# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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. 
# 
#######################################################################

data_NaB3P2S10
_database_code_depnum_ccdc_archive 'CCDC 2253257'
loop_
_audit_author_name
_audit_author_address
'Yi Huang' 'Harbin Institute of Technology'
_audit_update_record             
;
2023-03-31 deposited with the CCDC.	2023-05-23 downloaded from the CCDC.
;
_audit_creation_date             2023-03-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'B3 Na P2 S10'
_chemical_formula_sum            'B3 Na P2 S10'
_chemical_formula_weight         437.96
_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'
Na Na 0.0362 0.0249 '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'
S S 0.1246 0.1234 '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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   13.126(3)
_cell_length_b                   13.126(3)
_cell_length_c                   15.379(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2649.6(15)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3019
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.502
_cell_measurement_theta_min      3.104
_shelx_estimated_absorpt_T_max   0.805
_shelx_estimated_absorpt_T_min   0.777
_exptl_absorpt_coefficient_mu    1.895
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1680 before and 0.0858 after correction.
The Ratio of minimum to maximum transmission is 0.7099.
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    2.196
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14971
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         2.040
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1170
_reflns_number_total             1517
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1517
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0341
_refine_ls_restrained_S_all      1.071
_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)+(0.0233P)²+6.3878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0867
_refine_special_details          ?
_olex2_refinement_description    
;
;
_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
S2 S 0.62030(5) 0.21828(5) 0.79946(4) 0.01405(17) Uani 1 1 d . . . . .
S4 S 0.68705(6) 0.44887(6) 0.80986(5) 0.01832(19) Uani 1 1 d . . . . .
P1 P 0.56428(6) 0.48271(6) 0.73196(5) 0.01641(19) Uani 1 1 d . . . . .
S3 S 0.76472(6) 0.31183(6) 0.94217(5) 0.01864(19) Uani 1 1 d . . . . .
S1 S 0.46894(6) 0.14192(6) 0.65338(5) 0.01956(19) Uani 1 1 d . . . . .
S5 S 0.59646(6) 0.60009(6) 0.65848(5) 0.0244(2) Uani 1 1 d . . . . .
Na1 Na 0.500000 0.500000 0.500000 0.0971(14) Uani 1 2 d S . P . .
B1 B 0.500000 0.250000 0.7327(3) 0.0160(9) Uani 1 2 d S T P . .
B2 B 0.6442(2) 0.3337(2) 0.8759(2) 0.0161(7) Uani 1 1 d . . . . .

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
S2 0.0130(3) 0.0132(3) 0.0160(3) -0.0002(3) 0.0003(3) -0.0003(3)
S4 0.0151(4) 0.0159(4) 0.0240(4) 0.0043(3) -0.0009(3) -0.0028(3)
P1 0.0160(4) 0.0139(4) 0.0193(4) 0.0040(3) 0.0007(3) -0.0006(3)
S3 0.0136(4) 0.0176(4) 0.0247(4) 0.0027(3) -0.0040(3) -0.0019(3)
S1 0.0258(4) 0.0175(4) 0.0153(4) -0.0026(3) 0.0000(3) -0.0031(3)
S5 0.0259(4) 0.0201(4) 0.0271(4) 0.0114(3) 0.0009(3) -0.0028(3)
Na1 0.179(4) 0.078(2) 0.0343(14) 0.0001(15) -0.029(2) 0.048(2)
B1 0.016(2) 0.013(2) 0.019(2) 0.000 0.000 0.0004(17)
B2 0.0133(15) 0.0165(16) 0.0184(16) 0.0011(13) -0.0002(12) 0.0006(12)

_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
S2 B1 1.929(3) . ?
S2 B2 1.931(3) 11_667 ?
S2 B2 1.942(3) . ?
S4 P1 2.0566(11) . ?
S4 B2 1.906(3) . ?
P1 S3 2.0684(11) 16_657 ?
P1 S1 2.0801(11) 6_554 ?
P1 S5 1.9568(11) . ?
S3 B2 1.904(3) . ?
S1 Na1 3.0332(10) 6_554 ?
S1 B1 1.915(3) . ?
S5 Na1 3.0445(11) . ?
S5 Na1 3.1488(11) 8_454 ?

