#------------------------------------------------------------------------------ #$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/48/2204839.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_2204839 loop_ _publ_author_name 'Zeng, Xi-Rui' 'Huang, Lin' 'Lei, Liang-Ping' 'Tang, Shi-Hua' 'Peng, Shie-Ming' 'Lee, Gene-Hsiang' _publ_section_title (Acetato-\k^2^O,O')(di-2-pyridylamine-\kN)(trifluoroacetato-\kO)copper(II) _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m57 _journal_page_last m59 _journal_paper_doi 10.1107/S1600536804031514 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Cu (C2 F3 O2) (C2 H3 O2) (C10 H9 N3)]' _chemical_formula_moiety 'C14 H12 Cu F3 N3 O4' _chemical_formula_sum 'C14 H12 Cu F3 N3 O4' _chemical_formula_weight 406.81 _chemical_name_systematic ; (Acetato-\k^2^O,O')(di-2-pyridylamine-\kN)(trifluoroacetato-\kO)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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 87.199(15) _cell_angle_beta 84.592(14) _cell_angle_gamma 73.620(11) _cell_formula_units_Z 2 _cell_length_a 8.2533(11) _cell_length_b 8.7907(15) _cell_length_c 11.3643(14) _cell_measurement_reflns_used 2990 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24.97 _cell_measurement_theta_min 1.95 _cell_volume 787.3(2) _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL (Bruker, 2000)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Enraf--Nonius TurboCAD-4' _diffrn_measurement_method 'non-profiled \w/2\q' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0124 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 2985 _diffrn_reflns_theta_full 24.97 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_min 1.80 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.446 _exptl_absorpt_correction_T_max 0.612 _exptl_absorpt_correction_T_min 0.456 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 410 _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.34 _refine_diff_density_max 0.608 _refine_diff_density_min -0.401 _refine_ls_extinction_coef 0.014(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 239 _refine_ls_number_reflns 2775 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0371 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc 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_gt 0.1162 _refine_ls_wR_factor_ref 0.1252 _reflns_number_gt 2332 _reflns_number_total 2775 _reflns_threshold_expression I>2\s(I) _cod_data_source_file br6170.cif _cod_data_source_block I _cod_database_code 2204839 _cod_database_fobs_code 2204839 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_type_symbol Cu 0.08831(4) 0.12749(4) 0.66054(3) 0.0454(2) Uani d . 1 Cu F1 0.3557(6) 0.4085(4) 0.9629(3) 0.1261(12) Uani d . 1 F F2 0.1474(5) 0.3206(5) 0.9823(3) 0.1369(14) Uani d . 1 F F3 0.3755(6) 0.1732(4) 0.9214(3) 0.1342(14) Uani d . 1 F O1 0.2450(3) -0.0781(3) 0.7132(2) 0.0589(6) Uani d . 1 O O2 0.0431(3) 0.0627(3) 0.82814(19) 0.0571(6) Uani d . 