Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'P. Braunstein' _publ_contact_author_address ; Laboratoire de Chimie de Coordn. UMR 7177 CNRS Universite Louis Pasteur 4 rue Blaise Pascal Strasbourg Cedex 67070 FRANCE ; _publ_contact_author_email BRAUNSTEIN@CHIMIE.U-STRASBG.FR _publ_section_title ; Synthesis of nickel complexes with bidentate N,O-type ligands and application in the catalytic oligomerization of ethylene ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. Dowty, E. (1994). ATOMS for Mac. Version 3.0. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, E-U. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. Spek, A.L., PLATON 98, Utrecht University, The Netherland, 1998. ; loop_ _publ_author_name 'P. Braunstein' 'Anthony Kermagoret' 'Richard Welter' data_1 _database_code_depnum_ccdc_archive 'CCDC 664564' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H56 Cl4 N4 Ni2 O8' _chemical_formula_sum 'C30 H56 Cl4 N4 Ni2 O8' _chemical_formula_weight 860.01 _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.519(2) _cell_length_b 10.696(2) _cell_length_c 10.759(3) _cell_angle_alpha 79.71(5) _cell_angle_beta 66.07(5) _cell_angle_gamma 72.39(5) _cell_volume 952.4(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8497 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 1.320 _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 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14833 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 30.07 _reflns_number_total 5561 _reflns_number_gt 4446 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0350P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5561 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.2013 _refine_ls_wR_factor_gt 0.1923 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.00396(7) 0.12475(6) 0.37077(6) 0.01773(16) Uani 1 1 d . . . Cl1 Cl 0.14442(15) -0.10170(12) 0.38923(12) 0.0247(3) Uani 1 1 d . . . Cl2 Cl -0.28813(17) -0.16014(13) 0.37167(14) 0.0285(3) Uani 1 1 d . . . O1 O -0.1616(4) 0.0759(3) 0.3169(4) 0.0232(7) Uani 1 1 d . . . H1 H -0.1748 0.0027 0.3127 0.035 Uiso 1 1 calc . . . O2 O -0.3869(4) 0.4107(4) 0.3455(4) 0.0288(8) Uani 1 1 d . . . O3 O 0.1719(4) 0.1958(4) 0.4009(4) 0.0242(7) Uani 1 1 d . . . H3 H 0.1826 0.2044 0.4724 0.036 Uiso 1 1 calc . . . O4 O 0.4133(4) 0.1616(4) 0.0477(4) 0.0295(8) Uani 1 1 d . . . N1 N -0.1474(5) 0.3056(4) 0.3541(4) 0.0197(8) Uani 1 1 d . . . N2 N 0.1648(5) 0.1455(4) 0.1748(4) 0.0193(8) Uani 1 1 d . . . C1 C -0.3077(6) 0.1735(5) 0.3411(6) 0.0263(10) Uani 1 1 d . . . H1A H -0.3898 0.1518 0.4281 0.032 Uiso 1 1 calc . . . H1B H -0.3458 0.1799 0.2665 0.032 Uiso 1 1 calc . . . C2 C -0.2751(6) 0.2995(5) 0.3470(5) 0.0209(9) Uani 1 1 d . . . C3 C -0.3116(7) 0.5162(5) 0.3328(6) 0.0299(11) Uani 1 1 d . . . H3A H -0.3842 0.5845 0.3974 0.036 Uiso 1 1 calc . . . H3B H -0.2810 0.5577 0.2390 0.036 Uiso 1 1 calc . . . C4 C -0.1932(7) 0.4626(6) 0.5147(6) 0.0303(11) Uani 1 1 d . . . H4A H -0.2888 0.4345 0.5758 0.045 Uiso 1 1 calc . . . H4B H -0.2081 0.5551 0.5263 0.045 Uiso 1 1 calc . . . H4C H -0.1017 0.4087 0.5366 0.045 Uiso 1 1 calc . . . C5 C -0.0163(7) 0.4887(5) 0.2689(6) 0.0281(11) Uani 1 1 d . . . H5A H -0.0003 0.4767 0.1755 0.042 Uiso 1 1 calc . . . H5B H 0.0765 0.4352 0.2891 0.042 Uiso 1 1 calc . . . H5C H -0.0302 0.5815 0.2785 0.042 Uiso 1 1 calc . . . C6 C -0.1636(6) 0.4462(5) 0.3676(5) 0.0217(9) Uani 1 1 d . . . C7 C 0.3225(6) 0.1747(6) 0.2917(6) 0.0276(11) Uani 1 1 d . . . H7A H 0.3968 0.0941 0.3121 0.033 Uiso 1 1 calc . . . H7B H 0.3686 0.2502 0.2766 0.033 Uiso 1 1 calc . . . C8 C 0.2945(6) 0.1604(5) 0.1694(5) 0.0223(10) Uani 1 1 d . . . C9 C 0.3447(7) 0.1605(6) -0.0519(6) 0.0287(11) Uani 1 1 d . . . H9A H 0.4140 0.0921 -0.1173 0.034 Uiso 1 1 calc . . . H9B H 0.3303 0.2469 -0.1031 0.034 Uiso 1 1 calc . . . C10 C 0.1884(7) -0.0125(6) 0.0241(6) 0.0303(11) Uani 1 1 d . . . H10A H 0.2771 -0.0717 0.0466 0.045 Uiso 1 1 calc . . . H10B H 0.2033 -0.0251 -0.0688 0.045 Uiso 1 1 calc . . . H10C H 0.0884 -0.0319 0.0882 0.045 Uiso 1 1 calc . . . C11 C 0.0473(7) 0.2254(6) -0.0001(5) 0.0283(11) Uani 1 1 d . . . H11A H 0.0469 0.3155 0.0073 0.042 Uiso 1 1 calc . . . H11B H -0.0538 0.2078 0.0636 0.042 Uiso 1 1 calc . . . H11C H 0.0613 0.2147 -0.0934 0.042 Uiso 1 1 calc . . . C12 C 0.1829(6) 0.1296(5) 0.0341(5) 0.0231(10) Uani 1 1 d . . . C13 C 0.6159(7) 0.5310(6) 0.0302(6) 0.0308(12) Uani 1 1 d . . . H13A H 0.6496 0.5969 -0.0453 0.037 Uiso 1 1 calc . . . H13B H 0.6767 0.5207 0.0890 0.037 Uiso 1 1 calc . . . C14 C 0.6476(8) 0.4131(8) -0.0217(9) 0.053(2) Uani 1 1 d . . . H14A H 0.6224 0.3455 0.0540 0.063 Uiso 1 1 calc . . . H14B H 0.7621 0.3849 -0.0786 0.063 Uiso 1 1 calc . . . C15 C 0.4505(10) 0.5752(8) 0.1074(8) 0.0508(18) Uani 1 1 d . . . H15A H 0.4284 0.6619 0.1416 0.061 Uiso 1 1 calc . . . H15B H 0.4191 0.5126 0.1871 0.061 Uiso 1 1 calc . . . 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 0.0177(3) 0.0180(3) 0.0177(3) 0.0020(2) -0.0077(2) -0.0053(2) Cl1 0.0242(6) 0.0215(6) 0.0205(5) 0.0022(4) -0.0053(4) -0.0014(4) Cl2 0.0371(7) 0.0290(6) 0.0272(6) -0.0012(5) -0.0151(5) -0.0154(5) O1 0.0223(17) 0.0192(17) 0.0312(19) -0.0007(14) -0.0122(15) -0.0071(14) O2 0.0219(18) 0.0234(19) 0.040(2) -0.0013(16) -0.0153(16) 0.0007(15) O3 0.0226(17) 0.032(2) 0.0228(17) -0.0017(15) -0.0105(14) -0.0109(15) O4 0.0204(18) 0.039(2) 0.0250(19) 0.0027(16) -0.0045(15) -0.0109(16) N1 0.0214(19) 0.0166(18) 0.0209(19) 0.0015(15) -0.0093(16) -0.0044(15) N2 0.0189(18) 0.0198(19) 0.0192(19) 0.0029(15) -0.0081(15) -0.0059(15) C1 0.022(2) 0.026(3) 0.034(3) -0.001(2) -0.013(2) -0.007(2) C2 0.017(2) 0.023(2) 0.021(2) 0.0013(18) -0.0089(18) -0.0015(18) C3 0.032(3) 0.020(2) 0.039(3) -0.001(2) -0.017(2) -0.003(2) C4 0.038(3) 0.027(3) 0.028(3) -0.003(2) -0.013(2) -0.010(2) C5 0.032(3) 0.022(2) 0.030(3) 0.000(2) -0.009(2) -0.011(2) C6 0.027(2) 0.017(2) 0.022(2) 0.0005(17) -0.0105(19) -0.0059(18) C7 0.021(2) 0.036(3) 0.029(3) -0.004(2) -0.008(2) -0.011(2) C8 0.019(2) 0.023(2) 0.023(2) 0.0012(19) -0.0071(18) -0.0062(18) C9 0.025(3) 0.035(3) 0.022(2) 0.001(2) -0.006(2) -0.008(2) C10 0.031(3) 0.028(3) 0.036(3) -0.008(2) -0.016(2) -0.005(2) C11 0.029(3) 0.030(3) 0.022(2) -0.001(2) -0.012(2) 0.000(2) C12 0.024(2) 0.025(2) 0.020(2) -0.0005(18) -0.0102(19) -0.0036(19) C13 0.025(3) 0.045(3) 0.033(3) 0.002(2) -0.017(2) -0.018(2) C14 0.030(3) 0.056(5) 0.060(5) 0.019(4) -0.015(3) -0.011(3) C15 0.052(4) 0.057(5) 0.044(4) -0.004(3) -0.014(3) -0.021(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 Ni1 N1 2.062(4) . ? Ni1 N2 2.063(4) . ? Ni1 O1 2.108(4) . ? Ni1 O3 2.117(4) . ? Ni1 Cl1 2.3974(19) 2_556 ? Ni1 Cl1 2.4037(18) . ? Cl1 Ni1 2.3974(19) 2_556 ? O1 C1 1.420(6) . ? O1 H1 0.8400 . ? O2 C2 1.337(6) . ? O2 C3 1.470(7) . ? O3 C7 1.421(6) . ? O3 H3 0.8400 . ? O4 C8 1.339(6) . ? O4 C9 1.468(7) . ? N1 C2 1.271(6) . ? N1 C6 1.491(6) . ? N2 C8 1.269(6) . ? N2 C12 1.488(6) . ? C1 C2 1.489(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C6 1.541(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C6 1.523(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.518(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.486(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C9 C12 1.542(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C12 1.526(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.517(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 C14 1.370(11) . ? C13 C15 1.422(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.525(11) 2_665 ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C14 1.525(11) 2_665 ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? 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 Ni1 N2 92.89(17) . . ? N1 Ni1 O1 77.54(16) . . ? N2 Ni1 O1 96.51(16) . . ? N1 Ni1 O3 96.64(16) . . ? N2 Ni1 O3 77.39(16) . . ? O1 Ni1 O3 171.46(14) . . ? N1 Ni1 Cl1 91.51(14) . 2_556 ? N2 Ni1 Cl1 169.44(12) . 2_556 ? O1 Ni1 Cl1 93.80(12) . 2_556 ? O3 Ni1 Cl1 92.58(11) . 2_556 ? N1 Ni1 Cl1 169.79(12) . . ? N2 Ni1 Cl1 90.47(14) . . ? O1 Ni1 Cl1 92.51(11) . . ? O3 Ni1 Cl1 93.50(12) . . ? Cl1 Ni1 Cl1 86.84(8) 2_556 . ? Ni1 Cl1 Ni1 93.16(8) 2_556 . ? C1 O1 Ni1 114.6(3) . . ? C1 O1 H1 109.5 . . ? Ni1 O1 H1 131.3 . . ? C2 O2 C3 104.7(4) . . ? C7 O3 Ni1 113.8(3) . . ? C7 O3 H3 109.5 . . ? Ni1 O3 H3 131.2 . . ? C8 O4 C9 105.1(4) . . ? C2 N1 C6 107.2(4) . . ? C2 N1 Ni1 114.0(3) . . ? C6 N1 Ni1 138.1(3) . . ? C8 N2 C12 108.0(4) . . ? C8 N2 Ni1 113.7(3) . . ? C12 N2 Ni1 137.6(3) . . ? O1 C1 C2 106.3(4) . . ? O1 C1 H1A 110.5 . . ? C2 C1 H1A 110.5 . . ? O1 C1 H1B 110.5 . . ? C2 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? N1 C2 O2 119.1(5) . . ? N1 C2 C1 123.1(4) . . ? O2 C2 C1 117.8(4) . . ? O2 C3 C6 104.2(4) . . ? O2 C3 H3A 110.9 . . ? C6 C3 H3A 110.9 . . ? O2 C3 H3B 110.9 . . ? C6 C3 H3B 110.9 . . ? H3A C3 H3B 108.9 . . ? C6 C4 H4A 109.5 . . ? C6 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C6 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C5 110.8(4) . . ? N1 C6 C4 108.3(4) . . ? C5 C6 C4 111.4(5) . . ? N1 C6 C3 101.9(4) . . ? C5 C6 C3 112.4(4) . . ? C4 C6 C3 111.6(5) . . ? O3 C7 C8 106.4(4) . . ? O3 C7 H7A 110.4 . . ? C8 C7 H7A 110.4 . . ? O3 C7 H7B 110.4 . . ? C8 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? N2 C8 O4 118.7(5) . . ? N2 C8 C7 123.3(5) . . ? O4 C8 C7 118.0(4) . . ? O4 C9 C12 104.7(4) . . ? O4 C9 H9A 110.8 . . ? C12 C9 H9A 110.8 . . ? O4 C9 H9B 110.8 . . ? C12 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? C12 C10 H10A 109.5 . . ? C12 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C12 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C11 110.3(4) . . ? N2 C12 C10 108.5(4) . . ? C11 C12 C10 111.4(5) . . ? N2 C12 C9 102.0(4) . . ? C11 C12 C9 112.6(4) . . ? C10 C12 C9 111.6(5) . . ? C14 C13 C15 110.0(6) . . ? C14 C13 H13A 109.7 . . ? C15 C13 H13A 109.7 . . ? C14 C13 H13B 109.7 . . ? C15 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C13 C14 C15 110.7(6) . 2_665 ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 2_665 . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 2_665 . ? H14A C14 H14B 108.1 . . ? C13 C15 C14 111.2(6) . 2_665 ? C13 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 2_665 . ? C13 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 2_665 . ? H15A C15 H15B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 Cl1 Ni1 -80.9(7) . . . 2_556 ? N2 Ni1 Cl1 Ni1 169.79(12) . . . 2_556 ? O1 Ni1 Cl1 Ni1 -93.67(12) . . . 2_556 ? O3 Ni1 Cl1 Ni1 92.39(12) . . . 2_556 ? Cl1 Ni1 Cl1 Ni1 0.0 2_556 . . 2_556 ? N1 Ni1 O1 C1 -19.5(3) . . . . ? N2 Ni1 O1 C1 -111.0(4) . . . . ? O3 Ni1 O1 C1 -67.1(11) . . . . ? Cl1 Ni1 O1 C1 71.2(3) 2_556 . . . ? Cl1 Ni1 O1 C1 158.2(3) . . . . ? N1 Ni1 O3 C7 -112.8(4) . . . . ? N2 Ni1 O3 C7 -21.4(3) . . . . ? O1 Ni1 O3 C7 -66.3(11) . . . . ? Cl1 Ni1 O3 C7 155.3(3) 2_556 . . . ? Cl1 Ni1 O3 C7 68.3(3) . . . . ? N2 Ni1 N1 C2 108.5(4) . . . . ? O1 Ni1 N1 C2 12.4(4) . . . . ? O3 Ni1 N1 C2 -173.9(4) . . . . ? Cl1 Ni1 N1 C2 -81.1(4) 2_556 . . . ? Cl1 Ni1 N1 C2 -0.6(10) . . . . ? N2 Ni1 N1 C6 -82.9(5) . . . . ? O1 Ni1 N1 C6 -178.9(5) . . . . ? O3 Ni1 N1 C6 -5.3(5) . . . . ? Cl1 Ni1 N1 C6 87.5(5) 2_556 . . . ? Cl1 Ni1 N1 C6 168.0(5) . . . . ? N1 Ni1 N2 C8 110.4(4) . . . . ? O1 Ni1 N2 C8 -171.8(4) . . . . ? O3 Ni1 N2 C8 14.2(4) . . . . ? Cl1 Ni1 N2 C8 -4.1(10) 2_556 . . . ? Cl1 Ni1 N2 C8 -79.2(4) . . . . ? N1 Ni1 N2 C12 -80.6(5) . . . . ? O1 Ni1 N2 C12 -2.8(5) . . . . ? O3 Ni1 N2 C12 -176.7(5) . . . . ? Cl1 Ni1 N2 C12 164.9(5) 2_556 . . . ? Cl1 Ni1 N2 C12 89.8(5) . . . . ? Ni1 O1 C1 C2 21.4(5) . . . . ? C6 N1 C2 O2 3.3(6) . . . . ? Ni1 N1 C2 O2 175.4(4) . . . . ? C6 N1 C2 C1 -176.2(5) . . . . ? Ni1 N1 C2 C1 -4.2(6) . . . . ? C3 O2 C2 N1 8.1(6) . . . . ? C3 O2 C2 C1 -172.3(5) . . . . ? O1 C1 C2 N1 -11.7(7) . . . . ? O1 C1 C2 O2 168.8(4) . . . . ? C2 O2 C3 C6 -15.2(5) . . . . ? C2 N1 C6 C5 -132.3(5) . . . . ? Ni1 N1 C6 C5 58.6(6) . . . . ? C2 N1 C6 C4 105.2(5) . . . . ? Ni1 N1 C6 C4 -63.9(6) . . . . ? C2 N1 C6 C3 -12.5(5) . . . . ? Ni1 N1 C6 C3 178.4(4) . . . . ? O2 C3 C6 N1 16.6(5) . . . . ? O2 C3 C6 C5 135.2(5) . . . . ? O2 C3 C6 C4 -98.8(5) . . . . ? Ni1 O3 C7 C8 23.1(5) . . . . ? C12 N2 C8 O4 1.2(6) . . . . ? Ni1 N2 C8 O4 173.4(4) . . . . ? C12 N2 C8 C7 -177.9(5) . . . . ? Ni1 N2 C8 C7 -5.6(7) . . . . ? C9 O4 C8 N2 6.9(6) . . . . ? C9 O4 C8 C7 -174.0(5) . . . . ? O3 C7 C8 N2 -12.0(7) . . . . ? O3 C7 C8 O4 168.9(4) . . . . ? C8 O4 C9 C12 -11.3(5) . . . . ? C8 N2 C12 C11 -128.0(5) . . . . ? Ni1 N2 C12 C11 62.6(6) . . . . ? C8 N2 C12 C10 109.7(5) . . . . ? Ni1 N2 C12 C10 -59.8(6) . . . . ? C8 N2 C12 C9 -8.2(5) . . . . ? Ni1 N2 C12 C9 -177.7(4) . . . . ? O4 C9 C12 N2 11.7(5) . . . . ? O4 C9 C12 C11 129.8(5) . . . . ? O4 C9 C12 C10 -104.0(5) . . . . ? C15 C13 C14 C15 56.7(9) . . . 2_665 ? C14 C13 C15 C14 -57.0(9) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.007 _refine_diff_density_min -1.010 _refine_diff_density_rms 0.194 # Attachment 'Complex_Ni2py_16_3CH2Cl2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 664565' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H34 Cl10 N4 Ni2 O4' _chemical_formula_sum 'C27 H34 Cl10 N4 Ni2 O4' _chemical_formula_weight 950.50 _chemical_absolute_configuration . 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2260(2) _cell_length_b 11.5260(2) _cell_length_c 17.0800(5) _cell_angle_alpha 89.1500(10) _cell_angle_beta 77.9500(10) _cell_angle_gamma 74.3000(10) _cell_volume 1893.47(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13705 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 1.739 _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 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25759 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0971 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 29.99 _reflns_number_total 10998 _reflns_number_gt 6976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0800P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10998 _refine_ls_number_parameters 424 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1362 _refine_ls_R_factor_gt 0.0855 _refine_ls_wR_factor_ref 0.2302 _refine_ls_wR_factor_gt 0.2018 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.932 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.05482(7) 0.62822(6) 0.01909(4) 0.02199(17) Uani 1 1 d . . . Ni2 Ni 0.42302(7) 0.94112(6) 0.43232(4) 0.02119(17) Uani 1 1 d . . . Cl1 Cl -0.16203(14) 0.57707(12) 0.03343(9) 0.0269(3) Uani 1 1 d . . . Cl3 Cl 0.65549(13) 0.92845(12) 0.44838(8) 0.0255(3) Uani 1 1 d . . . Cl2 Cl 0.12284(18) 0.34667(14) 0.20570(9) 0.0370(4) Uani 1 1 d . . . Cl4 Cl 0.60320(18) 1.25159(15) 0.33374(9) 0.0364(4) Uani 1 1 d . . . Cl5 Cl 0.4305(5) 1.0190(4) 0.1013(3) 0.1431(18) Uani 1 1 d . . . Cl6 Cl 0.1808(5) 0.9430(4) 0.1390(3) 0.1388(16) Uani 1 1 d . . . Cl7 Cl 0.2534(6) 0.5167(5) 0.4053(3) 0.1469(18) Uani 1 1 d . . . Cl8 Cl 0.2760(6) 0.6484(5) 0.2661(3) 0.1379(16) Uani 1 1 d . . . Cl9 Cl 0.1952(4) 0.5942(4) 0.6066(4) 0.156(2) Uani 1 1 d D . . Cl10 Cl 0.1151(3) 0.3658(2) 0.58340(15) 0.0812(8) Uani 1 1 d . . . O1 O 0.0429(4) 0.7016(4) -0.0909(2) 0.0292(9) Uani 1 1 d . . . HO1 H -0.0179 0.7078 -0.1183 0.044 Uiso 1 1 calc . . . O2 O 0.4042(4) 0.7879(4) 0.4929(2) 0.0290(9) Uani 1 1 d . . . HO2 H 0.3873 0.7803 0.5427 0.043 Uiso 1 1 calc . . . O3 O 0.0818(5) 0.5865(4) 0.1333(3) 0.0347(10) Uani 1 1 d . . . HO3 H 0.1128 0.5188 0.1515 0.052 Uiso 1 1 calc . . . O4 O 0.4189(4) 1.0835(4) 0.3565(3) 0.0285(9) Uani 1 1 d . . . HO4 H 0.4768 1.1244 0.3497 0.043 Uiso 1 1 calc . . . N1 N 0.2458(5) 0.6625(4) -0.0163(3) 0.0246(10) Uani 1 1 d . . . N2 N -0.0502(5) 0.7887(4) 0.0830(3) 0.0288(10) Uani 1 1 d . . . N3 N 0.5008(5) 0.8091(5) 0.3424(3) 0.0293(11) Uani 1 1 d . . . N4 N 0.2259(5) 0.9777(4) 0.4087(3) 0.0255(10) Uani 1 1 d . . . C1 C 0.1746(7) 0.6929(7) -0.1432(4) 0.0426(17) Uani 1 1 d . . . H1A H 0.1690 0.7656 -0.1753 0.051 Uiso 1 1 calc . . . H1B H 0.2003 0.6214 -0.1804 0.051 Uiso 1 1 calc . . . C2 C 0.2831(6) 0.6818(5) -0.0937(4) 0.0305(13) Uani 1 1 d . . . C3 C 0.4158(7) 0.6890(7) -0.1279(4) 0.0406(16) Uani 1 1 d . . . H3 H 0.4401 0.7028 -0.1833 0.049 Uiso 1 1 calc . . . C4 C 0.5120(7) 0.6762(7) -0.0807(5) 0.0436(17) Uani 1 1 d . . . H4 H 0.6041 0.6790 -0.1034 0.052 Uiso 1 1 calc . . . C5 C 0.4732(7) 0.6594(7) -0.0005(5) 0.0436(17) Uani 1 1 d . . . H5 H 0.5373 0.6523 0.0335 0.052 Uiso 1 1 calc . . . C6 C 0.3395(7) 0.6529(6) 0.0300(4) 0.0353(14) Uani 1 1 d . . . H6 H 0.3126 0.6413 0.0856 0.042 Uiso 1 1 calc . . . C7 C -0.0218(11) 0.6625(8) 0.1948(5) 0.063(3) Uani 1 1 d . . . H7A H 0.0194 0.6723 0.2410 0.076 Uiso 1 1 calc . . . H7B H -0.0984 0.6248 0.2135 0.076 Uiso 1 1 calc . . . C8 C -0.0774(8) 0.7832(6) 0.1626(4) 0.0406(16) Uani 1 1 d . . . C9 C -0.1575(9) 0.8819(7) 0.2130(5) 0.051(2) Uani 1 1 d . . . H9 H -0.1736 0.8758 0.2695 0.062 Uiso 1 1 calc . . . C10 C -0.2128(8) 0.9880(7) 0.1797(6) 0.053(2) Uani 1 1 d . . . H10 H -0.2673 1.0569 0.2128 0.063 Uiso 1 1 calc . . . C11 C -0.1883(9) 0.9928(7) 0.0984(6) 0.057(2) Uani 1 1 d . . . H11 H -0.2281 1.0649 0.0742 0.068 Uiso 1 1 calc . . . C12 C -0.1055(8) 0.8931(6) 0.0510(5) 0.0442(17) Uani 1 1 d . . . H12 H -0.0872 0.8984 -0.0056 0.053 Uiso 1 1 calc . . . C13 C 0.4972(10) 0.6797(6) 0.4546(5) 0.053(2) Uani 1 1 d . . . H13A H 0.4556 0.6116 0.4671 0.064 Uiso 1 1 calc . . . H13B H 0.5850 0.6616 0.4740 0.064 Uiso 1 1 calc . . . C14 C 0.5255(10) 0.6958(7) 0.3661(5) 0.056(2) Uani 1 1 d . . . C15 C 0.5760(19) 0.5993(8) 0.3104(7) 0.128(7) Uani 1 1 d . . . H15 H 0.5934 0.5186 0.3271 0.154 Uiso 1 1 calc . . . C16 C 0.600(2) 0.6236(10) 0.2302(7) 0.146(8) Uani 1 1 d . . . H16 H 0.6319 0.5587 0.1912 0.175 Uiso 1 1 calc . . . C17 C 0.5794(14) 0.7393(9) 0.2058(5) 0.082(4) Uani 1 1 d . . . H17 H 0.5996 0.7564 0.1507 0.098 Uiso 1 1 calc . . . C18 C 0.5279(8) 0.8296(6) 0.2646(4) 0.0412(16) Uani 1 1 d . . . H18 H 0.5108 0.9109 0.2489 0.049 Uiso 1 1 calc . . . C19 C 0.2817(7) 1.1623(6) 0.3650(4) 0.0340(14) Uani 1 1 d . . . H19A H 0.2738 1.2092 0.3164 0.041 Uiso 1 1 calc . . . H19B H 0.2605 1.2195 0.4116 0.041 Uiso 1 1 calc . . . C20 C 0.1816(6) 1.0848(6) 0.3773(4) 0.0290(12) Uani 1 1 d . . . C21 C 0.0517(7) 1.1226(7) 0.3581(5) 0.0410(16) Uani 1 1 d . . . H21 H 0.0223 1.1990 0.3360 0.049 Uiso 1 1 calc . . . C22 C -0.0340(7) 1.0466(8) 0.3717(4) 0.0437(17) Uani 1 1 d . . . H22 H -0.1242 1.0706 0.3602 0.052 Uiso 1 1 calc . . . C23 C 0.0137(7) 0.9356(7) 0.4024(4) 0.0388(15) Uani 1 1 d . . . H23 H -0.0425 0.8811 0.4108 0.047 Uiso 1 1 calc . . . C24 C 0.1427(6) 0.9042(6) 0.4207(4) 0.0311(13) Uani 1 1 d . . . H24 H 0.1742 0.8280 0.4426 0.037 Uiso 1 1 calc . . . C25 C 0.2664(15) 1.0352(16) 0.1553(16) 0.178(10) Uani 1 1 d . . . H25A H 0.2712 1.0318 0.2126 0.213 Uiso 1 1 calc . . . H25B H 0.2105 1.1175 0.1473 0.213 Uiso 1 1 calc . . . C26 C 0.264(3) 0.5307(19) 0.3289(16) 0.256(17) Uani 1 1 d . . . H26A H 0.1830 0.5072 0.3177 0.308 Uiso 1 1 calc . . . H26B H 0.3461 0.4644 0.3045 0.308 Uiso 1 1 calc . . . C27 C 0.0658(11) 0.5260(13) 0.6039(10) 0.122(5) Uani 1 1 d D . . H27A H 0.0152 0.5650 0.5628 0.146 Uiso 1 1 calc . . . H27B H -0.0007 0.5436 0.6562 0.146 Uiso 1 1 calc . . . 