#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/83/2008300.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_2008300 loop_ _publ_author_name 'Stoll, Petra' 'N\"ather, Christian' 'Je\&s, Inke' 'Bensch, Wolfgang' _publ_section_title ; KCu~4~Se~3~ ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 286 _journal_page_last 288 _journal_paper_doi 10.1107/S0108270198014358 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac 'K Cu4 Se3' _chemical_formula_sum 'Cu4 K Se3' _chemical_formula_weight 530.14 _chemical_name_common 'Potassium tetracopper triselenide' _chemical_name_systematic ; ? ; _space_group_IT_number 123 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 4 2' _symmetry_space_group_name_H-M 'P 4/m m m' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 1 _cell_length_a 4.0188(3) _cell_length_b 4.0188(3) _cell_length_c 9.7200(10) _cell_measurement_reflns_used 82 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.5 _cell_measurement_theta_min 11 _cell_volume 156.99(2) _computing_cell_refinement 'Stoe DIF4' _computing_data_collection 'Stoe DIF4 (Stoe & Cie, 1992a)' _computing_data_reduction 'Stoe REDU4 (Stoe & Cie, 1992b)' _computing_molecular_graphics 'XP in SHELXTL/PC (Siemens, 1990)' _computing_publication_material 'CIFTAB in SHELXL93' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Stoe AED-II 4-circle' _diffrn_measurement_method '\w/\q scans' _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 0.058 _diffrn_reflns_av_sigmaI/netI 0.032 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 1026 _diffrn_reflns_theta_max 29.93 _diffrn_reflns_theta_min 5.07 _diffrn_standards_decay_% negligible _diffrn_standards_interval_time 120 _diffrn_standards_number 4 _exptl_absorpt_coefficient_mu 31.277 _exptl_absorpt_correction_T_max 0.535 _exptl_absorpt_correction_T_min 0.223 _exptl_absorpt_correction_type 'analytical (XP in SHELXTL/PC; Siemens, 1990)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 5.608 _exptl_crystal_description plates _exptl_crystal_F_000 237 _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.839 _refine_diff_density_min -1.002 _refine_ls_extinction_coef 0.070(10) _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_goodness_of_fit_all 1.170 _refine_ls_goodness_of_fit_obs 1.186 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 13 _refine_ls_number_reflns 174 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.170 _refine_ls_restrained_S_obs 1.186 _refine_ls_R_factor_all 0.028 _refine_ls_R_factor_obs 0.024 _refine_ls_shift/esd_max <0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0368P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.062 _refine_ls_wR_factor_obs 0.060 _reflns_number_observed 160 _reflns_number_total 174 _reflns_observed_criterion I>2sigma(I) _cod_data_source_file sk1247.cif _cod_data_source_block ps74a _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0368P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0368P)^2^] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M P4/mmm _cod_original_formula_sum 'K Cu4 Se3' _cod_database_code 2008300 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' 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 0.0266(5) 0.0173(4) 0.0276(5) 0 0 0 Se1 0.0150(4) 0.0150(4) 0.0117(4) 0 0 0 Se2 0.0140(3) 0.0140(3) 0.0148(4) 0 0 0 