Early stage of the single-crystal growth and tipping point of the cationic site preference in Gd-doped Zintl phase thermoelectric materials
Sa, Hayeon; Lee, Junsu; Hong, Yeongjin; Han, Mi-Kyung; Jo, Hongil; Moon, Dohyun; Ok, Kang Min; Kim, Sung-Jin; You, Tae-Soo; CrystEngComm 23 (2021) 7097–7107; doi:10.1039/D1CE00877C

data_7243576
_publ_section_title
;
 Early stage of the single-crystal growth and tipping point of the
 cationic site preference in Gd-doped Zintl phase thermoelectric materials
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              7097
_journal_page_last               7107
_journal_paper_doi               10.1039/D1CE00877C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'Ca10.63 Gd0.37 Sb9.74'
_chemical_formula_sum            'Ca10.63 Gd0.37 Sb9.74'
_chemical_formula_weight         1670.08
_chemical_name_systematic        Ca10.63(2)Gd0.37Sb9.74(1)
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_audit_block_doi                 10.25505/fiz.icsd.cc27y0bk
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2021-06-14 deposited with the CCDC.	2021-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9875(17)
_cell_length_b                   11.9875(17)
_cell_length_c                   17.360(3)
_cell_measurement_reflns_used    9424
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.410
_cell_measurement_theta_min      1.772
_cell_volume                     2494.6(7)
_computing_cell_refinement       '<i>HKL3000sm</i>(Otwinowski & Minor, 1997)'
_computing_data_collection
'<i>PAL BL2D-SMDC Program</i>(Shin et.al, 2016)'
_computing_data_reduction        '<i>HKL3000sm</i>(Otwinowski & Minor, 1997)'
_computing_molecular_graphics    '<i>DIAMOND 4</i>(Putz&Brandenburg, 2014)'
_computing_publication_material  '<i>publCIF</i>(Westrip, 2010)'
_computing_structure_refinement  '<i>SHELXL-2018</i>(Sheldrick, 2015b)'
_computing_structure_solution    '<i>SHELXT-2018</i>(Sheldrick, 2015a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.610
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9424
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         22.410
_diffrn_reflns_theta_min         1.772
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    8.783
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'<i>HKL3000sm Scalepack</i>(Otwinowski et.al,2003)'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    4.447
_exptl_crystal_density_meas      4.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2932
_exptl_crystal_preparation       'Thermoelectric properties'
_exptl_crystal_recrystallization_method Arc-melting
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.009
_refine_diff_density_max         1.478
_refine_diff_density_min         -2.276
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0486P)^2^+42.5657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                732
_reflns_number_total             770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00877c2.cif
_cod_data_source_block           JS92HY
_cod_depositor_comments
'Adding full bibliography for 7243575--7243577.cif.'
_cod_original_cell_volume        2494.7(9)
_cod_database_code               7243576
_shelx_estimated_absorpt_t_min   0.810
_shelx_estimated_absorpt_t_max   0.925
_shelxl_version_number           2013-3
_shelx_res_checksum              96949
_shelx_hkl_checksum              66419