Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Enbo Wang' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Changchun 130024 CHINA ; _publ_contact_author_email WANGENBO@PUBLIC.CC.JL.CN _publ_section_title ; Helix-Pillared 3D Mesomeric Networks: Syntheses, Structures, and Magnetisms ; loop_ _publ_author_name 'Enbo Wang.' 'Rodolphe Clerac' 'Yangguang Li.' 'Chao Qin.' 'Zhong-Min Su.' ; Xin-long Wang ; 'Lin Xu.' data_wbl14a _database_code_depnum_ccdc_archive 'CCDC 246455' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H12 N3 Ni O4.50' _chemical_formula_weight 389.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.342(4) _cell_length_b 11.443(2) _cell_length_c 13.936(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.82(3) _cell_angle_gamma 90.00 _cell_volume 3055.9(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 1.303 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6730 _exptl_absorpt_correction_T_max 0.7450 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 6613 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3487 _reflns_number_gt 2622 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+42.8860P] 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 3487 _refine_ls_number_parameters 248 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1452 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.077 _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 0.5000 0.62389(8) 0.2500 0.0169(2) Uani 1 2 d S . . Ni2 Ni 0.2500 0.2500 0.5000 0.0130(2) Uani 1 2 d S . . C1 C 0.3234(2) 0.4577(4) 0.4169(4) 0.0182(10) Uani 1 1 d . . . H1A H 0.3372 0.4709 0.4825 0.022 Uiso 1 1 calc R . . C2 C 0.3477(2) 0.5351(4) 0.3503(4) 0.0166(9) Uani 1 1 d D . . C3 C 0.3227(2) 0.5202(4) 0.2525(4) 0.0166(9) Uani 1 1 d . . . C4 C 0.2779(3) 0.4266(5) 0.2271(4) 0.0269(12) Uani 1 1 d . . . H4A H 0.2598 0.4148 0.1625 0.032 Uiso 1 1 calc R . . C5 C 0.2601(3) 0.3515(5) 0.2971(4) 0.0258(12) Uani 1 1 d . . . H5A H 0.2320 0.2876 0.2779 0.031 Uiso 1 1 calc R . . C6 C 0.3401(2) 0.6021(4) 0.1739(3) 0.0148(9) Uani 1 1 d . . . C7 C 0.3965(3) 0.6303(4) 0.3953(4) 0.0206(10) Uani 1 1 d D . . C8 C 0.0975(2) 0.5232(4) 0.5074(4) 0.0200(10) Uani 1 1 d . . . H8A H 0.1002 0.6040 0.5139 0.024 Uiso 1 1 calc R . . C9 C 0.1574(2) 0.4588(5) 0.5044(4) 0.0209(10) Uani 1 1 d . . . H9A H 0.1997 0.4980 0.5066 0.025 Uiso 1 1 calc R . . C10 C 0.0956(2) 0.2878(4) 0.4942(4) 0.0181(10) Uani 1 1 d . . . H10A H 0.0946 0.2066 0.4914 0.022 Uiso 1 1 calc R . . C11 C 0.0333(3) 0.3462(4) 0.4938(4) 0.0200(10) Uani 1 1 d . . . H11A H -0.0084 0.3049 0.4889 0.024 Uiso 1 1 calc R . . C12 C 0.0332(2) 0.4675(4) 0.5007(4) 0.0180(10) Uani 1 1 d . . . C13 C 0.4408(3) 0.8777(5) 0.2493(4) 0.0267(12) Uani 1 1 d . . . H13A H 0.3991 0.8371 0.2489 0.032 Uiso 1 1 calc R . . C14 C 0.4389(3) 0.9994(5) 0.2490(5) 0.0318(13) Uani 1 1 d . . . H14A H 0.3967 1.0385 0.2481 0.038 Uiso 1 1 calc R . . C15 C 0.5000 1.0614(6) 0.2500 0.0244(16) Uani 1 2 d S . . C16 C 0.5000 1.1930(6) 0.2500 0.0232(16) Uani 1 2 d S . . C17 C 0.4557(3) 1.2565(5) 0.1836(4) 0.0292(12) Uani 1 1 d . . . H17A H 0.4235 1.2180 0.1389 0.035 Uiso 1 1 calc R . . C18 C 0.4590(3) 1.3766(5) 0.1830(4) 0.0282(12) Uani 1 1 d . . . H18A H 0.4316 1.4170 0.1338 0.034 Uiso 1 1 calc R . . N1 N 0.5000 0.8166(5) 0.2500 0.0220(13) Uani 1 2 d S . . N2 N 0.5000 1.4377(6) 0.2500 0.0241(14) Uani 1 2 d S . . N3 N 0.1571(2) 0.3409(3) 0.4983(3) 0.0169(8) Uani 1 1 d . . . N4 N 0.2817(2) 0.3667(4) 0.3915(3) 0.0176(8) Uani 1 1 d . . . O1 O 0.3738(2) 0.6928(4) 0.4565(4) 0.0494(14) Uani 1 1 d . . . O2 O 0.45763(18) 0.6344(3) 0.3749(3) 0.0259(8) Uani 1 1 d . . . O3 O 0.28923(16) 0.6307(3) 0.1122(3) 0.0195(7) Uani 1 1 d . . . O4 O 0.40140(18) 0.6340(3) 0.1725(3) 0.0246(8) Uani 1 1 d . . . O1W O 0.2284(9) 0.7113(18) 0.4467(14) 0.063(5) Uani 0.32 1 d PU . . O1AW O 0.2446(19) 0.703(3) 0.521(3) 0.064(9) Uani 0.18 1 d PU . . 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 0.0141(4) 0.0135(4) 0.0226(5) 0.000 0.0006(3) 0.000 Ni2 0.0107(4) 0.0101(4) 0.0183(4) 0.0005(3) 0.0021(3) 0.0007(3) C1 0.019(2) 0.017(2) 0.018(2) 0.0005(19) 0.0022(18) 0.0002(19) C2 0.018(2) 0.011(2) 0.022(2) 0.0013(19) 0.0057(18) -0.0013(18) C3 0.014(2) 0.014(2) 0.022(2) 0.0005(19) 0.0012(17) 0.0008(17) C4 0.035(3) 0.021(3) 0.023(3) 0.004(2) -0.003(2) -0.011(2) C5 0.026(3) 0.020(3) 0.030(3) 0.001(2) 0.000(2) -0.014(2) C6 0.019(2) 0.009(2) 0.016(2) -0.0028(17) 0.0040(17) -0.0021(17) C7 0.024(2) 0.016(2) 0.022(3) -0.002(2) 0.0035(19) -0.007(2) C8 0.018(2) 0.012(2) 0.031(3) -0.002(2) 0.0035(19) 0.0022(18) C9 0.012(2) 0.021(3) 0.029(3) 0.002(2) 0.0005(19) -0.0006(19) C10 0.017(2) 0.012(2) 0.025(3) -0.0089(19) 0.0025(18) 0.0014(18) C11 0.014(2) 0.018(3) 0.027(3) -0.004(2) 0.0023(19) 0.0009(18) C12 0.014(2) 0.016(2) 0.024(3) -0.0044(19) 0.0010(18) 0.0022(18) C13 0.017(2) 0.022(3) 0.042(3) 0.000(2) 0.007(2) 0.000(2) C14 0.029(3) 0.021(3) 0.046(4) -0.001(3) 0.006(2) 0.004(2) C15 0.033(4) 0.014(4) 0.026(4) 0.000 0.003(3) 0.000 C16 0.026(4) 0.014(4) 0.031(4) 0.000 0.007(3) 