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
B1 S2 B2 106.13(12) . 11_667 ?
B1 S2 B2 106.62(12) . . ?
B2 S2 B2 106.07(10) 11_667 . ?
B2 S4 P1 104.51(11) . . ?
S4 P1 S3 110.01(5) . 16_657 ?
S4 P1 S1 109.44(5) . 6_554 ?
S3 P1 S1 108.65(5) 16_657 6_554 ?
S5 P1 S4 109.72(5) . . ?
S5 P1 S3 109.79(5) . 16_657 ?
S5 P1 S1 109.21(5) . 6_554 ?
B2 S3 P1 104.71(11) . 11_667 ?
P1 S1 Na1 89.82(4) 6_554 6_554 ?
B1 S1 P1 104.91(12) . 6_554 ?
B1 S1 Na1 157.18(8) . 6_554 ?
P1 S5 Na1 91.88(4) . . ?
P1 S5 Na1 111.84(4) . 8_454 ?
Na1 S5 Na1 153.34(3) . 8_454 ?
S1 Na1 S1 180.0 14_556 6_554 ?
S1 Na1 S5 97.44(3) 6_554 15_566 ?
S1 Na1 S5 65.58(3) 6_554 . ?
S1 Na1 S5 82.56(3) 14_556 15_566 ?
S1 Na1 S5 65.58(3) 14_556 9_666 ?
S1 Na1 S5 97.44(3) 14_556 7_544 ?
S1 Na1 S5 82.56(3) 6_554 7_544 ?
S1 Na1 S5 114.42(3) 6_554 9_666 ?
S1 Na1 S5 114.42(3) 14_556 . ?
S5 Na1 S5 68.03(3) . 15_566 ?
S5 Na1 S5 68.03(3) 9_666 7_544 ?
S5 Na1 S5 111.97(3) 9_666 15_566 ?
S5 Na1 S5 180.0 15_566 7_544 ?
S5 Na1 S5 180.0 9_666 . ?
S5 Na1 S5 111.97(3) . 7_544 ?
S2 B1 S2 115.7(2) . 6_554 ?
S1 B1 S2 108.95(4) . 6_554 ?
S1 B1 S2 108.95(4) 6_554 . ?
S1 B1 S2 110.70(4) 6_554 6_554 ?
S1 B1 S2 110.70(4) . . ?
S1 B1 S1 100.9(2) 6_554 . ?
S2 B2 S2 115.48(17) 16_657 . ?
S4 B2 S2 110.13(16) . . ?
S4 B2 S2 110.16(16) . 16_657 ?
S3 B2 S2 109.93(16) . . ?
S3 B2 S2 110.74(16) . 16_657 ?
S3 B2 S4 99.19(15) . . ?

_shelx_res_file                  
;
TITL shou2222_a.res in I4(1)/a
    shou2222.res
    created by SHELXL-2018/3 at 22:06:37 on 31-Mar-2023
REM Old TITL SHOU2222 in I4(1)/a
REM SHELXT solution in I4(1)/a: R1 0.119, Rweak 0.003, Alpha 0.020
REM <I/s> 0.225 for 57 systematic absences, Orientation as input
REM Formula found by SHELXT: B P S3
CELL 0.71073 13.1257 13.1257 15.3792 90 90 90
ZERR 8 0.0033 0.0033 0.0045 0 0 0
LATT 2
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.75-Y,0.25+X,0.25+Z
SYMM 0.75+Y,0.75-X,0.75+Z
SFAC B Na P S
UNIT 24 8 16 80

L.S. 40
PLAN  2
SIZE 0.13 0.14 0.12
TEMP 0
CONF
list 4
MORE -1
fmap 2 53
acta
OMIT 1 5 4
OMIT -3 5 6
REM <olex2.extras>
REM <HklSrc "%.\\shou2222.hkl">
REM </olex2.extras>

