Highly Distorted [HgS<sub>4</sub>] Motif-Driven Structural Symmetry Degradation and Strengthened Second-Harmonic Generation Response in the Defect Diamond-Like Chalcogenide Hg<sub>3</sub>P<sub>2</sub>S<sub>8</sub>.
Xing, Wenhao; Liang, Fei; Tang, Chunlan; Uykur, Ece; Lin, Zheshuai; Yao, Jiyong; Yin, Wenlong; Kang, Bin; ACS applied materials & interfaces  (2021) –; doi:10.1021/acsami.1c06933

data_4518923
_publ_section_title
;
 Highly Distorted [HgS<sub>4</sub>] Motif-Driven Structural Symmetry
 Degradation and Strengthened Second-Harmonic Generation Response in the
 Defect Diamond-Like Chalcogenide
 Hg<sub>3</sub>P<sub>2</sub>S<sub>8</sub>.
;
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_paper_doi               10.1021/acsami.1c06933
_journal_year                    2021
_chemical_formula_moiety         '0.25(Hg12 P8 S32)'
_chemical_formula_sum            'Hg3 P2 S8'
_chemical_formula_weight         920.19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-19
_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                   16.3786(8)
_cell_length_b                   8.1613(4)
_cell_length_c                   9.2723(5)
_cell_measurement_reflns_used    5190
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      26.3580
_cell_measurement_theta_min      3.5600
_cell_volume                     1239.43(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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    -28.00  51.00   0.50    9.00    --   -8.37  74.00  21.00  158
  2  \w    -13.00  54.00   0.50    9.00    --   -8.37  57.00  60.00  134
  3  \w    -20.00  63.00   0.50    9.00    --   -8.37  19.00   0.00  166
  4  \w    -24.00   7.00   0.50    9.00    --   -8.37 -99.00-150.00   62
  5  \w      8.00  42.00   0.50    9.00    --    9.46 -99.00-180.00   68
  6  \w     -6.00  24.00   0.50    9.00    --    9.46 -99.00 -30.00   60
  7  \w    -22.00  17.00   0.50    9.00    --   -8.37 -99.00 120.00   78
  8  \w    -80.00   5.00   0.50    9.00    --   -8.37 -74.00-106.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0554873000
_diffrn_orient_matrix_UB_12      -0.0284781000
_diffrn_orient_matrix_UB_13      -0.0261854000
_diffrn_orient_matrix_UB_21      -0.0066795000
_diffrn_orient_matrix_UB_22      -0.0719889000
_diffrn_orient_matrix_UB_23      0.0240144000
_diffrn_orient_matrix_UB_31      -0.0522250000
_diffrn_orient_matrix_UB_32      0.0395422000
_diffrn_orient_matrix_UB_33      0.0247481000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7688
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.551
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    38.623
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.931
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details
;
 Flack x determined using 532 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(7)
_refine_ls_extinction_coef       0.00057(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1260
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0153
_refine_ls_R_factor_gt           0.0145
_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^)+(0.0169P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0353
_refine_ls_wR_factor_ref         0.0356
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                1207
_reflns_number_total             1260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c06933_si_002.cif
_cod_data_source_block           Hg3P2S8
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               4518923
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         HgPS
_shelx_estimated_absorpt_t_max   0.512
_shelx_estimated_absorpt_t_min   0.390
_reflns_odcompleteness_completeness 83.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
;
_shelx_res_checksum              49995
_shelx_hkl_checksum              40549
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.451
_oxdiff_exptl_absorpt_empirical_full_min 0.564