# cm011633v.cif data_CuScO2sx290K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cu O2 Sc' _chemical_formula_weight 140.50 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sc' 'Sc' 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P63/mmc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 3.2146(10) _cell_length_b 3.2146(10) _cell_length_c 11.3857(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 101.89(5) _cell_formula_units_Z 4 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 17.5 _exptl_crystal_description 'Truncated hexagonal bipyramid' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 132 _exptl_absorpt_coefficient_mu 13.357 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.3622 _exptl_absorpt_correction_T_max 0.7758 _exptl_absorpt_process_details 'Sortav as programmed in WinGX V1.64.02' _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC6R' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 147 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1127 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 26.52 _diffrn_reflns_theta_max 50.04 _reflns_number_total 187 _reflns_number_gt 173 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'AFC diffractometer control program' _computing_cell_refinement 'AFC diffractometer control program' _computing_data_reduction 'Redrig' _computing_structure_solution 'SHELXS-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+0.0012P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.8(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 187 _refine_ls_number_parameters 9 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0235 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0358 _refine_ls_wR_factor_gt 0.0351 _refine_ls_goodness_of_fit_ref 1.255 _refine_ls_restrained_S_all 1.255 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.3333 0.6667 0.2500 0.02474(10) Uani 1 2 d S . . Sc2 Sc 1.0000 0.0000 0.5000 0.01864(10) Uani 1 2 d S . . O1 O 0.3333 0.6667 0 0.08928(7) 0.01947(12) Uani 1 4 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02799(11) 0.02799(11) 0.01823(11) 0.000 0.000 0.01400(6) Sc2 0.01765(11) 0.01765(11) 0.02062(11) 0.000 0.000 0.00882(5) O1 0.01990(15) 0.01990(15) 0.0186(2) 0.000 0.000 0.00995(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O1 1.8299(8) . ? Cu1 O1 1.8299(8) 14_556 ? Sc2 O1 2.1161(6) 13_766 ? Sc2 O1 2.1161(6) 13_666 ? Sc2 O1 2.1161(6) 1_645 ? Sc2 O1 2.1161(6) 1_545 ? Sc2 O1 2.1161(6) 13_656 ? Sc2 O1 2.1161(6) 1_655 ? Sc2 Sc2 3.2146(10) 1_445 ? Sc2 Sc2 3.2146(10) 1_665 ? Sc2 Sc2 3.2146(10) 1_655 ? Sc2 Sc2 3.2146(10) 1_455 ? Sc2 Sc2 3.2146(10) 1_565 ? Sc2 Sc2 3.2146(10) 1_545 ? O1 Sc2 2.1161(6) 1_565 ? O1 Sc2 2.1161(6) 1_465 ? O1 Sc2 2.1161(6) 1_455 ? 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_3 _geom_angle_publ_flag O1 Cu1 O1 180.0 . 14_556 ? O1 Sc2 O1 98.85(3) 13_766 13_666 ? O1 Sc2 O1 81.15(3) 13_766 1_645 ? O1 Sc2 O1 180.00(4) 13_666 1_645 ? O1 Sc2 O1 180.0 13_766 1_545 ? O1 Sc2 O1 81.15(3) 13_666 1_545 ? O1 Sc2 O1 98.85(3) 1_645 1_545 ? O1 Sc2 O1 98.85(3) 13_766 13_656 ? O1 Sc2 O1 98.85(3) 13_666 13_656 ? O1 Sc2 O1 81.15(3) 1_645 13_656 ? O1 Sc2 O1 81.15(3) 1_545 13_656 ? O1 Sc2 O1 81.15(3) 13_766 1_655 ? O1 Sc2 O1 81.15(3) 13_666 1_655 ? O1 Sc2 O1 98.85(3) 1_645 1_655 ? O1 Sc2 O1 98.85(3) 1_545 1_655 ? O1 Sc2 O1 180.0 13_656 1_655 ? O1 Sc2 Sc2 139.425(13) 13_766 1_445 ? O1 Sc2 Sc2 90.0 13_666 1_445 ? O1 Sc2 Sc2 90.0 1_645 1_445 ? O1 Sc2 Sc2 40.575(13) 1_545 1_445 ? O1 Sc2 Sc2 40.575(13) 13_656 1_445 ? O1 Sc2 Sc2 139.425(13) 1_655 1_445 ? O1 Sc2 Sc2 40.575(13) 13_766 1_665 ? O1 Sc2 Sc2 90.0 13_666 1_665 ? O1 Sc2 Sc2 90.0 1_645 1_665 ? O1 Sc2 Sc2 139.425(13) 1_545 1_665 ? O1 Sc2 Sc2 139.425(13) 13_656 1_665 ? O1 Sc2 Sc2 40.575(13) 1_655 1_665 ? Sc2 Sc2 Sc2 180.0 1_445 1_665 ? O1 Sc2 Sc2 40.575(13) 13_766 1_655 ? O1 Sc2 Sc2 139.425(13) 13_666 1_655 ? O1 Sc2 Sc2 40.575(13) 1_645 1_655 ? O1 Sc2 Sc2 139.425(13) 1_545 1_655 ? O1 Sc2 Sc2 90.0 13_656 1_655 ? O1 Sc2 Sc2 90.0 1_655 1_655 ? Sc2 Sc2 Sc2 120.0 1_445 1_655 ? Sc2 Sc2 Sc2 60.0 1_665 1_655 ? O1 Sc2 Sc2 139.425(13) 13_766 1_455 ? O1 Sc2 Sc2 40.575(13) 13_666 1_455 ? O1 Sc2 Sc2 139.425(13) 1_645 1_455 ? O1 Sc2 Sc2 40.575(13) 1_545 1_455 ? O1 Sc2 Sc2 90.0 13_656 1_455 ? O1 Sc2 Sc2 90.0 1_655 1_455 ? Sc2 Sc2 Sc2 60.0 1_445 1_455 ? Sc2 Sc2 Sc2 120.0 1_665 1_455 ? Sc2 Sc2 Sc2 180.0 1_655 1_455 ? O1 Sc2 Sc2 90.0 13_766 1_565 ? O1 Sc2 Sc2 40.575(13) 13_666 1_565 ? O1 Sc2 Sc2 139.425(13) 1_645 1_565 ? O1 Sc2 Sc2 90.0 1_545 1_565 ? O1 Sc2 Sc2 139.425(13) 13_656 1_565 ? O1 Sc2 Sc2 40.575(13) 1_655 1_565 ? Sc2 Sc2 Sc2 120.0 1_445 1_565 ? Sc2 Sc2 Sc2 60.0 1_665 1_565 ? Sc2 Sc2 Sc2 120.0 1_655 1_565 ? Sc2 Sc2 Sc2 60.0 1_455 1_565 ? O1 Sc2 Sc2 90.0 13_766 1_545 ? O1 Sc2 Sc2 139.425(13) 13_666 1_545 ? O1 Sc2 Sc2 40.575(13) 1_645 1_545 ? O1 Sc2 Sc2 90.0 1_545 1_545 ? O1 Sc2 Sc2 40.575(13) 13_656 1_545 ? O1 Sc2 Sc2 139.425(13) 1_655 1_545 ? Sc2 Sc2 Sc2 60.0 1_445 1_545 ? Sc2 Sc2 Sc2 120.0 1_665 1_545 ? Sc2 Sc2 Sc2 60.0 1_655 1_545 ? Sc2 Sc2 Sc2 120.0 1_455 1_545 ? Sc2 Sc2 Sc2 180.0 1_565 1_545 ? Cu1 O1 Sc2 118.71(2) . 1_565 ? Cu1 O1 Sc2 118.71(2) . 1_465 ? Sc2 O1 Sc2 98.85(3) 1_565 1_465 ? Cu1 O1 Sc2 118.71(2) . 1_455 ? Sc2 O1 Sc2 98.85(3) 1_565 1_455 ? Sc2 O1 Sc2 98.85(3) 1_465 1_455 ? _diffrn_measured_fraction_theta_max 0.695 _diffrn_reflns_theta_full 50.04 _diffrn_measured_fraction_theta_full 0.695 _refine_diff_density_max 0.259 _refine_diff_density_min -0.139 _refine_diff_density_rms 0.031 #===END data_CuScO2neutron11K _chemical_name_systematic ; 2H Copper Scandium Oxide ; _chemical_name_common ? _chemical_formula_moiety 'Cu O2 Sc' _chemical_formula_sum 'Cu O2 Sc' _chemical_formula_weight 140.50 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Cu CU 0.7718 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' Sc SC 1.2300 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' O O 0.5803 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P6c2c' _symmetry_space_group_name_H-M 'P63/mmc' _symmetry_Int_Tables_number 194 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 3.2163(4) _cell_length_b 3.2163(4) _cell_length_c 11.409(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 102.21(1) _cell_formula_units_Z 2 _cell_measurement_temperature 11(1) _cell_special_details ; Cell dimensions at this temperature were refined from the powder diffractogram. ; _exptl_crystal_density_diffrn 4.5652(4) _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _pd_spec_size_axial 50.8 _pd_spec_size_equat 12.7 _pd_spec_size_thick 12.7 _pd_spec_mounting 'vanadium can' _pd_spec_mount_mode transmission _pd_spec_orientation vertical _pd_spec_shape cylinder _pd_char_particle_morphology 'fine powder' _pd_char_colour blue _exptl_absorpt_coefficient_mu 0.0427 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.698 _exptl_special_details ; Neutron powder diffraction data were collected using the BT-1 32-counter high resolution diffractometer at the Center for Neutron Research at the National Institute of Standards and Technology. A Cu (311) monochromator, yielding a wavelength of 1.5402(2) was employed. Collimation of 15', 20', and 7' of arc were used before and after the monochromator, and after the sample, respectively. Data were collected at room temperature over a 2-theta range of 3-168 degrees. The powdered sample was sealed in a vanadium container of length 50 mm and diameter 15.6 mm inside a dry He-filled glovebox. A vacuum furnace was used for measurements above room temperature, a closed-cycle He refrigerator was used for temperatures below room temperature. ; _diffrn_ambient_temperature 11(1) _diffrn_radiation_source 'nuclear reactor' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.5402(2) _diffrn_radiation_monochromator 'Cu(311)' _diffrn_measurement_device_type 'neutron powder diffractometer' _pd_instr_geometry '32 detector neutron diffractometer with vertical focusing' _pd_instr_location 'NBSR BT-1, NIST (USA)' _pd_meas_scan_method step _pd_meas_special_details ; 32 He-3 detectors at 5 degree intervals with a 13 degree scan range covering 2Theta from 3 to 167 degrees ; _pd_meas_number_of_points 3300 _pd_meas_2theta_range_min 3.00 _pd_meas_2theta_range_max 167.95 _pd_meas_2theta_range_inc 0.05 _pd_proc_info_data_reduction ; Data from the 32 detector banks were converted to a pseudo-single detector format using 2-point linear interpolation, after correcting for variable detector height masking and detector sensitivity, as well as two-theta offset. Where needed, a constant was added or subracted to the data in each detector as determined by integrating the overlapped regions, to compensate for background variations. A Chebyshev polynomial fit was calculated for the absorption correction factors for successive values of theta (the factors were taken from the International Tables of X-ray Crystallography, Vol. II, p. 295-297) ; _computing_data_collection 'BT-1 Instrument Control Program' _computing_cell_refinement 'Fullprof' _computing_data_reduction '' _computing_structure_solution 'structure previously known' _computing_structure_refinement 'Fullprof' _computing_molecular_graphics 'Atom V4.1 for windows' _computing_publication_material '' _pd_proc_ls_profile_function 'Thompson-Cox-Hastings pseudo-Voigt' _pd_proc_ls_background_function '3rd order polynomial' _pd_proc_ls_pref_orient_corr none _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 153.5 _pd_proc_2theta_range_inc 0.05 _pd_proc_info_excluded_regions ; The region from 3.00 to 10.00 was excluded from the refinement as no reflections were present in this range. The region from 153.50 to 167.95 was excluded to ensure that the highest angle data were at the background level. ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_goodness_of_fit_all 1.79 _refine_ls_shift/su_max 0.01 _pd_proc_ls_prof_R_factor 4.74 _pd_proc_ls_prof_wR_factor 6.07 _pd_proc_ls_prof_wR_expected 4.54 _refine_special_details ; Structure refinement occurred in two separate steps, with global variables refined first followed by structural parameters. Global variables included cell dimensions (2), peak profile parameters (5), Lorentzian anisotropic peak broadening parameter (1) and background polynomial coeficients (4) for a total of 12 variables. Structural parameters included the overall scale factor (1), the z coordinate of the oxygen atom (1), and anisotropic displacement parameters for the three unique atomic sites (6) for a total of 8 variables. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity Cu CU 0.3333 0.6667 0.2500 0.0002(4) Uani 1 2 Sc SC 0.0000 0.0000 0.0000 0.0009(3) Uani 1 2 O O 0.3333 0.6667 0.08941(3) 0.0007(4) Uani 1 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0015(4) 0.0015(4) -0.0023(4) 0.000 0.000 0.0007(2) Sc 0.0013(3) 0.0013(3) 0.0001(3) 0.000 0.000 0.0007(2) O 0.0014(4) 0.0014(4) -0.0007(4) 0.000 0.000 0.0007(2) _geom_special_details ; Only unique bond lengths and angles between the major atomic sites are reported. ; 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 Cu O 1.8321(7) . ? Sc O 2.1186(3) . ? 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_3 _geom_angle_publ_flag O Cu O 180.00 14_556 . ? O Sc O 98.76(1) 1_545 . ? O Sc O 180.00 . 13 ? O Sc O 81.24(3) . 13_565 ? Cu O Sc 118.78(2) . . ? Sc O Sc 98.76(1) 1_565 . ? #===END data_CuScO2neutron50K _chemical_name_systematic ; 2H Copper Scandium Oxide ; _chemical_name_common ? _chemical_formula_moiety 'Cu O2 Sc' _chemical_formula_sum 'Cu O2 Sc' _chemical_formula_weight 140.50 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Cu CU 0.7718 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' Sc SC 1.2300 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' O O 0.5803 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P6c2c' _symmetry_space_group_name_H-M 'P63/mmc' _symmetry_Int_Tables_number 194 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 3.2162(4) _cell_length_b 3.2163(4) _cell_length_c 11.408(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 102.19(1) _cell_formula_units_Z 2 _cell_measurement_temperature 50(1) _cell_special_details ; Cell dimensions at this temperature were refined from the powder diffractogram. ; _exptl_crystal_density_diffrn 4.5661(4) _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _pd_spec_size_axial 50.8 _pd_spec_size_equat 12.7 _pd_spec_size_thick 12.7 _pd_spec_mounting 'vanadium can' _pd_spec_mount_mode transmission _pd_spec_orientation vertical _pd_spec_shape cylinder _pd_char_particle_morphology 'fine powder' _pd_char_colour blue _exptl_absorpt_coefficient_mu 0.0427 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.698 _exptl_special_details ; Neutron powder diffraction data were collected using the BT-1 32-counter high resolution diffractometer at the Center for Neutron Research at the National Institute of Standards and Technology. A Cu (311) monochromator, yielding a wavelength of 1.5402(2) was employed. Collimation of 15', 20', and 7' of arc were used before and after the monochromator, and after the sample, respectively. Data were collected at room temperature over a 2-theta range of 3-168 degrees. The powdered sample was sealed in a vanadium container of length 50 mm and diameter 15.6 mm inside a dry He-filled glovebox. A vacuum furnace was used for measurements above room temperature, a closed-cycle He refrigerator was used for temperatures below room temperature. ; _diffrn_ambient_temperature 50(1) _diffrn_radiation_source 'nuclear reactor' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.5402(2) _diffrn_radiation_monochromator 'Cu(311)' _diffrn_measurement_device_type 'neutron powder diffractometer' _pd_instr_geometry '32 detector neutron diffractometer with vertical focusing' _pd_instr_location 'NBSR BT-1, NIST (USA)' _pd_meas_scan_method step _pd_meas_special_details ; 32 He-3 detectors at 5 degree intervals with a 13 degree scan range covering 2Theta from 3 to 167 degrees ; _pd_meas_number_of_points 3300 _pd_meas_2theta_range_min 3.00 _pd_meas_2theta_range_max 167.95 _pd_meas_2theta_range_inc 0.05 _pd_proc_info_data_reduction ; Data from the 32 detector banks were converted to a pseudo-single detector format using 2-point linear interpolation, after correcting for variable detector height masking and detector sensitivity, as well as two-theta offset. Where needed, a constant was added or subracted to the data in each detector as determined by integrating the overlapped regions, to compensate for background variations. A Chebyshev polynomial fit was calculated for the absorption correction factors for successive values of theta (the factors were taken from the International Tables of X-ray Crystallography, Vol. II, p. 295-297) ; _computing_data_collection 'BT-1 Instrument Control Program' _computing_cell_refinement 'Fullprof' _computing_data_reduction '' _computing_structure_solution 'structure previously known' _computing_structure_refinement 'Fullprof' _computing_molecular_graphics 'Atom V4.1 for windows' _computing_publication_material '' _pd_proc_ls_profile_function 'Thompson-Cox-Hastings pseudo-Voigt' _pd_proc_ls_background_function '3rd order polynomial' _pd_proc_ls_pref_orient_corr none _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 153.5 _pd_proc_2theta_range_inc 0.05 _pd_proc_info_excluded_regions ; The region from 3.00 to 10.00 was excluded from the refinement as no reflections were present in this range. The region from 153.50 to 167.95 was excluded to ensure that the highest angle data were at the background level. ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_goodness_of_fit_all 1.79 _refine_ls_shift/su_max 0.01 _pd_proc_ls_prof_R_factor 4.74 _pd_proc_ls_prof_wR_factor 5.93 _pd_proc_ls_prof_wR_expected 4.65 _refine_special_details ; Structure refinement occurred in two separate steps, with global variables refined first followed by structural parameters. Global variables included cell dimensions (2), peak profile parameters (5), Lorentzian anisotropic size broadening parameter (1) and background polynomial coeficients (4) for a total of 12 variables. Structural parameters included the overall scale factor (1), the z coordinate of the oxygen atom (1), and anisotropic displacement parameters for the three unique atomic sites (6) for a total of 8 variables. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity Cu CU 0.3333 0.6667 0.2500 0.0007(4) Uani 1 2 Sc SC 0.0000 0.0000 0.0000 0.0009(3) Uani 1 2 O O 0.3333 0.6667 0.08943(3) 0.0004(4) Uani 1 4 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_goodness_of_fit_all 1.79 _refine_lO O 0.3333 0.6667 0.08943(5) 0.0004(4) Uani 1 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0025(3) 0.0025(3) -0.0028(4) 0.000 0.000 0.0013(2) Sc 0.0011(3) 0.0011(3) 0.0006(3) 0.000 0.000 0.0006(2) O 0.0008(3) 0.0008(3) -0.0004(4) 0.000 0.000 0.0004(2) _geom_special_details ; Only unique bond lengths and angles between the major atomic sites are reported. ; 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 Cu O 1.8318(7) . ? Sc O 2.1187(3) . ? 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_3 _geom_angle_publ_flag O Cu O 180.00 14_556 . ? O Sc O 98.75(1) 1_545 . ? O Sc O 180.00 . 13 ? O Sc O 81.25(3) . 13_565 ? Cu O Sc 118.79(2) . . ? Sc O Sc 98.75(1) 1_565 . ? #===END data_CuScO2neutron100K _chemical_name_systematic ; 2H Copper Scandium Oxide ; _chemical_name_common ? _chemical_formula_moiety 'Cu O2 Sc' _chemical_formula_sum 'Cu O2 Sc' _chemical_formula_weight 140.50 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Cu CU 0.7718 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' Sc SC 1.2300 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' O O 0.5803 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P6c2c' _symmetry_space_group_name_H-M 'P63/mmc' _symmetry_Int_Tables_number 194 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 3.2164(4) _cell_length_b 3.2164(4) _cell_length_c 11.407(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 102.20(1) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_special_details ; Cell dimensions at this temperature were refined from the powder diffractogram. ; _exptl_crystal_density_diffrn 4.5657(6) _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _pd_spec_size_axial 50.8 _pd_spec_size_equat 12.7 _pd_spec_size_thick 12.7 _pd_spec_mounting 'vanadium can' _pd_spec_mount_mode transmission _pd_spec_orientation vertical _pd_spec_shape cylinder _pd_char_particle_morphology 'fine powder' _pd_char_colour blue _exptl_absorpt_coefficient_mu 0.0427 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.698 _exptl_special_details ; Neutron powder diffraction data were collected using the BT-1 32-counter high resolution diffractometer at the Center for Neutron Research at the National Institute of Standards and Technology. A Cu (311) monochromator, yielding a wavelength of 1.5402(2) was employed. Collimation of 15', 20', and 7' of arc were used before and after the monochromator, and after the sample, respectively. Data were collected at room temperature over a 2-theta range of 3-168 degrees. The powdered sample was sealed in a vanadium container of length 50 mm and diameter 15.6 mm inside a dry He-filled glovebox. A vacuum furnace was used for measurements above room temperature, a closed-cycle He refrigerator was used for temperatures below room temperature. ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_source 'nuclear reactor' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.5402(2) _diffrn_radiation_monochromator 'Cu(311)' _diffrn_measurement_device_type 'neutron powder diffractometer' _pd_instr_geometry '32 detector neutron diffractometer with vertical focusing' _pd_instr_location 'NBSR BT-1, NIST (USA)' _pd_meas_scan_method step _pd_meas_special_details ; 32 He-3 detectors at 5 degree intervals with a 13 degree scan range covering 2Theta from 3 to 167 degrees ; _pd_meas_number_of_points 3300 _pd_meas_2theta_range_min 3.00 _pd_meas_2theta_range_max 167.95 _pd_meas_2theta_range_inc 0.05 _pd_proc_info_data_reduction ; Data from the 32 detector banks were converted to a pseudo-single detector format using 2-point linear interpolation, after correcting for variable detector height masking and detector sensitivity, as well as two-theta offset. Where needed, a constant was added or subracted to the data in each detector as determined by integrating the overlapped regions, to compensate for background variations. A Chebyshev polynomial fit was calculated for the absorption correction factors for successive values of theta (the factors were taken from the International Tables of X-ray Crystallography, Vol. II, p. 295-297) ; _computing_data_collection 'BT-1 Instrument Control Program' _computing_cell_refinement 'Fullprof' _computing_data_reduction '' _computing_structure_solution 'structure previously known' _computing_structure_refinement 'Fullprof' _computing_molecular_graphics 'Atom V4.1 for windows' _computing_publication_material '' _pd_proc_ls_profile_function 'Thompson-Cox-Hastings pseudo-Voigt' _pd_proc_ls_background_function '3rd order polynomial' _pd_proc_ls_pref_orient_corr none _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 153.5 _pd_proc_2theta_range_inc 0.05 _pd_proc_info_excluded_regions ; The region from 3.00 to 10.00 was excluded from the refinement as no reflections were present in this range. The region from 153.50 to 167.95 was excluded to ensure that the highest angle data were at the background level. ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_goodness_of_fit_all 1.63 _refine_ls_shift/su_max 0.01 _pd_proc_ls_prof_R_factor 4.55 _pd_proc_ls_prof_wR_factor 5.92 _pd_proc_ls_prof_wR_expected 4.64 _refine_special_details ; Structure refinement occurred in two separate steps, with global variables refined first followed by structural parameters. Global variables included cell dimensions (2), peak profile parameters (5), Lorentzian anisotropic peak broadening parameter (1) and background polynomial coeficients (4) for a total of 12 variables. Structural parameters included the overall scale factor (1), the z coordinate of the oxygen atom (1), and anisotropic displacement parameters for the three unique atomic sites (6) for a total of 8 variables. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity Cu CU 0.3333 0.6667 0.2500 0.0022(4) Uani 1 2 Sc SC 0.0000 0.0000 0.0000 0.0017(3) Uani 1 2 O O 0.3333 0.6667 0.08945(3) 0.0013(4) Uani 1 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0042(4) 0.0042(4) -0.0019(4) 0.000 0.000 0.0021(2) Sc 0.0017(3) 0.0017(3) 0.0016(3) 0.000 0.000 0.0009(2) O 0.0022(4) 0.0022(4) -0.0005(4) 0.000 0.000 0.0011(2) _geom_special_details ; Only unique bond lengths and angles between the major atomic sites are reported. ; 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 Cu O 1.8314(7) . ? Sc O 2.1188(3) . ? 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_3 _geom_angle_publ_flag O Cu O 180.00 14_556 . ? O Sc O 98.75(1) 1_545 . ? O Sc O 180.00 . 13 ? O Sc O 81.25(3) . 13_565 ? Cu O Sc 118.79(2) . . ? Sc O Sc 98.75(1) 1_565 . ? #===END data_CuScO2neutron150K _chemical_name_systematic ; 2H Copper Scandium Oxide ; _chemical_name_common ? _chemical_formula_moiety 'Cu O2 Sc' _chemical_formula_sum 'Cu O2 Sc' _chemical_formula_weight 140.50 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Cu CU 0.7718 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' Sc SC 1.2300 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' Mg MG 0.5375 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' O O 0.5803 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P6c2c' _symmetry_space_group_name_H-M 'P63/mmc' _symmetry_Int_Tables_number 194 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 3.2168(4) _cell_length_b 3.2168(4) _cell_length_c 11.406(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 102.21(1) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_special_details ; Cell dimensions at this temperature were refined from the powder diffractogram. ; _exptl_crystal_density_diffrn 4.5652(6) _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _pd_spec_size_axial 50.8 _pd_spec_size_equat 12.7 _pd_spec_size_thick 12.7 _pd_spec_mounting 'vanadium can' _pd_spec_mount_mode transmission _pd_spec_orientation vertical _pd_spec_shape cylinder _pd_char_particle_morphology 'fine powder' _pd_char_colour blue _exptl_absorpt_coefficient_mu 0.0427 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.698 _exptl_special_details ; Neutron powder diffraction data were collected using the BT-1 32-counter high resolution diffractometer at the Center for Neutron Research at the National Institute of Standards and Technology. A Cu (311) monochromator, yielding a wavelength of 1.5402(2) was employed. Collimation of 15', 20', and 7' of arc were used before and after the monochromator, and after the sample, respectively. Data were collected at room temperature over a 2-theta range of 3-168 degrees. The powdered sample was sealed in a vanadium container of length 50 mm and diameter 15.6 mm inside a dry He-filled glovebox. A vacuum furnace was used for measurements above room temperature, a closed-cycle He refrigerator was used for temperatures below room temperature. ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_source 'nuclear reactor' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.5402(2) _diffrn_radiation_monochromator 'Cu(311)' _diffrn_measurement_device_type 'neutron powder diffractometer' _pd_instr_geometry '32 detector neutron diffractometer with vertical focusing' _pd_instr_location 'NBSR BT-1, NIST (USA)' _pd_meas_scan_method step _pd_meas_special_details ; 32 He-3 detectors at 5 degree intervals with a 13 degree scan range covering 2Theta from 3 to 167 degrees ; _pd_meas_number_of_points 3300 _pd_meas_2theta_range_min 3.00 _pd_meas_2theta_range_max 167.95 _pd_meas_2theta_range_inc 0.05 _pd_proc_info_data_reduction ; Data from the 32 detector banks were converted to a pseudo-single detector format using 2-point linear interpolation, after correcting for variable detector height masking and detector sensitivity, as well as two-theta offset. Where needed, a constant was added or subracted to the data in each detector as determined by integrating the overlapped regions, to compensate for background variations. A Chebyshev polynomial fit was calculated for the absorption correction factors for successive values of theta (the factors were taken from the International Tables of X-ray Crystallography, Vol. II, p. 295-297) ; _computing_data_collection 'BT-1 Instrument Control Program' _computing_cell_refinement 'Fullprof' _computing_data_reduction '' _computing_structure_solution 'structure previously known' _computing_structure_refinement 'Fullprof' _computing_molecular_graphics 'Atom V4.1 for windows' _computing_publication_material '' _pd_proc_ls_profile_function 'Thompson-Cox-Hastings pseudo-Voigt' _pd_proc_ls_background_function '3rd order polynomial' _pd_proc_ls_pref_orient_corr none _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 153.5 _pd_proc_2theta_range_inc 0.05 _pd_proc_info_excluded_regions ; The region from 3.00 to 10.00 was excluded from the refinement as no significant reflections were present in this range. The region from 153.50 to 167.95 was excluded to ensure that the highest angle data was at the background level. ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_parameters 21 _refine_ls_number_restraints 0 _refine_ls_number_constraints 2 _refine_ls_goodness_of_fit_all 1.77 _refine_ls_shift/su_max 0.01 _pd_proc_ls_prof_R_factor 4.63 _pd_proc_ls_prof_wR_factor 6.07 _pd_proc_ls_prof_wR_expected 4.57 _refine_special_details ; Structure refinement occurred in two separate steps, with global variables refined first followed by structural parameters. Global variables included cell dimensions (2), peak profile parameters (5), Lorentzian anisotropic size broadening parameter (1) and background polynomial coeficients (4) for a total of 12 variables. Structural parameters included the overall scale factor (1), the z coordinate of the oxygen atom (1), the Mg/Sc ratio in the Sc site (1), and anisotropic displacement parameters for the three unique atomic sites (6) for a total of 9 variables. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity Cu CU 0.3333 0.6667 0.2500 0.0040(4) Uani 1 2 Sc SC 0.0000 0.0000 0.0000 0.0023(3) Uani 0.92(1) 2 Mg MG 0.0000 0.0000 0.0000 0.0023(3) Uani 0.08(1) 2 O O 0.3333 0.6667 0.08948(5) 0.0017(4) Uani 1 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0069(4) 0.0069(4) -0.0017(4) 0.000 0.000 0.0035(2) Sc 0.0020(3) 0.0020(3) 0.0027(3) 0.000 0.000 0.0010(2) O 0.0023(4) 0.0023(4) 0.0005(4) 0.000 0.000 0.0011(2) _geom_special_details ; Only unique bond lengths and angles between the major atomic sites are reported. ; 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 Cu O 1.8309(8) . ? Sc O 2.1192(4) . ? 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_3 _geom_angle_publ_flag O Cu O 180.00 14_556 . ? O Sc O 98.75(1) 1_545 . ? O Sc O 180.00 . 13 ? O Sc O 81.25(3) . 13_565 ? Cu O Sc 118.78(3) . . ? Sc O Sc 98.75(1) 1_565 . ? #===END data_CuScO2neutron200K _chemical_name_systematic ; 2H Copper Scandium Oxide ; _chemical_name_common ? _chemical_formula_moiety 'Cu O2 Sc' _chemical_formula_sum 'Cu O2 Sc' _chemical_formula_weight 140.50 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Cu CU 0.7718 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' Sc SC 1.2300 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' O O 0.5803 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P6c2c' _symmetry_space_group_name_H-M 'P63/mmc' _symmetry_Int_Tables_number 194 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 3.2173(4) _cell_length_b 3.2173(4) _cell_length_c 11.405(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 102.24(1) _cell_formula_units_Z 2 _cell_measurement_temperature 200(1) _cell_special_details ; Cell dimensions at this temperature were refined from the powder diffractogram. ; _exptl_crystal_density_diffrn 4.5639(6) _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _pd_spec_size_axial 50.8 _pd_spec_size_equat 12.7 _pd_spec_size_thick 12.7 _pd_spec_mounting 'vanadium can' _pd_spec_mount_mode transmission _pd_spec_orientation vertical _pd_spec_shape cylinder _pd_char_particle_morphology 'fine powder' _pd_char_colour blue _exptl_absorpt_coefficient_mu 0.0427 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.698 _exptl_special_details ; Neutron powder diffraction data were collected using the BT-1 32-counter high resolution diffractometer at the Center for Neutron Research at the National Institute of Standards and Technology. A Cu (311) monochromator, yielding a wavelength of 1.5402(2) was employed. Collimation of 15', 20', and 7' of arc were used before and after the monochromator, and after the sample, respectively. Data were collected at room temperature over a 2-theta range of 3-168 degrees. The powdered sample was sealed in a vanadium container of length 50 mm and diameter 15.6 mm inside a dry He-filled glovebox. A vacuum furnace was used for measurements above room temperature, a closed-cycle He refrigerator was used for temperatures below room temperature. ; _diffrn_ambient_temperature 200(1) _diffrn_radiation_source 'nuclear reactor' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.5402(2) _diffrn_radiation_monochromator 'Cu(311)' _diffrn_measurement_device_type 'neutron powder diffractometer' _pd_instr_geometry '32 detector neutron diffractometer with vertical focusing' _pd_instr_location 'NBSR BT-1, NIST (USA)' _pd_meas_scan_method step _pd_meas_special_details ; 32 He-3 detectors at 5 degree intervals with a 13 degree scan range covering 2Theta from 3 to 167 degrees ; _pd_meas_number_of_points 3300 _pd_meas_2theta_range_min 3.00 _pd_meas_2theta_range_max 167.95 _pd_meas_2theta_range_inc 0.05 _pd_proc_info_data_reduction ; Data from the 32 detector banks were converted to a pseudo-single detector format using 2-point linear interpolation, after correcting for variable detector height masking and detector sensitivity, as well as two-theta offset. Where needed, a constant was added or subracted to the data in each detector as determined by integrating the overlapped regions, to compensate for background variations. A Chebyshev polynomial fit was calculated for the absorption correction factors for successive values of theta (the factors were taken from the International Tables of X-ray Crystallography, Vol. II, p. 295-297) ; _computing_data_collection 'BT-1 Instrument Control Program' _computing_cell_refinement 'Fullprof' _computing_data_reduction '' _computing_structure_solution 'structure previously known' _computing_structure_refinement 'Fullprof' _computing_molecular_graphics 'Atom V4.1 for windows' _computing_publication_material '' _pd_proc_ls_profile_function 'Thompson-Cox-Hastings pseudo-Voigt' _pd_proc_ls_background_function '3rd order polynomial' _pd_proc_ls_pref_orient_corr none _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 153.5 _pd_proc_2theta_range_inc 0.05 _pd_proc_info_excluded_regions ; The region from 3.00 to 10.00 was excluded from the refinement as no reflections were present in this range. The region from 153.50 to 167.95 was excluded to ensure that the highest angle data were at the background level. ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_goodness_of_fit_all 1.68 _refine_ls_shift/su_max 0.01 _pd_proc_ls_prof_R_factor 4.41 _pd_proc_ls_prof_wR_factor 5.85 _pd_proc_ls_prof_wR_expected 4.52 _refine_special_details ; Structure refinement occurred in two separate steps, with global variables refined first followed by structural parameters. Global variables included cell dimensions (2), peak profile parameters (5), Lorentzian anisotropic peak broadening parameter (1) and background polynomial coeficients (4) for a total of 12 variables. Structural parameters included the overall scale factor (1), the z coordinate of the oxygen atom (1), and anisotropic displacement parameters for the three unique atomic sites (6) for a total of 8 variables. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity Cu CU 0.3333 0.6667 0.2500 0.0057(4) Uani 1 2 Sc SC 0.0000 0.0000 0.0000 0.0029(3) Uani 1 2 O O 0.3333 0.6667 0.08950(3) 0.0024(4) Uani 1 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0089(4) 0.0089(4) -0.0007(4) 0.000 0.000 0.0045(2) Sc 0.0025(3) 0.0025(3) 0.0037(3) 0.000 0.000 0.0013(2) O 0.0030(4) 0.0030(4) 0.0013(4) 0.000 0.000 0.0015(2) _geom_special_details ; Only unique bond lengths and angles between the major atomic sites are reported. ; 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 Cu O 1.8305(8) . ? Sc O 2.1195(4) . ? 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_3 _geom_angle_publ_flag O Cu O 180.00 14_556 . ? O Sc O 98.75(1) 1_545 . ? O Sc O 180.00 . 13 ? O Sc O 81.25(3) . 13_565 ? Cu O Sc 118.79(3) . . ? Sc O Sc 98.75(1) 1_565 . ? #===END data_CuScO2neutron250K _chemical_name_systematic ; 2H Copper Scandium Oxide ; _chemical_name_common ? _chemical_formula_moiety 'Cu O2 Sc' _chemical_formula_sum 'Cu O2 Sc' _chemical_formula_weight 140.50 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Cu CU 0.7718 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' Sc SC 1.2300 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' O O 0.5803 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P6c2c' _symmetry_space_group_name_H-M 'P63/mmc' _symmetry_Int_Tables_number 194 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 3.2182(4) _cell_length_b 3.2182(4) _cell_length_c 11.405(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 102.29(1) _cell_formula_units_Z 2 _cell_measurement_temperature 250(1) _cell_special_details ; Cell dimensions at this temperature were refined from the powder diffractogram. ; _exptl_crystal_density_diffrn 4.5617(6) _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _pd_spec_size_axial 50.8 _pd_spec_size_equat 12.7 _pd_spec_size_thick 12.7 _pd_spec_mounting 'vanadium can' _pd_spec_mount_mode transmission _pd_spec_orientation vertical _pd_spec_shape cylinder _pd_char_particle_morphology 'fine powder' _pd_char_colour blue _exptl_absorpt_coefficient_mu 0.0427 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.698 _exptl_special_details ; Neutron powder diffraction data were collected using the BT-1 32-counter high resolution diffractometer at the Center for Neutron Research at the National Institute of Standards and Technology. A Cu (311) monochromator, yielding a wavelength of 1.5402(2) was employed. Collimation of 15', 20', and 7' of arc were used before and after the monochromator, and after the sample, respectively. Data were collected at room temperature over a 2-theta range of 3-168 degrees. The powdered sample was sealed in a vanadium container of length 50 mm and diameter 15.6 mm inside a dry He-filled glovebox. A vacuum furnace was used for measurements above room temperature, a closed-cycle He refrigerator was used for temperatures below room temperature. ; _diffrn_ambient_temperature 250(1) _diffrn_radiation_source 'nuclear reactor' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.5402(2) _diffrn_radiation_monochromator 'Cu(311)' _diffrn_measurement_device_type 'neutron powder diffractometer' _pd_instr_geometry '32 detector neutron diffractometer with vertical focusing' _pd_instr_location 'NBSR BT-1, NIST (USA)' _pd_meas_scan_method step _pd_meas_special_details ; 32 He-3 detectors at 5 degree intervals with a 13 degree scan range covering 2Theta from 3 to 167 degrees ; _pd_meas_number_of_points 3300 _pd_meas_2theta_range_min 3.00 _pd_meas_2theta_range_max 167.95 _pd_meas_2theta_range_inc 0.05 _pd_proc_info_data_reduction ; Data from the 32 detector banks were converted to a pseudo-single detector format using 2-point linear interpolation, after correcting for variable detector height masking and detector sensitivity, as well as two-theta offset. Where needed, a constant was added or subracted to the data in each detector as determined by integrating the overlapped regions, to compensate for background variations. A Chebyshev polynomial fit was calculated for the absorption correction factors for successive values of theta (the factors were taken from the International Tables of X-ray Crystallography, Vol. II, p. 295-297) ; _computing_data_collection 'BT-1 Instrument Control Program' _computing_cell_refinement 'Fullprof' _computing_data_reduction '' _computing_structure_solution 'structure previously known' _computing_structure_refinement 'Fullprof' _computing_molecular_graphics 'Atom V4.1 for windows' _computing_publication_material '' _pd_proc_ls_profile_function 'Thompson-Cox-Hastings pseudo-Voigt' _pd_proc_ls_background_function '3rd order polynomial' _pd_proc_ls_pref_orient_corr none _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 153.5 _pd_proc_2theta_range_inc 0.05 _pd_proc_info_excluded_regions ; The region from 3.00 to 10.00 was excluded from the refinement as no reflections were present in this range. The region from 153.50 to 167.95 was excluded to ensure that the highest angle data were at the background level. ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_goodness_of_fit_all 1.69 _refine_ls_shift/su_max 0.01 _pd_proc_ls_prof_R_factor 4.56 _pd_proc_ls_prof_wR_factor 5.99 _pd_proc_ls_prof_wR_expected 4.61 _refine_special_details ; Structure refinement occurred in two separate steps, with global variables refined first followed by structural parameters. Global variables included cell dimensions (2), peak profile parameters (5), Lorentzian anisotropic size broadening parameter (1) and background polynomial coeficients (4) for a total of 12 variables. Structural parameters included the overall scale factor (1), the z coordinate of the oxygen atom (1), and anisotropic displacement parameters for the three unique atomic sites (6) for a total of 8 variables. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity Cu CU 0.3333 0.6667 0.2500 0.0071(4) Uani 1 2 Sc SC 0.0000 0.0000 0.0000 0.0033(3) Uani 1 2 O O 0.3333 0.6667 0.08953(4) 0.0029(4) Uani 1 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0114(4) 0.0114(4) -0.0013(4) 0.000 0.000 0.0057(2) Sc 0.0028(3) 0.0028(3) 0.0044(3) 0.000 0.000 0.0014(2) O 0.0033(4) 0.0033(4) 0.0021(4) 0.000 0.000 0.0017(2) _geom_special_details ; Only unique bond lengths and angles between the major atomic sites are reported. ; 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 Cu O 1.8302(8) . ? Sc O 2.1201(4) . ? 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_3 _geom_angle_publ_flag O Cu O 180.00 14_556 . ? O Sc O 98.75(2) 1_545 . ? O Sc O 180.00 . 13 ? O Sc O 81.25(3) . 13_565 ? Cu O Sc 118.79(3) . . ? Sc O Sc 98.75(2) 1_565 . ? #===END data_CuScO2neutron300K _chemical_name_systematic ; 2H Copper Scandium Oxide ; _chemical_name_common ? _chemical_formula_moiety 'Cu O2 Sc' _chemical_formula_sum 'Cu O2 Sc' _chemical_formula_weight 140.50 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Cu CU 0.7718 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' Sc SC 1.2300 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' O O 0.5803 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P6c2c' _symmetry_space_group_name_H-M 'P63/mmc' _symmetry_Int_Tables_number 194 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 3.2189(4) _cell_length_b 3.2189(4) _cell_length_c 11.404(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 102.33(1) _cell_formula_units_Z 2 _cell_measurement_temperature 300(1) _cell_special_details ; Cell dimensions at this temperature were refined from the powder diffractogram. ; _exptl_crystal_density_diffrn 4.5599(6) _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _pd_spec_size_axial 50.8 _pd_spec_size_equat 12.7 _pd_spec_size_thick 12.7 _pd_spec_mounting 'vanadium can' _pd_spec_mount_mode transmission _pd_spec_orientation vertical _pd_spec_shape cylinder _pd_char_particle_morphology 'fine powder' _pd_char_colour blue _exptl_absorpt_coefficient_mu 0.0427 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.698 _exptl_special_details ; Neutron powder diffraction data were collected using the BT-1 32-counter high resolution diffractometer at the Center for Neutron Research at the National Institute of Standards and Technology. A Cu (311) monochromator, yielding a wavelength of 1.5402(2) was employed. Collimation of 15', 20', and 7' of arc were used before and after the monochromator, and after the sample, respectively. Data were collected at room temperature over a 2-theta range of 3-168 degrees. The powdered sample was sealed in a vanadium container of length 50 mm and diameter 15.6 mm inside a dry He-filled glovebox. A vacuum furnace was used for measurements above room temperature, a closed-cycle He refrigerator was used for temperatures below room temperature. ; _diffrn_ambient_temperature 300(1) _diffrn_radiation_source 'nuclear reactor' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.5402(2) _diffrn_radiation_monochromator 'Cu(311)' _diffrn_measurement_device_type 'neutron powder diffractometer' _pd_instr_geometry '32 detector neutron diffractometer with vertical focusing' _pd_instr_location 'NBSR BT-1, NIST (USA)' _pd_meas_scan_method step _pd_meas_special_details ; 32 He-3 detectors at 5 degree intervals with a 13 degree scan range covering 2Theta from 3 to 167 degrees ; _pd_meas_number_of_points 3300 _pd_meas_2theta_range_min 3.00 _pd_meas_2theta_range_max 167.95 _pd_meas_2theta_range_inc 0.05 _pd_proc_info_data_reduction ; Data from the 32 detector banks were converted to a pseudo-single detector format using 2-point linear interpolation, after correcting for variable detector height masking and detector sensitivity, as well as two-theta offset. Where needed, a constant was added or subracted to the data in each detector as determined by integrating the overlapped regions, to compensate for background variations. A Chebyshev polynomial fit was calculated for the absorption correction factors for successive values of theta (the factors were taken from the International Tables of X-ray Crystallography, Vol. II, p. 295-297) ; _computing_data_collection 'BT-1 Instrument Control Program' _computing_cell_refinement 'Fullprof' _computing_data_reduction '' _computing_structure_solution 'structure previously known' _computing_structure_refinement 'Fullprof' _computing_molecular_graphics 'Atom V4.1 for windows' _computing_publication_material '' _pd_proc_ls_profile_function 'Thompson-Cox-Hastings pseudo-Voigt' _pd_proc_ls_background_function '3rd order polynomial' _pd_proc_ls_pref_orient_corr none _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 153.5 _pd_proc_2theta_range_inc 0.05 _pd_proc_info_excluded_regions ; The region from 3.00 to 10.00 was excluded from the refinement as no reflections were present in this range. The region from 153.50 to 167.95 was excluded to ensure that the highest angle data were at the background level. ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_goodness_of_fit_all 1.38 _refine_ls_shift/su_max 0.01 _pd_proc_ls_prof_R_factor 4.12 _pd_proc_ls_prof_wR_factor 5.47 _pd_proc_ls_prof_wR_expected 4.66 _refine_special_details ; Structure refinement occurred in two separate steps, with global variables refined first followed by structural parameters. Global variables included cell dimensions (2), peak profile parameters (5), Lorentzian anisotropic peak broadening parameter (1) and background polynomial coeficients (4) for a total of 12 variables. Structural parameters included the overall scale factor (1), the z coordinate of the oxygen atom (1), and anisotropic displacement parameters for the three unique atomic sites (6) for a total of 8 variables. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity Cu CU 0.3333 0.6667 0.2500 0.0100(4) Uani 1 2 Sc SC 0.0000 0.0000 0.0000 0.0050(3) Uani 1 2 O O 0.3333 0.6667 0.08955(4) 0.0045(4) Uani 1 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0148(4) 0.0148(4) 0.0004(4) 0.000 0.000 0.0074(2) Sc 0.0045(3) 0.0045(3) 0.0061(3) 0.000 0.000 0.0023(2) O 0.0054(4) 0.0054(4) 0.0026(4) 0.000 0.000 0.0027(2) _geom_special_details ; Only unique bond lengths and angles between the major atomic sites are reported. ; 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 Cu O 1.8298(7) . ? Sc O 2.1205(3) . ? 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_3 _geom_angle_publ_flag O Cu O 180.00 14_556 . ? O Sc O 98.75(1) 1_545 . ? O Sc O 180.00 . 13 ? O Sc O 81.25(3) . 