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_1572535
_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_absolute_configuration ad
_chemical_formula_moiety         'B3 K3 La2 O9'
_chemical_formula_sum            'B3 K3 La2 O9'
_chemical_formula_weight         571.55
_space_group_crystal_system      orthorhombic
_space_group_IT_number           30
_space_group_name_Hall           'P 2 -2bc'
_space_group_name_H-M_alt        'P n c 2'
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_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            4
_cell_length_a                   6.7996(13)
_cell_length_b                   16.420(3)
_cell_length_c                   9.4868(17)
_cell_measurement_reflns_used    1603
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      30.8490
_cell_measurement_theta_min      2.4600
_cell_volume                     1059.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.846
_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    -61.61  33.19   0.20    2.50    --  -16.77  75.16  36.71  474
  2  \f    151.13 301.93   0.20    2.50  74.14 -16.73  28.85    --   754
  3  \f    -25.75 154.25   1.00    1.00 -25.75   0.00  73.76    --   180
;
_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      -0.0022801000
_diffrn_orient_matrix_UB_12      -0.0011103000
_diffrn_orient_matrix_UB_13      0.0748647000
_diffrn_orient_matrix_UB_21      -0.1037967000
_diffrn_orient_matrix_UB_22      0.0053613000
_diffrn_orient_matrix_UB_23      -0.0014200000
_diffrn_orient_matrix_UB_31      -0.0127976000
_diffrn_orient_matrix_UB_32      -0.0429820000
_diffrn_orient_matrix_UB_33      -0.0021910000
_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  0.0801
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7260
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.582
_diffrn_reflns_theta_min         2.479
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.584
_exptl_crystal_description       plate
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.709
_refine_diff_density_min         -1.991
_refine_diff_density_rms         0.253
_refine_ls_abs_structure_details
;
 Flack x determined using 922 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3015
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0527P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0960
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.705
_reflns_number_gt                2442
_reflns_number_total             3015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05081a2.cif
_cod_data_source_block           mo_4_65_11_1_autored
_cod_depositor_comments
'Adding full bibliography for 1572534--1572535.cif.'
_cod_database_code               1572535
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.711
_olex2_refinement_description
;
1. Rigid bond restraints
 O3A, O3, B1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
2. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(O3A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(O3A)=1-FVAR(1)
 Sof(O3)=FVAR(1)
 Fixed Sof: La1(0.5) La3(0.5) O2(0.5) O5(0.5) O9(0.5)
;
_shelx_res_checksum              31105
_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 2.715
_oxdiff_exptl_absorpt_empirical_full_min 0.704