# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1615 data_global # 1. SUBMISSION DETAILS _publ_contact_autor ; Dirk Walther Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische und Analytische Chemie August-Bebel-Str. 2 D-07743 Jena Germany ; _publ_contact_author_phone '03641 9-48110 ' _publ_contact_author_fax '03641 9-48102 ' _publ_requested_journal 'Chem. Comm. ' # 2. TITLE AND AUTHOR LIST _publ_section_title ; Di- and oligonuclear Nickel-complexes with Oxalic amidinato Bridging Ligands: Syntheses, Structures and catalytical Reactions ; loop_ _publ_author_name _publ_author_address ' Walther, Dirk ' ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische und Analytische Chemie August-Bebel-Str. 2 D-07743 Jena Germany ; ' D\"ohler, Thomas ' ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische und Analytische Chemie August-Bebel-Str. 2 D-07743 Jena Germany ; ' Gorls, Helmar ' ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische Chemie und Analytische Chemie August-Bebel-Str. 2 07743 Jena Germany ; # data_4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C44 H50 N4 Ni2 O4' _chemical_formula_weight 816.30 _chemical_melting_point ? _chemical_compound_source ? 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.696(2) _cell_length_b 8.873(1) _cell_length_c 36.989(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.278(6) _cell_angle_gamma 90.00 _cell_volume 4123.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method ? _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.959 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method phi-scan _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4609 _diffrn_reflns_av_R_equivalents 0.0897 _diffrn_reflns_av_sigmaI/netI 0.1024 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 23.27 _reflns_number_total 3331 _reflns_number_observed 2607 _reflns_observed_criterion >2sigma(I) _computing_data_collection DENZO _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 158 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1326P)^2^+15.6052P] 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 rigid-group _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3173 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_obs 0.0805 _refine_ls_wR_factor_all 0.2709 _refine_ls_wR_factor_obs 0.2307 _refine_ls_goodness_of_fit_all 1.074 _refine_ls_goodness_of_fit_obs 1.149 _refine_ls_restrained_S_all 1.171 _refine_ls_restrained_S_obs 1.149 _refine_ls_shift/esd_max 0.025 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.57526(10) 0.1527(2) 0.08063(4) 0.0381(5) Uani 1 d . . Ni2 Ni 0.67667(10) 0.5881(2) 0.17400(4) 0.0355(5) Uani 1 d . . O1 O 0.7985(5) 0.7032(9) 0.1837(2) 0.045(2) Uani 1 d . . O2 O 0.6188(5) 0.6581(7) 0.2141(2) 0.039(2) Uani 1 d . . O3 O 0.4680(5) 0.0114(8) 0.0759(2) 0.045(2) Uani 1 d . . O4 O 0.6460(6) 0.0676(8) 0.0456(2) 0.046(2) Uani 1 d . . N1 N 0.6828(6) 0.2988(9) 0.0905(2) 0.034(2) Uani 1 d . . N2 N 0.5149(6) 0.2523(9) 0.1177(2) 0.033(2) Uani 1 d . . N3 N 0.7285(7) 0.5038(11) 0.1334(2) 0.041(2) Uani 1 d . . N4 N 0.5570(7) 0.4613(9) 0.1599(2) 0.032(2) Uani 1 d . . C1 C 0.6726(8) 0.3918(12) 0.1171(3) 0.033(3) Uani 1 d . . C2 C 0.5706(8) 0.3656(11) 0.1332(3) 0.031(2) Uani 1 d . . C3 C 0.8221(8) 0.7930(13) 0.2092(3) 0.043(3) Uani 1 d . . C4 C 0.7587(9) 0.8238(13) 0.2370(3) 0.047(3) Uani 1 d . . H4A H 0.7840(9) 0.8934(13) 0.2558(3) 0.056 Uiso 1 calc R . C5 C 0.6605(9) 0.7547(12) 0.2375(3) 0.043(3) Uani 1 d . . C6 C 0.5955(10) 0.7951(14) 0.2668(3) 0.058(3) Uani 1 d . . H6A H 0.5291(10) 0.7371(14) 0.2633(3) 0.087 Uiso 1 calc R . H6B H 0.5791(10) 0.9030(14) 0.2655(3) 0.087 Uiso 1 calc R . H6C H 0.6358(10) 0.7715(14) 0.2908(3) 0.087 Uiso 1 calc R . C7 C 0.9273(9) 0.8753(13) 0.2096(3) 0.052(3) Uani 1 d . . H7A H 0.9608(9) 0.8429(13) 0.1886(3) 0.077 Uiso 1 calc R . H7B H 0.9745(9) 0.8518(13) 0.2322(3) 0.077 Uiso 1 calc R . H7C H 0.9145(9) 0.9842(13) 0.2081(3) 0.077 Uiso 1 calc R . C8 C 0.4654(9) -0.1115(13) 0.0575(3) 0.046(3) Uani 1 d . . C9 C 0.5399(9) -0.1487(14) 0.0348(3) 0.046(3) Uani 1 d . . H9A H 0.5306(9) -0.2410(14) 0.0217(3) 0.055 Uiso 1 calc R . C10 C 0.6256(9) -0.0611(13) 0.0301(3) 0.041(3) Uani 1 d . . C11 C 0.7029(9) -0.1107(14) 0.0042(3) 