# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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. 
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data_1212_a
_database_code_depnum_ccdc_archive 'CCDC 2302636'
loop_
_audit_author_name
_audit_author_address
'Zhang Ruonan'
;University of Chinese Academy of Sciences
China
;
_audit_update_record             
;
2023-10-22 deposited with the CCDC.	2023-11-28 downloaded from the CCDC.
;
_audit_creation_date             2023-07-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'B4 O9 Pb Te'
_chemical_formula_sum            'B4 O9 Pb Te'
_chemical_formula_weight         522.03
_chemical_melting_point          ?
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.5740(3)
_cell_length_b                   6.7445(3)
_cell_length_c                   9.8903(5)
_cell_angle_alpha                70.105(2)
_cell_angle_beta                 78.877(2)
_cell_angle_gamma                61.726(2)
_cell_volume                     362.89(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4804
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      3.711
_shelx_estimated_absorpt_T_max   0.332
_shelx_estimated_absorpt_T_min   0.091
_exptl_absorpt_coefficient_mu    27.215
_exptl_absorpt_correction_T_max  0.2632
_exptl_absorpt_correction_T_min  0.1494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1424 before and 0.0606 after correction. The Ratio of minimum to maximum transmission is 0.5676. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.778
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.052
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10162
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         2.191
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1577
_reflns_number_total             1639
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.292
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       0.0048(5)
_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   1.112
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1639
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0214
_refine_ls_restrained_S_all      1.112
_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)+(0.0117P)²+1.1222P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0481
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_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
Pb1 Pb 0.65419(3) 0.57440(4) 0.13678(2) 0.01447(10) Uani 1 1 d . . . . .
Te1 Te 0.36065(6) 0.33696(6) 0.47857(4) 0.01378(11) Uani 1 1 d . . . . .
B1 B 0.1441(11) 0.6659(11) 0.2113(7) 0.0135(12) Uani 1 1 d . . . . .
B2 B 0.3426(10) 0.2340(11) 0.2138(7) 0.0125(12) Uani 1 1 d . . . . .
B3 B 0.7634(11) -0.0041(12) 0.1533(7) 0.0131(12) Uani 1 1 d . . . . .
B4 B 0.0815(11) 0.0688(11) 0.1792(7) 0.0116(12) Uani 1 1 d . . . . .
O1 O 0.2315(6) 0.8477(7) 0.1740(5) 0.0144(8) Uani 1 1 d . . . . .
O2 O 0.1099(7) 0.5927(7) 0.3693(5) 0.0152(8) Uani 1 1 d . . . . .
O3 O 0.3176(6) 0.4769(7) 0.1538(5) 0.0120(8) Uani 1 1 d . . . . .
O4 O 0.3903(7) 0.1392(7) 0.3677(5) 0.0170(9) Uani 1 1 d . . . . .
O5 O 0.1296(6) 0.2376(7) 0.1859(5) 0.0140(8) Uani 1 1 d . . . . .
O6 O -0.1545(6) 0.1416(7) 0.1708(5) 0.0149(8) Uani 1 1 d . . . . .
O7 O 0.5348(6) 0.0769(7) 0.1375(5) 0.0150(8) Uani 1 1 d . . . . .
O8 O 0.9145(6) -0.2257(7) 0.1510(5) 0.0145(8) Uani 1 1 d . . . . .
O9 O 0.6014(7) 0.4148(8) 0.3842(5) 0.0174(9) Uani 1 1 d . . . . .


_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
Pb1 O1 2.544(4) . ?
Pb1 O3 2.971(4) 2_665 ?
Pb1 O3 2.553(4) . ?
Pb1 O5 2.876(4) 1_655 ?
Pb1 O6 2.497(4) 1_655 ?
Pb1 O7 3.098(4) 1_565 ?
Pb1 O7 2.937(4) 2_665 ?
Pb1 O8 2.678(4) 1_565 ?
Pb1 O9 2.346(4) . ?
Te1 O2 1.894(4) . ?
Te1 O4 1.919(4) . ?
Te1 O4 2.822(4) 2_656 ?
Te1 O9 2.604(4) 2_666 ?
Te1 O9 1.880(4) . ?
B1 O1 1.499(7) . ?
B1 O2 1.476(8) . ?
B1 O3 1.454(8) . ?
B1 O8 1.474(7) 1_465 ?
B2 O3 1.478(7) . ?
B2 O4 1.468(8) . ?
B2 O5 1.466(7) . ?
B2 O7 1.482(8) . ?
B3 O6 1.393(7) 1_655 ?
B3 O7 1.355(7) . ?
B3 O8 1.352(8) . ?