1 O O3 0.2590(3) 0.2685(3) 0.7143(2) 0.0583(6) Uani d . 1 O O4 0.1937(4) 0.5188(3) 0.7713(2) 0.0826(9) Uani d . 1 O N1 0.1539(3) 0.1155(3) 0.4916(2) 0.0439(6) Uani d . 1 N N2 -0.0701(3) 0.3345(3) 0.4376(2) 0.0504(6) Uani d . 1 N H2B -0.1117 0.3905 0.3777 0.076(12) Uiso d R 1 H N3 -0.1113(3) 0.3081(3) 0.6457(2) 0.0460(6) Uani d . 1 N C1 0.2967(4) 0.0005(4) 0.4556(3) 0.0568(8) Uani d . 1 C H1A 0.3542 -0.0679 0.5125 0.044(8) Uiso d R 1 H C2 0.3587(5) -0.0194(5) 0.3408(3) 0.0654(10) Uani d . 1 C H2A 0.4571 -0.0990 0.3199 0.075(12) Uiso d R 1 H C3 0.2736(5) 0.0818(5) 0.2560(3) 0.0642(9) Uani d . 1 C H3A 0.3136 0.0701 0.1767 0.084(13) Uiso d R 1 H C4 0.1302(4) 0.1983(4) 0.2887(3) 0.0562(8) Uani d . 1 C H4A 0.0718 0.2665 0.2320 0.051(9) Uiso d R 1 H C5 0.0724(4) 0.2143(4) 0.4084(3) 0.0449(7) Uani d . 1 C C6 -0.1599(4) 0.3840(3) 0.5435(3) 0.0436(6) Uani d . 1 C C7 -0.3018(4) 0.5138(4) 0.5415(3) 0.0520(7) Uani d . 1 C H7A -0.3327 0.5651 0.4700 0.049(9) Uiso d R 1 H C8 -0.3961(4) 0.5671(4) 0.6440(3) 0.0578(8) Uani d . 1 C H8A -0.4915 0.6541 0.6434 0.059(10) Uiso d R 1 H C9 -0.3466(5) 0.4888(5) 0.7499(3) 0.0637(9) Uani d . 1 C H9A -0.4092 0.5218 0.8210 0.079(13) Uiso d R 1 H C10 -0.2062(5) 0.3641(4) 0.7474(3) 0.0615(9) Uani d . 1 C H10A -0.1728 0.3136 0.8186 0.062(11) Uiso d R 1 H C11 0.1706(4) -0.0558(4) 0.8149(3) 0.0513(7) Uani d . 1 C C12 0.2300(6) -0.1661(5) 0.9162(3) 0.0712(11) Uani d . 1 C H12A 0.1843 -0.2551 0.9161 0.13(2) Uiso d R 1 H H12B 0.3515 -0.2027 0.9089 0.15(3) Uiso d R 1 H H12C 0.1921 -0.1109 0.9890 0.084(13) Uiso d R 1 H C13 0.2405(4) 0.3735(4) 0.7860(3) 0.0476(7) Uani d . 1 C C14 0.2836(5) 0.3196(4) 0.9131(3) 0.0627(9) Uani d . 1 C 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 Cu 0.0482(3) 0.0486(3) 0.0346(3) -0.00578(17) -0.00511(16) 0.00166(16) F1 0.216(4) 0.127(2) 0.0733(18) -0.093(2) -0.078(2) 0.0247(16) F2 0.134(3) 0.214(4) 0.0616(17) -0.060(3) 0.0148(18) 0.022(2) F3 0.196(4) 0.0920(19) 0.086(2) 0.017(2) -0.058(2) 0.0163(16) O1 0.0673(15) 0.0525(13) 0.0486(13) -0.0047(11) -0.0030(11) 0.0046(10) O2 0.0623(14) 0.0589(13) 0.0421(12) -0.0061(11) -0.0015(10) 0.0057(10) O3 0.0631(14) 0.0652(14) 0.0482(13) -0.0187(11) -0.0050(11) -0.0135(11) O4 0.122(2) 0.0575(15) 0.0509(15) 0.0101(15) -0.0287(15) -0.0032(12) N1 0.0423(13) 0.0514(14) 0.0373(13) -0.0105(11) -0.0055(10) -0.0062(11) N2 0.0551(15) 0.0571(15) 0.0321(13) -0.0028(12) -0.0098(11) 0.0005(11) N3 0.0455(14) 0.0522(14) 0.0372(13) -0.0081(11) -0.0050(10) -0.0008(10) C1 0.0497(18) 0.066(2) 0.0480(18) -0.0033(15) -0.0080(14) -0.0048(15) C2 0.057(2) 0.073(2) 0.056(2) -0.0010(17) -0.0006(16) -0.0157(18) C3 0.067(2) 0.083(2) 0.0425(18) -0.0199(19) 0.0032(16) -0.0127(17) C4 0.059(2) 0.071(2) 0.0364(16) -0.0143(16) -0.0074(14) 0.0000(15) C5 0.0463(16) 0.0541(16) 0.0369(15) -0.0162(13) -0.0080(12) -0.0035(13) C6 0.0454(15) 0.0511(16) 0.0372(15) -0.0161(13) -0.0096(12) -0.0031(12) C7 0.0512(18) 0.0579(18) 0.0430(17) -0.0062(14) -0.0134(14) -0.0001(14) C8 