#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/33/2013315.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2013315 loop_ _publ_author_name 'Okabe, Nobuo' 'Muranishi, Yasunori' _publ_section_title ; Cobalt(II) and nickel(II) complexes of quinoline-2-carboxylate ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m228 _journal_page_last m230 _journal_paper_doi 10.1107/S0108270103008722 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Ni (C10 H6 N O2)2 (H2 O)2], 2C H4 O, 2H2 O' _chemical_formula_moiety 'C20 H16 N2 Ni O6, 2C H4 O, 2H2 O' _chemical_formula_sum 'C22 H28 N2 Ni O10' _chemical_formula_weight 539.15 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 76.74(2) _cell_angle_beta 74.390(10) _cell_angle_gamma 70.66(2) _cell_formula_units_Z 1 _cell_length_a 7.127(2) _cell_length_b 8.909(3) _cell_length_c 10.769(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 296.2 _cell_measurement_theta_max 14.9 _cell_measurement_theta_min 13.9 _cell_volume 613.9(3) _computing_cell_refinement 'MSC/AFC MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992) ; _computing_data_reduction 'TEXSAN (Molecular Structure & Rigaku, 2000)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material TEXSAN _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999) and DIRDIF94 (Beurskens et al., 1994)' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku AFC-5R' _diffrn_measurement_method \w-2\q _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 3003 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_standards_decay_% 5.47 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_T_max 0.919 _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour light-blue _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 282.0 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.44 _refine_diff_density_min -0.62 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment mixed _refine_ls_number_parameters 162 _refine_ls_number_reflns 2823 _refine_ls_R_factor_gt 0.0378 _refine_ls_shift/su_max -0.0020 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0624P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1111 _reflns_number_gt 2234 _reflns_number_total 2823 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ln1166.cif _cod_data_source_block II _cod_database_code 2013315 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ni1 0.5000 0.0000 1.0000 0.02890(10) Uani d S 1.00 . . Ni O1 0.7007(3) -0.0399(2) 1.1116(2) 0.0366(4) Uani d . 1.00 . . O O1M 0.1894(4) 0.1182(4) 0.5973(2) 0.0723(7) Uani d . 1.00 . . O O1W 0.7273(3) -0.1077(2) 0.8523(2) 0.0379(4) Uani d . 1.00 . . O O2 0.9096(3) 0.0582(2) 1.1655(2) 0.0444(4) Uani d . 1.00 . . O O2W 0.6249(4) 0.0356(3) 0.6180(2) 0.0677(6) Uani d . 1.00 . . O N1 0.5945(3) 0.2197(2) 0.9367(2) 0.0296(4) Uani d . 1.00 . . N C1 0.7352(3) 0.2131(3) 0.9980(2) 0.0316(5) Uani d . 1.00 . . C C2 0.8300(4) 0.3351(3) 0.9756(3) 0.0429(6) Uani d . 1.00 . . C C3 0.7745(4) 0.4684(3) 0.8861(3) 0.0471(6) Uani d . 1.00 . . C C4 0.6265(4) 0.4806(3) 0.8181(3) 0.0393(5) Uani d . 1.00 . . C C5 0.5616(5) 0.6161(3) 0.7244(3) 0.0535(7) Uani d . 1.00 . . C C6 0.4184(6) 0.6233(4) 0.6608(3) 0.0646(9) Uani d . 1.00 . . C C7 0.3303(6) 0.4961(4) 0.6888(3) 0.0631(9) Uani d . 1.00 . . C C8 0.3860(5) 0.3643(3) 0.7796(3) 0.0486(6) Uani d . 