B4 O1 1.356(7) 1_545 ?
B4 O5 1.341(7) . ?
B4 O6 1.399(7) . ?

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 Pb1 O3 55.17(12) . . ?
O1 Pb1 O3 104.45(12) . 2_665 ?
O1 Pb1 O5 162.91(13) . 1_655 ?
O1 Pb1 O7 62.38(11) . 1_565 ?
O1 Pb1 O7 69.90(12) . 2_665 ?
O1 Pb1 O8 108.81(12) . 1_565 ?
O3 Pb1 O3 78.64(13) . 2_665 ?
O3 Pb1 O5 125.62(11) . 1_655 ?
O3 Pb1 O7 114.34(11) 2_665 1_565 ?
O3 Pb1 O7 117.36(11) . 1_565 ?
O3 Pb1 O7 85.98(12) . 2_665 ?
O3 Pb1 O8 163.46(12) . 1_565 ?
O5 Pb1 O3 91.96(11) 1_655 2_665 ?
O5 Pb1 O7 115.26(10) 1_655 1_565 ?
O5 Pb1 O7 126.21(12) 1_655 2_665 ?
O6 Pb1 O1 129.69(12) 1_655 . ?
O6 Pb1 O3 76.23(12) 1_655 . ?
O6 Pb1 O3 74.81(13) 1_655 2_665 ?
O6 Pb1 O5 49.87(11) 1_655 1_655 ?
O6 Pb1 O7 123.04(12) 1_655 2_665 ?
O6 Pb1 O7 164.20(11) 1_655 1_565 ?
O6 Pb1 O8 118.00(12) 1_655 1_565 ?
O7 Pb1 O3 48.56(11) 2_665 2_665 ?
O7 Pb1 O7 68.44(13) 2_665 1_565 ?
O8 Pb1 O3 112.11(12) 1_565 2_665 ?
O8 Pb1 O5 68.15(11) 1_565 1_655 ?
O8 Pb1 O7 47.37(11) 1_565 1_565 ?
O8 Pb1 O7 92.08(12) 1_565 2_665 ?
O9 Pb1 O1 79.78(14) . . ?
O9 Pb1 O3 75.88(13) . . ?
O9 Pb1 O3 145.15(12) . 2_665 ?
O9 Pb1 O5 84.03(13) . 1_655 ?
O9 Pb1 O6 76.31(15) . 1_655 ?
O9 Pb1 O7 149.67(13) . 2_665 ?
O9 Pb1 O7 98.44(13) . 1_565 ?
O9 Pb1 O8 98.47(13) . 1_565 ?
O2 Te1 O4 153.64(15) . 2_656 ?
O2 Te1 O4 91.28(17) . . ?
O2 Te1 O9 94.61(15) . 2_666 ?
O4 Te1 O4 70.32(17) . 2_656 ?
O4 Te1 O9 169.66(16) . 2_666 ?
O9 Te1 O2 99.46(18) . . ?
O9 Te1 O4 97.34(18) . . ?
O9 Te1 O4 101.45(16) . 2_656 ?
O9 Te1 O4 106.63(12) 2_666 2_656 ?
O9 Te1 O9 73.33(18) . 2_666 ?
O2 B1 O1 107.7(5) . . ?
O3 B1 O1 106.1(5) . . ?
O3 B1 O2 113.6(5) . . ?
O3 B1 O8 113.5(5) . 1_465 ?
O8 B1 O1 109.2(5) 1_465 . ?
O8 B1 O2 106.5(5) 1_465 . ?
O3 B2 O7 110.3(5) . . ?
O4 B2 O3 112.0(5) . . ?
O4 B2 O7 108.1(5) . . ?
O5 B2 O3 107.3(4) . . ?
O5 B2 O4 111.9(5) . . ?
O5 B2 O7 107.1(4) . . ?
O7 B3 O6 120.1(5) . 1_655 ?
O8 B3 O6 119.3(5) . 1_655 ?
O8 B3 O7 120.6(5) . . ?
O1 B4 O6 118.3(5) 1_545 . ?
O5 B4 O1 128.2(5) . 1_545 ?
O5 B4 O6 113.4(5) . . ?
B1 O1 Pb1 96.4(3) . . ?
B4 O1 Pb1 144.4(3) 1_565 . ?
B4 O1 B1 119.0(4) 1_565 . ?
B1 O2 Te1 118.2(3) . . ?
B1 O3 Pb1 97.2(3) . . ?
B1 O3 B2 121.6(5) . . ?
B2 O3 Pb1 122.1(3) . . ?
B2 O4 Te1 121.5(3) . . ?