13_565 ? Cu O Sc 118.79(2) . . ? Sc O Sc 98.75(1) 1_565 . ? #===END data_CuScO2neutron573K _chemical_name_systematic ; 2H Copper Scandium Oxide ; _chemical_name_common ? _chemical_formula_moiety 'Cu O2 Sc' _chemical_formula_sum 'Cu O2 Sc' _chemical_formula_weight 140.50 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Cu CU 0.7718 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' Sc SC 1.2300 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' O O 0.5803 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P6c2c' _symmetry_space_group_name_H-M 'P63/mmc' _symmetry_Int_Tables_number 194 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 3.2275(4) _cell_length_b 3.2275(4) _cell_length_c 11.413(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 102.96(1) _cell_formula_units_Z 2 _cell_measurement_temperature 573(1) _cell_special_details ; Cell dimensions at this temperature were refined from the powder diffractogram. ; _exptl_crystal_density_diffrn 4.5320(6) _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _pd_spec_size_axial 50.8 _pd_spec_size_equat 12.7 _pd_spec_size_thick 12.7 _pd_spec_mounting 'vanadium can' _pd_spec_mount_mode transmission _pd_spec_orientation vertical _pd_spec_shape cylinder _pd_char_particle_morphology 'fine powder' _pd_char_colour blue _exptl_absorpt_coefficient_mu 0.0427 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.698 _exptl_special_details ; Neutron powder diffraction data were collected using the BT-1 32-counter high resolution diffractometer at the Center for Neutron Research at the National Institute of Standards and Technology. A Cu (311) monochromator, yielding a wavelength of 1.5402(2) was employed. Collimation of 15', 20', and 7' of arc were used before and after the monochromator, and after the sample, respectively. Data were collected at room temperature over a 2-theta range of 3-168 degrees. The powdered sample was sealed in a vanadium container of length 50 mm and diameter 15.6 mm inside a dry He-filled glovebox. A vacuum furnace was used for measurements above room temperature, a closed-cycle He refrigerator was used for temperatures below room temperature. ; _diffrn_ambient_temperature 573(1) _diffrn_radiation_source 'nuclear reactor' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.5402(2) _diffrn_radiation_monochromator 'Cu(311)' _diffrn_measurement_device_type 'neutron powder diffractometer' _pd_instr_geometry '32 detector neutron diffractometer with vertical focusing' _pd_instr_location 'NBSR BT-1, NIST (USA)' _pd_meas_scan_method step _pd_meas_special_details ; 32 He-3 detectors at 5 degree intervals with a 13 degree scan range covering 2Theta from 3 to 167 degrees ; _pd_meas_number_of_points 3300 _pd_meas_2theta_range_min 3.00 _pd_meas_2theta_range_max 167.95 _pd_meas_2theta_range_inc 0.05 _pd_proc_info_data_reduction ; Data from the 32 detector banks were converted to a pseudo-single detector format using 2-point linear interpolation, after correcting for variable detector height masking and detector sensitivity, as well as two-theta offset. Where needed, a constant was added or subracted to the data in each detector as determined by integrating the overlapped regions, to compensate for background variations. A Chebyshev polynomial fit was calculated for the absorption correction factors for successive values of theta (the factors were taken from the International Tables of X-ray Crystallography, Vol. II, p. 295-297) ; _computing_data_collection 'BT-1 Instrument Control Program' _computing_cell_refinement 'Fullprof' _computing_data_reduction '' _computing_structure_solution 'structure previously known' _computing_structure_refinement 'Fullprof' _computing_molecular_graphics 'Atom V4.1 for windows' _computing_publication_material '' _pd_proc_ls_profile_function 'Thompson-Cox-Hastings pseudo-Voigt' _pd_proc_ls_background_function '3rd order polynomial' _pd_proc_ls_pref_orient_corr none _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 153.5 _pd_proc_2theta_range_inc 0.05 _pd_proc_info_excluded_regions ; The region from 3.00 to 10.00 was excluded from the refinement as no reflections were present in this range. The region from 153.50 to 167.95 was excluded to ensure that the highest angle data were at the background level. ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_goodness_of_fit_all 1.40 _refine_ls_shift/su_max 0.01 _pd_proc_ls_prof_R_factor 5.40 _pd_proc_ls_prof_wR_factor 6.60 _pd_proc_ls_prof_wR_expected 5.58 _refine_special_details ; Structure refinement occurred in two separate steps, with global variables refined first followed by structural parameters. Global variables included cell dimensions (2), peak profile parameters (5), Lorentzian anisotropic peak broadening parameter (1) and background polynomial coeficients (4) for a total of 12 variables. Structural parameters included the overall scale factor (1), the z coordinate of the oxygen atom (1), and anisotropic displacement parameters for the three unique atomic sites (6) for a total of 8 variables. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity Cu CU 0.3333 0.6667 0.2500 0.0248(6) Uani 1 2 Sc SC 0.0000 0.0000 0.0000 0.0123(4) Uani 1 2 O O 0.3333 0.6667 0.08969(4) 0.0116(5) Uani 1 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0335(7) 0.0335(7) 0.0075(6) 0.000 0.000 0.0168(4) Sc 0.0112(4) 0.0112(4) 0.0145(4) 0.000 0.000 0.0056(2) O 0.0125(5) 0.0125(5) 0.0098(5) 0.000 0.000 0.0063(3) _geom_special_details ; Only unique bond lengths and angles between the major atomic sites are reported. ; 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 Cu O 1.830(1) . ? Sc O 2.1260(5) . ? 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_3 _geom_angle_publ_flag O Cu O 180.00 14_556 . ? O Sc O 98.76(2) 1_545 . ? O Sc O 180.00 . 13 ? O Sc O 81.24(4) . 13_565 ? Cu O Sc 118.78(3) . . ? Sc O Sc 98.76(2) 1_565 . ? #===END data_CuScO2neutron723K _chemical_name_systematic ; 2H Copper Scandium Oxide ; _chemical_name_common ? _chemical_formula_moiety 'Cu O2 Sc' _chemical_formula_sum 'Cu O2 Sc' _chemical_formula_weight 140.50 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Cu CU 0.7718 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' Sc SC 1.2300 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' O O 0.5803 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P6c2c' _symmetry_space_group_name_H-M 'P63/mmc' _symmetry_Int_Tables_number 194 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 3.2315(4) _cell_length_b 3.2315(4) _cell_length_c 11.418(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 103.26(1) _cell_formula_units_Z 2 _cell_measurement_temperature 723(1) _cell_special_details ; Cell dimensions at this temperature were refined from the powder diffractogram. ; _exptl_crystal_density_diffrn 4.5188(6) _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _pd_spec_size_axial 50.8 _pd_spec_size_equat 12.7 _pd_spec_size_thick 12.7 _pd_spec_mounting 'vanadium can' _pd_spec_mount_mode transmission _pd_spec_orientation vertical _pd_spec_shape cylinder _pd_char_particle_morphology 'fine powder' _pd_char_colour blue _exptl_absorpt_coefficient_mu 0.0427 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.698 _exptl_special_details ; Neutron powder diffraction data were collected using the BT-1 32-counter high resolution diffractometer at the Center for Neutron Research at the National Institute of Standards and Technology. A Cu (311) monochromator, yielding a wavelength of 1.5402(2) was employed. Collimation of 15', 20', and 7' of arc were used before and after the monochromator, and after the sample, respectively. Data were collected at room temperature over a 2-theta range of 3-168 degrees. The powdered sample was sealed in a vanadium container of length 50 mm and diameter 15.6 mm inside a dry He-filled glovebox. A vacuum furnace was used for measurements above room temperature, a closed-cycle He refrigerator was used for temperatures below room temperature. ; _diffrn_ambient_temperature 723(1) _diffrn_radiation_source 'nuclear reactor' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.5402(2) _diffrn_radiation_monochromator 'Cu(311)' _diffrn_measurement_device_type 'neutron powder diffractometer' _pd_instr_geometry '32 detector neutron diffractometer with vertical focusing' _pd_instr_location 'NBSR BT-1, NIST (USA)' _pd_meas_scan_method step _pd_meas_special_details ; 32 He-3 detectors at 5 degree intervals with a 13 degree scan range covering 2Theta from 3 to 167 degrees ; _pd_meas_number_of_points 3300 _pd_meas_2theta_range_min 3.00 _pd_meas_2theta_range_max 167.95 _pd_meas_2theta_range_inc 0.05 _pd_proc_info_data_reduction ; Data from the 32 detector banks were converted to a pseudo-single detector format using 2-point linear interpolation, after correcting for variable detector height masking and detector sensitivity, as well as two-theta offset. Where needed, a constant was added or subracted to the data in each detector as determined by integrating the overlapped regions, to compensate for background variations. A Chebyshev polynomial fit was calculated for the absorption correction factors for successive values of theta (the factors were taken from the International Tables of X-ray Crystallography, Vol. II, p. 295-297) ; _computing_data_collection 'BT-1 Instrument Control Program' _computing_cell_refinement 'Fullprof' _computing_data_reduction '' _computing_structure_solution 'structure previously known' _computing_structure_refinement 'Fullprof' _computing_molecular_graphics 'Atom V4.1 for windows' _computing_publication_material '' _pd_proc_ls_profile_function 'Thompson-Cox-Hastings pseudo-Voigt' _pd_proc_ls_background_function '3rd order polynomial' _pd_proc_ls_pref_orient_corr none _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 153.5 _pd_proc_2theta_range_inc 0.05 _pd_proc_info_excluded_regions ; The region from 3.00 to 10.00 was excluded from the refinement as no reflections were present in this range. The region from 153.50 to 167.95 was excluded to ensure that the highest angle data were at the background level. ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_goodness_of_fit_all 1.35 _refine_ls_shift/su_max 0.01 _pd_proc_ls_prof_R_factor 4.78 _pd_proc_ls_prof_wR_factor 5.83 _pd_proc_ls_prof_wR_expected 5.02 _refine_special_details ; Structure refinement occurred in two separate steps, with global variables refined first followed by structural parameters. Global variables included cell dimensions (2), peak profile parameters (5), Lorentzian anisotropic peak broadening parameter (1) and background polynomial coeficients (4) for a total of 12 variables. Structural parameters included the overall scale factor (1), the z coordinate of the oxygen atom (1), and anisotropic displacement parameters for the three unique atomic sites (6) for a total of 8 variables. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity Cu CU 0.3333 0.6667 0.2500 0.0298(6) Uani 1 2 Sc SC 0.0000 0.0000 0.0000 0.0146(4) Uani 1 2 O O 0.3333 0.6667 0.08976(5) 0.0141(5) Uani 1 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0396(7) 0.0396(7) 0.0102(6) 0.000 0.000 0.0198(4) Sc 0.0131(3) 0.0131(3) 0.0176(4) 0.000 0.000 0.0066(2) O 0.0152(5) 0.0152(5) 0.0119(5) 0.000 0.000 0.0076(3) _geom_special_details ; Only unique bond lengths and angles between the major atomic sites are reported. ; 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 Cu O 1.8296(9) . ? Sc O 2.1286(4) . ? 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_3 _geom_angle_publ_flag O Cu O 180.00 14_556 . ? O Sc O 98.76(2) 1_545 . ? O Sc O 180.00 . 13 ? O Sc O 81.24(4) . 13_565 ? Cu O Sc 118.78(3) . . ? Sc O Sc 98.76(2) 1_565 . ? #===END data_CuScO2neutron873K _chemical_name_systematic ; 2H Copper Scandium Oxide ; _chemical_name_common ? _chemical_formula_moiety 'Cu O2 Sc' _chemical_formula_sum 'Cu O2 Sc' _chemical_formula_weight 140.50 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Cu CU 0.7718 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' Sc SC 1.2300 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' O O 0.5803 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P6c2c' _symmetry_space_group_name_H-M 'P63/mmc' _symmetry_Int_Tables_number 194 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 3.2357(4) _cell_length_b 3.2357(4) _cell_length_c 11.423(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 103.57(1) _cell_formula_units_Z 2 _cell_measurement_temperature 873(1) _cell_special_details ; Cell dimensions at this temperature were refined from the powder diffractogram. ; _exptl_crystal_density_diffrn 4.5053(6) _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _pd_spec_size_axial 50.8 _pd_spec_size_equat 12.7 _pd_spec_size_thick 12.7 _pd_spec_mounting 'vanadium can' _pd_spec_mount_mode transmission _pd_spec_orientation vertical _pd_spec_shape cylinder _pd_char_particle_morphology 'fine powder' _pd_char_colour blue _exptl_absorpt_coefficient_mu 0.0427 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.698 _exptl_special_details ; Neutron powder diffraction data were collected using the BT-1 32-counter high resolution diffractometer at the Center for Neutron Research at the National Institute of Standards and Technology. A Cu (311) monochromator, yielding a wavelength of 1.5402(2) was employed. Collimation of 15', 20', and 7' of arc were used before and after the monochromator, and after the sample, respectively. Data were collected at room temperature over a 2-theta range of 3-168 degrees. The powdered sample was sealed in a vanadium container of length 50 mm and diameter 15.6 mm inside a dry He-filled glovebox. A vacuum furnace was used for measurements above room temperature, a closed-cycle He refrigerator was used for temperatures below room temperature. ; _diffrn_ambient_temperature 873(1) _diffrn_radiation_source 'nuclear reactor' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.5402(2) _diffrn_radiation_monochromator 'Cu(311)' _diffrn_measurement_device_type 'neutron powder diffractometer' _pd_instr_geometry '32 detector neutron diffractometer with vertical focusing' _pd_instr_location 'NBSR BT-1, NIST (USA)' _pd_meas_scan_method step _pd_meas_special_details ; 32 He-3 detectors at 5 degree intervals with a 13 degree scan range covering 2Theta from 3 to 167 degrees ; _pd_meas_number_of_points 3300 _pd_meas_2theta_range_min 3.00 _pd_meas_2theta_range_max 167.95 _pd_meas_2theta_range_inc 0.05 _pd_proc_info_data_reduction ; Data from the 32 detector banks were converted to a pseudo-single detector format using 2-point linear interpolation, after correcting for variable detector height masking and detector sensitivity, as well as two-theta offset. Where needed, a constant was added or subracted to the data in each detector as determined by integrating the overlapped regions, to compensate for background variations. A Chebyshev polynomial fit was calculated for the absorption correction factors for successive values of theta (the factors were taken from the International Tables of X-ray Crystallography, Vol. II, p. 295-297) ; _computing_data_collection 'BT-1 Instrument Control Program' _computing_cell_refinement 'Fullprof' _computing_data_reduction '' _computing_structure_solution 'structure previously known' _computing_structure_refinement 'Fullprof' _computing_molecular_graphics 'Atom V4.1 for windows' _computing_publication_material '' _pd_proc_ls_profile_function 'Thompson-Cox-Hastings pseudo-Voigt' _pd_proc_ls_background_function '3rd order polynomial' _pd_proc_ls_pref_orient_corr none _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 153.5 _pd_proc_2theta_range_inc 0.05 _pd_proc_info_excluded_regions ; The region from 3.00 to 10.00 was excluded from the refinement as no reflections were present in this range. The region from 153.50 to 167.95 was excluded to ensure that the highest angle data were at the background level. ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_goodness_of_fit_all 1.34 _refine_ls_shift/su_max 0.01 _pd_proc_ls_prof_R_factor 4.76 _pd_proc_ls_prof_wR_factor 5.70 _pd_proc_ls_prof_wR_expected 4.93 _refine_special_details ; Structure refinement occurred in two separate steps, with global variables refined first followed by structural parameters. Global variables included cell dimensions (2), peak profile parameters (5), Lorentzian anisotropic size broadening parameter (1) and background polynomial coeficients (4) for a total of 12 variables. Structural parameters included the overall scale factor (1), the z coordinate of the oxygen atom (1), and anisotropic displacement parameters for the three unique atomic sites (6) for a total of 8 variables. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity Cu CU 0.3333 0.6667 0.2500 0.0341(7) Uani 1 2 Sc SC 0.0000 0.0000 0.0000 0.0162(4) Uani 1 2 O O 0.3333 0.6667 0.08984(5) 0.0161(5) Uani 1 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0396(7) 0.0396(7) 0.0102(6) 0.000 0.000 0.0198(4) Sc 0.0131(3) 0.0131(3) 0.0176(4) 0.000 0.000 0.0066(2) O 0.0152(5) 0.0152(5) 0.0119(5) 0.000 0.000 0.0076(3) _geom_special_details ; Only unique bond lengths and angles between the major atomic sites are reported. ; 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 Cu O 1.830(1) . ? Sc O 2.1315(5) . ? 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_3 _geom_angle_publ_flag O Cu O 180.00 14_556 . ? O Sc O 98.76(2) 1_545 . ? O Sc O 180.00 . 13 ? O Sc O 81.24(4) . 13_565 ? Cu O Sc 118.78(3) . . ? Sc O Sc 98.76(2) 1_565 . ? #===END data_CuScO2neutron1073K _chemical_name_systematic ; 2H Copper Scandium Oxide ; _chemical_name_common ? _chemical_formula_moiety 'Cu O2 Sc' _chemical_formula_sum 'Cu O2 Sc' _chemical_formula_weight 140.50 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Cu CU 0.7718 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' Sc SC 1.2300 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' O O 0.5803 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P6c2c' _symmetry_space_group_name_H-M 'P63/mmc' _symmetry_Int_Tables_number 194 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 3.2422(4) _cell_length_b 3.2422(4) _cell_length_c 11.431(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 104.06(1) _cell_formula_units_Z 2 _cell_measurement_temperature 1073(1) _cell_special_details ; Cell dimensions at this temperature were refined from the powder diffractogram. ; _exptl_crystal_density_diffrn 4.4841(6) _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _pd_spec_size_axial 50.8 _pd_spec_size_equat 12.7 _pd_spec_size_thick 12.7 _pd_spec_mounting 'vanadium can' _pd_spec_mount_mode transmission _pd_spec_orientation vertical _pd_spec_shape cylinder _pd_char_particle_morphology 'fine powder' _pd_char_colour blue _exptl_absorpt_coefficient_mu 0.0427 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.698 _exptl_special_details ; Neutron powder diffraction data were collected using the BT-1 32-counter high resolution diffractometer at the Center for Neutron Research at the National Institute of Standards and Technology. A Cu (311) monochromator, yielding a wavelength of 1.5402(2) was employed. Collimation of 15', 20', and 7' of arc were used before and after the monochromator, and after the sample, respectively. Data were collected at room temperature over a 2-theta range of 3-168 degrees. The powdered sample was sealed in a vanadium container of length 50 mm and diameter 15.6 mm inside a dry He-filled glovebox. A vacuum furnace was used for measurements above room temperature, a closed-cycle He refrigerator was used for temperatures below room temperature. ; _diffrn_ambient_temperature 1073(1) _diffrn_radiation_source 'nuclear reactor' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.5402(2) _diffrn_radiation_monochromator 'Cu(311)' _diffrn_measurement_device_type 'neutron powder diffractometer' _pd_instr_geometry '32 detector neutron diffractometer with vertical focusing' _pd_instr_location 'NBSR