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 0.0249(4) 0.0218(3) 0.0216(3) 0.0030(3) -0.0062(3) -0.0093(3) Ni2 0.0207(3) 0.0238(3) 0.0209(3) 0.0010(3) -0.0057(3) -0.0083(3) Cl1 0.0252(6) 0.0251(6) 0.0308(7) -0.0024(5) -0.0026(5) -0.0097(5) Cl3 0.0195(6) 0.0298(7) 0.0269(7) -0.0037(5) -0.0050(5) -0.0059(5) Cl2 0.0520(10) 0.0363(8) 0.0299(8) 0.0109(6) -0.0186(7) -0.0172(7) Cl4 0.0466(9) 0.0390(8) 0.0299(8) 0.0100(6) -0.0092(6) -0.0216(7) Cl5 0.149(4) 0.126(3) 0.115(3) 0.050(3) 0.029(3) -0.019(3) Cl6 0.151(4) 0.120(3) 0.171(5) 0.008(3) -0.073(3) -0.053(3) Cl7 0.146(4) 0.134(4) 0.151(4) 0.019(3) 0.016(3) -0.059(3) Cl8 0.165(4) 0.149(4) 0.127(4) 0.020(3) -0.070(3) -0.062(3) Cl9 0.093(3) 0.106(3) 0.250(6) -0.036(3) 0.013(3) -0.032(2) Cl10 0.120(2) 0.0579(14) 0.0487(13) 0.0014(10) -0.0075(14) -0.0044(14) O1 0.029(2) 0.037(2) 0.027(2) 0.0118(17) -0.0124(17) -0.0139(18) O2 0.037(2) 0.030(2) 0.023(2) 0.0054(16) -0.0065(17) -0.0146(18) O3 0.051(3) 0.031(2) 0.024(2) 0.0026(17) -0.0120(19) -0.012(2) O4 0.028(2) 0.030(2) 0.031(2) 0.0071(17) -0.0073(17) -0.0142(17) N1 0.026(2) 0.023(2) 0.029(2) 0.0029(18) -0.0092(19) -0.0115(19) N2 0.027(2) 0.028(2) 0.033(3) -0.001(2) -0.005(2) -0.011(2) N3 0.034(3) 0.030(3) 0.024(2) -0.004(2) -0.003(2) -0.011(2) N4 0.022(2) 0.034(3) 0.023(2) -0.0001(19) -0.0052(18) -0.0109(19) C1 0.036(4) 0.070(5) 0.030(3) 0.019(3) -0.011(3) -0.026(3) C2 0.033(3) 0.029(3) 0.033(3) 0.010(2) -0.008(3) -0.015(2) C3 0.035(4) 0.048(4) 0.041(4) 0.016(3) -0.003(3) -0.019(3) C4 0.026(3) 0.044(4) 0.062(5) 0.007(3) -0.005(3) -0.016(3) C5 0.036(4) 0.043(4) 0.057(5) -0.001(3) -0.020(3) -0.011(3) C6 0.033(3) 0.041(4) 0.035(3) -0.002(3) -0.012(3) -0.012(3) C7 0.104(8) 0.048(5) 0.023(3) -0.001(3) -0.007(4) -0.002(5) C8 0.052(4) 0.033(3) 0.036(4) -0.005(3) -0.003(3) -0.013(3) C9 0.061(5) 0.048(4) 0.043(4) -0.014(3) 0.003(4) -0.022(4) C10 0.049(4) 0.034(4) 0.065(5) -0.018(4) 0.010(4) -0.010(3) C11 0.057(5) 0.030(4) 0.071(6) -0.002(4) -0.004(4) 0.001(3) C12 0.050(4) 0.029(3) 0.048(4) 0.006(3) -0.004(3) -0.006(3) C13 0.085(6) 0.024(3) 0.039(4) -0.001(3) 0.003(4) -0.007(3) C14 0.095(7) 0.030(4) 0.033(4) -0.003(3) 0.004(4) -0.015(4) C15 0.263(19) 0.030(5) 0.052(6) -0.013(4) 0.039(9) -0.030(7) C16 0.30(2) 0.047(6) 0.049(6) -0.026(5) 0.046(10) -0.040(9) C17 0.151(11) 0.056(5) 0.028(4) -0.012(4) 0.015(5) -0.037(6) C18 0.055(4) 0.039(4) 0.029(3) -0.007(3) 0.001(3) -0.018(3) C19 0.035(3) 0.030(3) 0.042(4) 0.010(3) -0.014(3) -0.013(3) C20 0.029(3) 0.037(3) 0.024(3) 0.004(2) -0.008(2) -0.012(2) C21 0.028(3) 0.051(4) 0.046(4) 0.010(3) -0.017(3) -0.007(3) C22 0.026(3) 0.066(5) 0.041(4) 0.003(3) -0.011(3) -0.012(3) C23 0.029(3) 0.058(4) 0.037(4) -0.002(3) -0.008(3) -0.023(3) C24 0.027(3) 0.045(4) 0.028(3) 0.004(3) -0.008(2) -0.019(3) C25 0.074(9) 0.124(13) 0.32(3) -0.117(16) -0.056(13) 0.013(9) C26 0.45(4) 0.22(2) 0.33(3) 0.22(2) -0.37(3) -0.27(2) C27 0.127(13) 0.109(11) 0.117(12) -0.027(9) 0.003(10) -0.031(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. 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 2.059(4) . ? Ni1 N1 2.062(5) . ? Ni1 O1 2.063(4) . ? Ni1 N2 2.064(5) . ? Ni1 Cl1 2.4086(15) . ? Ni1 Cl1 2.4195(15) 2_565 ? Ni2 N3 2.052(5) . ? Ni2 O2 2.067(4) . ? Ni2 N4 2.069(5) . ? Ni2 O4 2.072(4) . ? Ni2 Cl3 2.4106(15) 2_676 ? Ni2 Cl3 2.4147(15) . ? Cl1 Ni1 2.4195(15) 2_565 ? Cl3 Ni2 2.4106(15) 2_676 ? Cl5 C25 1.700(19) . ? Cl6 C25 1.608(17) . ? Cl7 C26 1.30(2) . ? Cl8 C26 1.732(15) . ? Cl9 C27 1.7203(10) . ? Cl10 C27 1.797(14) . ? O1 C1 1.432(8) . ? O1 HO1 0.8400 . ? O2 C13 1.417(8) . ? O2 HO2 0.8400 . ? O3 C7 1.433(9) . ? O3 HO3 0.8400 . ? O4 C19 1.430(8) . ? O4 HO4 0.8400 . ? N1 C2 1.330(8) . ? N1 C6 1.347(8) . ? N2 C8 1.333(9) . ? N2 C12 1.345(9) . ? N3 C18 1.332(8) . ? N3 C14 1.335(9) . ? N4 C24 1.339(7) . ? N4 C20 1.340(8) . ? C1 C2 1.507(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.385(9) . ? C3 C4 1.373(10) . ? C3 H3 0.9500 . ? C4 C5 1.370(11) . ? C4 H4 0.9500 . ? C5 C6 1.380(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.497(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.391(10) . ? C9 C10 1.370(12) . ? C9 H9 0.9500 . ? C10 C11 1.363(13) . ? C10 H10 0.9500 . ? C11 C12 1.380(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.498(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.387(11) . ? C15 C16 1.378(16) . ? C15 H15 0.9500 . ? C16 C17 1.365(15) . ? C16 H16 0.9500 . ? C17 C18 1.372(10) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.514(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.388(9) . ? C21 C22 1.383(10) . ? C21 H21 0.9500 . ? C22 C23 1.379(11) . ? C22 H22 0.9500 . ? C23 C24 1.372(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? 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 N1 93.78(19) . . ? O3 Ni1 O1 167.61(17) . . ? N1 Ni1 O1 77.82(18) . . ? O3 Ni1 N2 77.87(19) . . ? N1 Ni1 N2 98.03(19) . . ? O1 Ni1 N2 94.14(19) . . ? O3 Ni1 Cl1 95.95(14) . . ? N1 Ni1 Cl1 168.85(14) . . ? O1 Ni1 Cl1 93.38(12) . . ? N2 Ni1 Cl1 89.34(14) . . ? O3 Ni1 Cl1 93.40(13) . 2_565 ? N1 Ni1 Cl1 88.53(14) . 2_565 ? O1 Ni1 Cl1 95.44(13) . 2_565 ? N2 Ni1 Cl1 169.35(15) . 2_565 ? Cl1 Ni1 Cl1 85.48(5) . 2_565 ? N3 Ni2 O2 77.80(19) . . ? N3 Ni2 N4 91.7(2) . . ? O2 Ni2 N4 93.14(18) . . ? N3 Ni2 O4 95.15(19) . . ? O2 Ni2 O4 168.21(17) . . ? N4 Ni2 O4 77.49(18) . . ? N3 Ni2 Cl3 170.99(16) . 2_676 ? O2 Ni2 Cl3 94.30(12) . 2_676 ? N4 Ni2 Cl3 93.05(14) . 2_676 ? O4 Ni2 Cl3 93.34(13) . 2_676 ? N3 Ni2 Cl3 90.44(15) . . ? O2 Ni2 Cl3 96.35(13) . . ? N4 Ni2 Cl3 170.51(14) . . ? O4 Ni2 Cl3 93.11(12) . . ? Cl3 Ni2 Cl3 86.10(5) 2_676 . ? Ni1 Cl1 Ni1 94.52(5) . 2_565 ? Ni2 Cl3 Ni2 93.90(5) 2_676 . ? C1 O1 Ni1 114.5(4) . . ? C1 O1 HO1 109.5 . . ? Ni1 O1 HO1 130.1 . . ? C13 O2 Ni2 113.9(4) . . ? C13 O2 HO2 109.5 . . ? Ni2 O2 HO2 127.6 . . ? C7 O3 Ni1 113.7(4) . . ? C7 O3 HO3 109.5 . . ? Ni1 O3 HO3 129.1 . . ? C19 O4 Ni2 111.6(3) . . ? C19 O4 HO4 109.5 . . ? Ni2 O4 HO4 124.5 . . ? C2 N1 C6 118.5(5) . . ? C2 N1 Ni1 115.8(4) . . ? C6 N1 Ni1 125.2(4) . . ? C8 N2 C12 118.2(6) . . ? C8 N2 Ni1 116.2(4) . . ? C12 N2 Ni1 125.2(5) . . ? C18 N3 C14 119.6(6) . . ? C18 N3 Ni2 124.7(4) . . ? C14 N3 Ni2 115.7(4) . . ? C24 N4 C20 118.8(5) . . ? C24 N4 Ni2 126.0(4) . . ? C20 N4 Ni2 115.2(4) . . ? O1 C1 C2 109.2(5) . . ? O1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? O1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N1 C2 C3 121.9(6) . . ? N1 C2 C1 116.7(5) . . ? C3 C2 C1 121.4(6) . . ? C4 C3 C2 119.3(6) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 119.1(6) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 118.8(7) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? N1 C6 C5 122.3(6) . . ? N1 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? O3 C7 C8 109.7(6) . . ? O3 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? O3 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N2 C8 C9 122.4(7) . . ? N2 C8 C7 115.9(6) . . ? C9 C8 C7 121.6(7) . . ? C10 C9 C8 118.9(8) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C11 C10 C9 118.8(7) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 120.0(8) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? N2 C12 C11 121.7(7) . . ? N2 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? O2 C13 C14 108.3(6) . . ? O2 C13 H13A 110.0 . . ? C14 C13 H13A 110.0 . . ? O2 C13 H13B 110.0 . . ? C14 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? N3 C14 C15 120.7(8) . . ? N3 C14 C13 116.6(6) . . ? C15 C14 C13 122.7(8) . . ? C16 C15 C14 118.3(9) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C17 C16 C15 121.2(9) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 116.8(8) . . ? C16 C17 H17 121.6 . . ? C18 C17 H17 121.6 . . ? N3 C18 C17 123.3(7) . . ? N3 C18 H18 118.3 . . ? C17 C18 H18 118.3 . . ? O4 C19 C20 107.5(5) . . ? O4 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? O4 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? N4 C20 C21 122.1(6) . . ? N4 C20 C19 115.7(5) . . ? C21 C20 C19 122.2(6) . . ? C22 C21 C20 118.6(7) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C23 C22 C21 118.8(6) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C24 C23 C22 119.6(6) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? N4 C24 C23 122.1(6) . . ? N4 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? Cl6 C25 Cl5 120.0(10) . . ? Cl6 C25 H25A 107.3 . . ? Cl5 C25 H25A 107.3 . . ? Cl6 C25 H25B 107.3 . . ? Cl5 C25 H25B 107.3 . . ? H25A C25 H25B 106.9 . . ? Cl7 C26 Cl8 135.0(16) . . ? Cl7 C26 H26A 103.4 . . ? Cl8 C26 H26A 103.4 . . ? Cl7 C26 H26B 103.4 . . ? Cl8 C26 H26B 103.4 . . ? H26A C26 H26B 105.2 . . ? Cl9 C27 Cl10 118.0(8) . . ? Cl9 C27 H27A 107.8 . . ? Cl10 C27 H27A 107.8 . . ? Cl9 C27 H27B 107.8 . . ? Cl10 C27 H27B 107.8 . . ? H27A C27 H27B 107.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Ni1 Cl1 Ni1 -92.96(13) . . . 2_565 ? N1 Ni1 Cl1 Ni1 57.7(7) . . . 2_565 ? O1 Ni1 Cl1 Ni1 95.20(13) . . . 2_565 ? N2 Ni1 Cl1 Ni1 -170.69(16) . . . 2_565 ? Cl1 Ni1 Cl1 Ni1 0.0 2_565 . . 2_565 ? N3 Ni2 Cl3 Ni2 -171.68(15) . . . 2_676 ? O2 Ni2 Cl3 Ni2 -93.90(12) . . . 2_676 ? N4 Ni2 Cl3 Ni2 85.2(9) . . . 2_676 ? O4 Ni2 Cl3 Ni2 93.14(13) . . . 2_676 ? Cl3 Ni2 Cl3 Ni2 0.0 2_676 . . 2_676 ? O3 Ni1 O1 C1 70.5(10) . . . . ? N1 Ni1 O1 C1 22.5(5) . . . . ? N2 Ni1 O1 C1 119.8(5) . . . . ? Cl1 Ni1 O1 C1 -150.6(4) . . . . ? Cl1 Ni1 O1 C1 -64.8(4) 2_565 . . . ? N3 Ni2 O2 C13 23.8(5) . . . . ? N4 Ni2 O2 C13 114.9(5) . . . . ? O4 Ni2 O2 C13 78.0(10) . . . . ? Cl3 Ni2 O2 C13 -151.8(5) 2_676 . . . ? Cl3 Ni2 O2 C13 -65.2(5) . . . . ? N1 Ni1 O3 C7 120.5(6) . . . . ? O1 Ni1 O3 C7 73.8(10) . . . . ? N2 Ni1 O3 C7 23.1(5) . . . . ? Cl1 Ni1 O3 C7 -64.9(5) . . . . ? Cl1 Ni1 O3 C7 -150.7(5) 2_565 . . . ? N3 Ni2 O4 C19 121.1(4) . . . . ? O2 Ni2 O4 C19 68.4(10) . . . . ? N4 Ni2 O4 C19 30.4(4) . . . . ? Cl3 Ni2 O4 C19 -61.9(4) 2_676 . . . ? Cl3 Ni2 O4 C19 -148.2(4) . . . . ? O3 Ni1 N1 C2 172.7(4) . . . . ? O1 Ni1 N1 C2 -16.5(4) . . . . ? N2 Ni1 N1 C2 -109.0(4) . . . . ? Cl1 Ni1 N1 C2 21.9(10) . . . . ? Cl1 Ni1 N1 C2 79.4(4) 2_565 . . . ? O3 Ni1 N1 C6 0.8(5) . . . . ? O1 Ni1 N1 C6 171.6(5) . . . . ? N2 Ni1 N1 C6 79.1(5) . . . . ? Cl1 Ni1 N1 C6 -150.0(6) . . . . ? Cl1 Ni1 N1 C6 -92.5(5) 2_565 . . . ? O3 Ni1 N2 C8 -14.2(5) . . . . ? N1 Ni1 N2 C8 -106.3(5) . . . . ? O1 Ni1 N2 C8 175.4(5) . . . . ? Cl1 Ni1 N2 C8 82.1(5) . . . . ? Cl1 Ni1 N2 C8 21.3(11) 2_565 . . . ? O3 Ni1 N2 C12 173.6(6) . . . . ? N1 Ni1 N2 C12 81.4(6) . . . . ? O1 Ni1 N2 C12 3.1(6) . . . . ? Cl1 Ni1 N2 C12 -90.2(6) . . . . ? Cl1 Ni1 N2 C12 -151.0(7) 2_565 . . . ? O2 Ni2 N3 C18 168.7(6) . . . . ? N4 Ni2 N3 C18 75.9(6) . . . . ? O4 Ni2 N3 C18 -1.7(6) . . . . ? Cl3 Ni2 N3 C18 -162.1(7) 2_676 . . . ? Cl3 Ni2 N3 C18 -94.9(6) . . . . ? O2 Ni2 N3 C14 -11.8(6) . . . . ? N4 Ni2 N3 C14 -104.6(6) . . . . ? O4 Ni2 N3 C14 177.8(6) . . . . ? Cl3 Ni2 N3 C14 17.3(14) 2_676 . . . ? Cl3 Ni2 N3 C14 