#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/33/2013314.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_2013314 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_volume 59 _journal_year 2003 _chemical_formula_iupac '[Co (C10 H6 N O2)2 (H2 O)2], 2C H4 O, 2H2 O' _chemical_formula_moiety 'C20 H16 Co N2 O6, 2C H4 O, 2H2 O' _chemical_formula_sum 'C22 H28 Co N2 O10' _chemical_formula_weight 539.39 _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 76.35(2) _cell_angle_beta 74.38(2) _cell_angle_gamma 69.86(2) _cell_formula_units_Z 1 _cell_length_a 7.170(2) _cell_length_b 8.965(2) _cell_length_c 10.827(2) _cell_measurement_reflns_used 20 _cell_measurement_temperature 296.2 _cell_measurement_theta_max 14.7 _cell_measurement_theta_min 12.7 _cell_volume 621.3(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 0.051 _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 -14 _diffrn_reflns_number 3034 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_standards_decay_% 38.09 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 281.0 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.36 _refine_diff_density_min -0.62 _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 2855 _refine_ls_R_factor_gt 0.0463 _refine_ls_shift/su_max <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0516P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1291 _reflns_number_gt 1677 _reflns_number_total 2855 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ln1166.cif _[local]_cod_data_source_block I _cod_database_code 2013314 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 Co1 0.5000 0.0000 1.0000 0.0316(2) Uani d S 1.00 . . Co O1 0.7014(3) -0.0386(3) 1.1129(2) 0.0391(5) Uani d . 1.00 . . O O1M 0.1892(5) 0.1187(4) 0.5964(3) 0.0740(9) Uani d . 1.00 . . O O1W 0.7316(3) -0.1082(3) 0.8507(2) 0.0423(6) Uani d . 1.00 . . O O2 0.9090(3) 0.0582(3) 1.1682(2) 0.0476(6) Uani d . 1.00 . . O O2W 0.6247(4) 0.0316(4) 0.6181(3) 0.0719(9) Uani d . 1.00 . . O N1 0.5976(4) 0.2212(3) 0.9371(2) 0.0316(6) Uani d . 1.00 . . N C1 0.7362(5) 0.2139(4) 0.9997(3) 0.0355(7) Uani d . 1.00 . . C C2 0.8304(5) 0.3343(4) 0.9772(4) 0.0442(9) Uani d . 1.00 . . C C3 0.7746(5) 0.4673(4) 0.8875(4) 0.0490(9) Uani d . 1.00 . . C C4 0.6286(5) 0.4811(4) 0.8194(3) 0.0418(8) Uani d . 1.00 . . C C5 0.5646(6) 0.6153(4) 0.7241(4) 0.0570(10) Uani d . 1.00 . . C C6 0.4230(8) 0.6226(5) 0.6604(4) 0.0710(10) Uani d . 1.00 . . C C7 0.3348(7) 0.4980(5) 0.6883(4) 0.0680(10) Uani d . 1.00 . . C C8 0.3916(6) 0.3663(4) 0.7795(4) 0.0513(10) Uani d . 1.00 . . C C9 0.5401(5) 0.3542(4) 0.8462(3) 0.0361(7) Uani d . 1.00 . . C C10 0.7883(5) 0.0664(4) 1.1006(3) 0.0358(7) Uani d . 1.00 . . C C11 0.0264(8) 0.2507(7) 0.5727(6) 0.105(2) Uani d . 1.00 . . C H1A 0.6925 -0.0612 0.7755 0.0580 Uiso calc . 1.00 . . H H1B 0.8477 -0.0975 0.8562 0.0580 Uiso calc . 1.00 . . H H1M 0.1550 0.0625 0.6648 0.1109 Uiso calc . 1.00 . . H H2 0.9288 0.3236 1.0225 0.0531 Uiso calc . 1.00 . . H H2A 0.6886 0.0064 0.5396 0.0923 Uiso calc . 