#------------------------------------------------------------------------------
#$Date: 2022-06-22 00:54:16 +0300 (Wed, 22 Jun 2022) $
#$Revision: 276134 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/02/7130256.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7130256
loop_
_publ_author_name
'Breton, Logan S.'
'Morrison, Gregory'
'Lacroix, Matthew'
'Halasyamani, P. Shiv'
'Zur Loye, Hans-Conrad'
_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       'φ and ω 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 λ/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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0017P)²+0.1265P] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_data_source_file            d2cc01260j2.cif
_cod_data_source_block           lb2055a_os
_cod_database_code               7130256
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.38709(2) 0.07076(2) 0.38468(3) 0.01005(3) Uani 1 1 d . . . . .
S3 S -0.00326(5) -0.09076(6) 0.39805(6) 0.01313(7) Uani 1 1 d . . . . .
S1 S 0.70466(6) 0.13719(7) 0.58949(5) 0.01201(8) Uani 1 1 d . . . . .
S2 S 0.67408(6) 0.16604(7) 0.17572(5) 0.01083(7) Uani 1 1 d . . . . .
B1 B 0.6468(3) 0.4068(3) 0.0564(2) 0.0115(3) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S3 La1 S3 122.891(11) . 4 ?
S3 La1 S3 148.528(14) 4_545 4 ?
S3 La1 S3 88.048(7) 4_545 . ?
S3 La1 S1 83.167(12) 4_545 . ?
S1 La1 S3 119.631(15) 2_654 4 ?
S1 La1 S3 72.929(13) 4_455 . ?
S1 La1 S3 71.529(14) 2_654 . ?
S1 La1 S3 72.575(13) 2_654 4_545 ?
S1 La1 S3 69.369(12) . 4 ?
S1 La1 S3 133.697(16) 4_455 4_545 ?
S1 La1 S3 140.276(15) . . ?
S1 La1 S3 61.023(12) 4_455 4 ?
S1 La1 S1 85.602(14) 4_455 . ?
S1 La1 S1 134.145(8) 4_455 2_654 ?
S1 La1 S1 139.817(10) 2_654 . ?
S1 La1 S2 70.371(15) 4_455 2_655 ?
S1 La1 S2 79.035(11) 4_455 4_455 ?
S1 La1 S2 130.062(12) 4_455 . ?
S2 La1 S3 90.272(13) . 4_545 ?
S2 La1 S3 69.042(12) . 4 ?
S2 La1 S3 117.754(14) 2_655 4 ?
S2 La1 S3 70.443(12) 4_455 . ?
S2 La1 S3 69.325(13) 4_455 4 ?
S2 La1 S3 70.883(13) 2_655 . ?
S2 La1 S3 63.513(14) 2_655 4_545 ?
S2 La1 S3 134.092(14) 4_455 4_545 ?
S2 La1 S3 142.524(15) . . ?
S2 La1 S1 70.531(13) 2_655 . ?
S2 La1 S1 138.376(13) 4_455 . ?
S2 La1 S1 76.396(11) . . ?
S2 La1 S1 72.283(14) . 2_654 ?
S2 La1 S1 62.364(14) 4_455 2_654 ?
S2 La1 S1 121.891(11) 2_655 2_654 ?
S2 La1 S2 139.478(8) . 2_655 ?
S2 La1 S2 136.068(7) 4_455 2_655 ?
S2 La1 S2 84.438(13) . 4_455 ?
La1 S3 La1 148.529(14) 4_445 4_455 ?
La1 S3 La1 86.869(9) . 4_455 ?
La1 S3 La1 124.061(13) 4_445 . ?
B1 S3 La1 83.05(6) 3_545 4_455 ?
B1 S3 La1 81.56(6) 3_545 4_445 ?
B1 S3 La1 127.88(7) 3_545 . ?
La1 S1 La1 94.668(16) 4 . ?
La1 S1 La1 106.659(14) 2_655 . ?
La1 S1 La1 157.05(2) 4 2_655 ?
B1 S1 La1 107.31(6) 3_645 . ?
B1 S1 La1 93.37(6) 3_645 4 ?
B1 S1 La1 88.37(6) 3_645 2_655 ?
La1 S2 La1 110.073(14) . 2_654 ?
La1 S2 La1 153.151(17) 4 2_654 ?
La1 S2 La1 96.490(16) . 4 ?
B1 S2 La1 81.37(6) . 2_654 ?
B1 S2 La1 116.44(6) . . ?
B1 S2 La1 90.48(6) . 4 ?
S3 B1 S1 120.35(10) 3_554 3_654 ?
S3 B1 S2 122.91(11) 3_554 . ?
S2 B1 S1 116.23(11) . 3_654 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 S3 3.1539(4) . ?
La1 S3 3.2561(4) 4 ?
La1 S3 3.0234(4) 4_545 ?
La1 S1 3.0207(6) 2_654 ?
La1 S1 3.0818(5) . ?
La1 S1 2.9104(5) 4_455 ?
La1 S2 3.0201(5) 2_655 ?
La1 S2 2.9558(5) 4_455 ?
La1 S2 2.9526(5) . ?
S3 B1 1.800(2) 3_545 ?
S1 B1 1.8245(19) 3_645 ?
S2 B1 1.8204(19) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
La1 S2 B1 S3 -75.09(13) . . . 3_554 ?
La1 S2 B1 S3 -172.59(11) 4 . . 3_554 ?
La1 S2 B1 S3 33.10(11) 2_654 . . 3_554 ?
La1 S2 B1 S1 113.07(9) . . . 3_654 ?
La1 S2 B1 S1 -138.74(11) 2_654 . . 3_654 ?
La1 S2 B1 S1 15.58(10) 4 . . 3_654 ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.856(10)
2 0.144(10)
