Discovery of chalcogenides structures and compositions using mixed fluxes
Zhou, Xiuquan; Kolluru, Venkata Surya Chaitanya; Xu, Wenqian; Wang, Luqing; Chang, Tieyan; Chen, Yu-Sheng; Yu, Lei; Wen, Jianguo; Chan, Maria K. Y.; Chung, Duck Young; Kanatzidis, Mercouri G.; Nature 612 (2022) 72–77; doi:10.1038/s41586-022-05307-7

data_1568158
_publ_section_title
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 Discovery of chalcogenides structures and compositions using mixed fluxes
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_journal_issue                   7938
_journal_name_full               Nature
_journal_page_first              72
_journal_page_last               77
_journal_paper_doi               10.1038/s41586-022-05307-7
_journal_volume                  612
_journal_year                    2022
_chemical_formula_moiety         '0.25(Ba2.53 Cu7.31 K3.47 S3.63 Se4.37)'
_chemical_formula_sum            'Ba0.63 Cu1.83 K0.87 S0.9 Se1.1'
_chemical_formula_weight         352.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           55
_space_group_name_Hall           '-P 2 2ab'
_space_group_name_H-M_alt        'P b a m'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     iterative
_audit_contact_author_name
;
;
_audit_creation_date             2022-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4830(2)
_cell_length_b                   16.0919(4)
_cell_length_c                   4.10410(10)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.30
_cell_measurement_theta_min      2.72
_cell_volume                     494.20(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           Sychrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            23292
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         23.469
_diffrn_reflns_theta_min         1.472
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.814
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6433
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0849 before and 0.0713 after correction.
The Ratio of minimum to maximum transmission is 0.8636.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.738
_exptl_crystal_description       irregular
_exptl_crystal_F_000             627
_refine_diff_density_max         4.933
_refine_diff_density_min         -4.472
_refine_diff_density_rms         0.424
_refine_ls_extinction_coef       0.0024(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         1696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+5.1487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1487
_reflns_number_total             1696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            XXIX_Ba0.63Cu1.83K0.87S0.91Se1.09.cif
_cod_data_source_block           XXIX
_cod_original_formula_sum        'Ba0.63 Cu1.83 K0.87 S0.90 Se1.10'
_cod_database_code               1568158
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Shared sites
{Ba06, K06}
{Se03, S03}
{Se05, S05}
2. Uiso/Uaniso restraints and constraints
Uanis(Ba06) = Uanis(K06)
Uanis(Se03) = Uanis(S03)
Uanis(Se05) = Uanis(S05)
3. Others
 Sof(K06)=0.5*(1-FVAR(2))
 Sof(Ba06)=0.5*FVAR(2)
 Sof(S03)=0.5*(1-FVAR(3))
 Sof(Se03)=0.5*FVAR(3)
 Sof(S05)=0.5*(1-FVAR(4))
 Sof(Se05)=0.5*FVAR(4)
;
_olex2_submission_special_instructions 'No special instructions were received'