0.051(3) Uani 1 d . . H11A H 0.7592(9) -0.0351(14) 0.0044(3) 0.077 Uiso 1 calc R . H11B H 0.6645(9) -0.1210(14) -0.0206(3) 0.077 Uiso 1 calc R . H11C H 0.7347(9) -0.2078(14) 0.0124(3) 0.077 Uiso 1 calc R . C12 C 0.3717(9) -0.2125(13) 0.0608(4) 0.056(3) Uani 1 d . . H12A H 0.3283(9) -0.1675(13) 0.0778(4) 0.084 Uiso 1 calc R . H12B H 0.3974(9) -0.3115(13) 0.0699(4) 0.084 Uiso 1 calc R . H12C H 0.3285(9) -0.2241(13) 0.0368(4) 0.084 Uiso 1 calc R . C13 C 0.4194(8) 0.1961(10) 0.1305(3) 0.027(2) Uani 1 d . . C14 C 0.3194(8) 0.2535(11) 0.1167(3) 0.034(3) Uani 1 d . . C15 C 0.2330(9) 0.1960(13) 0.1307(3) 0.045(3) Uani 1 d . . H15A H 0.1646(9) 0.2365(13) 0.1223(3) 0.054 Uiso 1 calc R . C16 C 0.2415(9) 0.0826(12) 0.1562(4) 0.045(3) Uani 1 d . . C17 C 0.3427(9) 0.0196(13) 0.1684(3) 0.044(3) Uani 1 d . . H17A H 0.3497(9) -0.0600(13) 0.1857(3) 0.053 Uiso 1 calc R . C18 C 0.4329(8) 0.0752(11) 0.1547(3) 0.035(3) Uani 1 d . . C19 C 0.3081(8) 0.3754(11) 0.0883(3) 0.043(3) Uani 1 d . . H19A H 0.3784(8) 0.4005(11) 0.0820(3) 0.064 Uiso 1 calc R . H19B H 0.2768(8) 0.4650(11) 0.0980(3) 0.064 Uiso 1 calc R . H19C H 0.2618(8) 0.3403(11) 0.0665(3) 0.064 Uiso 1 calc R . C20 C 0.1445(10) 0.0250(16) 0.1726(4) 0.075(4) Uani 1 d . . H20A H 0.1667(10) -0.0556(16) 0.1902(4) 0.113 Uiso 1 calc R . H20B H 0.0913(10) -0.0142(16) 0.1530(4) 0.113 Uiso 1 calc R . H20C H 0.1135(10) 0.1080(16) 0.1850(4) 0.113 Uiso 1 calc R . C21 C 0.5408(8) 0.0105(13) 0.1681(4) 0.053(3) Uani 1 d . . H21A H 0.5335(8) -0.0735(13) 0.1848(4) 0.080 Uiso 1 calc R . H21B H 0.5861(8) 0.0886(13) 0.1811(4) 0.080 Uiso 1 calc R . H21C H 0.5734(8) -0.0258(13) 0.1473(4) 0.080 Uiso 1 calc R . C22 C 0.7768(8) 0.2940(11) 0.0729(3) 0.033(3) Uani 1 d . . C23 C 0.8581(8) 0.1958(13) 0.0880(3) 0.040(3) Uani 1 d . . C24 C 0.9447(9) 0.1775(13) 0.0694(4) 0.047(3) Uani 1 d . . H24A H 1.0001(9) 0.1104(13) 0.0791(4) 0.057 Uiso 1 calc R . C25 C 0.9533(10) 0.2549(14) 0.0368(4) 0.049(3) Uani 1 d . . C26 C 0.8713(11) 0.3468(14) 0.0229(3) 0.055(4) Uani 1 d . . H26A H 0.8755(11) 0.3985(14) 0.0006(3) 0.065 Uiso 1 calc R . C27 C 0.7801(9) 0.3679(12) 0.0404(3) 0.040(3) Uani 1 d . . C28 C 0.8484(10) 0.1083(14) 0.1223(4) 0.061(4) Uani 1 d . . H28A H 0.7826(10) 0.1373(14) 0.1314(4) 0.091 Uiso 1 calc R . H28B H 0.9096(10) 0.1303(14) 0.1408(4) 0.091 Uiso 1 calc R . H28C H 0.8466(10) 0.0002(14) 0.1168(4) 0.091 Uiso 1 calc R . C29 C 1.0491(10) 0.2310(19) 0.0171(5) 0.093(6) Uani 1 d . . H29A H 1.0995(10) 0.1623(19) 0.0313(5) 0.140 Uiso 1 calc R . H29B H 1.0840(10) 0.3279(19) 0.0142(5) 0.140 Uiso 1 calc R . H29C H 1.0256(10) 0.1872(19) -0.0071(5) 0.140 Uiso 1 calc R . C30 C 0.6879(9) 0.4642(13) 0.0241(3) 0.058(3) Uani 1 d . . H30A H 0.7033(9) 0.5083(13) 0.0011(3) 0.086 Uiso 1 calc R . H30B H 0.6767(9) 0.5450(13) 0.0412(3) 0.086 Uiso 1 calc R . H30C H 0.6235(9) 0.4021(13) 0.0193(3) 0.086 Uiso 1 calc R . C31 C 0.4611(8) 0.4718(12) 0.1760(3) 0.033(3) Uani 1 d . . C32 C 0.3921(9) 0.5895(13) 0.1666(3) 0.043(3) Uani 1 d . . H32A H 0.4095(9) 0.6646(13) 0.1501(3) 0.051 Uiso 1 calc R . C33 C 0.2973(10) 0.5994(14) 0.1809(3) 0.047(3) Uani 1 d . . H33A H 0.2493(10) 0.6794(14) 0.1735(3) 0.057 Uiso 1 calc R . C34 C 0.2719(9) 0.4942(14) 0.2058(3) 0.043(3) Uani 1 d . . C35 C 0.3459(9) 0.3846(15) 0.2163(3) 0.049(3) Uani 1 d . . H35A H 0.3318(9) 0.3142(15) 0.2343(3) 0.059 Uiso 1 calc R . C36 C 0.4404(9) 0.3713(12) 0.2018(3) 0.037(3) Uani 1 d . . H36A H 0.4897(9) 0.2935(12) 0.2098(3) 0.045 Uiso 1 calc R . C37 C 0.1649(10) 0.5024(17) 0.2208(4) 0.069(4) Uani 1 d . . H37A H 0.1237(10) 0.5885(17) 0.2098(4) 0.104 Uiso 1 calc R . H37B H 0.1782(10) 0.5147(17) 0.2474(4) 0.104 Uiso 1 calc R . H37C H 0.1248(10) 0.4092(17) 0.2147(4) 0.104 Uiso 1 calc R . C38 C 0.8226(9) 0.5593(12) 0.1205(3) 0.036(3) Uani 1 d . . C39 C 0.9222(9) 0.5018(13) 0.1336(3) 0.043(3) Uani 1 d . . H39A H 0.9291(9) 0.4212(13) 0.1506(3) 0.051 Uiso 1 calc R . C40 C 1.0117(9) 0.5627(12) 0.1216(3) 0.045(3) Uani 1 d . . H40A H 1.0791(9) 0.5181(12) 0.1295(3) 0.054 Uiso 1 calc R . C41 C 1.0064(9) 0.6866(11) 0.0984(3) 0.037(3) Uani 1 d . . C42 C 0.9069(9) 0.7442(12) 0.0858(3) 0.042(3) Uani 1 d . . H42A H 0.8999(9) 0.8262(12) 0.0692(3) 0.051 Uiso 1 calc R . C43 C 0.8174(9) 0.6831(11) 0.0975(3) 0.038(3) Uani 