0.000 C17 0.037(3) 0.017(3) 0.031(3) -0.003(2) -0.004(2) 0.002(2) C18 0.029(3) 0.023(3) 0.031(3) -0.003(2) -0.003(2) 0.005(2) N1 0.025(3) 0.012(3) 0.029(4) 0.000 0.003(3) 0.000 N2 0.023(3) 0.023(3) 0.027(4) 0.000 0.005(3) 0.000 N3 0.0142(19) 0.014(2) 0.022(2) -0.0006(16) -0.0001(15) 0.0043(15) N4 0.0179(19) 0.015(2) 0.020(2) -0.0012(17) 0.0037(16) -0.0026(16) O1 0.039(3) 0.045(3) 0.069(3) -0.039(3) 0.026(2) -0.017(2) O2 0.0203(18) 0.030(2) 0.029(2) -0.0057(17) 0.0064(15) -0.0107(16) O3 0.0148(16) 0.0162(17) 0.0259(19) 0.0029(15) -0.0026(13) 0.0025(13) O4 0.0161(17) 0.0264(19) 0.030(2) 0.0073(16) -0.0012(14) -0.0022(15) O1W 0.052(8) 0.071(9) 0.067(9) -0.015(7) 0.015(7) 0.001(7) O1AW 0.065(12) 0.057(12) 0.072(12) 0.009(9) 0.021(9) 0.002(9) _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 2.026(4) 2_655 ? Ni1 O2 2.026(4) . ? Ni1 O4 2.063(3) . ? Ni1 O4 2.063(3) 2_655 ? Ni1 N2 2.131(7) 1_545 ? Ni1 N1 2.205(6) . ? Ni2 N3 2.073(4) . ? Ni2 N3 2.073(4) 7_556 ? Ni2 O3 2.136(3) 4_545 ? Ni2 O3 2.136(3) 6_566 ? Ni2 N4 2.167(4) . ? Ni2 N4 2.167(4) 7_556 ? C1 N4 1.335(6) . ? C1 C2 1.409(7) . ? C1 H1A 0.9300 . ? C2 C3 1.393(7) . ? C2 C7 1.520(6) . ? C3 C4 1.393(7) . ? C3 C6 1.514(7) . ? C4 C5 1.379(7) . ? C4 H4A 0.9300 . ? C5 N4 1.336(7) . ? C5 H5A 0.9300 . ? C6 O4 1.243(6) . ? C6 O3 1.258(6) . ? C7 O1 1.238(6) . ? C7 O2 1.254(6) . ? C8 C9 1.378(7) . ? C8 C12 1.390(7) . ? C8 H8A 0.9300 . ? C9 N3 1.352(6) . ? C9 H9A 0.9300 . ? C10 N3 1.330(6) . ? C10 C11 1.378(7) . ? C10 H10A 0.9300 . ? C11 C12 1.392(7) . ? C11 H11A 0.9300 . ? C12 C12 1.482(9) 5_566 ? C13 N1 1.341(6) . ? C13 C14 1.393(8) . ? C13 H13A 0.9300 . ? C14 C15 1.377(7) . ? C14 H14A 0.9300 . ? C15 C14 1.377(7) 2_655 ? C15 C16 1.506(10) . ? C16 C17 1.379(7) . ? C16 C17 1.379(7) 2_655 ? C17 C18 1.375(8) . ? C17 H17A 0.9300 . ? C18 N2 1.337(6) . ? C18 H18A 0.9300 . ? N1 C13 1.341(6) 2_655 ? N2 C18 1.337(6) 2_655 ? N2 Ni1 2.131(7) 1_565 ? O3 Ni2 2.136(3) 4 ? O1W O1AW 1.04(4) . ? O1W O1AW 1.17(4) 7_566 ? O1AW O1W 1.17(4) 7_566 ? O1AW O1AW 1.24(7) 7_566 ? 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 O2 173.2(2) 2_655 . ? O2 Ni1 O4 90.01(15) 2_655 . ? O2 Ni1 O4 89.61(15) . . ? O2 Ni1 O4 89.61(15) 2_655 2_655 ? O2 Ni1 O4 90.01(15) . 2_655 ? O4 Ni1 O4 173.6(2) . 2_655 ? O2 Ni1 N2 93.41(11) 2_655 1_545 ? O2 Ni1 N2 93.41(11) . 1_545 ? O4 Ni1 N2 93.22(11) . 1_545 ? O4 Ni1 N2 93.22(11) 2_655 1_545 ? O2 Ni1 N1 86.59(11) 2_655 . ? O2 Ni1 N1 86.59(11) . . ? O4 Ni1 N1 86.78(11) . . ? O4 Ni1 N1 86.78(11) 2_655 . ? N2 Ni1 N1 180.000(1) 1_545 . ? N3 Ni2 N3 180.0(2) . 7_556 ? N3 Ni2 O3 95.23(14) . 4_545 ? N3 Ni2 O3 84.77(14) 7_556 4_545 ? N3 Ni2 O3 84.77(14) . 6_566 ? N3 Ni2 O3 95.23(14) 7_556 6_566 ? O3 Ni2 O3 180.00(14) 4_545 6_566 ? N3 Ni2 N4 90.55(16) . . ? N3 Ni2 N4 89.45(16) 7_556 . ? O3 Ni2 N4 89.39(14) 4_545 . ? O3 Ni2 N4 90.61(14) 6_566 . ? N3 Ni2 N4 89.45(16) . 7_556 ? N3 Ni2 N4 90.55(16) 7_556 7_556 ? O3 Ni2 N4 90.61(14) 4_545 7_556 ? O3 Ni2 N4 89.39(14) 6_566 7_556 ? N4 Ni2 N4 180.0 . 7_556 ? N4 C1 C2 124.0(5) . . ? N4 C1 H1A 118.0 . . ? C2 C1 H1A 118.0 . . ? C3 C2 C1 117.7(4) . . ? C3 C2 C7 127.2(4) . . ? C1 C2 C7 115.0(4) . . ? C4 C3 C2 117.6(5) . . ? C4 C3 C6 118.9(4) . . ? C2 C3 C6 123.4(4) . . ? C5 C4 C3 120.3(5) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? N4 C5 C4 122.8(5) . . ? N4 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? O4 C6 O3 124.9(4) . . ? O4 C6 C3 119.9(4) . . ? O3 C6 C3 115.2(4) . . ? O1 C7 O2 124.6(5) . . ? O1 C7 C2 116.1(4) . . ? O2 C7 C2 119.0(4) . . ? C9 C8 C12 120.1(5) . . ? C9 C8 H8A 120.0 . . ? C12 C8 H8A 120.0 . . ? N3 C9 C8 122.6(5) . . ? N3 C9 H9A 118.7 . . ? C8 C9 H9A 118.7 . . ? N3 C10 C11 123.8(5) . . ? N3 C10 H10A 118.1 . . ? C11 C10 H10A 118.1 . . ? C10 C11 C12 119.5(5) . . ? C10 C11 H11A 120.2 . . ? C12 C11 H11A 120.2 . . ? C8 C12 C11 116.9(4) . . ? C8 C12 C12 122.5(6) . 5_566 ? C11 C12 C12 120.6(5) . 5_566 ? N1 C13 C14 122.9(5) . . ? N1 C13 H13A 118.5 . . ? C14 C13 H13A 118.5 . . ? C15 C14 C13 119.6(5) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C14 C15 C14 117.9(7) . 2_655 ? C14 C15 C16 121.0(4) . . ? C14 C15 C16 121.0(4) 2_655 . ? C17 C16 C17 116.4(7) . 2_655 ? C17 C16 C15 121.8(3) . . ? C17 C16 C15 121.8(3) 2_655 . ? C18 C17 C16 120.4(5) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? N2 C18 C17 122.8(5) . . ? N2 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? C13 N1 C13 117.1(7) 2_655 . ? C13 N1 Ni1 121.5(3) 2_655 . ? C13 N1 Ni1 121.5(3) . . ? C18 N2 C18 117.0(7) . 2_655 ? C18 N2 Ni1 121.5(3) . 1_565 ? C18 N2 Ni1 121.5(3) 2_655 1_565 ? C10 N3 C9 117.0(4) . . ? C10 N3 Ni2 122.7(3) . . ? C9 N3 Ni2 120.3(3) . . ? C1 N4 C5 117.3(4) . . ? C1 N4 Ni2 120.9(3) . . ? C5 N4 Ni2 121.8(3) . . ? C7 O2 Ni1 134.1(3) . . ? C6 O3 Ni2 146.4(3) . 4 ? C6 O4 Ni1 142.3(3) . . ? O1AW O1W O1AW 68(3) . 7_566 ? O1W O1AW O1W 112(3) . 7_566 ? O1W O1AW O1AW 61(3) . 