Lanthanide Thioborates, an Emerging Class of Nonlinear Optical Materials, Efficiently Synthesized Using the Boron-Chalcogen Mixture Method
Breton, Logan S.; Morrison, Gregory; Lacroix, Matthew; Halasyamani, P. Shiv; Zur Loye, Hans-Conrad; Chemical Communications  (2022) –; doi:10.1039/D2CC01260J

data_7130256
_publ_section_title
;
 Lanthanide Thioborates, an Emerging Class of Nonlinear Optical Materials,
 Efficiently Synthesized Using the Boron-Chalcogen Mixture Method
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01260J
_journal_year                    2022
_chemical_formula_moiety         'B La S3'
_chemical_formula_sum            'B La S3'
_chemical_formula_weight         245.90
_chemical_name_systematic        'Lanthanum Orthothioborate'
_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_primary     direct
_audit_creation_date             2022-01-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-25 deposited with the CCDC.	2022-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6766(2)
_cell_length_b                   6.04450(10)
_cell_length_c                   8.9940(2)
_cell_measurement_reflns_used    9730
_cell_measurement_temperature    301.76
_cell_measurement_theta_max      36.29
_cell_measurement_theta_min      2.65
_cell_volume                     417.332(16)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      301.76
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            44332
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.286
_diffrn_reflns_theta_min         4.062
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.504
_exptl_absorpt_correction_T_max  0.2740
_exptl_absorpt_correction_T_min  0.1896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1116 before and 0.0541 after correction.
The Ratio of minimum to maximum transmission is 0.6920.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.914
_exptl_crystal_description       block/shard
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.144(10)
_refine_ls_extinction_coef       0.0091(4)
_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   1.194
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         2007
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0076
_refine_ls_R_factor_gt           0.0076
_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^)+(0.0017P)^2^+0.1265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0177
_refine_ls_wR_factor_ref         0.0177
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2007
_reflns_number_total             2007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01260j2.cif
_cod_data_source_block           lb2055a_os
_cod_database_code               7130256
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.545
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.856(10)
 0.144(10)
;
_shelx_res_checksum              84747
_shelx_hkl_checksum              63609
_olex2_submission_special_instructions 'No special instructions were received'