# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_11111
_database_code_depnum_ccdc_archive 'CCDC 2123526'
loop_
_audit_author_name
_audit_author_address
JB
;Xinjiang Technical Institute of Physics and Chemistry
China
;
_audit_update_record             
;
2021-11-22 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_audit_creation_date             2021-08-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(Al8 B12 F12 O32 Pb8)'
_chemical_formula_sum            'Al2 B3 F3 O8 Pb2'
_chemical_formula_weight         685.77
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_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      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   9.8591(4)
_cell_length_b                   8.6238(4)
_cell_length_c                   9.3131(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     791.83(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2592
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      4.13
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    42.783
_exptl_absorpt_correction_T_max  0.4692
_exptl_absorpt_correction_T_min  0.2308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1558 before and 0.0663 after correction. The Ratio of minimum to maximum transmission is 0.4919. 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    5.753
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0344
_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       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7001
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         3.138
_diffrn_ambient_temperature      296.0
_diffrn_detector_area_resol_mean ?
_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       '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                789
_reflns_number_total             912
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.445
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.247
_refine_ls_extinction_coef       0.00044(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         912
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0197
_refine_ls_restrained_S_all      1.020
_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)+(0.0054P)²+2.2713P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0408
_refine_ls_wR_factor_ref         0.0429
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(F1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(B2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     iterative
_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 0.20836(2) 0.51194(2) 0.64560(2) 0.01014(10) Uani 1 1 d . . . A 4
Al1 Al 0.52521(17) 0.6491(2) 0.56593(18) 0.0065(3) Uani 1 1 d . . . . .
F1 F 0.5612(4) 0.8470(4) 0.5168(3) 0.0124(7) Uani 1 1 d . U . . .
F2 F 0.500000 0.7182(5) 0.750000 0.0083(9) Uani 1 2 d S T P . .
O1 O 0.3411(4) 0.6993(5) 0.5297(4) 0.0088(8) Uani 1 1 d . . . . .
O2 O 0.4661(4) 0.4482(5) 0.6212(4) 0.0064(8) Uani 1 1 d . . . . .
O3 O 0.7095(4) 0.6173(5) 0.6027(4) 0.0090(8) Uani 1 1 d . . . . .
O4 O 0.3791(4) 0.2541(5) 0.7787(4) 0.0096(8) Uani 1 1 d . . . . .
B2 B 0.500000 0.3556(10) 0.750000 0.0030(16) Uani 1 2 d S TU P A .
B1 B 0.8083(7) 0.7286(8) 0.5961(6) 0.0080(13) 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 F1 2.423(3) 4_466 ?
Pb1 O1 2.343(4) . ?
Pb1 O2 2.610(4) . ?
Pb1 O3 2.642(4) 3_656 ?
Pb1 O3 2.692(4) 5_666 ?
Pb1 O4 2.577(4) 8_665 ?
Al1 Al1 2.893(3) 5_666 ?
Al1 F1 1.802(4) . ?
Al1 F2 1.832(2) . ?
Al1 O1 1.896(4) . ?
Al1 O2 1.936(4) 5_666 ?
Al1 O2 1.899(4) . ?
Al1 O3 1.869(4) . ?
O1 B1 1.366(7) 4_466 ?
O2 B2 1.479(6) . ?
O3 B1 1.369(8) . ?
O4 B2 1.503(6) . ?
O4 B1 1.377(7) 6_557 ?

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
F1 Pb1 O2 129.36(12) 4_466 . ?
F1 Pb1 O3 124.39(12) 4_466 3_656 ?
F1 Pb1 O3 81.48(12) 4_466 5_666 ?
F1 Pb1 O4 72.13(11) 4_466 8_665 ?
O1 Pb1 F1 72.59(13) . 4_466 ?
O1 Pb1 O2 63.97(13) . . ?
O1 Pb1 O3 90.01(13) . 3_656 ?
O1 Pb1 O3 73.85(13) . 5_666 ?
O1 Pb1 O4 81.35(13) . 8_665 ?
O2 Pb1 O3 81.45(12) . 3_656 ?
O2 Pb1 O3 62.93(11) . 5_666 ?
O3 Pb1 O3 144.36(17) 3_656 5_666 ?
O4 Pb1 O2 122.57(13) 8_665 . ?
O4 Pb1 O3 148.15(12) 8_665 5_666 ?