7_566 ? O1W O1AW O1AW 51(3) 7_566 7_566 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.804 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.129 data_wbl13b _database_code_depnum_ccdc_archive 'CCDC 246456' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H35 N4 Ni3 O18.50' _chemical_formula_weight 1019.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 22.635(5) _cell_length_b 17.286(4) _cell_length_c 10.058(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3935.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2092 _exptl_absorpt_coefficient_mu 1.509 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6438 _exptl_absorpt_correction_T_max 0.7324 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 8730 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8730 _reflns_number_gt 7583 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_number_reflns 8730 _refine_ls_number_parameters 599 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 1.018 _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 0.091362(15) 0.75657(2) -0.56031(5) 0.01421(8) Uani 1 1 d . . . Ni2 Ni 0.131861(15) 0.75623(2) -0.05405(5) 0.01438(8) Uani 1 1 d . . . Ni3 Ni -0.198709(17) 0.50518(2) 0.18582(7) 0.02216(10) Uani 1 1 d . . . C1 C 0.06073(14) 0.60758(17) 0.1028(3) 0.0162(6) Uani 1 1 d . . . C2 C 0.00280(14) 0.59512(18) 0.1452(3) 0.0168(6) Uani 1 1 d . . . H2A H -0.0115 0.6222 0.2184 0.020 Uiso 1 1 calc R . . C3 C -0.03382(14) 0.54325(19) 0.0803(3) 0.0183(6) Uani 1 1 d . . . C4 C -0.01190(16) 0.4999(2) -0.0245(3) 0.0246(7) Uani 1 1 d . . . H4A H -0.0357 0.4637 -0.0670 0.030 Uiso 1 1 calc R . . C5 C 0.04595(15) 0.51124(18) -0.0651(4) 0.0248(7) Uani 1 1 d . . . H5A H 0.0613 0.4804 -0.1325 0.030 Uiso 1 1 calc R . . C6 C 0.08171(14) 0.56771(19) -0.0074(3) 0.0179(6) Uani 1 1 d . . . C7 C 0.09586(12) 0.66608(16) 0.1859(3) 0.0134(5) Uani 1 1 d . . . C8 C 0.13758(14) 0.58145(19) -0.0886(3) 0.0199(7) Uani 1 1 d . . . C9 C -0.09697(14) 0.53305(19) 0.1218(3) 0.0188(6) Uani 1 1 d . . . C10 C 0.07127(14) 0.93203(18) -0.1025(3) 0.0176(6) Uani 1 1 d . . . C11 C 0.04983(14) 0.89552(17) -0.2164(3) 0.0158(6) Uani 1 1 d . . . C12 C -0.00970(14) 0.90342(18) -0.2488(3) 0.0174(6) Uani 1 1 d . . . H12A H -0.0245 0.8783 -0.3235 0.021 Uiso 1 1 calc R . . C13 C -0.04730(14) 0.94834(19) -0.1713(3) 0.0193(6) Uani 1 1 d . . . C14 C -0.02447(15) 0.98718(19) -0.0606(4) 0.0254(7) Uani 1 1 d . . . H14A H -0.0490 1.0186 -0.0097 0.030 Uiso 1 1 calc R . . C15 C 0.03471(17) 0.9789(2) -0.0266(3) 0.0255(8) Uani 1 1 d . . . H15A H 0.0498 1.0047 0.0471 0.031 Uiso 1 1 calc R . . C16 C -0.11227(15) 0.9559(2) -0.2022(4) 0.0242(7) Uani 1 1 d . . . C17 C 0.13367(13) 0.92288(17) -0.0531(4) 0.0206(6) Uani 1 1 d . . . C18 C 0.08889(12) 0.84384(17) -0.2986(3) 0.0149(6) Uani 1 1 d . . . C19 C 0.21600(15) 0.8135(2) -0.5257(4) 0.0282(8) Uani 1 1 d . . . H19A H 0.1965 0.8592 -0.5047 0.034 Uiso 1 1 calc R . . C20 C 0.21268(15) 0.6860(2) -0.5820(4) 0.0281(8) Uani 1 1 d . . . H20A H 0.1908 0.6416 -0.5998 0.034 Uiso 1 1 calc R . . C21 C 0.27670(16) 0.8135(2) -0.5248(4) 0.0297(9) Uani 1 1 d . . . H21A H 0.2972 0.8585 -0.5038 0.036 Uiso 1 1 calc R . . C22 C 0.30752(12) 0.74609(19) -0.5553(5) 0.0208(6) Uani 1 1 d . . . C23 C 0.27318(16) 0.6808(2) -0.5847(4) 0.0313(9) Uani 1 1 d . . . H23A H 0.2913 0.6341 -0.6060 0.038 Uiso 1 1 calc R . . C24 C 0.46717(16) 0.8044(2) -0.5251(4) 0.0328(9) Uani 1 1 d . . . H24A H 0.4882 0.8480 -0.4985 0.039 Uiso 1 1 calc R . . C25 C 0.40653(16) 0.8076(2) -0.5218(5) 0.0356(10) Uani 1 1 d . . . H25A H 0.3877 0.8528 -0.4951 0.043 Uiso 1 1 calc R . . C26 C 0.37332(13) 0.74343(18) -0.5583(7) 0.0203(6) Uani 1 1 d . . . C27 C 0.46575(15) 0.6808(2) -0.5977(4) 0.0286(8) Uani 1 1 d . . . H27A H 0.4856 0.6365 -0.6247 0.034 Uiso 1 1 calc R . . C28 C 0.25560(19) 0.7725(3) -0.1622(4) 0.0380(11) Uani 1 1 d . . . H28A H 0.2354 0.7816 -0.2411 0.046 Uiso 1 1 calc R . . C29 C 0.31658(19) 0.7727(3) -0.1658(4) 0.0457(13) Uani 1 1 d . . . H29A H 0.3361 0.7824 -0.2454 0.055 Uiso 1 1 calc R . . C30 C 0.2549(2) 0.7512(3) 0.0583(5) 0.0441(14) Uani 1 1 d . . . H30A H 0.2341 0.7445 0.1371 0.053 Uiso 1 1 calc R . . C31 C 0.50588(15) 0.7109(2) 0.0390(3) 0.0223(7) Uani 1 1 d . . . H31A H 0.5256 0.6821 0.1032 0.027 Uiso 1 1 calc R . . C32 C 0.50801(14) 0.7915(2) -0.1413(3) 0.0204(6) Uani 1 1 d . . . H32A H 0.5294 0.8191 -0.2046 0.024 Uiso 1 1 calc R . . C33 C 0.44719(15) 0.7965(2) -0.1436(3) 0.0228(7) Uani 1 1 d . . . H33A H 0.4285 0.8269 -0.2073 0.027 Uiso 1 1 calc R . . C34 C 0.41381(13) 0.75601(18) -0.0508(6) 0.0198(6) Uani 1 1 d . . . C35 C 0.34838(13) 0.75870(18) -0.0521(6) 0.0211(6) Uani 1 1 d . . . C36 C 0.3161(2) 0.7510(3) 0.0632(5) 0.0419(13) Uani 1 1 d . . . H36A H 0.3353 0.7458 0.1444 0.050 Uiso 1 1 calc R . . C37 C 0.44452(16) 0.7126(2) 0.0417(3) 0.0239(7) Uani 1 1 d . . . H37A H 0.4241 0.6845 0.1058 0.029 Uiso 1 1 calc R . . C38 C 0.40471(15) 0.6789(2) -0.5947(4) 0.0305(9) Uani 1 1 d . . . H38A H 0.3848 0.6337 -0.6175 0.037 Uiso 1 1 calc R . . N1 N 0.18350(10) 0.75118(16) -0.5554(5) 0.0196(5) Uani 1 1 d . . . N2 N 0.49769(11) 0.74226(14) -0.5642(4) 0.0192(5) Uani 1 1 d . . . N3 N 0.22450(10) 0.76042(14) -0.0545(4) 