#------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_Cu2Se3Sn #------------------ SUBMISSION DETAILS --------------------------------------# _publ_contact_author_name 'Yuri Grin' _publ_contact_author_address ; Max-Planck-Institut f\"ur Chemische Physik fester Stoffe N\"othnitzer Str. 40 D-01187 Dresden Germany ; _publ_contact_author_email grin@cpfs.mpg.de _publ_contact_author_fax 49(351)46464002 _publ_contact_author_phone 49(351)46464000 _publ_requested_journal 'Inorganic Chemistry' #------------------ TITLE AND AUTHOR LIST------------------------------------# _publ_section_title ; A new monoclinic modification of Cu2SnSe3 and its thermoelectric properties ; loop_ _publ_author_name _publ_author_address 'Jing Fan' ; Max-Planck-Institut f\"ur Chemische Physik fester Stoffe N\"othnitzer Str. 40 D-01187 Dresden Germany CAS Key Laboratory of Energy-conversion Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, 1295 Dingxi Road, 200050 Shanghai, China University of Chinese Academy of Sciences, 19 Yuquan Road, 100049 Beijing, P.R. China ; 'Wilder Carrillo-Cabrera' ; Max-Planck-Institut f\"ur Chemische Physik fester Stoffe N\"othnitzer Str. 40 D-01187 Dresden Germany ; 'Lev Akselrud' ; Max-Planck-Institut f\"ur Chemische Physik fester Stoffe N\"othnitzer Str. 40 D-01187 Dresden Germany ; 'Iryna Antonyshyn' ; Max-Planck-Institut f\"ur Chemische Physik fester Stoffe N\"othnitzer Str. 40 D-01187 Dresden Germany ; 'Lidong Chen' ; CAS Key Laboratory of Energy-conversion Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, 1295 Dingxi Road, 200050 Shanghai, China ; 'Yuri Grin' ; Max-Planck-Institut f\"ur Chemische Physik fester Stoffe N\"othnitzer Str. 40 D-01187 Dresden Germany ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# _audit_creation_date ? _audit_creation_method 'WinCSD program' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_sum 'Cu2 Se3 Sn' _chemical_formula_weight 482.65 _chemical_melting_point ? _chemical_compound_source 'synthesis as described' loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 16.00 .259 .509 WinCSD Se Se 24.00 .295 .932 WinCSD Sn Sn 8.00 -3.534 .578 WinCSD #------------------ UNIT CELL INFORMATION -----------------------------------# loop_ _symmetry_equiv_pos_as_xyz ' x, y, z' ' x, -y, 1/2+z' ' 1/2+x, 1/2+y, z' ' 1/2+x, 1/2-y, 1/2+z' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _cell_length_a 6.9714(2) _cell_length_b 12.0787(5) _cell_length_c 13.3935(5) _cell_angle_alpha 90 _cell_angle_beta 99.865(5) _cell_angle_gamma 90 _cell_volume 1111.13(7) _cell_formula_units_Z 8 _cell_measurement_wavelength 1.54056 _cell_measurement_radiation CuK\a1 _cell_measurement_temperature 295 _cell_measurement_reflns_used 75 _cell_measurement_theta_min 3 _cell_measurement_theta_max 100.3 _cell_special_details ; The lattice parameters were refined from XRPD data by using Si as an internal standard. ; #------------------ POWDER SPECIMEN AND CRYSTAL DATA ----------------------# _exptl_crystal_density_diffrn 5.771 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _pd_spec_mounting 'glass capillary' _pd_spec_mount_mode 'transmission' _pd_spec_shape 'cylinder' _pd_char_particle_morphology 