Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;The crystal and molecular structures of the related nickel(II) complexes of open-chain and macrocyclic oxamide-based ligands and the peculiarities of water aggregates in their crystal lattices ; _publ_contact_author_name 'Yaroslaw Lampeka' _publ_contact_author_email LAMPEKA@IPHCH.KIEV.UA loop_ _publ_author_name Y.Lampeka S.P.Gavrish P.Lightfoot H.Pritzkow # Attachment 'cif.cif' data_NiL1_4H2O _database_code_depnum_ccdc_archive 'CCDC 648827' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H20 N4 Ni O6' _chemical_formula_weight 302.97 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 7.8979(6) _cell_length_b 7.6099(6) _cell_length_c 20.9804(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1260.97(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description hexagonal _exptl_crystal_colour green _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 1.562 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8329 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12970 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 33.18 _reflns_number_total 4009 _reflns_number_gt 3931 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.0688P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0089(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.699(9) _refine_ls_number_reflns 4009 _refine_ls_number_parameters 236 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0609 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.805355(17) 0.545869(15) 0.031486(9) 0.01490(5) Uani 1 1 d . . . O1 O 0.66858(14) 1.01672(13) 0.08946(5) 0.01922(17) Uani 1 1 d . . . O2 O 0.78175(14) 1.02485(12) -0.03927(6) 0.01911(18) Uani 1 1 d . . . O3 O 1.22143(17) 0.92823(16) 0.33162(7) 0.0222(2) Uani 1 1 d . . . O4 O 0.71966(17) 1.06686(14) 0.21753(6) 0.0218(2) Uani 1 1 d . . . O5 O 0.92359(15) 0.83617(17) 0.28287(7) 0.0291(2) Uani 1 1 d . . . O6 O 0.90854(17) 1.3536(2) 0.25523(9) 0.0421(4) Uani 1 1 d . . . N1 N 0.76240(16) 0.38757(13) 0.10118(6) 0.01892(19) Uani 1 1 d . . . N2 N 0.71795(15) 0.71696(14) 0.08356(6) 0.01686(19) Uani 1 1 d . . . N3 N 0.82728(14) 0.72482(14) -0.02662(6) 0.01699(19) Uani 1 1 d . . . N4 N 0.90173(15) 0.39615(13) -0.03310(6) 0.0195(2) Uani 1 1 d . . . C1 C 0.62091(19) 0.46623(15) 0.13927(8) 0.0210(2) Uani 1 1 d . . . C2 C 0.65800(19) 0.66245(16) 0.14625(7) 0.0199(2) Uani 1 1 d . . . C3 C 0.71662(16) 0.87825(15) 0.06130(7) 0.0151(2) Uani 1 1 d . . . C4 C 0.78112(16) 0.88294(15) -0.00784(7) 0.0149(2) Uani 1 1 d . . . C5 C 0.89338(18) 