O4 Pb1 O3 52.90(12) 8_665 3_656 ?
F1 Al1 Al1 140.17(15) . 5_666 ?
F1 Al1 F2 87.48(19) . . ?
F1 Al1 O1 85.84(18) . . ?
F1 Al1 O2 173.3(2) . . ?
F1 Al1 O2 99.97(18) . 5_666 ?
F1 Al1 O3 89.64(19) . . ?
F2 Al1 Al1 131.55(17) . 5_666 ?
F2 Al1 O1 87.83(14) . . ?
F2 Al1 O2 171.6(2) . 5_666 ?
F2 Al1 O2 90.11(18) . . ?
F2 Al1 O3 90.47(13) . . ?
O1 Al1 Al1 87.87(15) . 5_666 ?
O1 Al1 O2 88.92(18) . 5_666 ?
O1 Al1 O2 87.9(2) . . ?
O2 Al1 Al1 40.56(13) 5_666 5_666 ?
O2 Al1 Al1 41.51(11) . 5_666 ?
O2 Al1 O2 82.07(17) . 5_666 ?
O3 Al1 Al1 96.57(16) . 5_666 ?
O3 Al1 O1 175.2(2) . . ?
O3 Al1 O2 93.35(18) . 5_666 ?
O3 Al1 O2 96.6(2) . . ?
Al1 F1 Pb1 138.75(19) . 4_566 ?
Al1 F2 Al1 142.0(3) 3_656 . ?
Al1 O1 Pb1 107.20(19) . . ?
B1 O1 Pb1 125.2(4) 4_466 . ?
B1 O1 Al1 118.9(4) 4_466 . ?
Al1 O2 Pb1 102.28(17) 5_666 . ?
Al1 O2 Pb1 97.47(17) . . ?
Al1 O2 Al1 97.93(17) . 5_666 ?
B2 O2 Pb1 105.24(19) . . ?
B2 O2 Al1 119.1(4) . 5_666 ?
B2 O2 Al1 130.0(4) . . ?
Al1 O3 Pb1 120.73(18) . 3_656 ?
Al1 O3 Pb1 101.29(15) . 5_666 ?
B1 O3 Pb1 93.6(3) . 3_656 ?
B1 O3 Pb1 92.2(3) . 5_666 ?
B1 O3 Al1 125.5(4) . . ?
B2 O4 Pb1 130.7(3) . 8_655 ?
B1 O4 Pb1 96.2(3) 6_557 8_655 ?
B1 O4 B2 130.2(4) 6_557 . ?
O2 B2 O2 114.7(6) . 3_656 ?
O2 B2 O4 106.2(2) 3_656 3_656 ?
O2 B2 O4 110.4(2) 3_656 . ?
O2 B2 O4 110.5(2) . 3_656 ?
O2 B2 O4 106.2(2) . . ?
O4 B2 O4 108.8(6) . 3_656 ?
O1 B1 O3 121.7(5) 4_566 . ?
O1 B1 O4 122.3(6) 4_566 6_667 ?
O3 B1 O4 115.8(5) . 6_667 ?

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
Pb1 O2 B2 O2 -85.14(17) . . . 3_656 ?
Pb1 O2 B2 O4 37.1(4) . . . . ?
Pb1 O2 B2 O4 154.9(3) . . . 3_656 ?
Pb1 O3 B1 O1 41.1(6) 5_666 . . 4_566 ?
Pb1 O3 B1 O1 163.2(5) 3_656 . . 4_566 ?
Pb1 O3 B1 O4 -133.9(5) 5_666 . . 6_667 ?
Pb1 O3 B1 O4 -11.8(5) 3_656 . . 6_667 ?
Pb1 O4 B2 O2 -161.9(3) 8_655 . . 3_656 ?
Pb1 O4 B2 O2 73.2(6) 8_655 . . . ?
Pb1 O4 B2 O4 -45.7(2) 8_655 . . 3_656 ?
Al1 Al1 F1 Pb1 -46.0(4) 5_666 . . 4_566 ?
Al1 Al1 F2 Al1 17.98(12) 5_666 . . 3_656 ?
Al1 Al1 O1 Pb1 58.23(15) 5_666 . . . ?
Al1 Al1 O1 B1 -91.2(4) 5_666 . . 4_466 ?
Al1 Al1 O2 Pb1 -103.58(19) 5_666 . . . ?