WGHT    0.023300    6.387800
FVAR       0.12713
S2    4    0.620304    0.218277    0.799464    11.00000    0.01299    0.01318 =
         0.01599   -0.00020    0.00033   -0.00035
S4    4    0.687051    0.448868    0.809865    11.00000    0.01506    0.01591 =
         0.02400    0.00434   -0.00087   -0.00283
P1    3    0.564282    0.482713    0.731956    11.00000    0.01599    0.01393 =
         0.01932    0.00399    0.00066   -0.00064
S3    4    0.764723    0.311833    0.942169    11.00000    0.01358    0.01761 =
         0.02472    0.00266   -0.00399   -0.00186
S1    4    0.468940    0.141922    0.653380    11.00000    0.02584    0.01752 =
         0.01533   -0.00259    0.00000   -0.00307
S5    4    0.596455    0.600089    0.658476    11.00000    0.02589    0.02012 =
         0.02709    0.01140    0.00089   -0.00280
NA1   2    0.500000    0.500000    0.500000    10.50000    0.17919    0.07773 =
         0.03432    0.00009   -0.02852    0.04832
B1    1    0.500000    0.250000    0.732688    10.50000    0.01566    0.01306 =
         0.01914    0.00000    0.00000    0.00040
B2    1    0.644227    0.333674    0.875860    11.00000    0.01329    0.01648 =
         0.01842    0.00105   -0.00019    0.00055
HKLF 4




REM  shou2222_a.res in I4(1)/a
REM wR2 = 0.0867, GooF = S = 1.071, Restrained GooF = 1.071 for all data
REM R1 = 0.0341 for 1170 Fo > 4sig(Fo) and 0.0499 for all 1517 data
REM 75 parameters refined using 0 restraints

END

WGHT      0.0233      6.3876

REM Highest difference peak  0.564,  deepest hole -0.409,  1-sigma level  0.114
Q1    1   0.4527  0.0838  0.6884  11.00000  0.05    0.56
Q2    1   0.6355  0.4608  0.7735  11.00000  0.05    0.50
;
_shelx_res_checksum              6736
_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_KB3P2S10
_database_code_depnum_ccdc_archive 'CCDC 2253258'
loop_
_audit_author_name
_audit_author_address
'Yi Huang' 'Harbin Institute of Technology'
_audit_update_record             
;
2023-03-31 deposited with the CCDC.	2023-05-23 downloaded from the CCDC.
;
_audit_creation_date             2023-03-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'B3 K P2 S10'
_chemical_formula_sum            'B3 K P2 S10'
_chemical_formula_weight         454.07
_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'
K K 0.2009 0.2494 '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'
S S 0.1246 0.1234 '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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   13.0262(8)
_cell_length_b                   13.0262(8)
_cell_length_c                   16.5387(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2806.3(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2003
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.366
_cell_measurement_theta_min      3.127
_shelx_estimated_absorpt_T_max   0.805
_shelx_estimated_absorpt_T_min   0.776
_exptl_absorpt_coefficient_mu    2.055
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_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    2.149
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10257
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.466
_diffrn_reflns_theta_min         1.990
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1075
_reflns_number_total             1605
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.0029(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   1.060
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1605
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0465
_refine_ls_restrained_S_all      1.060
_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)+(0.0760P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1391
_refine_special_details          ?
_olex2_refinement_description    
;
;
_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
S4 S 0.62214(7) 0.27923(7) 0.30511(6) 0.0222(3) Uani 1 1 d . . . . .
S3 S 0.70446(8) 0.43293(8) 0.43721(6) 0.0283(3) Uani 1 1 d . . . . .
S2 S 0.56863(8) 0.51499(8) 0.31310(7) 0.0291(3) Uani 1 1 d . . . . .
S5 S 0.52774(9) 0.14106(8) 0.16918(7) 0.0308(3) Uani 1 1 d . . . . .
P1 P 0.44242(9) 0.48542(8) 0.24122(6) 0.0269(3) Uani 1 1 d . . . . .
S1 S 0.41551(9) 0.60346(9) 0.17211(7) 0.0366(3) Uani 1 1 d . . . . .
K1 K 0.250000 0.750000 0.250000 0.1046(11) Uani 1 2 d S . P . .
B1 B 0.5875(3) 0.3933(3) 0.3753(3) 0.0227(9) Uani 1 1 d . . . . .
B2 B 0.500000 0.250000 0.2427(4) 0.0254(13) Uani 1 2 d S T 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
S4 0.0212(5) 0.0193(5) 0.0261(6) 0.0020(4) 0.0020(4) 0.0020(4)
S3 0.0233(5) 0.0242(5) 0.0373(6) 0.0015(4) -0.0041(4) -0.0057(4)
S2 0.0277(6) 0.0209(5) 0.0389(6) 0.0053(4) 0.0000(4) -0.0012(4)
S5 0.0399(6) 0.0261(6) 0.0264(6) -0.0037(4) -0.0014(4) 0.0092(5)
P1 0.0277(6) 0.0212(6) 0.0318(6) 0.0044(4) 0.0020(4) 0.0050(4)
S1 0.0405(7) 0.0277(6) 0.0417(7) 0.0122(5) 0.0063(5) 0.0097(5)
K1 0.1114(19) 0.167(3) 0.0350(10) 0.0041(12) 0.0066(11) 0.1006(19)
B1 0.019(2) 0.024(2) 0.025(2) -0.0016(17) -0.0011(17) -0.0031(17)
B2 0.025(3) 0.028(3) 0.023(3) 0.000 0.000 0.007(3)

