# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2022

####################################################################### 
# 
# 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_(M2pda)Pb2I6-298K
_database_code_depnum_ccdc_archive 'CCDC 2183780'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2022-07-04 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_audit_creation_date             2022-05-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(I24 Pb8), C5 N2'
_chemical_formula_sum            'C5 H12.58 I6 N2 Pb2'
_chemical_formula_weight         1276.53
_chemical_melting_point          ?
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'
H H 0.0000 0.0000 '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'

_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      orthorhombic
_space_group_IT_number           55
_space_group_name_H-M_alt        'P b a m'
_space_group_name_Hall           '-P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'

_cell_length_a                   9.2222(5)
_cell_length_b                   17.7717(7)
_cell_length_c                   6.4398(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1055.45(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2727
_cell_measurement_temperature    297.01(10)
_cell_measurement_theta_max      29.6030
_cell_measurement_theta_min      2.2570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    24.688
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.017
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1077
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.829
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5319
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.105
_diffrn_reflns_theta_min         2.292
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.829
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -15.00  30.00   0.50    1.00    --  -11.22 -99.00 120.00   90
  2  ω     -3.00  23.00   0.50    1.00    --   10.60 -99.00 -60.00   52
  3  ω    -18.00  25.00   0.50    1.00    --  -11.22 -99.00 -90.00   86
  4  ω    -77.00   6.00   0.50    1.00    --  -11.22 -20.00-176.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0005486000
_diffrn_orient_matrix_UB_12      -0.0570886000
_diffrn_orient_matrix_UB_13      -0.0736774000
_diffrn_orient_matrix_UB_21      -0.0105809000
_diffrn_orient_matrix_UB_22      -0.0494646000
_diffrn_orient_matrix_UB_23      0.0792358000
_diffrn_orient_matrix_UB_31      -0.0384854000
_diffrn_orient_matrix_UB_32      0.0143662000
_diffrn_orient_matrix_UB_33      -0.0206984000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1140
_reflns_number_total             1395
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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         1.657
_refine_diff_density_min         -3.353
_refine_diff_density_rms         0.800
_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     56
_refine_ls_number_reflns         1395
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0508
_refine_ls_restrained_S_all      1.063
_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)+(0.0809P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1273
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N1B-C2 = N1B-C3 = N1A-C3 = N1A-C2
 1.47 with sigma of 0.01
 C2-C1
 1.53 with sigma of 0.01
2. Rigid body (RIGU) restrains
 C3, N1B, N1A, C2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: N1B(0.25) N1A(0.25) C2(0.5)
;
_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
Pb01 Pb 0.43603(5) 0.37189(2) 0.500000 0.0365(2) Uani 1 2 d S T P . .
I002 I 0.72729(10) 0.46896(4) 0.500000 0.0399(3) Uani 1 2 d S T P . .
I003 I 0.43100(12) 0.38012(6) 0.000000 0.0563(3) Uani 1 2 d S T P . .
I004 I 0.12435(12) 0.28380(6) 0.500000 0.0557(3) Uani 1 2 d S T P . .
C3 C 0.840(3) 0.3273(9) 1.000000 0.085(6) Uani 1 2 d DS TU P . .
N1B N 0.866(3) 0.4088(10) 1.000000 0.059(5) Uani 0.5 2 d DS TU P A 1
N1A N 0.995(3) 0.3447(12) 1.000000 0.086(8) Uani 0.5 2 d DS TU P A 2
C2 C 1.015(2) 0.4208(7) 0.920(4) 0.091(8) Uani 0.5 1 d D U . . .
C1 C 1.000000 0.500000 1.000000 0.150(16) Uani 1 4 d DS TU P A .

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
Pb01 0.0366(3) 0.0380(3) 0.0349(3) 0.000 0.000 0.00026(17)
I002 0.0333(5) 0.0420(4) 0.0444(5) 0.000 0.000 0.0022(3)
I003 0.0679(9) 0.0714(7) 0.0297(5) 0.000 0.000 -0.0023(5)
I004 0.0520(7) 0.0576(6) 0.0576(6) 0.000 0.000 -0.0213(4)
C3 0.097(14) 0.077(10) 0.082(13) 0.000 0.000 0.016(9)
N1B 0.063(13) 0.078(11) 0.035(11) 0.000 0.000 0.025(10)
N1A 0.092(15) 0.089(13) 0.08(2) 0.000 0.000 0.030(13)
C2 0.053(13) 0.110(13) 0.11(2) 0.027(11) -0.004(12) 0.018(10)
C1 0.20(4) 0.109(15) 0.14(3) 0.000 0.000 -0.025(19)

_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
Pb01 I002 3.1923(10) . ?
Pb01 I002 3.2043(9) 5_666 ?
Pb01 I003 3.22355(16) . ?
Pb01 I003 3.22355(16) 1_556 ?
Pb01 I004 3.2668(10) 7_665 ?
Pb01 I004 3.2730(10) . ?
C3 N1B 1.468(10) . ?
C3 N1A 1.458(10) . ?
N1B C2 1.483(10) . ?
N1B C2 1.483(10) 6_557 ?
N1A C2 1.460(10) . ?
N1A C2 1.460(10) 6_557 ?
C2 C2 1.03(5) 6_557 ?
C2 C1 1.505(9) . ?

