# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_725k23
_database_code_depnum_ccdc_archive 'CCDC 2327037'
loop_
_audit_author_name
_audit_author_address
'Peng-Fei Li'
;State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter
China
;
_audit_update_record             
;
2024-01-21 deposited with the CCDC.	2024-04-05 downloaded from the CCDC.
;
_audit_creation_date             2024-01-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'F6 O3 Pb2 Se Si'
_chemical_formula_sum            'F6 O3 Pb2 Se Si'
_chemical_formula_weight         683.43
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Se Se -0.0929 2.2259 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   13.8153(4)
_cell_length_b                   5.4470(2)
_cell_length_c                   9.6098(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     723.16(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8344
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      32.1570
_cell_measurement_theta_min      2.5410
_shelx_estimated_absorpt_T_max   0.104
_shelx_estimated_absorpt_T_min   0.063
_exptl_absorpt_coefficient_mu    51.788
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    6.277
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8697
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.986
_diffrn_reflns_theta_max         24.986
_diffrn_reflns_theta_min         2.582
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova (Mo) X-ray Source'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                693
_reflns_number_total             711
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.741
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.277
_refine_ls_extinction_coef       0.00189(13)
_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   1.030
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         711
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0189
_refine_ls_restrained_S_all      1.011
_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)+(0.0236P)²+5.4948P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0465
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(F3) \\sim Ueq, Uanis(Si1) \\sim Ueq: with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
Uanis(Si1) \\sim Ueq: with sigma of 0.000001 and sigma for terminal atoms of
0.000002
Uanis(O1) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of
0.00002
Uanis(O2) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of
0.00002
;
_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
Pb1 Pb 0.39153(2) 0.250000 -0.00459(3) 0.00388(16) Uani 1 2 d S T P . .
Pb2 Pb 0.57468(2) 0.250000 0.63940(4) 0.00677(16) Uani 1 2 d S T P . .
Se1 Se 0.56198(6) 0.250000 0.24192(9) 0.0029(2) Uani 1 2 d S T P . .
Si1 Si 0.73703(18) 0.750000 0.4008(3) 0.0049(5) Uani 1 2 d S TU P . .
F1 F 0.6950(3) 0.5265(7) 0.5049(4) 0.0110(9) Uani 1 1 d . . . . .
F2 F 0.8426(4) 0.750000 0.4914(5) 0.0072(12) Uani 1 2 d S T P . .
F3 F 0.6332(4) 0.750000 0.3110(6) 0.0141(12) Uani 1 2 d S TU P . .
O1 O 0.5027(3) 0.4817(8) 0.1538(5) 0.0052(9) Uani 1 1 d . U . . .
F4 F 0.7845(3) 0.5339(7) 0.2946(4) 0.0106(8) Uani 1 1 d . . . . .
O2 O 0.5000(5) 0.250000 0.3916(7) 0.0095(12) Uani 1 2 d S TU 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
Pb1 0.0021(2) 0.0056(2) 0.0039(2) 0.000 -0.00002(11) 0.000
Pb2 0.0041(2) 0.0119(2) 0.0044(2) 0.000 0.00067(13) 0.000
Se1 0.0018(4) 0.0054(4) 0.0015(4) 0.000 -0.0007(3) 0.000
Si1 0.0049(5) 0.0049(5) 0.0049(5) 0.000 -0.00001(10) 0.000
F1 0.013(2) 0.0102(19) 0.010(2) 0.0039(15) 0.0012(15) -0.0039(16)
F2 0.010(3) 0.007(3) 0.006(3) 0.000 -0.002(2) 0.000
F3 0.0140(12) 0.0141(12) 0.0141(12) 0.000 0.0000(2) 0.000
O1 0.0052(9) 0.0052(9) 0.0052(9) 0.00000(11) 0.00000(11) 0.00000(11)
F4 0.0127(19) 0.0145(19) 0.0047(18) -0.0031(15) -0.0001(16) 0.0010(16)
O2 0.0095(12) 0.0095(12) 0.0095(12) 0.000 0.00001(11) 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
Pb1 O1 2.504(4) . ?
Pb1 O1 2.515(4) 5_665 ?
Pb1 O1 2.515(4) 3_645 ?
Pb1 O1 2.504(4) 7_565 ?
Pb2 F1 2.589(4) 7_565 ?
Pb2 F1 2.589(4) . ?
Pb2 O1 2.689(4) 5_666 ?
Pb2 O1 2.689(4) 3_646 ?
Pb2 F4 2.719(4) 8_756 ?
Pb2 F4 2.719(4) 2_665 ?
Pb2 O2 2.595(7) . ?
Se1 O1 1.727(4) 7_565 ?
Se1 O1 1.727(4) . ?
Se1 O2 1.674(7) . ?
Si1 F1 1.679(4) . ?
Si1 F1 1.679(4) 7_575 ?
Si1 F2 1.699(6) . ?
Si1 F3 1.674(6) . ?
Si1 F4 1.691(4) . ?
Si1 F4 1.691(4) 7_575 ?