84.6(6) . . . . ? N3 Ni2 N4 C24 67.9(5) . . . . ? O2 Ni2 N4 C24 -10.0(5) . . . . ? O4 Ni2 N4 C24 162.8(5) . . . . ? Cl3 Ni2 N4 C24 -104.5(5) 2_676 . . . ? Cl3 Ni2 N4 C24 170.9(6) . . . . ? N3 Ni2 N4 C20 -110.9(4) . . . . ? O2 Ni2 N4 C20 171.2(4) . . . . ? O4 Ni2 N4 C20 -16.0(4) . . . . ? Cl3 Ni2 N4 C20 76.8(4) 2_676 . . . ? Cl3 Ni2 N4 C20 -7.8(12) . . . . ? Ni1 O1 C1 C2 -24.1(7) . . . . ? C6 N1 C2 C3 1.7(9) . . . . ? Ni1 N1 C2 C3 -170.8(5) . . . . ? C6 N1 C2 C1 -179.5(6) . . . . ? Ni1 N1 C2 C1 8.0(7) . . . . ? O1 C1 C2 N1 10.5(8) . . . . ? O1 C1 C2 C3 -170.7(6) . . . . ? N1 C2 C3 C4 -0.1(11) . . . . ? C1 C2 C3 C4 -178.8(7) . . . . ? C2 C3 C4 C5 -1.6(11) . . . . ? C3 C4 C5 C6 1.6(11) . . . . ? C2 N1 C6 C5 -1.6(10) . . . . ? Ni1 N1 C6 C5 170.1(5) . . . . ? C4 C5 C6 N1 0.0(11) . . . . ? Ni1 O3 C7 C8 -27.6(9) . . . . ? C12 N2 C8 C9 -1.6(11) . . . . ? Ni1 N2 C8 C9 -174.4(6) . . . . ? C12 N2 C8 C7 175.8(7) . . . . ? Ni1 N2 C8 C7 2.9(9) . . . . ? O3 C7 C8 N2 16.0(11) . . . . ? O3 C7 C8 C9 -166.6(7) . . . . ? N2 C8 C9 C10 1.3(12) . . . . ? C7 C8 C9 C10 -175.9(8) . . . . ? C8 C9 C10 C11 0.5(13) . . . . ? C9 C10 C11 C12 -1.9(14) . . . . ? C8 N2 C12 C11 0.1(11) . . . . ? Ni1 N2 C12 C11 172.2(6) . . . . ? C10 C11 C12 N2 1.7(13) . . . . ? Ni2 O2 C13 C14 -30.2(8) . . . . ? C18 N3 C14 C15 -1.6(16) . . . . ? Ni2 N3 C14 C15 178.9(11) . . . . ? C18 N3 C14 C13 177.9(8) . . . . ? Ni2 N3 C14 C13 -1.6(11) . . . . ? O2 C13 C14 N3 20.8(12) . . . . ? O2 C13 C14 C15 -159.8(12) . . . . ? N3 C14 C15 C16 0(2) . . . . ? C13 C14 C15 C16 -179.3(15) . . . . ? C14 C15 C16 C17 2(3) . . . . ? C15 C16 C17 C18 -3(3) . . . . ? C14 N3 C18 C17 0.8(13) . . . . ? Ni2 N3 C18 C17 -179.7(8) . . . . ? C16 C17 C18 N3 1.3(19) . . . . ? Ni2 O4 C19 C20 -38.0(6) . . . . ? C24 N4 C20 C21 1.1(9) . . . . ? Ni2 N4 C20 C21 179.9(5) . . . . ? C24 N4 C20 C19 -179.6(5) . . . . ? Ni2 N4 C20 C19 -0.7(7) . . . . ? O4 C19 C20 N4 25.4(7) . . . . ? O4 C19 C20 C21 -155.2(6) . . . . ? N4 C20 C21 C22 -0.2(11) . . . . ? C19 C20 C21 C22 -179.5(6) . . . . ? C20 C21 C22 C23 -1.3(11) . . . . ? C21 C22 C23 C24 1.8(11) . . . . ? C20 N4 C24 C23 -0.5(9) . . . . ? Ni2 N4 C24 C23 -179.2(5) . . . . ? C22 C23 C24 N4 -0.9(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.076 _refine_diff_density_min -2.240 _refine_diff_density_rms 0.191 # Attachment 'Complex_Ni4_Na3__21_.cif' data_Ni4_Na3_21 _database_code_depnum_ccdc_archive 'CCDC 664566' _audit_creation_date 10-09-07 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H54 N9 Na3 Ni4 O10, C4 H8 O, 0.5(C4 H8 O), 0.5(C4 H8 O), Cl' _chemical_formula_sum 'C62 H70 Cl N9 Na3 Ni4 O12' _chemical_formula_weight 1472.53 _chemical_absolute_configuration . 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/n _symmetry_space_group_name_Hall '-P 4a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z' '-x, -y, -z' 'y-1/2, -x, -z' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z' _cell_length_a 29.892(6) _cell_length_b 29.892(6) _cell_length_c 16.945(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15141(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16231 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6104 _exptl_absorpt_coefficient_mu 1.090 _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 173(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 '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17234 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1952 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.46 _reflns_number_total 17234 _reflns_number_gt 8546 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Squeeze procedure has been used to avoid the problem of small solvent disorder' ; _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^)+(0.0800P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17234 _refine_ls_number_parameters 815 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1922 _refine_ls_R_factor_gt 0.0959 _refine_ls_wR_factor_ref 0.2424 _refine_ls_wR_factor_gt 0.2201 _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_restrained_S_all 1.222 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.15274(3) 0.04185(3) 0.21729(5) 0.0258(2) Uani 1 1 d . . . Ni2 Ni 0.21449(3) -0.04026(3) 0.19535(5) 0.0274(2) Uani 1 1 d . . . Ni3 Ni 0.13688(3) -0.02237(3) 0.07584(5) 0.0282(3) Uani 1 1 d . . . Ni4 Ni 0.04882(3) -0.10740(3) 0.34290(5) 0.0289(3) Uani 1 1 d . . . Cl1 Cl 0.24320(7) 0.06788(9) -0.00428(13) 0.0605(7) Uani 1 1 d . . . Na1 Na 0.09708(9) -0.01267(9) 0.31539(14) 0.0313(7) Uani 1 1 d . . . Na2 Na 0.15376(10) -0.09964(10) 0.28278(15) 0.0376(8) Uani 1 1 d . . . Na3 Na 0.07348(10) -0.07094(10) 0.17086(14) 0.0313(7) Uani 1 1 d . . . O1 O 0.10087(15) 0.00429(16) 0.1732(2) 0.0258(11) Uani 1 1 d . . . O2 O 0.11695(16) 0.06022(16) 0.3147(3) 0.0323(12) Uani 1 1 d . . . O3 O 0.17348(15) -0.01595(16) 0.2812(2) 0.0269(11) Uani 1 1 d . . . O4 O 0.18863(15) 0.01223(16) 0.1286(2) 0.0251(11) Uani 1 1 d . . . H4O H 0.2092 0.0308 0.0955 0.030 Uiso 1 1 calc . . . O5 O 0.15799(16) -0.07364(16) 0.1486(2) 0.0294(12) Uani 1 1 d . . . O6 O 0.22857(16) -0.09742(17) 0.2574(3) 0.0341(13) Uani 1 1 d . . . O7 O 0.08190(16) -0.05913(17) 0.0433(2) 0.0323(12) Uani 1 1 d . . . O8 O 0.03203(16) -0.05152(16) 0.2791(2) 0.0303(12) Uani 1 1 d . . . O9 O 0.10488(17) -0.07699(16) 0.3875(2) 0.0324(12) Uani 1 1 d . . . O10 O 0.08577(17) -0.13186(16) 0.2510(2) 0.0330(12) Uani 1 1 d . . . O11 O 0.1043(4) -0.0803(3) 0.6577(5) 0.126(4) Uani 1 1 d . . . O13 O 0.1867(6) -0.2453(6) 0.4021(10) 0.114(6) Uiso 0.50 1 d P . . O15 O -0.0229(5) -0.2893(6) 0.4001(9) 0.091(5) Uiso 0.50 1 d P . . N1 N 0.1213(2) 0.0899(2) 0.1485(3) 0.0291(14) Uani 1 1 d . . . N2 N 0.1971(2) 0.0875(2) 0.2620(3) 0.0301(15) Uani 1 1 d . . . N3 N 0.2614(2) -0.0035(2) 0.2637(3) 0.0292(14) Uani 1 1 d . . . N4 N 0.2658(2) -0.0638(2) 0.1245(3) 0.0320(15) Uani 1 1 d . . . N5 N 0.1782(2) -0.0575(2) -0.0023(3) 0.0365(17) Uani 1 1 d . . . N6 N 0.1117(2) 0.0198(2) -0.0111(3) 0.0312(15) Uani 1 1 d . . . N7 N 0.0684(2) -0.1560(2) 0.4236(3) 0.0318(15) Uani 1 1 d . . . N8 N -0.0005(2) -0.1463(2) 0.2862(3) 0.0357(16) Uani 1 1 d . . . N9 N 0.0034(2) -0.0767(2) 0.4223(3) 0.0296(14) Uani 1 1 d . . . C1 C 0.0649(2) 0.0328(3) 0.1567(4) 0.0330(18) Uani 1 1 d . . . H1A H 0.0459 0.0353 0.2044 0.040 Uiso 1 1 calc . . . H1B H 0.0465 0.0193 0.1143 0.040 Uiso 1 1 calc . . . C2 C 0.0792(3) 0.0790(2) 0.1314(4) 0.0286(18) Uani 1 1 d . . . C3 C 0.0502(3) 0.1076(3) 0.0915(4) 0.0333(18) Uani 1 1 d . . . H3 H 0.0204 0.0987 0.0799 0.040 Uiso 1 1 calc . . . C4 C 0.0659(3) 0.1492(3) 0.0691(4) 0.044(2) Uani 1 1 d . . . H4 H 0.0468 0.1698 0.0428 0.053 Uiso 1 1 calc . . . C5 C 0.1099(3) 0.1606(3) 0.0854(4) 0.039(2) Uani 1 1 d . . . H5 H 0.1218 0.1887 0.0696 0.046 Uiso 1 1 calc . . . C6 C 0.1357(3) 0.1303(3) 0.1249(4) 0.038(2) Uani 1 1 d . . . H6 H 0.1658 0.1383 0.1364 0.045 Uiso 1 1 calc . . . C7 C 0.1359(3) 0.0953(3) 0.3548(4) 0.0353(19) Uani 1 1 d . . . H7A H 0.1375 0.0873 0.4115 0.042 Uiso 1 1 calc . . . H7B H 0.1158 0.1216 0.3501 0.042 Uiso 1 1 calc . . . C8 C 0.1821(3) 0.1088(3) 0.3274(4) 0.0332(19) Uani 1 1 d . . . C9 C 0.2074(3) 0.1415(3) 0.3653(5) 0.046(2) Uani 1 1 d . . . H9 H 0.1964 0.1555 0.4118 0.055 Uiso 1 1 calc . . . C10 C 0.2486(3) 0.1535(3) 0.3345(5) 0.051(2) Uani 1 1 d . . . H10 H 0.2663 0.1758 0.3595 0.061 Uiso 1 1 calc . . . C11 C 0.2636(3) 0.1325(3) 0.2664(5) 0.051(2) Uani 1 1 d . . . H11 H 0.2915 0.1408 0.2438 0.061 Uiso 1 1 calc . . . C12 C 0.2381(3) 0.0994(3) 0.2314(4) 0.0364(19) Uani 1 1 d . . . C13 C 0.0573(3) -0.0405(3) -0.0172(4) 0.0343(19) Uani 1 1 d . . . H13A H 0.0259 -0.0375 0.0004 0.041 Uiso 1 1 calc . . . H13B H 0.0578 -0.0612 -0.0627 0.041 Uiso 1 1 calc . . . C14 C 0.0736(2) 0.0044(3) -0.0442(4) 0.0301(18) Uani 1 1 d . . . C15 C 0.0516(3) 0.0289(3) -0.1016(4) 0.045(2) Uani 1 1 d . . . H15 H 0.0250 0.0174 -0.1248 0.054 Uiso 1 1 calc . . . C16 C 0.0678(3) 0.0699(3) -0.1254(4) 0.050(2) Uani 1 1 d . . . H16 H 0.0521 0.0873 -0.1631 0.060 Uiso 1 1 calc . . . C17 C 0.1081(3) 0.0853(3) -0.0929(4) 0.042(2) Uani 1 1 d . . . H17 H 0.1213 0.1126 -0.1099 0.050 Uiso 1 1 calc . . . C18 C 0.1280(3) 0.0593(3) -0.0352(4) 0.039(2) Uani 1 1 d . . . H18 H 0.1546 0.0701 -0.0113 0.047 Uiso 1 1 calc . . . C19 C 0.1978(2) -0.0085(3) 0.3507(4) 0.0305(18) Uani 1 1 d . . . H19A H 0.1982 -0.0364 0.3823 0.037 Uiso 1 1 calc . . . H19B H 0.1824 0.0148 0.3823 0.037 Uiso 1 1 calc . . . C20 C 0.2450(3) 0.0061(2) 0.3355(4) 0.0307(18) Uani 1 1 d . . . C21 C 0.2706(3) 0.0286(3) 0.3922(4) 0.037(2) Uani 1 1 d . . . H21 H 0.2583 0.0352 0.4426 0.045 Uiso 1 1 calc . . . C22 C 0.3139(3) 0.0410(3) 0.3743(5) 0.043(2) Uani 1 1 d . . . H22 H 0.3319 0.0559 0.4123 0.052 Uiso 1 1 calc . . . C23 C 0.3307(3) 0.0314(3) 0.2994(5) 0.044(2) Uani 1 1 d . . . H23 H 0.3603 0.0396 0.2852 0.053 Uiso 1 1 calc . . . C24 C 0.3032(3) 0.0096(3) 0.2464(4) 0.038(2) Uani 1 1 d . . . H24 H 0.3144 0.0036 0.1951 0.045 Uiso 1 1 calc . . . C25 C 0.2664(3) -0.1190(3) 0.2315(4) 0.043(2) Uani 1 1 d . . . H25A H 0.2590 -0.1508 0.2220 0.051 Uiso 1 1 calc . . . H25B H 0.2892 -0.1179 0.2738 0.051 Uiso 1 1 calc . . . C26 C 0.2867(3) -0.0995(3) 0.1562(4) 0.0347(19) Uani 1 1 d . . . C27 C 0.3259(3) -0.1154(3) 0.1228(5) 0.047(2) Uani 1 1 d . . . H27 H 0.3400 -0.1410 0.1449 0.056 Uiso 1 1 calc . . . C28 C 0.3448(3) -0.0948(3) 0.0584(5) 0.047(2) Uani 1 1 d . . . H28 H 0.3719 -0.1055 0.0361 0.056 Uiso 1 1 calc . . . C29 C 0.3231(3) -0.0582(3) 0.0275(4) 0.039(2) Uani 1 1 d . . . H29 H 0.3354 -0.0429 -0.0167 0.046 Uiso 1 1 calc . . . C30 C 0.2833(3) -0.0435(3) 0.0608(4) 0.038(2) Uani 1 1 d . . . H30 H 0.2683 -0.0186 0.0383 0.046 Uiso 1 1 calc . . . C31 C 0.1686(3) -0.1109(3) 0.1030(4) 0.0361(19) Uani 1 1 d . . . H31A H 0.1412 -0.1290 0.0952 0.043 Uiso 1 1 calc . . . H31B H 0.1905 -0.1295 0.1321 0.043 Uiso 1 1 calc . . . C32 C 0.1877(3) -0.0992(3) 0.0239(4) 0.042(2) Uani 1 1 d . . . C33 C 0.2130(3) -0.1290(3) -0.0229(5) 0.054(2) Uani 1 1 d . . . H33 H 0.2188 -0.1584 -0.0046 0.065 Uiso 1 1 calc . . . C34 C 