 1 1 calc R . . C36 C 0.5928(3) -0.11163(16) -0.04180(17) 0.0662(10) Uani 1 1 d . . . H36 H 0.5567 -0.1274 -0.0773 0.079 Uiso 1 1 calc R . . C37 C 0.6934(3) -0.12389(17) -0.01916(17) 0.0676(10) Uani 1 1 d . . . H37 H 0.7269 -0.1478 -0.0397 0.081 Uiso 1 1 calc R . . C38 C 0.7436(3) -0.10084(15) 0.03336(16) 0.0593(9) Uani 1 1 d . . . H38 H 0.8113 -0.1093 0.0493 0.071 Uiso 1 1 calc R . . C39 C 0.6930(2) -0.06443(13) 0.06311(13) 0.0481(7) Uani 1 1 d . . . C40 C 0.7427(2) -0.03662(13) 0.11947(13) 0.0469(7) Uani 1 1 d . . . C41 C 0.8409(3) -0.04749(16) 0.14997(16) 0.0619(9) Uani 1 1 d . . . H41 H 0.8797 -0.0724 0.1343 0.074 Uiso 1 1 calc R . . C42 C 0.8815(3) -0.02166(18) 0.20343(16) 0.0681(10) Uani 1 1 d . . . H42 H 0.9475 -0.0291 0.2242 0.082 Uiso 1 1 calc R . . C43 C 0.8242(3) 0.01482(16) 0.22560(16) 0.0623(9) Uani 1 1 d . . . H43 H 0.8499 0.0327 0.2618 0.075 Uiso 1 1 calc R . . C44 C 0.7267(3) 0.02468(15) 0.19311(16) 0.0603(8) Uani 1 1 d . . . H44 H 0.6875 0.0498 0.2083 0.072 Uiso 1 1 calc R . . C45 C 0.4823(3) 0.06795(18) 0.19646(16) 0.0654(9) Uani 1 1 d . . . H45 H 0.4666 0.0339 0.2097 0.079 Uiso 1 1 calc R . . C46 C 0.4797(3) 0.1123(2) 0.23294(19) 0.0785(12) Uani 1 1 d . . . H46 H 0.4644 0.1081 0.2704 0.094 Uiso 1 1 calc R . . C47 C 0.5000(4) 0.1622(2) 0.2132(3) 0.0912(16) Uani 1 1 d . . . H47 H 0.4975 0.1930 0.2366 0.109 Uiso 1 1 calc R . . C48 C 0.5246(4) 0.16679(17) 0.1572(2) 0.0812(13) Uani 1 1 d . . . H48 H 0.5387 0.2006 0.1427 0.097 Uiso 1 1 calc R . . C49 C 0.5276(2) 0.12041(15) 0.12367(15) 0.0558(8) Uani 1 1 d . . . C50 C 0.5567(2) 0.12136(15) 0.06488(16) 0.0564(8) Uani 1 1 d . . . C51 C 0.5728(4) 0.16932(18) 0.0358(2) 0.0783(12) Uani 1 1 d . . . H51 H 0.5675 0.2029 0.0537 0.094 Uiso 1 1 calc R . . C52 C 0.5964(4) 0.1666(2) -0.0189(2) 0.0886(15) Uani 1 1 d . . . H52 H 0.6069 0.1983 -0.0388 0.106 Uiso 1 1 calc R . . C53 C 0.6045(3) 0.1172(2) -0.04421(19) 0.0776(12) Uani 1 1 d . . . H53 H 0.6187 0.1149 -0.0821 0.093 Uiso 1 1 calc R . . C54 C 0.5914(3) 0.07063(18) -0.01324(16) 0.0661(9) Uani 1 1 d . . . H54 H 0.5995 0.0370 -0.0302 0.079 Uiso 1 1 calc R . . C55 C 0.5334(3) -0.07834(16) 0.19075(15) 0.0638(9) Uani 1 1 d . . . H55 H 0.6018 -0.0701 0.2044 0.077 Uiso 1 1 calc R . . C56 C 0.4908(3) -0.11510(18) 0.22252(17) 0.0745(11) Uani 1 1 d . . . H56 H 0.5286 -0.1305 0.2578 0.089 Uiso 1 1 calc R . . C57 C 0.3902(4) -0.12899(19) 0.2012(2) 0.0811(12) Uani 1 1 d . . . H57 H 0.3596 -0.1548 0.2211 0.097 Uiso 1 1 calc R . . C58 C 0.3371(3) -0.10424(17) 0.15064(18) 0.0717(10) Uani 1 1 d . . . H58 H 0.2689 -0.1126 0.1362 0.086 Uiso 1 1 calc R . . C59 C 0.3831(2) -0.06690(14) 0.12036(14) 0.0517(7) Uani 1 1 d . . . C60 C 0.3306(2) -0.03818(14) 0.06485(14) 0.0517(7) Uani 1 1 d . . . C61 C 0.2298(3) -0.04878(19) 0.03668(17) 0.0694(10) Uani 1 1 d . . . H61 H 0.1922 -0.0740 0.0528 0.083 Uiso 1 1 calc R . . C62 C 0.1876(3) -0.0214(2) -0.01494(18) 0.0780(12) Uani 1 1 d . . . H62 H 0.1209 -0.0284 -0.0348 0.094 Uiso 1 1 calc R . . C63 C 0.2430(3) 0.01599(19) -0.03722(17) 0.0713(11) Uani 1 1 d . . . H63 H 0.2147 0.0350 -0.0722 0.086 Uiso 1 1 calc R . . C64 C 0.3416(3) 0.02525(16) -0.00711(15) 0.0589(8) Uani 1 1 d . . . H64 H 0.3793 0.0512 -0.0222 0.071 Uiso 1 1 calc R . . O1 O 0.3423(3) 0.90710(14) 0.3513(2) 0.1205(14) Uani 1 1 d U . . H1A H 0.2779 0.9069 0.3410 0.181 Uiso 1 1 d R . . H1B H 0.3636 0.8755 0.3454 0.181 Uiso 1 1 d R . . O2 O 0.7464(3) 0.90349(13) 0.31325(15) 0.0888(9) Uani 1 1 d . . . H2A H 0.8104 0.9075 0.3215 0.133 Uiso 1 1 d R . . H2B H 0.7199 0.9326 0.3228 0.133 Uiso 1 1 d R . . O3 O 0.6480(3) 0.99224(16) 0.3435(3) 0.156(2) Uani 1 1 d . . . H3A H 0.6697 1.0240 0.3385 0.234 Uiso 1 1 d R . . H3B H 0.5854 0.9945 0.3437 0.234 Uiso 1 1 d R . . O4 O 0.2764(4) 0.31057(18) 0.3935(2) 0.1355(15) Uani 1 1 d U . . H4A H 0.3108 0.2849 0.3830 0.203 Uiso 1 1 d R . . H4B H 0.2641 0.3338 0.3651 0.203 Uiso 1 1 d R . . O5 O 0.0364(3) 0.04898(14) 0.33599(19) 0.1213(14) Uani 1 1 d . . . H5A H 0.0512 0.0158 0.3440 0.182 Uiso 1 1 d R . . H5B H 0.0904 0.0660 0.3343 0.182 Uiso 1 1 d R . . O6 O 0.4792(4) 0.24217(19) 0.3454(3) 0.169(2) Uani 1 1 d U . . H6A H 0.4224 0.2259 0.3394 0.254 Uiso 1 1 d R . . H6B H 0.4697 0.2744 0.3317 0.254 Uiso 1 1 d R . . O7 O 0.6731(3) 0.19977(14) 0.35748(17) 0.1070(11) Uani 1 1 d . . . H7A H 0.7242 0.2195 0.3565 0.161 Uiso 1 1 d R . . H7B H 0.6210 0.2200 0.3532 0.161 Uiso 1 1 d R . . O8 O 0.4492(3) 0.99668(15) 0.3452(3) 0.154(2) Uani 1 1 d . . . H8A H 0.4066 0.9717 0.3320 0.232 Uiso 1 1 d R . . H8B H 0.4185 1.0225 0.3582 0.232 Uiso 1 1 d R . . O9 O 0.7256(3) 0.09465(14) 0.32881(17) 0.1047(11) Uani 1 1 d . . . H9A H 0.6982 0.1234 0.3386 0.157 Uiso 1 1 d R . . H9B H 0.7854 0.0925 0.3506 0.157 Uiso 1 1 d R . . O10 O 0.9136(5) 0.0955(3) 0.4025(3) 0.187(2) Uani 1 1 d U . . H10A H 0.9468 0.1072 0.4363 0.281 Uiso 1 1 d R . . H10B H 0.9525 0.0755 0.3873 0.281 Uiso 1 1 d R . . C1 C 0.2139(12) 0.1464(7) 0.3546(9) 0.057(4) Uani 0.50 1 d PD A 1 N1 N 0.2284(17) 0.0950(7) 0.3755(8) 0.099(7) Uani 0.50 1 d PD A 1 N2 N 0.3243(17) 0.0860(6) 0.3735(7) 0.094(8) Uani 0.50 1 d PD A 1 N3 N 0.3627(12) 0.1282(10) 0.3532(8) 0.093(7) Uani 0.50 1 d PD A 1 N4 N 0.2958(12) 0.1677(6) 0.3405(8) 0.060(4) Uani 0.50 1 d PD A 1 N5 N 0.1246(9) 0.1719(4) 0.3586(5) 0.057(2) Uani 0.50 1 d P A 1 N6 N 0.1158(8) 0.2188(3) 0.3445(3) 0.0598(16) Uani 0.50 1 d P A 1 C2 C 0.0251(12) 0.2441(6) 0.3478(8) 0.051(4) Uani 0.50 1 d PD A 1 N7 N -0.0494(15) 0.2199(6) 0.3674(8) 0.079(5) Uani 0.50 1 d PDU A 1 N8 N -0.1289(13) 0.2549(7) 0.3568(8) 0.072(4) Uani 0.50 1 d PDU A 1 N9 N -0.0971(15) 0.2984(7) 0.3313(10) 0.088(6) Uani 0.50 1 d PD A 1 N10 N -0.0030(14) 0.2922(6) 0.3255(9) 0.078(4) Uani 0.50 1 d PD A 1 C1' C 0.2392(10) 0.1578(5) 0.3505(7) 0.036(3) Uani 0.50 1 d PD B 2 N1' N 0.2374(9) 0.1074(5) 0.3741(5) 0.047(2) Uani 0.50 1 d PD B 2 N2' N 0.3280(9) 0.0881(5) 0.3725(6) 0.068(6) Uani 0.50 1 d PD B 2 N3' N 0.3800(11) 0.1236(6) 0.3499(7) 0.058(3) Uani 0.50 1 d PD B 2 N4' N 0.3270(11) 0.1682(7) 0.3354(8) 0.060(3) Uani 0.50 1 d PD B 2 N5' N 0.1609(5) 0.1982(4) 0.3391(3) 0.0504(14) Uani 0.50 1 d P B 2 N6' N 0.0889(6) 0.1879(5) 0.3641(4) 0.050(2) Uani 0.50 1 d P B 2 C2' C 0.0143(10) 0.2275(6) 0.3526(7) 0.044(3) Uani 0.50 1 d PD B 2 N7' N -0.0635(11) 0.2213(6) 0.3780(7) 0.069(4) Uani 0.50 1 d PD B 2 N8' N -0.1186(11) 0.2668(7) 0.3647(8) 0.071(4) Uani 0.50 1 d PDU B 2 N9' N -0.0729(15) 0.2989(7) 0.3320(8) 0.073(4) Uani 0.50 1 d PD B 2 N10' N 0.0105(12) 0.2742(5) 0.3242(8) 0.064(3) Uani 0.50 1 d PD B 2 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 