# 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_01a
_database_code_depnum_ccdc_archive 'CCDC 2043215'
loop_
_audit_author_name
_audit_author_address
'Ce Tao'
;university of chinese academy of science
China
;
_audit_update_record             
;
2020-11-09 deposited with the CCDC.	2021-09-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-24
_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         '0.5(O24 Pb6 Si6 Tb4)'
_chemical_formula_sum            'O12 Pb3 Si3 Tb2'
_chemical_formula_weight         1215.66
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Tb Tb -0.1723 4.1537 '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      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'

_cell_length_a                   9.6395(2)
_cell_length_b                   9.6395(2)
_cell_length_c                   6.8787(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     553.54(3)
_cell_formula_units_Z            2.00004
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    58.468
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    7.294
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             1028
_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  0.0667
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5914
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.068
_diffrn_reflns_theta_min         2.440
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                494
_reflns_number_total             522
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.797
_refine_diff_density_min         -4.084
_refine_diff_density_rms         0.624
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         522
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0442
_refine_ls_restrained_S_all      1.136
_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)+(0.0653P)²+27.4284P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1221
_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
Pb01 Pb -0.00574(9) 0.75377(9) 0.750000 0.0206(3) Uani 1 2 d S T P . .
Tb02 Tb 0.333333 0.666667 0.50381(13) 0.0095(3) Uani 1 3 d S T P . .
Si Si 0.4139(6) 1.0302(6) 0.750000 0.0101(9) Uani 1 2 d S T P . .
O3 O 0.3533(18) 0.8400(16) 0.750000 0.017(3) Uani 1 2 d S T P . .
O1 O 0.6080(15) 1.1385(15) 0.750000 0.019(3) Uani 1 2 d S T P . .
O2 O 0.3635(17) 1.0953(14) 0.942(2) 0.035(3) 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
Pb01 Si 3.162(5) 3_465 ?
Pb01 Si 3.764(2) 8_456 ?
Pb01 Si 3.764(2) 8_457 ?
Pb01 Si 3.455(5) 2_665 ?
Pb01 Si 3.562(5) . ?
Pb01 O1 2.375(13) 2_665 ?
Pb01 O2 2.384(12) 5_454 ?
Pb01 O2 2.562(14) 3_465 ?
Pb01 O2 2.384(12) 8_457 ?
Pb01 O2 2.562(14) 12_467 ?
Tb02 Si 3.225(4) 9_656 ?
Tb02 Si 3.225(4) 7_676 ?
Tb02 Si 3.225(4) 8_456 ?
Tb02 O3 2.319(9) 2_665 ?
Tb02 O3 2.319(9) . ?
Tb02 O3 2.319(9) 3_565 ?
Tb02 O1 2.415(9) 9_656 ?
Tb02 O1 2.415(9) 8_456 ?
Tb02 O1 2.415(9) 7_676 ?
Tb02 O2 2.698(14) 5_454 ?
Tb02 O2 2.698(14) 6_654 ?
Tb02 O2 2.698(14) 4_674 ?
Si O3 1.622(14) . ?
Si O1 1.624(14) . ?
Si O2 1.638(12) . ?
Si O2 1.638(12) 10_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
Si Pb01 Si 90.32(16) 3_465 2_665 ?
Si Pb01 Si 89.62(5) . 8_457 ?
Si Pb01 Si 96.05(5) 3_465 8_457 ?
Si Pb01 Si 165.89(11) 3_465 . ?
Si Pb01 Si 89.62(5) . 8_456 ?
Si Pb01 Si 103.78(15) 2_665 . ?
Si Pb01 Si 66.88(7) 2_665 8_457 ?
Si Pb01 Si 96.05(5) 3_465 8_456 ?
Si Pb01 Si 132.08(14) 8_456 8_457 ?
Si Pb01 Si 66.88(7) 2_665 8_456 ?
O1 Pb01 Si 128.2(3) 2_665 . ?
O1 Pb01 Si 65.9(3) 2_665 3_465 ?
O1 Pb01 Si 71.65(11) 2_665 8_457 ?
O1 Pb01 Si 71.65(11) 2_665 8_456 ?
O1 Pb01 Si 24.4(3) 2_665 2_665 ?
O1 Pb01 O2 84.6(3) 2_665 5_454 ?
O1 Pb01 O2 69.4(4) 2_665 3_465 ?
O1 Pb01 O2 69.4(4) 2_665 12_467 ?
O1 Pb01 O2 84.6(3) 2_665 8_457 ?
O2 Pb01 Si 74.3(4) 8_457 2_665 ?