0.0479(18) 0.0638(19) 0.056(2) -0.0060(15) -0.0062(15) -0.0018(15) C9 0.056(2) 0.075(2) 0.0490(19) -0.0013(17) 0.0011(16) -0.0075(17) C10 0.062(2) 0.075(2) 0.0382(17) -0.0054(17) -0.0032(15) 0.0021(15) C11 0.0601(19) 0.0496(17) 0.0439(17) -0.0143(15) -0.0080(14) 0.0025(14) C12 0.096(3) 0.058(2) 0.051(2) -0.007(2) -0.013(2) 0.0098(17) C13 0.0461(16) 0.0544(18) 0.0398(16) -0.0082(13) -0.0080(12) -0.0026(13) C14 0.080(2) 0.063(2) 0.0457(19) -0.0189(18) -0.0149(17) 0.0054(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 _geom_angle_publ_flag N1 Cu N3 94.58(11) yes N1 Cu O2 161.08(11) ? N3 Cu O2 99.61(10) yes N1 Cu O1 98.99(10) yes N3 Cu O1 162.51(11) ? O2 Cu O1 64.90(9) yes N1 Cu O3 99.66(9) yes N3 Cu O3 96.25(10) yes O2 Cu O3 91.21(10) yes O1 Cu O3 92.31(10) yes N1 Cu C11 131.08(11) ? N3 Cu C11 131.97(11) ? O2 Cu C11 32.55(10) ? O1 Cu C11 32.43(10) ? O3 Cu C11 90.44(10) ? C11 O1 Cu 88.59(19) ? C11 O2 Cu 89.01(19) ? C13 O3 Cu 133.6(2) ? C5 N1 C1 117.8(3) ? C5 N1 Cu 125.2(2) ? C1 N1 Cu 117.0(2) ? C5 N2 C6 132.8(3) ? C5 N2 H2B 113.6 ? C6 N2 H2B 113.6 ? C6 N3 C10 117.6(3) ? C6 N3 Cu 125.2(2) ? C10 N3 Cu 117.2(2) ? N1 C1 C2 123.2(3) ? N1 C1 H1A 118.3 ? C2 C1 H1A 118.4 ? C1 C2 C3 118.6(3) ? C1 C2 H2A 120.6 ? C3 C2 H2A 120.8 ? C4 C3 C2 119.8(3) ? C4 C3 H3A 120.1 ? C2 C3 H3A 120.1 ? C3 C4 C5 119.3(3) ? C3 C4 H4A 120.3 ? C5 C4 H4A 120.5 ? N1 C5 N2 121.3(3) ? N1 C5 C4 121.3(3) ? N2 C5 C4 117.4(3) ? N3 C6 N2 120.8(3) ? N3 C6 C7 121.3(3) ? N2 C6 C7 117.8(3) ? C8 C7 C6 120.2(3) ? C8 C7 H7A 119.8 ? C6 C7 H7A 120.0 ? C7 C8 C9 118.7(3) ? C7 C8 H8A 120.7 ? C9 C8 H8A 120.6 ? C10 C9 C8 118.9(3) ? C10 C9 H9A 120.5 ? C8 C9 H9A 120.5 ? C9 C10 N3 123.3(3) ? C9 C10 H10A 118.4 ? N3 C10 H10A 118.3 ? O2 C11 O1 117.2(3) ? O2 C11 C12 121.3(3) ? O1 C11 C12 121.5(3) ? O2 C11 Cu 58.44(16) ? O1 C11 Cu 58.99(16) ? C12 C11 Cu 176.1(3) ? C11 C12 H12A 109.6 ? C11 C12 H12B 109.6 ? H12A C12 H12B 109.5 ? C11 C12 H12C 109.3 ? H12A C12 H12C 109.5 ? H12B C12 H12C 109.5 ? O4 C13 O3 129.4(3) ? O4 C13 C14 113.9(3) ? O3 C13 C14 116.7(3) ? F1 C14 F3 108.7(4) ? F1 C14 F2 105.4(4) ? F3 C14 F2 103.0(4) ? F1 C14 C13 113.8(3) ? F3 C14 C13 113.5(3) ? F2 C14 C13 111.5(3) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Cu N1 1.945(2) yes Cu N3 1.953(3) yes Cu O2 1.993(2) yes Cu O1 2.005(2) yes Cu O3 2.262(2) yes Cu C11 2.338(3) ? F1 C14 1.286(5) ? F2 C14 1.308(5) ? F3 C14 1.301(5) ? O1 C11 1.254(4) ? O2 C11 1.258(4) ? O3 C13 1.229(4) ? O4 C13 1.234(4) ? N1 C5 1.345(4) ? N1 C1 1.362(4) ? N2 C5 1.368(4) ? N2 C6 1.374(4) ? N2 H2B 0.8600 ? N3 C6 1.348(4) ? N3 C10 1.363(4) ? C1 C2 1.357(5) ? C1 H1A 0.9299 ? C2 C3 1.381(5) ? C2 H2A 0.9300 ? C3 C4 1.363(5) ? C3 H3A 0.9300 ? C4 C5 1.398(4) ? C4 H4A 0.9300 ? C6 C7 1.387(4) ? C7 C8 1.364(5) ? C7 H7A 0.9300 ? C8 C9 1.393(5) ? C8 H8A 0.9300 ? C9 C10 1.351(5) ? C9 H9A 0.9300 ? C10 H10A 0.9300 ? C11 C12 1.494(4) ? C12 H12A 0.9600 ? C12 H12B 0.9600 ? C12 H12C 0.9601 ? C13 C14 1.539(4) ?