0.2291(3) -0.1153(4) -0.0946(6) 0.070(3) Uani 1 1 d . . . H34 H 0.2467 -0.1349 -0.1260 0.084 Uiso 1 1 calc . . . C35 C 0.2195(3) -0.0733(4) -0.1198(4) 0.061(3) Uani 1 1 d . . . H35 H 0.2300 -0.0637 -0.1699 0.073 Uiso 1 1 calc . . . C36 C 0.1942(3) -0.0437(3) -0.0735(4) 0.047(2) Uani 1 1 d . . . H36 H 0.1884 -0.0142 -0.0917 0.057 Uiso 1 1 calc . . . C37 C 0.0662(3) -0.1696(3) 0.2191(4) 0.038(2) Uani 1 1 d . . . H37A H 0.0781 -0.1964 0.2466 0.046 Uiso 1 1 calc . . . H37B H 0.0748 -0.1720 0.1628 0.046 Uiso 1 1 calc . . . C38 C 0.0155(3) -0.1696(2) 0.2253(4) 0.0345(19) Uani 1 1 d . . . C39 C -0.0043(3) -0.0298(3) 0.3064(4) 0.0348(19) Uani 1 1 d . . . H39A H -0.0299 -0.0366 0.2714 0.042 Uiso 1 1 calc . . . H39B H 0.0014 0.0028 0.3030 0.042 Uiso 1 1 calc . . . C40 C -0.0175(2) -0.0411(3) 0.3913(4) 0.0297(18) Uani 1 1 d . . . C41 C 0.1155(3) -0.0937(3) 0.4607(4) 0.045(2) Uani 1 1 d . . . H41A H 0.1024 -0.0740 0.5016 0.054 Uiso 1 1 calc . . . H41B H 0.1484 -0.0931 0.4672 0.054 Uiso 1 1 calc . . . C42 C 0.0991(3) -0.1414(3) 0.4744(4) 0.037(2) Uani 1 1 d . . . C43 C -0.0129(3) -0.1923(3) 0.1718(4) 0.044(2) Uani 1 1 d . . . H43 H -0.0007 -0.2079 0.1279 0.053 Uiso 1 1 calc . . . C44 C -0.0579(3) -0.1915(3) 0.1839(5) 0.050(2) Uani 1 1 d . . . H44 H -0.0774 -0.2070 0.1489 0.060 Uiso 1 1 calc . . . C45 C -0.0753(3) -0.1682(3) 0.2470(5) 0.050(2) Uani 1 1 d . . . H45 H -0.1066 -0.1668 0.2558 0.060 Uiso 1 1 calc . . . C46 C -0.0461(3) -0.1469(3) 0.2968(4) 0.044(2) Uani 1 1 d . . . H46 H -0.0581 -0.1318 0.3413 0.052 Uiso 1 1 calc . . . C47 C 0.1137(3) -0.1683(3) 0.5371(4) 0.050(2) Uani 1 1 d . . . H47 H 0.1351 -0.1572 0.5737 0.061 Uiso 1 1 calc . . . C48 C 0.0970(4) -0.2105(3) 0.5453(5) 0.060(3) Uani 1 1 d . . . H48 H 0.1064 -0.2289 0.5879 0.073 Uiso 1 1 calc . . . C49 C 0.0664(3) -0.2263(3) 0.4913(5) 0.053(2) Uani 1 1 d . . . H49 H 0.0551 -0.2560 0.4952 0.063 Uiso 1 1 calc . . . C50 C 0.0524(3) -0.1986(3) 0.4320(4) 0.041(2) Uani 1 1 d . . . H50 H 0.0309 -0.2093 0.3953 0.049 Uiso 1 1 calc . . . C51 C -0.0082(3) -0.0886(3) 0.4961(4) 0.036(2) Uani 1 1 d . . . H51 H 0.0061 -0.1140 0.5186 0.043 Uiso 1 1 calc . . . C52 C -0.0395(3) -0.0663(3) 0.5413(4) 0.039(2) Uani 1 1 d . . . H52 H -0.0462 -0.0757 0.5935 0.047 Uiso 1 1 calc . . . C53 C -0.0604(3) -0.0303(3) 0.5083(4) 0.043(2) Uani 1 1 d . . . H53 H -0.0826 -0.0145 0.5371 0.052 Uiso 1 1 calc . . . C54 C -0.0490(3) -0.0168(3) 0.4330(4) 0.039(2) Uani 1 1 d . . . H54 H -0.0627 0.0088 0.4102 0.046 Uiso 1 1 calc . . . C55 C 0.0650(5) -0.1022(5) 0.6864(6) 0.109(5) Uani 1 1 d . . . H55A H 0.0693 -0.1350 0.6874 0.130 Uiso 1 1 calc . . . H55B H 0.0388 -0.0951 0.6530 0.130 Uiso 1 1 calc . . . C56 C 0.1336(4) -0.0776(5) 0.7182(6) 0.099(5) Uani 1 1 d . . . H56A H 0.1580 -0.0563 0.7066 0.119 Uiso 1 1 calc . . . H56B H 0.1466 -0.1073 0.7307 0.119 Uiso 1 1 calc . . . C57 C 0.1039(4) -0.0607(4) 0.7854(6) 0.079(3) Uani 1 1 d . . . H57A H 0.1007 -0.0278 0.7840 0.095 Uiso 1 1 calc . . . H57B H 0.1158 -0.0698 0.8376 0.095 Uiso 1 1 calc . . . C58 C 0.0590(3) -0.0846(4) 0.7667(6) 0.067(3) Uani 1 1 d . . . H58A H 0.0533 -0.1091 0.8046 0.081 Uiso 1 1 calc . . . H58B H 0.0338 -0.0632 0.7687 0.081 Uiso 1 1 calc . . . C59 C -0.0341(8) -0.3306(8) 0.4104(12) 0.074(6) Uiso 0.50 1 d P . . H59A H -0.0542 -0.3333 0.4566 0.089 Uiso 0.50 1 calc P . . H59B H -0.0071 -0.3490 0.4202 0.089 Uiso 0.50 1 calc P . . C60 C -0.0572(9) -0.3466(9) 0.3390(15) 0.099(8) Uiso 0.50 1 d P . . H60A H -0.0899 -0.3485 0.3477 0.118 Uiso 0.50 1 calc P . . H60B H -0.0458 -0.3763 0.3228 0.118 Uiso 0.50 1 calc P . . C61 C 0.1816(7) -0.2156(7) 0.2767(11) 0.061(5) Uiso 0.50 1 d P . . H61A H 0.1590 -0.1989 0.2456 0.073 Uiso 0.50 1 calc P . . H61B H 0.2110 -0.2101 0.2516 0.073 Uiso 0.50 1 calc P . . C62 C -0.0233(8) -0.2815(8) 0.3250(13) 0.083(7) Uiso 0.50 1 d P . . H62A H 0.0080 -0.2803 0.3064 0.100 Uiso 0.50 1 calc P . . H62B H -0.0365 -0.2516 0.3164 0.100 Uiso 0.50 1 calc P . . C63 C 0.1828(7) -0.1977(7) 0.3482(12) 0.072(6) Uiso 0.50 1 d P . . H63A H 0.1552 -0.1807 0.3603 0.086 Uiso 0.50 1 calc P . . H63B H 0.2092 -0.1781 0.3554 0.086 Uiso 0.50 1 calc P . . C64 C 0.1726(8) -0.2583(8) 0.2695(13) 0.075(6) Uiso 0.50 1 d P . . H64A H 0.1453 -0.2630 0.2374 0.090 Uiso 0.50 1 calc P . . H64B H 0.1978 -0.2744 0.2447 0.090 Uiso 0.50 1 calc P . . C65 C -0.0462(7) -0.3118(7) 0.2788(11) 0.066(6) Uiso 0.50 1 d P . . H65A H -0.0271 -0.3240 0.2361 0.079 Uiso 0.50 1 calc P . . H65B H -0.0735 -0.2985 0.2556 0.079 Uiso 0.50 1 calc P . . C66 C 0.1669(8) -0.2706(8) 0.3364(14) 0.087(7) Uiso 0.50 1 d P . . H66A H 0.1782 -0.3017 0.3401 0.104 Uiso 0.50 1 calc P . . H66B H 0.1342 -0.2719 0.3456 0.104 Uiso 0.50 1 calc P . . 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 0.0226(5) 0.0316(6) 0.0231(4) -0.0010(4) 0.0015(4) -0.0006(5) Ni2 0.0244(6) 0.0340(6) 0.0239(4) -0.0032(4) 0.0021(4) 0.0024(5) Ni3 0.0249(6) 0.0406(6) 0.0190(4) -0.0018(4) 0.0022(4) -0.0031(5) Ni4 0.0330(6) 0.0311(6) 0.0228(4) 0.0006(4) 0.0056(4) -0.0004(5) Cl1 0.0353(14) 0.089(2) 0.0568(13) 0.0121(12) -0.0002(10) -0.0112(13) Na1 0.0325(18) 0.0337(18) 0.0279(14) -0.0015(12) 0.0054(12) -0.0015(14) Na2 0.0324(18) 0.050(2) 0.0305(14) -0.0047(14) 0.0051(13) 0.0035(16) Na3 0.0333(17) 0.0358(18) 0.0247(14) 0.0008(12) 0.0048(12) -0.0057(14) O1 0.023(3) 0.030(3) 0.025(2) -0.003(2) 0.001(2) -0.001(2) O2 0.033(3) 0.033(3) 0.031(3) -0.006(2) 0.005(2) -0.002(3) O3 0.022(3) 0.037(3) 0.022(2) -0.001(2) -0.001(2) 0.001(2) O4 0.021(3) 0.034(3) 0.020(2) 0.000(2) 0.0008(19) -0.003(2) O5 0.027(3) 0.037(3) 0.024(2) -0.007(2) 0.003(2) 0.003(2) O6 0.028(3) 0.038(3) 0.036(3) 0.003(2) 0.003(2) 0.010(3) O7 0.031(3) 0.044(3) 0.022(2) -0.001(2) -0.001(2) -0.004(3) O8 0.034(3) 0.031(3) 0.026(2) 0.003(2) 0.008(2) 0.001(3) O9 0.037(3) 0.037(3) 0.024(2) 0.002(2) 0.003(2) -0.002(3) O10 0.043(3) 0.029(3) 0.027(2) -0.006(2) 0.010(2) 0.003(3) O11 0.164(10) 0.137(9) 0.076(6) -0.016(6) 0.031(6) -0.013(8) N1 0.020(4) 0.029(4) 0.038(3) 0.000(3) 0.003(3) 0.004(3) N2 0.028(4) 0.031(4) 0.031(3) 0.000(3) 0.000(3) 0.004(3) N3 0.030(4) 0.029(4) 0.029(3) -0.004(3) 0.001(3) 0.006(3) N4 0.030(4) 0.040(4) 0.026(3) -0.006(3) -0.001(3) -0.006(3) N5 0.021(4) 0.061(5) 0.027(3) -0.007(3) -0.001(3) -0.008(4) N6 0.024(4) 0.046(4) 0.024(3) 0.004(3) 0.005(3) -0.005(3) N7 0.035(4) 0.036(4) 0.024(3) 0.003(3) 0.005(3) -0.001(3) N8 0.037(4) 0.033(4) 0.036(4) 0.004(3) 0.003(3) 0.001(3) N9 0.030(4) 0.036(4) 0.024(3) 0.001(3) 0.004(3) 0.000(3) C1 0.024(4) 0.040(5) 0.034(4) -0.006(3) 0.000(3) 0.000(4) C2 0.031(5) 0.030(5) 0.025(4) 0.000(3) 0.005(3) 0.004(4) C3 0.027(5) 0.037(5) 0.036(4) -0.002(4) -0.002(3) 0.002(4) C4 0.048(6) 0.041(6) 0.043(5) 0.000(4) -0.006(4) 0.009(5) C5 0.037(5) 0.037(5) 0.042(4) 0.012(4) 0.000(4) -0.002(4) C6 0.031(5) 0.042(5) 0.040(4) 0.011(4) -0.002(4) -0.001(4) C7 0.030(5) 0.039(5) 0.037(4) -0.009(4) 0.002(3) -0.001(4) C8 0.032(5) 0.030(5) 0.038(4) 0.006(3) -0.009(3) 0.008(4) C9 0.050(6) 0.041(6) 0.046(5) -0.011(4) -0.005(4) -0.006(5) C10 0.047(6) 0.041(6) 0.066(6) -0.010(5) -0.004(5) -0.017(5) C11 0.041(6) 0.053(6) 0.060(6) 0.010(5) 0.001(4) -0.004(5) C12 0.024(5) 0.038(5) 0.047(5) 0.010(4) -0.012(4) -0.002(4) C13 0.031(5) 0.044(5) 0.028(4) -0.006(3) 0.001(3) -0.001(4) C14 0.025(4) 0.050(5) 0.015(3) -0.004(3) 0.001(3) -0.008(4) C15 0.045(6) 0.058(6) 0.032(4) -0.002(4) -0.014(4) -0.005(5) C16 0.054(6) 0.064(7) 0.032(4) 0.002(4) -0.012(4) 0.008(5) C17 0.049(6) 0.048(6) 0.029(4) 0.013(4) -0.001(4) -0.001(5) C18 0.027(5) 0.063(6) 0.027(4) -0.003(4) 0.005(3) -0.006(4) C19 0.021(4) 0.049(5) 0.021(3) 0.001(3) -0.005(3) 0.004(4) C20 0.033(5) 0.031(5) 0.028(4) 0.005(3) -0.009(3) 0.006(4) C21 0.039(5) 0.043(5) 0.030(4) 0.001(4) -0.009(4) -0.003(4) C22 0.042(6) 0.044(6) 0.044(5) 0.002(4) -0.018(4) 0.001(4) C23 0.031(5) 0.049(6) 0.052(5) 0.003(4) -0.003(4) -0.001(4) C24 0.037(5) 0.040(5) 0.036(4) -0.001(4) 0.002(4) 0.000(4) C25 0.033(5) 0.049(6) 0.046(5) 0.009(4) 0.004(4) 0.008(4) C26 0.024(4) 0.045(5) 0.035(4) -0.007(4) -0.009(3) 0.003(4) C27 0.042(6) 0.051(6) 0.047(5) -0.014(4) -0.001(4) 0.010(5) C28 0.036(5) 0.063(7) 0.042(5) -0.024(4) 0.004(4) 0.009(5) C29 0.030(5) 0.056(6) 0.029(4) -0.008(4) 0.009(3) 0.003(4) C30 0.035(5) 0.051(6) 0.029(4) -0.008(4) -0.002(3) -0.013(4) C31 0.040(5) 0.034(5) 0.035(4) -0.012(3) 0.001(4) -0.004(4) C32 0.032(5) 0.058(6) 0.035(4) -0.013(4) -0.002(4) -0.011(5) C33 0.039(6) 0.062(7) 0.062(6) -0.022(5) 0.006(5) -0.005(5) C34 0.057(7) 0.095(9) 0.058(6) -0.035(6) 0.027(5) -0.015(7) C35 0.045(6) 0.115(10) 0.023(4) -0.025(5) 0.018(4) -0.027(6) C36 0.034(5) 0.082(7) 0.026(4) -0.007(4) 0.003(4) -0.011(5) C37 0.049(6) 0.038(5) 0.027(4) -0.007(3) 0.011(4) 0.001(4) C38 0.051(6) 0.019(4) 0.033(4) 0.004(3) 0.001(4) -0.004(4) C39 0.035(5) 0.038(5) 0.031(4) 0.004(3) 0.006(3) 0.002(4) C40 0.032(5) 0.030(5) 0.026(4) -0.002(3) 0.003(3) -0.006(4) C41 0.042(5) 0.059(6) 0.033(4) 0.005(4) -0.005(4) 0.005(5) C42 0.045(5) 0.034(5) 0.030(4) 0.001(3) 0.008(4) 0.012(4) C43 0.051(6) 0.041(5) 0.039(4) -0.004(4) 0.002(4) -0.007(5) C44 0.054(7) 0.046(6) 0.051(5) -0.008(4) -0.010(5) -0.009(5) C45 0.037(5) 0.061(6) 0.052(5) 0.001(5) -0.008(4) -0.005(5) C46 0.059(6) 0.032(5) 0.040(5) 0.001(4) 0.002(4) 0.000(5) C47 0.061(7) 0.055(6) 0.035(4) 0.008(4) -0.014(4) 0.002(5) C48 0.083(8) 0.052(7) 0.046(5) 0.016(5) -0.006(5) 0.020(6) C49 0.057(6) 0.040(6) 0.060(6) 0.012(5) 0.004(5) 0.008(5) C50 0.045(6) 0.042(6) 0.035(4) 0.003(4) 0.010(4) 0.008(5) C51 0.042(5) 0.038(5) 0.028(4) 0.002(3) 0.006(3) -0.007(4) C52 0.041(5) 0.045(6) 0.032(4) -0.001(4) 0.010(4) -0.007(4) C53 0.039(5) 0.054(6) 0.037(4) -0.006(4) 0.011(4) 0.010(5) C54 0.037(5) 0.047(5) 0.032(4) -0.005(4) 0.001(4) 0.010(4) C55 0.113(11) 0.162(14) 0.050(6) -0.004(7) 0.014(7) -0.077(11) C56 0.050(7) 0.193(15) 0.053(6) 0.020(8) -0.004(6) -0.003(8) C57 0.066(8) 0.096(9) 0.076(7) -0.037(6) 0.007(6) -0.018(7) C58 0.064(7) 0.079(8) 0.059(6) 0.008(5) 0.005(5) 0.011(6) _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 O2 2.042(4) . ? Ni1 O4 2.047(4) . ? Ni1 