K 0.0202(7) 0.0202(7) 0.0226(10) 0 0 0 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 _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Cu 0 0.5 0.16146(8) 0.0238(3) Uani d S 1 . Cu Se1 0.5 0.5 0 0.0139(3) Uani d S 1 . Se Se2 0 0 0.30109(7) 0.0143(3) Uani d S 1 . Se K 0.5 0.5 0.5 0.0210(5) Uani d S 1 . K loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 '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' Se Se -0.0929 2.2259 '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 Se2 Cu Se2 1_565 . 111.93(4) y Se2 Cu Se1 1_565 1_455 110.152(8) n Se2 Cu Se1 . 1_455 110.152(8) y Se2 Cu Se1 1_565 . 110.152(8) n Se2 Cu Se1 . . 110.152(8) n Se1 Cu Se1 1_455 . 104.02(3) y Se2 Cu Cu 1_565 3 125.872(10) n Se2 Cu Cu . 3 54.128(10) n Se1 Cu Cu 1_455 3 56.133(7) n Se1 Cu Cu . 3 123.867(7) n Se2 Cu Cu 1_565 3_665 54.128(10) n Se2 Cu Cu . 3_665 125.872(10) n Se1 Cu Cu 1_455 3_665 123.867(7) n Se1 Cu Cu . 3_665 56.133(7) n Cu Cu Cu 3 3_665 180.00(6) n Se2 Cu Cu 1_565 3_655 125.872(10) n Se2 Cu Cu . 3_655 54.128(10) n Se1 Cu Cu 1_455 3_655 123.867(7) n Se1 Cu Cu . 3_655 56.133(7) n Cu Cu Cu 3 3_655 90.0 n Cu Cu Cu 3_665 3_655 90.0 n Se2 Cu Cu 1_565 3_565 54.128(10) n Se2 Cu Cu . 3_565 125.872(10) n Se1 Cu Cu 1_455 3_565 56.133(7) n Se1 Cu Cu . 3_565 123.867(7) n Cu Cu Cu 3 3_565 90.0 n Cu Cu Cu 3_665 3_565 90.0 n Cu Cu Cu 3_655 3_565 180.00(6) n Se2 Cu K 1_565 . 61.47(2) n Se2 Cu K . . 61.47(2) n Se1 Cu K 1_455 . 159.40(2) n Se1 Cu K . . 96.581(10) n Cu Cu K 3 . 111.624(4) n Cu Cu K 3_665 . 68.376(4) n Cu Cu K 3_655 . 68.376(4) n Cu Cu K 3_565 . 111.624(4) n Se2 Cu K 1_565 1_455 61.47(2) n Se2 Cu K . 1_455 61.47(2) n Se1 Cu K 1_455 1_455 96.581(10) n Se1 Cu K . 1_455 159.40(2) n Cu Cu K 3 1_455 68.376(4) n Cu Cu K 3_665 1_455 111.624(4) n Cu Cu K 3_655 1_455 111.624(4) n Cu Cu K 3_565 1_455 68.376(4) n K Cu K . 1_455 62.821(13) n Cu Se1 Cu 11 9_565 67.735(14) n Cu Se1 Cu 11 3_665 180.0 n Cu Se1 Cu 9_565 3_665 112.265(14) n Cu Se1 Cu 11 1_655 112.265(14) n Cu Se1 Cu 9_565 1_655 180.0 n Cu Se1 Cu 3_665 1_655 67.735(14) n Cu Se1 Cu 11 11_565 104.02(3) n Cu Se1 Cu 9_565 11_565 67.735(14) n Cu Se1 Cu 3_665 11_565 75.98(3) n Cu Se1 Cu 1_655 11_565 112.265(14) n Cu Se1 Cu 11 9_665 67.735(14) n Cu Se1 Cu 9_565 9_665 104.02(3) n Cu Se1 Cu 3_665 9_665 112.265(14) n Cu Se1 Cu 1_655 9_665 75.98(3) n Cu Se1 Cu 11_565 9_665 67.735(14) n Cu Se1 Cu 11 . 112.265(14) n Cu Se1 Cu 9_565 . 75.98(3) n Cu Se1 Cu 3_665 . 67.735(14) n Cu Se1 Cu 1_655 . 104.02(3) n Cu Se1 Cu 11_565 . 112.265(14) n Cu Se1 Cu 9_665 . 180.0 n Cu Se1 Cu 11 3_655 75.98(3) n Cu Se1 Cu 9_565 3_655 112.265(14) n Cu Se1 Cu 3_665 3_655 104.02(3) n Cu Se1 Cu 1_655 3_655 67.735(14) n Cu Se1 Cu 11_565 3_655 180.0 n Cu Se1 Cu 9_665 3_655 112.265(14) n Cu Se1 Cu . 3_655 67.735(14) n Cu Se2 Cu 3 1_545 71.74(2) n Cu Se2 Cu 3 3_655 111.93(4) n Cu Se2 Cu 1_545 3_655 71.74(2) n Cu Se2 Cu 3 . 71.74(2) n Cu Se2 Cu 1_545 . 111.93(4) n Cu Se2 Cu 3_655 . 71.74(2) n Cu Se2 K 3 . 143.065(4) n Cu Se2 K 1_545 . 143.065(4) n Cu Se2 K 3_655 . 80.233(14) n Cu Se2 K . . 80.233(13) n Cu Se2 K 3 1_455 80.233(13) n Cu Se2 K 1_545 1_455 143.065(4) n Cu Se2 K 3_655 1_455 143.065(4) n Cu Se2 K . 1_455 80.233(13) n K Se2 K . 1_455 71.553(9) n Cu Se2 K 3 1_445 80.233(13) n Cu Se2 K 1_545 1_445 80.233(13) n Cu Se2 K 3_655 1_445 143.065(4) n Cu Se2 K . 