B2 O5 Pb1 137.4(3) . 1_455 ?
B4 O5 Pb1 90.2(3) . 1_455 ?
B4 O5 B2 132.4(5) . . ?
B3 O6 Pb1 130.8(3) 1_455 1_455 ?
B3 O6 B4 121.8(5) 1_455 . ?
B4 O6 Pb1 105.9(3) . 1_455 ?
B3 O7 B2 126.1(5) . . ?
B1 O8 Pb1 129.8(3) 1_645 1_545 ?
B3 O8 Pb1 105.3(3) . 1_545 ?
B3 O8 B1 119.3(5) . 1_645 ?
Te1 O9 Pb1 127.81(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
O1 B1 O2 Te1 -90.1(5) . . . . ?
O1 B1 O3 Pb1 20.9(4) . . . . ?
O1 B1 O3 B2 155.9(4) . . . . ?
O1 B4 O5 Pb1 170.3(6) 1_545 . . 1_455 ?
O1 B4 O5 B2 -12.0(11) 1_545 . . . ?
O1 B4 O6 Pb1 -169.3(4) 1_545 . . 1_455 ?
O1 B4 O6 B3 -1.9(9) 1_545 . . 1_455 ?
O2 Te1 O9 Pb1 -38.9(3) . . . . ?
O2 B1 O1 Pb1 101.0(4) . . . . ?
O2 B1 O1 B4 -75.5(6) . . . 1_565 ?
O2 B1 O3 Pb1 -97.2(4) . . . . ?
O2 B1 O3 B2 37.8(7) . . . . ?
O3 B1 O1 Pb1 -20.9(4) . . . . ?
O3 B1 O1 B4 162.6(5) . . . 1_565 ?
O3 B1 O2 Te1 27.1(6) . . . . ?
O3 B2 O4 Te1 11.2(6) . . . . ?
O3 B2 O5 Pb1 -24.8(7) . . . 1_455 ?
O3 B2 O5 B4 158.6(6) . . . . ?
O3 B2 O7 B3 74.6(7) . . . . ?
O4 Te1 O2 B1 -54.5(4) . . . . ?
O4 Te1 O2 B1 -99.0(5) 2_656 . . . ?
O4 Te1 O9 Pb1 53.7(3) . . . . ?
O4 Te1 O9 Pb1 125.0(2) 2_656 . . . ?
O4 B2 O3 Pb1 65.7(6) . . . . ?
O4 B2 O3 B1 -58.4(6) . . . . ?
O4 B2 O5 Pb1 98.5(5) . . . 1_455 ?
O4 B2 O5 B4 -78.1(8) . . . . ?
O4 B2 O7 B3 -48.3(7) . . . . ?
O5 B2 O3 Pb1 -171.1(3) . . . . ?
O5 B2 O3 B1 64.8(6) . . . . ?
O5 B2 O4 Te1 -109.3(4) . . . . ?
O5 B2 O7 B3 -169.0(5) . . . . ?
O5 B4 O6 Pb1 8.2(6) . . . 1_455 ?
O5 B4 O6 B3 175.6(5) . . . 1_455 ?
O6 B3 O7 B2 -38.2(9) 1_655 . . . ?
O6 B3 O8 Pb1 175.5(4) 1_655 . . 1_545 ?
O6 B3 O8 B1 19.2(9) 1_655 . . 1_645 ?
O6 B4 O5 Pb1 -6.8(5) . . . 1_455 ?
O6 B4 O5 B2 170.9(5) . . . . ?
O7 B2 O3 Pb1 -54.7(6) . . . . ?
O7 B2 O3 B1 -178.8(4) . . . . ?
O7 B2 O4 Te1 133.0(4) . . . . ?
O7 B2 O5 Pb1 -143.2(4) . . . 1_455 ?
O7 B2 O5 B4 40.1(8) . . . . ?
O7 B3 O8 Pb1 -5.0(7) . . . 1_545 ?
O7 B3 O8 B1 -161.3(5) . . . 1_645 ?
O8 B1 O1 Pb1 -143.7(4) 1_465 . . . ?
O8 B1 O1 B4 39.8(7) 1_465 . . 1_565 ?
O8 B1 O2 Te1 152.9(3) 1_465 . . . ?
O8 B1 O3 Pb1 140.9(4) 1_465 . . . ?
O8 B1 O3 B2 -84.2(6) 1_465 . . . ?
O8 B3 O7 B2 142.3(6) . . . . ?
O9 Te1 O2 B1 43.2(4) . . . . ?
O9 Te1 O2 B1 117.0(4) 2_666 . . . ?
O9 Te1 O9 Pb1 -130.9(3) 2_666 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