0.0186(5) Uani 1 1 d . . . N4 N 0.53791(10) 0.74902(15) -0.0523(5) 0.0183(5) Uani 1 1 d . . . O1 O 0.14667(10) 0.64776(13) -0.1349(2) 0.0212(5) Uani 1 1 d . . . O2 O -0.12456(10) 0.58685(13) 0.1771(3) 0.0251(5) Uani 1 1 d . . . O3 O -0.12064(11) 0.46743(14) 0.1032(3) 0.0264(5) Uani 1 1 d . . . O4 O 0.17101(12) 0.96948(18) -0.0938(3) 0.0404(7) Uani 1 1 d . . . O5 O 0.14231(11) 0.86920(14) 0.0315(2) 0.0222(5) Uani 1 1 d . . . O6 O -0.13444(11) 0.91041(18) -0.2846(3) 0.0402(8) Uani 1 1 d . . . O7 O -0.13996(11) 1.00921(16) -0.1415(3) 0.0324(6) Uani 1 1 d . . . O8 O 0.12690(10) 0.80123(13) -0.2424(2) 0.0171(4) Uani 1 1 d . . . O9 O 0.08106(11) 0.84585(14) -0.4230(2) 0.0192(5) Uani 1 1 d . . . O10 O 0.08425(11) 0.66502(14) 0.3086(2) 0.0195(5) Uani 1 1 d . . . O11 O 0.08982(11) 0.67795(15) -0.4057(2) 0.0202(5) Uani 1 1 d D . . H3 H 0.0939 0.6286 -0.3909 0.030 Uiso 1 1 d RD . . H4 H 0.1115 0.6943 -0.3505 0.030 Uiso 1 1 d RD . . O12 O 0.09385(11) 0.84495(15) -0.6997(2) 0.0214(5) Uani 1 1 d D . . H1 H 0.1123 0.8374 -0.7905 0.032 Uiso 1 1 d RD . . H2 H 0.1048 0.8820 -0.6688 0.032 Uiso 1 1 d RD . . O13 O 0.16753(11) 0.52215(15) -0.1199(3) 0.0271(6) Uani 1 1 d . . . O14 O -0.24703(10) 0.40614(14) 0.1913(3) 0.0295(5) Uani 1 1 d D . . H5 H -0.2391 0.3861 0.2521 0.044 Uiso 1 1 d RD . . H6 H -0.2812 0.4124 0.2044 0.044 Uiso 1 1 d RD . . O15 O -0.26775(11) 0.57104(16) 0.2425(3) 0.0342(6) Uani 1 1 d D . . H7 H -0.2929 0.5998 0.1670 0.051 Uiso 1 1 d RD . . H8 H -0.2977 0.5416 0.2859 0.051 Uiso 1 1 d RD . . O16 O -0.22072(13) 0.5351(2) -0.0028(3) 0.0504(9) Uani 1 1 d D . . H9 H -0.1929 0.5339 -0.0647 0.076 Uiso 1 1 d RD . . H10 H -0.2548 0.5188 -0.0171 0.076 Uiso 1 1 d RD . . O17 O 0.13181(10) 0.71208(14) 0.1329(2) 0.0200(5) Uani 1 1 d . . . O1W O 0.1581(4) 1.0451(4) -0.3486(7) 0.061(2) Uani 0.55 1 d PU . . O2W O 0.1907(11) 1.0172(13) -0.358(2) 0.063(6) Uani 0.20 1 d PU . . O3W O -0.1439(4) 0.5347(6) -0.2211(9) 0.068(3) Uani 0.43 1 d PU . . O4W O 0.2772(6) 0.9984(7) -0.3758(12) 0.066(3) Uani 0.32 1 d PU . . 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 0.00922(17) 0.01864(17) 0.01476(16) -0.00133(19) -0.0001(2) -0.00028(13) Ni2 0.00825(17) 0.02059(18) 0.01429(15) 0.00022(18) 0.0002(2) 0.00009(13) Ni3 0.01306(17) 0.0270(2) 0.02643(18) 0.0012(2) 0.00056(19) 0.00004(17) C1 0.0150(15) 0.0155(14) 0.0182(13) -0.0008(12) 0.0014(11) -0.0033(11) C2 0.0176(16) 0.0163(14) 0.0165(13) -0.0017(11) 0.0009(11) -0.0018(12) C3 0.0145(16) 0.0215(16) 0.0190(14) 0.0026(12) 0.0035(12) -0.0018(12) C4 0.0240(19) 0.0237(16) 0.0261(17) -0.0083(13) 0.0023(12) -0.0092(14) C5 0.0236(17) 0.0265(15) 0.0241(15) -0.0083(16) 0.0072(16) -0.0056(12) C6 0.0146(15) 0.0205(15) 0.0184(13) 0.0020(12) 0.0006(12) -0.0012(12) C7 0.0101(13) 0.0161(13) 0.0141(12) -0.0013(12) 0.0002(12) 0.0017(10) C8 0.0144(15) 0.0255(16) 0.0197(15) -0.0042(12) 0.0023(11) -0.0010(12) C9 0.0151(16) 0.0208(16) 0.0206(14) 0.0017(13) 0.0005(12) -0.0034(13) C10 0.0144(15) 0.0176(14) 0.0209(13) 0.0002(11) -0.0060(11) 0.0010(12) C11 0.0159(15) 0.0148(14) 0.0166(13) 0.0004(12) 0.0002(11) 0.0030(12) C12 0.0174(16) 0.0179(15) 0.0169(13) -0.0018(11) -0.0049(12) 0.0029(12) C13 0.0153(16) 0.0232(16) 0.0193(15) -0.0004(12) -0.0011(12) 0.0047(13) C14 0.0210(16) 0.0284(16) 0.0267(15) -0.0085(17) -0.0015(15) 0.0117(13) C15 0.0198(17) 0.0266(16) 0.0301(19) -0.0126(14) -0.0079(13) 0.0063(13) C16 0.0166(17) 0.0266(17) 0.0294(17) 0.0033(14) -0.0005(13) 0.0033(13) C17 0.0152(15) 0.0235(14) 0.0232(14) -0.0069(15) -0.0016(14) 0.0032(11) C18 0.0116(13) 0.0161(13) 0.0169(14) -0.0018(11) -0.0018(12) -0.0010(11) C19 0.0121(16) 0.0281(17) 0.044(2) -0.0071(15) -0.0013(14) 0.0013(13) C20 0.0172(17) 0.0233(16) 0.044(2) -0.0041(15) 0.0005(15) -0.0032(13) C21 0.0137(17) 0.0278(17) 0.048(2) -0.0099(16) -0.0004(15) -0.0002(14) C22 0.0097(13) 0.0286(15) 0.0241(13) 0.0029(14) 0.004(2) 0.0006(11) C23 0.0190(19) 0.0246(17) 0.050(3) -0.0052(16) 0.0011(16) 0.0035(14) C24 0.0136(17) 0.0312(19) 0.053(3) -0.0074(17) -0.0020(16) -0.0036(14) C25 0.0149(18) 0.0309(19) 0.061(3) -0.0106(17) 0.0024(17) 0.0025(14) C26 0.0130(13) 0.0265(15) 0.0213(13) 0.0036(15) -0.001(2) 0.0003(12) C27 0.0127(17) 0.0280(18) 0.045(2) -0.0090(15) 0.0008(14) 0.0017(13) C28 0.017(2) 0.069(3) 0.028(2) 0.020(2) -0.0040(15) -0.0014(19) C29 0.015(2) 0.091(4) 0.031(2) 0.025(2) 0.0037(17) 0.003(2) C30 0.017(2) 0.086(4) 0.029(2) 0.019(2) 0.0026(17) 0.001(2) C31 0.0129(16) 0.0311(18) 0.0229(15) 0.0032(14) -0.0002(12) 0.0007(13) C32 0.0135(15) 0.0291(17) 0.0186(14) 0.0049(13) 0.0030(13) -0.0018(13) C33 0.0145(16) 0.0327(19) 0.0212(15) 0.0082(14) 0.0009(13) 0.0018(14) C34 0.0104(13) 0.0268(15) 0.0223(16) 0.0005(15) 0.0009(18) 0.0000(12) C35 0.0110(13) 0.0292(16) 0.0231(15) 0.0050(16) 0.0001(19) 0.0017(12) C36 0.019(2) 0.082(4) 0.0252(19) 0.0153(19) -0.0027(16) 0.003(2) C37 0.0161(17) 0.036(2) 0.0196(15) 0.0069(14) 0.0034(13) -0.0018(14) C38 0.0130(17) 0.0304(19) 0.048(2) -0.0066(16) 0.0003(15) -0.0038(14) N1 0.0116(11) 0.0277(13) 0.0194(11) 0.0000(12) -0.0019(18) -0.0006(10) N2 