O2 Pb01 Si 146.3(3) 3_465 . ?
O2 Pb01 Si 131.8(4) 5_454 8_457 ?
O2 Pb01 Si 72.8(3) 8_457 . ?
O2 Pb01 Si 90.1(3) 3_465 2_665 ?
O2 Pb01 Si 74.3(4) 5_454 2_665 ?
O2 Pb01 Si 67.5(3) 3_465 8_457 ?
O2 Pb01 Si 131.8(4) 8_457 8_456 ?
O2 Pb01 Si 111.8(3) 8_457 3_465 ?
O2 Pb01 Si 31.1(3) 3_465 3_465 ?
O2 Pb01 Si 16.9(3) 8_457 8_457 ?
O2 Pb01 Si 67.5(3) 12_467 8_456 ?
O2 Pb01 Si 124.1(3) 12_467 8_457 ?
O2 Pb01 Si 31.1(3) 12_467 3_465 ?
O2 Pb01 Si 111.8(3) 5_454 3_465 ?
O2 Pb01 Si 146.3(3) 12_467 . ?
O2 Pb01 Si 90.1(3) 12_467 2_665 ?
O2 Pb01 Si 124.1(3) 3_465 8_456 ?
O2 Pb01 Si 16.9(3) 5_454 8_456 ?
O2 Pb01 Si 72.8(3) 5_454 . ?
O2 Pb01 O2 125.3(7) 8_457 5_454 ?
O2 Pb01 O2 140.9(5) 8_457 12_467 ?
O2 Pb01 O2 81.94(19) 5_454 12_467 ?
O2 Pb01 O2 81.94(19) 8_457 3_465 ?
O2 Pb01 O2 140.9(5) 5_454 3_465 ?
O2 Pb01 O2 62.1(6) 12_467 3_465 ?
Si Tb02 Si 93.46(7) 7_676 9_656 ?
Si Tb02 Si 93.46(7) 8_456 7_676 ?
Si Tb02 Si 93.46(7) 8_456 9_656 ?
O3 Tb02 Si 89.4(3) 3_565 9_656 ?
O3 Tb02 Si 161.8(3) 2_665 7_676 ?
O3 Tb02 Si 161.8(3) . 9_656 ?
O3 Tb02 Si 89.4(3) 2_665 8_456 ?
O3 Tb02 Si 104.3(3) 3_565 7_676 ?
O3 Tb02 Si 161.8(3) 3_565 8_456 ?
O3 Tb02 Si 104.3(3) 2_665 9_656 ?
O3 Tb02 Si 89.4(3) . 7_676 ?
O3 Tb02 Si 104.3(3) . 8_456 ?
O3 Tb02 O3 72.5(4) 2_665 3_565 ?
O3 Tb02 O3 72.5(4) . 2_665 ?
O3 Tb02 O3 72.5(4) . 3_565 ?
O3 Tb02 O1 146.9(5) 3_565 8_456 ?
O3 Tb02 O1 133.0(4) 3_565 7_676 ?
O3 Tb02 O1 133.0(4) 2_665 9_656 ?
O3 Tb02 O1 146.9(5) . 9_656 ?
O3 Tb02 O1 133.0(4) . 8_456 ?
O3 Tb02 O1 93.7(3) 3_565 9_656 ?
O3 Tb02 O1 93.7(3) 2_665 8_456 ?
O3 Tb02 O1 146.9(5) 2_665 7_676 ?
O3 Tb02 O1 93.7(3) . 7_676 ?
O3 Tb02 O2 141.8(4) . 6_654 ?
O3 Tb02 O2 141.8(4) 3_565 5_454 ?
O3 Tb02 O2 141.8(4) 2_665 4_674 ?
O3 Tb02 O2 73.8(4) 2_665 6_654 ?
O3 Tb02 O2 80.7(5) . 4_674 ?
O3 Tb02 O2 80.7(5) 3_565 6_654 ?
O3 Tb02 O2 73.8(4) 3_565 4_674 ?
O3 Tb02 O2 80.7(5) 2_665 5_454 ?
O3 Tb02 O2 73.8(4) . 5_454 ?
O1 Tb02 Si 64.4(3) 7_676 8_456 ?
O1 Tb02 Si 64.4(3) 9_656 7_676 ?
O1 Tb02 Si 64.4(3) 8_456 9_656 ?
O1 Tb02 Si 29.2(3) 8_456 8_456 ?
O1 Tb02 Si 97.5(2) 7_676 9_656 ?
O1 Tb02 Si 97.5(2) 9_656 8_456 ?