0.0558(2) 0.0479(2) 0.03598(17) 0.00050(16) 0.01223(15) -0.00008(18) Ni2 0.04414(19) 0.04847(19) 0.04166(19) -0.00150(18) 0.00616(14) 0.00349(19) N11 0.0654(19) 0.070(2) 0.109(3) 0.001(2) 0.0033(19) -0.0033(17) N12 0.081(2) 0.070(2) 0.097(2) -0.0158(19) -0.0036(19) -0.0047(19) N13 0.087(2) 0.087(3) 0.114(3) -0.002(2) 0.033(2) 0.010(2) N14 0.081(2) 0.066(2) 0.131(3) -0.014(2) 0.010(2) -0.0056(18) N15 0.099(3) 0.094(3) 0.097(3) 0.020(2) 0.020(2) 0.036(2) N16 0.099(3) 0.077(2) 0.101(3) 0.015(2) 0.030(2) 0.035(2) N17 0.152(4) 0.077(3) 0.096(3) -0.002(2) 0.011(3) 0.053(3) N18 0.130(3) 0.071(2) 0.088(2) -0.0051(19) 0.016(2) 0.038(2) N19 0.143(4) 0.097(3) 0.100(3) 0.006(3) 0.015(3) 0.057(3) N20 0.203(5) 0.082(3) 0.108(3) -0.003(2) 0.047(3) 0.054(3) N21 0.0573(15) 0.0445(15) 0.0439(13) 0.0041(11) 0.0146(12) -0.0024(11) N22 0.0733(17) 0.0505(16) 0.0425(13) 0.0096(12) 0.0131(13) 0.0010(13) N23 0.0662(17) 0.0678(18) 0.0398(13) -0.0068(12) 0.0195(13) 0.0027(14) N24 0.0644(16) 0.0496(15) 0.0398(12) 0.0001(11) 0.0154(12) -0.0047(12) N25 0.0506(13) 0.0484(16) 0.0412(12) -0.0028(11) 0.0056(11) 0.0030(11) N26 0.0527(14) 0.0621(18) 0.0417(13) -0.0019(12) 0.0010(11) 0.0030(12) N27 0.0436(13) 0.0504(15) 0.0445(12) -0.0051(11) 0.0057(11) 0.0001(10) N28 0.0444(13) 0.0494(16) 0.0480(13) -0.0055(11) 0.0043(12) -0.0034(11) N29 0.0508(14) 0.0571(18) 0.0522(14) -0.0048(12) 0.0122(12) 0.0059(12) N30 0.0516(14) 0.0550(17) 0.0512(14) 0.0006(12) 0.0125(12) 0.0003(12) N31 0.0547(15) 0.0525(16) 0.0459(13) 0.0009(12) 0.0055(12) 0.0023(12) N32 0.0483(14) 0.0551(17) 0.0442(13) -0.0016(11) 0.0045(12) 0.0074(12) C3 0.063(2) 0.068(2) 0.077(2) 0.0021(19) 0.0086(18) 0.0028(18) C4 0.063(2) 0.053(2) 0.085(2) 0.0045(18) 0.0216(18) 0.0084(15) C5 0.0637(19) 0.0498(18) 0.0461(15) 0.0066(14) 0.0167(15) 0.0004(14) C6 0.080(2) 0.055(2) 0.0509(17) 0.0076(15) 0.0247(17) -0.0017(17) C7 0.083(3) 0.080(3) 0.063(2) 0.0040(19) 0.038(2) 0.005(2) C8 0.077(2) 0.065(2) 0.067(2) 0.0055(18) 0.0306(19) 0.0140(18) C9 0.0563(17) 0.0457(18) 0.0487(15) -0.0004(13) 0.0166(14) 0.0023(13) C10 0.0656(19) 0.0445(18) 0.0444(15) -0.0006(13) 0.0076(15) 0.0048(14) C11 0.093(3) 0.065(2) 0.0586(19) 0.0028(17) 0.013(2) 0.024(2) C12 0.109(3) 0.068(3) 0.064(2) 0.0154(19) 0.007(2) 0.023(2) C13 0.116(3) 0.071(3) 0.056(2) 0.0256(19) 0.004(2) -0.002(2) C14 0.084(2) 0.070(2) 0.0524(18) 0.0176(17) 0.0181(18) 0.0027(19) C15 0.092(3) 0.092(3) 0.057(2) -0.014(2) 0.027(2) 0.005(2) C16 0.111(4) 0.133(5) 0.049(2) 0.004(2) 0.044(2) 0.030(3) C17 0.101(4) 0.129(5) 0.077(3) 0.007(3) 0.057(3) 0.004(3) C18 0.083(3) 0.107(4) 0.078(3) 0.014(2) 0.040(2) -0.014(2) C19 0.064(2) 0.068(2) 0.0516(17) 0.0117(16) 0.0198(16) 0.0054(17) C20 0.0542(17) 0.053(2) 0.0519(16) 0.0085(14) 0.0094(14) -0.0020(14) C21 0.073(2) 0.088(3) 0.087(3) 0.002(2) 0.019(2) -0.023(2) C22 0.087(3) 0.087(3) 0.077(3) -0.016(2) 0.001(2) -0.025(2) C23 0.101(3) 0.066(2) 0.0539(19) -0.0124(18) 0.005(2) -0.004(2) C24 0.082(2) 0.060(2) 0.0475(16) -0.0088(15) 0.0183(16) -0.0069(17) C25 0.0577(18) 0.067(2) 0.0526(17) -0.0077(16) 0.0000(15) 0.0019(15) C26 0.067(2) 0.085(3) 0.0528(18) 0.0088(19) -0.0017(17) 0.0111(19) C27 0.086(3) 0.068(3) 0.063(2) 0.0155(18) 0.009(2) 0.017(2) C28 0.084(3) 0.053(2) 0.065(2) 0.0055(16) 0.009(2) 0.0029(17) C29 0.0505(17) 0.053(2) 0.0444(14) 0.0005(13) 0.0121(13) 0.0021(13) C30 0.0548(17) 0.054(2) 0.0448(15) -0.0037(14) 0.0116(13) -0.0072(14) C31 0.069(2) 0.059(2) 0.0605(19) -0.0048(16) 0.0054(17) -0.0085(16) C32 0.084(3) 0.075(3) 0.064(2) -0.018(2) 0.004(2) -0.021(2) C33 0.074(2) 0.096(3) 0.0519(19) -0.005(2) -0.0074(18) -0.006(2) C34 0.072(2) 0.079(3) 0.0499(17) -0.0021(17) -0.0024(17) 0.0028(19) C35 0.0589(18) 0.058(2) 0.0507(16) -0.0080(15) -0.0001(15) 0.0024(15) C36 0.069(2) 0.070(2) 0.0551(18) -0.0244(17) 0.0045(16) 0.0004(18) C37 0.073(2) 0.071(3) 0.061(2) -0.0151(18) 0.0191(18) 0.0075(18) C38 0.0533(18) 0.064(2) 0.0601(18) -0.0087(17) 0.0119(15) 0.0122(16) C39 0.0485(16) 0.0481(18) 0.0457(14) 0.0023(13) 0.0063(13) 0.0028(13) C40 0.0441(15) 0.0510(19) 0.0442(14) 0.0038(13) 0.0073(13) -0.0007(13) C41 0.0514(18) 0.071(2) 0.0584(18) 0.0007(17) 0.0017(15) 0.0092(16) C42 0.056(2) 0.083(3) 0.0559(19) 0.0100(19) -0.0087(17) -0.0006(18) C43 0.061(2) 0.069(2) 0.0497(17) -0.0042(16) -0.0037(16) -0.0145(17) C44 0.0593(19) 0.059(2) 0.0573(18) -0.0108(16) 0.0036(16) -0.0010(16) C45 0.064(2) 0.075(3) 0.062(2) -0.0075(18) 0.0243(17) 0.0059(18) C46 0.074(3) 0.099(4) 0.067(2) -0.022(2) 0.024(2) 0.003(2) C47 0.101(4) 0.087(4) 0.091(3) -0.042(3) 0.032(3) 0.002(2) C48 0.091(3) 0.058(3) 0.097(3) -0.012(2) 0.024(3) 0.001(2) C49 0.0546(18) 0.051(2) 0.0603(18) -0.0093(16) 0.0107(15) 0.0029(15) C50 0.0524(17) 0.055(2) 0.0590(18) 0.0018(16) 0.0078(15) -0.0003(15) C51 0.095(3) 0.059(3) 0.081(3) 0.010(2) 0.020(2) -0.003(2) C52 0.105(4) 0.072(3) 0.091(3) 0.027(2) 0.027(3) 0.000(2) C53 0.080(3) 0.097(4) 0.060(2) 0.016(2) 0.026(2) -0.005(2) C54 0.069(2) 0.072(3) 0.0604(19) 0.0046(18) 0.0211(18) 0.0005(18) C55 0.061(2) 0.072(2) 0.0559(18) 0.0124(17) 0.0080(16) 0.0076(17) C56 0.091(3) 0.073(3) 0.057(2) 0.0158(18) 0.013(2) 0.008(2) C57 0.092(3) 0.071(3) 0.082(3) 0.014(2) 0.022(2) -0.013(2) C58 0.071(2) 0.075(3) 0.068(2) 0.006(2) 0.0117(19) -0.0113(19) C59 0.0520(17) 0.053(2) 0.0502(16) -0.0031(14) 0.0113(14) -0.0009(14) C60 0.0519(17) 0.056(2) 0.0464(15) -0.0075(14) 0.0091(14) 0.0027(14) C61 0.0512(18) 0.094(3) 0.062(2) -0.006(2) 0.0100(16) -0.0115(18) C62 0.0449(18) 0.117(4) 0.065(2) -0.007(2) -0.0038(17) 0.005(2) C63 0.059(2) 0.092(3) 0.0555(19) 0.0054(19) -0.0014(17) 0.021(2) C64 0.0557(18) 0.064(2) 0.0537(17) 0.0077(16) 0.0054(15) 0.0103(15) O1 0.086(2) 0.071(2) 0.211(4) -0.022(2) 0.049(2) -0.0015(16) O2 0.094(2) 0.074(2) 0.097(2) -0.0190(16) 0.0186(17) -0.0090(15) O3 0.102(3) 0.070(2) 0.318(7) -0.015(3) 0.093(4) 0.0012(19) O4 0.175(4) 0.109(3) 0.113(3) -0.012(2) 0.013(3) -0.015(3) O5 0.097(2) 0.084(2) 0.153(3) -0.002(2) -0.036(2) -0.0079(18) O6 0.129(3) 0.106(3) 0.292(6) 0.020(4) 0.088(4) -0.009(3) O7 0.125(3) 0.067(2) 0.129(3) 0.0196(19) 0.029(2) -0.0038(18) O8 0.084(2) 0.072(2) 0.322(8) -0.018(3) 0.075(4) 0.0009(17) O9 0.126(3) 0.086(2) 0.120(3) -0.015(2) 0.065(2) -0.018(2) O10 0.159(4) 0.233(6) 0.176(4) 0.058(4) 0.051(4) 0.007(4) C1 0.040(7) 0.082(11) 0.048(5) -0.019(6) 0.009(5) -0.024(6) N1 0.088(9) 0.086(12) 0.119(10) 0.018(7) 0.014(7) -0.010(7) N2 0.104(15) 0.089(13) 0.072(10) -0.035(9) -0.016(8) -0.006(10) N3 0.053(8) 0.157(16) 0.065(8) -0.041(9) 0.002(6) 0.024(10) N4 0.039(9) 0.074(5) 0.065(6) 0.004(4) 0.010(6) -0.024(6) N5 