Supplementary Material (ESI) for Journal of Materials Chemistry This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Allen, Stephen' 'Bickley, Jamie F.' 'Blyr, Alexandra' 'Davies, Hywel O.' 'Garcia, Joanne' 'Impey, Susan' 'Jones, Anthony C.' 'Leedham, Timothy J.' 'Rougier, Aline' 'Steiner, Alexander' 'Williams, P.' _publ_contact_author_name 'Prof Anthony C Jones' _publ_contact_author_address ; Department of Chemistry University of Liverpool Liverpool L69 7ZD UNITED KINGDOM ; _publ_contact_author_email 'TONY@TJCONSULTANCY.DEMON.CO.UK' _publ_section_title ; Synthesis and Crystal Structures of Dimethylaminoethanol Adducts of Ni (II) Acetate and Ni (II) Acetylacetonate. Precursors for the Sol-Gel Deposition of Electrochromic Nickel Oxide Thin Films ; data_tony25 _database_code_CSD 156618 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H25 N Ni O5' _chemical_formula_weight 346.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 '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' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.2850 1.1130 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.737(8) _cell_length_b 10.309(7) _cell_length_c 11.812(8) _cell_angle_alpha 105.97(8) _cell_angle_beta 104.33(11) _cell_angle_gamma 97.56(11) _cell_volume 857.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 1.15 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe IPDS' _diffrn_measurement_method 'image plate' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5380 _diffrn_reflns_av_R_equivalents 0.0851 _diffrn_reflns_av_sigmaI/netI 0.0940 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 24.25 _reflns_number_total 2519 _reflns_number_gt 1798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _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 w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2519 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.1023(7) -0.2381(6) 0.2176(5) 0.0536(14) Uani 1 d . . . H1A H 0.9871 -0.2932 0.1591 0.064 Uiso 1 calc R . . H1B H 1.1037 -0.2375 0.3001 0.064 Uiso 1 calc R . . H1C H 1.2018 -0.2775 0.1964 0.064 Uiso 1 calc R . . C2 C 1.1270(7) -0.1004(6) 0.0861(4) 0.0487(13) Uani 1 d . . . H2A H 1.0131 -0.1566 0.0267 0.058 Uiso 1 calc R . . H2B H 1.2280 -0.1397 0.0678 0.058 Uiso 1 calc R . . H2C H 1.1416 -0.0072 0.0815 0.058 Uiso 1 calc R . . C3 C 1.2995(6) -0.0101(5) 0.3018(4) 0.0410(12) Uani 1 d . . . H3A H 1.3271 0.0759 0.2833 0.049 Uiso 