# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_251
_database_code_depnum_ccdc_archive 'CCDC 2125608'
loop_
_audit_author_name
_audit_author_address
'Dongsheng Yuan'
;National Institute for Materials Science (NIMS)
Japan
;
_audit_update_record             
;
2021-12-01 deposited with the CCDC.	2022-01-23 downloaded from the CCDC.
;
_audit_creation_date             2021-05-27
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        LaB3O6
_chemical_formula_moiety         '0.25(B12 La4 O24)'
_chemical_formula_sum            'B3 La O6'
_chemical_formula_weight         267.34
_chemical_melting_point          ?
_chemical_oxdiff_formula         'La B3 O6'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2yaR'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   6.5475(10)
_cell_length_b                   8.2077(12)
_cell_length_c                   8.0215(11)
_cell_angle_alpha                90
_cell_angle_beta                 93.701(13)
_cell_angle_gamma                90
_cell_volume                     430.18(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1257
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      30.3510
_cell_measurement_theta_min      3.5130
_shelx_estimated_absorpt_T_max   0.638
_shelx_estimated_absorpt_T_min   0.327
_exptl_absorpt_coefficient_mu    9.870
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.128
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1880
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.411
_diffrn_reflns_theta_min         3.555
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     82.00 108.00   0.50    3.00    --   20.00  54.00-150.00   52
  2  ω    -74.00  69.00   0.50    3.00    --   20.00  54.00 -30.00  286
  3  ω     74.00 106.00   0.50    3.00    --   20.00  54.00 -30.00   64
  4  ω    -71.00  29.00   0.50    3.00    --   20.00  54.00 120.00  200
  5  ω     54.00  79.00   0.50    3.00    --   20.00  54.00 120.00   50
  6  ω    -51.00 -25.00   0.50    3.00    --   20.00  54.00-180.00   52
  7  ω     -8.00  91.00   0.50    3.00    --   20.00  54.00-180.00  198
  8  ω    -45.00 -15.00   0.50    3.00    --   20.00  54.00-120.00   60
  9  ω     47.00  72.00   0.50    3.00    --   20.00  54.00-120.00   50
 10  ω    -68.00 -43.00   0.50    3.00    --   20.00  54.00  30.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1070917000
_diffrn_orient_matrix_UB_12      -0.0128562000
_diffrn_orient_matrix_UB_13      0.0117541000
_diffrn_orient_matrix_UB_21      0.0032221000
_diffrn_orient_matrix_UB_22      -0.0219381000
_diffrn_orient_matrix_UB_23      -0.0854280000
_diffrn_orient_matrix_UB_31      0.0175742000
_diffrn_orient_matrix_UB_32      0.0824922000
_diffrn_orient_matrix_UB_33      -0.0207586000
_diffrn_oxdiff_digest_frames     
;
0120d87065dbf5791d67dc0019171dde3000025cb3b
;
_diffrn_oxdiff_digest_hkl        
;
01e356b16e64cbc4a2e26dc74414c47eb5967c
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                605
_reflns_number_total             624
_reflns_odcompleteness_completeness 99.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.129
_refine_diff_density_min         -1.929
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       0.0021(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   1.051
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         624
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0205
_refine_ls_restrained_S_all      1.051
_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/[σ²(Fo²)+(0.0204P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0455
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
La La 0.750000 0.19929(3) 0.500000 0.00681(11) Uani 1 2 d S T P . .
O1 O 0.7059(4) 0.4163(3) 0.7023(3) 0.0122(5) Uani 1 1 d . . . . .
O2 O 0.6095(3) 0.6141(3) 0.8943(3) 0.0091(4) Uani 1 1 d . . . . .
O3 O 0.6114(4) 0.6876(3) 0.6031(3) 0.0094(5) Uani 1 1 d . . . . .
B1 B 0.6463(5) 0.5694(4) 0.7261(4) 0.0076(6) Uani 1 1 d . . . . .
B2 B 0.750000 0.7784(6) 0.500000 0.0070(9) Uani 1 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
La 0.00912(16) 0.00419(16) 0.00723(15) 0.000 0.00137(10) 0.000
O1 0.0200(12) 0.0068(11) 0.0101(10) -0.0002(9) 0.0028(9) 0.0043(9)
O2 0.0110(11) 0.0073(11) 0.0090(9) -0.0026(9) 0.0022(8) -0.0015(9)
O3 0.0090(11) 0.0081(12) 0.0114(11) 0.0034(8) 0.0030(9) 0.0006(8)
B1 0.0063(14) 0.0065(16) 0.0101(14) -0.0006(13) 0.0003(12) -0.0004(12)
B2 0.008(2) 0.004(2) 0.009(2) 0.000 0.0026(18) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
La O1 2.440(2) 2_656 ?
La O1 2.568(2) 8_554 ?
La O1 2.440(2) . ?
La O1 2.568(2) 7_656 ?
La O2 2.842(2) 7_656 ?
La O2 2.647(2) 3_544 ?
La O2 2.842(2) 8_554 ?
La O2 2.647(2) 4_546 ?
La O3 2.625(3) 6_665 ?
La O3 2.625(3) 5_666 ?
La B1 3.156(4) 8_554 ?
La B1 3.156(4) 7_656 ?
O1 B1 1.333(4) . ?
O2 B1 1.433(4) . ?
O2 B2 1.498(4) 7_666 ?
O3 B1 1.392(4) . ?
O3 B2 1.470(3) . ?