0.056(6) 0.050(6) 0.066(4) 0.004(4) 0.018(4) 0.002(4) N6 0.068(5) 0.057(5) 0.057(4) -0.004(4) 0.020(3) -0.002(4) C2 0.067(6) 0.029(9) 0.054(6) 0.002(5) 0.011(4) -0.005(6) N7 0.102(9) 0.063(6) 0.078(8) 0.013(5) 0.032(6) 0.019(6) N8 0.097(7) 0.061(6) 0.069(6) -0.003(5) 0.040(5) 0.005(5) N9 0.074(9) 0.061(8) 0.138(13) 0.022(7) 0.039(7) 0.008(5) N10 0.084(9) 0.054(8) 0.103(7) 0.024(7) 0.034(6) 0.022(7) C1' 0.023(6) 0.040(5) 0.044(4) -0.011(4) 0.006(5) -0.007(5) N1' 0.052(6) 0.032(5) 0.061(4) 0.010(3) 0.019(4) 0.005(3) N2' 0.049(7) 0.068(9) 0.091(10) 0.022(7) 0.023(6) 0.026(6) N3' 0.040(5) 0.079(7) 0.055(6) -0.008(5) 0.010(4) 0.009(4) N4' 0.035(8) 0.092(7) 0.055(4) -0.006(4) 0.014(5) -0.019(6) N5' 0.049(3) 0.052(4) 0.055(3) 0.008(3) 0.020(3) 0.002(4) N6' 0.050(5) 0.046(5) 0.060(4) 0.009(4) 0.023(3) 0.006(4) C2' 0.052(5) 0.034(7) 0.051(5) -0.003(5) 0.024(4) -0.008(5) N7' 0.073(6) 0.088(8) 0.055(5) 0.021(4) 0.035(4) 0.029(5) N8' 0.077(6) 0.070(8) 0.066(6) -0.004(5) 0.018(4) 0.032(6) N9' 0.069(9) 0.071(8) 0.080(7) 0.021(5) 0.022(5) 0.028(6) N10' 0.065(5) 0.041(8) 0.093(6) 0.019(7) 0.031(5) 0.017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N25 2.083(3) . ? Ni1 N24 2.085(3) . ? Ni1 N21 2.086(3) . ? Ni1 N26 2.086(3) . ? Ni1 N22 2.089(3) . ? Ni1 N23 2.095(3) . ? Ni2 N30 2.089(3) . ? Ni2 N29 2.089(3) . ? Ni2 N31 2.092(3) . ? Ni2 N27 2.092(3) . ? Ni2 N28 2.094(2) . ? Ni2 N32 2.095(3) . ? N11 C3 1.294(5) . ? N11 N12 1.309(5) . ? N12 N13 1.291(5) . ? N13 N14 1.330(5) . ? N14 C3 1.307(5) . ? N15 N16 1.252(6) . ? N15 C3 1.432(6) . ? N16 C4 1.430(5) . ? N17 C4 1.245(5) . ? N17 N18 1.371(5) . ? N18 N19 1.228(6) . ? N19 N20 1.326(7) . ? N20 C4 1.298(6) . ? N21 C5 1.333(4) . ? N21 C9 1.351(4) . ? N22 C14 1.332(4) . ? N22 C10 1.343(4) . ? N23 C15 1.337(5) . ? N23 C19 1.340(5) . ? N24 C24 1.336(4) . ? N24 C20 1.346(4) . ? N25 C25 1.342(4) . ? N25 C29 1.342(4) . ? N26 C30 1.343(4) . ? N26 C34 1.353(4) . ? N27 C35 1.332(4) . ? N27 C39 1.348(4) . ? N28 C44 1.329(4) . ? N28 C40 1.355(4) . ? N29 C49 1.334(5) . ? N29 C45 1.336(4) . ? N30 C50 1.345(5) . ? N30 C54 1.346(5) . ? N31 C55 1.335(4) . ? N31 C59 1.352(4) . ? N32 C60 1.333(4) . ? N32 C64 1.336(4) . ? C5 C6 1.370(5) . ? C5 H5 0.9300 . ? C6 C7 1.371(6) . ? C6 H6 0.9300 . ? C7 C8 1.374(5) . ? C7 H7 0.9300 . ? C8 C9 1.383(5) . ? C8 H8 0.9300 . ? C9 C10 1.475(4) . ? C10 C11 1.389(5) . ? C11 C12 1.372(6) . ? C11 H11 0.9300 . ? C12 C13 1.385(7) . ? C12 H12 0.9300 . ? C13 C14 1.383(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.377(7) . ? C15 H15 0.9300 . ? C16 C17 1.329(7) . ? C16 H16 0.9300 . ? C17 C18 1.366(7) . ? C17 H17 0.9300 . ? C18 C19 1.385(5) . ? C18 H18 0.9300 . ? C19 C20 1.476(5) . ? C20 C21 1.371(5) . ? C21 C22 1.383(7) . ? C21 H21 0.9300 . ? C22 C23 1.357(7) . ? C22 H22 0.9300 . ? C23 C24 1.374(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.366(5) . ? C25 H25 0.9300 . ? C26 C27 1.358(6) . ? C26 H26 0.9300 . ? C27 C28 1.363(6) . ? C27 H27 0.9300 . ? C28 C29 1.398(5) . ? C28 H28 0.9300 . ? C29 C30 1.472(4) . ? C30 C31 1.380(5) . ? C31 C32 1.383(6) . ? C31 H31 0.9300 . ? C32 C33 1.351(6) . ? C32 H32 0.9300 . ? C33 C34 1.390(6) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.375(5) . ? C35 H35 0.9300 . ? C36 C37 1.377(5) . ? C36 H36 0.9300 . ? C37 C38 1.359(5) . ? C37 H37 0.9300 . ? C38 C39 1.393(5) . ? C38 H38 0.9300 . ? C39 C40 1.476(4) . ? C40 C41 1.379(4) . ? C41 C42 1.374(5) . ? C41 H41 0.9300 . ? C42 C43 1.356(6) . ? C42 H42 0.9300 . ? C43 C44 1.382(5) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C46 1.376(6) . ? C45 H45 0.9300 . ? C46 C47 1.355(7) . ? C46 H46 0.9300 . ? C47 C48 1.396(8) . ? C47 H47 0.9300 . ? C48 C49 1.378(5) . ? C48 H48 0.9300 . ? C49 C50 1.482(4) . ? C50 C51 1.393(6) . ? C51 C52 1.358(7) . ? C51 H51 0.9300 . ? C52 C53 1.358(7) . ? C52 H52 0.9300 . ? C53 C54 1.377(6) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C56 1.366(6) . ? C55 H55 0.9300 . ? C56 C57 1.380(6) . ? C56 H56 0.9300 . ? C57 C58 1.357(6) . ? C57 H57 0.9300 . ? C58 C59 1.379(5) . ? C58 H58 0.9300 . ? C59 C60 1.482(4) . ? C60 C61 1.395(5) . ? C61 C62 1.364(6) . ? C61 H61 0.9300 . ? C62 C63 1.356(6) . ? C62 H62 0.9300 . ? C63 C64 1.376(5) . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? O1 H1A 0.8499 . ? O1 H1B 0.8498 . ? O2 H2A 0.8499 . ? O2 H2B 0.8498 . ? O3 H3A 0.8500 . ? O3 H3B 0.8500 . ? O4 H4A 0.8500 . ? O4 H4B 0.8501 . ? O5 H5A 0.8499 . ? O5 H5B 0.8499 . ? O6 H6A 0.8502 . ? O6 H6B 0.8497 . ? O7 H7A 0.8498 . ? O7 H7B 0.8500 . ? O8 H8A 0.8500 . ? O8 H8B 0.8500 . ? O9 H9A 0.8500 . ? O9 H9B 0.8500 . ? O10 H10A 0.8500 . ? O10 H10B 0.8500 . ? C1 N4 1.330(11) . ? C1 N1 1.347(13) . ? C1 N5 1.38(2) . ? N1 N2 1.328(12) . ? N2 N3 1.293(14) . ? N3 N4 1.314(12) . ? N5 N6 1.194(14) . ? N6 C2 1.395(19) . ? C2 N10 1.308(11) . ? C2 N7 1.333(12) . ? N7 N8 1.356(12) . ? N8 N9 1.334(13) . ? N9 N10 1.320(12) . ? C1' N4' 1.336(10) . ? C1' N1' 1.351(11) . ? C1' N5' 1.433(15) . ? N1' N2' 1.324(9) . ? N2' N3' 1.300(12) . ? N3' N4' 1.311(12) . ? N5' N6' 1.263(13) . ? N6' C2' 1.384(17) . ? C2' N10' 1.313(11) . ? C2' N7' 1.321(11) . ? N7' N8' 1.340(11) . ? N8' N9' 1.330(12) . ? N9' N10' 1.330(12) . ? 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 N25 Ni1 N24 96.91(11) . . ? N25 Ni1 N21 93.06(10) . . ? N24 Ni1 N21 94.37(10) . . ? N25 Ni1 N26 78.38(9) . . ? N24 Ni1 N26 172.34(12) . . ? N21 Ni1 N26 91.93(11) . . ? N25 Ni1 N22 169.39(12) . . ? N24 Ni1 N22 90.56(10) . . ? N21 Ni1 N22 78.82(11) . . ? N26 Ni1 N22 94.93(11) . . ? N25 Ni1 N23 93.46(11) . . ? N24 Ni1 N23 78.67(11) . . ? N21 Ni1 N23 170.99(10) . . ? N26 Ni1 N23 95.47(11) . . ? N22 Ni1 N23 95.40(12) . . ? N30 Ni2 N29 78.55(9) . . ? N30 Ni2 N31 170.29(11) . . ? N29 Ni2 N31 95.32(11) . . ? N30 Ni2 N27 94.55(11) . . ? N29 Ni2 N27 168.33(10) . . ? N31 Ni2 N27 92.69(9) . . ? N30 Ni2 N28 93.62(10) . . ? N29 Ni2 N28 91.73(10) . . ? N31 Ni2 N28 94.08(10) . . ? N27 Ni2 N28 79.22(9) . . ? N30 Ni2 N32 94.36(11) . . ? N29 Ni2 N32 94.29(10) . . ? N31 Ni2 N32 78.48(10) . . ? N27 Ni2 N32 95.62(10) . . ? N28 Ni2 N32 170.82(9) . . ? C3 N11 N12 105.8(4) . . ? N13 N12 N11 109.2(4) . . ? N12 N13 N14 108.8(4) . . ? C3 N14 N13 104.6(4) . . ? N16 N15 C3 122.2(4) . . ? N15 N16 C4 122.7(4) . . ? C4 N17 N18 104.2(4) . . ? N19 N18 N17 108.9(4) . . ? N18 N19 N20 109.6(6) . . ? C4 N20 N19 104.5(4) . . ? C5 N21 C9 118.0(3) . . ? C5 N21 Ni1 127.2(2) . . ? C9 N21 Ni1 114.7(2) . . ? C14 N22 C10 118.7(3) . . ? C14 N22 Ni1 126.5(3) . . ? C10 N22 Ni1 114.7(2) . . ? C15 N23 C19 118.7(3) . . ? C15 N23 Ni1 126.8(3) . . ? C19 N23 Ni1 