Al1 Al1 O2 B2 139.3(5) 5_666 . . . ?
Al1 Al1 O3 Pb1 43.76(15) 5_666 . . 5_666 ?
Al1 Al1 O3 Pb1 -94.4(2) 5_666 . . 3_656 ?
Al1 Al1 O3 B1 144.7(4) 5_666 . . . ?
Al1 O2 B2 O2 161.0(3) 5_666 . . 3_656 ?
Al1 O2 B2 O2 28.7(2) . . . 3_656 ?
Al1 O2 B2 O4 41.1(5) 5_666 . . 3_656 ?
Al1 O2 B2 O4 -76.7(4) 5_666 . . . ?
Al1 O2 B2 O4 151.0(4) . . . . ?
Al1 O2 B2 O4 -91.2(6) . . . 3_656 ?
Al1 O3 B1 O1 -64.4(7) . . . 4_566 ?
Al1 O3 B1 O4 120.5(5) . . . 6_667 ?
F1 Al1 F2 Al1 -170.86(13) . . . 3_656 ?
F1 Al1 O1 Pb1 -161.12(18) . . . . ?
F1 Al1 O1 B1 49.5(4) . . . 4_466 ?
F1 Al1 O3 Pb1 125.1(2) . . . 3_656 ?
F1 Al1 O3 Pb1 -96.80(16) . . . 5_666 ?
F1 Al1 O3 B1 4.2(4) . . . . ?
F2 Al1 F1 Pb1 144.3(3) . . . 4_566 ?
F2 Al1 O1 Pb1 -73.5(2) . . . . ?
F2 Al1 O1 B1 137.1(5) . . . 4_466 ?
F2 Al1 O2 Pb1 73.45(11) . . . . ?
F2 Al1 O2 Al1 177.03(17) . . . 5_666 ?
F2 Al1 O2 B2 -43.7(4) . . . . ?
F2 Al1 O3 Pb1 37.6(2) . . . 3_656 ?
F2 Al1 O3 Pb1 175.72(18) . . . 5_666 ?
F2 Al1 O3 B1 -83.3(4) . . . . ?
O1 Al1 F1 Pb1 -127.7(3) . . . 4_566 ?
O1 Al1 F2 Al1 103.21(14) . . . 3_656 ?
O1 Al1 O2 Pb1 -14.38(15) . . . . ?
O1 Al1 O2 Al1 89.20(19) . . . 5_666 ?
O1 Al1 O2 B2 -131.5(4) . . . . ?
O2 Al1 F1 Pb1 -39.5(3) 5_666 . . 4_566 ?
O2 Al1 F2 Al1 15.35(13) . . . 3_656 ?
O2 Al1 O1 Pb1 16.69(18) . . . . ?
O2 Al1 O1 Pb1 98.80(19) 5_666 . . . ?
O2 Al1 O1 B1 -50.6(4) 5_666 . . 4_466 ?
O2 Al1 O1 B1 -132.7(4) . . . 4_466 ?
O2 Al1 O2 Pb1 -103.58(19) 5_666 . . . ?
O2 Al1 O2 Al1 0.001(0) 5_666 . . 5_666 ?
O2 Al1 O2 B2 139.3(5) 5_666 . . . ?
O2 Al1 O3 Pb1 3.17(19) 5_666 . . 5_666 ?
O2 Al1 O3 Pb1 -52.6(2) . . . 3_656 ?
O2 Al1 O3 Pb1 85.56(16) . . . 5_666 ?
O2 Al1 O3 Pb1 -135.0(2) 5_666 . . 3_656 ?
O2 Al1 O3 B1 -173.5(4) . . . . ?
O2 Al1 O3 B1 104.1(4) 5_666 . . . ?
O3 Al1 F1 Pb1 53.8(3) . . . 4_566 ?
O3 Al1 F2 Al1 -81.25(14) . . . 3_656 ?
O3 Al1 O2 Pb1 163.93(15) . . . . ?
O3 Al1 O2 Al1 -92.48(19) . . . 5_666 ?
O3 Al1 O2 B2 46.8(4) . . . . ?
B1 O4 B2 O2 -5.8(8) 6_557 . . 3_656 ?
B1 O4 B2 O2 -130.7(5) 6_557 . . . ?
B1 O4 B2 O4 110.4(6) 6_557 . . 3_656 ?

_olex2_submission_special_instructions 'No special instructions were received'
