#------------------------------------------------------------------------------ #$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/03/2200318.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_2200318 loop_ _publ_author_name 'Okabe, Nobuo' 'Saishu, Hiroko' _publ_section_title ; Bisaquabis(8-hydroxyquinolinato-N,O)copper(II) ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m251 _journal_page_last m252 _journal_paper_doi 10.1107/S1600536801008297 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Cu (C9 H6 N1 O1)2 (H 2O)2]' _chemical_formula_moiety 'C18 H16 Cu N2 O4' _chemical_formula_sum 'C18 H16 Cu N2 O4' _chemical_formula_weight 387.88 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _cell_angle_alpha 90 _cell_angle_beta 106.39(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.425(3) _cell_length_b 5.542(3) _cell_length_c 12.950(4) _cell_measurement_reflns_used 24 _cell_measurement_temperature 296.2 _cell_measurement_theta_max 15.0 _cell_measurement_theta_min 14.9 _cell_volume 786.6(5) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, Rigaku Corporation, 1999a) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation and Rigaku Corporation, 1999b)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material TEXSAN _computing_structure_refinement 'SHELXL97 (Scheldrick, 1997)' _computing_structure_solution 'SAPI91 (Fan, 1991)' _diffrn_measured_fraction_theta_full 1.00 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measurement_device_type 'Rigaku AFC-5R' _diffrn_measurement_method \w-2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .7107 _diffrn_reflns_av_R_equivalents .011 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 2094 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 4 _diffrn_standards_decay_% .09 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.415 _exptl_absorpt_correction_T_max .654 _exptl_absorpt_correction_T_min .512 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour 'light blue' _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 398.0 _exptl_crystal_size_max .50 _exptl_crystal_size_mid .40 _exptl_crystal_size_min .30 _refine_diff_density_max .65 _refine_diff_density_min -.64 _refine_ls_extinction_coef .0000 _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref .914 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 115 _refine_ls_number_reflns 1516 _refine_ls_R_factor_gt .0327 _refine_ls_shift/su_max .0000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1109 _reflns_number_gt 1516 _reflns_number_total 1813 _reflns_threshold_expression I>2\s(I) _cod_data_source_file na6078.cif _cod_data_source_block I _cod_original_cell_volume 786.7(5) _cod_original_sg_symbol_H-M 'P 21/a' _cod_database_code 2200318 _cod_database_fobs_code 2200318 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-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 Cu1 .0000 .0000 .0000 .0258(2) Uani d S 1.00 . . Cu O1 .07900(10) .2427(2) -.06860(10) .0295(3) Uani d . 1.00 . . O O2 -.16340(10) .2844(3) .0027(2) .0462(4) Uani d . 