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
I002 Pb01 I002 85.33(3) . 5_666 ?
I002 Pb01 I003 87.32(2) 5_666 . ?
I002 Pb01 I003 89.29(2) . . ?
I002 Pb01 I003 87.32(2) 5_666 1_556 ?
I002 Pb01 I003 89.29(2) . 1_556 ?
I002 Pb01 I004 175.92(3) 5_666 7_665 ?
I002 Pb01 I004 175.86(3) . . ?
I002 Pb01 I004 90.54(3) 5_666 . ?
I002 Pb01 I004 90.60(3) . 7_665 ?
I003 Pb01 I003 174.55(4) 1_556 . ?
I003 Pb01 I004 90.52(2) . . ?
I003 Pb01 I004 92.64(2) 1_556 7_665 ?
I003 Pb01 I004 92.64(2) . 7_665 ?
I003 Pb01 I004 90.52(2) 1_556 . ?
I004 Pb01 I004 93.542(13) 7_665 . ?
Pb01 I002 Pb01 94.68(3) . 5_666 ?
Pb01 I003 Pb01 174.55(4) . 1_554 ?
Pb01 I004 Pb01 150.69(4) 7_565 . ?
C3 N1B C2 107.1(16) . 6_557 ?
C3 N1B C2 107.1(16) . . ?
C2 N1B C2 41(2) 6_557 . ?
C3 N1A C2 108.9(17) . 6_557 ?
C3 N1A C2 108.9(17) . . ?
C2 N1A C2 41(2) . 6_557 ?
N1B C2 C1 85.9(11) . . ?
N1A C2 C1 137.0(19) . . ?
C2 C2 N1B 69.6(10) 6_557 . ?
C2 C2 N1A 69.3(10) 6_557 . ?
C2 C2 C1 69.9(10) 6_557 . ?
C2 C1 C2 180.0 5_767 . ?
C2 C1 C2 139.8(19) 2_765 . ?
C2 C1 C2 40.2(19) 5_767 2_765 ?
C2 C1 C2 139.8(19) 5_767 6_557 ?
C2 C1 C2 180.0 6_557 2_765 ?
C2 C1 C2 40.2(19) 6_557 . ?

_shelx_res_file                  
;
TITL 111_a.res in Pbam
    fcc_083_03_2_298k.res
    created by SHELXL-2018/3 at 18:53:03 on 17-May-2022
REM Old TITL 111 in Pbam
REM SHELXT solution in Pbam: R1 0.123, Rweak 0.005, Alpha 0.017
REM <I/s> 0.866 for 115 systematic absences, Orientation as input
REM Formula found by SHELXT: I3 Pb
CELL 0.71073 9.2222 17.7717 6.4398 90 90 90
ZERR 2 0.0005 0.0007 0.0003 0 0 0
LATT 1
SYMM -X,-Y,+Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H I N Pb
UNIT 10 25.16 12 4 4
DFIX 1.47 0.01 N1B C2 N1B C3 N1A C3 N1A C2
DFIX 1.53 0.01 C2 C1
RIGU C3 N1B N1A C2 C1

L.S. 30 0 0
PLAN  1
BOND
list 4
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\111.hkl">
REM </olex2.extras>

WGHT    0.080900
FVAR       0.17595
PB01  5    0.436030    0.371891    0.500000    10.50000    0.03664    0.03800 =
         0.03490    0.00000    0.00000    0.00026
I002  3    0.727288    0.468963    0.500000    10.50000    0.03334    0.04201 =
         0.04439    0.00000    0.00000    0.00217
I003  3    0.431001    0.380116    0.000000    10.50000    0.06792    0.07137 =
         0.02968    0.00000    0.00000   -0.00231
I004  3    0.124347    0.283804    0.500000    10.50000    0.05205    0.05760 =
         0.05759    0.00000    0.00000   -0.02134
C3    1    0.840156    0.327271    1.000000    10.50000    0.09709    0.07666 =
         0.08238    0.00000    0.00000    0.01626
PART 1
N1B   4    0.866227    0.408774    1.000000    10.25000    0.06252    0.07782 =
         0.03539    0.00000    0.00000    0.02511
PART 0
PART 2
N1A   4    0.994654    0.344734    1.000000    10.25000    0.09188    0.08883 =
         0.07689    0.00000    0.00000    0.03021
PART 0
C2    1    1.015162    0.420845    0.919689    10.50000    0.05316    0.10966 =
         0.10944    0.02736   -0.00366    0.01788
C1    1    1.000000    0.500000    1.000000    10.25000    0.20121    0.10855 =
         0.14071    0.00000    0.00000   -0.02457
HKLF 4