1 calc R . . H3B H 1.3980 -0.0593 0.2932 0.049 Uiso 1 calc R . . C4 C 1.2900(6) 0.0230(6) 0.4326(4) 0.0436(13) Uani 1 d . . . H4A H 1.2763 -0.0615 0.4553 0.052 Uiso 1 calc R . . H4B H 1.4019 0.0873 0.4899 0.052 Uiso 1 calc R . . C5 C 1.1385(8) 0.3996(6) 0.2274(5) 0.0604(15) Uani 1 d . . . H5A H 1.1205 0.4916 0.2631 0.073 Uiso 1 calc R . . H5B H 1.1010 0.3751 0.1382 0.073 Uiso 1 calc R . . H5C H 1.2665 0.3977 0.2567 0.073 Uiso 1 calc R . . C6 C 1.0247(6) 0.2967(5) 0.2653(4) 0.0365(11) Uani 1 d . . . C7 C 0.9166(6) 0.3454(5) 0.3391(4) 0.0422(11) Uani 1 d . . . H7 H 0.9255 0.4413 0.3678 0.051 Uiso 1 calc R . . C8 C 0.7953(6) 0.2609(5) 0.3736(4) 0.0384(11) Uani 1 d . . . C9 C 0.6748(6) 0.3320(6) 0.4431(4) 0.0476(12) Uani 1 d . . . H9A H 0.7042 0.4305 0.4563 0.057 Uiso 1 calc R . . H9B H 0.6957 0.3161 0.5222 0.057 Uiso 1 calc R . . H9C H 0.5476 0.2949 0.3953 0.057 Uiso 1 calc R . . C10 C 0.4993(6) -0.2102(6) -0.0717(4) 0.0524(14) Uani 1 d . . . H10A H 0.4155 -0.2982 -0.0944 0.063 Uiso 1 calc R . . H10B H 0.5755 -0.2168 -0.1262 0.063 Uiso 1 calc R . . H10C H 0.4306 -0.1391 -0.0790 0.063 Uiso 1 calc R . . C11 C 0.6186(6) -0.1734(5) 0.0603(4) 0.0364(11) Uani 1 d . . . C12 C 0.5899(6) -0.2688(5) 0.1239(4) 0.0410(11) Uani 1 d . . . H12 H 0.5022 -0.3512 0.0801 0.049 Uiso 1 calc R . . C13 C 0.6822(6) -0.2491(5) 0.2464(4) 0.0379(11) Uani 1 d . . . C14 C 0.6325(7) -0.3594(5) 0.3021(5) 0.0513(14) Uani 1 d . . . H14A H 0.5355 -0.4329 0.2409 0.062 Uiso 1 calc R . . H14B H 0.5915 -0.3193 0.3726 0.062 Uiso 1 calc R . . H14C H 0.7388 -0.3965 0.3284 0.062 Uiso 1 calc R . . O1 O 1.1359(4) 0.0840(4) 0.4376(3) 0.0388(8) Uani 1 d . . . H1 H 1.1345 0.1123 0.5103 0.058 Uiso 1 calc R . . O2 O 1.0373(4) 0.1728(4) 0.2242(3) 0.0380(8) Uani 1 d . . . O3 O 0.7707(4) 0.1321(3) 0.3504(3) 0.0386(8) Uani 1 d . . . O4 O 0.8099(4) -0.1455(3) 0.3185(3) 0.0353(7) Uani 1 d . . . O5 O 0.7341(4) -0.0619(3) 0.1027(3) 0.0381(8) Uani 1 d . . . N1 N 1.1241(5) -0.0966(4) 0.2132(3) 0.0362(9) Uani 1 d . . . Ni1 Ni 0.92312(7) 0.01337(6) 0.26945(5) 0.0329(2) Uani 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 C1 0.059(3) 0.054(4) 0.065(4) 0.028(3) 0.033(3) 0.022(3) C2 0.058(3) 0.065(4) 0.034(3) 0.019(3) 0.022(2) 0.025(3) C3 0.041(2) 0.051(3) 0.036(2) 0.017(2) 0.015(2) 0.015(2) C4 0.036(2) 0.065(4) 0.034(2) 0.021(3) 0.0094(19) 0.012(2) C5 0.085(4) 0.046(3) 0.061(3) 0.023(3) 0.040(3) 0.005(3) C6 0.049(3) 0.029(3) 0.031(2) 0.010(2) 0.012(2) 