'isoform' _pd_char_colour 'metallic-grey' _exptl_absorpt_coefficient_mu 9.59 #------------------ DATA COLLECTION INFORMATION -----------------------------# _exptl_special_details ; The measurement was performed at ID31 beamline at ESRF ; _pd_instr_location ; European Synchrotron Radiation Facility (ESRF) ; _diffrn_reflns_number 1336 _diffrn_ambient_temperature 295 _diffrn_source 'synchrotron' _diffrn_source_target '' _diffrn_source_type 'high resolution beamline ID31' _diffrn_measurement_device_type 'ID31 beamline at ESRF' _diffrn_detector 'Nine crystal multi-analyser stage' _diffrn_detector_type 'position sensitive detector' _pd_meas_scan_method 'step' _pd_meas_special_details ; ? ; loop_ _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.430459 _diffrn_radiation_monochromator 'Si 111 crystal' _pd_meas_number_of_points 30001 _pd_meas_2theta_range_min 3 _pd_meas_2theta_range_max 33 _pd_meas_2theta_range_inc 0.001 _reflns_number_total 1336 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ? _computing_cell_refinement 'WinCSD (Akselrud et al, 1993)' _computing_data_reduction 'WinCSD (Akselrud et al, 1993)' _computing_structure_solution 'WinCSD (Akselrud et al, 1993)' _computing_structure_refinement 'WinCSD (Akselrud et al, 1993)' _computing_molecular_graphics ? _computing_publication_material ; WinCSD (Akselrud et al, 1993) L.G. Akselrud, P.Yu. Zavalii, Yu.N. Grin, V.K. Pecharsky, B. Baumgartner, E. W\"olfel, (1993) Materials Science Forum, 133-136, 335-340 ; #------------------ REFINEMENT INFORMATION ----------------------------------# _pd_proc_ls_special_details ; ? ; _pd_proc_ls_profile_function pseudo-Voit _pd_proc_ls_pref_orient_corr ; Preffered orientation was refined using WinCSD formula (V.K. Pecharskii, L.G. Akselrud, P.Yu. Zavalii (1987) Soviet Physics Crystallogr., 32, 514-516): I~corr~=I~obs~/[1+(\t^2^-1)^.^sin^2^\f]^1/2^ 'Axis' 1 1 0, \t=1.37(1) ; _pd_proc_ls_prof_R_factor 0.1034 _pd_proc_ls_prof_wR_factor 0.1558 _pd_proc_ls_prof_wR_expected ? _refine_ls_R_factor_I 0.0596 _refine_special_details ; ? ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_weighting_details '1/[Y~i~+\s(Y~i~)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 88 _refine_ls_number_restraints ? _refine_ls_number_constraints ? #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy Cu1 Cu -0.0023(8) 0.0824(4) 0.7595(4) Uovl 0.013 4 1.0 Cu2 Cu -0.0093(7) 0.2480(3) 0.2542(4) Uovl 0.013 4 1.0 Cu3 Cu 0.2367(7) -0.0818(4) 0.0059(3) Uovl 0.013 4 1.0 Cu4 Cu 0.7464(7) 0.0864(3) 0.0049(3) Uovl 0.013 4 1.0 Se1 Se 0.0446(6) 0.0817(4) -0.0577(3) Uovl 0.013 4 1.0 Se2 Se 0.0495(5) 0.4255(4) -0.0505(3) Uovl 0.013 4 1.0 Se3 Se 0.3015(6) 0.2541(3) 0.1953(3) Uovl 0.013 4 1.0 Se4 Se 0.5704(6) 0.2561(4) -0.0572(3) Uovl 0.013 4 1.0 Se5 Se 0.3050(6) 0.0927(4) 0.6920(4) Uovl 0.013 4 1.0 Se6 Se 0.3261(6) 0.4210(4) 0.6921(3) Uovl 0.013 4 1.0 Sn1 Sn 0.2500(3) 0.2500(2) 0.0000(2) Uovl 0.013 4 1.0 Sn2 Sn -0.0018(7) 0.4204(2) 0.7542(3) Uovl 0.013 4 1.