#------------------------------------------------------------------------------ #$Date: 2011-09-10 05:16:28 +0200 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006453.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_2006453 loop_ _publ_author_name 'Halasyamani, S.' 'Heier, K. R.' 'Stern, C. L.' 'Poeppelmeier, K. R.' _publ_section_title ; CuW(py)~2~(H~2~ O)~2~O~2~F~4~ and CuW(py)~4~O~2~F~4~ ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1240 _journal_page_last 1244 _journal_volume 53 _journal_year 1997 _chemical_formula_moiety '[Cu(C~5~H~5~N)~4~] ^2+^ [WO~2~F~4~] ^2-^' _chemical_formula_sum 'C20 H20 Cu F4 N4 O2 W' _chemical_formula_weight 671.79 _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 97.33(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.450(2) _cell_length_b 13.396(3) _cell_length_c 16.067(7) _cell_measurement_reflns_used 25 _cell_measurement_temperature 153.2 _cell_measurement_theta_max 11.9 _cell_measurement_theta_min 10.0 _cell_volume 2230.8(12) _computing_cell_refinement 'DIRDIF92 (Beurskens et al., 1992)' _computing_data_collection 'CAD4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1992)' _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 153.2 _diffrn_measurement_device CAD4 _diffrn_measurement_method '\w/\q scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.04 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 2167 _diffrn_reflns_theta_max 24.97 _diffrn_standards_decay_% -0.9 _diffrn_standards_interval_count 90 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 6.17 _exptl_absorpt_correction_T_max 0.25 _exptl_absorpt_correction_T_min 0.15 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa_analytical _exptl_crystal_colour blue _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_meas 1.90(5) _exptl_crystal_density_method 'flotation pycnometry' _exptl_crystal_description faceted _exptl_crystal_F_000 1292.00 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.26 _refine_diff_density_max 1.0 _refine_diff_density_min -2.3 _refine_ls_extinction_coef 25.49971 _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_goodness_of_fit_obs 4.45 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 149 _refine_ls_number_reflns 1730 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.038 _refine_ls_shift/esd_max 0.10 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1/\s^2^(F)' _refine_ls_wR_factor_obs 0.050 _reflns_number_observed 1730 _reflns_number_total 2049 _reflns_observed_criterion >3\s(I) _[local]_cod_data_source_file bk1279.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M 'C 2/c ' _cod_original_cell_volume 2230.8(10) _cod_database_code 2006453 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 W 0.0224(3) 0.0284(3) 0.0375(3) -0.0082(2) -0.0022(2) -0.0085(2) Cu 0.0142(6) 0.0210(7) 0.0139(6) -0.0004(5) 0.0044(5) 0.0008(5) X1 0.032(3) 0.027(3) 0.006(2) 0.005(2) 0.008(2) 0.000(2) X2 0.035(3) 0.039(3) 0.030(3) 0.008(3) 0.017(2) 0.007(2) X3 0.017(2) 0.031(3) 0.030(3) -0.004(2) -0.003(2) -0.013(2) N1 0.014(3) 0.023(3) 0.009(3) 0.001(3) 0.002(2) 0.006(3) N2 0.016(3) 0.024(4) 0.018(3) 0.000(3) 0.000(2) -0.002(3) C1 0.019(4) 0.025(4) 0.028(4) 0.003(3) 0.007(3) 0.000(4) C2 0.036(5) 0.030(5) 0.029(5) -0.005(4) -0.002(4) -0.004(4) C3 0.026(4) 0.036(5) 0.036(5) -0.013(4) -0.004(4) 0.003(4) C4 0.011(4) 0.026(5) 0.074(7) -0.004(3) 0.009(4) 0.007(5) C5 0.016(4) 0.021(4) 0.040(5) 0.000(3) 0.004(4) 0.005(4) C6 0.025(4) 0.024(4) 0.027(4) 0.005(4) 0.006(3) -0.001(4) C7 0.034(5) 0.031(5) 0.027(4) 0.013(4) -0.001(4) 0.005(4) C8 0.034(5) 0.046(5) 0.015(4) 0.007(4) 