1.00 . . O N1 -.07950(10) -.1042(3) -.15260(10) .0272(3) Uani d . 1.00 . . N C1 -.1564(2) -.2821(4) -.1911(2) .0336(4) Uani d . 1.00 . . C C2 -.2040(2) -.3229(4) -.3026(2) .0411(5) Uani d . 1.00 . . C C3 -.1695(2) -.1795(4) -.3732(2) .0398(5) Uani d . 1.00 . . C C4 -.0415(2) .1698(5) -.4012(2) .0405(5) Uani d . 1.00 . . C C5 .0422(2) .3417(5) -.3551(2) .0430(5) Uani d . 1.00 . . C C6 .0851(2) .3710(4) -.2429(2) .0378(5) Uani d . 1.00 . . C C7 .0439(2) .2251(4) -.1743(2) .0279(4) Uani d . 1.00 . . C C8 -.0428(2) .0403(4) -.2221(2) .0265(4) Uani d . 1.00 . . C C9 -.0851(2) .0120(3) -.3353(2) .0323(5) Uani d . 1.00 . . C H1 -.1804 -.3856 -.1422 .0403 Uiso calc . 1.00 . . H H2 -.2601 -.4508 -.3281 .0493 Uiso calc . 1.00 . . H H3 -.2017 -.2065 -.4484 .0478 Uiso calc . 1.00 . . H H4 -.0703 .1566 -.4774 .0486 Uiso calc . 1.00 . . H H5 .0727 .4449 -.4001 .0516 Uiso calc . 1.00 . . H H6 .1433 .4933 -.2139 .0453 Uiso calc . 1.00 . . H H7 -.2442 .2862 -.0254 .0506 Uiso calc . 1.00 . . H H8 -.1391 .4104 .0244 .0564 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 Cu1 .0264(2) .0266(2) .0232(2) -.00750(10) .0049(2) -.00160(10) O1 .0304(7) .0288(7) .0276(7) -.0094(6) .0053(5) -.0012(6) O2 .0295(8) .0287(8) .0760(10) .0010(6) .0078(7) -.0094(8) N1 .0231(7) .0288(9) .0276(8) -.0007(6) .0038(6) -.0025(7) C1 .0322(10) .0310(10) .0360(10) -.0047(8) .0067(8) -.0032(8) C2 .0360(10) .0410(10) .0410(10) -.0069(9) .0014(9) -.0126(10) C3 .0370(10) .0450(10) .0320(10) -.0002(9) .0010(8) -.0097(9) C4 .0450(10) .0490(10) .0273(10) .0080(10) .0092(9) .0027(9) C5 .0440(10) .0510(10) .0370(10) .0010(10) .0151(10) .0120(10) C6 .0360(10) .0410(10) .0360(10) -.0061(9) .0098(9) .0038(9) C7 .0243(9) .0274(9) .0311(9) .0014(7) .0063(7) .0002(8) C8 .0245(9) .0273(9) .0269(10) .0029(7) .0057(8) -.0013(7) C9 .0300(10) .0370(10) .0270(10) .0070(7) .0048(9) -.0027(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .003 .002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H .000 .000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O .011 .006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N .006 .003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu .320 1.265 ;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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Cu1 O2 1_555 1_555 90.88(6) yes O1 Cu1 O2 1_555 3_555 89.12(6) no O1 Cu1 N1 1_555 1_555 83.70(6) yes O1 Cu1 N1 1_555 3_555 96.30(6) no O2 Cu1 N1 1_555 1_555 93.67(6) yes O2 Cu1 N1 1_555 3_555 86.33(6) no Cu1 O1 C7 1_555 1_555 112.00(10) yes Cu1 O2 H7 1_555 1_555 134.9 no Cu1 O2 H8 1_555 1_555 112.8 no H7 O2 H8 1_555 1_555 111.2 no Cu1 N1 C1 1_555 1_555 130.7(2) yes Cu1 N1 C8 1_555 1_555 110.10(10) yes C1 N1 C8 1_555 1_555 119.2(2) yes N1 C1 C2 1_555 1_555 121.9(2) yes N1 C1 H1 1_555 1_555 119.0 no C2 C1 H1 1_555 1_555 119.0 no C1 C2 C3 1_555 1_555 119.8(2) yes C1 C2 H2 1_555 1_555 120.1 no C3 C2 H2 1_555 1_555 120.1 no C2 C3 C9 1_555 1_555 120.2(2) yes C2 C3 H3 1_555 1_555 119.9 no C9 C3 H3 1_555 1_555 119.9 no C5 C4 C9 1_555 1_555 119.5(2) yes C5 