Tetrahedron-based deep-ultraviolet nonlinear optical crystal with optimized KBe2BO3F2-like structure and disordered cations
Xu, Junxin; Sha, Hongyuan; Shang, Yanran; Wang, Zujian; Su, Rongbing; He, Chao; Yang, Xiaoming; Long, Xifa; New Journal of Chemistry 47 (2023) 7521–7526; doi:10.1039/D3NJ01114C

data_7062386
_publ_section_title
;
 Tetrahedron-based deep-ultraviolet nonlinear optical crystal with
 optimized KBe2BO3F2-like structure and disordered cations
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7521
_journal_page_last               7526
_journal_paper_doi               10.1039/D3NJ01114C
_journal_volume                  47
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         'Li2 O8 Rb S2, H4 N'
_chemical_formula_sum            'H4 Li2 N O8 Rb S2'
_chemical_formula_weight         309.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-14 deposited with the CCDC.	2023-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.751(4)
_cell_length_b                   9.112(4)
_cell_length_c                   5.291(4)
_cell_measurement_reflns_used    1685
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5010
_cell_measurement_theta_min      2.2257
_cell_volume                     421.9(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2518
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.228
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.376
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.6396
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.436
_exptl_crystal_description       prism
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         740
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0374P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                684
_reflns_number_total             740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01114c1.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7062386.cif.'
_cod_database_code               7062386
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.448
_shelx_estimated_absorpt_t_min   0.251
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.92(3)
 0.08(3)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups
3. Shared sites
{Rb1, N1}
4. Uiso/Uaniso restraints and constraints
Uanis(Rb1) = Uanis(N1)
5. Others
 Fixed Sof: Rb1(0.5) N1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5)
6.a Riding coordinates:
 N1(H1A,H1B,H1C), N1(H1D)
;
_shelx_res_checksum              55646
_shelx_hkl_checksum              54409
_olex2_submission_special_instructions 'No special instructions were received'