0.67888(16) -0.08935(7) 0.0194(2) Uani 1 1 d . . . C6 C 0.8636(2) 0.48065(18) -0.09592(8) 0.0221(2) Uani 1 1 d . . . H1A H 0.610(3) 0.411(3) 0.1818(10) 0.021(5) Uiso 1 1 d . . . H1B H 0.516(4) 0.445(2) 0.1134(12) 0.027(6) Uiso 1 1 d . . . H2A H 0.560(2) 0.732(3) 0.1570(11) 0.016(5) Uiso 1 1 d . . . H2B H 0.749(3) 0.679(3) 0.1767(11) 0.021(4) Uiso 1 1 d . . . H5A H 1.006(3) 0.705(3) -0.0925(11) 0.029(5) Uiso 1 1 d . . . H5B H 0.841(3) 0.745(3) -0.1213(12) 0.027(5) Uiso 1 1 d . . . H6A H 0.936(3) 0.437(3) -0.1308(12) 0.024(5) Uiso 1 1 d . . . H6B H 0.752(4) 0.453(3) -0.1055(13) 0.024(6) Uiso 1 1 d . . . H11N H 0.738(3) 0.273(3) 0.0947(10) 0.016(4) Uiso 1 1 d . . . H12N H 0.846(4) 0.394(4) 0.1227(15) 0.037(6) Uiso 1 1 d . . . H31O H 1.220(4) 0.942(3) 0.3619(16) 0.025(7) Uiso 1 1 d . . . H32O H 1.145(5) 0.904(4) 0.3192(16) 0.045(8) Uiso 1 1 d . . . H41N H 0.878(3) 0.283(3) -0.0359(10) 0.027(5) Uiso 1 1 d . . . H41O H 0.707(3) 1.045(3) 0.1813(16) 0.022(7) Uiso 1 1 d . . . H42N H 1.011(3) 0.394(3) -0.0307(11) 0.028(5) Uiso 1 1 d . . . H42O H 0.622(5) 1.085(4) 0.2304(15) 0.048(8) Uiso 1 1 d . . . H51O H 0.873(5) 0.766(4) 0.2993(16) 0.052(8) Uiso 1 1 d . . . H52O H 0.865(4) 0.907(4) 0.2684(15) 0.037(6) Uiso 1 1 d . . . H61O H 0.857(4) 1.277(4) 0.2462(15) 0.047(7) Uiso 1 1 d . . . H62O H 0.850(4) 1.404(4) 0.2755(15) 0.036(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01737(7) 0.00937(6) 0.01795(8) 0.00018(6) -0.00017(7) 0.00045(4) O1 0.0271(4) 0.0117(3) 0.0189(5) -0.0019(3) 0.0010(4) 0.0018(3) O2 0.0275(5) 0.0117(3) 0.0181(5) 0.0023(3) 0.0010(4) -0.0008(3) O3 0.0230(5) 0.0252(5) 0.0184(5) -0.0023(4) 0.0000(4) -0.0016(4) O4 0.0240(5) 0.0218(5) 0.0196(5) -0.0004(4) -0.0008(4) 0.0004(4) O5 0.0233(5) 0.0312(5) 0.0329(6) 0.0086(5) -0.0039(4) -0.0023(4) O6 0.0270(6) 0.0358(6) 0.0635(10) -0.0236(6) 0.0155(6) -0.0090(5) N1 0.0210(5) 0.0124(4) 0.0234(6) 0.0030(3) -0.0017(4) 0.0002(4) N2 0.0232(5) 0.0115(4) 0.0158(5) 0.0019(3) 0.0014(4) 0.0009(3) N3 0.0231(5) 0.0111(4) 0.0167(5) -0.0007(3) 0.0011(4) 0.0014(3) N4 0.0204(5) 0.0121(4) 0.0260(6) -0.0025(3) 0.0008(4) 0.0006(3) C1 0.0233(6) 0.0146(5) 0.0253(7) 0.0041(4) 0.0030(5) -0.0019(4) C2 0.0269(6) 0.0156(5) 0.0171(6) 0.0025(4) 0.0031(5) -0.0005(4) C3 0.0174(5) 0.0114(5) 0.0164(6) 0.0006(4) -0.0023(4) -0.0001(4) C4 0.0174(5) 0.0120(4) 0.0152(5) -0.0001(3) -0.0005(4) -0.0011(4) C5 0.0245(6) 0.0167(5) 0.0169(5) -0.0011(4) 0.0027(4) 0.0011(4) C6 0.0269(6) 0.0180(5) 0.0214(6) -0.0057(4) 0.0015(5) 0.0003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.8345(11) . ? Ni1 N3 1.8360(11) . ? Ni1 