1 d . . H43A H 0.7500(9) 0.7276(11) 0.0894(3) 0.045 Uiso 1 calc R . C44 C 1.1059(9) 0.7514(15) 0.0859(4) 0.062(4) Uani 1 d . . H44A H 1.1684(9) 0.6955(15) 0.0974(4) 0.093 Uiso 1 calc R . H44B H 1.1130(9) 0.8577(15) 0.0929(4) 0.093 Uiso 1 calc R . H44C H 1.1003(9) 0.7427(15) 0.0592(4) 0.093 Uiso 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 0.0300(10) 0.0374(9) 0.0489(8) -0.0111(7) 0.0129(6) -0.0105(7) Ni2 0.0270(10) 0.0390(10) 0.0420(8) -0.0081(6) 0.0101(6) -0.0070(7) O1 0.032(5) 0.058(5) 0.048(4) -0.012(4) 0.015(3) -0.022(4) O2 0.034(5) 0.031(4) 0.054(5) -0.011(4) 0.013(3) -0.002(4) O3 0.036(5) 0.040(5) 0.063(5) -0.020(4) 0.023(4) -0.016(4) O4 0.040(5) 0.047(5) 0.055(5) -0.016(4) 0.017(4) -0.010(4) N1 0.020(5) 0.034(5) 0.050(5) -0.006(4) 0.016(4) -0.010(4) N2 0.027(6) 0.018(5) 0.055(5) -0.004(4) 0.013(4) -0.011(4) N3 0.031(6) 0.052(6) 0.040(5) -0.016(5) 0.012(4) -0.016(5) N4 0.021(6) 0.022(5) 0.054(5) -0.002(4) 0.013(4) -0.010(4) C1 0.013(7) 0.048(7) 0.039(6) -0.001(5) 0.012(4) 0.004(5) C2 0.022(7) 0.028(6) 0.046(6) 0.001(5) 0.013(4) -0.009(5) C3 0.030(8) 0.053(8) 0.046(6) -0.009(6) 0.002(5) -0.009(6) C4 0.046(8) 0.053(8) 0.041(6) -0.018(6) 0.004(5) -0.003(7) C5 0.046(9) 0.032(7) 0.052(7) -0.010(5) 0.008(5) -0.010(6) C6 0.064(9) 0.065(9) 0.048(7) -0.017(6) 0.019(6) -0.012(7) C7 0.043(8) 0.042(7) 0.072(8) -0.005(6) 0.016(6) -0.016(6) C8 0.042(9) 0.048(8) 0.049(6) -0.003(6) 0.007(5) -0.011(6) C9 0.035(8) 0.052(8) 0.051(7) -0.001(6) 0.010(5) -0.003(7) C10 0.043(8) 0.040(7) 0.041(6) -0.007(5) 0.003(5) 0.015(6) C11 0.033(8) 0.062(8) 0.060(7) -0.011(6) 0.012(5) 0.011(6) C12 0.050(9) 0.038(7) 0.086(9) -0.021(7) 0.027(6) -0.032(7) C13 0.014(6) 0.012(5) 0.059(6) -0.012(5) 0.016(4) 0.002(4) C14 0.028(7) 0.030(6) 0.047(6) -0.004(5) 0.012(5) 0.001(5) C15 0.019(7) 0.046(8) 0.070(8) -0.013(6) 0.010(5) -0.006(6) C16 0.036(8) 0.032(7) 0.070(8) -0.002(6) 0.017(6) -0.013(6) C17 0.046(8) 0.034(7) 0.055(7) 0.004(6) 0.018(5) 0.000(6) C18 0.020(7) 0.027(6) 0.061(7) 0.007(5) 0.015(5) -0.003(5) C19 0.044(8) 0.027(6) 0.056(7) -0.001(5) 0.000(5) -0.005(5) C20 0.046(9) 0.086(11) 0.103(12) -0.009(9) 0.042(8) -0.033(9) C21 0.035(8) 0.037(7) 0.087(10) 0.003(7) 0.010(6) -0.002(6) C22 0.021(7) 0.027(6) 0.052(6) -0.016(5) 0.012(5) -0.007(5) C23 0.015(7) 0.050(8) 0.056(7) -0.005(6) 0.004(5) 0.000(6) C24 0.026(8) 0.041(7) 0.076(8) -0.014(6) 0.009(6) -0.006(6) C25 0.033(8) 0.041(8) 0.077(9) -0.025(7) 0.019(6) -0.017(7) C26 0.066(10) 0.053(8) 0.048(7) -0.015(6) 0.023(6) -0.034(8) C27 0.042(8) 0.026(6) 0.052(6) -0.019(5) 0.012(5) -0.016(6) C28 0.062(9) 0.054(9) 0.064(8) 0.005(7) -0.002(6) 0.013(7) C29 0.047(10) 0.125(14) 0.119(14) -0.062(11) 0.053(9) -0.039(10) C30 0.067(9) 0.042(8) 0.063(8) -0.014(6) 0.004(6) -0.005(7) C31 0.019(7) 0.038(7) 0.044(6) -0.002(5) 0.010(4) -0.010(6) C32 0.033(8) 0.038(7) 0.058(7) 0.004(6) 0.008(5) -0.008(6) C33 0.030(8) 0.049(8) 0.062(8) -0.013(6) 0.005(5) 0.000(6) C34 0.022(8) 0.055(8) 0.056(7) -0.017(6) 0.013(5) -0.006(6) C35 0.032(8) 0.070(9) 0.048(6) -0.006(6) 0.014(5) -0.018(7) C36 0.021(7) 0.037(7) 0.055(7) -0.008(5) 0.008(5) -0.004(5) C37 0.029(8) 0.104(11) 0.081(10) -0.029(9) 0.032(6) -0.011(8) C38 0.035(8) 0.032(7) 0.041(6) -0.003(5) 0.008(5) -0.016(6) C39 0.028(8) 0.049(8) 0.053(7) 0.003(6) 0.010(5) -0.004(6) C40 0.026(8) 0.047(7) 0.064(7) 0.004(6) 0.015(5) 0.005(6) C41 0.033(8) 0.023(6) 0.057(7) -0.010(5) 0.014(5) -0.009(5) C42 0.038(8) 0.035(7) 0.055(7) 0.003(5) 0.014(5) -0.012(6) C43 0.028(7) 0.033(7) 0.054(6) -0.004(5) 0.012(5) -0.003(6) C44 0.036(8) 0.073(10) 0.085(10) -0.012(8) 0.033(6) -0.019(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 Ni1 O3 1.841(7) . ? Ni1 O4 1.843(7) . ? Ni1 N2 1.886(8) . ? Ni1 N1 1.880(8) . ? Ni2 O1 1.845(7) . ? Ni2 O2 1.854(7) . ? Ni2 N3 1.879(8) . ? Ni2 N4 1.902(8) . ? O1 C3 1.240(12) . ? O2 C5 1.278(12) . ? O3 C8 1.285(13) . ? O4 C10 1.288(12) . ? N1 C1 1.304(12) . ? N1 C22 1.440(12) . ? N2 C2 1.311(12) . ? N2 C13 1.451(12) . ? N3 C1 1.316(13) . ? N3 C38 1.437(12) . ? N4 C2 1.334(12) . ? N4 C31 1.432(12) . ? C1 C2 1.518(13) . ? C3 C4 1.420(14) . ? C3 C7 1.522(14) . ? C4 C5 1.392(14) . ? C5 C6 1.497(14) . ? C8 C9 1.390(15) . ? C8 C12 1.509(14) . ? C9 C10 1.368(15) . ? C10 C11 