114.5(2) . . ? C24 N24 C20 118.6(3) . . ? C24 N24 Ni1 126.4(2) . . ? C20 N24 Ni1 115.0(2) . . ? C25 N25 C29 118.3(3) . . ? C25 N25 Ni1 126.8(2) . . ? C29 N25 Ni1 114.39(19) . . ? C30 N26 C34 118.2(3) . . ? C30 N26 Ni1 115.42(19) . . ? C34 N26 Ni1 126.3(3) . . ? C35 N27 C39 118.1(3) . . ? C35 N27 Ni2 127.4(2) . . ? C39 N27 Ni2 114.5(2) . . ? C44 N28 C40 118.2(3) . . ? C44 N28 Ni2 127.7(2) . . ? C40 N28 Ni2 113.90(19) . . ? C49 N29 C45 118.4(3) . . ? C49 N29 Ni2 115.0(2) . . ? C45 N29 Ni2 125.9(3) . . ? C50 N30 C54 118.2(3) . . ? C50 N30 Ni2 114.8(2) . . ? C54 N30 Ni2 126.9(3) . . ? C55 N31 C59 118.2(3) . . ? C55 N31 Ni2 126.8(2) . . ? C59 N31 Ni2 114.9(2) . . ? C60 N32 C64 118.4(3) . . ? C60 N32 Ni2 115.1(2) . . ? C64 N32 Ni2 126.5(2) . . ? N11 C3 N14 111.6(4) . . ? N11 C3 N15 124.7(4) . . ? N14 C3 N15 122.6(4) . . ? N17 C4 N20 112.8(4) . . ? N17 C4 N16 131.4(4) . . ? N20 C4 N16 115.8(4) . . ? N21 C5 C6 123.6(3) . . ? N21 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C5 C6 C7 118.9(3) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C6 C7 C8 118.2(4) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 120.9 . . ? C7 C8 C9 120.6(4) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? N21 C9 C8 120.7(3) . . ? N21 C9 C10 115.7(3) . . ? C8 C9 C10 123.6(3) . . ? N22 C10 C11 121.6(3) . . ? N22 C10 C9 115.9(3) . . ? C11 C10 C9 122.5(3) . . ? C12 C11 C10 119.7(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 118.3(4) . . ? C11 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? C14 C13 C12 119.2(4) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? N22 C14 C13 122.4(4) . . ? N22 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? N23 C15 C16 121.7(5) . . ? N23 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C17 C16 C15 119.6(4) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.1(4) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C19 118.9(5) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? N23 C19 C18 121.0(4) . . ? N23 C19 C20 116.3(3) . . ? C18 C19 C20 122.7(4) . . ? N24 C20 C21 120.1(3) . . ? N24 C20 C19 115.5(3) . . ? C21 C20 C19 124.3(3) . . ? C20 C21 C22 121.2(4) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 118.1(4) . . ? C23 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? C22 C23 C24 118.9(4) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? N24 C24 C23 123.2(4) . . ? N24 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? N25 C25 C26 123.0(3) . . ? N25 C25 H25 118.5 . . ? C26 C25 H25 118.5 . . ? C27 C26 C25 118.5(3) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C26 C27 C28 120.3(4) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C29 118.7(4) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? N25 C29 C28 121.1(3) . . ? N25 C29 C30 116.4(3) . . ? C28 C29 C30 122.5(3) . . ? N26 C30 C31 122.0(3) . . ? N26 C30 C29 114.8(3) . . ? C31 C30 C29 123.2(3) . . ? C30 C31 C32 119.4(4) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C33 C32 C31 118.9(4) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C32 C33 C34 119.9(3) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? N26 C34 C33 121.5(4) . . ? N26 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? N27 C35 C36 123.6(3) . . ? N27 C35 H35 118.2 . . ? C36 C35 H35 118.2 . . ? C35 C36 C37 118.1(3) . . ? C35 C36 H36 121.0 . . ? C37 C36 H36 121.0 . . ? C38 C37 C36 119.6(3) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 119.6(3) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? N27 C39 C38 121.1(3) . . ? N27 C39 C40 115.9(3) . . ? C38 C39 C40 122.9(3) . . ? N28 C40 C41 120.5(3) . . ? N28 C40 C39 116.4(2) . . ? C41 C40 C39 123.1(3) . . ? C42 C41 C40 120.3(3) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C43 C42 C41 119.2(3) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C42 C43 C44 118.3(3) . . ? C42 C43 H43 120.8 . . ? C44 C43 H43 120.8 . . ? N28 C44 C43 123.5(4) . . ? N28 C44 H44 118.3 . . ? C43 C44 H44 118.3 . . ? N29 C45 C46 123.1(4) . . ? N29 C45 H45 118.4 . . ? C46 C45 H45 118.4 . . ? C47 C46 C45 118.7(4) . . ? C47 C46 H46 120.7 . . ? C45 C46 H46 120.7 . . ? C46 C47 C48 119.1(4) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? C49 C48 C47 119.0(4) . . ? C49 C48 H48 120.5 . . ? C47 C48 H48 120.5 . . ? N29 C49 C48 121.7(4) . . ? N29 C49 C50 115.8(3) . . ? C48 C49 C50 122.5(4) . . ? N30 C50 C51 121.3(4) . . ? N30 C50 C49 115.5(3) . . ? C51 C50 C49 123.2(4) . . ? C52 C51 C50 119.4(4) . . ? C52 C51 H51 120.3 . . ? C50 C51 H51 120.3 . . ? C51 C52 C53 119.6(4) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C52 C53 C54 119.4(4) . . ? C52 C53 H53 120.3 . . ? C54 C53 H53 120.3 . . ? N30 C54 C53 122.1(4) . . ? N30 C54 H54 119.0 . . ? C53 C54 H54 119.0 . . ? N31 C55 C56 123.2(4) . . ? N31 C55 H55 118.4 . . ? C56 C55 H55 118.4 . . ? C55 C56 C57 118.6(4) . . ? C55 C56 H56 120.7 . . ? C57 C56 H56 120.7 . . ? C58 C57 C56 118.6(4) . . ? C58 C57 H57 120.7 . . ? C56 C57 H57 120.7 . . ? C57 C58 C59 120.8(4) . . ? C57 C58 H58 119.6 . . ? C59 C58 H58 119.6 . . ? N31 C59 C58 120.5(3) . . ? N31 C59 C60 115.3(3) . . ? C58 C59 C60 124.1(3) . . ? N32 C60 C61 121.6(3) . . ? N32 C60 C59 116.1(3) . . ? C61 C60 C59 122.2(3) . . ? C62 C61 C60 118.7(4) . . ? C62 C61 H61 120.6 . . ? C60 C61 H61 120.6 . . ? C63 C62 C61 119.9(3) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C62 C63 C64 118.8(4) . . ? C62 C63 H63 120.6 . . ? C64 C63 H63 120.6 . . ? N32 C64 C63 122.5(4) . . ? N32 C64 H64 118.7 . . ? C63 C64 H64 118.7 . . ? H1A O1 H1B 108.4 . . ? H2A O2 H2B 108.3 . . ? H3A O3 H3B 108.4 . . ? H4A O4 H4B 107.9 . . ? H5A O5 H5B 108.4 . . ? H6A O6 H6B 108.8 . . ? H7A O7 H7B 108.8 . . ? H8A O8 H8B 108.4 . . ? H9A O9 H9B 108.3 . . ? H10A O10 H10B 108.5 . . ? N4 C1 N1 113.1(12) . . ? N4 C1 N5 128.9(17) . . ? N1 C1 N5 117.3(18) . . ? N2 N1 C1 102.1(12) . . ? N3 N2 N1 110.7(12) . . ? N2 N3 N4 110.9(12) . . ? N3 N4 C1 103.1(11) . . ? N6 N5 C1 117.0(17) . . ? N5 N6 C2 116.8(16) . . ? N10 C2 N7 110.9(11) . . ? N10 C2 N6 124.3(15) . . ? N7 C2 N6 124.3(13) . . ? C2 N7 N8 106.8(10) . . ? N9 N8 N7 105.3(11) . . ? N10 N9 N8 111.5(12) . . ? C2 N10 N9 105.6(12) . . ? N4' C1' N1' 112.1(9) . . ? N4' C1' N5' 119.0(11) . . ? N1' C1' N5' 128.9(11) . . ? N2' N1' C1' 102.6(8) . . ? N3' N2' N1' 111.0(9) . . ? N2' N3' N4' 110.2(12) . . ? N3' N4' C1' 104.1(11) . . ? N6' N5' C1' 113.2(12) . . ? N5' N6' C2' 112.3(13) . . ? N10' C2' N7' 111.8(11) . . ? N10' C2' N6' 130.7(11) . . ? N7' C2' N6' 117.2(12) . . ? C2' N7' N8' 105.3(11) . . ? N9' N8' N7' 108.4(11) . . ? N10' N9' N8' 108.8(10) . . ? C2' N10' N9' 105.8(10) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.721 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.048 # Attachment '- Zn1.cif' data_Zn1 _database_code_depnum_ccdc_archive 'CCDC 788078' #TrackingRef '- Zn1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H36 N12 O9 Zn' _chemical_formula_weight 786.