N1 1.9247(12) . ? Ni1 N4 1.9270(12) . ? O1 C3 1.2662(16) . ? O2 C4 1.2653(15) . ? O3 H31O 0.64(3) . ? O3 H32O 0.68(4) . ? O4 H41O 0.78(3) . ? O4 H42O 0.83(4) . ? O5 H51O 0.75(4) . ? O5 H52O 0.77(3) . ? O6 H61O 0.74(4) . ? O6 H62O 0.73(3) . ? N1 C1 1.499(2) . ? N1 H11N 0.90(2) . ? N1 H12N 0.80(3) . ? N2 C3 1.3133(16) . ? N2 C2 1.4582(17) . ? N3 C4 1.3176(16) . ? N3 C5 1.4583(18) . ? N4 C6 1.497(2) . ? N4 H41N 0.88(2) . ? N4 H42N 0.87(2) . ? C1 C2 1.5288(17) . ? C1 H1A 0.99(2) . ? C1 H1B 1.00(3) . ? C2 H2A 0.968(18) . ? C2 H2B 0.97(2) . ? C3 C4 1.5378(19) . ? C5 C6 1.5330(18) . ? C5 H5A 0.91(2) . ? C5 H5B 0.94(2) . ? C6 H6A 0.98(3) . ? C6 H6B 0.93(3) . ? 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 N3 84.52(5) . . ? N2 Ni1 N1 85.72(5) . . ? N3 Ni1 N1 170.18(5) . . ? N2 Ni1 N4 170.76(5) . . ? N3 Ni1 N4 86.24(5) . . ? N1 Ni1 N4 103.52(5) . . ? H31O O3 H32O 114(4) . . ? H41O O4 H42O 103(3) . . ? H51O O5 H52O 112(3) . . ? H61O O6 H62O 102(3) . . ? C1 N1 Ni1 106.65(8) . . ? C1 N1 H11N 108.1(13) . . ? Ni1 N1 H11N 121.8(13) . . ? C1 N1 H12N 107(2) . . ? Ni1 N1 H12N 104(2) . . ? H11N N1 H12N 108(3) . . ? C3 N2 C2 125.74(11) . . ? C3 N2 Ni1 117.03(10) . . ? C2 N2 Ni1 117.23(8) . . ? C4 N3 C5 126.01(11) . . ? C4 N3 Ni1 116.91(9) . . ? C5 N3 Ni1 117.08(8) . . ? C6 N4 Ni1 106.59(8) . . ? C6 N4 H41N 108.4(15) . . ? Ni1 N4 H41N 122.5(15) . . ? C6 N4 H42N 105.0(15) . . ? Ni1 N4 H42N 111.2(16) . . ? H41N N4 H42N 102(2) . . ? N1 C1 C2 107.36(11) . . ? N1 C1 H1A 112.2(13) . . ? C2 C1 H1A 110.2(13) . . ? N1 C1 H1B 105.2(14) . . ? C2 C1 H1B 111.4(11) . . ? H1A C1 H1B 110.3(19) . . ? N2 C2 C1 104.70(11) . . ? N2 C2 H2A 108.3(13) . . ? C1 C2 H2A 113.8(11) . . ? N2 C2 H2B 108.5(14) . . ? C1 C2 H2B 109.6(12) . . ? H2A C2 H2B 111.6(18) . . ? O1 C3 N2 127.89(13) . . ? O1 C3 C4 121.34(11) . . ? N2 C3 C4 110.76(11) . . ? O2 C4 N3 128.49(13) . . ? O2 C4 C3 120.84(12) . . ? N3 C4 C3 110.65(11) . . ? N3 C5 C6 105.19(11) . . ? N3 C5 H5A 111.2(14) . . ? C6 C5 H5A 111.0(14) . . ? N3 C5 H5B 111.0(15) . . ? C6 C5 H5B 113.4(15) . . ? H5A C5 H5B 105(2) . . ? N4 C6 C5 108.22(11) . . ? N4 C6 H6A 113.1(13) . . ? C5 C6 H6A 108.1(12) . . ? N4 C6 H6B 106.7(16) . . ? C5 C6 H6B 112.7(13) . . ? H6A C6 H6B 108(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 33.18 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.831 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.064 #===END data_NiL2_3H2O _database_code_depnum_ccdc_archive 'CCDC 648828' #------------------------------------------------------------------------------ _audit_creation_date 'Sat Feb 27 10:52:51 2005' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction teXsan _computing_structure_solution ? _computing_structure_refinement teXsan _computing_publication_material teXsan #------------------------------------------------------------------------------ _cell_length_a 9.280(4) _cell_length_b 10.809(3) _cell_length_c 7.634(2) _cell_angle_alpha 95.95(2) _cell_angle_beta 100.49(3) _cell_angle_gamma 72.66(2) _cell_volume 717.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 24.3 _cell_measurement_theta_max 24.8 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_meas ? _chemical_formula_weight 340.01 _chemical_formula_analytical ? _chemical_formula_sum 'C9 H23 N5 O5 Ni ' _chemical_formula_moiety 'C9 H23 N5 O5 Ni ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 360.00 _exptl_absorpt_coefficient_mu 1.379 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.714 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device AFC7S _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.95 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -1 -2 1 0 -2 0 -1 -2 _diffrn_reflns_number 2686 _reflns_number_total 2516 _reflns_number_observed 2247 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.02 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.03837 _diffrn_orient_matrix_UB_12 0.03951 _diffrn_orient_matrix_UB_13 -0.11852 _diffrn_orient_matrix_UB_21 0.01713 _diffrn_orient_matrix_UB_22 0.08377 _diffrn_orient_matrix_UB_23 0.05412 _diffrn_orient_matrix_UB_31 0.10635 _diffrn_orient_matrix_UB_32 -0.02902 _diffrn_orient_matrix_UB_33 -0.02865 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 18 0.003 0.002 'International Tables' H 0 46 0.000 0.000 'International Tables' N 0 10 0.006 0.003 'International Tables' Ni 0 2 0.339 1.112 'International Tables' O 0 10 0.011 0.006 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ni(1) 0.61504(4) 0.35918(3) 0.78702(4) 0.02837(10) Uij ? ? O(1) 0.3108(2) 0.6886(2) 0.6635(3) 0.0450(6) Uij ? ? O(2) 0.1708(2) 0.4968(2) 0.7155(3) 0.0407(6) Uij ? ? O(3) 0.4007(4) 0.8975(3) 0.5882(5) 0.072(1) Uij ? ? O(4) 0.7122(4) 0.8927(3) 0.6306(5) 0.068(1) Uij ? ? O(5) 0.0513(3) 0.3129(2) 0.4852(4) 0.0565(8) Uij ? ? N(1) 0.8119(2) 0.3741(2) 0.7724(3) 0.0322(6) Uij ? ? N(2) 0.5392(2) 0.5312(2) 0.7427(3) 0.0308(6) Uij ? ? N(3) 0.4170(2) 0.3668(2) 0.7901(3) 0.0308(6) Uij ? ? N(4) 0.6657(2) 0.1798(2) 0.8308(3) 0.0324(6) Uij ? ? N(5) 0.9408(2) 0.1549(2) 0.8764(3) 0.0378(7) Uij ? ? C(1) 0.8038(3) 0.5135(3) 0.8078(4) 0.0353(8) Uij ? ? C(2) 0.6506(3) 