0.007(3) 0.004(4) C9 0.033(5) 0.042(6) 0.022(4) 0.010(4) 0.008(4) 0.002(4) C10 0.022(4) 0.032(5) 0.027(4) 0.011(4) 0.008(3) 0.005(4) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type W 0.0000 0.5000 0.0000 0.0299(2) Uani Cu 0.2500 0.2500 0.0000 0.0161(3) Uani X1 0.1185(4) 0.3931(3) 0.0020(2) 0.0210(10) Uani X2 0.0477(5) 0.5452(4) -0.1007(3) 0.0330(10) Uani X3 0.1291(4) 0.5811(4) 0.0579(3) 0.0260(10) Uani N1 0.4070(5) 0.3346(5) 0.0347(3) 0.016(2) Uani N2 0.2394(6) 0.2289(5) 0.1266(4) 0.020(2) Uani C1 0.4042(7) 0.4153(6) 0.0823(5) 0.024(2) Uani C2 0.5128(9) 0.4689(7) 0.1134(5) 0.033(2) Uani C3 0.6310(8) 0.4394(7) 0.0920(5) 0.033(2) Uani C4 0.6370(7) 0.3573(6) 0.0399(6) 0.037(3) Uani C5 0.5246(7) 0.3071(6) 0.0111(5) 0.026(2) Uani C6 0.3089(7) 0.1570(6) 0.1670(5) 0.025(2) Uani C7 0.3115(8) 0.1420(6) 0.2521(5) 0.031(2) Uani C8 0.2385(8) 0.2026(7) 0.2969(5) 0.031(2) Uani C9 0.1679(8) 0.2777(7) 0.2557(5) 0.032(2) Uani C10 0.1688(8) 0.2885(6) 0.1706(5) 0.027(2) Uani H1 0.3230 0.4351 0.0957 0.0285 equiv H2 0.5063 0.5250 0.1488 0.0392 equiv H3 0.7072 0.4749 0.1127 0.0401 equiv H4 0.7173 0.3359 0.0243 0.0442 equiv H5 0.5283 0.2522 -0.0259 0.0307 equiv H6 0.3586 0.1144 0.1364 0.0300 equiv H7 0.3630 0.0904 0.2796 0.0376 equiv H8 0.2372 0.1923 0.3553 0.0377 equiv H9 0.1189 0.3218 0.2855 0.0384 equiv H10 0.1179 0.3397 0.1420 0.0320 equiv loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source W -0.849 6.872 'International Tables' Cu 0.320 1.265 'International Tables' N 0.006 0.003 'International Tables' C 0.003 0.002 'International Tables' H 0.000 0.000 'International Tables' O 0.011 0.006 'International Tables' F 0.017 0.010 'International Tables' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -6 4 -5 -3 2 -4 4 2 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 X1 W X1 ? 5_565 180.0 yes X1 W X2 ? ? 90.7(2) no X1 W X2 ? 5_565 89.3(2) no X1 W X3 ? ? 90.1(2) no X1 W X3 ? 5_565 89.9(2) no X1 W X2 ? 5_565 89.3(2) no X1 W X2 5_565 5_565 90.7(2) no X1 W X3 5_565 5_565 89.9(2) no X1 W X3 ? 5_565 90.1(2) no X2 W X2 ? 5_565 180.0 yes X2 W X3 ? ? 89.3(2) no X2 W X3 ? 5_565 90.7(2) no X2 W X3 5_565 ? 90.7(2) no X2 W X3 5_565 5_565 89.3(2) no X3 W X3 ? 5_565 180.0 yes X1 Cu X1 7 ? 180.0 no X1 Cu N1 ? ? 89.8(2) yes X1 Cu N1 7 ? 90.2(2) no X1 Cu N2 ? ? 89.8(2) yes X1 Cu N2 7 ? 90.2(2) no X1 Cu N1 ? 7 90.2(2) no X1 Cu N1 7 7 89.8(2) no X1 Cu N2 7 7 90.2(2) no X1 Cu N2 ? 7 89.8(2) no N1 Cu N1 ? 7_555 180.0 no N1 Cu N2 ? ? 87.1(2) yes N1 Cu N2 7 ? 92.9(2) no N1 Cu N2 7 7 92.9(2) no N1 Cu N2 ? 7 87.1(2) no N2 Cu N2 ? 7_555 180.00 no W X1 Cu ? ? 174.9(3) yes W X1 Cu ? ? 174.8787(2) no Cu N1 C1 ? ? 122.8(5) no Cu N1 C5 ? ? 119.7(5) no C1 N1 C5 ? ? 117.5(6) no Cu N2 C6 ? ? 119.0(5) no Cu N2 C10 ? ? 122.4(5) no C6 N2 C10 ? ? 118.5(6) no N1 C1 C2 ? ? 123.7(7) no C1 C2 C3 ? ? 118.5(8) no C2 C3 C4 ? ? 119.1(7) no C3 C4 C5 ? ? 119.1(7) no N1 C5 C4 ? ? 121.8(8) no N2 C6 C7 ? ? 122.1(7) no C6 C7 C8 ? ? 119.4(8) no C7 C8 C9 ? ? 118.8(7) no C8 C9 C10 ? ? 119.1(7) no N2 C10 C9 ? ? 122.2(7) no 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 W X1 ? 1.891(4) yes W X1 5_565 1.891(4) no W X2 ? 1.855(5) yes W X2 5_565 1.855(5) no W X3 ? 1.883(4) yes W X3 5_565 1.883(4) no Cu X1 ? 2.364(5) yes Cu X1 7 2.364(5) no Cu N1 ? 2.014(6) yes Cu N1 7 2.014(6) no Cu N2 ? 2.071(6) yes Cu N2 7 2.071(6) no N1 C1 ? 1.327(10) no N1 C5 ? 1.382(9) no N2 C6 ? 1.326(10) no N2 C10 ? 1.347(10) no C1 C2 ? 1.380(10) no C2 C3 ? 1.380(10) no C3 C4 ? 1.390(10) no C4 C5 ? 1.380(10) no C6 C7 ? 1.380(10) no C7 C8 ? 1.380(10) no C8 C9 ? 1.370(10) no C9 C10 ? 1.380(10) no