# Supplementary Information (SI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2026

####################################################################### 
# 
# 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_p21overn
_audit_block_doi                 10.25505/fiz.icsd.cc2mzdtv
_database_code_depnum_ccdc_archive 'CCDC 2442298'
loop_
_audit_author_name
_audit_author_address
'xifeng fu'
;Fujian Institute of Research on the Structure of Matter
China
;
_audit_update_record             
;
2025-09-15 deposited with the CCDC.	2026-05-26 downloaded from the CCDC.
;
_audit_creation_date             2025-08-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Au I3 Rb'
_chemical_formula_sum            'Au I3 Rb'
_chemical_formula_weight         663.14
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 '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                   7.4837(6)
_cell_length_b                   9.1874(8)
_cell_length_c                   11.7223(9)
_cell_angle_alpha                90
_cell_angle_beta                 91.347(3)
_cell_angle_gamma                90
_cell_volume                     805.75(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      30.86
_cell_measurement_theta_min      2.82
_shelx_estimated_absorpt_T_max   0.076
_shelx_estimated_absorpt_T_min   0.025
_exptl_absorpt_coefficient_mu    35.639
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.2785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1543 before and 0.1016 after correction.
The Ratio of minimum to maximum transmission is 0.3732.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.467
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2905
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24291
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.981
_diffrn_reflns_theta_max         24.981
_diffrn_reflns_theta_min         2.217
_diffrn_ambient_temperature      200.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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                1288
_reflns_number_total             1412
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         4.131
_refine_diff_density_min         -3.171
_refine_diff_density_rms         0.628
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         1412
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0732
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1181P)²+17.7437P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1999
_refine_ls_wR_factor_ref         0.2033
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9852(17)
 0.0148(17)
;
_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
Au01 Au 0.500000 0.500000 0.000000 0.0474(5) Uani 1 2 d S . P . .
Au02 Au 0.500000 0.500000 0.500000 0.0529(5) Uani 1 2 d S . P . .
I003 I 0.2148(2) 0.33572(15) 0.02731(13) 0.0557(5) Uani 1 1 d . . . . .
I004 I 0.2182(2) 0.34078(15) 0.47561(13) 0.0563(5) Uani 1 1 d . . . . .
I005 I 0.5544(2) 0.51344(17) 0.22439(15) 0.0585(5) Uani 1 1 d . . . . .
Rb06 Rb 0.4512(3) 0.1040(3) 0.2494(2) 0.0626(6) 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
Au01 0.0509(8) 0.0418(7) 0.0493(8) 0.0006(4) -0.0018(6) -0.0018(4)
Au02 0.0558(8) 0.0457(8) 0.0571(9) -0.0006(4) -0.0001(6) -0.0040(5)
I003 0.0550(9) 0.0504(9) 0.0615(10) 0.0041(6) -0.0032(6) -0.0053(6)
I004 0.0587(9) 0.0480(9) 0.0622(10) -0.0021(6) 0.0014(7) -0.0062(6)
I005 0.0631(10) 0.0632(10) 0.0490(10) -0.0007(6) -0.0035(7) -0.0042(6)
Rb06 0.0627(13) 0.0620(14) 0.0629(14) 0.0024(10) -0.0027(10) -0.0016(11)

_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
Au01 I003 2.6398(14) 3_665 ?
Au01 I003 2.6398(14) . ?
Au01 I005 2.6551(17) 3_665 ?
Au01 I005 2.6551(17) . ?
Au02 I004 2.5772(15) 3_666 ?
Au02 I004 2.5772(15) . ?
Au02 I005 3.2682(18) 3_666 ?
Au02 I005 3.2682(18) . ?
I003 Rb06 3.809(3) 4_565 ?
I003 Rb06 3.824(3) 2 ?
I003 Rb06 3.771(3) . ?
I004 Rb06 3.775(3) 2 ?
I004 Rb06 3.854(3) 4_566 ?
I004 Rb06 3.876(3) . ?
I005 Rb06 3.798(3) 2_655 ?
I005 Rb06 3.893(3) 2 ?
I005 Rb06 3.853(3) . ?