1_445 143.065(4) n K Se2 K . 1_445 111.54(2) n K Se2 K 1_455 1_445 71.553(9) n Cu Se2 K 3 1_545 143.065(4) n Cu Se2 K 1_545 1_545 80.233(13) n Cu Se2 K 3_655 1_545 80.233(13) n Cu Se2 K . 1_545 143.065(4) n K Se2 K . 1_545 71.553(9) n K Se2 K 1_455 1_545 111.54(2) n K Se2 K 1_445 1_545 71.553(9) n Se2 K Se2 9_666 . 180.0 n Se2 K Se2 9_666 9_566 71.553(9) n Se2 K Se2 . 9_566 108.447(9) n Se2 K Se2 9_666 9_656 71.553(9) n Se2 K Se2 . 9_656 108.447(9) n Se2 K Se2 9_566 9_656 111.54(2) n Se2 K Se2 9_666 9_556 111.54(2) n Se2 K Se2 . 9_556 68.46(2) n Se2 K Se2 9_566 9_556 71.553(9) n Se2 K Se2 9_656 9_556 71.553(9) n Se2 K Se2 9_666 1_665 68.46(2) n Se2 K Se2 . 1_665 111.54(2) n Se2 K Se2 9_566 1_665 108.447(9) n Se2 K Se2 9_656 1_665 108.447(9) n Se2 K Se2 9_556 1_665 180.0 n Se2 K Se2 9_666 1_565 108.447(9) n Se2 K Se2 . 1_565 71.553(9) n Se2 K Se2 9_566 1_565 68.46(2) n Se2 K Se2 9_656 1_565 180.0 n Se2 K Se2 9_556 1_565 108.447(9) n Se2 K Se2 1_665 1_565 71.553(9) n Se2 K Se2 9_666 1_655 108.447(9) n Se2 K Se2 . 1_655 71.553(9) n Se2 K Se2 9_566 1_655 180.0 n Se2 K Se2 9_656 1_655 68.46(2) n Se2 K Se2 9_556 1_655 108.447(9) n Se2 K Se2 1_665 1_655 71.553(9) n Se2 K Se2 1_565 1_655 111.54(2) n Se2 K Cu 9_666 3_655 141.700(8) n Se2 K Cu . 3_655 38.300(8) n Se2 K Cu 9_566 3_655 141.700(8) n Se2 K Cu 9_656 3_655 100.102(11) n Se2 K Cu 9_556 3_655 100.102(11) n Se2 K Cu 1_665 3_655 79.898(11) n Se2 K Cu 1_565 3_655 79.898(11) n Se2 K Cu 1_655 3_655 38.300(8) n Se2 K Cu 9_666 . 141.700(8) n Se2 K Cu . . 38.300(8) n Se2 K Cu 9_566 . 100.102(11) n Se2 K Cu 9_656 . 141.700(8) n Se2 K Cu 9_556 . 100.102(11) n Se2 K Cu 1_665 . 79.898(11) n Se2 K Cu 1_565 . 38.300(8) n Se2 K Cu 1_655 . 79.898(11) n Cu K Cu 3_655 . 43.249(9) n Se2 K Cu 9_666 9_666 38.300(8) n Se2 K Cu . 9_666 141.700(8) n Se2 K Cu 9_566 9_666 79.898(11) n Se2 K Cu 9_656 9_666 38.300(8) n Se2 K Cu 9_556 9_666 79.898(11) n Se2 K Cu 1_665 9_666 100.102(11) n Se2 K Cu 1_565 9_666 141.700(8) n Se2 K Cu 1_655 9_666 100.102(11) n Cu K Cu 3_655 9_666 136.751(9) n Cu K Cu . 9_666 180.0 n Se2 K Cu 9_666 11_566 38.300(8) n Se2 K Cu . 11_566 141.700(8) n Se2 K Cu 9_566 11_566 38.300(8) n Se2 K Cu 9_656 11_566 79.898(11) n Se2 K Cu 9_556 11_566 79.898(11) n Se2 K Cu 1_665 11_566 100.102(11) n Se2 K Cu 1_565 11_566 100.102(11) n Se2 K Cu 1_655 11_566 141.700(8) n Cu K Cu 3_655 11_566 180.0 n Cu K Cu . 11_566 136.751(9) n Cu K Cu 9_666 11_566 43.249(9) n 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 Cu Se2 1_565 2.4248(6) n Cu Se2 . 2.4248(6) y Cu Se1 1_455 2.5497(5) n Cu Se1 . 2.5497(5) y Cu Cu 3 2.8417(2) y Cu Cu 3_665 2.8417(2) n Cu Cu 3_655 2.8417(2) n Cu Cu 3_565 2.8417(2) n Cu K . 3.8556(7) n Cu K 1_455 3.8556(7) n Se1 Cu 11 2.5497(5) n Se1 Cu 9_565 2.5497(5) n Se1 Cu 3_665 2.5497(5) n Se1 Cu 1_655 2.5497(5) n Se1 Cu 11_565 2.5497(5) n Se1 Cu 9_665 2.5497(5) n Se1 Cu 3_655 2.5497(5) n Se2 Cu 3 2.4248(6) n Se2 Cu 1_545 2.4248(6) n Se2 Cu 3_655 2.4248(6) n Se2 K . 3.4371(4) y Se2 K 1_455 3.4371(4) n Se2 K 1_445 3.4371(4) n Se2 K 1_545 3.4371(4) n K Se2 9_666 3.4371(4) n K Se2 9_566 3.4371(4) n K Se2 9_656 3.4371(4) n K Se2 9_556 3.4371(4) n K Se2 1_665 3.4371(4) n K Se2 1_565 3.4371(4) n K Se2 1_655 3.4371(4) n K Cu 3_655 3.8556(7) n K Cu 9_666 3.8556(7) n K Cu 11_566 3.8556(7) n