_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
S4 B1 1.927(4) 11_666 ?
S4 B1 1.939(4) . ?
S4 B2 1.935(3) . ?
S3 P1 2.0567(15) 11_666 ?
S3 B1 1.907(4) . ?
S2 P1 2.0651(16) . ?
S2 B1 1.905(5) . ?
S5 P1 2.0700(15) 6_554 ?
S5 K1 3.3669(11) 7_544 ?
S5 B2 1.903(4) . ?
P1 S1 1.9477(14) . ?
S1 K1 3.1546(12) . ?
S1 K1 3.3361(12) 4_454 ?

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
B1 S4 B1 106.31(13) 11_666 . ?
B1 S4 B2 106.34(16) 11_666 . ?
B2 S4 B1 106.22(16) . . ?
B1 S3 P1 104.53(14) . 11_666 ?
B1 S2 P1 104.98(14) . . ?
P1 S5 K1 93.67(4) 6_554 7_544 ?
B2 S5 P1 105.17(16) . 6_554 ?
B2 S5 K1 156.54(13) . 7_544 ?
S3 P1 S2 109.71(6) 16_656 . ?
S3 P1 S5 108.92(6) 16_656 6_554 ?
S2 P1 S5 109.28(6) . 6_554 ?
S1 P1 S3 110.47(7) . 16_656 ?
S1 P1 S2 109.50(7) . . ?
S1 P1 S5 108.93(7) . 6_554 ?
P1 S1 K1 111.16(5) . . ?
P1 S1 K1 97.03(5) . 4_454 ?
K1 S1 K1 144.92(4) . 4_454 ?
S5 K1 S5 180.0 12_666 8_454 ?
S1 K1 S5 121.60(3) 3 12_666 ?
S1 K1 S5 121.60(3) 15_565 8_454 ?
S1 K1 S5 95.66(3) 13_565 8_454 ?
S1 K1 S5 84.34(3) 13_565 12_666 ?
S1 K1 S5 58.40(3) 3 8_454 ?
S1 K1 S5 95.66(3) . 12_666 ?
S1 K1 S5 58.40(3) 15_565 12_666 ?
S1 K1 S5 84.34(3) . 8_454 ?
S1 K1 S1 64.86(4) 13_565 3 ?
S1 K1 S1 180.0 13_565 . ?
S1 K1 S1 115.14(4) 13_565 15_565 ?
S1 K1 S1 64.86(4) . 15_565 ?
S1 K1 S1 180.00(4) 15_565 3 ?
S1 K1 S1 115.14(4) . 3 ?
S4 B1 S4 115.5(2) 16_656 . ?
S3 B1 S4 110.1(2) . . ?
S3 B1 S4 110.4(2) . 16_656 ?
S2 B1 S4 110.2(2) . . ?
S2 B1 S4 109.8(2) . 16_656 ?
S2 B1 S3 99.7(2) . . ?
S4 B2 S4 115.5(3) 6_554 . ?
S5 B2 S4 109.36(5) . . ?
S5 B2 S4 109.36(5) 6_554 6_554 ?
S5 B2 S4 110.51(5) 6_554 . ?
S5 B2 S4 110.51(5) . 6_554 ?
S5 B2 S5 100.6(3) 6_554 . ?

