# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2314 _publ_requested_journal 'Dalton' _publ_section_title ; Novel nickel(II) complexes with diazamesocyclic ligands functionalized by additioonal phenol donor pendant(s): synthesis, characterization, crystal structures and magnetic properties ; _publ_contact_author ; Xian-He Bu Department of Chemistry, Nankai University, Tianjin 300071,China ; _publ_contact_author_email 'buxh@nankai.edu.cn' data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H39 N10 Ni2 O2.5' _chemical_formula_weight 649.35 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.311(2) _cell_length_b 16.542(3) _cell_length_c 13.407(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.851(4) _cell_angle_gamma 90.00 _cell_volume 2916.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour green _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1374 _exptl_absorpt_coefficient_mu 1.338 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11942 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5135 _reflns_number_gt 3086 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0877P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5135 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1343 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _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 0.03669(5) 0.08905(4) 0.51973(4) 0.0298(2) Uani 1 1 d . . . O1 O -0.0324(3) 0.0184(2) 0.4083(2) 0.0354(8) Uani 1 1 d . . . O2 O 0.5653(3) 0.0293(2) -0.0493(3) 0.0514(10) Uani 1 1 d . . . Ni2 Ni 0.49667(5) 0.08161(4) 0.05612(5) 0.0404(2) Uani 1 1 d . . . O3 O -0.5000 0.0000 0.5000 0.30(3) Uani 0.50 2 d SP . . O3' O -0.4197(9) 0.0210(10) 0.6268(11) 0.202(6) Uani 0.75 1 d P . . C10 C -0.0345(4) 0.1851(3) 0.3405(4) 0.0385(13) Uani 1 1 d . . . H10A H -0.0943 0.1881 0.3736 0.046 Uiso 1 1 calc R . . H10B H -0.0328 0.2335 0.3000 0.046 Uiso 1 1 calc R . . N11 N 0.0590(3) 0.1835(2) 0.4203(3) 0.0348(10) Uani 1 1 d . . . C11 C -0.0442(4) 0.1127(3) 0.2719(4) 0.0334(12) Uani 1 1 d . . . N12 N 0.1691(3) 0.1311(3) 0.6041(3) 0.0400(11) Uani 1 1 d . . . H12B H 0.1817 0.0996 0.6603 0.048 Uiso 1 1 calc R . . C12 C -0.0609(4) 0.1269(3) 0.1673(4) 0.0425(14) Uani 1 1 d . . . H12A H -0.0625 0.1798 0.1437 0.051 Uiso 1 1 calc R . . N13 N -0.0749(4) 0.1453(3) 0.5793(4) 0.0479(12) Uani 1 1 d . . . C13 C -0.0749(5) 0.0642(4) 0.0992(4) 0.0493(16) Uani 1 1 d . . . H13B H -0.0864 0.0747 0.0302 0.059 Uiso 1 1 calc R . . N14 N -0.1608(5) 0.1290(3) 0.5517(4) 0.0593(14) Uani 1 1 d . . . C14 C -0.0717(4) -0.0140(3) 0.1340(4) 0.0454(14) Uani 1 1 d . . . H14A H -0.0808 -0.0567 0.0884 0.054 Uiso 1 1 calc R . . C15 C -0.0550(4) -0.0296(3) 0.2377(4) 