1.530(14) . ? C13 C14 1.395(13) . ? C13 C18 1.392(14) . ? C14 C15 1.376(14) . ? C14 C19 1.498(14) . ? C15 C16 1.37(2) . ? C16 C17 1.41(2) . ? C16 C20 1.537(15) . ? C17 C18 1.406(13) . ? C18 C21 1.503(14) . ? C22 C27 1.376(14) . ? C22 C23 1.404(14) . ? C23 C24 1.388(14) . ? C23 C28 1.50(2) . ? C24 C25 1.41(2) . ? C25 C26 1.36(2) . ? C25 C29 1.52(2) . ? C26 C27 1.419(15) . ? C27 C30 1.50(2) . ? C31 C36 1.361(14) . ? C31 C32 1.375(14) . ? C32 C33 1.385(14) . ? C33 C34 1.38(2) . ? C34 C35 1.37(2) . ? C34 C37 1.540(15) . ? C35 C36 1.386(14) . ? C38 C39 1.384(15) . ? C38 C43 1.385(14) . ? C39 C40 1.388(14) . ? C40 C41 1.390(15) . ? C41 C42 1.380(14) . ? C41 C44 1.519(14) . ? C42 C43 1.383(13) . ? 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 O3 Ni1 O4 94.8(3) . . ? O3 Ni1 N2 90.9(3) . . ? O4 Ni1 N2 174.2(3) . . ? O3 Ni1 N1 174.1(3) . . ? O4 Ni1 N1 90.3(3) . . ? N2 Ni1 N1 83.9(3) . . ? O1 Ni2 O2 94.4(3) . . ? O1 Ni2 N3 89.7(3) . . ? O2 Ni2 N3 175.5(3) . . ? O1 Ni2 N4 174.2(3) . . ? O2 Ni2 N4 91.4(3) . . ? N3 Ni2 N4 84.5(4) . . ? C3 O1 Ni2 127.4(7) . . ? C5 O2 Ni2 126.4(7) . . ? C8 O3 Ni1 126.1(7) . . ? C10 O4 Ni1 126.1(7) . . ? C1 N1 C22 122.6(8) . . ? C1 N1 Ni1 115.8(7) . . ? C22 N1 Ni1 121.1(6) . . ? C2 N2 C13 123.0(8) . . ? C2 N2 Ni1 115.2(7) . . ? C13 N2 Ni1 121.4(6) . . ? C1 N3 C38 121.7(8) . . ? C1 N3 Ni2 116.0(7) . . ? C38 N3 Ni2 122.2(7) . . ? C2 N4 C31 123.9(8) . . ? C2 N4 Ni2 113.3(7) . . ? C31 N4 Ni2 122.8(6) . . ? N3 C1 N1 135.8(10) . . ? N3 C1 C2 111.7(8) . . ? N1 C1 C2 112.4(9) . . ? N2 C2 N4 133.8(9) . . ? N2 C2 C1 112.6(9) . . ? N4 C2 C1 113.7(8) . . ? O1 C3 C4 125.2(10) . . ? O1 C3 C7 115.5(10) . . ? C4 C3 C7 119.3(11) . . ? C5 C4 C3 121.7(11) . . ? O2 C5 C4 124.9(10) . . ? O2 C5 C6 115.7(10) . . ? C4 C5 C6 119.5(11) . . ? O3 C8 C9 123.7(11) . . ? O3 C8 C12 114.8(10) . . ? C9 C8 C12 121.4(11) . . ? C10 C9 C8 124.4(12) . . ? O4 C10 C9 124.1(11) . . ? O4 C10 C11 115.2(11) . . ? C9 C10 C11 120.7(11) . . ? C14 C13 C18 122.5(9) . . ? C14 C13 N2 121.0(9) . . ? C18 C13 N2 116.3(8) . . ? C15 C14 C13 117.4(10) . . ? C15 C14 C19 122.0(10) . . ? C13 C14 C19 120.6(10) . . ? C14 C15 C16 122.8(10) . . ? C15 C16 C17 119.1(11) . . ? C15 C16 C20 121.8(11) . . ? C17 C16 C20 119.1(12) . . ? C18 C17 C16 119.8(11) . . ? C13 C18 C17 118.1(9) . . ? C13 C18 C21 121.9(9) . . ? C17 C18 C21 119.9(10) . . ? C27 C22 C23 122.1(10) . . ? C27 C22 N1 120.9(9) . . ? C23 C22 N1 116.6(10) . . ? C24 C23 C22 117.7(11) . . ? C24 C23 C28 121.6(10) . . ? C22 C23 C28 120.7(10) . . ? C23 C24 C25 122.2(11) . . ? C26 C25 C24 117.9(11) . . ? C26 C25 C29 121.3(13) . . ? C24 C25 C29 120.7(12) . . ? C25 C26 C27 122.3(12) . . ? C22 C27 C26 117.8(11) . . ? C22 C27 C30 120.1(10) . . ? C26 C27 C30 122.1(11) . . ? C36 C31 C32 119.6(10) . . ? C36 C31 N4 120.7(10) . . ? C32 C31 N4 119.6(9) . . ? C33 C32 C31 120.6(10) . . ? C32 C33 C34 120.7(11) . . ? C35 C34 C33 116.9(11) . . ? C35 C34 C37 122.4(12) . . ? C33 C34 C37 120.7(12) . . ? C34 C35 C36 123.2(11) . . ? C31 C36 C35 118.8(10) . . ? C39 C38 C43 117.9(10) . . ? C39 C38 N3 121.2(10) . . ? C43 C38 N3 120.5(10) . . ? C38 C39 C40 119.6(11) . . ? C41 C40 C39 122.4(10) . . ? C42 C41 C40 117.4(10) . . ? C42 C41 C44 121.2(10) . . ? C40 C41 C44 121.3(10) . . ? C41 C42 C43 120.3(11) . . ? C42 C43 C38 122.2(10) . . ? _refine_diff_density_max 0.385 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.114 #===END data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C112 H122 N12 Ni2 O4 Zn2' _chemical_formula_weight 1948.38 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' '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 I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 22.2023(8) _cell_length_b 21.6541(6) _cell_length_c 25.343(1) _cell_angle_alpha 90.00 _cell_angle_beta 105.960(2) _cell_angle_gamma 90.00 _cell_volume 11714.