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.7733(8) _cell_length_b 13.8712(4) _cell_length_c 22.7063(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.235(2) _cell_angle_gamma 90.00 _cell_volume 7428.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6215 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.520 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.242 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.128 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.729 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.847 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 29622 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8542 _reflns_number_gt 5131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0759P)^2^+3.2623P] 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 refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00060(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8534 _refine_ls_number_parameters 479 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1643 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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 Zn1 Zn 0.335335(16) 0.66597(3) 0.755704(16) 0.05369(16) Uani 1 1 d . . . N1 N 0.35419(11) 0.53441(19) 0.80428(12) 0.0565(7) Uani 1 1 d . . . N2 N 0.38460(11) 0.5850(2) 0.69950(12) 0.0567(7) Uani 1 1 d . . . N3 N 0.27448(11) 0.71833(18) 0.81137(11) 0.0530(6) Uani 1 1 d . . . N4 N 0.25463(12) 0.6186(2) 0.71071(12) 0.0597(7) Uani 1 1 d . . . N5 N 0.40561(11) 0.7460(2) 0.80101(11) 0.0547(7) Uani 1 1 d . . . N6 N 0.33508(12) 0.7977(2) 0.70516(12) 0.0601(7) Uani 1 1 d . . . N7 N 0.42617(11) 0.1293(2) 0.49873(14) 0.0616(7) Uani 1 1 d . . . N8 N 0.37143(12) 0.1484(2) 0.50054(14) 0.0618(7) Uani 1 1 d . . . N9 N 0.34400(11) 0.0676(2) 0.50631(13) 0.0593(7) Uani 1 1 d . . . N10 N 0.38015(11) -0.00582(19) 0.50829(12) 0.0564(7) Uani 1 1 d . . . N11 N 0.47834(10) -0.02341(17) 0.50416(12) 0.0502(6) Uani 1 1 d . . . N12 N 0.51715(13) 0.1653(2) 0.82926(18) 0.0751(9) Uani 1 1 d . . . C1 C 0.33793(16) 0.5124(3) 0.85675(16) 0.0675(9) Uani 1 1 d . . . H1 H 0.3164 0.5570 0.8748 0.081 Uiso 1 1 calc R . . C2 C 0.35156(18) 0.4267(3) 0.88526(17) 0.0780(11) Uani 1 1 d . . . H2 H 0.3396 0.4134 0.9219 0.094 Uiso 1 1 calc R . . C3 C 0.3828(2) 0.3618(3) 0.8587(2) 0.0832(12) Uani 1 1 d . . . H3 H 0.3923 0.3030 0.8770 0.100 Uiso 1 1 calc R . . C4 C 0.40064(17) 0.3831(3) 0.80485(17) 0.0737(10) Uani 1 1 d . . . H4 H 0.4226 0.3394 0.7866 0.088 Uiso 1 1 calc R . . C5 C 0.38532(14) 0.4701(2) 0.77832(15) 0.0549(8) Uani 1 1 d . . . C6 C 0.40225(14) 0.4987(2) 0.71995(15) 0.0558(8) Uani 1 1 d . . . C7 C 0.43377(17) 0.4391(3) 0.68804(19) 0.0790(11) Uani 1 1 d . . . H7 H 0.4461 0.3792 0.7030 0.095 Uiso 1 1 calc R . . C8 C 0.4466(2) 0.4698(4) 0.6339(2) 0.0940(14) Uani 1 1 d . . . H8 H 0.4678 0.4306 0.6119 0.113 Uiso 1 1 calc R . . C9 C 0.42831(19) 0.5576(4) 0.61223(18) 0.0857(12) Uani 1 1 d . . . H9 H 0.4363 0.5787 0.5753 0.103 Uiso 1 1 calc R . . C10 C 0.39778(16) 0.6140(3) 0.64656(16) 0.0710(10) Uani 1 1 d . . . H10 H 0.3858 0.6746 0.6326 0.085 Uiso 1 1 calc R . . C11 C 0.28722(17) 0.7648(3) 0.86303(16) 0.0669(9) Uani 1 1 d . . . H11 H 0.3252 0.7763 0.8767 0.080 Uiso 1 1 calc R . . C12 C 0.24693(18) 0.7959(3) 0.89641(17) 0.0775(11) Uani 1 1 d . . . H12 H 0.2572 0.8281 0.9321 0.093 Uiso 1 1 calc R . . C13 C 0.19099(19) 0.7787(3) 0.87620(18) 0.0815(12) Uani 1 1 d . . . H13 H 0.1627 0.7990 0.8981 0.098 Uiso 1 1 calc R . . C14 C 0.17713(17) 0.7307(3) 0.82306(17) 0.0719(10) Uani 1 1 d . . . H14 H 0.1394 0.7185 0.8088 0.086 Uiso 1 1 calc R . . C15 C 0.21976(14) 0.7012(2) 0.79141(14) 0.0513(7) Uani 1 1 d . . . C16 C 0.20861(14) 0.6478(2) 0.73450(14) 0.0503(7) Uani 1 1 d . . . C17 C 0.15461(15) 0.6298(3) 0.70698(16) 0.0639(9) Uani 1 1 d . . . H17 H 0.1232 0.6503 0.7241 0.077 Uiso 1 1 calc R . . C18 C 0.14792(17) 0.5812(3) 0.65403(18) 0.0779(11) Uani 1 1 d . . . H18 H 0.1118 0.5693 0.6345 0.094 Uiso 1 1 calc R . . C19 C 0.19455(19) 0.5503(3) 0.63010(18) 0.0872(13) Uani 1 1 d . . . H19 H 0.1907 0.5165 0.5944 0.105 Uiso 1 1 calc R . . C20 C 0.24710(17) 0.5698(3) 0.65949(17) 0.0780(11) Uani 1 1 d . . . H20 H 0.2789 0.5483 0.6432 0.094 Uiso 1 1 calc R . . C21 C 0.43941(15) 0.7167(3) 0.84910(16) 0.0658(9) Uani 1 1 d . . . H21 H 0.4345 0.6550 0.8637 0.079 Uiso 1 1 calc R . . C22 C 0.48097(17) 0.7740(3) 0.87775(17) 0.0770(11) Uani 1 1 d . . . H22 H 0.5038 0.7519 0.9113 0.092 Uiso 1 1 calc R . . C23 C 0.48836(18) 0.8641(4) 0.85625(19) 0.0807(12) Uani 1 1 d . . . H23 H 0.5161 0.9045 0.8753 0.097 Uiso 1 1 calc R . . C24 C 0.45489(17) 0.8946(3) 0.80666(18) 0.0732(10) Uani 1 1 d . . . H24 H 0.4600 0.9556 0.7912 0.088 Uiso 1 1 calc R . . C25 C 0.41325(14) 0.8342(2) 0.77953(15) 0.0546(8) Uani 1 1 d . . . C26 C 0.37534(15) 0.8620(2) 0.72554(15) 0.0567(8) Uani 1 1 d . . . C27 C 0.38053(19) 0.9481(3) 0.69672(18) 0.0767(11) Uani 1 1 d . . . H27 H 0.4084 0.9921 0.7112 0.092 Uiso 1 1 calc R . . C28 C 0.3440(2) 0.9686(3) 0.6460(2) 0.0919(14) Uani 1 1 d . . . H28 H 0.3470 1.0267 0.6261 0.110 Uiso 1 1 calc R . . C29 C 0.3039(2) 0.9031(4) 0.62548(19) 0.0882(13) Uani 1 1 d . . . H29 H 0.2792 0.9154 0.5912 0.106 Uiso 1 1 calc R . . C30 C 0.30019(17) 0.8189(3) 0.65596(17) 0.0740(11) Uani 1 1 d . . . H30 H 0.2723 0.7746 0.6419 0.089 Uiso 1 1 calc R . . C31 C 0.42981(12) 0.0349(2) 0.50347(13) 0.0459(7) Uani 1 1 d . . . O1 O 0.4964(3) 0.1024(4) 0.8508(2) 0.220(3) Uani 1 1 d . . . O2 O 0.5024(3) 0.2418(3) 0.8409(2) 0.205(3) Uani 1 1 d . . . O3 O 0.55052(19) 0.1526(5) 0.7968(3) 0.217(3) Uani 1 1 d . . . O4 O 0.51673(11) 0.25403(19) 0.53979(13) 0.0867(8) Uani 1 1 d D . . H5 H 0.5229 0.2432 0.5761 0.104 Uiso 1 1 d RD . . H6 H 0.4895 0.2197 0.5269 0.104 Uiso 1 1 d RD . . O5 O 0.35934(13) 0.3586(2) 0.48612(16) 0.0988(10) Uani 1 1 d D . . H15 H 0.3512 0.4093 0.4618 0.119 Uiso 1 1 d RD . . H16 H 0.3682 0.3013 0.4711 0.119 Uiso 1 1 d RD . . O6 O 0.47035(14) 0.4171(2) 0.48441(14) 0.0959(9) Uani 1 1 d D . . H26 H 0.4467 0.4142 0.4503 0.115 Uiso 1 1 d RD . . H25 H 0.5039 0.3864 0.4876 0.115 Uiso 1 1 d RD . . O7 O 0.61058(12) 0.2191(2) 0.48062(17) 0.1060(11) Uani 1 1 d D . . H31 H 0.6245 0.2143 0.5164 0.127 Uiso 1 1 d RD . . H32 H 0.6104 0.1612 0.4707 0.127 Uiso 1 1 d RD . . O8 O 0.22498(11) 0.0156(2) 0.49661(16) 0.1040(11) Uani 1 1 d D . . H33 H 0.2583 -0.0158 0.5031 0.125 Uiso 1 1 d RD . . H34 H 0.1950 -0.0125 0.4752 0.125 Uiso 1 1 d RD . . O9 O 0.21019(14) 0.8203(2) 0.4803(2) 0.1281(14) Uani 1 1 d D . . H35 H 0.1769 0.8009 0.4691 0.154 Uiso 1 1 d RD . . H36 H 0.2127 0.8024 0.5177 0.154 Uiso 1 1 d RD . . 