O1 Tb02 Si 29.2(3) 9_656 9_656 ?
O1 Tb02 Si 29.2(3) 7_676 7_676 ?
O1 Tb02 Si 97.5(2) 8_456 7_676 ?
O1 Tb02 O1 73.5(3) 7_676 8_456 ?
O1 Tb02 O1 73.5(3) 7_676 9_656 ?
O1 Tb02 O1 73.5(3) 8_456 9_656 ?
O1 Tb02 O2 59.5(4) 7_676 4_674 ?
O1 Tb02 O2 124.5(4) 8_456 4_674 ?
O1 Tb02 O2 66.5(4) 7_676 5_454 ?
O1 Tb02 O2 66.5(4) 9_656 4_674 ?
O1 Tb02 O2 59.5(4) 8_456 5_454 ?
O1 Tb02 O2 59.5(4) 9_656 6_654 ?
O1 Tb02 O2 124.5(3) 7_676 6_654 ?
O1 Tb02 O2 66.5(4) 8_456 6_654 ?
O1 Tb02 O2 124.5(3) 9_656 5_454 ?
O2 Tb02 Si 92.8(3) 6_654 8_456 ?
O2 Tb02 Si 123.9(3) 6_654 7_676 ?
O2 Tb02 Si 92.8(3) 5_454 7_676 ?
O2 Tb02 Si 30.5(3) 5_454 8_456 ?
O2 Tb02 Si 30.5(3) 6_654 9_656 ?
O2 Tb02 Si 123.9(3) 4_674 8_456 ?
O2 Tb02 Si 30.5(3) 4_674 7_676 ?
O2 Tb02 Si 123.9(3) 5_454 9_656 ?
O2 Tb02 Si 92.8(3) 4_674 9_656 ?
O2 Tb02 O2 117.57(15) 5_454 4_674 ?
O2 Tb02 O2 117.57(15) 4_674 6_654 ?
O2 Tb02 O2 117.57(15) 5_454 6_654 ?
O3 Si O1 112.0(7) . . ?
O3 Si O2 115.1(5) . . ?
O3 Si O2 115.1(5) . 10_557 ?
O1 Si O2 102.8(6) . 10_557 ?
O1 Si O2 102.8(6) . . ?
O2 Si O2 107.6(10) 10_557 . ?
Tb02 O3 Tb02 93.8(5) 10_557 . ?
Si O3 Tb02 131.9(3) . . ?
Si O3 Tb02 131.9(3) . 10_557 ?
Pb01 O1 Tb02 116.8(4) 3_565 4_675 ?
Pb01 O1 Tb02 116.8(4) 3_565 7_676 ?
Tb02 O1 Tb02 92.6(4) 4_675 7_676 ?
Si O1 Pb01 118.4(7) . 3_565 ?
Si O1 Tb02 104.3(5) . 4_675 ?
Si O1 Tb02 104.3(5) . 7_676 ?
Pb01 O2 Pb01 114.6(5) 9_667 2_675 ?
Pb01 O2 Tb02 101.7(4) 2_675 4_675 ?
Pb01 O2 Tb02 108.3(5) 9_667 4_675 ?
Si O2 Pb01 95.2(6) . 2_675 ?
Si O2 Pb01 137.9(7) . 9_667 ?
Si O2 Tb02 92.8(6) . 4_675 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_pb
_database_code_depnum_ccdc_archive 'CCDC 2043333'
loop_
_audit_author_name
_audit_author_address
'Ce Tao'
;university of chinese academy of science
China
;
_audit_update_record             
;
2020-11-09 deposited with the CCDC.	2021-09-07 downloaded from the CCDC.
;
_audit_creation_date             2020-02-01
_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         '0.5(O24 P4 Pb10 Si2)'
_chemical_formula_sum            'O12 P2 Pb5 Si'
_chemical_formula_weight         1317.95
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_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      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'

_cell_length_a                   9.7637(14)
_cell_length_b                   9.7637(14)
_cell_length_c                   7.2791(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     600.9(2)
_cell_formula_units_Z            2.00004
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    70.229
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    7.284
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1100
_exptl_crystal_preparation       ?
_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  0.0998
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5634
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.430
_diffrn_reflns_theta_min         3.693
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                482
_reflns_number_total             493
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.891
_refine_diff_density_min         -2.358
_refine_diff_density_rms         0.478
_refine_ls_extinction_coef       0.0045(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   1.416
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         493
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0564
_refine_ls_restrained_S_all      1.395
_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)+55.9231P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1023
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{P, Si}
2. Rigid bond restraints
 O1, O2, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uiso(P) = Uiso(Si)
4. Others
 Fixed Sof: P(0.33333) Si(0.1665)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_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 0.25030(13) 0.00021(14) 0.250000 0.0140(4) Uani 1 2 d S T P . .
