A Lithium-Scandium Sulfate with Second-Harmonic Generation Response and Deep-Ultraviolet Transparency
Geng, Zilong; Tang, Hong-Xin; Fu, Ruibiao; Ma, Zuju; Wu, Xintao; Dalton Transactions  (2023) –; doi:10.1039/D3DT03071G

data_7714123
_publ_section_title
;
 A Lithium-Scandium Sulfate with Second-Harmonic Generation Response and
 Deep-Ultraviolet Transparency
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03071G
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'H4 Li O10 S2 Sc'
_chemical_formula_sum            'H4 Li O10 S2 Sc'
_chemical_formula_weight         280.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-02-17 deposited with the CCDC.	2023-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.17110(10)
_cell_length_b                   8.62070(10)
_cell_length_c                   18.5151(2)
_cell_measurement_reflns_used    6566
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      59.8720
_cell_measurement_theta_min      4.1410
_cell_volume                     825.38(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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      5.00 106.00   0.50    0.05    --   76.11 -19.00   0.00  202
  2  \w     40.00 104.00   0.50    0.05    --   76.11 -77.00  30.00  128
  3  \w     51.00 142.00   0.50    0.05    --   76.11  19.00-150.00  182
  4  \w    102.00 149.00   0.50    0.05    --   76.11 125.00  90.00   94
  5  \w     23.00  63.00   0.50    0.05    --   76.11 -99.00  30.00   80
  6  \w     86.00 111.00   0.50    0.05    --   76.11-125.00-150.00   50
  7  \w     23.00  87.00   0.50    0.05    --   76.11-125.00  30.00  128
  8  \w     69.00  98.00   0.50    0.05    --   76.11 -99.00  30.00   58
  9  \w    -68.00  16.00   0.50    0.05    --   -0.94 -57.00-180.00  168
 10  \w    -65.00 -34.00   0.50    0.05    --   -0.94 -57.00 -90.00   62
 11  \w    -30.00   3.00   0.50    0.05    --   -0.94 -57.00 -90.00   66
 12  \w     -8.00  33.00   0.50    0.05    --   -0.94 -99.00  60.00   82
 13  \w   -150.00-104.00   0.50    0.05    --  -77.99-125.00 150.00   92
 14  \w    -71.00  -1.00   0.50    0.05    --  -77.99  38.00 -90.00  140
 15  \w    -63.00 -34.00   0.50    0.05    --  -77.99  38.00-150.00   58
 16  \w    -95.00 -37.00   0.50    0.05    --  -77.99  57.00-150.00  116
 17  \w    -48.00 -23.00   0.50    0.05    --  -77.99 125.00-120.00   50
 18  \w    -56.00 -31.00   0.50    0.05    --  -77.99 125.00-150.00   50
 19  \w   -111.00 -58.00   0.50    0.05    --  -77.99 125.00-150.00  106
 20  \w   -101.00 -75.00   0.50    0.05    --  -77.99 125.00-120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0002093000
_diffrn_orient_matrix_UB_12      -0.1525462000
_diffrn_orient_matrix_UB_13      0.0136650000
_diffrn_orient_matrix_UB_21      -0.0565449000
_diffrn_orient_matrix_UB_22      -0.0286789000
_diffrn_orient_matrix_UB_23      -0.0693310000
_diffrn_orient_matrix_UB_31      0.2526943000
_diffrn_orient_matrix_UB_32      -0.0062662000
_diffrn_orient_matrix_UB_33      -0.0154789000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6104
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        52.019
_diffrn_reflns_theta_max         52.019
_diffrn_reflns_theta_min         4.152
_diffrn_source                   GaK\a
_exptl_absorpt_coefficient_mu    8.584
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.98a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.254
_exptl_crystal_description       slice
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.128(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1381
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+0.4951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.644
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                1360
_reflns_number_total             1381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03071g2.cif
_cod_data_source_block           zl-li_autored
_cod_database_code               7714123
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Li Sc O N S'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.872(19)
 0.128(19)
2. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(S2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Rotating group:
 O9(H1,H2), O10(H3,H4)
;
_shelx_res_checksum              57389
_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 2.026
_oxdiff_exptl_absorpt_empirical_full_min 0.658