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 Zn1 0.0573(3) 0.0572(3) 0.0479(2) -0.00301(17) 0.01155(17) -0.00003(18) N1 0.0616(17) 0.0573(16) 0.0531(16) 0.0001(13) 0.0171(13) -0.0033(13) N2 0.0611(17) 0.0609(17) 0.0515(15) -0.0019(13) 0.0199(13) -0.0012(13) N3 0.0599(17) 0.0532(15) 0.0468(14) -0.0084(12) 0.0105(12) -0.0006(13) N4 0.0637(17) 0.0645(17) 0.0518(15) -0.0159(14) 0.0107(13) -0.0046(14) N5 0.0526(16) 0.0611(17) 0.0501(15) 0.0025(13) 0.0054(12) 0.0010(13) N6 0.0654(18) 0.0641(17) 0.0507(16) 0.0075(14) 0.0072(14) 0.0075(15) N7 0.0467(16) 0.0501(15) 0.089(2) 0.0061(15) 0.0127(14) 0.0001(13) N8 0.0473(16) 0.0582(17) 0.079(2) 0.0028(14) 0.0055(14) 0.0049(13) N9 0.0434(15) 0.0643(18) 0.0701(18) 0.0004(14) 0.0070(13) 0.0008(13) N10 0.0452(15) 0.0547(16) 0.0696(18) 0.0008(13) 0.0085(13) -0.0016(12) N11 0.0422(14) 0.0482(15) 0.0603(16) 0.0046(12) 0.0062(12) -0.0027(11) N12 0.0539(18) 0.0526(18) 0.123(3) -0.0050(18) 0.0276(19) 0.0015(15) C1 0.081(3) 0.068(2) 0.057(2) 0.0028(18) 0.0249(18) -0.0022(19) C2 0.089(3) 0.087(3) 0.059(2) 0.015(2) 0.017(2) -0.005(2) C3 0.096(3) 0.075(3) 0.078(3) 0.019(2) 0.007(2) 0.003(2) C4 0.082(3) 0.067(2) 0.072(2) 0.003(2) 0.011(2) 0.011(2) C5 0.0530(19) 0.0544(19) 0.0578(19) -0.0033(16) 0.0090(15) -0.0032(15) C6 0.0546(19) 0.058(2) 0.0567(19) -0.0100(16) 0.0146(15) -0.0053(16) C7 0.083(3) 0.076(3) 0.083(3) -0.011(2) 0.032(2) 0.009(2) C8 0.104(3) 0.101(3) 0.087(3) -0.018(3) 0.051(3) 0.011(3) C9 0.097(3) 0.102(3) 0.066(2) -0.007(2) 0.043(2) 0.000(3) C10 0.078(2) 0.079(3) 0.061(2) 0.0024(19) 0.0289(19) 0.003(2) C11 0.072(2) 0.070(2) 0.058(2) -0.0195(18) 0.0084(18) -0.0024(19) C12 0.087(3) 0.085(3) 0.062(2) -0.029(2) 0.014(2) 0.005(2) C13 0.083(3) 0.097(3) 0.071(2) -0.024(2) 0.030(2) 0.008(2) C14 0.065(2) 0.084(3) 0.069(2) -0.017(2) 0.0156(18) 0.0070(19) C15 0.058(2) 0.0485(17) 0.0488(17) -0.0028(14) 0.0107(15) 0.0012(15) C16 0.0556(19) 0.0485(17) 0.0475(17) -0.0029(13) 0.0090(14) -0.0054(14) C17 0.058(2) 0.067(2) 0.067(2) -0.0079(18) 0.0102(17) -0.0095(17) C18 0.070(2) 0.091(3) 0.071(2) -0.020(2) 0.001(2) -0.015(2) C19 0.089(3) 0.104(3) 0.067(2) -0.037(2) 0.002(2) -0.013(3) C20 0.076(3) 0.098(3) 0.061(2) -0.031(2) 0.0136(19) -0.006(2) C21 0.065(2) 0.074(2) 0.058(2) 0.0025(18) 0.0038(17) 0.0003(19) C22 0.062(2) 0.106(3) 0.060(2) -0.011(2) -0.0029(18) 0.002(2) C23 0.072(3) 0.101(3) 0.070(3) -0.022(2) 0.011(2) -0.025(2) C24 0.083(3) 0.072(2) 0.068(2) -0.012(2) 0.024(2) -0.017(2) C25 0.059(2) 0.0556(19) 0.0521(18) -0.0058(16) 0.0178(15) -0.0002(16) C26 0.070(2) 0.0523(18) 0.0515(19) 0.0006(15) 0.0216(16) 0.0087(16) C27 0.107(3) 0.059(2) 0.069(2) 0.0033(19) 0.028(2) 0.002(2) C28 0.139(4) 0.072(3) 0.070(3) 0.021(2) 0.035(3) 0.027(3) C29 0.104(4) 0.099(3) 0.063(2) 0.021(2) 0.012(2) 0.035(3) C30 0.073(3) 0.086(3) 0.062(2) 0.013(2) 0.0018(19) 0.008(2) C31 0.0390(16) 0.0453(16) 0.0522(17) 0.0029(13) 0.0011(13) -0.0034(13) O1 0.331(8) 0.166(5) 0.157(4) 0.021(4) 0.008(5) -0.154(5) O2 0.407(9) 0.075(2) 0.145(4) 0.011(2) 0.082(5) 0.068(4) O3 0.088(3) 0.380(9) 0.190(5) -0.069(5) 0.041(3) 0.061(4) O4 0.0806(18) 0.0750(17) 0.105(2) -0.0095(15) 0.0117(16) -0.0266(14) O5 0.103(2) 0.0604(16) 0.136(3) 0.0078(16) 0.024(2) 0.0164(15) O6 0.108(2) 0.0772(19) 0.109(2) -0.0108(16) 0.0411(19) -0.0066(17) O7 0.086(2) 0.0653(18) 0.169(3) 0.0117(19) 0.023(2) -0.0143(15) O8 0.0522(16) 0.083(2) 0.179(3) 0.028(2) 0.0237(18) 0.0033(14) O9 0.080(2) 0.102(3) 0.199(4) -0.011(2) 0.009(2) -0.0241(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.150(3) . ? Zn1 N2 2.153(3) . ? Zn1 N5 2.156(3) . ? Zn1 N6 2.157(3) . ? Zn1 N4 2.159(3) . ? Zn1 N3 2.163(2) . ? N1 C1 1.334(4) . ? N1 C5 1.342(4) . ? N2 C6 1.334(4) . ? N2 C10 1.342(4) . ? N3 C11 1.339(4) . ? N3 C15 1.344(4) . ? N4 C20 1.338(4) . ? N4 C16 1.342(4) . ? N5 C21 1.335(4) . ? N5 C25 1.339(4) . ? N6 C30 1.338(4) . ? N6 C26 1.347(4) . ? N7 C31 1.315(4) . ? N7 N8 1.334(4) . ? N8 N9 1.311(4) . ? N9 N10 1.330(4) . ? N10 C31 1.326(4) . ? N11 N11 1.252(5) 5_656 ? N11 C31 1.408(4) . ? N12 O1 1.143(5) . ? N12 O2 1.158(4) . ? N12 O3 1.163(5) . ? C1 C2 1.373(5) . ? C1 H1 0.9300 . ? C2 C3 1.356(6) . ? C2 H2 0.9300 . ? C3 C4 1.376(5) . ? C3 H3 0.9300 . ? C4 C5 1.377(5) . ? C4 H4 0.9300 . ? C5 C6 1.487(5) . ? C6 C7 1.381(5) . ? C7 C8 1.371(6) . ? C7 H7 0.9300 . ? C8 C9 1.364(6) . ? C8 H8 0.9300 . ? C9 C10 1.375(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.364(5) . ? C11 H11 0.9300 . ? C12 C13 1.372(5) . ? C12 H12 0.9300 . ? C13 C14 1.381(5) . ? C13 H13 0.9300 . ? C14 C15 1.377(5) . ? C14 H14 0.9300 . ? C15 C16 1.484(4) . ? C16 C17 1.378(5) . ? C17 C18 1.370(5) . ? C17 H17 0.9300 . ? C18 C19 1.363(6) . ? C18 H18 0.9300 . ? C19 C20 1.367(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.368(5) . ? C21 H21 0.9300 . ? C22 C23 1.361(6) . ? C22 H22 0.9300 . ? C23 C24 1.362(6) . ? C23 H23 0.9300 . ? C24 C25 1.381(5) . ? C24 H24 0.9300 . ? C25 C26 1.478(5) . ? C26 C27 1.375(5) . ? C27 C28 1.382(6) . ? C27 H27 0.9300 . ? C28 C29 1.357(6) . ? C28 H28 0.9300 . ? C29 C30 1.367(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? O4 H5 0.8319 . ? O4 H6 0.8275 . ? O5 H15 0.9002 . ? O5 H16 0.9001 . ? O6 H26 0.8999 . ? O6 H25 0.9000 . ? O7 H31 0.8406 . ? O7 H32 0.8352 . ? O8 H33 0.8998 . ? O8 H34 0.9001 . ? O9 H35 0.8438 . ? O9 H36 0.8797 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N2 76.57(10) . . ? N1 Zn1 N5 95.35(10) . . ? N2 Zn1 N5 96.00(10) . . ? N1 Zn1 N6 168.01(11) . . ? N2 Zn1 N6 95.25(10) . . ? N5 Zn1 N6 76.58(11) . . ? N1 Zn1 N4 95.73(11) . . ? N2 Zn1 N4 94.48(10) . . ? N5 Zn1 N4 166.25(11) . . ? N6 Zn1 N4 93.63(11) . . ? N1 Zn1 N3 95.56(10) . . ? N2 Zn1 N3 167.18(10) . . ? N5 Zn1 N3 94.78(10) . . ? N6 Zn1 N3 93.97(10) . . ? N4 Zn1 N3 76.05(10) . . ? C1 N1 C5 118.6(3) . . ? C1 N1 Zn1 126.0(2) . . ? C5 N1 Zn1 115.5(2) . . ? C6 N2 C10 118.9(3) . . ? C6 N2 Zn1 115.6(2) . . ? C10 N2 Zn1 125.5(2) . . ? C11 N3 C15 118.9(3) . . ? C11 N3 Zn1 125.4(2) . . ? C15 N3 Zn1 115.70(19) . . ? C20 N4 C16 118.4(3) . . ? C20 N4 Zn1 125.4(2) . . ? C16 N4 Zn1 116.0(2) . . ? C21 N5 C25 118.8(3) . . ? C21 N5 Zn1 125.7(2) . . ? C25 N5 Zn1 115.4(2) . . ? C30 N6 C26 118.7(3) . . ? C30 N6 Zn1 126.2(3) . . ? C26 N6 Zn1 