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
O1 La O1 86.20(10) 2_656 . ?
O1 La O1 70.26(8) . 7_656 ?
O1 La O1 151.32(7) 2_656 7_656 ?
O1 La O1 70.26(8) 2_656 8_554 ?
O1 La O1 151.32(7) . 8_554 ?
O1 La O1 136.63(10) 8_554 7_656 ?
O1 La O2 69.73(7) 8_554 3_544 ?
O1 La O2 51.21(7) 7_656 7_656 ?
O1 La O2 120.81(7) . 7_656 ?
O1 La O2 144.02(7) . 8_554 ?
O1 La O2 123.51(8) . 3_544 ?
O1 La O2 87.58(7) 7_656 8_554 ?
O1 La O2 120.81(7) 2_656 8_554 ?
O1 La O2 123.51(8) 2_656 4_546 ?
O1 La O2 51.21(7) 8_554 8_554 ?
O1 La O2 80.44(8) . 4_546 ?
O1 La O2 144.02(7) 2_656 7_656 ?
O1 La O2 98.69(7) 8_554 4_546 ?
O1 La O2 87.58(7) 8_554 7_656 ?
O1 La O2 69.73(7) 7_656 4_546 ?
O1 La O2 80.44(8) 2_656 3_544 ?
O1 La O2 98.69(7) 7_656 3_544 ?
O1 La O3 117.95(8) 7_656 5_666 ?
O1 La O3 78.04(8) 7_656 6_665 ?
O1 La O3 78.95(8) . 5_666 ?
O1 La O3 78.95(8) 2_656 6_665 ?
O1 La O3 71.04(8) 2_656 5_666 ?
O1 La O3 71.04(8) . 6_665 ?
O1 La O3 117.95(8) 8_554 6_665 ?
O1 La O3 78.04(8) 8_554 5_666 ?
O1 La B1 24.26(8) 7_656 7_656 ?
O1 La B1 160.75(9) 2_656 7_656 ?
O1 La B1 113.28(8) 8_554 7_656 ?
O1 La B1 94.39(8) 2_656 8_554 ?
O1 La B1 94.39(8) . 7_656 ?
O1 La B1 24.26(8) 8_554 8_554 ?
O1 La B1 113.28(8) 7_656 8_554 ?
O1 La B1 160.75(9) . 8_554 ?
O2 La O2 86.71(5) 4_546 7_656 ?
O2 La O2 65.11(8) 4_546 8_554 ?
O2 La O2 149.35(10) 4_546 3_544 ?
O2 La O2 65.11(8) 3_544 7_656 ?
O2 La O2 86.71(5) 3_544 8_554 ?
O2 La O2 50.39(9) 8_554 7_656 ?
O2 La B1 83.25(8) 4_546 8_554 ?
O2 La B1 75.41(8) 4_546 7_656 ?
O2 La B1 68.05(8) 8_554 7_656 ?
O2 La B1 75.41(8) 3_544 8_554 ?
O2 La B1 83.25(8) 3_544 7_656 ?
O2 La B1 27.00(8) 8_554 8_554 ?
O2 La B1 27.00(8) 7_656 7_656 ?
O2 La B1 68.05(8) 7_656 8_554 ?
O3 La O2 132.98(7) 5_666 7_656 ?
O3 La O2 52.58(7) 5_666 4_546 ?
O3 La O2 142.61(7) 5_666 3_544 ?
O3 La O2 87.61(7) 5_666 8_554 ?
O3 La O2 142.61(7) 6_665 4_546 ?
O3 La O2 52.58(7) 6_665 3_544 ?
O3 La O2 132.98(7) 6_665 8_554 ?
O3 La O2 87.61(7) 6_665 7_656 ?
O3 La O3 138.57(10) 6_665 5_666 ?
O3 La B1 83.04(8) 5_666 8_554 ?
O3 La B1 127.99(8) 6_665 8_554 ?
O3 La B1 127.99(8) 5_666 7_656 ?
O3 La B1 83.04(8) 6_665 7_656 ?
B1 La B1 91.33(13) 8_554 7_656 ?
La O1 La 109.74(8) . 7_656 ?
B1 O1 La 103.40(19) . 7_656 ?
B1 O1 La 146.3(2) . . ?
La O2 La 114.89(8) 3_455 7_656 ?
B1 O2 La 88.78(18) . 7_656 ?
B1 O2 La 125.2(2) . 3_455 ?
B1 O2 B2 123.3(2) . 7_666 ?
B2 O2 La 100.91(13) 7_666 3_455 ?
B2 O2 La 100.91(19) 7_666 7_656 ?
B1 O3 La 125.0(2) . 5_666 ?
B1 O3 B2 132.3(3) . . ?
B2 O3 La 102.71(15) . 5_666 ?
O1 B1 La 52.33(15) . 7_656 ?
O1 B1 O2 116.4(3) . . ?
O1 B1 O3 126.3(3) . . ?
O2 B1 La 64.21(16) . 7_656 ?
O3 B1 La 177.0(2) . 7_656 ?
O3 B1 O2 117.3(3) . . ?
O2 B2 O2 107.8(4) 7_666 8_564 ?
O3 B2 O2 111.06(13) . 7_666 ?
O3 B2 O2 103.79(13) . 8_564 ?
O3 B2 O2 111.06(13) 2_656 8_564 ?
O3 B2 O2 103.79(13) 2_656 7_666 ?
O3 B2 O3 119.1(4) . 2_656 ?

