#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2211417.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_2211417 loop_ _publ_author_name 'Becker, Richard' 'Berger, Helmuth' _publ_section_title ; Reinvestigation of CuSe~2~O~5~ ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i256 _journal_page_last i257 _journal_volume 62 _journal_year 2006 _chemical_formula_moiety 'Cu O5 Se2' _chemical_formula_sum 'Cu O5 Se2' _chemical_formula_weight 301.46 _chemical_name_systematic 'Copper(II) diselenium(IV) pentaoxide' _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' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 111.953(15) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 12.3869(19) _cell_length_b 4.8699(7) _cell_length_c 7.9917(13) _cell_measurement_reflns_used 1839 _cell_measurement_temperature 292(3) _cell_measurement_theta_max 0.64224 _cell_measurement_theta_min 0.21823 _cell_volume 447.13(13) _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2005)' _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2005)' _computing_data_reduction 'CrysAlis RED' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 292(3) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Oxford Xcalibur3 Diffractometer' _diffrn_measurement_method '\w scans at different \f' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 1839 _diffrn_reflns_theta_full 29.88 _diffrn_reflns_theta_max 29.88 _diffrn_reflns_theta_min 4.54 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 21.079 _exptl_absorpt_correction_T_max 0.64224 _exptl_absorpt_correction_T_min 0.21823 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; [X-RED32 (Stoe, 2001) and X-SHAPE (Stoe, 1999)' ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 4.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 548 _exptl_crystal_size_max 0.317 _exptl_crystal_size_mid 0.079 _exptl_crystal_size_min 0.040 _refine_diff_density_max 1.150 _refine_diff_density_min -0.949 _refine_ls_extinction_coef 0.0038(6) _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 0.989 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 40 _refine_ls_number_reflns 655 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.989 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0276 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.0701 _reflns_number_gt 571 _reflns_number_total 655 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file hb2184.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M C2/c _[local]_cod_cif_authors_sg_Hall -C2yc _cod_original_cell_volume 447.13(12) _cod_database_code 2211417 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_type_symbol _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 Se Se 0.13990(4) 0.06450(9) 0.82983(5) 0.01230(18) Uani d . 1 Cu Cu 0.0000 0.5000 0.5000 0.0148(2) Uani d S 1 O O1 0.0000 -0.1180(10) 0.7500 0.0151(9) Uani d S 1 O O2 0.1256(3) 0.2753(8) 0.6593(4) 0.0222(7) Uani d . 1 O O3 0.1262(3) 0.2725(7) 0.9874(4) 0.0206(7) Uani d . 1 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 Se 0.0089(2) 0.0126(3) 0.0148(2) 0.00123(15) 0.00365(15) -0.00009(14) Cu 0.0102(4) 0.0165(4) 0.0168(4) -0.0014(3) 0.0042(3) 0.0030(3) O1 0.0093(19) 0.016(2) 0.0192(19) 0.000 0.0039(16) 0.000 O2 0.0140(15) 0.0255(19) 0.0246(15) 0.0026(14) 0.0044(12) 0.0140(14) O3 0.0120(14) 0.0213(18) 0.0267(15) 0.0020(13) 0.0052(12) -0.0098(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O2 Se O3 . . 103.50(19) O2 Se O1 . . 102.50(14) O3 Se O1 . . 101.91(14) O2 Cu O2 5_566 . 180.0000(10) O2 Cu O3 5_566 6_565 96.16(14) O2 Cu O3 . 6_565 83.84(14) O2 Cu O3 5_566 2_556 83.84(14) O2 Cu O3 . 2_556 96.16(14) O3 Cu O3 6_565 2_556 180.0(2) O2 Cu O1 5_566 1_565 82.90(11) O2 Cu O1 . 1_565 97.10(11) O3 Cu O1 6_565 1_565 82.52(11) O3 Cu O1 2_556 1_565 97.48(11) O2 Cu O1 5_566 5_556 97.10(11) O2 Cu O1 . 5_556 82.90(11) O3 Cu O1 6_565 5_556 97.48(11) O3 Cu O1 2_556 5_556 82.52(11) O1 Cu O1 1_565 5_556 180.0 Se O1 Se . 2_556 122.1(3) Se O1 Cu . 1_545 109.02(6) Se O1 Cu 2_556 1_545 109.49(6) Se O1 Cu . 2_546 109.49(6) Se O1 Cu 2_556 2_546 109.02(6) Cu O1 Cu 1_545 2_546 94.09(15) Se O1 Cu . 2_556 66.41(12) Se O1 Cu 2_556 2_556 66.04(12) Cu O1 Cu 1_545 2_556 166.53(11) Cu O1 Cu 2_546 2_556 99.38(3) Se O1 Cu . . 66.04(12) Se O1 Cu 2_556 . 66.41(12) Cu O1 Cu 1_545 . 99.38(3) Cu O1 Cu 2_546 . 166.53(11) Cu O1 Cu 2_556 . 67.16(8) Se O2 Cu . . 134.49(19) Se O2 Cu . 2_556 62.17(10) Cu O2 Cu . 2_556 82.18(11) Se O3 Cu . 2_556 133.77(17) Se O3 Se . 7_557 100.73(13) Cu O3 Se 2_556 7_557 120.04(14) Se O3 Cu . . 61.39(9) Cu O3 Cu 2_556 . 81.71(10) Se O3 Cu 7_557 . 113.52(10) 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 Se O2 . 1.662(3) yes Se O3 . 1.673(3) yes Se O1 . 1.837(2) yes Cu O2 5_566 1.938(3) n Cu O2 . 1.938(3) yes Cu O3 6_565 1.949(3) yes Cu O3 2_556 1.949(3) n Cu O1 1_565 2.730(3) yes Cu O1 5_556 2.730(3) n O1 Se 2_556 1.837(2) n O1 Cu 1_545 2.730(3) n O1 Cu 2_546 2.730(3) n O1 Cu 2_556 3.612(4) n O2 Cu 2_556 3.768(3) n O3 Cu 2_556 1.949(3) n O3 Se 7_557 2.827(3) n