115.1(2) . . ? C31 N7 N8 104.4(3) . . ? N9 N8 N7 109.5(3) . . ? N8 N9 N10 109.3(2) . . ? C31 N10 N9 104.4(3) . . ? N11 N11 C31 112.9(3) 5_656 . ? O1 N12 O2 116.2(6) . . ? O1 N12 O3 121.5(6) . . ? O2 N12 O3 122.3(6) . . ? N1 C1 C2 122.8(4) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 118.4(4) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 118.9(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.4(3) . . ? N1 C5 C6 116.1(3) . . ? C4 C5 C6 122.5(3) . . ? N2 C6 C7 121.5(3) . . ? N2 C6 C5 116.2(3) . . ? C7 C6 C5 122.3(3) . . ? C8 C7 C6 118.8(4) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 120.3(4) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 118.1(4) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 121.0 . . ? N2 C10 C9 122.5(4) . . ? N2 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? N3 C11 C12 122.8(4) . . ? N3 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C11 C12 C13 118.5(3) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C12 C13 C14 119.4(3) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 119.3(4) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.4 . . ? N3 C15 C14 121.1(3) . . ? N3 C15 C16 116.2(3) . . ? C14 C15 C16 122.7(3) . . ? N4 C16 C17 121.5(3) . . ? N4 C16 C15 115.8(3) . . ? C17 C16 C15 122.7(3) . . ? C18 C17 C16 119.1(3) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C19 C18 C17 119.6(4) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 118.8(4) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? N4 C20 C19 122.6(4) . . ? N4 C20 H20 118.7 . . ? C19 C20 H20 118.7 . . ? N5 C21 C22 122.4(4) . . ? N5 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C23 C22 C21 118.8(4) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C24 C23 C22 119.6(4) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 119.4(4) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? N5 C25 C24 121.0(3) . . ? N5 C25 C26 116.3(3) . . ? C24 C25 C26 122.7(3) . . ? N6 C26 C27 120.9(3) . . ? N6 C26 C25 116.4(3) . . ? C27 C26 C25 122.6(4) . . ? C26 C27 C28 119.4(4) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C29 C28 C27 119.2(4) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C28 C29 C30 119.1(4) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? N6 C30 C29 122.6(4) . . ? N6 C30 H30 118.7 . . ? C29 C30 H30 118.7 . . ? N7 C31 N10 112.4(3) . . ? N7 C31 N11 128.2(3) . . ? N10 C31 N11 119.4(3) . . ? H5 O4 H6 106.2 . . ? H15 O5 H16 120.0 . . ? H26 O6 H25 120.0 . . ? H31 O7 H32 99.9 . . ? H33 O8 H34 120.0 . . ? H35 O9 H36 98.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.800 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.056 # Attachment '- Zn2.cif' data_Zn2 _database_code_depnum_ccdc_archive 'CCDC 788079' #TrackingRef '- Zn2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H30 N26 O2 Zn' _chemical_formula_weight 611.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pcca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 23.7645(6) _cell_length_b 7.2375(2) _cell_length_c 14.5854(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2508.62(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3059 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 26.500 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.192 _exptl_crystal_size_min 0.126 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 1.047 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.786 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11035 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.50 _reflns_number_total 2603 _reflns_number_gt 2001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+0.8181P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2582 _refine_ls_number_parameters 206 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Zn1 Zn 0.5000 0.71384(5) 1.2500 0.02933(12) Uani 1 2 d S . . C1 C 0.67997(8) 0.7453(3) 1.18755(14) 0.0290(4) Uani 1 1 d . . . C2 C 0.82680(8) 0.7770(3) 1.17434(14) 0.0299(4) Uani 1 1 d . . . C3 C 0.44722(8) 0.6126(3) 1.07632(13) 0.0324(5) Uani 1 1 d . . . H3A H 0.4086 0.6275 1.0966 0.039 Uiso 1 1 calc R . . H3B H 0.4470 0.5398 1.0205 0.039 Uiso 1 1 calc R . . C4 C 0.47282(9) 0.8001(3) 1.05742(13) 0.0337(5) Uani 1 1 d . . . H4A H 0.5090 0.7847 1.0277 0.040 Uiso 1 1 calc R . . H4B H 0.4485 0.8690 1.0163 0.040 Uiso 1 1 calc R . . N1 N 0.65993(7) 0.7173(3) 1.10346(12) 0.0423(5) Uani 1 1 d . . . N2 N 0.60439(7) 0.7019(3) 1.11509(12) 0.0438(5) Uani 1 1 d . . . N3 N 0.59263(7) 0.7212(2) 1.20282(12) 0.0315(4) Uani 1 1 d . . . N4 N 0.63969(7) 0.7490(2) 1.25033(11) 0.0327(4) Uani 1 1 d . . . N5 N 0.73648(7) 0.7634(2) 1.21393(12) 0.0335(4) Uani 1 1 d . . . N6 N 0.77009(7) 0.7662(2) 1.14746(12) 0.0333(4) Uani 1 1 d . . . N7 N 0.86639(7) 0.7997(3) 1.11093(12) 0.0374(4) Uani 1 1 d . . . N8 N 0.91458(7) 0.8017(3) 1.15800(13) 0.0403(4) Uani 1 1 d . . . N9 N 0.90355(8) 0.7796(3) 1.24615(12) 0.0390(4) Uani 1 1 d . . . N10 N 0.84802(8) 0.7640(3) 1.25815(11) 0.0358(4) Uani 1 1 d . . . N11 N 0.47986(6) 0.5157(2) 1.14746(10) 0.0300(4) Uani 1 1 d . . . H11A H 0.5115 0.4678 1.1233 0.036 Uiso 1 1 calc R . . H11B H 0.4594 0.4231 1.1717 0.036 Uiso 1 1 calc R . . N12 N 0.48012(7) 0.9041(2) 1.14388(10) 0.0299(4) Uani 1 1 d . . . H12A H 0.4482 0.9651 1.1577 0.036 Uiso 1 1 calc R . . H12B H 0.5080 0.9873 1.1377 0.036 Uiso 1 1 calc R . . C5 C 0.7281(2) 0.5388(7) 0.9547(4) 0.0475(14) Uani 0.50 1 d P . 1 H5A H 0.7059 0.4667 0.9130 0.057 Uiso 0.50 1 d PR . 1 H5B H 0.7129 0.5155 1.0146 0.057 Uiso 0.50 1 d PR . 1 N13 N 0.7131(8) 0.727(3) 0.9283(12) 0.025(3) Uani 0.50 1 d P A 1 H13A H 0.6920 0.7368 0.8774 0.030 Uiso 0.50 1 d PR A 1 H13B H 0.7441 0.7975 0.9222 0.030 Uiso 0.50 1 d PR A 1 H13F H 0.695(2) 0.769(7) 0.968(4) 0.030 Uiso 0.50 1 d P B 1 C5' C 0.7265(2) 0.5376(7) 0.8990(4) 0.0425(13) Uani 0.50 1 d P A -1 H5'A H 0.7103 0.5162 0.8397 0.051 Uiso 0.50 1 d PR A -1 H5'B H 0.7043 0.4697 0.9426 0.051 Uiso 0.50 1 d PR A -1 N13' N 0.7185(9) 0.739(3) 0.9288(13) 0.037(4) Uani 0.50 1 d P A -1 H13E H 0.6976 0.7458 0.9802 0.044 Uiso 0.50 1 d PR A -1 H13C H 0.7012 0.7977 0.8824 0.044 Uiso 0.50 1 d PR A -1 H13D H 0.7524 0.7909 0.9378 0.044 Uiso 0.50 1 d PR A -1 O1 O 0.82413(7) 0.9010(2) 0.93024(12) 0.0401(4) Uani 1 1 d D . . H9 H 0.8411(11) 0.875(4) 0.9775(12) 0.077(10) Uiso 1 1 d D . . H10 H 0.8408(11) 0.864(4) 0.8869(12) 0.067(10) Uiso 1 1 d 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 Zn1 0.0315(2) 0.0347(2) 0.02171(17) 0.000 -0.00404(13) 0.000 C1 0.0203(9) 0.0392(12) 0.0275(10) 0.0006(8) 0.0010(8) -0.0014(8) C2 0.0220(10) 0.0374(11) 0.0305(11) -0.0001(8) 