0.007(2) C7 0.050(3) 0.036(3) 0.041(3) 0.012(2) 0.017(2) 0.006(2) C8 0.041(2) 0.038(3) 0.034(2) 0.010(2) 0.0074(19) 0.011(2) C9 0.056(3) 0.049(3) 0.042(3) 0.013(3) 0.021(2) 0.015(3) C10 0.048(3) 0.064(4) 0.036(3) 0.009(3) 0.007(2) 0.009(3) C11 0.039(2) 0.043(3) 0.029(2) 0.008(2) 0.0144(19) 0.015(2) C12 0.043(2) 0.038(3) 0.039(3) 0.009(2) 0.010(2) 0.008(2) C13 0.039(2) 0.036(3) 0.046(3) 0.015(2) 0.020(2) 0.013(2) C14 0.061(3) 0.042(3) 0.054(3) 0.025(3) 0.017(2) -0.002(3) O1 0.0402(16) 0.053(2) 0.0275(15) 0.0149(16) 0.0126(13) 0.0146(15) O2 0.0483(17) 0.042(2) 0.0327(16) 0.0176(16) 0.0182(14) 0.0147(16) O3 0.0460(17) 0.040(2) 0.0397(17) 0.0193(16) 0.0197(14) 0.0140(15) O4 0.0393(16) 0.037(2) 0.0317(16) 0.0149(15) 0.0112(13) 0.0076(15) O5 0.0423(17) 0.044(2) 0.0308(16) 0.0163(16) 0.0106(14) 0.0088(16) N1 0.046(2) 0.040(3) 0.0331(19) 0.0206(19) 0.0182(16) 0.0128(18) Ni1 0.0404(3) 0.0363(4) 0.0273(3) 0.0161(3) 0.0122(2) 0.0095(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 C1 N1 1.463(6) . ? C2 N1 1.496(5) . ? C3 N1 1.482(6) . ? C3 C4 1.510(6) . ? C4 O1 1.426(6) . ? C5 C6 1.520(6) . ? C6 O2 1.262(6) . ? C6 C7 1.393(6) . ? C7 C8 1.406(6) . ? C8 O3 1.258(6) . ? C8 C9 1.519(7) . ? C10 C11 1.516(6) . ? C11 O5 1.250(6) . ? C11 C12 1.419(7) . ? C12 C13 1.390(6) . ? C13 O4 1.285(6) . ? C13 C14 1.514(6) . ? O2 Ni1 2.026(3) . ? O3 Ni1 2.024(4) . ? O4 Ni1 2.045(3) . ? O5 Ni1 2.013(4) . ? N1 Ni1 2.169(4) . ? 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 C3 C4 110.8(3) . . ? O1 C4 C3 107.2(4) . . ? O2 C6 C7 126.3(4) . . ? O2 C6 C5 115.2(4) . . ? C7 C6 C5 118.5(4) . . ? C6 C7 C8 124.5(5) . . ? O3 C8 C7 127.5(4) . . ? O3 C8 C9 115.9(4) . . ? C7 C8 C9 116.6(5) . . ? O5 C11 C12 126.0(4) . . ? O5 C11 C10 116.8(4) . . ? C12 C11 C10 117.2(4) . . ? C13 C12 C11 124.8(4) . . ? O4 C13 C12 126.0(4) . . ? O4 C13 C14 115.5(4) . . ? C12 C13 C14 118.4(4) . . ? C6 O2 Ni1 125.3(3) . . ? C8 O3 Ni1 124.2(3) . . ? C13 O4 Ni1 125.6(3) . . ? C11 O5 Ni1 127.4(3) . . ? C1 N1 C3 110.5(4) . . ? C1 N1 C2 108.3(4) . . ? C3 N1 C2 108.3(3) . . ? C1 N1 Ni1 114.8(3) . . ? C3 N1 Ni1 103.2(3) . . ? C2 N1 Ni1 111.6(3) . . ? O5 Ni1 O3 95.01(15) . . ? O5 Ni1 O2 91.33(16) . . ? O3 Ni1 O2 90.65(14) . . ? O5 Ni1 O4 89.65(16) . . ? O3 Ni1 O4 88.87(14) . . ? O2 Ni1 O4 178.94(13) . . ? O5 Ni1 N1 95.04(16) . . ? O3 Ni1 N1 169.90(13) . . ? O2 Ni1 N1 88.07(15) . . ? O4 Ni1 N1 92.24(14) . . ? 