N2 2.047(6) . ? Ni1 O1 2.055(5) . ? Ni1 N1 2.075(6) . ? Ni1 O3 2.131(5) . ? Ni1 Na1 2.861(3) . ? Ni2 O3 2.037(4) . ? Ni2 O6 2.050(5) . ? Ni2 N4 2.070(6) . ? Ni2 O4 2.083(5) . ? Ni2 O5 2.116(5) . ? Ni2 N3 2.125(6) . ? Ni2 Na2 2.940(3) . ? Ni3 O7 2.052(5) . ? Ni3 O4 2.065(4) . ? Ni3 O5 2.065(5) . ? Ni3 N6 2.080(6) . ? Ni3 N5 2.093(6) . ? Ni3 O1 2.126(4) . ? Ni3 Na3 2.880(3) . ? Ni4 O10 2.045(4) . ? Ni4 O9 2.051(5) . ? Ni4 O8 2.052(5) . ? Ni4 N7 2.080(6) . ? Ni4 N8 2.108(6) . ? Ni4 N9 2.120(6) . ? Ni4 Na3 3.198(3) . ? Ni4 Na1 3.212(3) . ? Ni4 Na2 3.306(3) . ? Na1 O2 2.259(6) . ? Na1 O9 2.290(5) . ? Na1 O8 2.347(6) . ? Na1 O3 2.358(5) . ? Na1 O1 2.464(5) . ? Na1 Na3 3.087(4) . ? Na1 Na2 3.152(4) . ? Na2 O6 2.278(6) . ? Na2 O10 2.313(6) . ? Na2 O9 2.396(5) . ? Na2 O5 2.407(5) . ? Na2 O3 2.570(6) . ? Na2 Na3 3.177(4) . ? Na3 O7 2.204(5) . ? Na3 O8 2.289(5) . ? Na3 O10 2.301(5) . ? Na3 O1 2.394(5) . ? Na3 O5 2.555(5) . ? O1 C1 1.400(9) . ? O2 C7 1.372(9) . ? O3 C19 1.402(8) . ? O4 H4O 1.0000 . ? O5 C31 1.392(8) . ? O6 C25 1.374(9) . ? O7 C13 1.379(8) . ? O8 C39 1.347(8) . ? O9 C41 1.375(8) . ? O10 C37 1.381(9) . ? O11 C56 1.352(13) . ? O11 C55 1.429(14) . ? O13 C66 1.47(3) . ? O13 C63 1.70(3) . ? O15 C59 1.29(2) . ? O15 C62 1.29(2) . ? N1 C2 1.333(9) . ? N1 C6 1.342(9) . ? N2 C8 1.355(9) . ? N2 C12 1.378(9) . ? N3 C24 1.341(9) . ? N3 C20 1.342(9) . ? N4 C30 1.346(9) . ? N4 C26 1.349(9) . ? N5 C32 1.353(10) . ? N5 C36 1.363(9) . ? N6 C18 1.342(10) . ? N6 C14 1.350(9) . ? N7 C42 1.332(9) . ? N7 C50 1.366(10) . ? N8 C38 1.335(9) . ? N8 C46 1.375(10) . ? N9 C40 1.340(9) . ? N9 C51 1.346(8) . ? C1 C2 1.509(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.391(10) . ? C3 C4 1.385(11) . ? C3 H3 0.9500 . ? C4 C5 1.386(11) . ? C4 H4 0.9500 . ? C5 C6 1.366(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.514(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.392(11) . ? C9 C10 1.385(12) . ? C9 H9 0.9500 . ? C10 C11 1.390(12) . ? C10 H10 0.9500 . ? C11 C12 1.382(11) . ? C11 H11 0.9500 . ? C13 C14 1.499(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.385(11) . ? C15 C16 1.377(12) . ? C15 H15 0.9500 . ? C16 C17 1.402(12) . ? C16 H16 0.9500 . ? C17 C18 1.382(11) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.500(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.401(10) . ? C21 C22 1.379(11) . ? C21 H21 0.9500 . ? C22 C23 1.395(11) . ? C22 H22 0.9500 . ? C23 C24 1.381(11) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.528(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.383(11) . ? C27 C28 1.374(12) . ? C27 H27 0.9500 . ? C28 C29 1.375(11) . ? C28 H28 0.9500 . ? C29 C30 1.388(10) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.499(10) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.410(11) . ? C33 C34 1.369(13) . ? C33 H33 0.9500 . ? C34 C35 1.359(15) . ? C34 H34 0.9500 . ? C35 C36 1.402(13) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.520(11) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C43 1.416(11) . ? C39 C40 1.529(9) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C54 1.385(10) . ? C41 C42 1.524(11) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C47 1.402(10) . ? C43 C44 1.361(12) . ? C43 H43 0.9500 . ? C44 C45 1.378(12) . ? C44 H44 0.9500 . ? C45 C46 1.369(11) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.364(13) . ? C47 H47 0.9500 . ? C48 C49 1.378(13) . ? C48 H48 0.9500 . ? C49 C50 1.369(11) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.380(11) . ? C51 H51 0.9500 . ? C52 C53 1.365(11) . ? C52 H52 0.9500 . ? C53 C54 1.380(10) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C58 1.469(14) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.528(15) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.553(14) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.47(3) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C65 1.49(3) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C64 1.31(3) . ? C61 C63 1.32(2) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C65 1.38(3) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C66 1.20(3) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? 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 O4 169.69(19) . . ? O2 Ni1 N2 82.0(2) . . ? O4 Ni1 N2 102.7(2) . . ? O2 Ni1 O1 92.59(18) . . ? O4 Ni1 O1 83.84(18) . . ? N2 Ni1 O1 170.8(2) . . ? O2 Ni1 N1 91.8(2) . . ? O4 Ni1 N1 97.2(2) . . ? N2 Ni1 N1 92.3(2) . . ? O1 Ni1 N1 80.4(2) . . ? O2 Ni1 O3 87.68(18) . . ? O4 Ni1 O3 82.53(17) . . ? N2 Ni1 O3 99.4(2) . . ? O1 Ni1 O3 87.77(18) . . ? N1 Ni1 O3 168.1(2) . . ? O2 Ni1 Na1 51.61(15) . . ? O4 Ni1 Na1 118.99(14) . . ? N2 Ni1 Na1 122.76(17) . . ? O1 Ni1 Na1 57.38(13) . . ? N1 Ni1 Na1 117.22(18) . . ? O3 Ni1 Na1 53.99(14) . . ? O3 Ni2 O6 93.13(19) . . ? O3 Ni2 N4 168.9(2) . . ? O6 Ni2 N4 82.0(2) . . ? O3 Ni2 O4 84.01(17) . . ? O6 Ni2 O4 169.29(19) . . ? N4 Ni2 O4 102.5(2) . . ? O3 Ni2 O5 87.43(17) . . ? O6 Ni2 O5 87.86(19) . . ? N4 Ni2 O5 102.3(2) . . ? O4 Ni2 O5 81.70(18) . . ? O3 Ni2 N3 79.8(2) . . ? O6 Ni2 N3 90.9(2) . . ? N4 Ni2 N3 90.2(2) . . ? O4 Ni2 N3 98.7(2) . . ? O5 Ni2 N3 167.12(19) . . ? O3 Ni2 Na2 58.91(15) . . ? O6 Ni2 Na2 50.58(15) . . ? N4 Ni2 Na2 122.94(19) . . ? O4 Ni2 Na2 119.95(14) . . ? O5 Ni2 Na2 53.91(13) . . ? N3 Ni2 Na2 116.41(16) . . ? O7 Ni3 O4 169.89(17) . . ? O7 Ni3 O5 90.42(19) . . ? O4 Ni3 O5 83.36(18) . . ? O7 Ni3 N6 81.1(2) . . ? O4 Ni3 N6 105.9(2) . . ? O5 Ni3 N6 169.4(2) . . ? O7 Ni3 N5 91.9(2) . . ? O4 Ni3 N5 94.8(2) . . ? O5 Ni3 N5 79.9(2) . . ? N6 Ni3 N5 94.0(2) . . ? O7 Ni3 O1 90.20(18) . . ? O4 Ni3 O1 81.67(17) . . ? O5 Ni3 O1 88.25(17) . . ? N6 Ni3 O1 98.0(2) . . ? N5 Ni3 O1 168.0(2) . . ? O7 Ni3 Na3 49.68(13) . . ? O4 Ni3 Na3 120.23(13) . . ? O5 Ni3 Na3 59.55(14) . . ? N6 Ni3 Na3 117.61(17) . . ? N5 Ni3 Na3 119.2(2) . . ? O1 Ni3 Na3 54.66(14) . . ? O10 Ni4 O9 89.88(19) . . ? O10 Ni4 O8 91.26(18) . . ? O9 Ni4 O8 91.90(19) . . ? O10 Ni4 N7 95.7(2) . . ? O9 Ni4 N7 80.6(2) . . ? O8 Ni4 N7 169.8(2) . . ? O10 Ni4 N8 80.4(2) . . ? O9 Ni4 N8 169.5(2) . . ? O8 Ni4 N8 92.1(2) . . ? N7 Ni4 N8 96.4(2) . . ? O10 Ni4 N9 169.7(2) . . ? O9 Ni4 N9 95.6(2) . . ? O8 Ni4 N9 79.9(2) . . ? N7 Ni4 N9 93.8(2) . . ? N8 Ni4 N9 94.6(2) . . ? O10 Ni4 Na3 45.81(14) . . ? O9 Ni4 Na3 89.81(13) . . ? O8 Ni4 Na3 45.49(13) . . ? N7 Ni4 Na3 140.57(17) . . ? N8 Ni4 Na3 86.17(17) . . ? N9 Ni4 Na3 125.35(17) . . ? O10 Ni4 Na1 87.82(15) . . ? O9 Ni4 Na1 45.23(14) . . ? O8 Ni4 Na1 46.82(15) . . ? N7 Ni4 Na1 125.80(19) . . ? N8 Ni4 Na1 137.18(17) . . ? N9 Ni4 Na1 89.90(17) . . ? Na3 Ni4 Na1 57.58(7) . . ? O10 Ni4 Na2 43.77(15) . . ? O9 Ni4 Na2 46.15(14) . . ? O8 Ni4 Na2 90.73(14) . . ? N7 Ni4 Na2 89.09(18) . . ? N8 Ni4 Na2 124.15(18) . . ? N9 Ni4 Na2 140.61(17) . . ? Na3 Ni4 Na2 58.44(7) . . ? Na1 Ni4 Na2 57.81(7) . . ? O2 Na1 O9 141.8(2) . . ? O2 Na1 O8 133.9(2) . . ? O9 Na1 O8 78.96(19) . . ? O2 Na1 O3 77.53(19) . . ? O9 Na1 O3 89.86(19) . . ? O8 Na1 O3 135.86(19) . . ? O2 Na1 O1 77.55(18) . . ? O9 Na1 O1 133.6(2) . . ? O8 Na1 O1 83.34(17) . . ? O3 Na1 O1 73.98(16) . . ? O2 Na1 Ni1 45.13(12) . . ? O9 Na1 Ni1 136.80(17) . . ? O8 Na1 Ni1 127.71(14) . . ? O3 Na1 Ni1 46.99(12) . . ? O1 Na1 Ni1 44.62(12) . . ? O2 Na1 Na3 126.90(16) . . ? O9 Na1 Na3 88.45(15) . . ? O8 Na1 Na3 47.45(13) . . ? O3 Na1 Na3 90.18(14) . . ? O1 Na1 Na3 49.54(13) . . ? Ni1 Na1 Na3 89.62(8) . . ? O2 Na1 Na2 130.80(17) . . ? O9 Na1 Na2 49.18(14) . . ? O8 Na1 Na2 89.51(15) . . ? O3 Na1 Na2 53.28(14) . . ? O1 Na1 Na2 88.49(14) . . ? Ni1 Na1 Na2 93.17(9) . . ? Na3 Na1 Na2 61.21(9) . . ? O2 Na1 Ni4 165.79(17) . . ? O9 Na1 Ni4 39.48(13) . . ? O8 Na1 Ni4 39.60(12) . . ? O3 Na1 Ni4 115.72(16) . . ? O1 Na1 Ni4 110.11(14) . . ? Ni1 Na1 Ni4 147.95(10) . . ? Na3 Na1 Ni4 60.99(7) . . ? Na2 Na1 Ni4 62.60(8) . . ? O6 Na2 O10 146.2(2) . . ? O6 Na2 O9 136.9(2) . . ? O10 Na2 O9 75.79(18) . . ? O6 Na2 O5 76.14(18) . . ? O10 Na2 O5 87.72(18) . . ? O9 Na2 O5 129.8(2) . . ? O6 Na2 O3 75.21(19) . . ? O10 Na2 O3 127.2(2) . . ? O9 Na2 O3 82.67(17) . . ? O5 Na2 O3 70.36(17) . . ? O6 Na2 Ni2 44.03(13) . . ? O10 Na2 Ni2 132.58(16) . . ? O9 Na2 Ni2 125.39(17) . . ? O5 Na2 Ni2 45.28(13) . . ? O3 Na2 Ni2 42.74(11) . . ? O6 Na2 Na1 122.46(18) . . ? O10 Na2 Na1 84.94(15) . . ? O9 Na2 Na1 46.32(13) . . ? O5 Na2 Na1 85.84(15) . . ? O3 Na2 Na1 47.33(12) . . ? Ni2 Na2 Na1 85.54(10) . . ? O6 Na2 Na3 128.37(16) . . ? O10 Na2 Na3 46.32(14) . . ? O9 Na2 Na3 84.56(15) . . ? O5 Na2 Na3 52.28(13) . . ? O3 Na2 Na3 84.50(14) . . ? Ni2 Na2 Na3 90.15(9) . . ? Na1 Na2 Na3 58.39(9) . . ? O6 Na2 Ni4 172.54(17) . . ? O10 Na2 Ni4 37.71(11) . . ? O9 Na2 Ni4 38.11(12) . . ? O5 Na2 Ni4 111.32(15) . . ? O3 Na2 Ni4 106.80(14) . . ? Ni2 Na2 Ni4 141.58(11) . . ? Na1 Na2 Ni4 59.59(7) . . ? Na3 Na2 Ni4 59.08(7) . . ? O7 Na3 O8 143.8(2) . . ? O7 Na3 O10 133.4(2) . . ? O8 Na3 O10 79.29(18) . . ? O7 Na3 O1 80.04(18) . . ? O8 Na3 O1 86.17(18) . . ? O10 Na3 O1 132.8(2) . . ? O7 Na3 O5 75.36(17) . . ? O8 Na3 O5 131.42(19) . . ? O10 Na3 O5 84.51(19) . . ? O1 Na3 O5 72.19(17) . . ? O7 Na3 Ni3 45.24(13) . . ? O8 Na3 Ni3 132.58(17) . . ? O10 Na3 Ni3 128.60(17) . . ? O1 Na3 Ni3 46.42(11) . . ? O5 Na3 Ni3 44.17(12) . . ? O7 Na3 Na1 131.40(18) . . ? O8 Na3 Na1 49.05(14) . . ? O10 Na3 Na1 86.68(14) . . ? O1 Na3 Na1 51.56(12) . . ? O5 Na3 Na1 84.79(13) . . ? Ni3 Na3 Na1 90.50(9) . . ? O7 Na3 Na2 122.84(17) . . ? O8 Na3 Na2 89.93(15) . . ? O10 Na3 Na2 46.64(15) . . ? O1 Na3 Na2 89.15(15) . . ? O5 Na3 Na2 48.16(12) . . ? Ni3 Na3 Na2 88.44(9) . . ? Na1 Na3 Na2 60.40(9) . . ? O7 Na3 Ni4 167.05(18) . . ? O8 Na3 Ni4 39.73(12) . . ? O10 Na3 Ni4 39.59(12) . . ? O1 Na3 Ni4 112.55(13) . . ? O5 Na3 Ni4 110.59(13) . . ? Ni3 Na3 Ni4 146.42(10) . . ? Na1 Na3 Ni4 61.43(7) . . ? Na2 Na3 Ni4 62.48(7) . . ? C1 O1 Ni1 108.7(4) . . ? C1 O1 Ni3 117.5(4) . . ? Ni1 O1 Ni3 96.01(19) . . ? C1 O1 Na3 107.8(4) . . ? Ni1 O1 Na3 141.0(2) . . ? Ni3 O1 Na3 78.92(16) . . ? C1 O1 Na1 106.6(4) . . ? Ni1 O1 Na1 78.00(15) . . ? Ni3 O1 Na1 134.8(2) . . ? Na3 O1 Na1 78.90(16) . . ? C7 O2 Ni1 113.0(4) . . ? C7 O2 Na1 147.5(4) . . ? Ni1 O2 Na1 83.25(18) . . ? C19 O3 Ni2 110.2(4) . . ? C19 O3 Ni1 116.6(4) . . ? Ni2 O3 Ni1 95.80(17) . . ? C19 O3 Na1 106.8(4) . . ? Ni2 O3 Na1 140.6(2) . . ? Ni1 O3 Na1 79.02(16) . . ? C19 O3 Na2 105.4(4) . . ? Ni2 O3 Na2 78.36(16) . . ? Ni1 O3 Na2 136.7(2) . . ? Na1 O3 Na2 79.39(17) . . ? Ni1 O4 Ni3 98.16(19) . . ? Ni1 O4 Ni2 97.01(17) . . ? Ni3 O4 Ni2 97.8(2) . . ? Ni1 O4 H4O 119.6 . . ? Ni3 O4 H4O 119.6 . . ? Ni2 O4 H4O 119.6 . . ? C31 O5 Ni3 109.4(4) . . ? C31 O5 Ni2 113.8(4) . . ? Ni3 O5 Ni2 96.7(2) . . ? C31 O5 Na2 106.2(4) . . ? Ni3 O5 Na2 142.0(2) . . ? Ni2 O5 Na2 80.81(16) . . ? C31 O5 Na3 109.4(4) . . ? Ni3 O5 Na3 76.28(16) . . ? Ni2 O5 Na3 136.0(2) . . ? Na2 O5 Na3 79.56(16) . . ? C25 O6 Ni2 113.4(4) . . ? C25 O6 Na2 148.7(5) . . ? Ni2 O6 Na2 85.39(19) . . ? C13 O7 Ni3 114.2(4) . . ? C13 O7 Na3 137.1(4) . . ? Ni3 O7 Na3 85.08(18) . . ? C39 O8 Ni4 114.2(4) . . ? C39 O8 Na3 146.5(4) . . ? Ni4 O8 Na3 94.8(2) . . ? C39 O8 Na1 109.8(4) . . ? Ni4 O8 Na1 93.6(2) . . ? Na3 O8 Na1 83.50(18) . . ? C41 O9 Ni4 111.1(5) . . ? C41 O9 Na1 144.2(5) . . ? Ni4 O9 Na1 95.3(2) . . ? C41 O9 Na2 115.1(5) . . ? Ni4 O9 Na2 95.74(19) . . ? Na1 O9 Na2 84.49(17) . . ? C37 O10 Ni4 111.2(4) . . ? C37 O10 Na3 110.4(4) . . ? Ni4 O10 Na3 94.6(2) . . ? C37 O10 Na2 143.4(5) . . ? Ni4 O10 Na2 98.5(2) . . ? Na3 O10 Na2 87.0(2) . . ? C56 O11 C55 107.4(9) . . ? C66 O13 C63 89.8(15) . . ? C59 O15 C62 107.6(19) . . ? C2 N1 C6 117.3(6) . . ? C2 N1 Ni1 112.4(5) . . ? C6 N1 Ni1 130.2(5) . . ? C8 N2 C12 118.7(6) . . ? C8 N2 Ni1 113.7(5) . . ? C12 N2 Ni1 127.5(5) . . ? C24 N3 C20 118.4(6) . . ? C24 N3 Ni2 130.3(5) . . ? C20 N3 Ni2 111.3(5) . . ? C30 N4 C26 119.7(7) . . ? C30 N4 Ni2 126.9(6) . . ? C26 N4 Ni2 112.5(5) . . ? C32 N5 C36 119.7(7) . . ? C32 N5 Ni3 112.3(5) . . ? C36 N5 Ni3 128.0(6) . . ? C18 N6 C14 118.7(6) . . ? C18 N6 Ni3 128.2(5) . . ? C14 N6 Ni3 113.1(5) . . ? C42 N7 C50 118.7(6) . . ? C42 N7 Ni4 112.9(5) . . ? C50 N7 Ni4 128.3(5) . . ? C38 N8 C46 116.6(7) . . ? C38 N8 Ni4 113.0(5) . . ? C46 N8 Ni4 129.9(5) . . ? C40 N9 C51 117.0(6) . . ? C40 N9 Ni4 113.1(4) . . ? C51 N9 Ni4 129.8(5) . . ? O1 C1 C2 113.4(6) . . ? O1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? O1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? N1 C2 C3 122.9(7) . . ? N1 C2 C1 115.4(6) . . ? C3 C2 C1 121.6(7) . . ? C4 C3 C2 118.4(7) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 119.2(8) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 118.1(8) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? N1 C6 C5 124.2(7) . . ? N1 C6 H6 117.9 . . ? C5 C6 H6 117.9 . . ? O2 C7 C8 115.3(6) . . ? O2 C7 H7A 108.4 . . ? C8 C7 H7A 108.4 . . ? O2 C7 H7B 108.4 . . ? C8 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? N2 C8 C9 122.0(7) . . ? N2 C8 C7 115.3(6) . . ? C9 C8 C7 122.7(7) . . ? C10 C9 C8 119.4(8) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 118.9(8) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C12 C11 C10 120.1(8) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? N2 C12 C11 121.0(8) . . ? O7 C13 C14 114.6(6) . . ? O7 C13 H13A 108.6 . . ? C14 C13 H13A 108.6 . . ? O7 C13 H13B 108.6 . . ? C14 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? N6 C14 C15 120.8(7) . . ? N6 C14 C13 116.8(6) . . ? C15 C14 C13 122.3(7) . . ? C16 C15 C14 120.5(7) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 118.8(8) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C18 C17 C16 117.5(8) . . ? C18 C17 H17 121.3 . . ? C16 C17 H17 121.3 . . ? N6 C18 C17 123.7(7) . . ? N6 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? O3 C19 C20 112.9(5) . . ? O3 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? O3 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? N3 C20 C21 121.7(7) . . ? N3 C20 C19 116.0(6) . . ? C21 C20 C19 122.4(6) . . ? C22 C21 C20 119.4(7) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 118.8(7) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C24 C23 C22 118.3(8) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? N3 C24 C23 123.4(7) . . ? N3 C24 H24 118.3 . . ? C23 C24 H24 118.3 . . ? O6 C25 C26 114.5(6) . . ? O6 C25 H25A 108.6 . . ? C26 C25 H25A 108.6 . . ? O6 C25 H25B 108.6 . . ? C26 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? N4 C26 C27 120.1(7) . . ? N4 C26 C25 116.7(7) . . ? C27 C26 C25 123.2(7) . . ? C28 C27 C26 121.3(8) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 117.8(7) . . ? C27 C28 H28 121.1 . . ? C29 C28 H28 121.1 . . ? C28 C29 C30 120.0(7) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? N4 C30 C29 121.2(8) . . ? N4 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? O5 C31 C32 113.4(7) . . ? O5 C31 H31A 108.9 . . ? C32 C31 H31A 108.9 . . ? O5 C31 H31B 108.9 . . ? C32 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? N5 C32 C33 120.7(8) . . ? N5 C32 C31 115.3(7) . . ? C33 C32 C31 124.1(9) . . ? C34 C33 C32 119.9(10) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C33 118.7(9) . . ? C35 C34 H34 120.7 . . ? C33 C34 H34 120.7 . . ? C34 C35 C36 121.4(8) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? N5 C36 C35 119.6(9) . . ? N5 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? O10 C37 C38 113.3(6) . . ? O10 C37 H37A 108.9 . . ? C38 C37 H37A 108.9 . . ? O10 C37 H37B 108.9 . . ? C38 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? N8 C38 C43 122.1(8) . . ? N8 C38 C37 114.2(7) . . ? C43 C38 C37 123.7(7) . . ? O8 C39 C40 115.0(6) . . ? O8 C39 H39A 108.5 . . ? C40 C39 H39A 108.5 . . ? O8 C39 H39B 108.5 . . ? C40 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? N9 C40 C54 122.2(6) . . ? N9 C40 C39 115.1(6) . . ? C54 C40 C39 122.6(7) . . ? O9 C41 C42 113.8(6) . . ? O9 C41 H41A 108.8 . . ? C42 C41 H41A 108.8 . . ? O9 C41 H41B 108.8 . . ? C42 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? N7 C42 C47 121.0(8) . . ? N7 C42 C41 115.5(6) . . ? C47 C42 C41 123.5(8) . . ? C44 C43 C38 119.2(7) . . ? C44 C43 H43 120.4 . . ? C38 C43 H43 120.4 . . ? C43 C44 C45 119.8(8) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C46 C45 C44 118.3(8) . . ? C46 C45 H45 120.9 . . ? C44 C45 H45 120.9 . . ? C45 C46 N8 123.9(7) . . ? C45 C46 H46 118.0 . . ? N8 C46 H46 118.0 . . ? C48 C47 C42 119.6(8) . . ? C48 C47 H47 120.2 . . ? C42 C47 H47 120.2 . . ? C47 C48 C49 119.5(8) . . ? C47 C48 H48 120.2 . . ? C49 C48 H48 120.2 . . ? C50 C49 C48 118.8(8) . . ? C50 C49 H49 120.6 . . ? C48 C49 H49 120.6 . . ? N7 C50 C49 122.3(8) . . ? N7 C50 H50 118.9 . . ? C49 C50 H50 118.9 . . ? N9 C51 C52 124.2(7) . . ? N9 C51 H51 117.9 . . ? C52 C51 H51 117.9 . . ? C53 C52 C51 117.6(7) . . ? C53 C52 H52 121.2 . . ? C51 C52 H52 121.2 . . ? C52 C53 C54 119.8(7) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C53 C54 C40 119.1(7) . . ? C53 C54 H54 120.5 . . ? C40 C54 H54 120.5 . . ? O11 C55 C58 104.6(9) . . ? O11 C55 H55A 110.8 . . ? C58 C55 H55A 110.8 . . ? O11 C55 H55B 110.8 . . ? C58 C55 H55B 110.8 . . ? H55A C55 H55B 108.9 . . ? O11 C56 C57 102.1(9) . . ? O11 C56 H56A 111.3 . . ? C57 C56 H56A 111.3 . . ? O11 C56 H56B 111.3 . . ? C57 C56 H56B 111.3 . . ? H56A C56 H56B 109.2 . . ? C56 C57 C58 101.3(8) . . ? C56 C57 H57A 111.5 . . ? C58 C57 H57A 111.5 . . ? C56 C57 H57B 111.5 . . ? C58 C57 H57B 111.5 . . ? H57A C57 H57B 109.3 . . ? C55 C58 C57 104.4(9) . . ? C55 C58 H58A 110.9 . . ? C57 C58 H58A 110.9 . . ? C55 C58 H58B 110.9 . . ? C57 C58 H58B 110.9 . . ? H58A C58 H58B 108.9 . . ? O15 C59 C60 109(2) . . ? O15 C59 H59A 109.9 . . ? C60 C59 H59A 109.9 . . ? O15 C59 H59B 109.9 . . ? C60 C59 H59B 109.9 . . ? H59A C59 H59B 108.3 . . ? C59 C60 C65 104(2) . . ? C59 C60 H60A 111.1 . . ? C65 C60 H60A 111.1 . . ? C59 C60 H60B 111.1 . . ? C65 C60 H60B 111.1 . . ? H60A C60 H60B 109.0 . . ? C64 C61 C63 119(2) . . ? C64 C61 H61A 107.6 . . ? C63 C61 H61A 107.6 . . ? C64 C61 H61B 107.6 . . ? C63 C61 H61B 107.6 . . ? H61A C61 H61B 107.0 . . ? O15 C62 C65 116(2) . . ? O15 C62 H62A 108.2 . . ? C65 C62 H62A 108.2 . . ? O15 C62 H62B 108.2 . . ? C65 C62 H62B 108.2 . . ? H62A C62 H62B 107.3 . . ? C61 C63 O13 98.9(17) . . ? C61 C63 H63A 112.0 . . ? O13 C63 H63A 112.0 . . ? C61 C63 H63B 112.0 . . ? O13 C63 H63B 112.0 . . ? H63A C63 H63B 109.7 . . ? C66 C64 C61 104(2) . . ? C66 C64 H64A 111.0 . . ? C61 C64 H64A 111.0 . . ? C66 C64 H64B 111.0 . . ? C61 C64 H64B 111.0 . . ? H64A C64 H64B 109.0 . . ? C62 C65 C60 100.2(18) . . ? C62 C65 H65A 111.7 . . ? C60 C65 H65A 111.7 . . ? C62 C65 H65B 111.7 . . ? C60 C65 H65B 111.7 . . ? H65A C65 H65B 109.5 . . ? C64 C66 O13 120(2) . . ? C64 C66 H66A 107.4 . . ? O13 C66 H66A 107.4 . . ? C64 C66 H66B 107.4 . . ? O13 C66 H66B 107.4 . . ? H66A C66 H66B 106.9 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.634 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.230 # Attachment 'Complex_Ni_18_CH2Cl2.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 664567' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H21 N3 Ni O3, C H2 Cl2, 2 (Cl)' _chemical_formula_sum 'C19 H23 Cl4 N3 Ni O3' _chemical_formula_weight 541.91 _chemical_absolute_configuration . 