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 O1 60.55(19) . 7_565 ?
O1 Pb1 O1 106.44(9) 7_565 5_665 ?
O1 Pb1 O1 72.38(17) . 5_665 ?
O1 Pb1 O1 71.04(19) 5_665 3_645 ?
O1 Pb1 O1 72.38(17) 7_565 3_645 ?
O1 Pb1 O1 106.44(9) . 3_645 ?
F1 Pb2 F1 71.14(18) 7_565 . ?
F1 Pb2 O1 107.95(13) 7_565 3_646 ?
F1 Pb2 O1 160.15(13) 7_565 5_666 ?
F1 Pb2 O1 160.15(13) . 3_646 ?
F1 Pb2 O1 107.95(13) . 5_666 ?
F1 Pb2 F4 64.05(11) 7_565 8_756 ?
F1 Pb2 F4 93.79(12) 7_565 2_665 ?
F1 Pb2 F4 64.05(11) . 2_665 ?
F1 Pb2 F4 93.79(12) . 8_756 ?
F1 Pb2 O2 78.30(15) 7_565 . ?
F1 Pb2 O2 78.30(15) . . ?
O1 Pb2 O1 65.85(18) 5_666 3_646 ?
O1 Pb2 F4 69.13(12) 3_646 8_756 ?
O1 Pb2 F4 69.13(12) 5_666 2_665 ?
O1 Pb2 F4 96.57(12) 5_666 8_756 ?
O1 Pb2 F4 96.57(12) 3_646 2_665 ?
F4 Pb2 F4 51.30(15) 2_665 8_756 ?
O2 Pb2 O1 121.35(15) . 3_646 ?
O2 Pb2 O1 121.35(15) . 5_666 ?
O2 Pb2 F4 141.96(13) . 2_665 ?
O2 Pb2 F4 141.96(13) . 8_756 ?
O1 Se1 O1 93.9(3) 7_565 . ?
O2 Se1 O1 100.3(2) . . ?
O2 Se1 O1 100.3(2) . 7_565 ?
F1 Si1 F1 92.9(3) . 7_575 ?
F1 Si1 F2 89.5(2) . . ?
F1 Si1 F2 89.5(2) 7_575 . ?
F1 Si1 F4 89.38(19) . . ?
F1 Si1 F4 177.0(2) 7_575 . ?
F1 Si1 F4 89.38(19) 7_575 7_575 ?
F1 Si1 F4 177.0(2) . 7_575 ?
F2 Si1 F4 88.6(2) . . ?
F2 Si1 F4 88.6(2) . 7_575 ?
F3 Si1 F1 90.6(2) . 7_575 ?
F3 Si1 F1 90.6(2) . . ?
F3 Si1 F2 179.8(3) . . ?
F3 Si1 F4 91.2(2) . 7_575 ?
F3 Si1 F4 91.2(2) . . ?
F4 Si1 F4 88.2(3) . 7_575 ?
Si1 F1 Pb2 160.2(2) . . ?
Pb1 O1 Pb1 107.62(17) . 5_665 ?
Pb1 O1 Pb2 109.67(15) 5_665 5_666 ?
Pb1 O1 Pb2 118.65(16) . 5_666 ?
Se1 O1 Pb1 115.4(2) . 5_665 ?
Se1 O1 Pb1 102.75(18) . . ?
Se1 O1 Pb2 102.9(2) . 5_666 ?
Si1 F4 Pb2 107.90(18) . 2_664 ?
Se1 O2 Pb2 125.8(3) . . ?