0.0005(8) -0.0009(8) C3 0.0243(10) 0.0459(13) 0.0270(9) -0.0063(9) -0.0031(8) -0.0009(8) C4 0.0271(11) 0.0510(13) 0.0229(10) 0.0038(9) -0.0024(8) 0.0002(9) N1 0.0198(9) 0.0785(14) 0.0286(9) -0.0018(9) 0.0023(7) -0.0037(9) N2 0.0224(9) 0.0778(15) 0.0313(9) -0.0039(9) 0.0008(8) -0.0028(9) N3 0.0211(8) 0.0434(10) 0.0302(9) -0.0009(8) 0.0013(7) -0.0010(7) N4 0.0213(9) 0.0488(11) 0.0281(9) -0.0006(8) 0.0013(7) -0.0018(7) N5 0.0220(9) 0.0490(11) 0.0295(9) 0.0007(8) 0.0008(8) -0.0020(7) N6 0.0212(8) 0.0486(11) 0.0300(9) 0.0004(8) 0.0022(7) -0.0021(7) N7 0.0222(9) 0.0592(12) 0.0309(9) 0.0022(8) 0.0023(8) -0.0024(8) N8 0.0237(9) 0.0574(12) 0.0400(10) 0.0027(9) 0.0006(8) -0.0015(8) N9 0.0239(9) 0.0537(11) 0.0392(10) 0.0026(9) -0.0035(8) -0.0017(8) N10 0.0243(9) 0.0525(11) 0.0308(9) 0.0013(8) -0.0018(7) -0.0013(7) N11 0.0243(8) 0.0368(9) 0.0290(8) -0.0024(7) 0.0035(7) 0.0006(7) N12 0.0240(8) 0.0356(9) 0.0301(8) 0.0029(7) 0.0005(7) -0.0007(7) C5 0.044(3) 0.033(3) 0.065(3) 0.004(3) 0.023(3) 0.007(2) N13 0.016(3) 0.031(5) 0.028(5) -0.007(4) 0.005(3) -0.002(3) C5' 0.050(3) 0.027(3) 0.051(3) -0.007(3) -0.023(3) 0.006(2) N13' 0.039(7) 0.027(5) 0.045(7) 0.010(4) 0.000(5) 0.014(5) O1 0.0404(9) 0.0423(10) 0.0376(9) 0.0008(8) 0.0001(8) 0.0084(7) _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 Zn1 N12 2.1251(16) 3_657 ? Zn1 N12 2.1251(16) . ? Zn1 N11 2.1266(16) . ? Zn1 N11 2.1266(16) 3_657 ? Zn1 N3 2.3070(16) 3_657 ? Zn1 N3 2.3070(16) . ? C1 N4 1.325(3) . ? C1 N1 1.331(3) . ? C1 N5 1.403(2) . ? C2 N10 1.326(3) . ? C2 N7 1.329(3) . ? C2 N6 1.406(2) . ? C3 N11 1.473(2) . ? C3 C4 1.513(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N12 1.479(2) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? N1 N2 1.336(2) . ? N2 N3 1.317(2) . ? N3 N4 1.331(2) . ? N5 N6 1.256(2) . ? N7 N8 1.335(2) . ? N8 N9 1.322(2) . ? N9 N10 1.336(3) . ? N11 H11A 0.9000 . ? N11 H11B 0.9000 . ? N12 H12A 0.9000 . ? N12 H12B 0.9000 . ? C5 C5' 0.812(6) . ? C5 C5 1.183(10) 2_665 ? C5 N13 1.461(18) . ? C5 N13' 1.513(19) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5'B 0.7747 . ? N13 C5' 1.473(18) . ? N13 H13A 0.8998 . ? N13 H13B 0.9000 . ? N13 H13F 0.79(5) . ? N13 H13E 0.8514 . ? N13 H13C 0.8885 . ? N13 H13D 1.0504 . ? C5' N13' 1.531(19) . ? C5' H5A 0.7383 . ? C5' H5'A 0.9600 . ? C5' H5'B 0.9601 . ? N13' H13A 0.9798 . ? N13' H13B 0.7497 . ? N13' H13F 0.84(6) . ? N13' H13E 0.9001 . ? N13' H13C 0.9000 . ? N13' H13D 0.8999 . ? O1 H9 0.821(16) . ? O1 H10 0.791(16) . ? 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 N12 Zn1 N12 99.20(9) 3_657 . ? N12 Zn1 N11 177.92(6) 3_657 . ? N12 Zn1 N11 82.81(6) . . ? N12 Zn1 N11 82.81(6) 3_657 3_657 ? N12 Zn1 N11 177.92(6) . 3_657 ? N11 Zn1 N11 95.19(9) . 3_657 ? N12 Zn1 N3 88.85(6) 3_657 3_657 ? N12 Zn1 N3 89.44(6) . 3_657 ? N11 Zn1 N3 90.60(6) . 3_657 ? N11 Zn1 N3 91.18(6) 3_657 3_657 ? N12 Zn1 N3 89.44(6) 3_657 . ? N12 Zn1 N3 88.85(6) . . ? N11 Zn1 N3 91.18(6) . . ? N11 Zn1 N3 90.60(6) 3_657 . ? N3 Zn1 N3 177.36(9) 3_657 . ? N4 C1 N1 112.42(17) . . ? N4 C1 N5 120.00(18) . . ? N1 C1 N5 127.54(18) . . ? N10 C2 N7 112.40(18) . . ? N10 C2 N6 128.16(18) . . ? N7 C2 N6 119.43(18) . . ? N11 C3 C4 110.10(15) . . ? N11 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N11 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.2 . . ? N12 C4 C3 110.40(15) . . ? N12 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N12 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C1 N1 N2 104.43(17) . . ? N3 N2 N1 108.92(17) . . ? N2 N3 N4 110.10(16) . . ? N2 N3 Zn1 119.32(12) . . ? N4 N3 Zn1 130.54(13) . . ? C1 N4 N3 104.13(16) . . ? N6 N5 C1 113.47(17) . . ? N5 N6 C2 113.27(17) . . ? C2 N7 N8 104.52(16) . . ? N9 N8 N7 109.18(17) . . ? N8 N9 N10 109.49(16) . . ? C2 N10 N9 104.41(16) . . ? C3 N11 Zn1 107.04(12) . . ? C3 N11 H11A 110.3 . . ? Zn1 N11 H11A 110.3 . . ? C3 N11 H11B 110.3 . . ? Zn1 N11 H11B 110.3 . . ? H11A N11 H11B 108.6 . . ? C4 N12 Zn1 108.49(12) . . ? C4 N12 H12A 110.0 . . ? Zn1 N12 H12A 110.0 . . ? C4 N12 H12B 110.0 . . ? Zn1 N12 H12B 110.0 . . ? H12A N12 H12B 108.4 . . ? C5' C5 C5 92.0(6) . 2_665 ? C5' C5 N13 74.7(9) . . ? C5 C5 N13 131.1(11) 2_665 . ? C5' C5 N13' 75.8(10) . . ? C5 C5 N13' 125.9(11) 2_665 . ? N13 C5 N13' 5.5(16) . . ? C5' C5 H5A 48.4 . . ? C5 C5 H5A 103.1 2_665 . ? N13 C5 H5A 102.0 . . ? N13' C5 H5A 106.2 . . ? C5' C5 H5B 152.9 . . ? C5 C5 H5B 104.3 2_665 . ? N13 C5 H5B 108.2 . . ? N13' C5 H5B 109.8 . . ? H5A C5 H5B 106.0 . . ? C5' C5 H5'B 74.4 . . ? C5 C5 H5'B 109.5 2_665 . ? N13 C5 H5'B 111.5 . . ? N13' C5 H5'B 116.8 . . ? H5A C5 H5'B 26.3 . . ? H5B C5 H5'B 79.7 . . ? C5 N13 C5' 32.1(5) . . ? C5 N13 H13A 115.1 . . ? C5' N13 H13A 87.2 . . ? C5 N13 H13B 110.7 . . ? C5' N13 H13B 108.7 . . ? H13A N13 H13B 109.4 . . ? C5 N13 H13F 107(3) . . ? C5' N13 H13F 134(3) . . ? H13A N13 H13F 105.7 . . ? H13B N13 H13F 108.2 . . ? C5 N13 H13E 91.0 . . ? C5' N13 H13E 119.8 . . ? H13A N13 H13E 118.7 . . ? H13B N13 H13E 110.8 . . ? H13F N13 H13E 17.2 . . ? C5 N13 H13C 144.2 . . ? C5' N13 H13C 112.6 . . ? H13A N13 H13C 32.3 . . ? H13B N13 H13C 82.1 . . ? H13F N13 H13C 99.2 . . ? H13E N13 H13C 116.3 . . ? C5 N13 H13D 99.1 . . ? C5' N13 H13D 104.7 . . ? H13A N13 H13D 124.8 . . ? H13B N13 H13D 15.7 . . ? H13F N13 H13D 103.3 . . ? H13E N13 H13D 101.5 . . ? H13C N13 H13D 97.6 . . ? C5 C5' N13 73.1(9) . . ? C5 C5' N13' 73.3(9) . . ? N13 C5' N13' 5.4(16) . . ? C5 C5' H5A 76.3 . . ? N13 C5' H5A 115.1 . . ? N13' C5' H5A 120.0 . . ? C5 C5' H5'A 157.2 . . ? N13 C5' H5'A 109.0 . . ? N13' C5' H5'A 111.1 . . ? H5A C5' H5'A 82.6 . . ? C5 C5' H5'B 51.0 . . ? N13 C5' H5'B 99.6 . . ? N13' C5' H5'B 103.4 . . ? H5A C5' H5'B 25.6 . . ? H5'A C5' H5'B 107.1 . . ? C5 N13' C5' 31.0(4) . . ? C5 N13' H13A 105.9 . . ? C5' N13' H13A 81.3 . . ? C5 N13' H13B 116.9 . . ? C5' N13' H13B 113.7 . . ? H13A N13' H13B 115.6 . . ? C5 N13' H13F 101(4) . . ? C5' N13' H13F 122(5) . . ? H13A N13' H13F 95.5 . . ? H13B N13' H13F 119.2 . . ? C5 N13' H13E 86.0 . . ? C5' N13' H13E 111.0 . . ? H13A N13' H13E 106.5 . . ? H13B N13' H13E 121.5 . . ? H13F N13' H13E 16.3 . . ? C5 N13' H13C 135.3 . . ? C5' N13' H13C 107.1 . . ? H13A N13' H13C 30.3 . . ? H13B N13' H13C 90.3 . . ? H13F N13' H13C 94.8 . . ? H13E N13' H13C 110.4 . . ? C5 N13' H13D 103.3 . . ? C5' N13' H13D 109.2 . . ? H13A N13' H13D 133.9 . . ? H13B N13' H13D 18.6 . . ? H13F N13' H13D 113.3 . . ? H13E N13' H13D 110.4 . . ? H13C N13' H13D 108.7 . . ? H9 O1 H10 110(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.296 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.052