0.0102(11) 0.0277(12) 0.0196(12) 0.0049(13) -0.0001(14) 0.0027(10) N3 0.0091(11) 0.0222(12) 0.0247(12) 0.0044(14) -0.0030(15) -0.0012(9) N4 0.0093(11) 0.0261(12) 0.0196(12) -0.0021(11) -0.0005(15) 0.0002(10) O1 0.0218(12) 0.0201(12) 0.0218(11) -0.0029(9) 0.0079(10) -0.0018(10) O2 0.0167(11) 0.0256(12) 0.0331(13) -0.0027(11) 0.0051(11) -0.0009(9) O3 0.0168(12) 0.0213(12) 0.0412(14) -0.0024(11) 0.0080(10) -0.0043(10) O4 0.0222(14) 0.0464(16) 0.0525(18) 0.0138(14) -0.0113(12) -0.0099(12) O5 0.0199(12) 0.0254(12) 0.0212(11) -0.0022(10) -0.0073(9) 0.0027(10) O6 0.0166(12) 0.0519(18) 0.0521(19) -0.0220(15) -0.0088(12) 0.0050(12) O7 0.0164(12) 0.0328(14) 0.0482(15) -0.0097(12) -0.0037(11) 0.0088(11) O8 0.0145(11) 0.0227(11) 0.0141(10) 0.0006(8) -0.0012(8) 0.0049(9) O9 0.0207(13) 0.0223(12) 0.0145(10) -0.0024(9) -0.0015(9) 0.0033(10) O10 0.0201(12) 0.0236(12) 0.0147(10) -0.0019(9) 0.0019(9) -0.0040(10) O11 0.0199(13) 0.0247(13) 0.0159(10) 0.0008(9) -0.0011(9) 0.0000(10) O12 0.0213(13) 0.0248(13) 0.0182(11) 0.0018(9) 0.0018(9) -0.0018(10) O13 0.0246(13) 0.0285(13) 0.0282(12) -0.0014(10) 0.0055(10) 0.0070(10) O14 0.0193(11) 0.0338(13) 0.0355(13) 0.0002(12) -0.0034(12) -0.0042(10) O15 0.0220(14) 0.0342(15) 0.0463(15) 0.0005(12) 0.0075(12) 0.0018(11) O16 0.0202(14) 0.098(3) 0.0333(14) 0.0161(17) -0.0053(12) 0.0007(16) O17 0.0165(12) 0.0285(13) 0.0149(10) 0.0019(9) 0.0004(8) -0.0060(10) O1W 0.074(5) 0.055(4) 0.055(4) 0.008(3) -0.006(4) -0.007(4) O2W 0.071(10) 0.065(9) 0.052(8) -0.001(7) -0.004(7) -0.019(8) O3W 0.068(5) 0.070(5) 0.065(5) -0.015(4) 0.032(4) 0.017(4) O4W 0.059(6) 0.089(7) 0.051(5) 0.008(5) 0.030(5) 0.003(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 O11 2.066(3) . ? Ni1 O10 2.066(2) 1_554 ? Ni1 O12 2.074(3) . ? Ni1 O9 2.084(2) . ? Ni1 N1 2.088(2) . ? Ni1 N2 2.121(3) 3_465 ? Ni2 O17 2.029(2) . ? Ni2 O8 2.051(2) . ? Ni2 O1 2.071(2) . ? Ni2 N3 2.098(2) . ? Ni2 N4 2.129(2) 3_465 ? Ni2 O5 2.147(2) . ? Ni3 O15 2.016(3) . ? Ni3 O16 2.028(3) . ? Ni3 O14 2.032(2) . ? Ni3 O3 2.059(2) . ? Ni3 O13 2.131(3) 2_565 ? Ni3 O2 2.195(2) . ? Ni3 C9 2.439(3) . ? C1 C6 1.388(4) . ? C1 C2 1.396(4) . ? C1 C7 1.534(4) . ? C2 C3 1.385(4) . ? C2 H2A 0.9300 . ? C3 C4 1.385(5) . ? C3 C9 1.500(4) . ? C4 C5 1.386(5) . ? C4 H4A 0.9300 . ? C5 C6 1.395(5) . ? C5 H5A 0.9300 . ? C6 C8 1.524(4) . ? C7 O17 1.256(4) . ? C7 O10 1.262(4) . ? C8 O1 1.254(4) . ? C8 O13 1.269(4) . ? C9 O2 1.250(4) . ? C9 O3 1.268(4) . ? C10 C15 1.387(5) . ? C10 C11 1.395(4) . ? C10 C17 1.506(4) . ? C11 C12 1.393(4) . ? C11 C18 1.504(4) . ? C12 C13 1.391(4) . ? C12 H12A 0.9300 . ? C13 C14 1.399(5) . ? C13 C16 1.509(5) . ? C14 C15 1.390(5) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 O6 1.248(5) . ? C16 O7 1.271(4) . ? C17 O4 1.237(4) . ? C17 O5 1.274(4) . ? C18 O9 1.264(4) . ? C18 O8 1.266(4) . ? C19 N1 1.338(5) . ? C19 C21 1.374(5) . ? C19 H19A 0.9300 . ? C20 N1 1.333(4) . ? C20 C23 1.373(5) . ? C20 H20A 0.9300 . ? C21 C22 1.393(5) . ? C21 H21A 0.9300 . ? C22 C23 1.402(5) . ? C22 C26 1.490(4) . ? C23 H23A 0.9300 . ? C24 N2 1.337(5) . ? C24 C25 1.374(5) . ? C24 H24A 0.9300 . ? C25 C26 1.390(5) . ? C25 H25A 0.9300 . ? C26 C38 1.372(5) . ? C27 N2 1.328(4) . ? C27 C38 1.382(5) . ? C27 H27A 0.9300 . ? C28 N3 1.309(6) . ? C28 C29 1.381(6) . ? C28 H28A 0.9300 . ? C29 C35 1.373(7) . ? C29 H29A 0.9300 . ? C30 N3 1.337(6) . ? C30 C36 1.384(7) . ? C30 H30A 0.9300 . ? C31 N4 1.343(5) . ? C31 C37 1.389(5) . ? C31 H31A 0.9300 . ? C32 N4 1.341(5) . ? C32 C33 1.380(5) . ? C32 H32A 0.9300 . ? C33 C34 1.390(6) . ? C33 H33A 0.9300 . ? C34 C37 1.383(6) . ? C34 C35 1.482(4) . ? C35 C36 1.378(7) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? N2 Ni1 2.121(3) 3_565 ? N4 Ni2 2.129(2) 3_565 ? O10 Ni1 2.066(2) 1_556 ? O11 H3 0.8706 . ? O11 H4 0.7932 . ? O12 H1 1.0123 . ? O12 H2 0.7542 . ? O13 Ni3 2.131(3) 2_564 ? O14 H5 0.7255 . ? O14 H6 0.7915 . ? O15 H7 1.0707 . ? O15 H8 0.9528 . ? O16 H9 0.8866 . ? O16 H10 0.8340 . ? O1W O2W 0.89(2) . ? 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 O11 Ni1 O10 88.58(9) . 1_554 ? O11 Ni1 O12 173.67(11) . . ? O10 Ni1 O12 97.75(11) 1_554 . ? O11 Ni1 O9 89.21(10) . . ? O10 Ni1 O9 168.92(9) 1_554 . ? O12 Ni1 O9 84.60(9) . . ? O11 Ni1 N1 88.26(13) . . ? O10 Ni1 N1 93.37(13) 1_554 . ? O12 Ni1 N1 91.25(13) . . ? O9 Ni1 N1 97.42(13) . . ? O11 Ni1 N2 90.19(12) . 3_465 ? O10 Ni1 N2 85.27(12) 1_554 3_465 ? O12 Ni1 N2 90.44(12) . 3_465 ? O9 Ni1 N2 83.88(12) . 3_465 ? N1 Ni1 N2 177.96(11) . 3_465 ? O17 Ni2 O8 176.82(8) . . ? O17 Ni2 O1 91.35(10) . . ? O8 Ni2 O1 89.40(10) . . ? O17 Ni2 N3 90.88(13) . . ? O8 Ni2 N3 92.28(13) . . ? O1 Ni2 N3 82.46(10) . . ? O17 Ni2 N4 88.61(14) . 3_465 ? O8 Ni2 N4 88.23(14) . 3_465 ? O1 Ni2 N4 97.26(11) . 3_465 ? N3 Ni2 N4 179.41(15) . 3_465 ? O17 Ni2 O5 88.31(10) . . ? O8 Ni2 O5 91.80(9) . . ? O1 Ni2 O5 164.36(9) . . ? N3 Ni2 O5 81.91(11) . . ? N4 Ni2 O5 98.37(11) 3_465 . ? O15 Ni3 O16 85.98(13) . . ? O15 Ni3 O14 92.92(10) . . ? O16 Ni3 O14 96.19(13) . . ? O15 Ni3 O3 163.44(11) . . ? O16 Ni3 O3 85.09(12) . . ? O14 Ni3 O3 101.88(10) . . ? O15 Ni3 O13 97.05(11) . 