# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2022871'
_audit_update_record             
;
2020-08-12 deposited with the CCDC.	2020-10-30 downloaded from the CCDC.
;
_audit_creation_date             2020-02-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_publ_section_exptl              
;
Any special experimental details
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'P Pb S3'
_chemical_formula_sum            'P Pb S3'
_chemical_formula_weight         334.34
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   6.603(3)
_cell_length_b                   7.456(4)
_cell_length_c                   9.401(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.618(6)
_cell_angle_gamma                90
_cell_volume                     462.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1131
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      3.49
_shelx_estimated_absorpt_T_max   0.103
_shelx_estimated_absorpt_T_min   0.049
_exptl_absorpt_coefficient_mu    37.960
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1193 before and 0.0360 after correction.
The Ratio of minimum to maximum transmission is 0.5783.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.800
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2689
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.346
_diffrn_reflns_theta_min         3.488
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_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                897
_reflns_number_total             1042
_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 V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 (Sheldrick, 2015)'
_refine_diff_density_max         0.951
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       0.0024(2)
_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   1.002
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         1042
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0227
_refine_ls_restrained_S_all      1.002
_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)+(0.0162P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0430
_refine_ls_wR_factor_ref         0.0444
_refine_special_details          ?
_olex2_refinement_description    
;
;
_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 0.96073(4) 0.61723(4) 0.74937(3) 0.02206(11) Uani 1 1 d . . . . .
S1 S 0.6551(2) 0.8017(2) 0.55606(15) 0.0138(3) Uani 1 1 d . . . . .
P1 P 0.4387(2) 0.6096(2) 0.56545(14) 0.0091(3) Uani 1 1 d . . . . .
S3 S 0.3990(2) 0.5052(2) 0.76098(15) 0.0146(3) Uani 1 1 d . . . . .
S2 S 0.1810(2) 0.6939(2) 0.46438(15) 0.0133(3) 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
Pb1 0.02143(15) 0.02130(17) 0.02348(16) -0.00060(12) 0.00103(9) 0.00109(11)
S1 0.0129(7) 0.0123(8) 0.0160(7) 0.0000(6) -0.0025(6) -0.0021(6)
P1 0.0098(7) 0.0099(8) 0.0077(6) 0.0009(6) 0.0001(5) 0.0011(6)
S3 0.0190(7) 0.0162(8) 0.0085(7) 0.0015(6) 0.0022(6) 0.0038(6)
S2 0.0098(7) 0.0173(8) 0.0126(7) 0.0002(6) -0.0021(5) 0.0017(6)

_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 S1 3.0100(17) . ?
Pb1 S1 3.0893(19) 2_646 ?
Pb1 S3 3.040(2) 2_656 ?
Pb1 S3 3.011(2) 1_655 ?
Pb1 S2 3.1129(17) 4_676 ?
S1 P1 2.027(2) . ?
P1 P1 2.213(3) 3_666 ?
P1 S3 2.020(2) . ?
P1 S2 2.025(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
S1 Pb1 S1 122.17(4) . 2_646 ?
S1 Pb1 S3 75.25(5) . 2_656 ?
S1 Pb1 S3 140.89(4) . 1_655 ?
S1 Pb1 S2 78.39(5) 2_646 4_676 ?
S1 Pb1 S2 77.60(5) . 4_676 ?
S3 Pb1 S1 91.21(4) 1_655 2_646 ?
S3 Pb1 S1 145.52(4) 2_656 2_646 ?
S3 Pb1 S3 88.38(3) 1_655 2_656 ?
S3 Pb1 S2 133.56(4) 1_655 4_676 ?
S3 Pb1 S2 77.12(5) 2_656 4_676 ?
Pb1 S1 Pb1 99.41(5) . 2_656 ?
P1 S1 Pb1 96.44(7) . . ?
P1 S1 Pb1 109.01(8) . 2_656 ?
S1 P1 P1 103.18(10) . 3_666 ?
S3 P1 S1 114.93(9) . . ?
S3 P1 P1 106.29(11) . 3_666 ?
S3 P1 S2 114.70(9) . . ?
S2 P1 S1 110.12(10) . . ?
S2 P1 P1 106.51(10) . 3_666 ?
Pb1 S3 Pb1 123.78(5) 1_455 2_646 ?
P1 S3 Pb1 90.53(6) . 1_455 ?
P1 S3 Pb1 106.86(7) . 2_646 ?
P1 S2 Pb1 86.51(7) . 4_575 ?

_shelx_res_file                  
;
TITL 1_a.res in P2(1)/n
    1.res
    created by SHELXL-2018/3 at 17:14:10 on 27-Feb-2020
CELL 0.71073 6.6031 7.4563 9.4008 90 91.618 90
ZERR 4 0.0032 0.0036 0.0046 0 0.006 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC P Pb S
UNIT 4 4 12

L.S. 50
PLAN  5
SIZE 0.11 0.13 0.2
TEMP 23
fmap 2
acta
OMIT 1 0 1
REM <olex2.extras>
REM <HklSrc "%.\\1.hkl">
REM </olex2.extras>

WGHT    0.016200
EXTI    0.002391
FVAR       0.33580
PB1   2    0.960725    0.617228    0.749373    11.00000    0.02143    0.02130 =
         0.02348   -0.00060    0.00103    0.00109
S1    3    0.655105    0.801720    0.556061    11.00000    0.01285    0.01233 =
         0.01601    0.00003   -0.00246   -0.00207
P1    1    0.438671    0.609576    0.565454    11.00000    0.00982    0.00994 =
         0.00767    0.00086    0.00013    0.00106
S3    3    0.399045    0.505231    0.760975    11.00000    0.01903    0.01623 =
         0.00851    0.00149    0.00219    0.00384
S2    3    0.181034    0.693917    0.464383    11.00000    0.00983    0.01732 =
         0.01263    0.00022   -0.00213    0.00171
HKLF 4




REM  1_a.res in P2(1)/n
REM wR2 = 0.0444, GooF = S = 1.002, Restrained GooF = 1.002 for all data
REM R1 = 0.0227 for 897 Fo > 4sig(Fo) and 0.0290 for all 1042 data
REM 47 parameters refined using 0 restraints

END

WGHT      0.0163      0.0000

REM Highest difference peak  0.951,  deepest hole -1.080,  1-sigma level  0.225
Q1    1   1.0897  0.6399  0.6417  11.00000  0.05    0.95
Q2    1   0.2872  0.6358  0.4983  11.00000  0.05    0.94
Q3    1   0.8653  0.8957  0.5141  11.00000  0.05    0.86
Q4    1   0.9395  0.5190  0.7040  11.00000  0.05    0.83
Q5    1   0.8712  0.5236  0.7343  11.00000  0.05    0.81
;
_shelx_res_checksum              66438
_olex2_submission_special_instructions 'No special instructions were received'
