# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_aspbicn2
_database_code_depnum_ccdc_archive 'CCDC 2211751'
loop_
_audit_author_name
_audit_author_address
'Markus Stroebele'
;University of Tuebingen
Germany
;
_audit_update_record             
;
2022-10-07 deposited with the CCDC.	2024-03-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 I15 N20 Pb17.50'
_chemical_formula_weight         5929.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   10.71440(10)
_cell_length_b                   10.71440(10)
_cell_length_c                   29.4426(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2927.13(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    6.728
_exptl_crystal_F_000             4860
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.073
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.006
_exptl_absorpt_coefficient_mu    58.057
_shelx_estimated_absorpt_T_min   0.101
_shelx_estimated_absorpt_T_max   0.722
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            130367
_diffrn_reflns_av_unetI/netI     0.0079
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.195
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1750
_reflns_number_gt                1698
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0102P)²+68.3982P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1750
_refine_ls_number_parameters     71
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0212
_refine_ls_wR_factor_ref         0.0435
_refine_ls_wR_factor_gt          0.0432
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 -0.21139(2) 0.21139(2) 0.67292(2) 0.01309(6) Uani 1 2 d S T P . .
Pb2 Pb -0.666667 -0.333333 0.67125(2) 0.02010(11) Uani 1 6 d S T P . .
Pb3 Pb -0.41586(3) -0.20793(2) 0.56014(2) 0.01211(6) Uani 1 2 d S T P . .
N1 N -0.5693(3) -0.1387(7) 0.61111(19) 0.0086(10) Uani 1 2 d S T P . .
N2 N -0.4400(4) 0.1201(7) 0.6302(2) 0.0109(11) Uani 1 2 d S T P . .
N3 N -0.5655(4) -0.1309(8) 0.5095(2) 0.0150(12) Uani 1 2 d S T P . .
N4 N -0.333333 0.333333 0.7089(4) 0.0092(18) Uani 1 6 d S T P . .
C1 C -0.5048(4) -0.0095(8) 0.6214(2) 0.0079(11) Uani 1 2 d S T P . .
C2 C -0.500000 0.000000 0.500000 0.0111(18) Uani 1 4 d S T P . .
C3 C -0.333333 0.333333 0.750000 0.010(3) Uani 1 12 d S T P . .
Pb4 Pb -0.333333 0.333333 0.55141(2) 0.01806(11) Uani 1 6 d S T P . .
Pb5 Pb 0.000000 0.000000 0.61669(2) 0.00983(11) Uani 0.75 6 d S T P . .
I1 I -0.14828(3) 0.14828(3) 0.55761(2) 0.01136(9) Uani 1 2 d S T P . .
I2 I 0.13801(3) -0.13801(3) 0.67313(2) 0.01382(9) Uani 1 2 d S T P . .
I3 I -0.51216(4) -0.02431(8) 0.750000 0.01394(13) Uani 1 4 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
Pb1 0.01239(9) 0.01239(9) 0.01520(12) 0.00163(5) -0.00163(5) 0.00673(10)
Pb2 0.02539(17) 0.02539(17) 0.0095(2) 0.000 0.000 0.01269(8)
Pb3 0.01262(12) 0.01015(9) 0.01438(12) 0.00092(5) 0.00183(10) 0.00631(6)
N1 0.0096(18) 0.007(3) 0.008(2) 0.001(2) 0.0004(10) 0.0036(13)
N2 0.0087(18) 0.013(3) 0.013(3) -0.001(2) -0.0004(11) 0.0063(14)
N3 0.014(2) 0.019(3) 0.014(3) -0.002(3) -0.0008(13) 0.0097(16)
N4 0.010(3) 0.010(3) 0.007(4) 0.000 0.000 0.0051(14)
C1 0.0071(19) 0.010(3) 0.008(3) -0.001(2) -0.0007(12) 0.0050(15)
C2 0.008(3) 0.024(5) 0.006(4) -0.003(4) -0.0014(19) 0.012(3)
C3 0.009(4) 0.009(4) 0.013(7) 0.000 0.000 0.004(2)
Pb4 0.01905(15) 0.01905(15) 0.0161(2) 0.000 0.000 0.00953(8)
Pb5 0.00811(15) 0.00811(15) 0.0133(3) 0.000 0.000 0.00405(7)
I1 0.01025(14) 0.01025(14) 0.01263(19) 0.00112(8) -0.00112(8) 0.00442(16)
I2 0.00965(14) 0.00965(14) 0.0208(2) 0.00171(9) -0.00171(9) 0.00377(16)
I3 0.0150(2) 0.0128(3) 0.0133(3) 0.000 0.000 0.00641(15)