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
I003 Au01 I003 180.0 3_665 . ?
I003 Au01 I005 90.69(5) . . ?
I003 Au01 I005 90.69(5) 3_665 3_665 ?
I003 Au01 I005 89.31(5) 3_665 . ?
I003 Au01 I005 89.31(5) . 3_665 ?
I005 Au01 I005 180.0 . 3_665 ?
I004 Au02 I004 180.0 . 3_666 ?
I004 Au02 I005 88.14(5) 3_666 . ?
I004 Au02 I005 91.86(5) 3_666 3_666 ?
I004 Au02 I005 88.14(5) . 3_666 ?
I004 Au02 I005 91.86(5) . . ?
I005 Au02 I005 180.0 3_666 . ?
Au01 I003 Rb06 102.54(6) . 4_565 ?
Au01 I003 Rb06 92.23(5) . . ?
Au01 I003 Rb06 89.49(5) . 2 ?
Rb06 I003 Rb06 92.64(4) . 2 ?
Rb06 I003 Rb06 153.84(5) . 4_565 ?
Rb06 I003 Rb06 108.77(6) 4_565 2 ?
Au02 I004 Rb06 88.53(5) . 2 ?
Au02 I004 Rb06 105.77(6) . 4_566 ?
Au02 I004 Rb06 90.82(5) . . ?
Rb06 I004 Rb06 91.75(5) 2 . ?
Rb06 I004 Rb06 153.39(5) 4_566 . ?
Rb06 I004 Rb06 108.98(6) 2 4_566 ?
Au01 I005 Au02 163.30(7) . . ?
Au01 I005 Rb06 102.53(7) . 2_655 ?
Au01 I005 Rb06 87.79(6) . 2 ?
Au01 I005 Rb06 90.20(6) . . ?
Au02 I005 Rb06 81.84(5) . . ?
Au02 I005 Rb06 94.13(5) . 2_655 ?
Au02 I005 Rb06 77.65(5) . 2 ?
Rb06 I005 Rb06 113.86(7) 2_655 . ?
Rb06 I005 Rb06 153.33(8) 2_655 2 ?
Rb06 I005 Rb06 90.32(5) . 2 ?
I003 Rb06 I003 137.17(7) . 4_666 ?
I003 Rb06 I003 132.98(7) . 2_545 ?
I003 Rb06 I003 71.23(6) 4_666 2_545 ?
I003 Rb06 I004 66.10(5) . 4_665 ?
I003 Rb06 I004 64.25(5) 4_666 . ?
I003 Rb06 I004 86.80(6) . . ?
I003 Rb06 I004 115.14(7) 4_666 4_665 ?
I003 Rb06 I004 74.62(5) 2_545 . ?
I003 Rb06 I004 146.94(8) 2_545 4_665 ?
I003 Rb06 I004 74.64(5) . 2_545 ?
I003 Rb06 I005 59.20(5) . . ?
I003 Rb06 I005 74.58(5) . 2_545 ?
I003 Rb06 I005 58.42(5) 2_545 2_545 ?
I003 Rb06 I005 79.77(6) 4_666 . ?
I003 Rb06 I005 116.63(7) 4_666 2_545 ?
I003 Rb06 I005 138.61(8) 2_545 . ?
I003 Rb06 I005 128.31(8) . 2_645 ?
I004 Rb06 I003 87.49(6) 2_545 2_545 ?
I004 Rb06 I003 148.12(8) 2_545 4_666 ?
I004 Rb06 I004 71.02(6) 2_545 4_665 ?
I004 Rb06 I004 138.27(7) 4_665 . ?
I004 Rb06 I004 133.51(7) 2_545 . ?
I004 Rb06 I005 103.10(7) 2_545 2_645 ?
I004 Rb06 I005 67.18(5) . 2_545 ?
I004 Rb06 I005 66.88(5) 2_545 2_545 ?
I004 Rb06 I005 129.56(7) 2_545 . ?
I004 Rb06 I005 128.16(7) 4_665 2_545 ?
I005 Rb06 I003 58.58(5) 2_645 4_666 ?
I005 Rb06 I003 97.75(7) 2_645 2_545 ?
I005 Rb06 I004 66.31(5) . . ?
I005 Rb06 I004 72.50(6) . 4_665 ?
I005 Rb06 I004 121.38(7) 2_645 . ?
I005 Rb06 I004 64.73(5) 2_645 4_665 ?
I005 Rb06 I005 114.31(7) . 2_545 ?
I005 Rb06 I005 153.33(8) 2_645 2_545 ?
I005 Rb06 I005 91.34(6) 2_645 . ?

