# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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_Goldberger_AsPbSn_R-3m
_database_code_depnum_ccdc_archive 'CCDC 2063177'
loop_
_audit_author_name
_audit_author_address
'Curtis E. Moore'
;The Ohio State University, Department of Chemistry and Biochemistry
United States of America
;
_audit_update_record             
;
2021-04-15 deposited with the CCDC.	2021-05-10 downloaded from the CCDC.
;
_audit_creation_date             2021-04-01
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'Lead Tin Arsenide'
_chemical_formula_moiety         'As3 Pb0.676 Sn3.324'
_chemical_formula_sum            'As3 Pb0.676 Sn3.324'
_chemical_formula_weight         759.40
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
As As 0.0499 2.0058 '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'
Sn Sn -0.6537 1.4246 '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      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m'
_space_group_name_Hall           '-R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'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+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'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+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-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+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-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+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   4.0967(3)
_cell_length_b                   4.0967(3)
_cell_length_c                   36.401(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     529.07(9)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    1540
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      30.361
_cell_measurement_theta_min      5.857
_shelx_estimated_absorpt_T_max   0.240
_shelx_estimated_absorpt_T_min   0.193
_exptl_absorpt_coefficient_mu    41.573
_exptl_absorpt_correction_T_max  0.0326
_exptl_absorpt_correction_T_min  0.0053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1631 before and 0.0644 after correction.
The Ratio of minimum to maximum transmission is 0.2231.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'Metallic Silver'
_exptl_crystal_colour_lustre     Metallic
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    Silver
_exptl_crystal_density_diffrn    7.150
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             962
_exptl_crystal_size_max          0.059
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.048
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            7396
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.553
_diffrn_reflns_theta_min         1.678
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa APEX II'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              fine-focus
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                173
_reflns_number_total             257
_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 (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.205
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.354
_refine_ls_extinction_coef       0.00045(13)
_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   1.084
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         257
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0272
_refine_ls_restrained_S_all      1.084
_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)+(0.0411P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0732
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{Pb2, Sn2}
2. Uiso/Uaniso restraints and constraints
Uanis(Pb2) = Uanis(Sn2)
3. Others
 Sof(Pb2)=0.16667*(1-FVAR(2))
 Sof(Sn2)=0.16667*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
As1 As 0.333333 0.666667 0.59815(3) 0.0308(3) Uani 1 6 d S T P . .
As2 As 1.000000 0.000000 0.500000 0.0326(4) Uani 1 12 d S T P . .
Sn1 Sn 0.000000 1.000000 0.63616(3) 0.0308(3) Uani 1 6 d S T P A 1
Sn2 Sn 0.666667 0.333333 0.54473(2) 0.0327(3) Uani 0.662(5) 6 d S T P A 1
Pb2 Pb 0.666667 0.333333 0.54473(2) 0.0327(3) Uani 0.338(5) 6 d S T P A 2


_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
As1 Sn1 2.7402(9) . ?
As1 Sn1 2.7402(9) 1_655 ?
As1 Sn1 2.7402(9) 1_545 ?
As1 Sn2 3.0619(10) 1_455 ?
As1 Sn2 3.0619(10) 1_565 ?
As1 Sn2 3.0619(10) . ?
As1 Pb2 3.0619(10) . ?
As2 Sn2 2.8715(4) 19_656 ?
As2 Sn2 2.8715(4) 1_545 ?
As2 Sn2 2.8715(4) 19_766 ?
As2 Sn2 2.8714(4) . ?
As2 Sn2 2.8715(4) 19_756 ?
As2 Sn2 2.8715(4) 1_655 ?
As2 Pb2 2.8714(4) . ?
Sn1 Sn1 3.2448(13) 25_476 ?
Sn1 Sn1 3.2448(13) 25_576 ?
Sn1 Sn1 3.2448(13) 25_466 ?