1.00 . . C C9 0.5374(4) 0.3522(3) 0.8456(2) 0.0339(5) Uani d . 1.00 . . C C10 0.7869(3) 0.0667(3) 1.0991(2) 0.0315(5) Uani d . 1.00 . . C C11 0.0245(7) 0.2483(6) 0.5724(5) 0.098(2) Uani d . 1.00 . . C H1A 0.6925 -0.0612 0.7755 0.0602 Uiso calc . 1.00 . . H H1B 0.8477 -0.0975 0.8562 0.0602 Uiso calc . 1.00 . . H H1M 0.1565 0.0643 0.6677 0.1085 Uiso calc . 1.00 . . H H2 0.9288 0.3252 1.0208 0.0515 Uiso calc . 1.00 . . H H2A 0.6886 0.0064 0.5396 0.0826 Uiso calc . 1.00 . . H H2B 0.4915 0.0710 0.6299 0.0826 Uiso calc . 1.00 . . H H3 0.8346 0.5508 0.8704 0.0565 Uiso calc . 1.00 . . H H5 0.6182 0.7010 0.7066 0.0642 Uiso calc . 1.00 . . H H6 0.3782 0.7120 0.5987 0.0775 Uiso calc . 1.00 . . H H7 0.2321 0.5018 0.6445 0.0758 Uiso calc . 1.00 . . H H8 0.3239 0.2826 0.7979 0.0583 Uiso calc . 1.00 . . H H11A -0.0964 0.2139 0.5964 0.1477 Uiso calc . 1.00 . . H H11B 0.0474 0.2913 0.4811 0.1477 Uiso calc . 1.00 . . H H11C 0.0082 0.3299 0.6224 0.1477 Uiso calc . 1.00 . . H 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 Ni1 0.0323(2) 0.0239(2) 0.0336(2) -0.0128(2) -0.0113(2) 0.0016(2) O1 0.0427(9) 0.0314(8) 0.0418(9) -0.0187(7) -0.0188(7) 0.0064(7) O1M 0.0630(10) 0.091(2) 0.0450(10) -0.0090(10) -0.0070(10) 0.0000(10) O1W 0.0384(9) 0.0385(9) 0.0416(9) -0.0173(7) -0.0090(7) -0.0052(7) O2 0.0422(10) 0.0520(10) 0.0470(10) -0.0221(8) -0.0173(8) -0.0012(8) O2W 0.0610(10) 0.083(2) 0.0500(10) -0.0080(10) -0.0120(10) -0.0120(10) N1 0.0334(9) 0.0237(9) 0.0316(9) -0.0115(7) -0.0043(7) -0.0022(7) C1 0.0340(10) 0.0260(10) 0.0360(10) -0.0114(9) -0.0034(9) -0.0053(9) C2 0.0450(10) 0.0380(10) 0.055(2) -0.0240(10) -0.0100(10) -0.0070(10) C3 0.053(2) 0.0330(10) 0.058(2) -0.0250(10) -0.0020(10) -0.0050(10) C4 0.0470(10) 0.0250(10) 0.0420(10) -0.0144(10) 0.0020(10) -0.0036(9) C5 0.070(2) 0.0280(10) 0.056(2) -0.0210(10) -0.0070(10) 0.0060(10) C6 0.093(3) 0.0330(10) 0.059(2) -0.019(2) -0.025(2) 0.0190(10) C7 0.084(2) 0.043(2) 0.066(2) -0.022(2) -0.039(2) 0.0180(10) C8 0.065(2) 0.0340(10) 0.052(2) -0.0200(10) -0.0240(10) 0.0080(10) C9 0.0410(10) 0.0220(10) 0.0350(10) -0.0098(9) -0.0028(9) -0.0014(9) C10 0.0280(10) 0.0330(10) 0.0340(10) -0.0104(9) -0.0054(9) -0.0057(9) C11 0.082(3) 0.082(3) 0.094(3) 0.003(2) -0.004(2) 0.003(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Ni1 O1 2_657 180.0 no O1 Ni1 O1W . 91.65(7) yes O1 Ni1 O1W 2_657 88.35(7) no O1 Ni1 N1 . 78.83(8) yes O1 Ni1 N1 2_657 101.17(8) no O1W Ni1 O1W 2_657 180.0 no O1W Ni1 N1 . 90.20(7) yes O1W Ni1 N1 2_657 89.80(7) no N1 Ni1 N1 2_657 180.0 no Ni1 O1 C10 . 117.90(10) no C11 O1M H1M . 109.5 no Ni1 O1W H1A . 108.5 no Ni1 O1W H1B . 109.2 no H1A O1W H1B . 112.2 no H2A O2W H2B . 114.7 no Ni1 N1 C1 . 110.00(10) no Ni1 N1 C9 . 131.3(2) no C1 N1 C9 . 118.6(2) no N1 C1 C2 . 123.5(2) no N1 C1 C10 . 116.0(2) no C2 C1 C10 . 120.4(3) no C1 C2 C3 . 118.7(3) no C1 C2 H2 . 120.6 no C3 C2 H2 . 120.6 no C2 C3 C4 . 119.8(3) no C2 C3 H3 . 120.1 no C4 C3 H3 . 120.1 no C3 C4 C5 . 122.5(3) no C3 C4 C9 . 118.3(2) no C5 C4 C9 . 119.2(3) no C4 C5 C6 . 120.7(3) no C4 C5 H5 . 119.6 no C6 C5 H5 . 119.6 no C5 C6 C7 . 119.8(3) no C5 C6 H6 . 120.1 no C7 C6 H6 . 120.1 no C6 C7 C8 . 121.4(4) no C6 C7 H7 . 119.3 no C8 C7 H7 . 119.3 no C7 C8 C9 . 120.0(3) no C7 C8 H8 . 120.0 no C9 C8 H8 . 120.0 no N1 C9 C4 . 121.0(3) no N1 C9 C8 . 120.2(2) no C4 C9 C8 . 118.8(2) no O1 C10 O2 . 123.9(2) no O1 C10 C1 . 117.1(2) no O2 C10 C1 . 119.0(2) no O1M C11 H11A . 109.5 no O1M C11 H11B . 109.5 no O1M C11 H11C . 109.5 no H11A C11 H11B . 109.5 no H11A C11 H11C . 109.5 no H11B C11 H11C . 109.5 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 O1 . . 2.003(2) yes Ni1 O1W . . 2.088(2) yes Ni1 N1 . . 2.182(2) yes O1 C10 . . 1.257(4) no O1M C11 . . 1.387(5) no O1M H1M . . 0.820 no O1W H1A . . 0.896 no O1W H1B . . 0.905 no O2 C10 . . 1.245(4) no O2W H2A . . 0.896 no O2W H2B . . 0.880 no N1 C1 . . 1.321(4) no N1 C9 . . 1.373(3) no C1 C2 . . 1.406(4) no C1 C10 . . 1.506(3) no C2 C3 . . 1.365(4) no C2 H2 . . 0.930 no C3 C4 . . 1.401(5) no C3 H3 . . 0.930 no C4 C5 . . 1.418(4) no C4 C9 . . 1.423(4) no C5 C6 . . 1.352(6) no C5 H5 . . 0.930 no C6 C7 . . 1.408(6) no C6 H6 . . 0.930 no C7 C8 . . 1.366(4) no C7 H7 . . 0.930 no C8 C9 . . 1.408(5) no C8 H8 . . 0.930 no C11 H11A . . 0.960 no C11 H11B . . 0.960 no C11 H11C . . 0.960 no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 O1 O2 3.480(2) 2_757 O1 C2 3.550(3) 2_757 O1M O2W 2.759(4) 2_656 O1W O2 2.717(3) 2_757 O2 C10 3.253(3) 2_757 O2 C1 3.294(3) 2_757 O2 C6 3.564(4) 2_667 O2W C11 3.506(5) 2_656 C1 C5 3.504(4) 2_667 C1 C10 3.545(3) 2_757 C2 C4 3.531(3) 2_667 C3 C9 3.486(4) 2_667 C10 C10 3.237(4) 2_757 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O1W H1A O2W . 0.90 1.83 2.725(3) 179 O1W H1B O2 2_757 0.91 1.82 2.716(2) 170 O1M H1M O2 2_657 0.82 1.90 2.723(3) 177 O2W H2A O1M 2_656 0.90 1.89 2.759(4) 162 O2W H2B O1M . 0.88 2.16 3.002(4) 159 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_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ni1 O1 C10 O2 . . . 177.7(2) no Ni1 O1 C10 C1 . . . -1.8(2) no Ni1 O1 C10 O2 2_657 2_657 2_657 -177.7(2) no Ni1 O1 C10 C1 2_657 2_657 2_657 1.8(2) no Ni1 N1 C1 C2 . . . 178.3(2) no Ni1 N1 C1 C10 . . . -3.5(2) no Ni1 N1 C9 C4 . . . -178.0(2) no Ni1 N1 C9 C8 . . . 3.2(3) no Ni1 N1 C1 C2 2_657 2_657 2_657 -178.3(2) no Ni1 N1 C1 C10 2_657 2_657 2_657 3.5(2) no Ni1 N1 C9 C4 2_657 2_657 2_657 178.0(2) no Ni1 N1 C9 C8 2_657 2_657 2_657 -3.2(3) no O1 Ni1 N1 C1 . . . 2.10(10) no O1 Ni1 N1 C9 . . . 179.8(2) no O1 Ni1 N1 C1 . 2_657 2_657 177.90(10) no O1 Ni1 N1 C9 . 2_657 2_657 0.2(2) no O1 C10 C1 N1 . . . 3.7(3) no O1 C10 C1 C2 . . . -178.1(2) no O1W Ni1 O1 C10 . . . 89.8(2) no O1W Ni1 O1 C10 . 2_657 2_657 90.2(2) no O1W Ni1 N1 C1 . . . -89.60(10) no O1W Ni1 N1 C9 . . . 88.2(2) no O1W Ni1 N1 C1 . 2_657 2_657 -90.40(10) no O1W Ni1 N1 C9 . 2_657 2_657 91.8(2) no O2 C10 C1 N1 . . . -175.8(2) no O2 C10 C1 C2 . . . 2.4(3) no N1 Ni1 O1 C10 . . . -0.10(10) no N1 Ni1 O1 C10 . 2_657 2_657 -179.90(10) no N1 C1 C2 C3 . . . 0.2(4) no N1 C9 C4 C3 . . . 0.1(3) no N1 C9 C4 C5 . . . -179.3(2) no N1 C9 C8 C7 . . . -179.7(2) no C1 N1 C9 C4 . . . -0.4(3) no C1 N1 C9 C8 . . . -179.2(2) no C1 C2 C3 C4 . . . -0.5(4) no C2 C1 N1 C9 . . . 0.2(3) no C2 C3 C4 C5 . . . 179.7(2) no C2 C3 C4 C9 . . . 0.4(4) no C3 C2 C1 C10 . . . -177.9(2) no C3 C4 C5 C6 . . . 180.0(3) no C3 C4 C9 C8 . . . 178.9(2) no C4 C5 C6 C7 . . . 0.9(4) no C4 C9 C8 C7 . . . 1.4(4) no C5 C4 C9 C8 . . . -0.5(3) no C5 C6 C7 C8 . . . 0.1(5) no C6 C5 C4 C9 . . . -0.7(4) no C6 C7 C8 C9 . . . -1.3(4) no C9 N1 C1 C10 . . . 178.4(2) no C9 N1 C1 C10 . . . 178.4(2) no