_shelx_res_file                  
;
TITL p21overn_a.res in P2(1)/n
    p21overn.res
    created by SHELXL-2018/3 at 11:10:15 on 25-Aug-2025
REM Old TITL p21overn in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.259, Rweak 0.008, Alpha 0.017
REM <I/s> 0.760 for 114 systematic absences, Orientation as input
REM Formula found by SHELXT: Rb I3 Au
CELL 0.71073 7.4837 9.1874 11.7223 90 91.347 90
ZERR 4 0.0006 0.0008 0.0009 0 0.003 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC Au I Rb
UNIT 4 12 4

L.S. 4
PLAN  8 0 0
SIZE 0.15 0.15 0.4
TEMP -73.15
CONF
list 4
MORE -1
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 1 2
OMIT 0 50
REM <olex2.extras>
REM <HklSrc "%.\\spherical.hkl">
REM </olex2.extras>

WGHT    0.118100   17.743702
BASF   0.01482
FVAR       0.10076
AU01  1    0.500000    0.500000    0.000000    10.50000    0.05091    0.04184 =
         0.04927    0.00061   -0.00183   -0.00176
AU02  1    0.500000    0.500000    0.500000    10.50000    0.05578    0.04568 =
         0.05707   -0.00063   -0.00006   -0.00403
I003  2    0.214788    0.335721    0.027310    11.00000    0.05495    0.05038 =
         0.06146    0.00405   -0.00316   -0.00526
I004  2    0.218166    0.340775    0.475608    11.00000    0.05868    0.04804 =
         0.06224   -0.00211    0.00139   -0.00623
I005  2    0.554422    0.513445    0.224386    11.00000    0.06314    0.06316 =
         0.04896   -0.00074   -0.00348   -0.00424
RB06  3    0.451184    0.103993    0.249372    11.00000    0.06273    0.06202 =
         0.06286    0.00237   -0.00267   -0.00165
HKLF 4




REM  p21overn_a.res in P2(1)/n
REM wR2 = 0.2033, GooF = S = 1.066, Restrained GooF = 1.066 for all data
REM R1 = 0.0732 for 1288 Fo > 4sig(Fo) and 0.0761 for all 1412 data
REM 50 parameters refined using 0 restraints

END

WGHT      0.1181     17.7376

REM Highest difference peak  4.131,  deepest hole -3.171,  1-sigma level  0.628
Q1    1   0.3717  0.5049 -0.0100  11.00000  0.05    4.13
Q2    1   0.3660  0.4948  0.4907  11.00000  0.05    3.92
Q3    1   0.3434  0.3418  0.0337  11.00000  0.05    3.14
Q4    1   0.5541  0.5134  0.3102  11.00000  0.05    2.91
Q5    1   0.3397  0.3340  0.4828  11.00000  0.05    2.67
Q6    1   0.6814  0.5183  0.2305  11.00000  0.05    2.63
Q7    1   0.0904  0.3358  0.4756  11.00000  0.05    2.55
Q8    1   0.4151  0.5098  0.2054  11.00000  0.05    2.21
;
_shelx_res_checksum              31324
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9852(17)
2 0.0148(17)

# start Validation Reply Form
_vrf_RINTA01_p21overn            
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: There is a serious twinning phenomenon in the crystal.
;
_vrf_PLAT020_p21overn            
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.290 Report
RESPONSE: There is a serious twinning phenomenon in the crystal.
;
# end Validation Reply Form