0.0416(14) Uani 1 1 d . . . H15A H -0.0517 -0.0828 0.2606 0.050 Uiso 1 1 calc R . . N15 N -0.2450(6) 0.1129(6) 0.5292(7) 0.124(3) Uani 1 1 d . . . C16 C -0.0431(4) 0.0336(3) 0.3071(3) 0.0321(12) Uani 1 1 d . . . C21 C 0.0589(4) 0.2634(3) 0.4710(4) 0.0430(14) Uani 1 1 d . . . H21A H -0.0035 0.2687 0.4995 0.052 Uiso 1 1 calc R . . H21B H 0.0592 0.3056 0.4208 0.052 Uiso 1 1 calc R . . N21 N 0.4900(4) 0.1022(3) 0.2064(4) 0.0591(14) Uani 1 1 d . . . H21C H 0.4493 0.0636 0.2274 0.071 Uiso 1 1 calc R . . C22 C 0.1486(5) 0.2766(3) 0.5543(4) 0.0521(16) Uani 1 1 d . . . H22A H 0.2105 0.2764 0.5244 0.062 Uiso 1 1 calc R . . H22B H 0.1422 0.3297 0.5833 0.062 Uiso 1 1 calc R . . N22 N 0.5861(4) 0.1855(3) 0.0625(4) 0.0565(13) Uani 1 1 d . . . C23 C 0.1593(4) 0.2148(3) 0.6384(4) 0.0468(15) Uani 1 1 d . . . H23A H 0.2187 0.2281 0.6871 0.056 Uiso 1 1 calc R . . H23B H 0.1003 0.2183 0.6727 0.056 Uiso 1 1 calc R . . N23 N 0.3740(5) 0.1401(4) -0.0220(5) 0.086(2) Uani 1 1 d . . . C24 C 0.2548(5) 0.1186(4) 0.5463(4) 0.0572(17) Uani 1 1 d . . . H24A H 0.2948 0.0726 0.5742 0.069 Uiso 1 1 calc R . . H24B H 0.2985 0.1659 0.5541 0.069 Uiso 1 1 calc R . . N24 N 0.3454(5) 0.1305(4) -0.1064(5) 0.0707(17) Uani 1 1 d . . . C25 C 0.2182(5) 0.1039(4) 0.4329(4) 0.0550(17) Uani 1 1 d . . . H25A H 0.2776 0.0964 0.4000 0.066 Uiso 1 1 calc R . . H25B H 0.1801 0.0537 0.4259 0.066 Uiso 1 1 calc R . . N25 N 0.3154(6) 0.1233(5) -0.1880(6) 0.121(3) Uani 1 1 d . . . C26 C 0.1537(4) 0.1686(4) 0.3777(4) 0.0464(15) Uani 1 1 d . . . H26A H 0.1927 0.2183 0.3804 0.056 Uiso 1 1 calc R . . H26B H 0.1362 0.1532 0.3074 0.056 Uiso 1 1 calc R . . C30 C 0.6061(5) 0.2014(4) -0.0432(5) 0.0643(18) Uani 1 1 d . . . H30A H 0.5412 0.2056 -0.0871 0.077 Uiso 1 1 calc R . . H30B H 0.6397 0.2534 -0.0440 0.077 Uiso 1 1 calc R . . C31 C 0.6691(4) 0.1397(4) -0.0863(4) 0.0417(13) Uani 1 1 d . . . C32 C 0.7509(4) 0.1668(4) -0.1309(4) 0.0550(16) Uani 1 1 d . . . H32A H 0.7663 0.2216 -0.1302 0.066 Uiso 1 1 calc R . . C33 C 0.8101(5) 0.1122(5) -0.1766(5) 0.0624(18) Uani 1 1 d . . . H33A H 0.8629 0.1310 -0.2085 0.075 Uiso 1 1 calc R . . C34 C 0.7902(5) 0.0314(5) -0.1743(5) 0.0617(18) Uani 1 1 d . . . H34A H 0.8304 -0.0050 -0.2035 0.074 Uiso 1 1 calc R . . C35 C 0.7110(4) 0.0038(4) -0.1290(4) 0.0534(16) Uani 1 1 d . . . H35A H 0.7002 -0.0516 -0.1257 0.064 Uiso 1 1 calc R . . C36 C 0.6457(4) 0.0569(4) -0.0875(4) 0.0437(14) Uani 1 1 d . . . C41 C 0.4453(5) 0.1817(4) 0.2228(5) 0.0623(18) Uani 1 1 d . . . H41A H 0.3804 0.1862 0.1790 0.075 Uiso 1 1 calc R . . H41B H 0.4324 0.1845 0.2919 0.075 Uiso 1 1 calc R . . C42 C 0.5076(6) 0.2497(5) 0.2043(5) 0.080(2) Uani 1 1 d . . . H42A H 0.5713 0.2463 0.2503 0.096 Uiso 1 1 calc