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4176 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7901 _exptl_absorpt_correction_T_max 0.8608 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22567 _diffrn_reflns_av_R_equivalents 0.0911 _diffrn_reflns_av_sigmaI/netI 0.1305 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 26.42 _reflns_number_total 11922 _reflns_number_gt 6125 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.1336P)^2^+11.1118P] 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 rigid-group _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11922 _refine_ls_number_parameters 615 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1752 _refine_ls_R_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.2610 _refine_ls_wR_factor_gt 0.2171 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.013 _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 Zn Zn 0.63156(3) 0.69975(3) 0.43474(3) 0.0430(2) Uani 1 1 d . . . Ni Ni 0.38637(3) 0.69204(3) 0.34254(3) 0.0470(3) Uani 1 1 d . . . O1 O 0.33263(19) 0.6292(2) 0.3112(2) 0.0658(14) Uani 1 1 d . . . O2 O 0.32267(19) 0.7489(2) 0.34019(19) 0.0586(12) Uani 1 1 d . . . N1 N 0.4558(2) 0.6377(2) 0.3543(2) 0.0432(12) Uani 1 1 d . . . N2 N 0.4484(2) 0.7522(2) 0.3701(2) 0.0443(12) Uani 1 1 d . . . N3 N 0.5674(2) 0.6372(2) 0.3979(2) 0.0425(12) Uani 1 1 d . . . N4 N 0.5607(2) 0.7598(2) 0.4093(2) 0.0421(12) Uani 1 1 d . . . N5 N 0.7182(2) 0.6945(2) 0.4263(2) 0.0407(11) Uani 1 1 d . . . N6 N 0.6756(2) 0.7016(2) 0.5150(2) 0.0421(12) Uani 1 1 d . . . C1 C 0.5102(2) 0.6616(2) 0.3797(2) 0.0366(13) Uani 1 1 d . . . C2 C 0.5058(2) 0.7311(3) 0.3875(2) 0.0391(13) Uani 1 1 d . . . C3 C 0.4476(3) 0.5741(3) 0.3380(3) 0.0440(15) Uani 1 1 d . . . C4 C 0.4320(3) 0.5306(3) 0.3723(3) 0.0605(18) Uani 1 1 d . . . C5 C 0.4234(4) 0.4694(3) 0.3549(4) 0.076(2) Uani 1 1 d . . . H5A H 0.4135 0.4395 0.3786 0.092 Uiso 1 1 calc R . . C6 C 0.4288(3) 0.4511(3) 0.3047(4) 0.065(2) Uani 1 1 d . . . C7 C 0.4424(3) 0.4943(3) 0.2712(3) 0.065(2) Uani 1 1 d . . . H7A H 0.4457 0.4818 0.2362 0.078 Uiso 1 1 calc R . . C8 C 0.4517(3) 0.5568(3) 0.2860(3) 0.0554(17) Uani 1 1 d . . . C9 C 0.4223(5) 0.5501(4) 0.4272(4) 0.094(3) Uani 1 1 d . . . H9A H 0.4118 0.5138 0.4460 0.141 Uiso 1 1 calc R . . H9B H 0.3879 0.5800 0.4209 0.141 Uiso 1 1 calc R . . H9C H 0.4608 0.5690 0.4500 0.141 Uiso 1 1 calc R . . C10 C 0.4214(4) 0.3820(3) 0.2898(5) 0.102(3) Uani 1 1 d . . . H10A H 0.4263 0.3759 0.2529 0.153 Uiso 1 1 calc R . . H10B H 0.3797 0.3680 0.2907 0.153 Uiso 1 1 calc R . . H10C H 0.4535 0.3582 0.3163 0.153 Uiso 1 1 calc R . . C11 C 0.4658(5) 0.6049(4) 0.2470(4) 0.100(3) Uani 1 1 d . . . H11A H 0.4667 0.5848 0.2126 0.150 Uiso 1 1 calc R . . H11B H 0.5065 0.6240 0.2639 0.150 Uiso 1 1 calc R . . H11C H 0.4331 0.6367 0.2395 0.150 Uiso 1 1 calc R . . C12 C 0.4357(2) 0.8170(3) 0.3588(3) 0.0429(15) Uani 1 1 d . . . C13 C 0.4424(3) 0.8395(3) 0.3083(3) 0.0546(18) Uani 1 1 d . . . C14 C 0.4336(3) 0.9031(3) 0.2978(3) 0.064(2) Uani 1 1 d . . . H14A H 0.4396 0.9193 0.2648 0.077 Uiso 1 1 calc R . . C15 C 0.4168(3) 0.9423(3) 0.3333(4) 0.068(2) Uani 1 1 d . . . C16 C 0.4058(3) 0.9177(3) 0.3802(4) 0.067(2) Uani 1 1 d . . . H16A H 0.3916 0.9446 0.4039 0.081 Uiso 1 1 calc R . . C17 C 0.4145(3) 0.8548(3) 0.3945(3) 0.0529(17) Uani 1 1 d . . . C18 C 0.4627(4) 0.7972(3) 0.2681(3) 0.071(2) Uani 1 1 d . . . H18A H 0.4646 0.8210 0.2357 0.107 Uiso 1 1 calc R . . H18B H 0.4324 0.7635 0.2569 0.107 Uiso 1 1 calc R . . H18C H 0.5041 0.7800 0.2858 0.107 Uiso 1 1 calc R . . C19 C 0.4117(4) 1.0116(3) 0.3215(4) 0.106(4) Uani 1 1 d . . . H19A H 0.4213 1.0198 0.2867 0.159 Uiso 1 1 calc R . . H19B H 0.4415 1.0337 0.3512 0.159 Uiso 1 1 calc R . . H19C H 0.3690 1.0255 0.3191 0.159 Uiso 1 1 calc R . . C20 C 0.4038(3) 0.8297(3) 0.4453(3) 0.068(2) Uani 1 1 d . . . H20A H 0.4126 0.7853 0.4475 0.102 Uiso 1 1 calc R . . H20B H 0.3601 0.8367 0.4450 0.102 Uiso 1 1 calc R . . H20C H 0.4316 0.8506 0.4771 0.102 Uiso 1 1 calc R . . C21 C 0.5826(2) 0.5737(3) 0.3933(2) 0.0409(14) Uani 1 1 d . . . C22 C 0.5796(4) 0.5314(3) 0.4330(3) 0.073(2) Uani 1 1 d . . . H22A H 0.5675 0.5446 0.4644 0.087 Uiso 1 1 calc R . . C23 C 0.5937(4) 0.4705(3) 0.4277(4) 0.083(3) Uani 1 1 d . . . H23A H 0.5900 0.4420 0.4552 0.100 Uiso 1 1 calc R . . C24 C 0.6132(3) 0.4491(3) 0.3837(3) 0.069(2) Uani 1 1 d . . . C25 C 0.6202(4) 0.4921(4) 0.3461(3) 0.070(2) Uani 1 1 d . . . H25A H 0.6353 0.4796 0.3162 0.084 Uiso 1 1 calc R . . C26 C 0.6055(4) 0.5538(3) 0.3511(3) 0.065(2) Uani 1 1 d . . . H26A H 0.6113 0.5828 0.3248 0.078 Uiso 1 1 calc R . . C27 C 0.6256(5) 0.3804(4) 0.3768(4) 