#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/14/2011439.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_2011439 loop_ _publ_author_name 'Gueddi, A.' 'Mernari, B.' 'Giorgi, M.' 'Pierrot, M.' _publ_section_title ; Two 2,5-bis(2-pyridinyl)-1,3,4-oxadiazole--metal complexes (M = Cu and~Ni) ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first e426 _journal_page_last e428 _journal_paper_doi 10.1107/S0108270100011707 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[Cu (C12 H8 N4 O)2 (H2 O)2] (C F3 S O3)2' _chemical_formula_moiety 'C24 H20 Cu1 N8 O4 2+, 2 C F3 S O3 1-' _chemical_formula_sum 'C26 H20 Cu F6 N8 O10 S2' _chemical_formula_weight 846.15 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90 _cell_angle_beta 147.261(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 13.5897(5) _cell_length_b 10.0316(4) _cell_length_c 22.6240(10) _cell_measurement_reflns_used 12050 _cell_measurement_temperature 298 _cell_measurement_theta_max 25.8 _cell_measurement_theta_min 1.0 _cell_volume 1668.00(18) _computing_data_collection 'KappaCCD Software (Nonius, 1997)' _computing_data_reduction 'DENZO and SCALEPAK (Otwinowski & Minor, 1997)' _computing_publication_material 'maxus(Mackay et al., 1999)' _computing_structure_refinement 'maxus (Mackay et al., 1999)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_measurement_device KappaCCD _diffrn_measurement_method \f _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .035 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 3270 _diffrn_reflns_theta_max 25.8 _exptl_absorpt_coefficient_mu .881 _exptl_absorpt_correction_type none _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 854 _exptl_crystal_size_max .20 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .10 _refine_diff_density_max .59 _refine_diff_density_min -.60 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.496 _refine_ls_goodness_of_fit_ref 1.635 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 270 _refine_ls_number_reflns 2633 _refine_ls_R_factor_all .076 _refine_ls_R_factor_gt .065 _refine_ls_shift/su_max .045 _refine_ls_shift/su_mean .007 _refine_ls_structure_factor_coef F^2^ _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + 0.03Fo^2^]' _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_all .074 _refine_ls_wR_factor_ref .074 _reflns_number_gt 2633 _reflns_number_total 3117 _reflns_threshold_expression I>3\s(I) _cod_data_source_file qa0347.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_atom_site_adp_type' tag value 'Uij' was replaced with 'Uani' value 21 time. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1668.0(3) _cod_original_sg_symbol_H-M 'P 21/c' _cod_original_formula_sum 'C26 H20 Cu1 F6 N8 O10 S2' _cod_database_code 2011439 _cod_database_fobs_code 2011439 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z '-X,+Y+ 1/2,-Z+ 1/2' '+X,-Y+ 1/2,+Z+ 1/2' 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_occupancy Cu1 1.0000(3) .5000(2) .50000(16) .08456(9) Uani 1.00 O4 .88392(7) .26501(5) .57921(4) .0841(3) Uani 1.00 O19 .69698(8) .56133(6) .34268(5) .1149(4) Uani 1.00 N1 .92817(9) .34318(6) .51247(5) .0768(4) Uani 1.00 N2 .86069(9) .21457(6) .47217(5) .0898(4) Uani 1.00 N7 1.03524(8) .58187(6) .60042(5) .0704(4) Uani 1.00 N13 .74169(11) .02811(7) .54208(6) .1321(5) Uani 1.00 C5 .93850(11) .36881(7) .57385(6) .0729(4) Uani 1.00 C3 .83674(11) .17214(7) .51331(6) .0780(5) Uani 1.00 C6 .99967(10) .49651(8) .62737(6) .0714(5) Uani 1.00 C8 1.09227(12) .70333(8) .64321(7) .0944(5) Uani 1.00 C9 1.11811(13) .74222(9) .71454(8) .1114(6) Uani 1.00 C10 1.08246(14) .65414(9) .74097(8) .1243(6) Uani 1.00 C11 1.02302(13) .52982(8) .69742(7) .1076(5) Uani 1.00 C12 .76331(11) .04330(7) .49486(7) .0784(4) Uani 1.00 C14 .66667(16) -.08712(10) .52078(9) .1560(8) Uani 1.00 C15 .61301(14) -.18473(9) .45611(9) .1281(6) Uani 1.00 C16 .63885(16) -.16700(9) .41041(9) .1445(7) Uani 1.00 C17 .71696(14) -.04974(8) .43012(8) .1212(6) Uani 1.00 H8 1.1217(11) .7529(8) .6280(6) .0500(7) Uiso 1.00 H9 1.1613(11) .8179(8) .7442(7) .0500(7) Uiso 1.00 H10 1.1198(10) .6758(7) .8026(6) 0(5) Uiso 1.00 H11 .9888(11) .4706(8) .7062(6) .0500(7) Uiso 1.00 H14 .6549(11) -.0938(7) .5550(6) 0(3) Uiso 1.00 H15 .5553(3) -.2631(2) .44249(16) .0500(7) Uiso 1.00 H16 .6065(3) -.2373(2) .36690(16) .0500(7) Uiso 1.00 H17 .732347 -.036731 .396240 .050000 Uiso 1.00 H19A .6226(3) .5319(2) .33417(16) .0500(7) Uiso 1.00 H19B .644975 .631429 .291909 .050000 Uiso 1.00 S20 .37858(4) .38621(3) .29278(2) .11292(17) Uani 1.00 F32 .3724(2) .50027(16) .39320(12) .0784(4) Uiso .44 F39 .5129(3) .29317(18) .45801(16) .0754(6) Uiso .41 O21 .5490(3) .4675(2) .37437(16) .0655(5) Uiso .41 O24 .2115(2) .45422(17) .19804(12) .0625(4) Uiso .60 C30 .38942(16) .36836(12) .37608(10) .1293(8) Uani 1.00 F31 .5072(6) .5073(4) .4360(3) .1422(11) Uiso .24 F33 .2989(2) .43978(19) .36146(13) .0798(4) Uiso .44 F34 .2520(3) .3407(2) .33626(15) .0940(5) Uiso .41 F35 .2481(3) .2661(2) .31740(14) .0786(5) Uiso .36 F50 .5468(2) .33319(15) .47854(12) .0740(5) Uiso .52 O22 .4969(4) .5165(3) .3475(2) .0763(9) Uiso .27 O23 .2763(8) .5090(6) .2261(5) .0922(17) Uiso .14 O25 .2063(5) .4013(3) .1878(3) .0791(11) Uiso .25 O26 .5352(3) .3929(3) .3441(2) .0677(6) Uiso .29 O27 .4690(5) .3028(4) .3000(3) .0766(9) Uiso .24 O28 .4158(4) .2589(2) .29189(19) .0917(6) Uiso .42 O29 .3251(4) .2289(3) .2642(2) .1055(8) Uiso .35 F36 .3161(6) .2120(4) .3286(3) .1097(13) Uiso .18 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 .05604(9) .03569(7) .04817(8) -.00915(7) .04809(8) -.00507(7) O4 .0547(4) .0366(3) .0471(3) -.0074(2) .0461(3) -.0020(2) O19 .0585(4) .0716(4) .0663(4) .0057(3) .0534(4) .0178(3) N1 .0472(4) .0374(4) .0428(4) -.0066(3) .0400(4) -.0042(3) N2 .0573(5) .0389(4) .0508(4) -.0049(3) .0484(4) -.0009(3) N7 .0419(4) .0343(3) .0405(4) -.0055(3) .0365(4) -.0043(3) N13 .0909(6) .0428(5) .0781(5) -.0145(4) .0780(6) -.0069(4) C5 .0442(5) .0377(4) .0402(5) -.0035(3) .0374(5) .0013(3) C3 .0492(5) .0365(4) .0428(5) -.0028(4) .0408(5) .0002(4) C6 .0426(5) .0391(4) .0394(4) -.0048(4) .0366(4) -.0020(4) C8 .0586(6) .0453(5) .0528(5) -.0083(4) .0497(5) -.0047(4) C9 .0721(7) .0436(5) .0629(6) -.0144(5) .0594(6) -.0166(5) C10 .0845(7) .0562(6) .0669(6) -.0112(5) .0699(7) -.0109(5) C11 .0713(6) .0476(6) .0599(6) -.0061(4) .0603(6) -.0027(4) C12 .0474(5) .0331(4) .0447(5) -.0023(3) .0392(5) .0031(3) C14 .1010(9) .0571(6) .0951(9) -.0167(6) .0902(9) -.0044(6) C15 .0733(8) .0455(6) .0786(7) -.0179(5) .0628(7) -.0053(5) C16 .0938(9) .0475(6) .0810(8) -.0183(5) .0736(8) -.0217(5) C17 .0813(7) .0470(5) .0670(6) -.0087(5) .0663(7) -.0077(4) S20 .05818(18) .0833(2) .06017(17) .00497(14) .05187(17) -.00015(14) C30 .0577(8) .0894(9) .0721(8) .0134(6) .0505(8) .0163(7) 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 'Waasmaier & Kirfel, 1995' 'H ' 'H ' .0000 .0000 'Waasmaier & Kirfel, 1995' 'F ' 'F ' .0171 .0103 'Waasmaier & Kirfel, 1995' 'N ' 'N ' .0061 .0033 'Waasmaier & Kirfel, 1995' 'O ' 'O ' .0106 .0060 'Waasmaier & Kirfel, 1995' 'S ' 'S ' .1246 .1234 'Waasmaier & Kirfel, 1995' Cu Cu .3201 1.2651 'Waasmaier & Kirfel, 1995' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O19 Cu1 N1 88.72(2) ? O19 Cu1 N7 93.01(2) y N1 Cu1 N7 81.12(3) y C5 O4 C3 102.52(6) y N2 N1 C5 107.66(6) y N1 N2 C3 105.13(6) y C6 N7 C8 117.56(7) y C12 N13 C14 115.20(8) y O4 C5 N1 111.86(6) y O4 C5 C6 125.59(7) y N1 C5 C6 122.55(7) y O4 C3 N2 112.83(6) y O4 C3 C12 119.45(7) y N2 C3 C12 127.70(7) y N7 C6 C5 110.69(6) y N7 C6 C11 122.91(7) y C5 C6 C11 126.39(7) y N7 C8 C9 121.86(8) y C8 C9 C10 119.46(8) y C9 C10 C11 119.43(9) y C6 C11 C10 118.78(8) y N13 C12 C3 115.43(7) y N13 C12 C17 124.60(7) y C3 C12 C17 119.93(8) y N13 C14 C15 124.71(10) y C14 C15 C16 118.67(9) y C15 C16 C17 119.14(9) y C12 C17 C16 117.66(9) y 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 O19 . . 2.3125(6) y Cu1 N7 . . 2.0579(5) y Cu1 N1 . . 1.9926(5) y O4 C5 . . 1.3418(9) y O4 C3 . . 1.3762(9) y N1 N2 . . 1.3894(9) y N1 C5 . . 1.2986(10) y N2 C3 . . 1.2895(10) y N7 C6 . . 1.3545(10) y N7 C8 . . 1.3268(10) y N13 C12 . . 1.3338(11) y N13 C14 . . 1.3347(13) y C5 C6 . . 1.4509(11) y C3 C12 . . 1.4629(10) y C6 C11 . . 1.3704(11) y C8 C9 . . 1.3880(13) y C9 C10 . . 1.3640(13) y C10 C11 . . 1.3564(12) y C12 C17 . . 1.3642(12) y C14 C15 . . 1.3552(15) y C15 C16 . . 1.355(2) y C16 C17 . . 1.3830(13) y