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_7130259
_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 Nd S3'
_chemical_formula_sum            'B Nd S3'
_chemical_formula_weight         251.23
_chemical_name_systematic        'Neodymium 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             2022-01-25
_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                   7.4818(2)
_cell_length_b                   6.00370(10)
_cell_length_c                   8.8530(2)
_cell_measurement_reflns_used    9768
_cell_measurement_temperature    300.33
_cell_measurement_theta_max      36.31
_cell_measurement_theta_min      4.10
_cell_volume                     397.663(15)
_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      300.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38285
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.310
_diffrn_reflns_theta_min         4.101
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.387
_exptl_absorpt_correction_T_max  0.2740
_exptl_absorpt_correction_T_min  0.1508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1359 before and 0.0556 after correction.
The Ratio of minimum to maximum transmission is 0.5504.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    4.196
_exptl_crystal_description       shard
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.021(9)
_refine_ls_extinction_coef       0.0149(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   1.146
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         1916
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0081
_refine_ls_R_factor_gt           0.0080
_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^)+(0.0054P)^2^+0.0437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0178
_refine_ls_wR_factor_ref         0.0178
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                1910
_reflns_number_total             1916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01260j2.cif
_cod_data_source_block           lb2047a_os_pna21
_cod_database_code               7130259
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.479
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.979(9)
 0.021(9)
;
_shelx_res_checksum              8977
_shelx_hkl_checksum              33204
_olex2_submission_special_instructions 'No special instructions were received'