2_565 ? O16 Ni3 O13 174.64(12) . 2_565 ? O14 Ni3 O13 88.09(11) . 2_565 ? O3 Ni3 O13 90.89(11) . 2_565 ? O15 Ni3 O2 103.94(10) . . ? O16 Ni3 O2 89.22(12) . . ? O14 Ni3 O2 162.64(9) . . ? O3 Ni3 O2 62.05(9) . . ? O13 Ni3 O2 85.76(11) 2_565 . ? O15 Ni3 C9 134.03(11) . . ? O16 Ni3 C9 86.26(12) . . ? O14 Ni3 C9 132.97(11) . . ? O3 Ni3 C9 31.32(10) . . ? O13 Ni3 C9 88.46(10) 2_565 . ? O2 Ni3 C9 30.74(10) . . ? C6 C1 C2 119.2(3) . . ? C6 C1 C7 125.8(3) . . ? C2 C1 C7 115.0(3) . . ? C3 C2 C1 121.2(3) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C2 C3 C4 119.6(3) . . ? C2 C3 C9 121.0(3) . . ? C4 C3 C9 119.3(3) . . ? C3 C4 C5 119.1(3) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C4 C5 C6 121.6(3) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C1 C6 C5 118.8(3) . . ? C1 C6 C8 129.3(3) . . ? C5 C6 C8 111.6(3) . . ? O17 C7 O10 124.0(3) . . ? O17 C7 C1 121.4(3) . . ? O10 C7 C1 114.6(3) . . ? O1 C8 O13 124.0(3) . . ? O1 C8 C6 118.5(3) . . ? O13 C8 C6 116.8(3) . . ? O2 C9 O3 121.3(3) . . ? O2 C9 C3 120.8(3) . . ? O3 C9 C3 117.8(3) . . ? O2 C9 Ni3 63.78(17) . . ? O3 C9 Ni3 57.55(17) . . ? C3 C9 Ni3 175.3(2) . . ? C15 C10 C11 120.6(3) . . ? C15 C10 C17 116.0(3) . . ? C11 C10 C17 123.4(3) . . ? C12 C11 C10 119.0(3) . . ? C12 C11 C18 119.9(3) . . ? C10 C11 C18 121.0(3) . . ? C13 C12 C11 121.0(3) . . ? C13 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? C12 C13 C14 119.2(3) . . ? C12 C13 C16 122.0(3) . . ? C14 C13 C16 118.8(3) . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C10 C15 C14 119.9(3) . . ? C10 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? O6 C16 O7 125.3(3) . . ? O6 C16 C13 118.3(3) . . ? O7 C16 C13 116.4(3) . . ? O4 C17 O5 126.2(3) . . ? O4 C17 C10 117.6(3) . . ? O5 C17 C10 116.2(3) . . ? O9 C18 O8 123.6(3) . . ? O9 C18 C11 116.4(3) . . ? O8 C18 C11 120.0(3) . . ? N1 C19 C21 123.5(3) . . ? N1 C19 H19A 118.3 . . ? C21 C19 H19A 118.3 . . ? N1 C20 C23 123.6(3) . . ? N1 C20 H20A 118.2 . . ? C23 C20 H20A 118.2 . . ? C19 C21 C22 119.9(3) . . ? C19 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C21 C22 C23 116.3(3) . . ? C21 C22 C26 122.1(3) . . ? C23 C22 C26 121.7(3) . . ? C20 C23 C22 119.7(3) . . ? C20 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? N2 C24 C25 123.7(3) . . ? N2 C24 H24A 118.1 . . ? C25 C24 H24A 118.1 . . ? C24 C25 C26 120.1(3) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C38 C26 C25 116.1(3) . . ? C38 C26 C22 123.2(3) . . ? C25 C26 C22 120.7(3) . . ? N2 C27 C38 123.9(3) . . ? N2 C27 H27A 118.0 . . ? C38 C27 H27A 118.0 . . ? N3 C28 C29 124.1(4) . . ? N3 C28 H28A 118.0 . . ? C29 C28 H28A 118.0 . . ? C35 C29 C28 120.1(4) . . ? C35 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? N3 C30 C36 123.1(4) . . ? N3 C30 H30A 118.5 . . ? C36 C30 H30A 118.5 . . ? N4 C31 C37 122.9(3) . . ? N4 C31 H31A 118.6 . . ? C37 C31 H31A 118.6 . . ? N4 C32 C33 123.3(3) . . ? N4 C32 H32A 118.4 . . ? C33 C32 H32A 118.4 . . ? C32 C33 C34 120.0(3) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C37 C34 C33 116.9(3) . . ? C37 C34 C35 121.7(4) . . ? C33 C34 C35 121.4(4) . . ? C29 C35 C36 116.1(3) . . ? C29 C35 C34 122.5(4) . . ? C36 C35 C34 121.3(4) . . ? C35 C36 C30 120.0(4) . . ? C35 C36 H36A 120.0 . . ? C30 C36 H36A 120.0 . . ? C34 C37 C31 120.0(3) . . ? C34 C37 H37A 120.0 . . ? C31 C37 H37A 120.0 . . ? C26 C38 C27 120.2(3) . . ? C26 C38 H38A 119.9 . . ? C27 C38 H38A 119.9 . . ? C20 N1 C19 116.9(3) . . ? C20 N1 Ni1 121.9(2) . . ? C19 N1 Ni1 121.2(2) . . ? C27 N2 C24 115.9(3) . . ? C27 N2 Ni1 123.8(2) . 3_565 ? C24 N2 Ni1 120.2(2) . 3_565 ? C28 N3 C30 116.4(3) . . ? C28 N3 Ni2 123.0(3) . . ? C30 N3 Ni2 120.6(3) . . ? C32 N4 C31 116.9(2) . . ? C32 N4 Ni2 121.5(3) . 3_565 ? C31 N4 Ni2 121.6(3) . 3_565 ? C8 O1 Ni2 130.9(2) . . ? C9 O2 Ni3 85.49(19) . . ? C9 O3 Ni3 91.1(2) . . ? C17 O5 Ni2 112.2(2) . . ? C18 O8 Ni2 132.1(2) . . ? C18 O9 Ni1 128.3(2) . . ? C7 O10 Ni1 126.6(2) . 1_556 ? Ni1 O11 H3 140.5 . . ? Ni1 O11 H4 106.4 . . ? H3 O11 H4 99.4 . . ? Ni1 O12 H1 121.8 . . ? Ni1 O12 H2 110.8 . . ? H1 O12 H2 110.3 . . ? C8 O13 Ni3 125.7(2) . 2_564 ? Ni3 O14 H5 107.0 . . ? Ni3 O14 H6 114.5 . . ? H5 O14 H6 99.5 . . ? Ni3 O15 H7 118.3 . . ? Ni3 O15 H8 112.2 . . ? H7 O15 H8 101.2 . . ? Ni3 O16 H9 118.5 . . ? Ni3 O16 H10 107.6 . . ? H9 O16 H10 121.9 . . ? C7 O17 Ni2 129.1(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.777 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.092 data_qc52 _database_code_depnum_ccdc_archive 'CCDC 246457' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H40 N4 Ni2 O20' _chemical_formula_weight 990.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.032(3) _cell_length_b 11.238(2) _cell_length_c 12.259(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.85(3) _cell_angle_gamma 90.00 _cell_volume 1928.