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 C3 C4 O1 -54.5(5) . . . . ? O2 C6 C7 C8 -3.9(7) . . . . ? C5 C6 C7 C8 175.3(4) . . . . ? C6 C7 C8 O3 4.0(8) . . . . ? C6 C7 C8 C9 -173.7(4) . . . . ? O5 C11 C12 C13 2.9(8) . . . . ? C10 C11 C12 C13 -177.5(4) . . . . ? C11 C12 C13 O4 -2.5(7) . . . . ? C11 C12 C13 C14 178.5(4) . . . . ? C7 C6 O2 Ni1 -6.8(6) . . . . ? C5 C6 O2 Ni1 174.0(3) . . . . ? C7 C8 O3 Ni1 6.6(6) . . . . ? C9 C8 O3 Ni1 -175.7(3) . . . . ? C12 C13 O4 Ni1 -4.0(6) . . . . ? C14 C13 O4 Ni1 175.1(3) . . . . ? C12 C11 O5 Ni1 3.4(7) . . . . ? C10 C11 O5 Ni1 -176.2(3) . . . . ? C4 C3 N1 C1 -73.7(5) . . . . ? C4 C3 N1 C2 167.9(4) . . . . ? C4 C3 N1 Ni1 49.5(4) . . . . ? C11 O5 Ni1 O3 -95.6(4) . . . . ? C11 O5 Ni1 O2 173.6(4) . . . . ? C11 O5 Ni1 O4 -6.8(4) . . . . ? C11 O5 Ni1 N1 85.4(4) . . . . ? C8 O3 Ni1 O5 -103.3(4) . . . . ? C8 O3 Ni1 O2 -11.9(3) . . . . ? C8 O3 Ni1 O4 167.2(3) . . . . ? C8 O3 Ni1 N1 70.7(8) . . . . ? C6 O2 Ni1 O5 107.1(3) . . . . ? C6 O2 Ni1 O3 12.1(3) . . . . ? C6 O2 Ni1 O4 -51(7) . . . . ? C6 O2 Ni1 N1 -157.9(3) . . . . ? C13 O4 Ni1 O5 7.0(3) . . . . ? C13 O4 Ni1 O3 102.1(4) . . . . ? C13 O4 Ni1 O2 165(7) . . . . ? C13 O4 Ni1 N1 -88.0(4) . . . . ? C1 N1 Ni1 O5 -84.7(3) . . . . ? C3 N1 Ni1 O5 154.9(2) . . . . ? C2 N1 Ni1 O5 38.9(3) . . . . ? C1 N1 Ni1 O3 101.2(8) . . . . ? C3 N1 Ni1 O3 -19.1(8) . . . . ? C2 N1 Ni1 O3 -135.1(7) . . . . ? C1 N1 Ni1 O2 -175.9(3) . . . . ? C3 N1 Ni1 O2 63.8(3) . . . . ? C2 N1 Ni1 O2 -52.3(3) . . . . ? C1 N1 Ni1 O4 5.1(3) . . . . ? C3 N1 Ni1 O4 -115.2(3) . . . . ? C2 N1 Ni1 O4 128.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 24.25 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.538 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.082 data_tony36 _database_code_CSD 156619 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 N2 Ni O6' _chemical_formula_weight 355.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 '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' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.2850 1.1130 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2993(14) _cell_length_b 8.5256(14) _cell_length_c 13.017(2) _cell_angle_alpha 95.917(19) _cell_angle_beta 95.92(2) _cell_angle_gamma 109.469(19) _cell_volume 854.