#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/22/2012259.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_2012259 loop_ _publ_author_name 'Bond, Andrew D.' 'Feeder, Neil' 'Teat, Simon J.' 'Jones, William' _publ_section_title ; Bis[1-hydroxypyridine-2(1H)-thionato-S,O]copper(II) ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1157 _journal_page_last 1158 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Cu (C5 H4 N O S)2]' _chemical_formula_moiety 'C10 H8 Cu N2 O2 S2' _chemical_formula_sum 'C10 H8 Cu N2 O2 S2' _chemical_formula_weight 315.84 _chemical_name_common Cu(PT)~2~ _chemical_name_systematic ; Bis(1-hydroxy-2(1H)-pyridinethiolato-S^2^,O)copper(II) ; _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 81.096(4) _cell_angle_beta 86.190(4) _cell_angle_gamma 85.197(4) _cell_formula_units_Z 1 _cell_length_a 4.0545(7) _cell_length_b 7.5723(12) _cell_length_c 9.0629(14) _cell_measurement_reflns_used 1797 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 29.06 _cell_measurement_theta_min 3.18 _cell_volume 273.53(8) _computing_cell_refinement 'LSCELL (Clegg, 1997)' _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_molecular_graphics 'XP in SHELXTL (Siemens, 1996) and CAMERON (Watkin et al., 1996)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 8.192 _diffrn_measured_fraction_theta_full .968 _diffrn_measured_fraction_theta_max .871 _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'thin slice \w-scans' _diffrn_radiation_monochromator 'silicon 111' _diffrn_radiation_source 'Daresbury SRS, Station 9.8' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength .6884 _diffrn_reflns_av_R_equivalents .044 _diffrn_reflns_av_sigmaI/netI .078 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 2505 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 29.18 _diffrn_reflns_theta_min 2.21 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.365 _exptl_absorpt_correction_T_max .977 _exptl_absorpt_correction_T_min .911 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1997)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 159 _exptl_crystal_size_max .04 _exptl_crystal_size_mid .02 _exptl_crystal_size_min .01 _refine_diff_density_max 1.29 _refine_diff_density_min -1.04 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 79 _refine_ls_number_reflns 1430 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.011 _refine_ls_R_factor_all .084 _refine_ls_R_factor_gt .061 _refine_ls_shift/su_max .011 _refine_ls_shift/su_mean .001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.1051P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .161 _reflns_number_gt 1074 _reflns_number_total 1430 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file gd1171.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M P-1 _cod_database_code 2012259 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 Cu1 .0000 .0000 .0000 .0156(3) Uani d S 1 . . Cu S1 .3100(3) .08589(14) -.20927(12) .0220(3) Uani d . 1 . . S O1 .0855(8) -.2449(4) -.0387(3) .0202(7) Uani d . 1 . . O N1 .3049(9) -.2690(5) -.1544(4) .0162(7) Uani d . 1 . . N C1 .4313(11) -.1253(6) -.2437(5) .0163(8) Uani d . 1 . . C C2 .6546(10) -.1627(6) -.3620(5) .0178(9) Uani d . 1 . . C H2 .7483 -.0665 -.4267 .021 Uiso calc R 1 . . H C3 .7394(12) -.3346(7) -.3859(5) .0234(10) Uani d . 1 . . C H3 .8884 -.3574 -.4674 .028 Uiso calc R 1 . . H C4 .6059(12) -.4779(6) -.2897(5) .0224(9) Uani d . 1 . . C H4 .6656 -.5982 -.3044 .027 Uiso calc R 1 . . H C5 .3904(12) -.4416(6) -.1754(5) .0194(9) Uani d . 1 . . C H5 .2982 -.5372 -.1095 .023 Uiso calc R 1 . . 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 .0202(4) .0153(4) .0118(4) -.0028(3) .0023(3) -.0045(3) S1 .0284(7) .0167(6) .0205(6) -.0027(5) .0067(5) -.0040(5) O1 .0260(16) .0195(15) .0146(15) -.0034(13) .0077(13) -.0045(12) N1 .0149(16) .0232(19) .0124(17) -.0029(15) -.0004(13) -.0082(14) C1 .0154(18) .020(2) .0136(19) -.0007(16) -.0043(16) -.0007(15) C2 .0131(18) .024(2) .015(2) -.0021(17) .0008(16) -.0006(16) C3 .025(2) .026(2) .020(2) .0003(19) .0013(19) -.0074(18) C4 .027(2) .018(2) .021(2) -.0022(19) .0023(19) -.0025(17) C5 .026(2) .0161(19) .016(2) -.0014(18) -.0054(18) -.0025(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 O1 2 1.939(3) no Cu1 O1 . 1.939(3) yes Cu1 S1 2 2.2445(11) no Cu1 S1 . 2.2445(11) yes S1 C1 . 1.703(4) yes O1 N1 . 1.354(5) yes N1 C5 . 1.362(6) yes N1 C1 . 1.366(6) yes C1 C2 . 1.405(6) yes C2 C3 . 1.365(6) yes C2 H2 . .9500 no C3 C4 . 1.405(7) yes C3 H3 . .9500 no C4 C5 . 1.356(7) yes C4 H4 . .9500 no C5 H5 . .9500 no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu .3201 1.2651 'International Tables 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_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Cu1 O1 2 . 180.0 yes O1 Cu1 S1 2 2 87.96(9) yes O1 Cu1 S1 . 2 92.04(9) yes O1 Cu1 S1 2 . 92.04(9) yes O1 Cu1 S1 . . 87.96(9) yes S1 Cu1 S1 2 . 180.0 yes C1 S1 Cu1 . . 95.67(15) yes N1 O1 Cu1 . . 115.7(3) yes O1 N1 C5 . . 116.6(4) yes O1 N1 C1 . . 120.6(4) yes C5 N1 C1 . . 122.8(4) no N1 C1 C2 . . 116.7(4) no N1 C1 S1 . . 119.6(3) no C2 C1 S1 . . 123.6(3) no C3 C2 C1 . . 121.2(4) no C3 C2 H2 . . 119.4 no C1 C2 H2 . . 119.4 no C2 C3 C4 . . 119.8(4) no C2 C3 H3 . . 120.1 no C4 C3 H3 . . 120.1 no C5 C4 C3 . . 118.9(4) no C5 C4 H4 . . 120.6 no C3 C4 H4 . . 120.6 no C4 C5 N1 . . 120.5(4) no C4 C5 H5 . . 119.7 no N1 C5 H5 . . 119.7 no 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 _geom_torsion_publ_flag O1 Cu1 S1 C1 2 174.65(17) no O1 Cu1 S1 C1 . -5.35(17) no S1 Cu1 O1 N1 2 -173.5(3) no S1 Cu1 O1 N1 . 6.5(3) no Cu1 O1 N1 C5 . 174.5(3) no Cu1 O1 N1 C1 . -5.3(5) no O1 N1 C1 C2 . -179.3(4) no C5 N1 C1 C2 . .9(6) no O1 N1 C1 S1 . -.3(6) no C5 N1 C1 S1 . 179.9(3) no Cu1 S1 C1 N1 . 4.5(4) no Cu1 S1 C1 C2 . -176.5(4) no N1 C1 C2 C3 . .0(7) no S1 C1 C2 C3 . -179.0(3) no C1 C2 C3 C4 . -.9(7) no C2 C3 C4 C5 . .9(7) no C3 C4 C5 N1 . .0(7) no O1 N1 C5 C4 . 179.3(4) no C1 N1 C5 C4 . -.9(7) no _cod_database_fobs_code 2012259