_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 N2 2.478(4) . ?
Pb1 N2 2.478(4) 2_565 ?
Pb1 N4 2.499(4) . ?
Pb2 N1 2.529(6) . ?
Pb2 N1 2.529(6) 2_455 ?
Pb2 N1 2.529(6) 3_445 ?
Pb3 N1 2.594(4) 3_445 ?
Pb3 N1 2.594(4) . ?
Pb3 N3 2.606(4) . ?
Pb3 N3 2.606(4) 3_445 ?
N1 C1 1.236(9) . ?
N2 C1 1.230(9) . ?
N3 C2 1.247(7) . ?
N3 Pb4 2.597(7) 13_456 ?
N4 C3 1.209(10) . ?
Pb5 I2 3.0528(6) 2 ?
Pb5 I2 3.0528(6) 3 ?
Pb5 I2 3.0529(6) . ?
Pb5 I1 3.2554(6) . ?
Pb5 I1 3.2555(6) 2 ?
Pb5 I1 3.2555(6) 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
N2 Pb1 N2 87.5(3) . 2_565 ?
N2 Pb1 N4 75.52(19) . . ?
N2 Pb1 N4 75.52(19) 2_565 . ?
N1 Pb2 N1 76.4(2) . 2_455 ?
N1 Pb2 N1 76.4(2) . 3_445 ?
N1 Pb2 N1 76.4(2) 2_455 3_445 ?
N1 Pb3 N1 74.2(3) 3_445 . ?
N1 Pb3 N3 114.50(18) 3_445 . ?
N1 Pb3 N3 70.24(16) . . ?
N1 Pb3 N3 70.24(16) 3_445 3_445 ?
N1 Pb3 N3 114.50(18) . 3_445 ?
N3 Pb3 N3 77.2(3) . 3_445 ?
C1 N1 Pb2 121.3(5) . . ?
C1 N1 Pb3 112.5(3) . 2_455 ?
Pb2 N1 Pb3 103.19(16) . 2_455 ?
C1 N1 Pb3 112.5(3) . . ?
Pb2 N1 Pb3 103.19(16) . . ?
Pb3 N1 Pb3 102.0(2) 2_455 . ?
C1 N2 Pb1 116.2(3) . . ?
C1 N2 Pb1 116.2(3) . 3_455 ?
Pb1 N2 Pb1 104.5(2) . 3_455 ?
C2 N3 Pb4 123.3(4) . 13_456 ?
C2 N3 Pb3 113.3(2) . . ?
Pb4 N3 Pb3 101.34(19) 13_456 . ?
C2 N3 Pb3 113.3(2) . 2_455 ?
Pb4 N3 Pb3 101.34(19) 13_456 2_455 ?
Pb3 N3 Pb3 101.3(2) . 2_455 ?
C3 N4 Pb1 115.1(2) . . ?
C3 N4 Pb1 115.1(2) . 3_455 ?
Pb1 N4 Pb1 103.3(3) . 3_455 ?
C3 N4 Pb1 115.1(2) . 2_565 ?
Pb1 N4 Pb1 103.3(3) . 2_565 ?
Pb1 N4 Pb1 103.3(3) 3_455 2_565 ?
N2 C1 N1 177.9(7) . . ?
N3 C2 N3 180.0 13_456 . ?
N4 C3 N4 180.0 . 16_557 ?
N3 Pb4 N3 77.5(2) 13_456 14_556 ?
N3 Pb4 N3 77.5(2) 13_456 15_566 ?
N3 Pb4 N3 77.5(2) 14_556 15_566 ?
I2 Pb5 I2 93.193(19) 2 3 ?
I2 Pb5 I2 93.192(19) 2 . ?
I2 Pb5 I2 93.192(19) 3 . ?
I2 Pb5 I1 86.345(9) 2 . ?
I2 Pb5 I1 86.345(9) 3 . ?
I2 Pb5 I1 179.32(2) . . ?
I2 Pb5 I1 179.33(2) 2 2 ?
I2 Pb5 I1 86.345(8) 3 2 ?
I2 Pb5 I1 86.345(9) . 2 ?
I1 Pb5 I1 94.114(17) . 2 ?
I2 Pb5 I1 86.345(9) 2 3 ?
I2 Pb5 I1 179.33(2) 3 3 ?
I2 Pb5 I1 86.345(9) . 3 ?
I1 Pb5 I1 94.114(17) . 3 ?
I1 Pb5 I1 94.112(17) 2 3 ?