REM  111_a.res in Pbam
REM wR2 = 0.1273, GooF = S = 1.066, Restrained GooF = 1.063 for all data
REM R1 = 0.0508 for 1140 Fo > 4sig(Fo) and 0.0612 for all 1395 data
REM 56 parameters refined using 29 restraints

END

WGHT      0.0809      0.0000

REM Highest difference peak  1.657,  deepest hole -3.353,  1-sigma level  0.800
Q1    1   0.4304  0.3763  0.2972  11.00000  0.05    1.66
;
_shelx_res_checksum              53649
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.608
_oxdiff_exptl_absorpt_empirical_full_min 0.170
####################################################################### 
# 
# 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_(M2pda)Pb2I6-100K
_database_code_depnum_ccdc_archive 'CCDC 2183781'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2022-07-04 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_audit_creation_date             2022-07-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(I12 Pb4), C5 H16 N2'
_chemical_formula_sum            'C5 H16 I6 N2 Pb2'
_chemical_formula_weight         1279.98
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
H H 0.0000 0.0000 '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'

_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      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.1348(10)
_cell_length_b                   17.6663(19)
_cell_length_c                   6.4266(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1037.1(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1293
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.3460
_cell_measurement_theta_min      3.1880
_shelx_estimated_absorpt_T_max   0.238
_shelx_estimated_absorpt_T_min   0.152
_exptl_absorpt_coefficient_mu    25.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.099
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3562
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.788
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.346
_diffrn_reflns_theta_min         2.306
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -28.00  48.00   1.00    3.00    --  -11.27  77.00  90.00   76
  2  ω     35.00  88.00   1.00    3.00    --   11.90 178.00 -30.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0288180000
_diffrn_orient_matrix_UB_12      -0.0219872000
_diffrn_orient_matrix_UB_13      -0.0370786000
_diffrn_orient_matrix_UB_21      0.0846356000
_diffrn_orient_matrix_UB_22      -0.0499046000
_diffrn_orient_matrix_UB_23      -0.0007326000
_diffrn_orient_matrix_UB_31      -0.0647908000
_diffrn_orient_matrix_UB_32      -0.0551420000
_diffrn_orient_matrix_UB_33      0.0154560000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.548
_reflns_Friedel_fraction_full    0.908
_reflns_Friedel_fraction_max     0.670
_reflns_number_gt                1966
_reflns_number_total             2249
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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         6.419
_refine_diff_density_min         -4.401
_refine_diff_density_rms         0.607
_refine_ls_abs_structure_details 
;
 Flack x determined using 537 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.48(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         2249
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0709
_refine_ls_restrained_S_all      1.098
_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)+(0.0052P)²+135.8706P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1421
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-N1
 1.47 with sigma of 0.01
 N1-C2
 1.47 with sigma of 0.01
 C2-C3
 1.53 with sigma of 0.01
 N1-C1 \\sim N1-C2
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2 \\sim C3: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
4. Rigid body (RIGU) restrains
 N1, C1, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H3A(0.5) H3B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
6.b Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
;
_atom_sites_solution_hydrogens   geom
_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 0.56326(5) 0.62827(2) 0.50666(10) 0.01550(10) Uani 1 1 d . . . . .
I1 I 0.26924(8) 0.53207(5) 0.52171(17) 0.0185(2) Uani 1 1 d . . . . .
I2 I 0.56366(9) 0.61844(6) 0.02664(14) 0.0256(2) Uani 1 1 d . . . . .
I3 I 0.38073(9) 0.78566(5) 0.5014(2) 0.0266(2) Uani 1 1 d . . . . .
N1 N 0.0044(4) 0.64430(19) 1.0230(13) 0.060(3) Uani 1 1 d D U . . .
H1A H -0.022676 0.641362 1.159060 0.072 Uiso 1 1 calc R . . . .
H1B H -0.054401 0.679117 0.960459 0.072 Uiso 1 1 calc R . . . .
C1 C 0.1570(4) 0.6710(5) 1.012(4) 0.0424(17) Uani 1 1 d D U . . .
H1C H 0.160294 0.719781 0.939772 0.064 Uiso 1 1 calc GR . . . .
H1D H 0.216256 0.633951 0.935940 0.064 Uiso 1 1 calc GR . . . .
H1E H 0.195883 0.676920 1.153240 0.064 Uiso 1 1 calc GR . . . .
C2 C -0.0202(16) 0.5703(2) 0.9247(10) 0.058(3) Uani 1 1 d D U . . .
H2A H 0.046864 0.566145 0.804241 0.070 Uiso 1 1 calc R . . . .
H2B H -0.121360 0.569663 0.869273 0.070 Uiso 1 1 calc R . . . .
C3 C 0.000000 0.500000 1.0592(14) 0.064(6) Uani 1 2 d DS TU P . .
H3A H -0.086749 0.493323 1.149679 0.077 Uiso 0.5 1 calc R . . . .
H3B H 0.086749 0.506677 1.149679 0.077 Uiso 0.5 1 calc R . . . .

