Crystal structure across the β to α phase transition in thermoelectric Cu<sub>2-<i>x</i></sub> Se.
Eikeland, Espen; Blichfeld, Anders B.; Borup, Kasper A.; Zhao, Kunpeng; Overgaard, Jacob; Shi, Xun; Chen, Lidong; Iversen, Bo B.; IUCrJ 4 (2017) 476–485; doi:10.1107/S2052252517005553

data_1556753
_publ_section_title
;
 Crystal structure across the \b to \a phase transition in thermoelectric
 Cu<sub>2-<i>x</i></sub> Se.
;
_journal_coeditor_code           LC5071SUP1
_journal_issue                   'Pt 4'
_journal_name_full               IUCrJ
_journal_page_first              476
_journal_page_last               485
_journal_paper_doi               10.1107/S2052252517005553
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         '0.06(Cu32), 1(Se)'
_chemical_formula_sum            'Cu1.94 Se'
_chemical_formula_weight         202.55
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_audit_creation_date             2017-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.8538(3)
_cell_length_b                   5.8538(3)
_cell_length_c                   5.8538(3)
_cell_measurement_reflns_used    163
_cell_measurement_temperature    400.00(11)
_cell_measurement_theta_max      24.8490
_cell_measurement_theta_min      6.0070
_cell_volume                     200.592(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -82.00 -35.00   1.00   90.00    --   18.69-178.00 -90.00   47
  2  \w    -28.00  87.00   1.00   90.00    --   18.69  38.00  30.00  115
  3  \w    -66.00  71.00   1.00   90.00    --  -19.62  38.00  30.00  137
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            277
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.961
_diffrn_reflns_theta_min         6.036
_exptl_absorpt_coefficient_mu    38.257
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    6.707
_exptl_crystal_description       irregular
_exptl_crystal_F_000             362
_exptl_crystal_size_max          0.0908
_exptl_crystal_size_mid          0.0493
_exptl_crystal_size_min          0.0167
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.292
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     6
_refine_ls_number_reflns         22
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.261
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+16.3542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22
_reflns_number_total             22
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lc5071.cif
_cod_data_source_block           Cu1p95Se_CVT1_400K
_cod_original_cell_volume        200.59(3)
_cod_database_code               1556753
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Cu2) = Uanis(Cu1)
2. Others
 2*[Sof(Cu1)]+8*[Sof(Cu2)]=1.95 with esd of 0.01
;