A-site cation manipulation of exemplary second harmonic generation response and optical anisotropy in rare-earth borates.
Song, Jie; Zhao, Huijian; Li, Conggang; Ye, Ning; Hu, Zhanggui; Wu, Yicheng; Chemical science 15 (2024) 16196–16204; doi:10.1039/d4sc05081a

data_1572534
_publ_section_title
;
 A-site cation manipulation of exemplary second harmonic generation
 response and optical anisotropy in rare-earth borates.
;
_journal_issue                   39
_journal_name_full               'Chemical science'
_journal_page_first              16196
_journal_page_last               16204
_journal_paper_doi               10.1039/d4sc05081a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'B3 K2 La2 Na O9'
_chemical_formula_sum            'B3 K2 La2 Na O9'
_chemical_formula_weight         555.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           38
_space_group_name_Hall           'A 2 -2'
_space_group_name_H-M_alt        'A m m 2'
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-20
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2024-07-30 deposited with the CCDC.	2024-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.1775(4)
_cell_length_b                   11.4157(10)
_cell_length_c                   7.2715(5)
_cell_measurement_reflns_used    1121
_cell_measurement_temperature    297
_cell_measurement_theta_max      31.6350
_cell_measurement_theta_min      3.3110
_cell_volume                     429.78(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      297
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.862
_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    -47.72  74.08   0.30    2.00    --  -16.77  50.43-109.55  406
  2  \f     55.13 214.43   0.30    2.00  74.14 -16.73  28.85    --   531
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0062274000
_diffrn_orient_matrix_UB_12      0.0191842000
_diffrn_orient_matrix_UB_13      -0.0926118000
_diffrn_orient_matrix_UB_21      0.1358306000
_diffrn_orient_matrix_UB_22      0.0065451000
_diffrn_orient_matrix_UB_23      0.0078277000
_diffrn_orient_matrix_UB_31      0.0171183000
_diffrn_orient_matrix_UB_32      -0.0587356000
_diffrn_orient_matrix_UB_33      -0.0294892000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1389
_diffrn_reflns_point_group_measured_fraction_full 0.877
_diffrn_reflns_point_group_measured_fraction_max 0.729
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.736
_diffrn_reflns_theta_min         3.322
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.856
_exptl_absorpt_correction_T_max  0.03422
_exptl_absorpt_correction_T_min  0.01200
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.292
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         2.794
_refine_diff_density_min         -2.572
_refine_diff_density_rms         0.445
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(10)
_refine_ls_extinction_coef       0.017(5)
_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   1.121
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         613
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0497
_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^)+(0.1080P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1279
_reflns_Friedel_coverage         0.580
_reflns_Friedel_fraction_full    0.770
_reflns_Friedel_fraction_max     0.575
_reflns_number_gt                601
_reflns_number_total             613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05081a2.cif
_cod_data_source_block           mo_3171_autored
_cod_depositor_comments
'Adding full bibliography for 1572534--1572535.cif.'
_cod_database_code               1572534
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97(10)
 0.03(10)
2. Uiso/Uaniso restraints and constraints
Uanis(B3) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
;
_shelx_res_checksum              62894
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.283
_oxdiff_exptl_absorpt_empirical_full_min 0.367