BT-1, NIST (USA)' _pd_meas_scan_method step _pd_meas_special_details ; 32 He-3 detectors at 5 degree intervals with a 13 degree scan range covering 2Theta from 3 to 167 degrees ; _pd_meas_number_of_points 3300 _pd_meas_2theta_range_min 3.00 _pd_meas_2theta_range_max 167.95 _pd_meas_2theta_range_inc 0.05 _pd_proc_info_data_reduction ; Data from the 32 detector banks were converted to a pseudo-single detector format using 2-point linear interpolation, after correcting for variable detector height masking and detector sensitivity, as well as two-theta offset. Where needed, a constant was added or subracted to the data in each detector as determined by integrating the overlapped regions, to compensate for background variations. A Chebyshev polynomial fit was calculated for the absorption correction factors for successive values of theta (the factors were taken from the International Tables of X-ray Crystallography, Vol. II, p. 295-297) ; _computing_data_collection 'BT-1 Instrument Control Program' _computing_cell_refinement 'Fullprof' _computing_data_reduction '' _computing_structure_solution 'structure previously known' _computing_structure_refinement 'Fullprof' _computing_molecular_graphics 'Atom V4.1 for windows' _computing_publication_material '' _pd_proc_ls_profile_function 'Thompson-Cox-Hastings pseudo-Voigt' _pd_proc_ls_background_function '3rd order polynomial' _pd_proc_ls_pref_orient_corr none _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 153.5 _pd_proc_2theta_range_inc 0.05 _pd_proc_info_excluded_regions ; The region from 3.00 to 10.00 was excluded from the refinement as no reflections were present in this range. The region from 153.50 to 167.95 was excluded to ensure that the highest angle data were at the background level. ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_goodness_of_fit_all 1.40 _refine_ls_shift/su_max 0.01 _pd_proc_ls_prof_R_factor 4.70 _pd_proc_ls_prof_wR_factor 5.72 _pd_proc_ls_prof_wR_expected 4.83 _refine_special_details ; Structure refinement occurred in two separate steps, with global variables refined first followed by structural parameters. Global variables included cell dimensions (2), peak profile parameters (5), Lorentzian anisotropic peak broadening parameter (1) and background polynomial coeficients (4) for a total of 12 variables. Structural parameters included the overall scale factor (1), the z coordinate of the oxygen atom (1), and anisotropic displacement parameters for the three unique atomic sites (6) for a total of 8 variables. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity Cu CU 0.3333 0.6667 0.2500 0.0426(9) Uani 1 2 Sc SC 0.0000 0.0000 0.0000 0.0198(4) Uani 1 2 O O 0.3333 0.6667 0.08994(5) 0.0198(6) Uani 1 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0562(9) 0.0562(9) 0.0152(7) 0.000 0.000 0.0281(5) Sc 0.0176(4) 0.0176(4) 0.0243(5) 0.000 0.000 0.0088(2) O 0.0215(6) 0.0215(6) 0.0164(5) 0.000 0.000 0.0108(3) _geom_special_details ; Only unique bond lengths and angles between the major atomic sites are reported. ; 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 Cu O 1.830(1) . ? Sc O 2.1356(5) . ? 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_3 _geom_angle_publ_flag O Cu O 180.00 14_556 . ? O Sc O 98.77(2) 1_545 . ? O Sc O 180.00 . 13 ? O Sc O 81.24(5) . 13_565 ? Cu O Sc 118.78(4) . . ? Sc O Sc 98.77(2) 1_565 . ? #===END data_CuScO2neutron1206K _chemical_name_systematic ; 2H Copper Scandium Oxide ; _chemical_name_common ? _chemical_formula_moiety 'Cu O2 Sc' _chemical_formula_sum 'Cu O2 Sc' _chemical_formula_weight 140.50 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Cu CU 0.7718 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' Sc SC 1.2300 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' O O 0.5803 'Neutron News, Vol. 3, No. 3, 1992, pp. 29-37' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P6c2c' _symmetry_space_group_name_H-M 'P63/mmc' _symmetry_Int_Tables_number 194 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z' '-y, x-y, z' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z-1/2' 'y, x, z-1/2' '-y, -x, z' '-x+y, y, z' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z' 'y, -x+y, -z' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' 'x-y, x, -z' _cell_length_a 3.2472(4) _cell_length_b 3.2472(4) _cell_length_c 11.436(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 104.43(1) _cell_formula_units_Z 2 _cell_measurement_temperature 1206(1) _cell_special_details ; Cell dimensions at this temperature were refined from the powder diffractogram. ; _exptl_crystal_density_diffrn 4.4682(6) _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _pd_spec_size_axial 50.8 _pd_spec_size_equat 12.7 _pd_spec_size_thick 12.7 _pd_spec_mounting 'vanadium can' _pd_spec_mount_mode transmission _pd_spec_orientation vertical _pd_spec_shape cylinder _pd_char_particle_morphology 'fine powder' _pd_char_colour blue _exptl_absorpt_coefficient_mu 0.0427 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.698 _exptl_special_details ; Neutron powder diffraction data were collected using the BT-1 32-counter high resolution diffractometer at the Center for Neutron Research at the National Institute of Standards and Technology. A Cu (311) monochromator, yielding a wavelength of 1.5402(2) was employed. Collimation of 15', 20', and 7' of arc were used before and after the monochromator, and after the sample, respectively. Data were collected at room temperature over a 2-theta range of 3-168 degrees. The powdered sample was sealed in a vanadium container of length 50 mm and diameter 15.6 mm inside a dry He-filled glovebox. A vacuum furnace was used for measurements above room temperature, a closed-cycle He refrigerator was used for temperatures below room temperature. ; _diffrn_ambient_temperature 1206(1) _diffrn_radiation_source 'nuclear reactor' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.5402(2) _diffrn_radiation_monochromator 'Cu(311)' _diffrn_measurement_device_type 'neutron powder diffractometer' _pd_instr_geometry '32 detector neutron diffractometer with vertical focusing' _pd_instr_location 'NBSR BT-1, NIST (USA)' _pd_meas_scan_method step _pd_meas_special_details ; 32 He-3 detectors at 5 degree intervals with a 13 degree scan range covering 2Theta from 3 to 167 degrees ; _pd_meas_number_of_points 3300 _pd_meas_2theta_range_min 3.00 _pd_meas_2theta_range_max 167.95 _pd_meas_2theta_range_inc 0.05 _pd_proc_info_data_reduction ; Data from the 32 detector banks were converted to a pseudo-single detector format using 2-point linear interpolation, after correcting for variable detector height masking and detector sensitivity, as well as two-theta offset. Where needed, a constant was added or subracted to the data in each detector as determined by integrating the overlapped regions, to compensate for background variations. A Chebyshev polynomial fit was calculated for the absorption correction factors for successive values of theta (the factors were taken from the International Tables of X-ray Crystallography, Vol. II, p. 295-297) ; _computing_data_collection 'BT-1 Instrument Control Program' _computing_cell_refinement 'Fullprof' _computing_data_reduction '' _computing_structure_solution 'structure previously known' _computing_structure_refinement 'Fullprof' _computing_molecular_graphics 'Atom V4.1 for windows' _computing_publication_material '' _pd_proc_ls_profile_function 'Thompson-Cox-Hastings pseudo-Voigt' _pd_proc_ls_background_function '3rd order polynomial' _pd_proc_ls_pref_orient_corr none _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 153.5 _pd_proc_2theta_range_inc 0.05 _pd_proc_info_excluded_regions ; The region from 3.00 to 10.00 was excluded from the refinement as no reflections were present in this range. The region from 153.50 to 167.95 was excluded to ensure that the highest angle data were at the background level. ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_goodness_of_fit_all 1.47 _refine_ls_shift/su_max 0.01 _pd_proc_ls_prof_R_factor 4.78 _pd_proc_ls_prof_wR_factor 5.87 _pd_proc_ls_prof_wR_expected 4.85 _refine_special_details ; Structure refinement occurred in two separate steps, with global variables refined first followed by structural parameters. Global variables included cell dimensions (2), peak profile parameters (5), Lorentzian anisotropic peak broadening parameter (1) and background polynomial coeficients (4) for a total of 12 variables. Structural parameters included the overall scale factor (1), the z coordinate of the oxygen atom (1), and anisotropic displacement parameters for the three unique atomic sites (6) for a total of 8 variables. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity Cu CU 0.3333 0.6667 0.2500 0.048(1) Uani 1 2 Sc SC 0.0000 0.0000 0.0000 0.0230(5) Uani 1 2 O O 0.3333 0.6667 0.09000(5) 0.0236(6) Uani 1 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.064(1) 0.064(1) 0.0178(8) 0.000 0.000 0.032(1) Sc 0.0201(4) 0.0201(4) 0.0289(5) 0.000 0.000 0.0101(2) O 0.0253(6) 0.0253(6) 0.0203(6) 0.000 0.000 0.0127(3) _geom_special_details ; Only unique bond lengths and angles between the major atomic sites are reported. ; 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 Cu O 1.830(1) . ? Sc O 2.1387(6) . ? 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_3 _geom_angle_publ_flag O Cu O 180.00 14_556 . ? O Sc O 98.78(2) 1_545 . ? O Sc O 180.00 . 13 ? O Sc O 81.22(5) . 13_565 ? Cu O Sc 118.77(4) . . ? Sc O Sc 98.78(2) 1_565 . ? #===END