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8048 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.301 _exptl_crystal_size_mid 0.274 _exptl_crystal_size_min 0.197 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.732 _exptl_absorpt_correction_T_max 0.810 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_decay_% ? _diffrn_reflns_number 8048 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4409 _reflns_number_gt 3233 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.0439P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4409 _refine_ls_number_parameters 303 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.19050(3) 0.2500 0.01447(11) Uani 1 2 d S . . Ni2 Ni 0.5000 -0.10370(3) -0.2500 0.01690(11) Uani 1 2 d S . . C1 C 0.22699(14) 0.23879(19) -0.08237(19) 0.0170(5) Uani 1 1 d . . . C2 C 0.20364(14) 0.28960(19) 0.01596(19) 0.0162(4) Uani 1 1 d . . . C3 C 0.21740(15) 0.41189(19) 0.0338(2) 0.0200(5) Uani 1 1 d . . . H3A H 0.2023 0.4454 0.0998 0.024 Uiso 1 1 calc R . . C4 C 0.25320(15) 0.4831(2) -0.0460(2) 0.0206(5) Uani 1 1 d . . . C5 C 0.27319(16) 0.4333(2) -0.1458(2) 0.0248(5) Uani 1 1 d . . . H5A H 0.2954 0.4811 -0.2006 0.030 Uiso 1 1 calc R . . C6 C 0.26009(16) 0.3129(2) -0.1632(2) 0.0244(5) Uani 1 1 d . . . H6A H 0.2736 0.2804 -0.2302 0.029 Uiso 1 1 calc R . . C7 C 0.22203(15) 0.1054(2) -0.1014(2) 0.0205(5) Uani 1 1 d . . . C8 C 0.16649(15) 0.21989(19) 0.11037(19) 0.0178(5) Uani 1 1 d . . . C9 C 0.27479(16) 0.6125(2) -0.0279(2) 0.0249(5) Uani 1 1 d . . . C10 C 0.02959(16) -0.0553(2) 0.1649(2) 0.0241(5) Uani 1 1 d . . . H10A H 0.0508 -0.0135 0.1058 0.029 Uiso 1 1 calc R . . C11 C 0.02996(16) -0.1781(2) 0.1610(2) 0.0252(5) Uani 1 1 d . . . H11A H 0.0499 -0.2176 0.0999 0.030 Uiso 1 1 calc R . . C12 C 0.0000 -0.2421(3) 0.2500 0.0206(7) Uani 1 2 d S . . C13 C 0.0000 -0.3740(3) 0.2500 0.0194(7) Uani 1 2 d S . . C14 C -0.02093(16) -0.4382(2) 0.1542(2) 0.0233(5) Uani 1 1 d . . . H14A H -0.0344 -0.3987 0.0883 0.028 Uiso 1 1 calc R . . C15 C -0.02156(16) -0.5616(2) 0.1577(2) 0.0237(5) Uani 1 1 d . . . H15A H -0.0376 -0.6034 0.0936 0.028 Uiso 1 1 calc R . . C16 C 0.53777(17) -0.3510(2) -0.1641(2) 0.0262(5) Uani 1 1 d . . . H16A H 0.5645 -0.3094 -0.1041 0.031 Uiso 1 1 calc R . . C17 C 0.53868(16) -0.4740(2) -0.1611(2) 0.0259(5) Uani 1 1 d . . . H17A H 0.5651 -0.5134 -0.0996 0.031 Uiso 1 1 calc R . . C18 C 0.5000 -0.5385(3) -0.2500 0.0208(7) Uani 1 2 d S . . C19 C 0.5000 -0.6707(3) -0.2500 0.0215(7) Uani 1 2 d S . . C20 C 0.49694(17) -0.7349(2) -0.1535(2) 0.0255(5) Uani 1 1 d . . . H20A H 0.4955 -0.6954 -0.0870 0.031 Uiso 1 1 calc R . . C21 C 0.49604(16) -0.8572(2) -0.1568(2) 0.0241(5) Uani 1 1 d . . . H21A H 0.4925 -0.8987 -0.0916 0.029 Uiso 1 1 calc R . . N1 N 0.0000 -0.6231(2) 0.2500 0.0205(6) Uani 1 2 d S . . N2 N 0.0000 0.0064(2) 0.2500 0.0200(6) Uani 1 2 d S . . N3 N 0.5000 -0.9194(2) -0.2500 0.0200(6) Uani 1 2 d S . . N4 N 0.5000 -0.2893(2) -0.2500 0.0200(6) Uani 1 2 d S . . O1 O 0.26270(13) 0.06542(15) -0.18210(15) 0.0316(4) Uani 1 1 d . . . O2 O 0.18126(12) 0.04264(14) -0.03429(15) 0.0280(4) Uani 1 1 d . . . O3 O 0.22760(11) 0.18762(16) 0.18417(14) 0.0307(4) Uani 1 1 d . . . O4 O 0.07758(10) 0.21030(13) 0.11313(13) 0.0195(3) Uani 1 1 d . . . O5 O 0.23690(14) 0.65729(16) 0.05922(16) 0.0384(5) Uani 1 1 d . . . H9 H 0.2456 0.7384 0.0582 0.086(13) Uiso 1 1 d R . . O6 O 0.32434(14) 0.66915(16) -0.08555(18) 0.0419(5) Uani 1 1 d . . . O7 O 0.60841(11) -0.10242(15) -0.12390(14) 0.0255(4) Uani 1 1 d D . . H3 H 0.6566 -0.1354 -0.1452 0.027(7) Uiso 1 1 d RD . . H4 H 0.6186 -0.0385 -0.1142 0.059(12) Uiso 1 1 d RD . . O8 O 0.39775(12) -0.10318(16) -0.13324(15) 0.0273(4) Uani 1 1 d D . . H5 H 0.3751 -0.1712 -0.1187 0.055(10) Uiso 1 1 d RD . . H6 H 0.3670 -0.0594 -0.1507 0.069(14) Uiso 1 1 d RD . . O9 O -0.12359(11) 0.18355(14) 0.14152(14) 0.0227(4) Uani 1 1 d D . . H1 H -0.1749 0.1852 0.1999 0.075(12) Uiso 1 1 d RD . . H2 H -0.1393 0.1312 0.1030 0.065(12) Uiso 1 1 d RD . . O1W O 0.27314(12) 0.88251(15) 0.10123(16) 0.0298(4) Uani 1 1 d D . . H7 H 0.2681 0.8982 0.1649 0.048(10) Uiso 1 1 d RD . . H8 H 0.2390 0.9346 0.0603 0.063(11) Uiso 1 1 d RD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01637(19) 0.0098(2) 0.0177(2) 0.000 0.00433(15) 0.000 Ni2 0.0174(2) 0.0088(2) 0.0247(3) 0.000 0.00351(16) 0.000 C1 0.0155(10) 0.0153(11) 0.0204(12) -0.0001(9) 0.0034(9) -0.0004(8) C2 0.0148(9) 0.0157(11) 0.0182(12) 0.0019(9) 0.0023(8) 0.0009(8) C3 0.0207(11) 0.0192(12) 0.0205(13) -0.0019(9) 0.0036(9) -0.0003(9) C4 0.0206(10) 0.0157(11) 0.0256(14) 0.0028(9) 0.0018(9) -0.0011(9) C5 0.0274(12) 0.0253(13) 0.0227(14) 0.0058(11) 0.0087(10) -0.0026(10) C6 0.0305(12) 0.0238(12) 0.0199(13) -0.0001(10) 0.0096(10) 0.0017(10) C7 0.0190(10) 0.0201(12) 0.0220(13) -0.0019(10) -0.0014(9) 0.0032(9) C8 0.0224(11) 0.0126(11) 0.0189(12) -0.0003(9) 0.0052(9) 0.0017(8) C9 0.0264(12) 0.0200(12) 0.0282(15) 0.0024(10) 0.0017(10) 0.0003(9) C10 0.0301(12) 0.0169(12) 0.0261(14) 0.0010(10) 0.0071(10) -0.0007(9) C11 0.0306(12) 0.0178(12) 0.0280(14) -0.0031(10) 0.0080(10) 0.0019(9) C12 0.0197(15) 0.0159(16) 0.0254(19) 0.000 -0.0036(13) 0.000 C13 0.0207(15) 0.0129(16) 0.0244(19) 0.000 0.0005(13) 0.000 C14 