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 380 _exptl_absorpt_coefficient_mu 1.161 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe IPDS' _diffrn_measurement_method 'Image plate' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5492 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 24.21 _reflns_number_total 2544 _reflns_number_gt 1936 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _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 w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2544 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2855(4) 0.3639(4) 0.0660(3) 0.0436(9) Uani 1 d . . . H1A H 0.2165 0.4007 0.0145 0.052 Uiso 1 calc R . . H1B H 0.3728 0.3338 0.0315 0.052 Uiso 1 calc R . . C2 C 0.3733(4) 0.5053(4) 0.1547(3) 0.0401(8) Uani 1 d . . . H2A H 0.4539 0.4736 0.2014 0.048 Uiso 1 calc R . . H2B H 0.4397 0.6059 0.1269 0.048 Uiso 1 calc R . . C3 C 0.3324(5) 0.6354(4) 0.3185(3) 0.0472(9) Uani 1 d . . . H3A H 0.3838 0.5667 0.3556 0.057 Uiso 1 calc R . . H3B H 0.2481 0.6604 0.3574 0.057 Uiso 1 calc R . . H3C H 0.4218 0.7396 0.3112 0.057 Uiso 1 calc R . . C4 C 0.1702(4) 0.6517(4) 0.1604(3) 0.0411(8) Uani 1 d . . . H4A H 0.0865 0.6759 0.2002 0.049 Uiso 1 calc R . . H4B H 0.1133 0.5946 0.0912 0.049 Uiso 1 calc R . . H4C H 0.2607 0.7561 0.1547 0.049 Uiso 1 calc R . . C5 C -0.2533(4) 0.1583(4) 0.0730(3) 0.0418(8) Uani 1 d . . . H5A H -0.2097 0.0936 0.0233 0.050 Uiso 1 calc R . . H5B H -0.3589 0.1680 0.0376 0.050 Uiso 1 calc R . . C6 C -0.2939(4) 0.0679(4) 0.1651(3) 0.0397(8) Uani 1 d . . . H6A H -0.3491 0.1260 0.2111 0.048 Uiso 1 calc R . . H6B H -0.3747 -0.0468 0.1412 0.048 Uiso 1 calc R . . C7 C -0.1619(5) 0.0306(5) 0.3304(3) 0.0470(9) Uani 1 d . . . H7A H -0.1925 0.1205 0.3655 0.056 Uiso 1 calc R . . H7B H -0.0568 0.0265 0.3684 0.056 Uiso 1 calc R . . H7C H -0.2548 -0.0758 0.3279 0.056 Uiso 1 calc R . . C8 C -0.0878(4) -0.0760(4) 0.1724(3) 0.0433(9) Uani 1 d . . . H8A H 0.0171 -0.0794 0.2111 0.052 Uiso 1 calc R . . H8B H -0.0692 -0.0577 0.1016 0.052 Uiso 1 calc R . . H8C H -0.1809 -0.1819 0.1709 0.052 Uiso 1 calc R . . C9 C 0.3215(4) 0.1740(4) 0.3228(3) 0.0337(8) Uani 1 d . . . C10 C 0.4068(6) 0.1370(6) 0.4205(3) 0.0642(12) Uani 1 d . . . H10A H 0.4809 0.0746 0.4020 0.077 Uiso 1 calc R . . H10B H 0.3190 0.0706 0.4577 0.077 Uiso 1 calc R . . H10C H 0.4754 0.2417 0.4647 0.077 Uiso 1 calc R . . C11 C -0.1535(4) 0.4867(4) 0.3231(3) 0.0326(7) Uani 1 d . . . C12 C -0.1884(6) 0.5746(6) 0.4195(3) 0.0615(12) Uani 1 d . . . H12A H -0.2740 0.6251 0.4004 0.074 Uiso 1 calc R . . H12B H -0.0824 0.6615 0.4539 0.074 Uiso 1 calc R . . H12C H -0.2315 0.4940 0.4664 0.074 