R . . H42B H 0.4736 0.2988 0.2202 0.096 Uiso 1 1 calc R . . C43 C 0.5320(6) 0.2567(5) 0.0943(6) 0.077(2) Uani 1 1 d . . . H43A H 0.4688 0.2637 0.0483 0.092 Uiso 1 1 calc R . . H43B H 0.5732 0.3045 0.0895 0.092 Uiso 1 1 calc R . . C44 C 0.6814(5) 0.1704(4) 0.1334(5) 0.0651(19) Uani 1 1 d . . . H44A H 0.6951 0.2165 0.1781 0.078 Uiso 1 1 calc R . . H44B H 0.7373 0.1655 0.0951 0.078 Uiso 1 1 calc R . . C45 C 0.6768(5) 0.0959(5) 0.1953(6) 0.071(2) Uani 1 1 d . . . H45A H 0.6690 0.0503 0.1493 0.085 Uiso 1 1 calc R . . H45B H 0.7424 0.0899 0.2375 0.085 Uiso 1 1 calc R . . C46 C 0.5984(5) 0.0881(5) 0.2615(5) 0.075(2) Uani 1 1 d . . . H46A H 0.6126 0.1267 0.3163 0.090 Uiso 1 1 calc R . . H46B H 0.6024 0.0343 0.2908 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0376(4) 0.0333(4) 0.0183(3) 0.0032(3) 0.0042(3) 0.0019(3) O1 0.056(2) 0.0376(19) 0.0121(16) 0.0068(14) 0.0040(15) -0.0009(17) O2 0.049(2) 0.067(3) 0.043(2) -0.012(2) 0.0231(19) -0.014(2) Ni2 0.0340(4) 0.0606(5) 0.0270(4) -0.0044(3) 0.0061(3) 0.0009(3) O3 0.45(5) 0.30(4) 0.21(3) 0.17(3) 0.22(4) 0.30(4) O3' 0.151(10) 0.305(17) 0.169(12) 0.055(12) 0.086(9) 0.042(10) C10 0.049(3) 0.043(3) 0.024(3) 0.011(2) 0.005(2) 0.011(3) N11 0.044(3) 0.038(2) 0.024(2) 0.0012(18) 0.0059(19) 0.000(2) C11 0.041(3) 0.039(3) 0.020(3) 0.006(2) 0.002(2) 0.008(2) N12 0.038(3) 0.052(3) 0.029(2) 0.003(2) 0.0002(19) -0.005(2) C12 0.056(4) 0.043(3) 0.028(3) 0.014(3) 0.004(3) 0.004(3) N13 0.052(3) 0.055(3) 0.041(3) 0.001(2) 0.020(2) 0.013(3) C13 0.073(4) 0.059(4) 0.015(3) 0.007(3) 0.002(3) 0.002(3) N14 0.049(4) 0.075(4) 0.055(3) 0.007(3) 0.013(3) 0.018(3) C14 0.068(4) 0.046(3) 0.022(3) -0.003(2) 0.009(3) 0.006(3) C15 0.057(4) 0.043(3) 0.023(3) 0.005(2) 0.003(2) 0.005(3) N15 0.056(5) 0.163(8) 0.149(8) -0.012(6) -0.001(5) 0.010(5) C16 0.035(3) 0.045(3) 0.016(2) 0.004(2) 0.003(2) 0.005(2) C21 0.065(4) 0.032(3) 0.033(3) 0.004(2) 0.008(3) -0.002(3) N21 0.063(4) 0.077(4) 0.038(3) -0.008(3) 0.012(3) -0.008(3) C22 0.067(4) 0.048(3) 0.042(4) -0.009(3) 0.011(3) -0.020(3) N22 0.054(3) 0.071(3) 0.044(3) -0.002(3) 0.007(3) 0.010(3) C23 0.049(4) 0.058(4) 0.030(3) -0.006(3) -0.004(3) -0.012(3) N23 0.081(5) 0.108(5) 0.063(4) -0.008(4) -0.006(3) 0.042(4) C24 0.040(4) 0.085(5) 0.045(4) 0.004(3) 0.000(3) -0.002(3) N24 0.071(4) 0.092(5) 0.043(4) 0.013(3) -0.011(3) 0.006(3) C25 0.046(4) 0.081(5) 0.040(4) 0.001(3) 0.015(3) 0.007(3) N25 0.124(6) 0.144(7) 0.075(5) 0.040(5) -0.049(5) -0.012(6) C26 0.052(4) 0.060(4) 0.029(3) -0.001(3) 0.013(3) -0.010(3) C30 0.059(4) 0.082(5) 0.051(4) 0.016(4) 0.005(3) -0.002(4) C31 0.036(3) 0.059(4) 0.031(3) 0.003(3) 0.007(2) 0.007(3) C32 0.043(4) 0.076(4) 0.045(4) 0.010(3) 0.004(3) -0.005(3) C33 