_shelx_res_file                  
;
TITL exp_251_a.res in I2/a
    exp_251.res
    created by SHELXL-2018/3 at 18:16:19 on 27-May-2021
REM Old TITL exp_251 in Ia
REM SHELXT solution in I2/a: R1 0.030, Rweak 0.006, Alpha 0.030
REM <I/s> 1.205 for 32 systematic absences, Orientation as input
REM Formula found by SHELXT: B3 O6 La
CELL 0.71073 6.5475 8.2077 8.0215 90 93.701 90
ZERR 4 0.001 0.0012 0.0011 0 0.013 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC B La O
UNIT 12 4 24

L.S. 50
PLAN  5
SIZE 0.05 0.097 0.146
TEMP 23
list 4
fmap 2 53
acta
OMIT 2 1 1
OMIT 2 5 9
OMIT 6 7 3
OMIT 0 4 0
OMIT 5 6 1
REM <olex2.extras>
REM <HklSrc "%.\\exp_251.hkl">
REM </olex2.extras>

WGHT    0.020400
EXTI    0.002111
FVAR       0.44516
LA    2    0.750000    0.199290    0.500000    10.50000    0.00912    0.00419 =
         0.00723    0.00000    0.00137    0.00000
O1    3    0.705868    0.416322    0.702349    11.00000    0.01998    0.00683 =
         0.01015   -0.00018    0.00280    0.00433
O2    3    0.609509    0.614066    0.894297    11.00000    0.01103    0.00731 =
         0.00905   -0.00257    0.00216   -0.00153
O3    3    0.611360    0.687566    0.603112    11.00000    0.00902    0.00815 =
         0.01143    0.00337    0.00298    0.00060
B1    1    0.646303    0.569442    0.726101    11.00000    0.00628    0.00650 =
         0.01011   -0.00057    0.00033   -0.00044
B2    1    0.750000    0.778387    0.500000    10.50000    0.00787    0.00430 =
         0.00904    0.00000    0.00264    0.00000
HKLF 4




REM  exp_251_a.res in I2/a
REM wR2 = 0.0455, GooF = S = 1.051, Restrained GooF = 1.051 for all data
REM R1 = 0.0205 for 605 Fo > 4sig(Fo) and 0.0211 for all 624 data
REM 48 parameters refined using 0 restraints

END

WGHT      0.0204      0.0000

REM Highest difference peak  1.129,  deepest hole -1.929,  1-sigma level  0.214
Q1    1   0.7660  0.1987  0.3757  11.00000  0.05    1.13
Q2    1   0.6199  0.1383  0.5141  11.00000  0.05    0.86
Q3    1   0.6262  0.2581  0.5028  11.00000  0.05    0.76
Q4    1   0.7680  0.3028  0.4165  11.00000  0.05    0.74
Q5    1   0.8171  0.3920  0.8197  11.00000  0.05    0.72
;
_shelx_res_checksum              10590
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.685
_oxdiff_exptl_absorpt_empirical_full_min 0.803
_exptl_crystal_recrystallization_method 'Single crystal growth'
_exptl_crystal_preparation       Luminescent