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 0.00649(16) 0.02047(18) 0.01953(19) -0.0006(3) -0.0004(2) 0.00078(16)
I1 0.0072(3) 0.0230(4) 0.0253(4) 0.0043(5) 0.0002(4) 0.0023(3)
I2 0.0140(3) 0.0506(5) 0.0122(3) -0.0024(5) 0.0005(4) -0.0066(4)
I3 0.0150(3) 0.0305(4) 0.0343(5) 0.0019(6) 0.0006(5) 0.0115(3)
N1 0.047(4) 0.051(4) 0.083(9) 0.032(4) -0.011(7) 0.002(4)
C1 0.041(2) 0.046(3) 0.040(3) 0.000(3) 0.001(2) 0.004(2)
C2 0.026(7) 0.052(3) 0.097(8) 0.019(3) 0.004(7) 0.003(4)
C3 0.088(15) 0.043(4) 0.063(10) 0.000 0.000 0.006(7)

_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 I1 3.1797(9) . ?
Pb1 I1 3.2210(9) 2_665 ?
Pb1 I2 3.3463(12) 1_556 ?
Pb1 I2 3.0897(12) . ?
Pb1 I3 3.2422(10) . ?
Pb1 I3 3.2750(10) 4_566 ?
N1 C1 1.473(5) . ?
N1 C2 1.469(6) . ?
C2 C3 1.525(6) . ?

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
I1 Pb1 I1 86.00(2) . 2_665 ?
I1 Pb1 I2 86.72(3) . 1_556 ?
I1 Pb1 I2 85.63(3) 2_665 1_556 ?
I1 Pb1 I3 175.27(3) . 4_566 ?
I1 Pb1 I3 91.39(2) . . ?
I1 Pb1 I3 89.32(2) 2_665 4_566 ?
I1 Pb1 I3 177.19(3) 2_665 . ?
I2 Pb1 I1 88.85(3) . 2_665 ?
I2 Pb1 I1 90.08(3) . . ?
I2 Pb1 I2 173.80(4) . 1_556 ?
I2 Pb1 I3 92.20(3) . . ?
I2 Pb1 I3 90.53(3) . 4_566 ?
I3 Pb1 I2 92.23(3) 4_566 1_556 ?
I3 Pb1 I2 93.18(3) . 1_556 ?
I3 Pb1 I3 93.270(16) . 4_566 ?
Pb1 I1 Pb1 93.89(2) . 2_665 ?
Pb1 I2 Pb1 173.80(4) . 1_554 ?
Pb1 I3 Pb1 148.62(3) . 4_466 ?
C2 N1 C1 114.1(9) . . ?
N1 C2 C3 117.5(6) . . ?
C2 C3 C2 110.9(7) . 2_565 ?

_shelx_res_file                  
;
TITL 1_a.res in P2(1)2(1)2
    u9.res
    created by SHELXL-2018/3 at 19:50:36 on 04-Jul-2022
REM Old TITL 1_a.res in Pbam
REM SHELXT solution in P2(1)2(1)2: R1 0.129, Rweak 0.014, Alpha 0.007
REM <I/s> 1.014 for 16 systematic absences, Orientation as input
REM Flack x = 0.493 ( 0.019 ) from 580 Parsons' quotients
REM Formula found by SHELXT: N I3 Pb
CELL 0.71073 9.1348 17.6663 6.4266 90 90 90
ZERR 2 0.001 0.0019 0.001 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H I N Pb
UNIT 10 32 12 4 4
DFIX 1.47 0.01 C1 N1
DFIX 1.47 0.01 N1 C2
DFIX 1.53 0.01 C2 C3
SADI 0.01 N1 C1 N1 C2
SIMU 0.04 0.08 1.7 N1 > C3
RIGU N1 > C3
ISOR 0.01 0.005 C1

L.S. 50
PLAN  1
SIZE 0.08 0.1 0.12
TEMP -173.15(10)
BOND
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\u9.hkl">
REM </olex2.extras>

WGHT    0.005200  135.870605
FVAR       0.12845
PB1   5    0.563256    0.628270    0.506657    11.00000    0.00649    0.02047 =
         0.01953   -0.00057   -0.00038    0.00078
I1    3    0.269244    0.532073    0.521710    11.00000    0.00720    0.02300 =
         0.02527    0.00427    0.00022    0.00231
I2    3    0.563656    0.618441    0.026642    11.00000    0.01403    0.05059 =
         0.01218   -0.00244    0.00046   -0.00662
I3    3    0.380735    0.785658    0.501374    11.00000    0.01504    0.03049 =
         0.03430    0.00191    0.00057    0.01153
N1    4    0.004367    0.644303    1.023018    11.00000    0.04659    0.05075 =
         0.08295    0.03234   -0.01120    0.00224
AFIX  23
H1A   2   -0.022676    0.641362    1.159060    11.00000   -1.20000
H1B   2   -0.054401    0.679117    0.960459    11.00000   -1.20000
AFIX   0
C1    1    0.156972    0.670970    1.012077    11.00000    0.04142    0.04604 =
         0.03965   -0.00044    0.00149    0.00352
AFIX 137
H1C   2    0.160294    0.719781    0.939772    11.00000   -1.50000
H1D   2    0.216256    0.633951    0.935940    11.00000   -1.50000
H1E   2    0.195883    0.676920    1.153240    11.00000   -1.50000
AFIX   0
C2    1   -0.020240    0.570308    0.924664    11.00000    0.02561    0.05239 =
         0.09660    0.01870    0.00449    0.00290
AFIX  23
H2A   2    0.046864    0.566145    0.804241    11.00000   -1.20000
H2B   2   -0.121360    0.569663    0.869273    11.00000   -1.20000
AFIX   0
C3    1    0.000000    0.500000    1.059183    10.50000    0.08764    0.04261 =
         0.06276    0.00000    0.00000    0.00645
AFIX  23
H3A   2   -0.086749    0.493323    1.149679    10.50000   -1.20000
H3B   2    0.086749    0.506677    1.149679    10.50000   -1.20000
AFIX   0
HKLF 4