_shelx_res_file                  
;
TITL kbps111111111_a.res in I4(1)/a
    kbps111111111.res
    created by SHELXL-2018/3 at 21:53:44 on 31-Mar-2023
REM Old TITL KBPS111111111 in I4(1)/a
REM SHELXT solution in I4(1)/a: R1 0.178, Rweak 0.003, Alpha 0.021
REM <I/s> 0.231 for 57 systematic absences, Orientation as input
REM Formula found by SHELXT: B3 P2 S6 K5
CELL 0.71073 13.0262 13.0262 16.5387 90 90 90
ZERR 8 0.0008 0.0008 0.0017 0 0 0
LATT 2
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.75-Y,0.25+X,0.25+Z
SYMM 0.75+Y,0.75-X,0.75+Z
SFAC B K P S
UNIT 24 8 16 80

L.S. 50
PLAN  2
SIZE 0.13 0.12 0.11
TEMP 0
CONF
list 4
MORE -1
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\kbps111111111.hkl">
REM </olex2.extras>

WGHT    0.076000
EXTI    0.002907
FVAR       0.22385
S4    4    0.622139    0.279227    0.305114    11.00000    0.02122    0.01928 =
         0.02612    0.00204    0.00200    0.00199
S3    4    0.704461    0.432935    0.437210    11.00000    0.02333    0.02418 =
         0.03726    0.00150   -0.00408   -0.00571
S2    4    0.568631    0.514987    0.313096    11.00000    0.02769    0.02087 =
         0.03886    0.00526    0.00000   -0.00124
S5    4    0.527740    0.141059    0.169182    11.00000    0.03988    0.02615 =
         0.02638   -0.00371   -0.00143    0.00918
P1    3    0.442416    0.485418    0.241218    11.00000    0.02773    0.02122 =
         0.03175    0.00439    0.00196    0.00498
S1    4    0.415510    0.603459    0.172108    11.00000    0.04049    0.02768 =
         0.04169    0.01217    0.00634    0.00972
K1    2    0.250000    0.750000    0.250000    10.50000    0.11143    0.16732 =
         0.03502    0.00413    0.00658    0.10063
B1    1    0.587543    0.393321    0.375276    11.00000    0.01943    0.02353 =
         0.02505   -0.00159   -0.00112   -0.00306
B2    1    0.500000    0.250000    0.242656    10.50000    0.02466    0.02811 =
         0.02337    0.00000    0.00000    0.00729
HKLF 4




REM  kbps111111111_a.res in I4(1)/a
REM wR2 = 0.1391, GooF = S = 1.060, Restrained GooF = 1.060 for all data
REM R1 = 0.0465 for 1075 Fo > 4sig(Fo) and 0.0710 for all 1605 data
REM 76 parameters refined using 0 restraints

END

WGHT      0.0760      0.0000

REM Highest difference peak  0.553,  deepest hole -0.736,  1-sigma level  0.128
Q1    1   0.2543  0.7020  0.2210  11.00000  0.05    0.55
Q2    1   0.6877  0.3588  0.4680  11.00000  0.05    0.50
;
_shelx_res_checksum              71740
_olex2_submission_special_instructions 'No special instructions were received'