1.00 . . H H2B 0.4915 0.0710 0.6299 0.0923 Uiso calc . 1.00 . . H H3 0.8342 0.5490 0.8718 0.0587 Uiso calc . 1.00 . . H H5 0.6210 0.6993 0.7053 0.0686 Uiso calc . 1.00 . . H H6 0.3837 0.7110 0.5976 0.0848 Uiso calc . 1.00 . . H H7 0.2365 0.5050 0.6443 0.0816 Uiso calc . 1.00 . . H H8 0.3316 0.2846 0.7973 0.0615 Uiso calc . 1.00 . . H H11A -0.0210 0.3101 0.6439 0.1261 Uiso calc . 1.00 . . H H11B -0.0808 0.2157 0.5634 0.1261 Uiso calc . 1.00 . . H H11C 0.0676 0.3183 0.4942 0.1261 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 Co1 0.0327(4) 0.0297(4) 0.0355(4) -0.0130(3) -0.0124(3) 0.0009(3) O1 0.0440(10) 0.0350(10) 0.0450(10) -0.0200(10) -0.0190(10) 0.0050(10) O1M 0.064(2) 0.093(3) 0.048(2) -0.008(2) -0.0090(10) -0.005(2) O1W 0.0400(10) 0.0450(10) 0.0470(10) -0.0180(10) -0.0090(10) -0.0080(10) O2 0.0430(10) 0.060(2) 0.0490(10) -0.0230(10) -0.0200(10) -0.0020(10) O2W 0.062(2) 0.092(2) 0.051(2) -0.009(2) -0.0120(10) -0.012(2) N1 0.0320(10) 0.0260(10) 0.0340(10) -0.0080(10) -0.0050(10) -0.0040(10) C1 0.035(2) 0.032(2) 0.038(2) -0.0080(10) -0.0040(10) -0.0090(10) C2 0.044(2) 0.044(2) 0.054(2) -0.026(2) -0.008(2) -0.010(2) C3 0.051(2) 0.037(2) 0.061(2) -0.026(2) 0.000(2) -0.006(2) C4 0.049(2) 0.027(2) 0.045(2) -0.016(2) 0.002(2) -0.004(2) C5 0.076(3) 0.029(2) 0.059(3) -0.018(2) -0.007(2) 0.005(2) C6 0.101(4) 0.038(2) 0.067(3) -0.021(2) -0.031(3) 0.018(2) C7 0.090(3) 0.049(3) 0.069(3) -0.023(2) -0.042(3) 0.015(2) C8 0.063(2) 0.038(2) 0.054(2) -0.018(2) -0.022(2) 0.007(2) C9 0.042(2) 0.025(2) 0.037(2) -0.0090(10) -0.0030(10) -0.0040(10) C10 0.026(2) 0.042(2) 0.037(2) -0.0080(10) -0.0030(10) -0.009(2) C11 0.085(4) 0.085(4) 0.097(4) 0.008(3) -0.002(3) 0.005(3) 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 Co1 O1 . . 2.026(3) yes Co1 O1W . . 2.120(2) yes Co1 N1 . . 2.224(3) yes O1 C10 . . 1.262(5) no O1M C11 . . 1.377(6) no O1M H1M . . 0.820 no O1W H1A . . 0.894 no O1W H1B . . 0.889 no O2 C10 . . 1.250(5) no O2W H2A . . 0.891 no O2W H2B . . 0.881 no N1 C1 . . 1.322(5) no N1 C9 . . 1.373(4) no C1 C2 . . 1.405(6) no C1 C10 . . 1.509(4) no C2 C3 . . 1.363(5) no C2 H2 . . 0.930 no C3 C4 . . 1.393(6) no C3 H3 . . 0.930 no C4 C5 . . 1.418(5) no C4 C9 . . 1.422(6) no C5 C6 . . 1.349(8) no C5 H5 . . 0.930 no C6 C7 . . 1.402(8) no C6 H6 . . 0.930 no C7 C8 . . 1.367(5) no C7 H7 . . 0.930 no C8 C9 . . 1.402(6) no C8 H8 . . 0.930 no C11 H11A . . 0.960 no C11 H11B . . 0.960 no C11 H11C . . 0.960 no 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) ; Co Co 0.349 0.972 ;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 Co1 O1 2_657 180.0 no O1 Co1 O1W . 92.03(9) yes O1 Co1 O1W 2_657 87.97(9) no O1 Co1 N1 . 77.36(10) yes O1 Co1 N1 2_657 102.64(10) no O1W Co1 O1W 2_657 180.0 no O1W Co1 N1 . 89.64(9) no O1W Co1 N1 2_657 90.36(9) no N1 Co1 N1 2_657 180.0 no Co1 O1 C10 . 119.0(2) no C11 O1M H1M . 109.5 no Co1 O1W H1A . 107.2 no Co1 O1W H1B . 108.0 no H1A O1W H1B . 114.5 no H2A O2W H2B . 115.6 no Co1 N1 C1 . 