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
Sn1 As1 Sn1 96.75(4) . 1_655 ?
Sn1 As1 Sn1 96.75(4) . 1_545 ?
Sn1 As1 Sn1 96.75(4) 1_655 1_545 ?
Sn1 As1 Sn2 89.271(16) . 1_455 ?
Sn1 As1 Sn2 89.271(16) . 1_565 ?
Sn1 As1 Sn2 170.90(5) 1_655 1_455 ?
Sn1 As1 Sn2 89.272(16) 1_655 . ?
Sn1 As1 Sn2 89.271(16) 1_655 1_565 ?
Sn1 As1 Sn2 89.271(16) 1_545 1_455 ?
Sn1 As1 Sn2 89.272(16) 1_545 . ?
Sn1 As1 Sn2 170.90(5) . . ?
Sn1 As1 Sn2 170.90(5) 1_545 1_565 ?
Sn2 As1 Sn2 83.98(3) 1_455 . ?
Sn2 As1 Sn2 83.98(3) 1_455 1_565 ?
Sn2 As1 Sn2 83.98(3) 1_565 . ?
Sn2 As2 Sn2 180.0 . 19_756 ?
Sn2 As2 Sn2 88.984(16) 19_756 1_655 ?
Sn2 As2 Sn2 91.016(16) 19_756 19_766 ?
Sn2 As2 Sn2 88.984(16) 1_655 19_766 ?
Sn2 As2 Sn2 88.984(16) . 19_766 ?
Sn2 As2 Sn2 91.016(16) 1_655 1_545 ?
Sn2 As2 Sn2 91.016(16) . 1_545 ?
Sn2 As2 Sn2 88.984(16) . 19_656 ?
Sn2 As2 Sn2 88.984(16) 19_656 1_545 ?
Sn2 As2 Sn2 88.984(16) 19_756 1_545 ?
Sn2 As2 Sn2 180.0 19_766 1_545 ?
Sn2 As2 Sn2 91.016(16) 19_656 19_766 ?
Sn2 As2 Sn2 180.00(2) 19_656 1_655 ?
Sn2 As2 Sn2 91.016(16) . 1_655 ?
Sn2 As2 Sn2 91.016(16) 19_756 19_656 ?
Pb2 As2 Sn2 88.984(16) . 19_766 ?
As1 Sn1 As1 96.75(4) 1_455 . ?
As1 Sn1 As1 96.75(4) 1_455 1_565 ?
As1 Sn1 As1 96.75(4) 1_565 . ?
As1 Sn1 Sn1 167.12(5) 1_455 25_576 ?
As1 Sn1 Sn1 91.779(18) 1_565 25_476 ?
As1 Sn1 Sn1 91.779(18) 1_455 25_476 ?
As1 Sn1 Sn1 91.779(18) 1_565 25_576 ?
As1 Sn1 Sn1 167.12(5) 1_565 25_466 ?
As1 Sn1 Sn1 91.780(18) . 25_466 ?
As1 Sn1 Sn1 91.779(18) 1_455 25_466 ?
As1 Sn1 Sn1 91.780(18) . 25_576 ?
As1 Sn1 Sn1 167.12(5) . 25_476 ?
Sn1 Sn1 Sn1 78.29(4) 25_576 25_476 ?
Sn1 Sn1 Sn1 78.29(4) 25_576 25_466 ?
Sn1 Sn1 Sn1 78.29(4) 25_466 25_476 ?
As1 Sn2 As1 83.97(3) 1_545 . ?
As1 Sn2 As1 83.97(3) 1_655 1_545 ?
As1 Sn2 As1 83.97(3) 1_655 . ?
As2 Sn2 As1 92.405(14) . 1_545 ?
As2 Sn2 As1 92.405(14) 1_565 1_655 ?
As2 Sn2 As1 175.12(3) 1_565 1_545 ?
As2 Sn2 As1 92.405(14) 1_455 1_545 ?
As2 Sn2 As1 92.404(14) 1_455 . ?
As2 Sn2 As1 175.12(3) 1_455 1_655 ?
As2 Sn2 As1 92.404(14) 1_565 . ?
As2 Sn2 As1 92.405(14) . 1_655 ?
As2 Sn2 As1 175.12(3) . . ?
As2 Sn2 As2 91.017(16) 1_455 1_565 ?
As2 Sn2 As2 91.017(16) . 1_455 ?
As2 Sn2 As2 91.017(16) . 1_565 ?
As1 Pb2 As1 83.97(3) 1_655 1_545 ?
As1 Pb2 As1 83.97(3) 1_655 . ?
As1 Pb2 As1 83.97(3) 1_545 . ?
As2 Pb2 As1 175.12(3) 1_455 1_655 ?
As2 Pb2 As1 175.12(3) 1_565 1_545 ?
As2 Pb2 As1 92.404(14) 1_565 . ?
As2 Pb2 As1 92.405(14) 1_565 1_655 ?
As2 Pb2 As1 92.405(14) . 1_655 ?
As2 Pb2 As1 92.405(14) . 1_545 ?
As2 Pb2 As1 92.405(14) 1_455 1_545 ?
As2 Pb2 As1 92.404(14) 1_455 . ?
As2 Pb2 As1 175.12(3) . . ?
As2 Pb2 As2 91.017(16) 1_455 1_565 ?
As2 Pb2 As2 91.017(16) . 1_565 ?
As2 Pb2 As2 91.017(16) . 1_455 ?

_olex2_submission_special_instructions 'No special instructions were received'