0.102(3) Uani 1 1 d . . . H27A H 0.6186 0.3572 0.4078 0.153 Uiso 1 1 calc R . . H27B H 0.6691 0.3748 0.3758 0.153 Uiso 1 1 calc R . . H27C H 0.5972 0.3652 0.3425 0.153 Uiso 1 1 calc R . . C28 C 0.5661(3) 0.8246(3) 0.4240(3) 0.0437(15) Uani 1 1 d . . . C29 C 0.5794(3) 0.8679(3) 0.3879(3) 0.0550(17) Uani 1 1 d . . . H29A H 0.5852 0.8550 0.3538 0.066 Uiso 1 1 calc R . . C30 C 0.5843(3) 0.9304(3) 0.4024(3) 0.065(2) Uani 1 1 d . . . H30A H 0.5921 0.9599 0.3773 0.078 Uiso 1 1 calc R . . C31 C 0.5778(3) 0.9501(3) 0.4526(4) 0.069(2) Uani 1 1 d . . . C32 C 0.5680(3) 0.9062(3) 0.4888(3) 0.068(2) Uani 1 1 d . . . H32A H 0.5649 0.9187 0.5239 0.081 Uiso 1 1 calc R . . C33 C 0.5625(3) 0.8443(3) 0.4748(3) 0.0548(17) Uani 1 1 d . . . H33A H 0.5561 0.8149 0.5006 0.066 Uiso 1 1 calc R . . C34 C 0.5805(5) 1.0193(4) 0.4658(4) 0.103(3) Uani 1 1 d . . . H34A H 0.5880 1.0425 0.4350 0.154 Uiso 1 1 calc R . . H34B H 0.6145 1.0272 0.4990 0.154 Uiso 1 1 calc R . . H34C H 0.5406 1.0323 0.4717 0.154 Uiso 1 1 calc R . . C35 C 0.7620(2) 0.6988(2) 0.4747(2) 0.0369(12) Uani 1 1 d . . . C36 C 0.7059(3) 0.7049(3) 0.3283(3) 0.0533(17) Uani 1 1 d . . . C37 C 0.7303(2) 0.6727(3) 0.3773(2) 0.0413(14) Uani 1 1 d . . . C38 C 0.7607(3) 0.6157(3) 0.3759(3) 0.0535(17) Uani 1 1 d . . . C39 C 0.7677(3) 0.5938(3) 0.3266(3) 0.0628(19) Uani 1 1 d . . . H39A H 0.7883 0.5555 0.3262 0.075 Uiso 1 1 calc R . . C40 C 0.7452(4) 0.6264(3) 0.2771(3) 0.067(2) Uani 1 1 d . . . C41 C 0.7153(3) 0.6805(3) 0.2798(3) 0.0598(19) Uani 1 1 d . . . H41A H 0.6998 0.7033 0.2468 0.072 Uiso 1 1 calc R . . C42 C 0.7794(4) 0.5734(3) 0.4272(3) 0.077(2) Uani 1 1 d . . . H42A H 0.7993 0.5359 0.4185 0.115 Uiso 1 1 calc R . . H42B H 0.7418 0.5623 0.4383 0.115 Uiso 1 1 calc R . . H42C H 0.8088 0.5953 0.4573 0.115 Uiso 1 1 calc R . . C43 C 0.7534(4) 0.6006(4) 0.2238(3) 0.089(3) Uani 1 1 d . . . H43A H 0.7352 0.6293 0.1938 0.133 Uiso 1 1 calc R . . H43B H 0.7323 0.5606 0.2162 0.133 Uiso 1 1 calc R . . H43C H 0.7982 0.5954 0.2271 0.133 Uiso 1 1 calc R . . C44 C 0.6712(3) 0.7631(3) 0.3279(3) 0.073(2) Uani 1 1 d . . . H44A H 0.6697 0.7728 0.3653 0.110 Uiso 1 1 calc R . . H44B H 0.6285 0.7586 0.3040 0.110 Uiso 1 1 calc R . . H44C H 0.6925 0.7966 0.3142 0.110 Uiso 1 1 calc R . . C45 C 0.6426(3) 0.7177(3) 0.5538(3) 0.0461(15) Uani 1 1 d . . . C46 C 0.5852(3) 0.6892(3) 0.5496(3) 0.067(2) Uani 1 1 d . . . H46A H 0.5723 0.6555 0.5251 0.081 Uiso 1 1 calc R . . C47 C 0.5467(5) 0.7095(4) 0.5808(5) 0.100(3) Uani 1 1 d . . . H47A H 0.5078 0.6894 0.5775 0.120 Uiso 1 1 calc R . . C48 C 0.5646(5) 0.7599(5) 0.6177(4) 0.097(3) Uani 1 1 d . . . C49 C 0.6207(4) 0.7871(4) 0.6217(3) 0.073(2) Uani 1 1 d . . . H49A H 0.6334 0.8208 0.6463 0.088 Uiso 1 1 calc R . . C50 C 0.6606(3) 0.7675(3) 0.5910(3) 0.0603(19) Uani 1 1 d . . . H50A H 0.6997 0.7876 0.5951 0.072 Uiso 1 1 calc R . . C51 C 0.5197(7) 0.7839(6) 0.6507(6) 0.155(6) Uani 1 1 d . . . H51A H 0.5395 0.8186 0.6739 0.232 Uiso 1 1 calc R . . H51B H 0.5111 0.7506 0.6737 0.232 Uiso 1 1 calc R . . H51C H 0.4804 0.7977 0.6251 0.232 Uiso 1 1 calc R . . C52 C 0.2727(3) 0.6336(3) 0.2916(3) 0.068(2) Uani 1 1 d . . . C53 C 0.2382(3) 0.6849(3) 0.2961(3) 0.070(2) Uani 1 1 d . . . H53A H 0.1940 0.6831 0.2814 0.084 Uiso 1 1 calc R . . C54 C 0.2640(3) 0.7388(3) 0.3208(3) 0.0591(18) Uani 1 1 d . . . C55 C 0.2428(4) 0.5748(4) 0.2633(4) 0.103(4) Uani 1 1 d . . . H55A H 0.2755 0.5442 0.2641 0.154 Uiso 1 1 calc R . . H55B H 0.2203 0.5841 0.2251 0.154 Uiso 1 1 calc R . . H55C H 0.2135 0.5584 0.2824 0.154 Uiso 1 1 calc R . . C56 C 0.2234(3) 0.7918(4) 0.3294(4) 0.089(3) Uani 1 1 d . . . H56A H 0.2500 0.8261 0.3472 0.133 Uiso 1 1 calc R . . H56B H 0.1974 0.7782 0.3529 0.133 Uiso 1 1 calc R . . H56C H 0.1963 0.8054 0.2939 0.133 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 Zn 0.0247(3) 0.0427(4) 0.0518(4) -0.0019(3) -0.0057(3) -0.0002(3) Ni 0.0246(4) 0.0480(5) 0.0619(6) 0.0002(4) 0.0007(3) -0.0033(3) O1 0.033(2) 0.058(3) 0.094(4) 0.000(3) -0.004(2) -0.0096(19) O2 0.034(2) 0.062(3) 0.072(3) 0.002(2) 0.003(2) 0.0025(19) N1 0.024(2) 0.038(3) 0.060(3) -0.005(2) -0.002(2) -0.0036(19) N2 0.028(2) 0.046(3) 0.053(3) -0.006(2) 0.002(2) -0.004(2) N3 0.030(2) 0.038(2) 0.051(3) -0.003(2) -0.003(2) 0.0003(19) N4 0.030(3) 0.040(3) 0.047(3) -0.005(2) -0.005(2) -0.0026(19) N5 0.028(2) 0.042(3) 0.044(3) 0.003(2) -0.003(2) 0.0002(19) N6 0.023(2) 0.048(3) 0.049(3) 0.001(2) 0.000(2) -0.0011(19) C1 0.031(3) 0.038(3) 0.036(3) 0.001(2) 0.001(2) -0.002(2) C2 0.032(3) 0.044(3) 0.036(3) 0.000(3) 0.002(2) -0.001(2) C3 0.028(3) 0.047(3) 0.050(4) -0.001(3) -0.001(3) -0.001(2) C4 0.066(5) 0.051(4) 0.064(5) 0.000(3) 0.018(4) -0.001(3) C5 0.080(6) 0.048(4) 0.105(7) 0.005(4) 0.032(5) -0.001(4) C6 0.054(4) 0.050(4) 0.090(6) -0.017(4) 0.016(4) -0.015(3) C7 0.045(4) 0.075(5) 0.073(5) -0.029(4) 0.013(4) -0.002(3) C8 0.046(4) 0.057(4) 0.060(5) -0.003(3) 0.008(3) 0.003(3) C9 0.148(9) 0.071(5) 0.081(6) 0.007(5) 0.062(6) -0.009(5) C10 0.087(6) 0.054(4) 0.158(10) -0.043(5) 0.023(6) -0.002(4) C11 0.146(9) 0.085(6) 0.087(7) -0.002(5) 0.063(6) 0.002(6) C12 0.024(3) 0.039(3) 0.058(4) 0.002(3) -0.001(3) -0.001(2) C13 0.031(3) 0.054(4) 0.065(5) 0.009(3) -0.009(3) -0.007(3) C14 0.042(4) 0.064(4) 0.076(5) 0.020(4) -0.004(3) -0.007(3) C15 0.047(4) 0.051(4) 0.089(6) 0.002(4) -0.011(4) 0.005(3) C16 0.037(4) 0.058(4) 0.097(6) -0.019(4) 0.005(4) 0.002(3) C17 0.028(3) 0.057(4) 0.069(5) -0.011(3) 0.005(3) 0.002(3) C18 0.081(5) 0.071(5) 0.058(5) 0.006(4) 0.013(4) -0.004(4) C19 0.096(7) 0.050(4) 0.147(9) 0.004(5) -0.011(6) 0.007(4) C20 0.058(4) 0.072(5) 0.078(6) -0.012(4) 0.027(4) 0.003(4) C21 0.029(3) 0.046(3) 0.040(3) -0.007(3) -0.003(2) -0.001(2) C22 0.111(7) 0.053(4) 0.058(5) 0.002(4) 0.028(4) 0.016(4) C23 0.123(8) 0.053(4) 0.074(6) 0.003(4) 0.028(5) 0.020(5) C24 0.059(4) 0.055(4) 0.075(5) -0.013(4) -0.012(4) 0.016(3) C25 0.076(5) 0.068(5) 0.069(5) -0.019(4) 0.026(4) 0.003(4) C26 0.074(5) 0.056(4) 0.062(5) -0.005(4) 0.014(4) -0.002(3) C27 0.123(8) 0.066(5) 0.100(7) -0.017(5) 0.000(6) 0.029(5) C28 0.031(3) 0.038(3) 0.053(4) 0.001(3) -0.004(3) 0.003(2) C29 0.050(4) 0.048(4) 0.061(4) -0.002(3) 0.005(3) 0.000(3) C30 0.057(4) 0.044(4) 0.081(6) 0.006(4) -0.005(4) -0.002(3) C31 0.057(5) 0.049(4) 0.088(6) -0.017(4) -0.002(4) 0.004(3) C32 0.062(5) 0.062(5) 0.068(5) -0.026(4) -0.001(4) 0.011(3) C33 0.046(4) 0.061(4) 0.052(4) -0.004(3) 0.005(3) 0.008(3) C34 0.114(8) 0.056(5) 0.126(8) -0.031(5) 0.013(6) -0.003(5) C35 0.028(3) 0.031(3) 0.045(3) 0.000(2) -0.001(2) 0.000(2) C36 0.053(4) 0.051(4) 0.047(4) 0.004(3) 0.000(3) -0.004(3) C37 0.027(3) 0.045(3) 0.045(4) 0.001(3) -0.001(2) -0.006(2) C38 0.048(4) 0.057(4) 0.047(4) -0.006(3) -0.001(3) -0.002(3) C39 0.059(4) 0.056(4) 0.066(5) -0.006(4) 0.006(4) 0.001(3) C40 0.069(5) 0.066(5) 0.059(5) -0.013(4) 0.007(4) -0.012(4) C41 0.056(4) 0.070(5) 0.043(4) 0.013(3) -0.004(3) -0.008(3) C42 0.089(6) 0.053(4) 0.074(5) 0.004(4) 0.001(4) 0.016(4) C43 0.090(6) 0.110(7) 0.073(6) -0.020(5) 0.034(5) -0.018(5) C44 0.061(5) 0.077(5) 0.070(5) 0.019(4) 0.000(4) 0.009(4) C45 0.041(3) 0.046(3) 0.050(4) 0.008(3) 0.009(3) 0.009(3) C46 0.052(4) 0.066(4) 0.094(6) 0.006(4) 0.037(4) -0.002(3) C47 0.086(7) 0.080(6) 0.161(10) 0.013(6) 0.077(7) 0.006(5) C48 0.105(8) 0.101(7) 0.110(8) 0.026(6) 0.072(7) 0.031(6) C49 0.079(6) 0.082(5) 0.056(5) -0.006(4) 0.015(4) 0.033(5) C50 0.045(4) 0.076(5) 0.049(4) 0.001(4) -0.005(3) 0.008(3) C51 0.205(14) 0.125(9) 0.199(14) -0.001(9) 0.164(13) 0.022(9) C52 0.035(4) 0.069(5) 0.086(6) 0.017(4) -0.006(3) -0.017(3) C53 0.023(3) 0.075(5) 0.102(6) 0.018(4) 0.000(3) -0.002(3) C54 0.033(3) 0.072(5) 0.068(5) 0.009(4) 0.006(3) -0.003(3) C55 0.045(4) 0.072(5) 0.154(9) 0.010(5) -0.034(5) -0.025(4) C56 0.040(4) 0.103(6) 0.117(7) -0.004(5) 0.011(4) 0.015(4) _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 Zn N5 1.996(5) . ? Zn N6 2.000(5) . ? Zn N3 2.002(4) . ? Zn N4 2.007(4) . ? Ni O1 1.840(4) . ? Ni O2 1.864(4) . ? Ni N2 1.885(4) . ? Ni N1 1.897(4) . ? O1 C52 1.290(7) . ? O2 C54 1.279(7) . ? N1 C1 1.309(6) . ? N1 C3 1.434(7) . ? N2 C2 1.312(7) . ? N2 C12 1.443(7) . ? N3 C1 1.334(7) . ? N3 C21 1.428(7) . ? N4 C2 1.344(7) . ? N4 C28 1.447(7) . ? N5 C35 1.343(7) . ? N5 C37 1.422(8) . ? N6 C35 1.338(7) 2_656 ? N6 C45 1.423(8) . ? C1 C2 1.524(8) . ? C3 C4 1.390(9) . ? C3 C8 1.396(9) . ? C4 C5 1.392(10) . ? C4 C9 1.526(11) . ? C5 C6 1.369(11) . ? C6 C7 1.352(11) . ? C6 C10 1.541(9) . ? C7 C8 1.406(9) . ? C8 C11 1.525(11) . ? C12 C17 1.394(9) . ? C12 C13 1.414(9) . ? C13 C14 1.408(9) . ? C13 C18 1.528(10) . ? C14 C15 1.360(11) . ? C15 C16 1.384(11) . ? C15 C19 1.527(10) . ? C16 C17 1.409(9) . ? C17 C20 1.476(10) . ? C21 C26 1.372(9) . ? C21 C22 1.376(9) . ? C22 C23 1.371(9) . ? C23 C24 1.383(11) . ? C24 C25 1.372(11) . ? C24 C27 1.533(10) . ? C25 C26 1.389(10) . ? C28 C33 1.380(9) . ? C28 C29 1.396(9) . ? C29 C30 1.398(9) . ? C30 C31 1.387(11) . ? C31 C32 1.378(11) . ? C31 C34 1.531(10) . ? C32 C33 1.383(9) . ? C35 N6 1.338(7) 2_656 ? C35 C35 1.518(12) 2_656 ? C36 C37 1.397(8) . ? C36 C41 1.406(10) . ? C36 C44 1.476(9) . ? C37 C38 1.411(8) . ? C38 C39 1.385(10) . ? C38 C42 1.551(10) . ? C39 C40 1.405(10) . ? C40 C41 1.356(10) . ? C40 C43 1.519(10) . ? C45 C46 1.395(9) . ? C45 C50 1.416(9) . ? C46 C47 1.386(11) . ? C47 C48 1.421(14) . ? C48 C49 1.358(12) . ? C48 C51 1.554(12) . ? C49 C50 1.395(10) . ? C52 C53 1.373(10) . ? C52 C55 1.520(10) . ? C53 C54 1.372(10) . ? C54 C56 1.512(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Zn N6 83.88(19) . . ? N5 Zn N3 119.67(19) . . ? N6 Zn N3 125.06(19) . . ? N5 Zn N4 134.18(19) . . ? N6 Zn N4 115.73(19) . . ? N3 Zn N4 83.92(18) . . ? O1 Ni O2 94.5(2) . . ? O1 Ni N2 172.8(2) . . ? O2 Ni N2 91.5(2) . . ? O1 Ni N1 90.67(19) . . ? O2 Ni N1 172.6(2) . . ? N2 Ni N1 83.75(19) . . ? C52 O1 Ni 126.1(5) . . ? C54 O2 Ni 125.7(5) . . ? C1 N1 C3 123.2(4) . . ? C1 N1 Ni 115.6(4) . . ? C3 N1 Ni 121.1(3) . . ? C2 N2 C12 121.6(5) . . ? C2 N2 Ni 115.2(4) . . ? C12 N2 Ni 121.0(3) . . ? C1 N3 C21 125.3(4) . . ? C1 N3 Zn 112.4(3) . . ? C21 N3 Zn 122.3(3) . . ? C2 N4 C28 123.8(4) . . ? C2 N4 Zn 111.9(3) . . ? C28 N4 Zn 122.9(3) . . ? C35 N5 C37 123.9(5) . . ? C35 N5 Zn 112.1(4) . . ? C37 N5 Zn 122.1(3) . . ? C35 N6 C45 125.3(5) 2_656 . ? C35 N6 Zn 112.8(4) 2_656 . ? C45 N6 Zn 120.5(3) . . ? N1 C1 N3 132.4(5) . . ? N1 C1 C2 111.7(4) . . ? N3 C1 C2 115.8(4) . . ? N2 C2 N4 131.5(5) . . ? N2 C2 C1 113.1(5) . . ? N4 C2 C1 115.3(5) . . ? C4 C3 C8 120.0(6) . . ? C4 C3 N1 120.3(6) . . ? C8 C3 N1 119.6(6) . . ? C5 C4 C3 118.9(7) . . ? C5 C4 C9 120.8(7) . . ? C3 C4 C9 120.3(6) . . ? C6 C5 C4 122.1(7) . . ? C7 C6 C5 118.3(7) . . ? C7 C6 C10 123.0(8) . . ? C5 C6 C10 118.7(8) . . ? C6 C7 C8 122.7(7) . . ? C3 C8 C7 117.9(7) . . ? C3 C8 C11 120.4(6) . . ? C7 C8 C11 121.7(7) . . ? C17 C12 C13 121.5(6) . . ? C17 C12 N2 121.7(6) . . ? C13 C12 N2 116.8(6) . . ? C14 C13 C12 117.7(7) . . ? C14 C13 C18 120.8(7) . . ? C12 C13 C18 121.4(6) . . ? C15 C14 C13 122.3(8) . . ? C14 C15 C16 118.2(7) . . ? C14 C15 C19 120.1(9) . . ? C16 C15 C19 121.6(8) . . ? C15 C16 C17 123.3(7) . . ? C12 C17 C16 116.7(7) . . ? C12 C17 C20 120.9(6) . . ? C16 C17 C20 122.4(7) . . ? C26 C21 C22 117.6(6) . . ? C26 C21 N3 120.9(6) . . ? C22 C21 N3 121.3(6) . . ? C23 C22 C21 120.7(7) . . ? C22 C23 C24 122.1(8) . . ? C25 C24 C23 117.0(7) . . ? C25 C24 C27 121.5(8) . . ? C23 C24 C27 121.5(8) . . ? C24 C25 C26 121.0(7) . . ? C21 C26 C25 121.3(7) . . ? C33 C28 C29 118.7(6) . . ? C33 C28 N4 121.1(6) . . ? C29 C28 N4 120.1(6) . . ? C28 C29 C30 119.5(7) . . ? C31 C30 C29 121.3(7) . . ? C32 C31 C30 118.2(6) . . ? C32 C31 C34 122.3(8) . . ? C30 C31 C34 119.6(8) . . ? C31 C32 C33 121.2(7) . . ? C28 C33 C32 120.9(7) . . ? N6 C35 N5 129.2(6) 2_656 . ? N6 C35 C35 114.9(6) 2_656 2_656 ? N5 C35 C35 115.9(6) . 2_656 ? C37 C36 C41 118.4(6) . . ? C37 C36 C44 120.4(6) . . ? C41 C36 C44 121.2(6) . . ? C36 C37 C38 119.1(6) . . ? C36 C37 N5 119.4(5) . . ? C38 C37 N5 121.2(5) . . ? C39 C38 C37 119.6(6) . . ? C39 C38 C42 118.9(6) . . ? C37 C38 C42 121.1(6) . . ? C38 C39 C40 122.2(7) . . ? C41 C40 C39 116.6(7) . . ? C41 C40 C43 122.8(7) . . ? C39 C40 C43 120.6(7) . . ? C40 C41 C36 124.1(6) . . ? C46 C45 C50 118.2(7) . . ? C46 C45 N6 118.2(6) . . ? C50 C45 N6 122.8(6) . . ? C47 C46 C45 120.6(8) . . ? C46 C47 C48 121.0(9) . . ? C49 C48 C47 117.8(8) . . ? C49 C48 C51 121.7(11) . . ? C47 C48 C51 120.5(10) . . ? C48 C49 C50 122.5(8) . . ? C49 C50 C45 119.8(7) . . ? O1 C52 C53 124.6(7) . . ? O1 C52 C55 112.9(7) . . ? C53 C52 C55 122.4(6) . . ? C54 C53 C52 123.6(6) . . ? O2 C54 C53 125.0(7) . . ? O2 C54 C56 113.6(6) . . ? C53 C54 C56 121.4(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.927 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.091