110.7(2) no Co1 N1 C9 . 130.7(3) no C1 N1 C9 . 118.6(3) no N1 C1 C2 . 123.5(3) no N1 C1 C10 . 115.8(3) no C2 C1 C10 . 120.7(3) no C1 C2 C3 . 118.6(4) no C1 C2 H2 . 120.7 no C3 C2 H2 . 120.7 no C2 C3 C4 . 120.1(4) no C2 C3 H3 . 119.9 no C4 C3 H3 . 119.9 no C3 C4 C5 . 123.1(4) no C3 C4 C9 . 118.4(3) no C5 C4 C9 . 118.5(4) no C4 C5 C6 . 120.8(4) no C4 C5 H5 . 119.6 no C6 C5 H5 . 119.6 no C5 C6 C7 . 120.5(4) no C5 C6 H6 . 119.8 no C7 C6 H6 . 119.8 no C6 C7 C8 . 120.8(5) no C6 C7 H7 . 119.6 no C8 C7 H7 . 119.6 no C7 C8 C9 . 120.1(4) no C7 C8 H8 . 119.9 no C9 C8 H8 . 119.9 no N1 C9 C4 . 120.7(3) no N1 C9 C8 . 119.9(3) no C4 C9 C8 . 119.3(3) no O1 C10 O2 . 124.5(3) no O1 C10 C1 . 117.1(3) no O2 C10 C1 . 118.4(4) 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_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 O1 O2 3.526(3) 2_757 O1 C2 3.546(4) 2_757 O1M O2W 2.750(4) 2_656 O1W O2 2.711(4) 2_757 O2 C10 3.300(4) 2_757 O2 C1 3.325(4) 2_757 O2 C6 3.568(5) 2_667 O2W C11 3.501(6) 2_656 C1 C5 3.514(5) 2_667 C1 C10 3.537(4) 2_757 C2 C4 3.534(4) 2_667 C3 C9 3.486(5) 2_667 C10 C10 3.248(6) 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 . 0.89 1.83 2.719(4) 177 O1W H1B O2 2_757 0.89 1.84 2.711(3) 168 O1M H1M O2 2_657 0.82 1.90 2.720(4) 173 O2W H2A O1M 2_656 0.89 1.90 2.750(4) 160 O2W H2B O1M . 0.88 2.17 3.007(4) 158 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 Co1 O1 C10 O2 . . . 177.2(2) no Co1 O1 C10 C1 . . . -0.8(3) no Co1 O1 C10 O2 2_657 2_657 2_657 -177.2(2) no Co1 O1 C10 C1 2_657 2_657 2_657 0.8(3) no Co1 N1 C1 C2 . . . 178.0(2) no Co1 N1 C1 C10 . . . -2.6(3) no Co1 N1 C9 C4 . . . -178.2(2) no Co1 N1 C9 C8 . . . 2.3(4) no Co1 N1 C1 C2 2_657 2_657 2_657 -178.0(2) no Co1 N1 C1 C10 2_657 2_657 2_657 2.6(3) no Co1 N1 C9 C4 2_657 2_657 2_657 178.2(2) no Co1 N1 C9 C8 2_657 2_657 2_657 -2.3(4) no O1 Co1 N1 C1 . . . 1.8(2) no O1 Co1 N1 C9 . . . -179.6(3) no O1 Co1 N1 C1 . 2_657 2_657 178.2(2) no O1 Co1 N1 C9 . 2_657 2_657 -0.4(3) no O1 C10 C1 N1 . . . 2.4(4) no O1 C10 C1 C2 . . . -178.2(3) no O1W Co1 O1 C10 . . . 88.7(2) no O1W Co1 O1 C10 . 2_657 2_657 91.3(2) no O1W Co1 N1 C1 . . . -90.4(2) no O1W Co1 N1 C9 . . . 88.3(2) no O1W Co1 N1 C1 . 2_657 2_657 -89.6(2) no O1W Co1 N1 C9 . 2_657 2_657 91.7(2) no O2 C10 C1 N1 . . . -175.6(3) no O2 C10 C1 C2 . . . 3.8(4) no N1 Co1 O1 C10 . . . -0.5(2) no N1 Co1 O1 C10 . 2_657 2_657 -179.5(2) no N1 C1 C2 C3 . . . 1.0(5) no N1 C9 C4 C3 . . . -0.1(4) no N1 C9 C4 C5 . . . 179.7(3) no N1 C9 C8 C7 . . . -179.6(3) no C1 N1 C9 C4 . . . 0.4(4) no C1 N1 C9 C8 . . . -179.2(3) no C1 C2 C3 C4 . . . -0.7(5) no C2 C1 N1 C9 . . . -0.8(4) no C2 C3 C4 C5 . . . -179.5(3) no C2 C3 C4 C9 . . . 0.3(5) no C3 C2 C1 C10 . . . -178.3(3) no C3 C4 C5 C6 . . . 179.8(4) no C3 C4 C9 C8 . . . 179.5(3) no C4 C5 C6 C7 . . . 0.6(6) no C4 C9 C8 C7 . . . 0.9(5) no C5 C4 C9 C8 . . . -0.8(5) no C5 C6 C7 C8 . . . -0.6(6) no C6 C5 C4 C9 . . . 0.0(5) no C6 C7 C8 C9 . . . -0.2(6) no C9 N1 C1 C10 . . . 178.5(2) no C9 N1 C1 C10 . . . 178.5(2) no