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Se6 2.382(7) 3_445 yes Cu1 Se1 2.412(6) 1_556 yes Cu1 Se5 2.467(7) . yes Cu1 Se3 2.469(6) 4_455 yes Cu2 Se5 2.387(6) 4_454 yes Cu2 Se6 2.418(6) 4_454 yes Cu2 Se3 2.430(7) . yes Cu2 Se4 2.491(6) 4_455 yes Cu3 Se4 2.355(6) 3_445 yes Cu3 Se2 2.429(6) 3_545 yes Cu3 Se1 2.456(6) . yes Cu3 Se5 2.459(6) 2_554 yes Cu4 Se1 2.372(6) 1_655 yes Cu4 Se2 2.421(6) 3_545 yes Cu4 Se4 2.460(6) . yes Cu4 Se6 2.475(6) 4_554 yes Sn1 Se4 2.484(5) . yes Sn1 Se1 2.529(5) . yes Sn1 Se2 2.565(4) . yes Sn1 Se3 2.580(5) . yes Sn2 Se5 2.539(5) 3_455 yes Sn2 Se6 2.563(6) . yes Sn2 Se3 2.564(5) 4_455 yes Sn2 Se2 2.578(5) 1_556 yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se6 Cu1 Se1 110.67(2) 3_445 . 1_556 yes Se6 Cu1 Se5 108.27(2) 3_445 . . yes Se6 Cu1 Se3 108.05(2) 3_445 . 4_455 yes Se1 Cu1 Se5 113.36(2) 1_556 . . yes Se1 Cu1 Se3 109.07(2) 1_556 . 4_455 yes Se5 Cu1 Se3 107.24(2) . . 4_455 yes Se5 Cu2 Se6 111.32(2) 4_454 . 4_454 yes Se5 Cu2 Se3 108.81(2) 4_454 . . yes Se5 Cu2 Se4 112.55(2) 4_454 . 4_455 yes Se6 Cu2 Se3 108.14(2) 4_454 . . yes Se6 Cu2 Se4 109.96(2) 4_454 . 4_455 yes Se3 Cu2 Se4 105.81(2) . . 4_455 yes Se4 Cu3 Se2 109.33(2) 3_445 . 3_545 yes Se4 Cu3 Se1 109.72(2) 3_445 . . yes Se4 Cu3 Se5 108.55(2) 3_445 . 2_554 yes Se2 Cu3 Se1 109.09(2) 3_545 . . yes Se2 Cu3 Se5 106.82(2) 3_545 . 2_554 yes Se1 Cu3 Se5 113.24(2) . . 2_554 yes Se1 Cu4 Se2 110.92(2) 1_655 . 3_545 yes Se1 Cu4 Se4 108.43(2) 1_655 . . yes Se1 Cu4 Se6 107.46(2) 1_655 . 4_554 yes Se2 Cu4 Se4 109.93(2) 3_545 . . yes Se2 Cu4 Se6 107.36(2) 3_545 . 4_554 yes Se4 Cu4 Se6 112.73(2) . . 4_554 yes Se4 Sn1 Se1 114.93(15) . . . yes Se4 Sn1 Se2 111.82(14) . . . yes Se4 Sn1 Se3 109.66(15) . . . yes Se1 Sn1 Se2 109.20(14) . . . yes Se1 Sn1 Se3 107.41(15) . . . yes Se2 Sn1 Se3 103.07(14) . . . yes Se5 Sn2 Se6 110.08(2) 3_455 . . yes Se5 Sn2 Se3 110.35(2) 3_455 . 4_455 yes Se5 Sn2 Se2 106.67(2) 3_455 . 1_556 yes Se6 Sn2 Se3 111.22(2) . . 4_455 yes Se6 Sn2 Se2 110.61(2) . . 1_556 yes Se3 Sn2 Se2 107.78(2) 4_455 . 1_556 yes Cu4 Se1 Cu1 112.62(2) 1_455 . 1_554 yes Cu4 Se1 Cu3 110.77(2) 1_455 . . yes Cu4 Se1 Sn1 110.89(2) 1_455 . . yes Cu1 Se1 Cu3 109.06(2) 1_554 . . yes Cu1 Se1 Sn1 106.18(2) 1_554 . . yes Cu3 Se1 Sn1 107.1(2) . . . yes Cu4 Se2 Cu3 115.22(2) 3_455 . 3_455 yes Cu4 Se2 Sn1 109.12(2) 3_455 . . yes Cu4 Se2 Sn2 107.67(2) 3_455 . 1_554 yes Cu3 Se2 Sn1 111.39(2) 3_455 . . yes Cu3 Se2 Sn2 109.81(2) 3_455 . 1_554 yes Sn1 Se2 Sn2 102.86(2) . . 1_554 yes Cu2 Se3 Cu1 112.52(2) . . 4_554 yes Cu2 Se3 Sn2 109.52(2) . . 4_554 yes Cu2 Se3 Sn1 110.6(2) . . . yes Cu1 Se3 Sn2 108.37(2) 4_554 . 4_554 yes Cu1 Se3 Sn1 109.95(2) 4_554 . . yes Sn2 Se3 Sn1 105.65(2) 4_554 . . yes Cu3 Se4 Cu4 112.57(2) 3_555 . . yes Cu3 Se4 Sn1 109.07(2) 3_555 . . yes Cu3 Se4 Cu2 113.09(2) 3_555 . 4_554 yes Cu4 Se4 Sn1 107.1(2) . . . yes Cu4 Se4 Cu2 109.78(2) . . 4_554 yes Sn1 Se4 Cu2 104.83(2) . . 4_554 yes Cu2 Se5 Cu3 113.31(2) 4_555 . 2_555 yes Cu2 Se5 Cu1 111.44(2) 4_555 . . yes Cu2 Se5 Sn2 108.69(2) 4_555 . 3_545 yes Cu3 Se5 Cu1 109.82(2) 2_555 . . yes Cu3 Se5 Sn2 106.76(2) 2_555 . 3_545 yes Cu1 Se5 Sn2 106.47(2) . . 3_545 yes Cu1 Se6 Cu2 112.52(3) 3_555 . 4_555 yes Cu1 Se6 Cu4 115.13(2) 3_555 . 4_455 yes Cu1 Se6 Sn2 107.31(2) 3_555 . . yes Cu2 Se6 Cu4 109.13(2) 4_555 . 4_455 yes Cu2 Se6 Sn2 106.45(2) 4_555 . . yes Cu4 Se6 Sn2 105.71(2) 4_455 . . yes