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' O O 0.0106 0.0060 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9430(4) _cell_length_b 11.3560(4) _cell_length_c 12.3210(5) _cell_angle_alpha 91.790(2) _cell_angle_beta 113.320(2) _cell_angle_gamma 118.250(2) _cell_volume 1192.48(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12347 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 1.287 _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 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15347 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0943 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6929 _reflns_number_gt 4133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0718P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6929 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1448 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _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 0.49743(4) 0.80661(4) 0.29379(3) 0.02659(12) Uani 1 1 d . . . Cl1 Cl 0.66402(9) 0.51473(9) 0.28686(7) 0.0459(2) Uani 1 1 d . . . Cl2 Cl 0.70760(8) 0.94663(8) 0.68916(6) 0.0393(2) Uani 1 1 d . . . Cl3 Cl 0.86890(15) 0.67786(15) -0.14704(16) 0.1222(6) Uani 1 1 d . . . Cl4 Cl 0.84862(17) 0.80503(16) 0.04391(10) 0.1049(5) Uani 1 1 d . . . O1 O 0.4839(2) 0.6470(2) 0.19795(16) 0.0371(5) Uani 1 1 d . . . HO1 H 0.5399 0.6131 0.2257 0.056 Uiso 1 1 calc . . . O2 O 0.57123(19) 0.7448(2) 0.45190(16) 0.0315(5) Uani 1 1 d . . . HO2 H 0.6183 0.8051 0.5186 0.047 Uiso 1 1 calc . . . O3 O 0.52951(19) 0.97720(19) 0.39058(16) 0.0295(4) Uani 1 1 d . . . HO3 H 0.4597 0.9957 0.3759 0.044 Uiso 1 1 calc . . . N1 N 0.4048(2) 0.8234(2) 0.11800(19) 0.0286(5) Uani 1 1 d . . . N2 N 0.2840(2) 0.6830(2) 0.2946(2) 0.0281(5) Uani 1 1 d . . . N3 N 0.7286(2) 0.9538(2) 0.34092(19) 0.0288(5) Uani 1 1 d . . . C1 C 0.4397(4) 0.6349(3) 0.0711(3) 0.0426(8) Uani 1 1 d . . . H1A H 0.3519 0.5391 0.0224 0.051 Uiso 1 1 calc . . . H1B H 0.5293 0.6544 0.0563 0.051 Uiso 1 1 calc . . . C2 C 0.3905(3) 0.7357(3) 0.0319(2) 0.0307(6) Uani 1 1 d . . . C3 C 0.3300(3) 0.7349(3) -0.0916(2) 0.0384(7) Uani 1 1 d . . . H3 H 0.3233 0.6735 -0.1509 0.046 Uiso 1 1 calc . . . C4 C 0.2803(4) 0.8252(4) -0.1253(3) 0.0462(9) Uani 1 1 d . . . H4 H 0.2369 0.8254 -0.2090 0.055 Uiso 1 1 calc . . . C5 C 0.2935(3) 0.9151(3) -0.0378(3) 0.0400(8) Uani 1 1 d . . . H5 H 0.2598 0.9779 -0.0598 0.048 Uiso 1 1 calc . . . C6 C 0.3572(3) 0.9115(3) 0.0832(2) 0.0329(7) Uani 1 1 d . . . H6 H 0.3677 0.9740 0.1440 0.039 Uiso 1 1 calc . . . C7 C 0.4436(3) 0.6211(3) 0.4512(3) 0.0361(7) Uani 1 1 d . . . H7A H 0.4631 0.6199 0.5367 0.043 Uiso 1 1 calc . . . H7B H 0.4366 0.5387 0.4130 0.043 Uiso 1 1 calc . . . C8 C 0.2907(3) 0.6141(3) 0.3809(2) 0.0296(6) Uani 1 1 d . . . C9 C 0.1651(3) 0.5395(3) 0.4040(3) 0.0357(7) Uani 1 1 d . . . H9 H 0.1738 0.4923 0.4663 0.043 Uiso 1 1 calc . . . C10 C 0.0270(3) 0.5343(3) 0.3352(3) 0.0397(7) Uani 1 1 d . . . H10 H -0.0613 0.4830 0.3488 0.048 Uiso 1 1 calc . . . C11 C 0.0200(3) 0.6054(3) 0.2464(3) 0.0400(8) Uani 1 1 d . . . H11 H -0.0734 0.6042 0.1983 0.048 Uiso 1 1 calc . . . C12 C 0.1492(3) 0.6779(3) 0.2280(3) 0.0348(7) Uani 1 1 d . . . H12 H 0.1431 0.7261 0.1663 0.042 Uiso 1 1 calc . . . C13 C 0.6785(3) 1.1028(3) 0.4389(2) 0.0314(6) Uani 1 1 d . . . H13A H 0.7218 1.1358 0.5287 0.038 Uiso 1 1 calc . . . H13B H 0.6670 1.1752 0.4014 0.038 Uiso 1 1 calc . . . C14 C 0.7880(3) 1.0788(3) 0.4123(2) 0.0286(6) Uani 1 1 d . . . C15 C 0.9456(3) 1.1833(3) 0.4593(3) 0.0356(7) Uani 1 1 d . . . H15 H 0.9872 1.2692 0.5133 0.043 Uiso 1 1 calc . . . C16 C 1.0398(3) 1.1595(4) 0.4259(3) 0.0415(8) Uani 1 1 d . . . H16 H 1.1466 1.2303 0.4546 0.050 Uiso 1 1 calc . . . C17 C 0.9783(3) 1.0324(4) 0.3506(3) 0.0409(8) Uani 1 1 d . . . H17 H 1.0412 1.0146 0.3258 0.049 Uiso 1 1 calc . . . C18 C 0.8236(3) 0.9317(3) 0.3122(3) 0.0354(7) Uani 1 1 d . . . H18 H 0.7824 0.8427 0.2633 0.042 Uiso 1 1 calc . . . C19 C 0.7754(4) 0.7497(4) -0.1122(3) 0.0656(11) Uani 1 1 d . . . H19A H 0.7894 0.8294 -0.1477 0.079 Uiso 1 1 calc . . . H19B H 0.6616 0.6797 -0.1497 0.079 Uiso 1 1 calc . . . 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 0.02611(19) 0.0336(2) 0.02309(19) 0.00708(15) 0.01117(14) 0.01819(16) Cl1 0.0481(4) 0.0589(5) 0.0415(4) 0.0107(4) 0.0168(4) 0.0394(4) Cl2 0.0375(4) 0.0576(5) 0.0307(4) 0.0073(3) 0.0131(3) 0.0332(4) Cl3 0.0938(9) 0.0916(10) 0.1586(14) -0.0333(10) 0.0789(9) 0.0212(8) Cl4 0.1577(13) 0.1297(12) 0.0523(6) 0.0183(7) 0.0417(7) 0.0998(11) O1 0.0488(12) 0.0439(12) 0.0286(11) 0.0088(9) 0.0150(9) 0.0340(10) O2 0.0298(10) 0.0430(12) 0.0256(10) 0.0107(9) 0.0120(8) 0.0227(9) O3 0.0260(9) 0.0327(11) 0.0327(10) 0.0044(8) 0.0144(8) 0.0173(8) N1 0.0266(11) 0.0318(13) 0.0255(12) 0.0069(10) 0.0108(9) 0.0151(10) N2 0.0277(11) 0.0297(13) 0.0284(12) 0.0074(10) 0.0113(9) 0.0176(10) N3 0.0258(11) 0.0399(14) 0.0244(11) 0.0083(10) 0.0128(9) 0.0191(10) C1 0.0553(19) 0.0453(19) 0.0296(16) 0.0043(14) 0.0169(14) 0.0311(16) C2 0.0292(13) 0.0336(16) 0.0245(14) 0.0049(12) 0.0127(11) 0.0133(12) C3 0.0421(16) 0.0456(19) 0.0228(14) 0.0035(13) 0.0142(12) 0.0209(15) C4 0.0486(18) 0.053(2) 0.0245(15) 0.0128(14) 0.0120(14) 0.0217(16) C5 0.0419(16) 0.0434(19) 0.0332(16) 0.0162(14) 0.0147(13) 0.0233(15) C6 0.0354(15) 0.0363(16) 0.0309(15) 0.0084(13) 0.0169(12) 0.0207(13) C7 0.0431(16) 0.0410(18) 0.0359(16) 0.0166(14) 0.0212(13) 0.0278(14) C8 0.0339(14) 0.0263(14) 0.0300(14) 0.0051(12) 0.0158(12) 0.0164(12) C9 0.0388(15) 0.0341(16) 0.0359(16) 0.0126(13) 0.0210(13) 0.0173(13) C10 0.0345(15) 0.0339(17) 0.0439(18) 0.0075(14) 0.0206(14) 0.0118(13) C11 0.0277(14) 0.0437(19) 0.0428(17) 0.0090(15) 0.0135(13) 0.0173(14) C12 0.0286(14) 0.0385(17) 0.0325(15) 0.0093(13) 0.0103(12) 0.0175(13) C13 0.0287(13) 0.0293(15) 0.0348(15) 0.0037(12) 0.0159(12) 0.0137(12) C14 0.0288(13) 0.0375(16) 0.0231(13) 0.0109(12) 0.0138(11) 0.0186(12) C15 0.0315(14) 0.0365(17) 0.0358(16) 0.0126(13) 0.0173(12) 0.0145(13) C16 0.0282(15) 0.052(2) 0.0418(18) 0.0215(16) 0.0181(13) 0.0177(14) C17 0.0337(15) 0.062(2) 0.0436(18) 0.0219(16) 0.0251(14) 0.0303(15) C18 0.0340(15) 0.0490(19) 0.0320(15) 0.0122(14) 0.0184(12) 0.0257(14) C19 0.069(2) 0.072(3) 0.051(2) 0.022(2) 0.0263(19) 0.036(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.055(2) . ? Ni1 N3 2.075(2) . ? Ni1 N2 2.083(2) . ? Cl3 C19 1.736(5) . ? Cl4 C19 1.722(4) . ? O1 C1 1.421(3) . ? O1 HO1 0.8400 . ? O2 C7 1.434(3) . ? O2 HO2 0.8400 . ? O3 C13 1.423(3) . ? O3 HO3 0.8400 . ? N1 C2 1.340(4) . ? N1 C6 1.341(4) . ? N2 C8 1.339(3) . ? N2 C12 1.346(3) . ? N3 C18 1.342(4) . ? N3 C14 1.344(4) . ? C1 C2 1.499(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.397(4) . ? C3 C4 1.377(5) . ? C3 H3 0.9500 . ? C4 C5 1.377(5) . ? C4 H4 0.9500 . ? C5 C6 1.384(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.510(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.381(4) . ? C9 C10 1.381(4) . ? C9 H9 0.9500 . ? C10 C11 1.379(4) . ? C10 H10 0.9500 . ? C11 C12 1.376(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.495(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.395(4) . ? C15 C16 1.377(4) . ? C15 H15 0.9500 . ? C16 C17 1.378(5) . ? C16 H16 0.9500 . ? C17 C18 1.377(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? 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 Ni1 N3 95.63(8) . . ? N1 Ni1 N2 96.41(8) . . ? N3 Ni1 N2 164.65(9) . . ? C1 O1 HO1 109.5 . . ? C7 O2 HO2 109.5 . . ? C13 O3 HO3 109.5 . . ? C2 N1 C6 118.4(2) . . ? C2 N1 Ni1 115.39(19) . . ? C6 N1 Ni1 126.2(2) . . ? C8 N2 C12 118.2(2) . . ? C8 N2 Ni1 114.39(17) . . ? C12 N2 Ni1 126.97(18) . . ? C18 N3 C14 118.5(2) . . ? C18 N3 Ni1 125.6(2) . . ? C14 N3 Ni1 115.77(18) . . ? O1 C1 C2 109.5(3) . . ? O1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? O1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? N1 C2 C3 122.1(3) . . ? N1 C2 C1 118.1(2) . . ? C3 C2 C1 119.8(3) . . ? C4 C3 C2 118.4(3) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 118.3(3) . . ? C4 C5 H5 120.9 . . ? C6 C5 H5 120.9 . . ? N1 C6 C5 122.8(3) . . ? N1 C6 H6 118.6 . . ? C5 C6 H6 118.6 . . ? O2 C7 C8 110.8(2) . . ? O2 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? N2 C8 C9 122.4(3) . . ? N2 C8 C7 116.0(2) . . ? C9 C8 C7 121.6(2) . . ? C10 C9 C8 119.1(3) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C11 C10 C9 118.6(3) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C12 C11 C10 119.5(3) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? N2 C12 C11 122.2(3) . . ? N2 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? O3 C13 C14 109.8(2) . . ? O3 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? O3 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? N3 C14 C15 121.6(3) . . ? N3 C14 C13 117.5(2) . . ? C15 C14 C13 120.8(3) . . ? C16 C15 C14 118.8(3) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 119.6(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 118.5(3) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? N3 C18 C17 122.8(3) . . ? N3 C18 H18 118.6 . . ? C17 C18 H18 118.6 . . ? Cl4 C19 Cl3 111.6(2) . . ? Cl4 C19 H19A 109.3 . . ? Cl3 C19 H19A 109.3 . . ? Cl4 C19 H19B 109.3 . . ? Cl3 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ni1 N1 C2 91.63(19) . . . . ? N2 Ni1 N1 C2 -97.92(18) . . . . ? N3 Ni1 N1 C6 -89.1(2) . . . . ? N2 Ni1 N1 C6 81.3(2) . . . . ? N1 Ni1 N2 C8 160.7(2) . . . . ? N3 Ni1 N2 C8 -57.9(4) . . . . ? N1 Ni1 N2 C12 -26.9(3) . . . . ? N3 Ni1 N2 C12 114.5(4) . . . . ? N1 Ni1 N3 C18 -81.2(2) . . . . ? N2 Ni1 N3 C18 137.3(3) . . . . ? N1 Ni1 N3 C14 102.87(19) . . . . ? N2 Ni1 N3 C14 -38.6(4) . . . . ? C6 N1 C2 C3 0.9(4) . . . . ? Ni1 N1 C2 C3 -179.8(2) . . . . ? C6 N1 C2 C1 -178.3(2) . . . . ? Ni1 N1 C2 C1 1.0(3) . . . . ? O1 C1 C2 N1 4.3(4) . . . . ? O1 C1 C2 C3 -174.9(2) . . . . ? N1 C2 C3 C4 -1.6(4) . . . . ? C1 C2 C3 C4 177.5(3) . . . . ? C2 C3 C4 C5 1.2(5) . . . . ? C3 C4 C5 C6 -0.1(5) . . . . ? C2 N1 C6 C5 0.3(4) . . . . ? Ni1 N1 C6 C5 -178.9(2) . . . . ? C4 C5 C6 N1 -0.7(4) . . . . ? C12 N2 C8 C9 -0.5(4) . . . . ? Ni1 N2 C8 C9 172.7(2) . . . . ? C12 N2 C8 C7 178.9(3) . . . . ? Ni1 N2 C8 C7 -7.9(3) . . . . ? O2 C7 C8 N2 25.7(4) . . . . ? O2 C7 C8 C9 -155.0(3) . . . . ? N2 C8 C9 C10 0.6(5) . . . . ? C7 C8 C9 C10 -178.7(3) . . . . ? C8 C9 C10 C11 -0.6(5) . . . . ? C9 C10 C11 C12 0.6(5) . . . . ? C8 N2 C12 C11 0.4(4) . . . . ? Ni1 N2 C12 C11 -171.8(2) . . . . ? C10 C11 C12 N2 -0.4(5) . . . . ? C18 N3 C14 C15 -1.8(4) . . . . ? Ni1 N3 C14 C15 174.43(19) . . . . ? C18 N3 C14 C13 177.6(2) . . . . ? Ni1 N3 C14 C13 -6.1(3) . . . . ? O3 C13 C14 N3 6.0(3) . . . . ? O3 C13 C14 C15 -174.5(2) . . . . ? N3 C14 C15 C16 3.6(4) . . . . ? C13 C14 C15 C16 -175.9(3) . . . . ? C14 C15 C16 C17 -2.1(4) . . . . ? C15 C16 C17 C18 -0.9(4) . . . . ? C14 N3 C18 C17 -1.4(4) . . . . ? Ni1 N3 C18 C17 -177.2(2) . . . . ? C16 C17 C18 N3 2.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.706 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.123