Uiso 1 calc R . . N1 N 0.2461(3) 0.5433(3) 0.21378(19) 0.0284(6) Uani 1 d . . . N2 N -0.1339(3) 0.0620(3) 0.22357(19) 0.0290(6) Uani 1 d . . . O1 O 0.1761(3) 0.2204(3) 0.10412(16) 0.0321(5) Uani 1 d . . . H1 H 0.2364 0.1808 0.1409 0.048 Uiso 1 calc R . . O2 O -0.1267(2) 0.3224(3) 0.10546(16) 0.0310(5) Uani 1 d . . . H2 H -0.1669 0.3799 0.1434 0.046 Uiso 1 calc R . . O3 O 0.3523(3) 0.1186(3) 0.23721(18) 0.0428(6) Uani 1 d . . . O4 O 0.2205(3) 0.2551(3) 0.33483(15) 0.0311(5) Uani 1 d . . . O5 O -0.0442(3) 0.4141(3) 0.33457(16) 0.0320(5) Uani 1 d . . . O6 O -0.2330(3) 0.4923(3) 0.23641(18) 0.0417(6) Uani 1 d . . . Ni1 Ni 0.05745(5) 0.30424(5) 0.22361(3) 0.02292(13) Uani 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 C1 0.044(2) 0.046(2) 0.0404(19) 0.0090(17) 0.0214(16) 0.0096(17) C2 0.0280(17) 0.042(2) 0.048(2) 0.0076(17) 0.0084(15) 0.0071(15) C3 0.044(2) 0.039(2) 0.043(2) -0.0026(17) -0.0064(16) 0.0003(16) C4 0.0392(19) 0.0305(19) 0.055(2) 0.0155(17) 0.0068(16) 0.0107(15) C5 0.0343(18) 0.040(2) 0.0403(19) 0.0048(16) -0.0107(14) 0.0047(15) C6 0.0228(16) 0.0357(19) 0.055(2) 0.0061(17) 0.0001(15) 0.0047(14) C7 0.046(2) 0.051(2) 0.040(2) 0.0183(18) 0.0118(16) 0.0054(18) C8 0.0369(19) 0.0256(18) 0.064(2) 0.0031(17) 0.0038(17) 0.0091(15) C9 0.0276(16) 0.0331(18) 0.0425(19) 0.0045(15) 0.0022(14) 0.0146(14) C10 0.070(3) 0.087(3) 0.055(2) 0.011(2) -0.005(2) 0.056(3) C11 0.0289(17) 0.0304(18) 0.0441(19) 0.0104(15) 0.0099(14) 0.0148(14) C12 0.073(3) 0.083(3) 0.051(2) 0.007(2) 0.014(2) 0.056(3) N1 0.0231(13) 0.0283(14) 0.0307(13) 0.0033(12) 0.0007(10) 0.0063(11) N2 0.0245(13) 0.0286(14) 0.0336(14) 0.0073(12) 0.0049(11) 0.0081(11) O1 0.0332(12) 0.0331(13) 0.0302(12) 0.0031(10) 0.0077(9) 0.0111(10) O2 0.0286(11) 0.0308(12) 0.0304(12) 0.0050(10) -0.0012(9) 0.0078(9) O3 0.0382(13) 0.0509(16) 0.0485(14) 0.0025(12) 0.0084(11) 0.0284(12) O4 0.0322(12) 0.0384(13) 0.0287(11) 0.0048(10) 0.0020(9) 0.0211(10) O5 0.0324(12) 0.0400(13) 0.0313(11) 0.0069(10) 0.0049(9) 0.0220(10) O6 0.0382(13) 0.0502(16) 0.0449(14) 0.0084(12) 0.0004(10) 0.0271(11) Ni1 0.0199(2) 0.0250(2) 0.0244(2) 0.00449(15) 0.00195(13) 0.00874(15) _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 C1 O1 1.430(4) . ? C1 C2 1.507(5) . ? C2 N1 1.467(4) . ? C3 N1 1.480(4) . ? C4 N1 1.471(4) . ? C5 O2 1.431(4) . ? C5 C6 1.499(5) . ? C6 N2 1.480(4) . ? C7 N2 1.471(4) . ? C8 N2 1.471(4) . ? C9 O3 1.249(4) . ? C9 O4 1.263(4) . ? C9 C10 1.504(5) . ? C11 