REM  1_a.res in P2(1)2(1)2
REM wR2 = 0.1421, GooF = S = 1.107, Restrained GooF = 1.098 for all data
REM R1 = 0.0709 for 1966 Fo > 4sig(Fo) and 0.0800 for all 2249 data
REM 70 parameters refined using 43 restraints

END

WGHT      0.0052    135.8316

REM Highest difference peak  6.419,  deepest hole -4.401,  1-sigma level  0.607
Q1    1   0.5672  0.6236 -0.0989  11.00000  0.05    6.42
;
_shelx_res_checksum              56907
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.578
_oxdiff_exptl_absorpt_empirical_full_min 0.647
# start Validation Reply Form
_vrf_PLAT987_M2pdaPb2I6-100K     
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: Achiral organic cations crystallize in chiral space groups.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_(H2pda)Pb2I6-298K
_database_code_depnum_ccdc_archive 'CCDC 2183783'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2022-07-04 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_audit_creation_date             2022-05-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H7 N, I3 Pb'
_chemical_formula_sum            'C2 H7 I3 N Pb'
_chemical_formula_weight         632.98
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 N1 I1 Pb1'
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'
H H 0.0000 0.0000 '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'

_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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.5066(5)
_cell_length_b                   17.0103(14)
_cell_length_c                   9.2072(7)
_cell_angle_alpha                90
_cell_angle_beta                 92.815(7)
_cell_angle_gamma                90
_cell_volume                     1017.82(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2063
_cell_measurement_temperature    289.0(6)
_cell_measurement_theta_max      29.6900
_cell_measurement_theta_min      2.2146
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    25.599
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.131
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.782
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6884
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.782
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.828
_diffrn_reflns_theta_min         2.395
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      289.0(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.782
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -13.00  14.00   0.50    0.60    --   -6.24 -99.00  60.00   54
  2  ω      5.00  36.00   0.50    0.60    --    5.69 -99.00 120.00   62
  3  ω    -16.00  21.00   0.50    0.60    --   -6.24 -99.00 -90.00   74
  4  ω    -12.00  27.00   0.50    0.60    --    5.69 -99.00-150.00   78
  5  ω    -21.00  49.00   0.50    0.60    --   -6.24  57.00-150.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0886856000
_diffrn_orient_matrix_UB_12      0.0232610000
_diffrn_orient_matrix_UB_13      -0.0101769000
_diffrn_orient_matrix_UB_21      -0.0545994000
_diffrn_orient_matrix_UB_22      0.0340746000
_diffrn_orient_matrix_UB_23      0.0200793000
_diffrn_orient_matrix_UB_31      0.0327630000
_diffrn_orient_matrix_UB_32      -0.0060638000
_diffrn_orient_matrix_UB_33      0.0737471000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1678
_reflns_number_total             2504
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    ?
_refine_diff_density_max         1.342
_refine_diff_density_min         -2.278
_refine_diff_density_rms         0.384
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         2504
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0411
_refine_ls_restrained_S_all      0.952
_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)+(0.0422P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0994
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 N1(H1C,H1D,H1E)
;
_atom_sites_solution_hydrogens   geom
_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
C1 C 0.0556(19) 0.4757(10) 0.4466(12) 0.060(4) Uani 1 1 d . . . . .
H1A H 0.202869 0.481625 0.465061 0.072 Uiso 1 1 calc R . . . .
H1B H 0.021264 0.494323 0.348808 0.072 Uiso 1 1 calc R . . . .
C2 C -0.002(2) 0.3895(11) 0.4580(15) 0.076(5) Uani 1 1 d . . . . .
H2A H 0.048356 0.369341 0.551617 0.091 Uiso 1 1 calc R . . . .
H2B H -0.150584 0.384529 0.452368 0.091 Uiso 1 1 calc R . . . .
I1 I 0.46527(12) 0.53761(4) 0.77313(7) 0.0411(2) Uani 1 1 d . . . . .
I2 I 0.50123(14) 0.28587(5) 0.61778(9) 0.0552(2) Uani 1 1 d . . . . .
I3 I 1.00751(10) 0.36582(5) 0.93583(8) 0.0486(2) Uani 1 1 d . . . . .
N1 N 0.0846(19) 0.3424(9) 0.3417(12) 0.076(4) Uani 1 1 d . . . . .
H1C H -0.000789 0.343574 0.263173 0.114 Uiso 1 1 calc GR . . . .
H1D H 0.101012 0.292987 0.371678 0.114 Uiso 1 1 calc GR . . . .
H1E H 0.205871 0.362227 0.319862 0.114 Uiso 1 1 calc GR . . . .
Pb1 Pb 0.51558(6) 0.37155(2) 0.93186(4) 0.03509(14) 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
C1 0.040(7) 0.102(13) 0.039(7) 0.018(7) 0.010(5) 0.010(8)
C2 0.055(9) 0.120(15) 0.055(8) 0.019(9) 0.023(7) 0.017(9)
I1 0.0511(4) 0.0408(4) 0.0314(4) 0.0004(3) 0.0044(3) -0.0019(3)
I2 0.0653(5) 0.0503(5) 0.0503(4) -0.0205(4) 0.0069(4) -0.0045(4)
I3 0.0266(4) 0.0640(6) 0.0554(5) 0.0037(4) 0.0044(3) -0.0001(3)
N1 0.072(8) 0.104(11) 0.053(7) 0.017(7) 0.005(6) -0.012(8)
Pb1 0.0336(2) 0.0377(3) 0.0343(2) -0.00020(17) 0.00436(16) -0.00092(17)

_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
C1 C1 1.50(2) 3_566 ?
C1 C2 1.52(2) . ?
C2 N1 1.471(19) . ?
I1 Pb1 3.1222(8) 3_667 ?
I1 Pb1 3.1899(9) . ?
I2 Pb1 3.1820(9) 4_565 ?
I2 Pb1 3.2355(9) . ?
I3 Pb1 3.2007(8) . ?
I3 Pb1 3.3092(8) 1_655 ?

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
C1 C1 C2 111.0(14) 3_566 . ?
N1 C2 C1 111.8(11) . . ?
Pb1 I1 Pb1 92.34(2) 3_667 . ?
Pb1 I2 Pb1 149.27(3) 4_565 . ?
Pb1 I3 Pb1 176.34(4) . 1_655 ?
I1 Pb1 I1 87.66(2) 3_667 . ?
I1 Pb1 I2 177.03(3) 3_667 . ?
I1 Pb1 I2 87.10(2) 3_667 4_566 ?
I1 Pb1 I2 89.52(2) . . ?
I1 Pb1 I3 96.44(2) . . ?
I1 Pb1 I3 90.12(2) 3_667 1_455 ?
I1 Pb1 I3 90.46(2) 3_667 . ?
I1 Pb1 I3 87.19(2) . 1_455 ?
I2 Pb1 I1 170.62(2) 4_566 . ?
I2 Pb1 I2 95.823(15) 4_566 . ?
I2 Pb1 I3 85.04(2) 4_566 1_455 ?
I2 Pb1 I3 91.37(3) 4_566 . ?
I2 Pb1 I3 90.67(2) . 1_455 ?
I3 Pb1 I2 88.94(2) . . ?
I3 Pb1 I3 176.34(4) . 1_455 ?

_shelx_res_file                  
;
TITL 1 in P2(1)/c
    ccf-107-01-1.res
    created by SHELXL-2018/3 at 20:15:57 on 15-May-2022
CELL 0.71073 6.5066 17.0103 9.2072 90 92.815 90
ZERR 4 0.0005 0.0014 0.0007 0 0.007 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H I N Pb
UNIT 8 28 12 4 4

L.S. 50
PLAN  1
FREE C1 I1
BOND
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\ccf-107-01-1.hkl">
REM </olex2.extras>

WGHT    0.042200
FVAR       0.45153
C1    1    0.055624    0.475718    0.446589    11.00000    0.04005    0.10165 =
         0.03857    0.01774    0.01041    0.01006
AFIX  23
H1A   2    0.202869    0.481625    0.465061    11.00000   -1.20000
H1B   2    0.021264    0.494323    0.348808    11.00000   -1.20000
AFIX   0
C2    1   -0.001902    0.389534    0.457955    11.00000    0.05479    0.12009 =
         0.05455    0.01924    0.02328    0.01738
AFIX  23
H2A   2    0.048356    0.369341    0.551617    11.00000   -1.20000
H2B   2   -0.150584    0.384529    0.452368    11.00000   -1.20000
AFIX   0

I1    3    0.465271    0.537609    0.773127    11.00000    0.05113    0.04084 =
         0.03141    0.00035    0.00437   -0.00187
I2    3    0.501231    0.285871    0.617785    11.00000    0.06528    0.05025 =
         0.05034   -0.02048    0.00693   -0.00445
I3    3    1.007513    0.365819    0.935834    11.00000    0.02656    0.06398 =
         0.05544    0.00368    0.00444   -0.00014
N1    4    0.084588    0.342429    0.341686    11.00000    0.07237    0.10423 =
         0.05258    0.01668    0.00509   -0.01169
AFIX 137
H1C   2   -0.000789    0.343574    0.263173    11.00000   -1.50000
H1D   2    0.101012    0.292987    0.371678    11.00000   -1.50000
H1E   2    0.205871    0.362227    0.319862    11.00000   -1.50000
AFIX   0

PB1   5    0.515577    0.371545    0.931859    11.00000    0.03359    0.03765 =
         0.03429   -0.00020    0.00436   -0.00092
HKLF 4




REM  1 in P2(1)/c
REM wR2 = 0.0994, GooF = S = 0.952, Restrained GooF = 0.952 for all data
REM R1 = 0.0411 for 1678 Fo > 4sig(Fo) and 0.0737 for all 2504 data
REM 65 parameters refined using 0 restraints

END

WGHT      0.0422      0.0000

REM Highest difference peak  1.342,  deepest hole -2.278,  1-sigma level  0.384
Q1    1   0.6866  0.4499  1.0402  11.00000  0.05    1.34
;
_shelx_res_checksum              52242
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.342
_oxdiff_exptl_absorpt_empirical_full_min 0.576
####################################################################### 
# 
# 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_(Mpda)Pb2I6-298K
_database_code_depnum_ccdc_archive 'CCDC 2183782'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2022-07-04 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_audit_creation_date             2022-07-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(I24 Pb8), 2(C2 N)'
_chemical_formula_sum            'C4 I6 N2 H14 Pb2'
_chemical_formula_weight         1265.95
_chemical_melting_point          ?
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'

_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      orthorhombic
_space_group_IT_number           55
_space_group_name_H-M_alt        'P b a m'
_space_group_name_Hall           '-P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'

_cell_length_a                   8.9733(9)
_cell_length_b                   17.5285(11)
_cell_length_c                   6.4748(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1018.41(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1733
_cell_measurement_temperature    298.13(10)
_cell_measurement_theta_max      29.7020
_cell_measurement_theta_min      2.5350
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    25.582
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.082
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.824
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            4707
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.126
_diffrn_reflns_theta_min         2.324
_diffrn_ambient_temperature      298.13(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_device_type  'multiwire proportional'
_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                945
_reflns_number_total             1340
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.452
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.281
_refine_ls_extinction_coef       0.00163(16)
_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   1.043
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         1340
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0367
_refine_ls_restrained_S_all      1.036
_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)+(0.0430P)²+0.7084P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0894
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{C3, N3}
{C2, N2}
2. Restrained distances
 C2-C3
 1.49 with sigma of 0.01
 N2-N3
 1.49 with sigma of 0.01
 C3-C4
 1.49 with sigma of 0.01
 C4-C4_$1
 1.53 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C4 \\sim C4 \\sim C2 \\sim C2 \\sim C3 \\sim C3 \\sim N3 \\sim N3 \\sim N2
\\sim N2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C3) = Uiso(N3)
Uiso(C2) = Uiso(N2)
4. Rigid body (RIGU) restrains
 C4, C2, C3, N3, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C2(0.25) C3(0.25) N3(0.25) N2(0.25)
;
_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
Pb1 Pb 0.44586(6) 0.62833(2) 1.000000 0.0419(2) Uani 1 2 d S T P . .
I2 I 0.44546(13) 0.62755(5) 0.500000 0.0658(3) Uani 1 2 d S T P . .
I3 I 0.63421(14) 0.78220(6) 1.000000 0.0848(4) Uani 1 2 d S T P . .
I1 I 0.74087(10) 0.52730(4) 1.000000 0.0516(3) Uani 1 2 d S T P . .
C4 C 1.028(3) 0.5409(5) 0.500000 0.133(8) Uani 1 2 d DS TU P . .
C2 C 0.884(3) 0.6637(10) 0.500000 0.133(7) Uiso 0.5 2 d DS TU P A 1
C3 C 0.880(3) 0.5789(10) 0.500000 0.167(9) Uiso 0.5 2 d DS TU P A 1
N3 N 0.880(3) 0.5789(10) 0.500000 0.167(9) Uiso 0.5 2 d DS TU P A 2
N2 N 0.884(3) 0.6637(10) 0.500000 0.133(7) Uiso 0.5 2 d DS TU P A 2

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 0.0426(3) 0.0415(3) 0.0415(3) 0.000 0.000 -0.0005(2)
I2 0.0798(9) 0.0869(7) 0.0306(4) 0.000 0.000 -0.0028(5)
I3 0.0712(9) 0.0689(6) 0.1144(9) 0.000 0.000 -0.0354(6)
I1 0.0420(6) 0.0485(5) 0.0643(5) 0.000 0.000 -0.0003(4)
C4 0.124(11) 0.148(11) 0.127(11) 0.000 0.000 0.008(8)

_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 I2 3.2374(2) 1_556 ?
Pb1 I2 3.2374(2) . ?
Pb1 I3 3.2063(12) 7_575 ?
Pb1 I3 3.1828(10) . ?
Pb1 I1 3.1849(10) . ?
Pb1 I1 3.2015(9) 5_667 ?
C4 C4 1.520(10) 2_765 ?
C4 C3 1.485(10) . ?
C4 N3 1.485(10) . ?
C2 C3 1.488(7) . ?
N3 N2 1.488(7) . ?

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
I2 Pb1 I2 179.50(4) . 1_556 ?
I3 Pb1 I2 90.06(2) 7_575 1_556 ?
I3 Pb1 I2 90.241(19) . 1_556 ?
I3 Pb1 I2 90.06(2) 7_575 . ?
I3 Pb1 I2 90.240(19) . . ?
I3 Pb1 I3 92.789(15) . 7_575 ?
I3 Pb1 I1 91.71(3) . . ?
I3 Pb1 I1 179.48(4) . 5_667 ?
I1 Pb1 I2 89.92(2) . . ?
I1 Pb1 I2 89.759(19) 5_667 1_556 ?
I1 Pb1 I2 89.92(2) . 1_556 ?
I1 Pb1 I2 89.759(19) 5_667 . ?
I1 Pb1 I3 87.73(3) 5_667 7_575 ?
I1 Pb1 I3 175.50(3) . 7_575 ?
I1 Pb1 I1 87.78(3) . 5_667 ?
Pb1 I2 Pb1 179.50(4) 1_554 . ?
Pb1 I3 Pb1 151.36(5) . 7_675 ?
Pb1 I1 Pb1 92.22(3) . 5_667 ?
C3 C4 C4 97.1(18) . 2_765 ?
C4 C3 C2 115.2(17) . . ?
C4 N3 N2 115.2(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 C4 C3 C2 180.0 2_765 . . . ?
C4 C4 N3 N2 180.0 2_765 . . . ?

_shelx_res_file                  
;
TITL 1111_a.res in Pbam
    1111.res
    created by SHELXL-2018/3 at 16:24:42 on 04-Jul-2022
REM Old TITL 1111 in Pba2
REM SHELXT solution in Pbam: R1 0.151, Rweak 0.005, Alpha 0.025
REM <I/s> 0.503 for 114 systematic absences, Orientation as input
REM Formula found by SHELXT: I3 Pb
CELL 0.71073 8.9733 17.5285 6.4748 90 90 90
ZERR 2 0.0009 0.0011 0.0004 0 0 0
LATT 1
SYMM -X,-Y,+Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C I N Pb
UNIT 8 12 4 4
EQIV $1 2-X,1-Y,+Z
DFIX 1.49 0.01 C2 C3
DFIX 1.49 0.01 N2 N3
DFIX 1.49 0.01 C3 C4
DFIX 1.53 0.01 C4 C4_$1
SIMU 0.04 0.08 1.7 C4 C4 C2 C2 C3 C3 N3 N3 N2 N2
RIGU C4 > N2
ISOR 0.01 0.02 C4
EADP C3 N3
EADP C2 N2
EXYZ C3 N3
EXYZ C2 N2

L.S. 60 0 0
PLAN  1
CONF
list 4
MORE -1
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\1111.hkl">
REM </olex2.extras>

WGHT    0.043000    0.708400
EXTI    0.001629
FVAR       0.15186
PB1   4    0.445863    0.628332    1.000000    10.50000    0.04259    0.04153 =
         0.04152    0.00000    0.00000   -0.00049
I2    2    0.445463    0.627547    0.500000    10.50000    0.07981    0.08694 =
         0.03055    0.00000    0.00000   -0.00284
I3    2    0.634214    0.782196    1.000000    10.50000    0.07117    0.06893 =
         0.11439    0.00000    0.00000   -0.03545
I1    2    0.740865    0.527302    1.000000    10.50000    0.04196    0.04846 =
         0.06434    0.00000    0.00000   -0.00032
C4    1    1.028260    0.540874    0.500000    10.50000    0.12445    0.14826 =
         0.12730    0.00000    0.00000    0.00839
PART 1
C2    1    0.884335    0.663729    0.500000    10.25000    0.13330
C3    1    0.880307    0.578852    0.500000    10.25000    0.16681
PART 0
PART 2
N3    3    0.880307    0.578852    0.500000    10.25000    0.16681
N2    3    0.884335    0.663729    0.500000    10.25000    0.13330
HKLF 4




REM  1111_a.res in Pbam
REM wR2 = 0.0894, GooF = S = 1.043, Restrained GooF = 1.036 for all data
REM R1 = 0.0367 for 945 Fo > 4sig(Fo) and 0.0648 for all 1340 data
REM 38 parameters refined using 28 restraints

END

WGHT      0.0430      0.7084

REM Highest difference peak  1.452,  deepest hole -1.064,  1-sigma level  0.281
Q1    1   0.9973  0.5145  0.5000  10.50000  0.05    1.45
;
_shelx_res_checksum              29359
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT043_MpdaPb2I6-298K      
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      14.09 Check 
RESPONSE: Hydrogen atoms are not added because the cations are highly disordered.
;
# end Validation Reply Form
