Synthesis, crystal structure, photocatalysis, photocurrent response: one-dimensional K2HgSnSe4 and three-dimensional Na6Cu8Sn3Se13
Teri, Gele; Li, Na; Bai, Sagala; E., Namila; Baiyin, Menghe; CrystEngComm 23 (2021) 6079–6085; doi:10.1039/D1CE00821H

data_7243356
_publ_section_title
;
 Synthesis, crystal structure, photocatalysis, photocurrent response:
 one-dimensional K2HgSnSe4 and three-dimensional Na6Cu8Sn3Se13
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              6079
_journal_page_last               6085
_journal_paper_doi               10.1039/D1CE00821H
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         '0.5(Hg2 K4 Se8 Sn2)'
_chemical_formula_sum            'Hg K2 Se4 Sn'
_chemical_formula_weight         713.32
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-11-19
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2021-04-12 deposited with the CCDC.	2021-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0531(5)
_cell_length_b                   8.0531(5)
_cell_length_c                   6.9501(8)
_cell_measurement_reflns_used    293
_cell_measurement_temperature    292.22(10)
_cell_measurement_theta_max      28.0010
_cell_measurement_theta_min      3.8560
_cell_volume                     450.73(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.22(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9130
_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    -60.00 -21.00   1.00    1.31    --  -18.95 -30.00 134.00   39
  2  \w     39.00  94.00   1.00    1.31    --   18.88 178.00 -30.00   55
  3  \w     41.00  78.00   1.00    1.31    --   18.88 178.00  60.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0832831000
_diffrn_orient_matrix_UB_12      -0.0278580000
_diffrn_orient_matrix_UB_13      -0.0081173000
_diffrn_orient_matrix_UB_21      0.0136110000
_diffrn_orient_matrix_UB_22      -0.0192446000
_diffrn_orient_matrix_UB_23      -0.0982958000
_diffrn_orient_matrix_UB_31      0.0252277000
_diffrn_orient_matrix_UB_32      -0.0813395000
_diffrn_orient_matrix_UB_33      0.0260955000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            439
_diffrn_reflns_theta_full        25.60
_diffrn_reflns_theta_max         25.61
_diffrn_reflns_theta_min         3.58
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    36.763
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    5.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.067
_refine_diff_density_min         -5.803
_refine_diff_density_rms         0.850
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.330
_refine_ls_matrix_type           full
_refine_ls_number_parameters     11
_refine_ls_number_reflns         130
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.298
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0960
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+266.7308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2515
_refine_ls_wR_factor_ref         0.2524
_reflns_number_gt                124
_reflns_number_total             130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1ce00821h2.cif
_cod_data_source_block           exp_4
_cod_depositor_comments
'Adding full bibliography for 7243356--7243357.cif.'
_cod_database_code               7243356
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Hg1 \\sim Sn1: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
2. Others
 Fixed Sof: Hg1(0.0625) Sn1(0.0625)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 10.714
_oxdiff_exptl_absorpt_empirical_full_min 0.258