0.049(4) 0.095(6) 0.049(4) 0.004(4) 0.023(3) -0.008(4) C34 0.047(4) 0.089(5) 0.054(4) -0.020(4) 0.022(3) -0.004(4) C35 0.043(4) 0.070(4) 0.048(4) -0.010(3) 0.011(3) -0.006(3) C36 0.031(3) 0.076(4) 0.024(3) -0.006(3) 0.005(2) -0.003(3) C41 0.056(4) 0.083(5) 0.049(4) -0.013(4) 0.012(3) 0.010(4) C42 0.086(6) 0.091(6) 0.068(5) -0.031(4) 0.031(4) 0.003(5) C43 0.070(5) 0.075(5) 0.085(6) 0.002(4) 0.012(4) 0.006(4) C44 0.054(4) 0.093(5) 0.045(4) -0.001(4) -0.002(3) 0.013(4) C45 0.053(4) 0.094(6) 0.065(5) -0.023(4) 0.006(3) -0.010(4) C46 0.067(5) 0.122(6) 0.034(4) -0.003(4) -0.003(3) 0.003(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. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.004(3) . ? Ni1 N13 2.017(5) . ? Ni1 O1 2.028(3) 3_556 ? Ni1 N12 2.065(4) . ? Ni1 N11 2.105(4) . ? Ni1 Ni1 3.1232(13) 3_556 ? O1 C16 1.369(5) . ? O1 Ni1 2.028(3) 3_556 ? O2 C36 1.334(6) . ? O2 Ni2 1.996(4) . ? O2 Ni2 2.008(4) 3_655 ? Ni2 O2 2.008(4) 3_655 ? Ni2 N23 2.042(6) . ? Ni2 N21 2.057(5) . ? Ni2 N22 2.085(5) . ? C10 C11 1.501(7) . ? C10 N11 1.511(6) . ? N11 C26 1.482(7) . ? N11 C21 1.489(6) . ? C11 C16 1.389(7) . ? C11 C12 1.404(7) . ? N12 C23 1.470(7) . ? N12 C24 1.490(7) . ? C12 C13 1.377(8) . ? N13 N14 1.180(7) . ? C13 C14 1.374(8) . ? N14 N15 1.148(8) . ? C14 C15 1.396(7) . ? C15 C16 1.392(7) . ? C21 C22 1.518(7) . ? N21 C41 1.475(8) . ? N21 C46 1.534(8) . ? C22 C23 1.512(7) . ? N22 C43 1.479(8) . ? N22 C44 1.484(7) . ? N22 C30 1.505(8) . ? N23 N24 1.149(8) . ? C24 C25 1.542(8) . ? N24 N25 1.111(8) . ? C25 C26 1.495(8) . ? C30 C31 1.493(8) . ? C31 C32 1.395(8) . ? C31 C36 1.403(8) . ? C32 C33 1.399(9) . ? C33 C34 1.362(9) . ? C34 C35 1.371(8) . ? C35 C36 1.413(8) . ? C41 C42 1.443(9) . ? C42 C43 1.560(9) . ? C44 C45 1.491(9) . ? C45 C46 1.479(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 N13 106.47(19) . . ? O1 Ni1 O1 78.43(13) . 3_556 ? N13 Ni1 O1 98.01(17) . 3_556 ? O1 Ni1 N12 149.35(16) . . ? N13 Ni1 N12 104.2(2) . . ? O1 Ni1 N12 96.88(16) 3_556 . ? O1 Ni1 N11 93.07(14) . . ? N13 Ni1 N11 95.32(18) . . ? O1 Ni1 N11 165.78(15) 3_556 . ? C16 O1 Ni1 126.8(3) . . ? C16 O1 Ni1 128.8(3) . 3_556 ? Ni1 O1 Ni1 101.57(13) . 3_556 ? C36 O2 Ni2 127.1(4) . . ? C36 O2 Ni2 130.1(4) . 3_655 ? Ni2 O2 Ni2 101.44(16) . 3_655 ? O2 Ni2 O2 78.56(16) . 3_655 ? O2 Ni2 N23 105.0(2) . . ? O2 Ni2 N23 96.9(2) 3_655 . ? O2 Ni2 N21 149.2(2) . . ? O2 Ni2 N21 96.65(18) 3_655 . ? N23 Ni2 N21 105.7(2) . . ? O2 Ni2 N22 93.77(18) . . ? O2 Ni2 N22 169.45(18) 3_655 . ? N23 Ni2 N22 92.1(3) . . ? N21 Ni2 N22 86.2(2) . . ? C11 C10 N11 113.8(4) . . ? C26 N11 C21 112.6(4) . . ? C26 N11 C10 112.8(4) . . ? C21 N11 C10 104.6(4) . . ? C26 N11 Ni1 109.4(3) . . ? C21 N11 Ni1 