_refine_diff_density_max         3.882
_refine_diff_density_min         -3.547
_refine_diff_density_rms         0.216

_shelx_res_file                  
;
TITL aspbicn2_a.res in P6(3)/mmc
    aspbicn2.res
    created by SHELXL-2018/3 at 21:36:51 on 07-Oct-2022
REM Old TITL aspbicn2_a.res in P-6m2
REM SHELXT solution in P6(3)/mmc: R1 0.205, Rweak 0.003, Alpha 0.015
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: I17 Pb16
CELL 0.71073 10.7144 10.7144 29.4426 90 90 120
ZERR 2 0.0001 0.0001 0.0004 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,+X,0.5+Z
SYMM +Y,+X,-Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C I N Pb
UNIT 20 30 40 35

L.S. 4
PLAN  1
SIZE 0.006 0.055 0.073
TEMP -123
list 4
fmap 2
acta
SHEL 99 0.7
REM <olex2.extras>
REM <HklSrc "%.\\ASPbICN2.hkl">
REM </olex2.extras>

WGHT    0.010200   68.398201
FVAR       0.04473
PB1   4   -0.211393    0.211393    0.672924    10.50000    0.01239    0.01239 =
         0.01520    0.00163   -0.00163    0.00673
PB2   4   -0.666667   -0.333333    0.671248    10.16667    0.02539    0.02539 =
         0.00951    0.00000    0.00000    0.01269
PB3   4   -0.415862   -0.207931    0.560137    10.50000    0.01262    0.01015 =
         0.01438    0.00092    0.00183    0.00631
N1    3   -0.569347   -0.138695    0.611108    10.50000    0.00957    0.00730 =
         0.00809    0.00072    0.00036    0.00365
N2    3   -0.439962    0.120076    0.630203    10.50000    0.00873    0.01253 =
         0.01277   -0.00078   -0.00039    0.00627
N3    3   -0.565462   -0.130924    0.509537    10.50000    0.01377    0.01948 =
         0.01363   -0.00152   -0.00076    0.00974
N4    3   -0.333333    0.333333    0.708938    10.16667    0.01021    0.01021 =
         0.00727    0.00000    0.00000    0.00510
C1    1   -0.504772   -0.009544    0.621429    10.50000    0.00709    0.01005 =
         0.00753   -0.00142   -0.00071    0.00503
C2    1   -0.500000    0.000000    0.500000    10.25000    0.00809    0.02443 =
         0.00615   -0.00286   -0.00143    0.01222
C3    1   -0.333333    0.333333    0.750000    10.08333    0.00890    0.00890 =
         0.01300    0.00000    0.00000    0.00445
PB4   4   -0.333333    0.333333    0.551409    10.16667    0.01905    0.01905 =
         0.01607    0.00000    0.00000    0.00953
PB5   4    0.000000    0.000000    0.616692    10.12500    0.00811    0.00811 =
         0.01328    0.00000    0.00000    0.00405
I1    2   -0.148279    0.148279    0.557610    10.50000    0.01025    0.01025 =
         0.01263    0.00112   -0.00112    0.00442
I2    2    0.138007   -0.138007    0.673127    10.50000    0.00965    0.00965 =
         0.02076    0.00171   -0.00171    0.00377
I3    2   -0.512156   -0.024312    0.750000    10.25000    0.01498    0.01282 =
         0.01329    0.00000    0.00000    0.00641
HKLF 4




REM  aspbicn2_a.res in P6(3)/mmc
REM wR2 = 0.0435, GooF = S = 1.113, Restrained GooF = 1.113 for all data
REM R1 = 0.0212 for 1698 Fo > 4sig(Fo) and 0.0220 for all 1750 data
REM 71 parameters refined using 0 restraints

END

WGHT      0.0102     68.3639

REM Highest difference peak  3.882,  deepest hole -3.547,  1-sigma level  0.216
Q1    1  -0.7028 -0.4057  0.6779  10.50000  0.05    3.88
;
_shelx_res_checksum              21290
