High-pressure single crystal X-ray diffraction study of thermoelectric ZnSb and β-Zn4Sb3.
Borup, Mette Andersen; Blichfeld, Anders Bank; Madsen, Solveig Røgild; Iversen, Bo Brummerstedt; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15097–15103; doi:10.1039/c6dt02323a

data_7040413
_publ_section_title
;
 High-pressure single crystal X-ray diffraction study of thermoelectric
 ZnSb and \b-Zn4Sb3.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15097
_journal_page_last               15103
_journal_paper_doi               10.1039/c6dt02323a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'Sb30 Zn38.47'
_chemical_formula_sum            'Sb30 Zn38.48'
_chemical_formula_weight         6168.20
_chemical_name_systematic        'Zinc antimonide'
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-11 deposited with the CCDC.
2016-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   11.6998(12)
_cell_length_b                   11.6998(12)
_cell_length_c                   12.005(2)
_cell_measurement_pressure       7590000(120000)
_cell_measurement_reflns_used    917
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.87
_cell_measurement_theta_min      4.15
_cell_volume                     1423.1(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.877
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.877
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4013
_diffrn_reflns_point_group_measured_fraction_full 0.877
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.483
_diffrn_reflns_theta_min         2.748
_exptl_absorpt_coefficient_mu    15.680
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.6304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0918 before and 0.0644 after correction.
The Ratio of minimum to maximum transmission is 0.8467.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'metallic grayish gray'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    7.197
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2685
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.303
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         285
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.245
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0196P)^2^+116.4862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                234
_reflns_number_total             285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02323a2.cif
_cod_data_source_block           Zn4Sb3_EM_P8
_cod_depositor_comments
;Adding full bibliography for 7040405--7040434.cif.

 Adding full bibliography for 7040405--7040434.cif.
;
_cod_original_cell_volume        1423.1(4)
_cod_database_code               7040413
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uiso(Zn3) = Uiso(Zn4) = Uiso(Zn2)
2. Others
 1*[Sof(Zn1)]+1*[Sof(Zn3)]+1*[Sof(Zn4)]+1*[Sof(Zn2)]=1.068 with esd of 0.002
;