0.5961(3) 0.7182(3) 0.0333(8) Uij ? ? C(3) 0.3895(3) 0.5788(3) 0.7120(3) 0.0311(7) Uij ? ? C(4) 0.3132(3) 0.4748(3) 0.7411(3) 0.0304(7) Uij ? ? C(5) 0.3884(3) 0.2452(3) 0.8172(4) 0.0364(8) Uij ? ? C(6) 0.5389(3) 0.1605(3) 0.9090(4) 0.0378(8) Uij ? ? C(7) 0.8186(3) 0.1276(3) 0.9419(4) 0.0392(8) Uij ? ? C(8) 0.9404(3) 0.2880(3) 0.8934(4) 0.0406(8) Uij ? ? C(9) 0.9797(3) 0.0858(3) 0.7099(4) 0.0512(10) Uij ? ? H(1) 0.8838 0.5309 0.7615 0.0424 Uij ? ? H(2) 0.8147 0.5335 0.9328 0.0424 Uij ? ? H(3) 0.6516 0.6007 0.5949 0.0400 Uij ? ? H(4) 0.6273 0.6812 0.7729 0.0400 Uij ? ? H(5) 0.3571 0.2051 0.7059 0.0437 Uij ? ? H(6) 0.3115 0.2603 0.8902 0.0437 Uij ? ? H(7) 0.5514 0.1840 1.0331 0.0454 Uij ? ? H(8) 0.5397 0.0720 0.8918 0.0454 Uij ? ? H(9) 0.8147 0.1652 1.0598 0.0471 Uij ? ? H(10) 0.8396 0.0362 0.9440 0.0471 Uij ? ? H(11) 0.9317 0.3190 1.0133 0.0488 Uij ? ? H(12) 1.0344 0.2929 0.8665 0.0488 Uij ? ? H(13) 0.9090 0.1278 0.6127 0.0615 Uij ? ? H(14) 1.0801 0.0852 0.6981 0.0615 Uij ? ? H(15) 0.9755 -0.0010 0.7100 0.0615 Uij ? ? H(16) 0.8299 0.3506 0.6532 0.0386 Uij ? ? H(17) 0.6673 0.1329 0.7184 0.0389 Uij ? ? H(18) 0.376(5) 0.852(4) 0.624(6) 0.10(2) Uij ? ? H(19) 0.480(5) 0.891(5) 0.628(6) 0.12(2) Uij ? ? H(20) 0.795(5) 0.822(4) 0.607(6) 0.13(2) Uij ? ? H(21) 0.705(5) 0.930(4) 0.572(5) 0.05(2) Uij ? ? H(22) 0.084(4) 0.363(3) 0.562(5) 0.08(1) Uij ? ? H(23) -0.019(4) 0.351(3) 0.417(5) 0.07(1) Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0212(2) 0.0269(2) 0.0370(2) -0.0058(1) 0.0030(1) 0.0070(1) O(1) 0.033(1) 0.030(1) 0.066(1) 0.0007(9) 0.0018(10) 0.0149(10) O(2) 0.0193(10) 0.045(1) 0.055(1) -0.0056(9) 0.0019(9) 0.0083(10) O(3) 0.068(2) 0.052(2) 0.103(2) -0.017(2) 0.014(2) 0.027(2) O(4) 0.068(2) 0.055(2) 0.074(2) -0.011(2) 0.004(2) 0.005(2) O(5) 0.051(2) 0.045(2) 0.066(2) -0.008(1) -0.008(1) 0.015(1) N(1) 0.026(1) 0.031(1) 0.038(1) -0.007(1) 0.0066(10) 0.002(1) N(2) 0.024(1) 0.027(1) 0.042(1) -0.0072(10) 0.0045(10) 0.0074(10) N(3) 0.023(1) 0.029(1) 0.041(1) -0.0078(10) 0.0028(10) 0.0088(10) N(4) 0.029(1) 0.030(1) 0.038(1) -0.0057(10) 0.0062(10) 0.0043(10) N(5) 0.027(1) 0.033(1) 0.048(1) -0.001(1) 0.006(1) 0.004(1) C(1) 0.028(1) 0.035(2) 0.047(2) -0.012(1) 0.009(1) 0.002(1) C(2) 0.035(2) 0.031(2) 0.036(2) -0.011(1) 0.009(1) 0.003(1) C(3) 0.032(1) 0.033(2) 0.028(1) -0.008(1) 0.004(1) 0.002(1) C(4) 0.028(1) 0.035(2) 0.028(1) -0.008(1) 0.004(1) 0.001(1) C(5) 0.033(2) 0.036(2) 0.044(2) -0.014(1) 0.008(1) 0.004(1) C(6) 0.037(2) 0.034(2) 0.047(2) -0.010(1) 0.012(1) 0.010(1) C(7) 0.033(2) 0.035(2) 0.044(2) 0.001(1) 0.004(1) 