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
F1 Si1 F1 Pb2 64.4(7) 7_575 . . . ?
F1 Si1 F4 Pb2 -159.5(2) . . . 2_664 ?
F2 Si1 F1 Pb2 153.9(7) . . . . ?
F2 Si1 F4 Pb2 -69.96(19) . . . 2_664 ?
F3 Si1 F1 Pb2 -26.2(7) . . . . ?
F3 Si1 F4 Pb2 109.9(2) . . . 2_664 ?
O1 Se1 O1 Pb1 1.1(3) 7_565 . . . ?
O1 Se1 O1 Pb1 -115.72(17) 7_565 . . 5_665 ?
O1 Se1 O1 Pb2 124.87(14) 7_565 . . 5_666 ?
O1 Se1 O2 Pb2 -132.01(15) . . . . ?
O1 Se1 O2 Pb2 132.01(15) 7_565 . . . ?
F4 Si1 F1 Pb2 -117.4(7) . . . . ?
F4 Si1 F4 Pb2 18.7(3) 7_575 . . 2_664 ?
O2 Se1 O1 Pb1 -100.2(2) . . . . ?
O2 Se1 O1 Pb1 143.0(2) . . . 5_665 ?
O2 Se1 O1 Pb2 23.6(2) . . . 5_666 ?

_shelx_res_file                  
;
TITL 725k23_a.res in Pnma
    725k23.res
    created by SHELXL-2016/6 at 13:11:59 on 21-Jan-2024
REM Old TITL 725k23_a.res in Pnma
REM SHELXT solution in Pnma
REM R1 0.063, Rweak 0.003, Alpha 0.014, Orientation as input
REM Formula found by SHELXT: Se Pb2 F10
CELL 0.71073 13.8153 5.447 9.6098 90 90 90
ZERR 4 0.0004 0.0002 0.0003 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC F O Pb Se Si
UNIT 24 12 8 4 4
ISOR 0.0001 0.0002 F3 Si1
ISOR 0.000001 0.000002 Si1
ISOR 0.00001 0.00002 O1
ISOR 0.00001 0.00002 O2

L.S. 200 0 0
PLAN  1
SIZE 0.12 0.1 0.08
TEMP -173
CONF
list 4
MORE -1
fmap 2 53
acta
OMIT -3 50
REM <olex2.extras>
REM <HklSrc "%.\\725K23_sx.hkl">
REM </olex2.extras>

WGHT    0.023600    5.494801
EXTI    0.001888
FVAR       0.17820
PB1   3    0.391532    0.250000   -0.004594    10.50000    0.00212    0.00563 =
         0.00389    0.00000   -0.00002    0.00000
PB2   3    0.574682    0.250000    0.639399    10.50000    0.00406    0.01189 =
         0.00437    0.00000    0.00067    0.00000
SE1   4    0.561978    0.250000    0.241923    10.50000    0.00178    0.00543 =
         0.00154    0.00000   -0.00071    0.00000
SI1   5    0.737028    0.750000    0.400791    10.50000    0.00487    0.00491 =
         0.00487    0.00000   -0.00001    0.00000
F1    1    0.695044    0.526515    0.504900    11.00000    0.01295    0.01025 =
         0.00988    0.00392    0.00123   -0.00391
F2    1    0.842621    0.750000    0.491378    10.50000    0.00961    0.00656 =
         0.00557    0.00000   -0.00183    0.00000
F3    1    0.633184    0.750000    0.310958    10.50000    0.01405    0.01407 =
         0.01406    0.00000   -0.00005    0.00000
O1    2    0.502699    0.481714    0.153795    11.00000    0.00522    0.00521 =
         0.00522    0.00000    0.00000    0.00000
F4    1    0.784515    0.533920    0.294556    11.00000    0.01274    0.01453 =
         0.00466   -0.00315   -0.00011    0.00104
O2    2    0.500021    0.250000    0.391576    10.50000    0.00953    0.00954 =
         0.00953    0.00000    0.00001    0.00000
HKLF 4




REM  725k23_a.res in Pnma
REM R1 =  0.0189 for     693 Fo > 4sig(Fo)  and  0.0199 for all     711 data
REM     71 parameters refined using     24 restraints

END

WGHT      0.0156      4.7183

REM Highest difference peak  1.741,  deepest hole -1.256,  1-sigma level  0.277
Q1    1   0.3921  0.0772 -0.0017  11.00000  0.05    1.74
;
_shelx_res_checksum              71800
_olex2_submission_special_instructions 'No special instructions were received'
