# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_PbBSiO
_database_code_depnum_ccdc_archive 'CCDC 2089766'
loop_
_audit_author_name
_audit_author_address
'Kwang-Hwa Lii'
;National Central University
Taiwan
;
_audit_update_record             
;
2021-06-14 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B2 O25 Pb6 Si8'
_chemical_formula_weight         1889.48

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   9.5090(2)
_cell_length_b                   9.5090(2)
_cell_length_c                   42.3552(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3316.70(15)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9910
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      28.29

_exptl_crystal_description       lamellar
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    5.676
_exptl_crystal_F_000             4884
_exptl_transmission_factor_min   0.0215
_exptl_transmission_factor_max   0.2812
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.039
_exptl_absorpt_coefficient_mu    46.077
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   'Numerical Mu Calculated'
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  
'Bruker D8 QUEST CMOS PHOTON II four-circle KAPPA'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17373
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_theta_min         2.654
_diffrn_reflns_theta_max         28.292
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             928
_reflns_number_gt                851
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    Diamond
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+44.8389P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.000033(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         928
_refine_ls_number_parameters     66
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0147
_refine_ls_wR_factor_ref         0.0309
_refine_ls_wR_factor_gt          0.0301
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.44746(2) 0.33222(2) 0.47002(2) 0.01458(7) Uani 1 1 d . . . . .
B1 B 0.333333 0.666667 0.46561(13) 0.0128(17) Uani 0.817(13) 3 d S T P A 1
Si1 Si 0.333333 0.666667 0.46561(13) 0.0128(17) Uani 0.183(13) 3 d S T P A 1
Si2 Si 0.64650(13) 0.74143(13) 0.45065(3) 0.0079(4) Uani 0.933(8) 1 d . . P A 2
B2 B 0.64650(13) 0.74143(13) 0.45065(3) 0.0079(4) Uani 0.067(8) 1 d . . P A 2
Si3 Si 0.000000 0.000000 0.43818(5) 0.0077(3) Uani 1 3 d S T P . .
O1 O 0.5021(3) 0.7819(3) 0.45497(7) 0.0125(6) Uani 1 1 d . . . . .
O2 O 0.333333 0.666667 0.50211(12) 0.0099(10) Uani 1 3 d S T P . .
O3 O 0.6379(3) 0.6200(3) 0.47779(7) 0.0116(6) Uani 1 1 d . . . . .
O4 O 0.6469(4) 0.666667 0.416667 0.0172(9) Uani 1 2 d S T P . .
O5 O 0.8159(3) 0.9138(3) 0.45281(7) 0.0109(6) Uani 1 1 d . . . . .
O6 O 0.000000 0.000000 0.40068(12) 0.0118(10) Uani 1 3 d S T P . .


_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 O2 2.391(2) 19_666 ?
Pb1 O3 2.433(3) . ?
Pb1 O3 2.474(3) 19_666 ?
Pb1 O6 2.613(3) 10 ?
Pb1 O3 2.745(3) 2_655 ?
Pb1 Pb1 3.6011(3) 2_655 ?
Pb1 Pb1 3.6011(3) 3_665 ?
B1 O1 1.490(3) 2_665 ?
B1 O1 1.490(3) . ?
B1 O1 1.490(3) 3_565 ?
B1 O2 1.546(7) . ?
Si2 O3 1.602(3) . ?
Si2 O4 1.6061(15) . ?
Si2 O1 1.610(3) . ?
Si2 O5 1.627(3) . ?
Si3 O6 1.588(5) . ?
Si3 O5 1.639(3) 3_565 ?
Si3 O5 1.639(3) 1_445 ?
Si3 O5 1.639(3) 2_655 ?

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
O2 Pb1 O3 76.77(7) 19_666 . ?
O2 Pb1 O3 85.62(12) 19_666 19_666 ?
O3 Pb1 O3 78.51(10) . 19_666 ?
O2 Pb1 O6 66.86(14) 19_666 10 ?
O3 Pb1 O6 86.20(7) . 10 ?
O3 Pb1 O6 151.03(11) 19_666 10 ?
O2 Pb1 O3 70.99(6) 19_666 2_655 ?
O3 Pb1 O3 147.73(10) . 2_655 ?
O3 Pb1 O3 99.98(8) 19_666 2_655 ?
O6 Pb1 O3 80.14(6) 10 2_655 ?
O2 Pb1 Pb1 41.14(7) 19_666 2_655 ?
O3 Pb1 Pb1 108.98(7) . 2_655 ?
O3 Pb1 Pb1 116.34(6) 19_666 2_655 ?
O6 Pb1 Pb1 46.44(6) 10 2_655 ?
O3 Pb1 Pb1 42.48(5) 2_655 2_655 ?
O2 Pb1 Pb1 41.14(7) 19_666 3_665 ?
O3 Pb1 Pb1 49.61(7) . 3_665 ?
O3 Pb1 Pb1 106.42(6) 19_666 3_665 ?
O6 Pb1 Pb1 46.44(6) 10 3_665 ?
O3 Pb1 Pb1 101.93(5) 2_655 3_665 ?
Pb1 Pb1 Pb1 60.001(1) 2_655 3_665 ?
O1 B1 O1 111.3(2) 2_665 . ?
O1 B1 O1 111.3(2) 2_665 3_565 ?
O1 B1 O1 111.3(2) . 3_565 ?
O1 B1 O2 107.6(2) 2_665 . ?
O1 B1 O2 107.6(2) . . ?
O1 B1 O2 107.6(2) 3_565 . ?
O3 Si2 O4 109.55(14) . . ?
O3 Si2 O1 110.38(16) . . ?
O4 Si2 O1 113.5(2) . . ?
O3 Si2 O5 110.69(16) . . ?
O4 Si2 O5 106.03(15) . . ?
O1 Si2 O5 106.61(15) . . ?
O6 Si3 O5 112.22(12) . 3_565 ?
O6 Si3 O5 112.22(12) . 1_445 ?
O5 Si3 O5 106.59(13) 3_565 1_445 ?
O6 Si3 O5 112.22(12) . 2_655 ?
O5 Si3 O5 106.59(13) 3_565 2_655 ?
O5 Si3 O5 106.59(13) 1_445 2_655 ?
B1 O2 Pb1 119.58(10) . 20_566 ?
B1 O2 Pb1 119.58(10) . 21_556 ?
Pb1 O2 Pb1 97.73(13) 20_566 21_556 ?
B1 O2 Pb1 119.58(10) . 19_666 ?
Pb1 O2 Pb1 97.73(13) 20_566 19_666 ?
Pb1 O2 Pb1 97.73(13) 21_556 19_666 ?
Si2 O3 Pb1 117.02(15) . . ?
Pb1 O3 Pb1 101.49(10) . 19_666 ?
Si2 O3 Pb1 109.95(14) . 3_665 ?
Pb1 O3 Pb1 87.91(8) . 3_665 ?
Pb1 O3 Pb1 123.21(11) 19_666 3_665 ?
Si2 O4 Si2 154.2(3) 11_565 . ?
Si3 O6 Pb1 127.28(9) . 11_455 ?
Si3 O6 Pb1 127.28(9) . 10_445 ?
Pb1 O6 Pb1 87.12(13) 11_455 10_445 ?
Si3 O6 Pb1 127.28(9) . 12 ?
Pb1 O6 Pb1 87.12(13) 11_455 12 ?
Pb1 O6 Pb1 87.12(13) 10_445 12 ?

_refine_diff_density_max         0.975
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.168