C4 H4 1_555 1_555 120.2 no C9 C4 H4 1_555 1_555 120.2 no C4 C5 C6 1_555 1_555 122.1(2) yes C4 C5 H5 1_555 1_555 119.0 no C6 C5 H5 1_555 1_555 118.9 no C5 C6 C7 1_555 1_555 121.0(2) yes C5 C6 H6 1_555 1_555 119.5 no C7 C6 H6 1_555 1_555 119.5 no O1 C7 C6 1_555 1_555 124.5(2) yes O1 C7 C8 1_555 1_555 118.1(2) yes C6 C7 C8 1_555 1_555 117.4(2) yes N1 C8 C7 1_555 1_555 116.1(2) yes N1 C8 C9 1_555 1_555 122.8(2) yes C7 C8 C9 1_555 1_555 121.1(2) yes C3 C9 C4 1_555 1_555 125.1(2) yes C3 C9 C8 1_555 1_555 116.0(2) yes C4 C9 C8 1_555 1_555 118.9(2) yes 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 Cu1 O1 . . 1.966(2) yes Cu1 O2 . . 2.451(2) yes Cu1 N1 . . 2.013(2) yes O1 C7 . . 1.318(2) yes O2 H7 . . .892 no O2 H8 . . .775 no N1 C1 . . 1.321(3) yes N1 C8 . . 1.357(3) yes C1 C2 . . 1.411(3) yes C1 H1 . . .950 no C2 C3 . . 1.351(4) yes C2 H2 . . .950 no C3 C9 . . 1.425(3) yes C3 H3 . . .950 no C4 C5 . . 1.363(3) yes C4 C9 . . 1.408(4) yes C4 H4 . . .950 no C5 C6 . . 1.405(3) yes C5 H5 . . .950 no C6 C7 . . 1.378(3) yes C6 H6 . . .950 no C7 C8 . . 1.437(3) yes C8 C9 . . 1.417(3) yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 O1 O2 2.829(2) 4_555 O1 O2 2.839(2) 3_565 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 _geom_hbond_publ_flag O2 H7 O1 4_455 .89 1.94 2.829(2) 171 yes O2 H8 O1 3_565 .77 2.07 2.839(2) 175 yes 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_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O1 Cu1 N1 C1 1_555 1_555 1_555 1_555 178.4(2) yes O1 Cu1 N1 C8 1_555 1_555 1_555 1_555 -1.20(10) no O1 Cu1 N1 C1 1_555 1_555 3_555 3_555 1.6(2) no O1 Cu1 N1 C8 1_555 1_555 3_555 3_555 -178.80(10) no O1 C7 C6 C5 1_555 1_555 1_555 1_555 -179.5(2) no O1 C7 C8 N1 1_555 1_555 1_555 1_555 -1.1(3) no O1 C7 C8 C9 1_555 1_555 1_555 1_555 179.6(2) no O2 Cu1 O1 C7 1_555 1_555 1_555 1_555 -92.90(10) yes O2 Cu1 O1 C7 1_555 1_555 3_555 3_555 -87.10(10) no O2 Cu1 N1 C1 1_555 1_555 1_555 1_555 -91.2(2) yes O2 Cu1 N1 C8 1_555 1_555 1_555 1_555 89.30(10) yes O2 Cu1 N1 C1 1_555 1_555 3_555 3_555 -88.8(2) no O2 Cu1 N1 C8 1_555 1_555 3_555 3_555 90.70(10) no N1 Cu1 O1 C7 1_555 1_555 1_555 1_555 .70(10) no N1 Cu1 O1 C7 1_555 1_555 3_555 3_555 179.30(10) no N1 C1 C2 C3 1_555 1_555 1_555 1_555 .9(4) no N1 C8 C7 C6 1_555 1_555 1_555 1_555 178.5(2) no N1 C8 C9 C3 1_555 1_555 1_555 1_555 -.1(3) no N1 C8 C9 C4 1_555 1_555 1_555 1_555 -179.7(2) no C1 N1 C8 C7 1_555 1_555 1_555 1_555 -178.1(2) no C1 N1 C8 C9 1_555 1_555 1_555 1_555 1.2(3) no C1 C2 C3 C9 1_555 1_555 1_555 1_555 .2(4) no C2 C1 N1 C8 1_555 1_555 1_555 1_555 -1.6(3) no C2 C3 C9 C4 1_555 1_555 1_555 1_555 179.1(2) no C2 C3 C9 C8 1_555 1_555 1_555 1_555 -.6(3) no C3 C9 C4 C5 1_555 1_555 1_555 1_555 -178.0(2) no C3 C9 C8 C7 1_555 1_555 1_555 1_555 179.2(2) no C4 C5 C6 C7 1_555 1_555 1_555 1_555 .1(4) no C4 C9 C8 C7 1_555 1_555 1_555 1_555 -.5(3) no C5 C4 C9 C8 1_555 1_555 1_555 1_555 1.6(4) no C5 C6 C7 C8 1_555 1_555 1_555 1_555 1.0(3) no C6 C5 C4 C9 1_555 1_555 1_555 1_555 -1.5(4) no C6 C7 C8 C9 1_555 1_555 1_555 1_555 -.8(3) no