O6 1.260(4) . ? C11 O5 1.263(4) . ? C11 C12 1.498(5) . ? N1 Ni1 2.142(3) . ? N2 Ni1 2.145(3) . ? O4 Ni1 2.050(2) . ? O5 Ni1 2.043(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 O1 C1 C2 110.3(3) . . ? N1 C2 C1 110.9(3) . . ? O2 C5 C6 110.6(3) . . ? N2 C6 C5 110.3(2) . . ? O3 C9 O4 125.7(3) . . ? O3 C9 C10 117.7(3) . . ? O4 C9 C10 116.6(3) . . ? O6 C11 O5 124.6(3) . . ? O6 C11 C12 118.0(3) . . ? O5 C11 C12 117.4(3) . . ? C2 N1 C4 110.3(3) . . ? C2 N1 C3 109.6(2) . . ? C4 N1 C3 107.7(3) . . ? C2 N1 Ni1 105.47(19) . . ? C4 N1 Ni1 112.24(18) . . ? C3 N1 Ni1 111.5(2) . . ? C7 N2 C8 108.3(3) . . ? C7 N2 C6 109.7(2) . . ? C8 N2 C6 109.8(2) . . ? C7 N2 Ni1 111.24(19) . . ? C8 N2 Ni1 112.60(19) . . ? C6 N2 Ni1 105.2(2) . . ? C9 O4 Ni1 128.7(2) . . ? C11 O5 Ni1 129.2(2) . . ? O5 Ni1 O4 91.87(8) . . ? O5 Ni1 N1 90.64(9) . . ? O4 Ni1 N1 91.91(9) . . ? O5 Ni1 N2 91.78(9) . . ? O4 Ni1 N2 90.38(9) . . ? N1 Ni1 N2 176.61(10) . . ? 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 O1 C1 C2 N1 -54.2(4) . . . . ? O2 C5 C6 N2 -55.5(4) . . . . ? C1 C2 N1 C4 -81.4(3) . . . . ? C1 C2 N1 C3 160.2(3) . . . . ? C1 C2 N1 Ni1 40.0(3) . . . . ? C5 C6 N2 C7 159.7(3) . . . . ? C5 C6 N2 C8 -81.4(3) . . . . ? C5 C6 N2 Ni1 40.0(3) . . . . ? O3 C9 O4 Ni1 6.4(5) . . . . ? C10 C9 O4 Ni1 -171.4(3) . . . . ? O6 C11 O5 Ni1 6.3(5) . . . . ? C12 C11 O5 Ni1 -172.7(2) . . . . ? C11 O5 Ni1 O4 175.8(3) . . . . ? C11 O5 Ni1 N1 83.8(3) . . . . ? C11 O5 Ni1 N2 -93.8(3) . . . . ? C9 O4 Ni1 O5 174.7(3) . . . . ? C9 O4 Ni1 N1 -94.6(3) . . . . ? C9 O4 Ni1 N2 82.9(3) . . . . ? C2 N1 Ni1 O5 167.17(19) . . . . ? C4 N1 Ni1 O5 -72.7(2) . . . . ? C3 N1 Ni1 O5 48.2(2) . . . . ? C2 N1 Ni1 O4 75.28(19) . . . . ? C4 N1 Ni1 O4 -164.6(2) . . . . ? C3 N1 Ni1 O4 -43.7(2) . . . . ? C2 N1 Ni1 N2 -57.2(18) . . . . ? C4 N1 Ni1 N2 63.0(18) . . . . ? C3 N1 Ni1 N2 -176.1(16) . . . . ? C7 N2 Ni1 O5 -43.0(2) . . . . ? C8 N2 Ni1 O5 -164.7(2) . . . . ? C6 N2 Ni1 O5 75.72(19) . . . . ? C7 N2 Ni1 O4 48.9(2) . . . . ? C8 N2 Ni1 O4 -72.8(2) . . . . ? C6 N2 Ni1 O4 167.61(19) . . . . ? C7 N2 Ni1 N1 -178.6(16) . . . . ? C8 N2 Ni1 N1 59.6(18) . . . . ? C6 N2 Ni1 N1 -59.9(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O3 0.83 1.73 2.554(3) 169.2 . O2 H2 O6 0.83 1.71 2.536(3) 171.8 . _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 24.21 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.323 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.077