111.0(3) . . ? C10 N11 Ni1 106.3(3) . . ? C16 C11 C12 119.1(5) . . ? C16 C11 C10 123.2(4) . . ? C12 C11 C10 117.6(4) . . ? C23 N12 C24 113.9(5) . . ? C23 N12 Ni1 112.3(3) . . ? C24 N12 Ni1 109.0(3) . . ? C13 C12 C11 121.4(5) . . ? N14 N13 Ni1 120.6(4) . . ? C14 C13 C12 119.4(5) . . ? N15 N14 N13 177.3(8) . . ? C13 C14 C15 120.2(5) . . ? C16 C15 C14 120.7(5) . . ? O1 C16 C11 120.2(4) . . ? O1 C16 C15 120.6(4) . . ? C11 C16 C15 119.2(4) . . ? N11 C21 C22 114.1(4) . . ? C41 N21 C46 115.8(5) . . ? C41 N21 Ni2 111.9(4) . . ? C46 N21 Ni2 105.6(4) . . ? C23 C22 C21 115.1(4) . . ? C43 N22 C44 110.8(5) . . ? C43 N22 C30 107.2(5) . . ? C44 N22 C30 112.0(5) . . ? C43 N22 Ni2 111.6(4) . . ? C44 N22 Ni2 108.3(4) . . ? C30 N22 Ni2 106.9(4) . . ? N12 C23 C22 114.0(4) . . ? N24 N23 Ni2 123.8(5) . . ? N12 C24 C25 112.7(5) . . ? N25 N24 N23 177.5(9) . . ? C26 C25 C24 116.4(5) . . ? N11 C26 C25 112.8(4) . . ? C31 C30 N22 115.8(5) . . ? C32 C31 C36 119.6(5) . . ? C32 C31 C30 117.9(6) . . ? C36 C31 C30 122.4(5) . . ? C31 C32 C33 120.7(6) . . ? C34 C33 C32 119.8(6) . . ? C33 C34 C35 120.2(6) . . ? C34 C35 C36 121.9(6) . . ? O2 C36 C31 121.3(5) . . ? O2 C36 C35 121.1(6) . . ? C31 C36 C35 117.5(5) . . ? C42 C41 N21 114.4(6) . . ? C41 C42 C43 115.4(6) . . ? N22 C43 C42 113.2(6) . . ? N22 C44 C45 113.0(6) . . ? C46 C45 C44 119.9(7) . . ? C45 C46 N21 113.3(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.832 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.096 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H60 Cl2 N4 Ni3 O6' _chemical_formula_weight 987.99 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.0715(16) _cell_length_b 14.343(2) _cell_length_c 14.691(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.052(3) _cell_angle_gamma 90.00 _cell_volume 2205.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 1.440 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9840 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_sigmaI/netI 0.1096 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.39 _reflns_number_total 4331 _reflns_number_gt 2434 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1080P)^2^+5.4379P] 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 4331 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1464 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.2078 _refine_ls_wR_factor_gt 0.1599 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.205 _refine_ls_shift/su_mean 0.010 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 0.85739(9) 0.67848(6) 0.53404(6) 0.0387(3) Uani 1 1 d . . . Ni2 Ni 1.0000 0.5000 0.5000 0.0374(4) Uani 1 2 d S . . Cl1 Cl 0.8979(2) 0.65193(15) 0.69822(13) 0.0589(6) Uani 1 1 d . . . O1 O 1.0252(5) 0.6428(3) 0.5159(3) 0.0452(12) Uani 1 1 d . . . O2 O 0.8186(5) 0.5473(3) 0.4837(3) 0.0410(11) Uani 1 1 d . . . N1 N 0.8984(7) 0.8223(4) 0.5391(4) 0.0510(16) Uani 1 1 d . . . N2 N 0.6661(6) 0.7177(4) 0.4988(4) 0.0469(15) Uani 1 1 d . . . C1 C 1.0992(7) 0.7001(5) 0.4836(5) 0.0426(18) Uani 1 1 d . . . C2 C 1.1702(8) 0.6683(6) 0.4270(6) 0.055(2) Uani 1 1 d . . . H2A H 1.1701 0.6052 0.4124 0.066 Uiso 1 1 calc R . . C3 C 1.2404(8) 0.7299(6) 0.3928(6) 0.060(2) Uani 1 1 d . . . H3A H 1.2856 0.7073 0.3541 0.072 Uiso 1 1 calc R . . C4 C 1.2462(9) 0.8220(7) 0.4131(7) 0.069(3) Uani 1 1 d . . . H4A H 1.2925 0.8625 0.3876 0.082 Uiso 1 1 calc R . . C5 C 1.1823(9) 0.8538(6) 0.4721(7) 0.065(3) Uani 1 1 d . . . H5A H 1.1897 0.9164 0.4897 0.078 Uiso 1 1 calc R . . C6 C 1.1056(7) 0.7952(5) 0.5071(6) 0.0492(19) Uani 1 1 d . . . C7 C 1.0407(9) 0.8330(5) 0.5738(6) 0.061(2) Uani 1 1 d . . . H7A H 1.0611 0.8987 0.5843 0.074 Uiso 1 1 calc R . . H7B H 1.0750 0.8016 0.6355 0.074 Uiso 1 1 calc R . . C8 C 0.5911(7) 0.6309(6) 0.4974(5) 0.0486(19) Uani 1 1 d . . . H8A H 0.6241 0.6017 0.5602 0.058 Uiso 1 1 calc R . . H8B H 0.5032 0.6485 0.4878 0.058 Uiso 1 1 calc R . . C9 C 0.8379(9) 0.8601(5) 0.4397(6) 0.056(2) Uani 1 1 d . . . H9A H 0.9042 0.8727 0.4115 0.067 Uiso 1 1 calc R . . H9B H 0.7963 0.9187 0.4438 0.067 Uiso 1 1 calc R . . C10 C 0.7416(8) 0.7952(6) 0.3748(6) 0.052(2) Uani 1 1 d . . . H10A H 0.7516 0.7740 0.3179 0.062 Uiso 1 1 calc R . . C11 C 0.6272(8) 0.7645(6) 0.4033(5) 0.052(2) Uani 1 1 d . . . H11A H 0.5754 0.8186 0.4051 0.062 Uiso 1 1 calc R . . H11B H 0.5752 0.7221 0.3549 0.062 Uiso 1 1 calc R . . C12 C 0.8491(10) 0.8709(6) 0.6090(6) 0.067(3) Uani 1 1 d . . . H12A H 0.8803 0.9346 0.6158 0.080 Uiso 1 1 calc R . . H12B H 0.8849 0.8409 0.6712 0.080 Uiso 1 1 calc R . . C13 C 0.7072(10) 0.8733(6) 0.5842(7) 0.068(3) Uani 1 1 d . . . H13A H 0.6717 0.9075 0.5244 0.082 Uiso 1 1 calc R . . H13B H 0.6865 0.9078 0.6340 0.082 Uiso 1 1 calc R . . C14 C 0.6428(9) 0.7797(6) 0.5732(6) 0.058(2) Uani 1 1 d . . . H14A H 0.6720 0.7479 0.6348 0.070 Uiso 1 1 calc R . . H14B H 0.5515 0.7893 0.5568 0.070 Uiso 1 1 calc R . . C15 C 0.7043(7) 0.5175(5) 0.4235(5) 0.0384(16) Uani 1 1 d . . . C16 C 0.5911(7) 0.5605(5) 0.4236(5) 0.0461(18) Uani 1 1 d . . . C17 C 0.4746(8) 0.5288(6) 0.3581(6) 0.055(2) Uani 1 1 d . . . H17A H 0.3990 0.5584 0.3561 0.066 Uiso 1 1 calc R . . C18 C 0.4701(10) 0.4547(6) 0.2967(6) 0.063(2) Uani 1 1 d . . . H18A H 0.3922 0.4340 0.2547 0.076 Uiso 1 1 calc R . . C19 C 0.5816(8) 0.4123(6) 0.2983(5) 0.053(2) Uani 1 1 d . . . H19A H 0.5788 0.3622 0.2575 0.064 Uiso 1 1 calc R . . C20 C 0.6977(8) 0.4424(5) 0.3594(5) 0.0477(19) Uani 1 1 d . . . H20A H 0.7724 0.4134 0.3586 0.057 Uiso 1 1 calc R . . O3 O 0.9663(6) 0.5100(4) 0.3508(4) 0.0527(14) Uani 1 1 d . . . C21 C 0.8917(10) 0.5702(7) 0.2779(6) 0.068(3) Uani 1 1 d . . . H21A H 0.8868 0.6307 0.3061 0.082 Uiso 1 1 calc R . . H21B H 0.8056 0.5455 0.2528 0.082 Uiso 1 1 calc R . . C22 C 0.9422(14) 0.5825(11) 0.1979(8) 0.122(5) Uani 1 1 d . . . H22A H 0.8877 0.6240 0.1511 0.183 Uiso 1 1 calc R . . H22B H 0.9453 0.5232 0.1685 0.183 Uiso 1 1 calc R . . H22C H 1.0267 0.6083 0.2219 0.183 Uiso 1 1 calc R . . H3B H 1.020(12) 0.454(8) 0.329(8) 0.13(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0419(6) 0.0318(5) 0.0388(5) -0.0014(4) 0.0082(4) 0.0030(4) Ni2 0.0397(8) 0.0288(6) 0.0435(7) 0.0014(5) 0.0133(6) 0.0037(5) Cl1 0.0720(15) 0.0613(13) 0.0379(10) -0.0041(8) 0.0106(9) 0.0140(11) O1 0.045(3) 0.031(2) 0.061(3) 0.002(2) 0.018(2) 0.002(2) O2 0.034(3) 0.037(3) 0.046(3) -0.005(2) 0.005(2) 0.003(2) N1 0.066(5) 0.032(3) 0.052(4) -0.005(3) 0.016(3) 0.004(3) N2 0.055(4) 0.042(3) 0.044(3) 0.000(3) 0.016(3) 0.013(3) C1 0.036(4) 0.036(4) 0.047(4) 0.012(3) 0.001(3) -0.007(3) C2 0.055(5) 0.040(4) 0.071(5) 0.009(4) 0.022(4) 0.003(4) C3 0.048(5) 0.061(6) 0.072(6) 0.020(4) 0.022(4) 0.010(4) C4 0.051(6) 0.065(6) 0.091(7) 0.028(5) 0.024(5) -0.004(5) C5 0.058(6) 0.039(4) 0.083(6) 0.011(4) 0.003(5) -0.002(4) C6 0.035(4) 0.043(4) 0.060(5) 0.004(3) 0.003(4) -0.005(3) C7 0.065(6) 0.035(4) 0.071(5) -0.007(4) 0.003(4) -0.014(4) C8 0.038(4) 0.062(5) 0.047(4) 0.009(4) 0.015(3) 0.006(4) C9 0.065(6) 0.037(4) 0.063(5) 0.012(4) 0.017(4) 0.012(4) C10 0.047(5) 0.053(5) 0.054(4) 0.010(4) 0.015(4) 0.009(4) C11 0.049(5) 0.047(5) 0.052(4) 0.004(3) 0.004(4) 0.010(4) C12 0.091(8) 0.045(5) 0.058(5) -0.012(4) 0.017(5) 0.023(5) C13 0.081(7) 0.053(5) 0.074(6) -0.022(4) 0.030(5) 0.017(5) C14 0.070(6) 0.055(5) 0.055(5) -0.009(4) 0.028(4) 0.019(4) C15 0.040(4) 0.036(4) 0.036(3) 0.004(3) 0.009(3) -0.001(3) C16 0.044(5) 0.046(4) 0.046(4) 0.005(3) 0.012(4) -0.004(4) C17 0.046(5) 0.056(5) 0.062(5) 0.016(4) 0.015(4) 0.010(4) C18 0.068(7) 0.065(6) 0.047(5) 0.001(4) 0.006(4) -0.026(5) C19 0.058(6) 0.051(5) 0.050(4) -0.006(3) 0.017(4) -0.012(4) C20 0.053(5) 0.039(4) 0.048(4) -0.002(3) 0.013(4) -0.006(4) O3 0.064(4) 0.051(3) 0.044(3) 0.009(2) 0.019(3) 0.014(3) C21 0.077(7) 0.068(6) 0.057(5) 0.025(4) 0.019(5) 0.019(5) C22 0.131(12) 0.165(13) 0.067(7) 0.050(8) 0.029(7) 0.022(10) _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. ; 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 O2 2.016(5) . ? Ni1 O1 2.026(5) . ? Ni1 N2 2.087(7) . ? Ni1 N1 2.108(6) . ? Ni1 Cl1 2.336(2) . ? Ni2 O2 2.058(5) 3_766 ? Ni2 O2 2.058(5) . ? Ni2 O1 2.070(5) . ? Ni2 O1 2.070(5) 3_766 ? Ni2 O3 2.105(5) 3_766 ? Ni2 O3 2.105(5) . ? O1 C1 1.351(9) . ? O2 C15 1.355(8) . ? N1 C12 1.485(10) . ? N1 C9 1.496(10) . ? N1 C7 1.496(11) . ? N2 C11 1.486(9) . ? N2 C8 1.493(10) . ? N2 C14 1.495(9) . ? C1 C2 1.393(12) . ? C1 C6 1.404(10) . ? C2 C3 1.376(12) . ? C3 C4 1.351(13) . ? C4 C5 1.364(13) . ? C5 C6 1.406(12) . ? C6 C7 1.494(12) . ? C8 C16 1.481(11) . ? C9 C10 1.499(11) . ? C10 C11 1.523(12) . ? C12 C13 1.493(14) . ? C13 C14 1.505(12) . ? C15 C16 1.397(10) . ? C15 C20 1.416(10) . ? C16 C17 1.409(11) . ? C17 C18 1.384(12) . ? C18 C19 1.370(13) . ? C19 C20 1.375(11) . ? O3 C21 1.413(9) . ? C21 C22 1.468(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 O2 Ni1 O1 79.1(2) . . ? O2 Ni1 N2 94.8(2) . . ? O1 Ni1 N2 159.3(2) . . ? O2 Ni1 N1 160.7(2) . . ? O1 Ni1 N1 93.2(2) . . ? N2 Ni1 N1 86.3(3) . . ? O2 Ni1 Cl1 99.97(15) . . ? O1 Ni1 Cl1 102.66(15) . . ? N2 Ni1 Cl1 97.89(17) . . ? N1 Ni1 Cl1 99.00(18) . . ? O2 Ni2 O2 180.0(3) 3_766 . ? O2 Ni2 O1 102.89(19) 3_766 . ? O2 Ni2 O1 77.11(19) . . ? O2 Ni2 O1 77.11(19) 3_766 3_766 ? O2 Ni2 O1 102.89(19) . 3_766 ? O1 Ni2 O1 180.000(1) . 3_766 ? O2 Ni2 O3 91.2(2) 3_766 3_766 ? O2 Ni2 O3 88.8(2) . 3_766 ? O1 Ni2 O3 88.7(2) . 3_766 ? O1 Ni2 O3 91.3(2) 3_766 3_766 ? O2 Ni2 O3 88.8(2) 3_766 . ? O2 Ni2 O3 91.2(2) . . ? O1 Ni2 O3 91.3(2) . . ? O1 Ni2 O3 88.7(2) 3_766 . ? O3 Ni2 O3 180.000(1) 3_766 . ? C1 O1 Ni1 125.5(4) . . ? C1 O1 Ni2 129.5(5) . . ? Ni1 O1 Ni2 99.7(2) . . ? C15 O2 Ni1 125.2(4) . . ? C15 O2 Ni2 129.8(4) . . ? Ni1 O2 Ni2 100.5(2) . . ? C12 N1 C9 110.9(6) . . ? C12 N1 C7 107.4(6) . . ? C9 N1 C7 112.5(7) . . ? C12 N1 Ni1 111.1(5) . . ? C9 N1 Ni1 107.3(4) . . ? C7 N1 Ni1 107.6(5) . . ? C11 N2 C8 112.0(6) . . ? C11 N2 C14 110.8(6) . . ? C8 N2 C14 106.2(6) . . ? C11 N2 Ni1 108.3(5) . . ? C8 N2 Ni1 107.1(4) . . ? C14 N2 Ni1 112.5(5) . . ? O1 C1 C2 122.4(7) . . ? O1 C1 C6 119.5(7) . . ? C2 C1 C6 118.1(7) . . ? C3 C2 C1 120.3(8) . . ? C4 C3 C2 122.6(9) . . ? C3 C4 C5 118.0(9) . . ? C4 C5 C6 122.2(9) . . ? C1 C6 C5 118.7(8) . . ? C1 C6 C7 121.1(7) . . ? C5 C6 C7 120.1(8) . . ? C6 C7 N1 114.7(6) . . ? C16 C8 N2 116.5(6) . . ? N1 C9 C10 113.3(6) . . ? C9 C10 C11 119.1(7) . . ? N2 C11 C10 112.3(6) . . ? N1 C12 C13 115.9(7) . . ? C12 C13 C14 115.4(7) . . ? N2 C14 C13 114.9(7) . . ? O2 C15 C16 120.5(6) . . ? O2 C15 C20 120.5(7) . . ? C16 C15 C20 119.0(7) . . ? C15 C16 C17 118.6(7) . . ? C15 C16 C8 121.1(7) . . ? C17 C16 C8 120.0(8) . . ? C18 C17 C16 121.5(8) . . ? C19 C18 C17 119.3(8) . . ? C18 C19 C20 121.1(8) . . ? C19 C20 C15 120.5(8) . . ? C21 O3 Ni2 133.7(5) . . ? O3 C21 C22 113.5(9) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.647 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.097 #===END