Pb2 Pb 0.333333 -0.333333 0.00422(19) 0.0129(5) Uani 1 3 d S T P . .
P P 0.6209(8) 0.0188(8) 0.250000 0.0025(12) Uiso 0.6667 2 d S T P . .
Si Si 0.6209(8) 0.0188(8) 0.250000 0.0025(12) Uiso 0.333 2 d S T P . .
O1 O 0.7287(16) 0.0787(16) 0.4231(19) 0.011(3) Uani 1 1 d . U . . .
O2 O 0.507(2) 0.093(2) 0.250000 0.010(4) Uiso 1 2 d S TU P . .
O3 O 0.519(2) -0.167(2) 0.250000 0.009(4) Uiso 1 2 d S TU 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 Si 3.230(7) 8_666 ?
Pb1 O1 2.639(14) 5_665 ?
Pb1 O1 2.541(14) 4_654 ?
Pb1 O1 2.541(14) 7_656 ?
Pb1 O1 2.639(14) 8_666 ?
Pb1 O2 2.20(2) . ?
Pb1 O3 2.756(19) 3_545 ?
Pb2 Pb2 3.578(3) 8_656 ?
Pb2 O3 2.485(14) . ?
Pb2 O3 2.485(14) 3_545 ?
Pb2 O3 2.485(14) 8_656 ?
P O1 1.556(14) . ?
P O1 1.556(14) 10_556 ?
P O2 1.61(2) . ?
P O3 1.57(2) . ?

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 Si 28.6(3) 8_666 8_666 ?
O1 Pb1 Si 28.6(3) 5_665 8_666 ?
O1 Pb1 Si 106.8(3) 7_656 8_666 ?
O1 Pb1 Si 106.8(3) 4_654 8_666 ?
O1 Pb1 O1 134.9(5) 4_654 5_665 ?
O1 Pb1 O1 139.0(6) 4_654 7_656 ?
O1 Pb1 O1 79.1(3) 7_656 5_665 ?
O1 Pb1 O1 79.1(3) 4_654 8_666 ?
O1 Pb1 O1 134.9(5) 7_656 8_666 ?
O1 Pb1 O1 57.0(6) 5_665 8_666 ?
O1 Pb1 O3 150.8(3) 8_666 3_545 ?
O1 Pb1 O3 150.8(3) 5_665 3_545 ?
O1 Pb1 O3 71.7(3) 4_654 3_545 ?
O1 Pb1 O3 71.7(3) 7_656 3_545 ?
O2 Pb1 Si 76.4(5) . 8_666 ?
O2 Pb1 O1 79.3(6) . 5_665 ?
O2 Pb1 O1 82.9(4) . 7_656 ?
O2 Pb1 O1 82.9(4) . 4_654 ?
O2 Pb1 O1 79.3(6) . 8_666 ?
O2 Pb1 O3 95.7(7) . 3_545 ?
O3 Pb1 Si 172.1(4) 3_545 8_666 ?
O3 Pb2 Pb2 44.0(3) 3_545 8_656 ?
O3 Pb2 Pb2 43.9(3) . 8_656 ?
O3 Pb2 Pb2 44.0(3) 8_656 8_656 ?
O3 Pb2 O3 73.9(5) . 8_656 ?
O3 Pb2 O3 73.9(5) 3_545 8_656 ?
O3 Pb2 O3 73.9(5) 3_545 . ?
O1 P O1 108.1(11) . 10_556 ?
O1 P O2 108.8(7) 10_556 . ?
O1 P O2 108.8(7) . . ?
O1 P O3 110.7(7) . . ?
O1 P O3 110.7(7) 10_556 . ?
O3 P O2 109.7(11) . . ?
Pb1 O1 Pb1 115.6(5) 7_656 3_655 ?
P O1 Pb1 141.8(8) . 7_656 ?
P O1 Pb1 97.3(7) . 3_655 ?
P O2 Pb1 136.1(12) . . ?
Pb2 O3 Pb1 104.1(6) 8_656 8_656 ?
Pb2 O3 Pb1 104.1(6) . 8_656 ?
Pb2 O3 Pb2 92.1(7) 8_656 . ?
P O3 Pb1 101.5(9) . 8_656 ?
P O3 Pb2 126.1(6) . 8_656 ?
P O3 Pb2 126.1(6) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