0.0303(12) 0.0179(12) 0.0213(14) 0.0037(10) -0.0007(10) 0.0027(9) C15 0.0315(12) 0.0168(12) 0.0225(14) -0.0021(10) -0.0012(10) 0.0008(9) C16 0.0308(12) 0.0174(12) 0.0300(15) -0.0018(10) -0.0005(11) -0.0013(10) C17 0.0300(12) 0.0166(12) 0.0302(15) 0.0024(10) -0.0041(11) 0.0017(9) C18 0.0212(15) 0.0145(16) 0.027(2) 0.000 0.0054(14) 0.000 C19 0.0216(15) 0.0132(16) 0.030(2) 0.000 0.0025(14) 0.000 C20 0.0353(13) 0.0177(12) 0.0238(14) -0.0045(10) 0.0037(11) 0.0005(10) C21 0.0313(12) 0.0169(12) 0.0246(14) 0.0025(10) 0.0050(10) -0.0008(10) N1 0.0249(14) 0.0132(14) 0.0236(16) 0.000 0.0029(12) 0.000 N2 0.0208(13) 0.0156(14) 0.0238(16) 0.000 0.0021(11) 0.000 N3 0.0199(13) 0.0112(13) 0.0290(17) 0.000 0.0034(11) 0.000 N4 0.0202(13) 0.0134(14) 0.0267(17) 0.000 0.0038(11) 0.000 O1 0.0461(10) 0.0227(9) 0.0274(11) -0.0022(8) 0.0141(8) 0.0086(8) O2 0.0375(9) 0.0165(9) 0.0311(11) 0.0024(7) 0.0100(8) -0.0017(7) O3 0.0223(8) 0.0444(11) 0.0257(10) 0.0140(8) 0.0034(7) 0.0060(7) O4 0.0193(7) 0.0198(8) 0.0201(9) 0.0005(7) 0.0059(6) -0.0020(6) O5 0.0646(13) 0.0187(10) 0.0334(12) -0.0019(8) 0.0127(10) -0.0066(9) O6 0.0484(11) 0.0210(10) 0.0591(15) 0.0017(9) 0.0247(10) -0.0089(8) O7 0.0222(8) 0.0186(9) 0.0353(11) -0.0023(7) 0.0002(7) 0.0014(7) O8 0.0261(8) 0.0183(9) 0.0388(12) 0.0036(8) 0.0111(8) -0.0005(8) O9 0.0228(8) 0.0226(9) 0.0227(9) -0.0024(8) 0.0014(7) -0.0001(6) O1W 0.0414(10) 0.0213(9) 0.0268(11) -0.0003(8) 0.0018(8) 0.0007(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 2.069(3) . ? Ni1 O4 2.0725(17) 2 ? Ni1 O4 2.0725(17) . ? Ni1 N1 2.094(3) 1_565 ? Ni1 O9 2.1149(17) 2 ? Ni1 O9 2.1149(17) . ? Ni2 N3 2.071(3) 1_565 ? Ni2 N4 2.086(3) . ? Ni2 O8 2.0935(18) 2_654 ? Ni2 O8 2.0935(18) . ? Ni2 O7 2.0949(17) 2_654 ? Ni2 O7 2.0949(17) . ? C1 C2 1.393(3) . ? C1 C6 1.398(3) . ? C1 C7 1.518(3) . ? C2 C3 1.403(3) . ? C2 C8 1.519(3) . ? C3 C4 1.384(3) . ? C4 C5 1.390(3) . ? C4 C9 1.499(3) . ? C5 C6 1.381(3) . ? C7 O2 1.251(3) . ? C7 O1 1.257(3) . ? C8 O4 1.255(3) . ? C8 O3 1.257(3) . ? C9 O6 1.206(3) . ? C9 O5 1.324(3) . ? C10 N2 1.341(3) . ? C10 C11 1.380(3) . ? C11 C12 1.395(3) . ? C12 C11 1.395(3) 2 ? C12 C13 1.483(4) . ? C13 C14 1.393(3) . ? C13 C14 1.393(3) 2 ? C14 C15 1.387(3) . ? C15 N1 1.343(3) . ? C16 N4 1.340(3) . ? C16 C17 1.383(3) . ? C17 C18 1.389(3) . ? C18 C17 1.389(3) 2_654 ? C18 C19 1.485(4) . ? C19 C20 1.389(3) 2_654 ? C19 C20 1.389(3) . ? C20 C21 1.375(3) . ? C21 N3 1.344(3) . ? N1 C15 1.343(3) 2 ? N1 Ni1 2.094(3) 1_545 ? N2 C10 1.341(3) 2 ? N3 C21 1.344(3) 2_654 ? N3 Ni2 2.071(3) 1_545 ? N4 C16 1.340(3) 2_654 ? 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 N2 Ni1 O4 96.16(4) . 2 ? N2 Ni1 O4 96.16(4) . . ? O4 Ni1 O4 167.67(8) 2 . ? N2 Ni1 N1 180.0 . 1_565 ? O4 Ni1 N1 83.84(4) 2 1_565 ? O4 Ni1 N1 83.84(4) . 1_565 ? N2 Ni1 O9 87.88(5) . 2 ? O4 Ni1 O9 87.02(6) 2 2 ? O4 Ni1 O9 93.43(6) . 2 ? N1 Ni1 O9 92.12(5) 1_565 2 ? N2 Ni1 O9 87.88(5) . . ? O4 Ni1 O9 93.43(6) 2 . ? O4 Ni1 O9 87.02(6) . . ? N1 Ni1 O9 92.12(5) 1_565 . ? O9 Ni1 O9 175.77(9) 2 . ? N3 Ni2 N4 180.0 1_565 . ? N3 Ni2 O8 89.84(5) 1_565 2_654 ? N4 Ni2 O8 90.16(5) . 2_654 ? N3 Ni2 O8 89.84(5) 1_565 . ? N4 Ni2 O8 90.16(5) . . ? O8 Ni2 O8 179.68(10) 2_654 . ? N3 Ni2 O7 89.61(5) 1_565 2_654 ? N4 Ni2 O7 90.39(5) . 2_654 ? O8 Ni2 O7 89.57(7) 2_654 2_654 ? O8 Ni2 O7 90.42(7) . 2_654 ? N3 Ni2 O7 89.61(5) 1_565 . ? N4 Ni2 O7 90.39(5) . . ? O8 Ni2 O7 90.42(7) 2_654 . ? O8 Ni2 O7 89.57(7) . . ? O7 Ni2 O7 179.21(10) 2_654 . ? C2 C1 C6 118.6(2) . . ? C2 C1 C7 121.8(2) . . ? C6 C1 C7 119.6(2) . . ? C1 C2 C3 119.9(2) . . ? C1 C2 C8 124.12(19) . . ? C3 C2 C8 115.9(2) . . ? C4 C3 C2 120.6(2) . . ? C3 C4 C5 119.5(2) . . ? C3 C4 C9 122.4(2) . . ? C5 C4 C9 118.0(2) . . ? C6 C5 C4 119.9(2) . . ? C5 C6 C1 121.4(2) . . ? O2 C7 O1 124.6(2) . . ? O2 C7 C1 118.3(2) . . ? O1 C7 C1 117.1(2) . . ? O4 C8 O3 125.9(2) . . ? O4 C8 C2 117.23(19) . . ? O3 C8 C2 116.40(19) . . ? O6 C9 O5 123.4(2) . . ? O6 C9 C4 123.0(2) . . ? O5 C9 C4 113.6(2) . . ? N2 C10 C11 123.1(2) . . ? C10 C11 C12 119.1(2) . . ? C11 C12 C11 117.9(3) 2 . ? C11 C12 C13 121.04(15) 2 . ? C11 C12 C13 121.04(15) . . ? C14 C13 C14 117.6(3) . 2 ? C14 C13 C12 121.19(15) . . ? C14 C13 C12 121.19(15) 2 . ? C15 C14 C13 119.5(2) . . ? N1 C15 C14 122.6(2) . . ? N4 C16 C17 122.8(2) . . ? C16 C17 C18 119.9(2) . . ? C17 C18 C17 117.1(3) . 2_654 ? C17 C18 C19 121.47(15) . . ? C17 C18 C19 121.47(15) 2_654 . ? C20 C19 C20 117.4(3) 2_654 . ? C20 C19 C18 121.32(15) 2_654 . ? C20 C19 C18 121.32(15) . . ? C21 C20 C19 119.7(2) . . ? N3 C21 C20 123.0(2) . . ? C15 N1 C15 118.0(3) 2 . ? C15 N1 Ni1 120.99(14) 2 1_545 ? C15 N1 Ni1 120.99(14) . 1_545 ? C10 N2 C10 117.7(3) . 2 ? C10 N2 Ni1 121.14(14) . . ? C10 N2 Ni1 121.14(14) 2 . ? C21 N3 C21 117.2(3) . 2_654 ? C21 N3 Ni2 121.38(14) . 1_545 ? C21 N3 Ni2 121.38(14) 2_654 1_545 ? C16 N4 C16 117.6(3) 2_654 . ? C16 N4 Ni2 121.18(15) 2_654 . ? C16 N4 Ni2 121.18(15) . . ? C8 O4 Ni1 127.46(16) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.501 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.071