0.010(1) C(8) 0.024(1) 0.040(2) 0.053(2) -0.006(1) 0.000(1) 0.002(1) C(9) 0.046(2) 0.043(2) 0.063(2) -0.005(2) 0.018(2) -0.002(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2247 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0292 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0289 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.430 _refine_ls_shift/esd_max 0.0621 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.38 _refine_diff_density_max 0.70 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) N(1) 1.905(2) ? ? yes Ni(1) N(2) 1.825(2) ? ? yes Ni(1) N(3) 1.820(2) ? ? yes Ni(1) N(4) 1.905(2) ? ? yes O(1) O(3) 2.773(4) ? ? yes O(1) C(3) 1.247(3) ? ? yes O(2) O(5) 2.855(3) ? ? yes O(5) O(2) 2.794(3) 2_566 ? yes O(2) C(4) 1.253(3) ? ? yes O(3) O(4) 2.835(5) ? ? yes O(4) O(3) 2.786(5) 2_676 ? yes O(4) O(5) 2.815(4) 2_666 ? yes N(1) C(1) 1.485(3) ? ? yes N(1) C(8) 1.502(3) ? ? yes N(2) C(2) 1.458(3) ? ? yes N(2) C(3) 1.316(3) ? ? yes N(3) C(4) 1.311(3) ? ? yes N(3) C(5) 1.457(3) ? ? yes N(4) C(6) 1.487(3) ? ? yes N(4) C(7) 1.495(3) ? ? yes N(5) C(7) 1.435(3) ? ? yes N(5) C(8) 1.429(3) ? ? yes N(5) C(9) 1.454(4) ? ? yes C(1) C(2) 1.518(4) ? ? yes C(3) C(4) 1.549(4) ? ? yes C(5) C(6) 1.515(4) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ni(1) N(2) 87.43(9) ? ? ? yes N(1) Ni(1) N(3) 172.32(9) ? ? ? yes N(1) Ni(1) N(4) 100.38(9) ? ? ? yes N(2) Ni(1) N(3) 84.98(9) ? ? ? yes N(2) Ni(1) N(4) 172.13(9) ? ? ? yes N(3) Ni(1) N(4) 87.18(9) ? ? ? yes Ni(1) N(1) C(1) 106.7(2) ? ? ? yes Ni(1) N(1) C(8) 114.0(2) ? ? ? yes C(1) N(1) C(8) 112.4(2) ? ? ? yes Ni(1) N(2) C(2) 116.0(2) ? ? ? yes Ni(1) N(2) C(3) 116.9(2) ? ? ? yes C(2) N(2) C(3) 126.4(2) ? ? ? yes Ni(1) N(3) C(4) 116.8(2) ? ? ? yes Ni(1) N(3) C(5) 116.2(2) ? ? ? yes C(4) N(3) C(5) 126.2(2) ? ? ? yes Ni(1) N(4) C(6) 107.5(2) ? ? ? yes Ni(1) N(4) C(7) 114.4(2) ? ? ? yes C(6) N(4) C(7) 112.6(2) ? ? ? yes C(7) N(5) C(8) 115.5(2) ? ? ? yes C(7) N(5) C(9) 115.5(2) ? ? ? yes C(8) N(5) C(9) 115.6(2) ? ? ? yes N(1) C(1) C(2) 109.5(2) ? ? ? yes N(2) C(2) C(1) 105.5(2) ? ? ? yes O(1) C(3) N(2) 129.0(3) ? ? ? yes O(1) C(3) C(4) 121.0(2) ? ? ? yes N(2) C(3) C(4) 110.0(2) ? ? ? yes O(2) C(4) N(3) 127.7(3) ? ? ? yes O(2) C(4) C(3) 121.6(2) ? ? ? yes N(3) C(4) C(3) 110.7(2) ? ? ? yes N(3) C(5) C(6) 105.7(2) ? ? ? yes N(4) C(6) C(5) 108.9(2) ? ? ? yes N(4) C(7) N(5) 113.4(2) ? ? ? yes N(1) C(8) N(5) 113.7(2) ? ? ? yes #------------------------------------------------------------------------------ _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ;