# Supplementary Information (SI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_dpppyi_auto
_database_code_depnum_ccdc_archive 'CCDC 2494685'
loop_
_audit_author_name
_audit_author_address
'Alexandre Abherve' 'Laboratoire MOLTECH Anjou, CNRS, Univ Angers'
_audit_update_record             
;
2025-10-11 deposited with the CCDC.	2026-04-02 downloaded from the CCDC.
;
_audit_creation_date             2025-09-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7311)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
flavia.pop@univ-angers.fr
_chemical_name_common            ?
_chemical_name_systematic        DPPPyI2
_chemical_formula_moiety         'I, C9 H8 N2 O'
_chemical_formula_sum            'C9 H8 I N2 O'
_chemical_formula_weight         287.07
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H15 N4 O2 I2'
_chemical_oxdiff_usercomment     'DPPPyI2 evap acetone and ACN'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   4.9281(2)
_cell_length_b                   10.3820(4)
_cell_length_c                   18.3674(7)
_cell_angle_alpha                90
_cell_angle_beta                 92.341(3)
_cell_angle_gamma                90
_cell_volume                     938.96(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3067
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      71.6190
_cell_measurement_theta_min      4.7830
_cell_oxdiff_angle_alpha         90.011(5)
_cell_oxdiff_angle_beta          92.344(5)
_cell_oxdiff_angle_gamma         90.019(5)
_cell_oxdiff_length_a            4.9291(3)
_cell_oxdiff_length_b            10.3814(6)
_cell_oxdiff_length_c            18.3649(11)
_cell_oxdiff_measurement_reflns_used 3067
_cell_oxdiff_volume              938.97(9)
_shelx_estimated_absorpt_T_max   0.504
_shelx_estimated_absorpt_T_min   0.094
_exptl_absorpt_coefficient_mu    26.482
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.251
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.44.99a (Rigaku Oxford Diffraction, 2025)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.031
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             548
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 5 1 0.0148
0 -5 -1 0.0148
0 1 -5 0.0170
0 -1 5 0.0170
2 2 5 0.0477
-2 -2 -5 0.0477

_exptl_crystal_preparation       synthesis
_exptl_crystal_recrystallization_method 'evaporation from ethanol'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0006 4.9993 0.9974 -0.0703 -0.4649 0.5799
-0.0006 -4.9993 -0.9974 0.0703 0.4649 -0.5799
-0.0005 0.9998 -4.9995 0.0606 -0.4005 -0.1847
0.0005 -0.9998 4.9995 -0.0606 0.4005 0.1847
2.0002 2.0016 4.9947 -0.7124 0.0609 0.4073
-2.0002 -2.0016 -4.9947 0.7124 -0.0609 -0.4073

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4007
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.678
_diffrn_reflns_theta_min         4.819
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00 114.00   1.00    4.00    --   41.49  60.00 153.00   79
  2  ω    117.00 154.00   1.00   16.00    --  103.45  60.00 153.00   37
  3  ω     30.00 131.00   1.00   16.00    --  103.45 -60.00  14.00  101
  4  ω     82.00 107.00   1.00   16.00    --  103.45  60.00 153.00   25
  5  ω     54.00  95.00   1.00    4.00    --   41.49-125.00 -60.00   41
  6  ω      8.00  48.00   1.00    4.00    --   41.49-125.00 -60.00   40
  7  ω      7.00  33.00   1.00    4.00    --   41.49 -99.00  60.00   26
  8  ω    -26.00  70.00   1.00    4.00    --   41.49 -60.00  14.00   96
  9  ω    105.00 135.00   1.00   16.00    --  103.45 -77.00 -90.00   30
 10  ω     75.00 157.00   1.00   16.00    --  103.45  30.00 120.00   82
 11  ω     39.00  78.00   1.00   16.00    --  103.45 -77.00 -90.00   39
 12  ω     64.00 123.00   1.00   16.00    --  103.45 -30.00-150.00   59
 13  ω     32.00  61.00   1.00   16.00    --  103.45 -30.00-150.00   29
 14  ω     48.00 100.00   1.00   16.00    --  103.45-125.00  30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.3092563000
_diffrn_orient_matrix_UB_12      -0.0111675000
_diffrn_orient_matrix_UB_13      -0.0143141000
_diffrn_orient_matrix_UB_21      -0.0123711000
_diffrn_orient_matrix_UB_22      -0.1047993000
_diffrn_orient_matrix_UB_23      0.0591526000
_diffrn_orient_matrix_UB_31      -0.0453174000
_diffrn_orient_matrix_UB_32      0.1044693000
_diffrn_orient_matrix_UB_33      0.0578342000
_diffrn_oxdiff_digest_hkl        
;
438a43909f76fb03eb6870ae96a3d3883c54f7
;
_diffrn_oxdiff_digest_od_ed      
;

;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1728
_reflns_number_total             1780
_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 1.171.44.99a (Rigaku OD, 2025)'
_computing_data_collection       
'CrysAlisPro system (CCD 44.99a 64-bit (release 17-03-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.99a (Rigaku OD, 2025)'
_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         1.513
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.319
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1780
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0418
_refine_ls_restrained_S_all      1.319
_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)+(0.0117P)²+9.7146P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1033
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C8(H8), C5(H5), C6(H6), C7(H7)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_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
I1 I 0.80888(10) 0.67513(5) 0.37080(3) 0.03092(17) Uani 1 1 d . . . . .
O1 O 0.7747(10) -0.0054(5) 0.6467(3) 0.0259(11) Uani 1 1 d . . . . .
N1 N 0.6866(12) 0.1158(6) 0.5421(3) 0.0206(12) Uani 1 1 d . . . . .
H1 H 0.553517 0.163302 0.557977 0.025 Uiso 1 1 calc R U . . .
N2 N 0.4448(12) 0.3796(6) 0.3163(3) 0.0232(12) Uani 1 1 d . . . . .
C1 C 0.8234(14) 0.0197(7) 0.5842(4) 0.0209(14) Uani 1 1 d . . . . .
C8 C 0.3634(15) 0.3859(7) 0.3849(4) 0.0256(15) Uani 1 1 d . . . . .
H8 H 0.227902 0.446396 0.397062 0.031 Uiso 1 1 calc R U . . .
C4 C 0.6774(14) 0.2190(6) 0.4205(4) 0.0205(14) Uani 1 1 d . . . . .
C3 C 0.7865(14) 0.1260(6) 0.4734(3) 0.0199(13) Uani 1 1 d . . . . .
C5 C 0.7660(15) 0.2192(7) 0.3493(4) 0.0226(14) Uani 1 1 d . . . . .
H5 H 0.909423 0.163791 0.336192 0.027 Uiso 1 1 calc R U . . .
C6 C 0.4734(15) 0.3059(7) 0.4381(4) 0.0258(15) Uani 1 1 d . . . . .
H6 H 0.411245 0.309722 0.486301 0.031 Uiso 1 1 calc R U . . .
C2 C 0.9848(13) 0.0342(7) 0.4668(3) 0.0202(13) Uani 1 1 d . . . . .
C7 C 0.6447(14) 0.2998(7) 0.2981(4) 0.0232(14) Uani 1 1 d . . . . .
H7 H 0.703404 0.298899 0.249501 0.028 Uiso 1 1 calc R U . . .
C9 C 0.3158(16) 0.4642(8) 0.2607(4) 0.0287(16) Uani 1 1 d . . . . .
H9A H 0.178034 0.517627 0.283118 0.043 Uiso 1 1 calc R U . . .
H9B H 0.229653 0.411665 0.221937 0.043 Uiso 1 1 calc R U . . .
H9C H 0.453758 0.519823 0.240029 0.043 Uiso 1 1 calc R U . . .


_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
O1 C1 1.210(8) . ?
N1 H1 0.8800 . ?
N1 C1 1.416(9) . ?
N1 C3 1.378(8) . ?
N2 C8 1.340(9) . ?
N2 C7 1.340(9) . ?
N2 C9 1.472(9) . ?
C1 C2 1.468(9) 3_756 ?
C8 H8 0.9500 . ?
C8 C6 1.375(10) . ?
C4 C3 1.457(9) . ?
C4 C5 1.395(10) . ?
C4 C6 1.398(10) . ?
C3 C2 1.374(10) . ?
C5 H5 0.9500 . ?
C5 C7 1.377(10) . ?
C6 H6 0.9500 . ?
C2 C2 1.414(13) 3_756 ?
C7 H7 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?

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 N1 H1 124.0 . . ?
C3 N1 H1 124.0 . . ?
C3 N1 C1 112.0(6) . . ?
C8 N2 C9 119.1(6) . . ?
C7 N2 C8 121.0(6) . . ?
C7 N2 C9 119.9(6) . . ?
O1 C1 N1 124.1(6) . . ?
O1 C1 C2 132.9(7) . 3_756 ?
N1 C1 C2 103.0(5) . 3_756 ?
N2 C8 H8 119.5 . . ?
N2 C8 C6 120.9(7) . . ?
C6 C8 H8 119.5 . . ?
C5 C4 C3 120.3(6) . . ?
C5 C4 C6 118.1(6) . . ?
C6 C4 C3 121.5(6) . . ?
N1 C3 C4 121.8(6) . . ?
C2 C3 N1 108.0(6) . . ?
C2 C3 C4 130.2(6) . . ?
C4 C5 H5 120.1 . . ?
C7 C5 C4 119.8(7) . . ?
C7 C5 H5 120.1 . . ?
C8 C6 C4 119.4(7) . . ?
C8 C6 H6 120.3 . . ?
C4 C6 H6 120.3 . . ?
C3 C2 C1 143.1(6) . 3_756 ?
C3 C2 C2 108.9(7) . 3_756 ?
C2 C2 C1 108.1(7) 3_756 3_756 ?
N2 C7 C5 120.6(6) . . ?
N2 C7 H7 119.7 . . ?
C5 C7 H7 119.7 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

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
N1 C3 C2 C1 178.5(9) . . . 3_756 ?
N1 C3 C2 C2 -1.2(9) . . . 3_756 ?
N2 C8 C6 C4 1.5(11) . . . . ?
C1 N1 C3 C4 -179.8(6) . . . . ?
C1 N1 C3 C2 2.2(8) . . . . ?
C8 N2 C7 C5 2.1(11) . . . . ?
C4 C3 C2 C1 0.7(15) . . . 3_756 ?
C4 C3 C2 C2 -179.0(7) . . . 3_756 ?
C4 C5 C7 N2 0.9(11) . . . . ?
C3 N1 C1 O1 178.6(7) . . . . ?
C3 N1 C1 C2 -2.3(7) . . . 3_756 ?
C3 C4 C5 C7 174.3(6) . . . . ?
C3 C4 C6 C8 -175.5(7) . . . . ?
C5 C4 C3 N1 -174.2(6) . . . . ?
C5 C4 C3 C2 3.3(11) . . . . ?
C5 C4 C6 C8 1.4(11) . . . . ?
C6 C4 C3 N1 2.7(10) . . . . ?
C6 C4 C3 C2 -179.8(7) . . . . ?
C6 C4 C5 C7 -2.6(10) . . . . ?
C7 N2 C8 C6 -3.3(11) . . . . ?
C9 N2 C8 C6 178.2(7) . . . . ?
C9 N2 C7 C5 -179.4(7) . . . . ?

_olex2_exptl_crystal_mounting_method 'fomblin oil'
_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 1.350
_oxdiff_exptl_absorpt_empirical_full_min 0.769
####################################################################### 
# 
# 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_DPPPy-Pb2Br6
_database_code_depnum_ccdc_archive 'CCDC 2494687'
loop_
_audit_author_name
_audit_author_address
'Alexandre Abherve' 'Laboratoire MOLTECH Anjou, CNRS, Univ Angers'
_audit_update_record             
;
2025-10-11 deposited with the CCDC.	2026-04-02 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         'C18 H16 Br6 N4 O2 Pb2'
_chemical_formula_sum            'C18 H16 Br6 N4 O2 Pb2'
_chemical_formula_weight         1214.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.1449(2)
_cell_length_b                   17.5077(5)
_cell_length_c                   17.0660(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.779(3)
_cell_angle_gamma                90
_cell_volume                     1234.13(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    180.00(10)
_cell_measurement_reflns_used    3509
_cell_measurement_theta_min      3.5900
_cell_measurement_theta_max      75.9750

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.267
_exptl_crystal_F_000             1084
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    37.813
_shelx_estimated_absorpt_T_min   0.042
_shelx_estimated_absorpt_T_max   0.313
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.104
_exptl_absorpt_correction_T_max  0.505
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.719
_oxdiff_exptl_absorpt_empirical_full_max 1.530
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            5201
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.623
_diffrn_reflns_theta_max         76.031
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2499
_reflns_number_gt                2354
_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       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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)+(0.0813P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2499
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1172
_refine_ls_wR_factor_gt          0.1136
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_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
C1 C 0.368(2) 0.2489(4) 0.3377(4) 0.0315(15) Uani 1 1 d . . . . .
H1A H 0.494036 0.265016 0.386077 0.047 Uiso 1 1 calc R U . . .
H1B H 0.137339 0.248960 0.346164 0.047 Uiso 1 1 calc R U . . .
H1C H 0.434376 0.197360 0.323490 0.047 Uiso 1 1 calc R U . . .
C2 C 0.282(2) 0.2928(4) 0.2005(5) 0.0286(15) Uani 1 1 d . . . . .
H2 H 0.145950 0.249693 0.190033 0.034 Uiso 1 1 calc R U . . .
C3 C 0.3256(19) 0.3445(4) 0.1398(4) 0.0268(14) Uani 1 1 d . . . . .
H3 H 0.225423 0.336146 0.088419 0.032 Uiso 1 1 calc R U . . .
C4 C 0.522(2) 0.4097(4) 0.1564(5) 0.0306(17) Uani 1 1 d . . . . .
C5 C 0.672(2) 0.4175(4) 0.2340(5) 0.0295(16) Uani 1 1 d . . . . .
H5 H 0.807330 0.460061 0.247308 0.035 Uiso 1 1 calc R U . . .
C6 C 0.620(2) 0.3636(5) 0.2894(5) 0.0316(16) Uani 1 1 d . . . . .
H6 H 0.722962 0.369349 0.340936 0.038 Uiso 1 1 calc R U . . .
C7 C 0.5623(19) 0.4654(4) 0.0959(5) 0.0279(14) Uani 1 1 d . . . . .
C8 C 0.441(2) 0.4669(4) 0.0172(5) 0.0323(17) Uani 1 1 d . . . . .
C9 C 0.241(2) 0.4246(5) -0.0438(5) 0.0333(16) Uani 1 1 d . . . . .
N1 N 0.4276(18) 0.3026(3) 0.2733(4) 0.0291(13) Uani 1 1 d . . . . .
N2 N 0.7451(19) 0.5305(4) 0.1097(4) 0.0335(14) Uani 1 1 d . . . . .
H2A H 0.843141 0.542142 0.155853 0.040 Uiso 1 1 calc R U . . .
O1 O 0.0924(19) 0.3646(4) -0.0402(4) 0.0411(15) Uani 1 1 d . . . . .
Br1 Br 0.21891(16) 0.45453(4) 0.41955(4) 0.02242(19) Uani 1 1 d . . . . .
Br2 Br -0.23516(18) 0.30148(4) 0.53525(4) 0.0268(2) Uani 1 1 d . . . . .
Br3 Br 0.8046(2) 0.39662(5) 0.73507(4) 0.0288(2) Uani 1 1 d . . . . .
Pb1 Pb 0.28979(7) 0.41145(2) 0.58950(2) 0.02509(15) Uani 1 1 d . . . . .


_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 N1 1.482(10) . ?
C2 N1 1.347(10) . ?
C2 C3 1.399(11) . ?
C3 C4 1.417(10) . ?
C4 C5 1.421(12) . ?
C4 C7 1.440(12) . ?
C5 C6 1.364(12) . ?
C6 N1 1.348(11) . ?
C7 N2 1.378(10) . ?
C7 C8 1.395(11) . ?
C8 C8 1.405(16) 3_665 ?
C8 C9 1.474(12) . ?
C9 O1 1.222(11) . ?
C9 N2 1.378(12) 3_665 ?
Br1 Pb1 2.9875(7) . ?
Br1 Pb1 3.1191(7) 3_666 ?
Br1 Pb1 3.1498(7) 3_566 ?
Br2 Pb1 2.9572(8) 1_455 ?
Br2 Pb1 2.9938(8) . ?
Br3 Pb1 3.1478(8) . ?

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
N1 C2 C3 121.7(7) . . ?
C2 C3 C4 118.8(7) . . ?
C3 C4 C5 117.5(8) . . ?
C3 C4 C7 120.0(8) . . ?
C5 C4 C7 122.4(7) . . ?
C6 C5 C4 119.9(8) . . ?
N1 C6 C5 122.0(7) . . ?
N2 C7 C8 107.3(7) . . ?
N2 C7 C4 122.2(7) . . ?
C8 C7 C4 130.5(7) . . ?
C7 C8 C8 107.9(9) . 3_665 ?
C7 C8 C9 143.7(8) . . ?
C8 C8 C9 108.3(9) 3_665 . ?
O1 C9 N2 125.9(8) . 3_665 ?
O1 C9 C8 130.8(8) . . ?
N2 C9 C8 103.3(7) 3_665 . ?
C2 N1 C6 120.1(7) . . ?
C2 N1 C1 121.0(7) . . ?
C6 N1 C1 118.9(7) . . ?
C7 N2 C9 113.1(7) . 3_665 ?
Pb1 Br1 Pb1 103.07(2) . 3_666 ?
Pb1 Br1 Pb1 104.30(2) . 3_566 ?
Pb1 Br1 Pb1 82.780(19) 3_666 3_566 ?
Pb1 Br2 Pb1 88.29(2) 1_455 . ?
Br2 Pb1 Br1 82.80(2) 1_655 . ?
Br2 Pb1 Br2 88.29(2) 1_655 . ?
Br1 Pb1 Br2 81.48(2) . . ?
Br2 Pb1 Br1 91.13(2) 1_655 3_666 ?
Br1 Pb1 Br1 76.93(2) . 3_666 ?
Br2 Pb1 Br1 158.30(2) . 3_666 ?
Br2 Pb1 Br3 76.60(2) 1_655 . ?
Br1 Pb1 Br3 142.41(2) . . ?
Br2 Pb1 Br3 128.20(2) . . ?
Br1 Pb1 Br3 72.47(2) 3_666 . ?
Br2 Pb1 Br1 158.45(2) 1_655 3_566 ?
Br1 Pb1 Br1 75.70(2) . 3_566 ?
Br2 Pb1 Br1 89.86(2) . 3_566 ?
Br1 Pb1 Br1 82.780(19) 3_666 3_566 ?
Br3 Pb1 Br1 120.47(2) . 3_566 ?

_refine_diff_density_max         1.980
_refine_diff_density_min         -2.160
_refine_diff_density_rms         0.336



####################################################################### 
# 
# 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_DPPPy-Pb2Cl6
_database_code_depnum_ccdc_archive 'CCDC 2494686'
loop_
_audit_author_name
_audit_author_address
'Alexandre Abherve' 'Laboratoire MOLTECH Anjou, CNRS, Univ Angers'
_audit_update_record             
;
2025-10-11 deposited with the CCDC.	2026-04-02 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         'C18 H16 Cl6 N4 O2 Pb2'
_chemical_formula_sum            'C18 H16 Cl6 N4 O2 Pb2'
_chemical_formula_weight         947.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   4.0195(2)
_cell_length_b                   17.1565(7)
_cell_length_c                   16.7619(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.904(4)
_cell_angle_gamma                90
_cell_volume                     1147.53(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    201(2)
_cell_measurement_reflns_used    3174
_cell_measurement_theta_min      3.6130
_cell_measurement_theta_max      75.7540

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.742
_exptl_crystal_F_000             868
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    34.852
_shelx_estimated_absorpt_T_min   0.051
_shelx_estimated_absorpt_T_max   0.336
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.423
_oxdiff_exptl_absorpt_empirical_full_max 2.715
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      201(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            5136
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.700
_diffrn_reflns_theta_max         76.253
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2310
_reflns_number_gt                2127
_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       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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)+(0.0924P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2310
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1310
_refine_ls_wR_factor_gt          0.1270
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
C1 C 0.9247(18) 0.5337(5) 0.9820(5) 0.0223(15) Uani 1 1 d . . . . .
C2 C 0.773(2) 0.5772(5) 1.0447(5) 0.0237(16) Uani 1 1 d . . . . .
C3 C 0.9652(17) 0.5345(5) 0.9019(4) 0.0212(14) Uani 1 1 d . . . . .
C4 C 0.863(2) 0.5917(4) 0.8405(5) 0.0195(16) Uani 1 1 d . . . . .
C5 C 0.924(2) 0.5825(4) 0.7615(5) 0.0244(17) Uani 1 1 d . . . . .
H5 H 1.039453 0.537243 0.746969 0.029 Uiso 1 1 calc R U . . .
C6 C 0.8239(19) 0.6368(5) 0.7035(5) 0.0228(15) Uani 1 1 d . . . . .
H6 H 0.873100 0.629560 0.649952 0.027 Uiso 1 1 calc R U . . .
C7 C 0.587(2) 0.7119(5) 0.7995(5) 0.0252(16) Uani 1 1 d . . . . .
H7 H 0.467309 0.757103 0.812160 0.030 Uiso 1 1 calc R U . . .
C8 C 0.6872(18) 0.6594(5) 0.8581(5) 0.0242(15) Uani 1 1 d . . . . .
H8 H 0.638271 0.668318 0.911435 0.029 Uiso 1 1 calc R U . . .
C9 C 0.536(2) 0.7563(5) 0.6586(5) 0.0281(16) Uani 1 1 d . . . . .
H9A H 0.418486 0.799420 0.681336 0.042 Uiso 1 1 calc R U . . .
H9B H 0.728668 0.776720 0.634394 0.042 Uiso 1 1 calc R U . . .
H9C H 0.383476 0.729734 0.617411 0.042 Uiso 1 1 calc R U . . .
N1 N 0.8535(16) 0.5311(4) 1.1135(4) 0.0256(14) Uani 1 1 d . . . . .
H1 H 0.794901 0.542641 1.160993 0.031 Uiso 1 1 calc R U . . .
N2 N 0.6547(15) 0.7006(4) 0.7230(4) 0.0201(12) Uani 1 1 d . . . . .
O1 O 0.6116(16) 0.6372(4) 1.0431(4) 0.0308(13) Uani 1 1 d . . . . .
Cl1 Cl 0.5940(5) 0.60245(12) 0.27045(11) 0.0265(4) Uani 1 1 d . . . . .
Cl2 Cl 0.2926(4) 0.54333(11) 0.57786(10) 0.0201(4) Uani 1 1 d . . . . .
Cl3 Cl -0.2668(4) 0.69175(11) 0.46505(11) 0.0255(4) Uani 1 1 d . . . . .
Pb1 Pb 0.22392(6) 0.58677(2) 0.41252(2) 0.02025(18) Uani 1 1 d . . . . .


_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 C3 1.372(11) . ?
C1 C1 1.407(15) 3_767 ?
C1 C2 1.479(11) . ?
C2 O1 1.215(10) . ?
C2 N1 1.404(11) . ?
C3 N1 1.382(10) 3_767 ?
C3 C4 1.444(11) . ?
C4 C5 1.386(11) . ?
C4 C8 1.409(10) . ?
C5 C6 1.371(12) . ?
C6 N2 1.349(10) . ?
C7 N2 1.356(10) . ?
C7 C8 1.359(12) . ?
C9 N2 1.477(10) . ?
Cl1 Pb1 2.9677(18) . ?
Cl2 Pb1 2.8512(17) . ?
Cl2 Pb1 2.9511(18) 3_666 ?
Cl2 Pb1 3.0657(17) 3_566 ?
Cl3 Pb1 2.7887(18) 1_455 ?
Cl3 Pb1 2.8857(18) . ?

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
C3 C1 C1 109.5(9) . 3_767 ?
C3 C1 C2 142.9(8) . . ?
C1 C1 C2 107.6(9) 3_767 . ?
O1 C2 N1 124.3(8) . . ?
O1 C2 C1 132.6(8) . . ?
N1 C2 C1 103.0(7) . . ?
C1 C3 N1 107.5(7) . 3_767 ?
C1 C3 C4 130.3(7) . . ?
N1 C3 C4 122.1(7) 3_767 . ?
C5 C4 C8 116.5(7) . . ?
C5 C4 C3 122.4(7) . . ?
C8 C4 C3 121.1(7) . . ?
C6 C5 C4 121.9(8) . . ?
N2 C6 C5 119.6(7) . . ?
N2 C7 C8 120.9(7) . . ?
C7 C8 C4 120.5(7) . . ?
C3 N1 C2 112.4(7) 3_767 . ?
C6 N2 C7 120.6(7) . . ?
C6 N2 C9 118.4(6) . . ?
C7 N2 C9 120.9(7) . . ?
Pb1 Cl2 Pb1 103.71(5) . 3_666 ?
Pb1 Cl2 Pb1 104.74(5) . 3_566 ?
Pb1 Cl2 Pb1 83.81(5) 3_666 3_566 ?
Pb1 Cl3 Pb1 90.19(5) 1_455 . ?
Cl3 Pb1 Cl2 83.12(5) 1_655 . ?
Cl3 Pb1 Cl3 90.19(5) 1_655 . ?
Cl2 Pb1 Cl3 81.75(5) . . ?
Cl3 Pb1 Cl2 91.01(5) 1_655 3_666 ?
Cl2 Pb1 Cl2 76.29(5) . 3_666 ?
Cl3 Pb1 Cl2 157.69(5) . 3_666 ?
Cl3 Pb1 Cl1 77.00(6) 1_655 . ?
Cl2 Pb1 Cl1 143.55(5) . . ?
Cl3 Pb1 Cl1 127.96(6) . . ?
Cl2 Pb1 Cl1 73.87(5) 3_666 . ?
Cl3 Pb1 Cl2 158.38(5) 1_655 3_566 ?
Cl2 Pb1 Cl2 75.26(5) . 3_566 ?
Cl3 Pb1 Cl2 86.92(5) . 3_566 ?
Cl2 Pb1 Cl2 83.81(5) 3_666 3_566 ?
Cl1 Pb1 Cl2 121.07(5) . 3_566 ?

_refine_diff_density_max         2.631
_refine_diff_density_min         -2.363
_refine_diff_density_rms         0.364


# start Validation Reply Form
_vrf_PLAT971_DPPPy-Pb2Cl6        
;
PROBLEM: Check Calcd Resid. Dens.  1.72Ang From Cl1             2.75 eA-3  
RESPONSE: This residual density peak near the heavy atom is due to the use 
of Cu X-ray diffraction source and can not be assigned to 
unaccounted atom type or twinning error.
;
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2494690'
loop_
_audit_author_name
_audit_author_address
'Alexandre Abherve' 'Laboratoire MOLTECH Anjou, CNRS, Univ Angers'
_audit_update_record             
;
2025-10-11 deposited with the CCDC.	2026-04-02 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         'C24 H30 I6 N6 O4 Pb2'
_chemical_formula_sum            'C24 H30 I6 N6 O4 Pb2'
_chemical_formula_weight         1642.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.7310(5)
_cell_length_b                   8.2091(4)
_cell_length_c                   24.3633(18)
_cell_angle_alpha                90
_cell_angle_beta                 91.423(5)
_cell_angle_gamma                90
_cell_volume                     1945.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    200.01(10)
_cell_measurement_reflns_used    3137
_cell_measurement_theta_min      4.7590
_cell_measurement_theta_max      71.4160

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.803
_exptl_crystal_F_000             1460
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    54.300
_shelx_estimated_absorpt_T_min   0.022
_shelx_estimated_absorpt_T_max   0.220
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.012
_exptl_absorpt_correction_T_max  0.360
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.355
_oxdiff_exptl_absorpt_empirical_full_max 4.978
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200.01(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            7788
_diffrn_reflns_av_unetI/netI     0.0975
_diffrn_reflns_av_R_equivalents  0.0952
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.630
_diffrn_reflns_theta_max         72.414
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             3704
_reflns_number_gt                2821
_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       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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)+(0.1609P)²+49.6519P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3704
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0963
_refine_ls_wR_factor_ref         0.2943
_refine_ls_wR_factor_gt          0.2725
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.000
_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
C1 C 0.813(3) 0.436(5) 0.6936(17) 0.081(11) Uani 1 1 d . . . . .
H1A H 0.771581 0.326939 0.692750 0.122 Uiso 1 1 calc R U . . .
H1B H 0.907799 0.429094 0.681001 0.122 Uiso 1 1 calc R U . . .
H1C H 0.813161 0.478050 0.731196 0.122 Uiso 1 1 calc R U . . .
C2 C 0.626(3) 0.480(4) 0.6279(13) 0.059(7) Uani 1 1 d . . . . .
H2 H 0.602056 0.368275 0.632286 0.071 Uiso 1 1 calc R U . . .
C3 C 0.554(3) 0.574(3) 0.5923(13) 0.056(6) Uani 1 1 d . . . . .
H3 H 0.478341 0.528620 0.572181 0.067 Uiso 1 1 calc R U . . .
C4 C 0.587(3) 0.731(3) 0.5850(12) 0.054(6) Uani 1 1 d . . . . .
C5 C 0.696(3) 0.796(3) 0.6161(12) 0.055(6) Uani 1 1 d . . . . .
H5 H 0.719827 0.907759 0.612714 0.066 Uiso 1 1 calc R U . . .
C6 C 0.768(2) 0.699(3) 0.6511(12) 0.053(6) Uani 1 1 d . . . . .
H6 H 0.843669 0.742571 0.671467 0.064 Uiso 1 1 calc R U . . .
C7 C 0.518(2) 0.827(3) 0.5413(11) 0.047(5) Uani 1 1 d . . . . .
C8 C 0.638(2) 1.121(3) 0.5298(11) 0.048(5) Uani 1 1 d . . . . .
C9 C 0.546(2) 0.979(3) 0.5225(11) 0.043(5) Uani 1 1 d . . . . .
C10 C 0.043(4) 0.295(5) 0.4828(16) 0.085(10) Uani 1 1 d . . . . .
H10A H -0.033361 0.217598 0.482367 0.128 Uiso 1 1 calc R U . . .
H10B H 0.007503 0.406017 0.486999 0.128 Uiso 1 1 calc R U . . .
H10C H 0.092199 0.287196 0.448239 0.128 Uiso 1 1 calc R U . . .
C11 C 0.107(4) 0.113(5) 0.5618(19) 0.089(11) Uani 1 1 d . . . . .
H11A H 0.020757 0.063568 0.549136 0.134 Uiso 1 1 calc R U . . .
H11B H 0.182311 0.034349 0.558262 0.134 Uiso 1 1 calc R U . . .
H11C H 0.100381 0.145729 0.600299 0.134 Uiso 1 1 calc R U . . .
C12 C 0.249(3) 0.348(4) 0.5371(14) 0.064(8) Uani 1 1 d . . . . .
H12 H 0.306405 0.315468 0.567242 0.076 Uiso 1 1 calc R U . . .
N1 N 0.734(2) 0.544(3) 0.6576(10) 0.051(5) Uani 1 1 d . . . . .
N2 N 0.4043(19) 0.770(3) 0.5099(10) 0.051(5) Uani 1 1 d . . . . .
H2A H 0.365178 0.674292 0.515130 0.062 Uiso 1 1 calc R U . . .
N3 N 0.136(2) 0.258(3) 0.5280(12) 0.064(6) Uani 1 1 d . . . . .
O1 O 0.734(2) 1.145(3) 0.5618(10) 0.069(5) Uani 1 1 d . . . . .
O2 O 0.286(2) 0.464(2) 0.5118(9) 0.066(5) Uani 1 1 d . . . . .
I1 I 0.00055(14) 0.05572(19) 0.72314(8) 0.0544(5) Uani 1 1 d . . . . .
I2 I 0.06653(16) -0.40914(18) 0.82081(7) 0.0514(5) Uani 1 1 d . . . . .
I3 I 0.17984(17) -0.3863(2) 0.64990(7) 0.0565(5) Uani 1 1 d . . . . .
Pb1 Pb 0.24916(8) -0.17006(11) 0.75010(4) 0.0438(4) Uani 1 1 d . . . . .


_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 N1 1.46(4) . ?
C2 C3 1.34(4) . ?
C2 N1 1.37(4) . ?
C3 C4 1.34(4) . ?
C4 C5 1.39(4) . ?
C4 C7 1.48(4) . ?
C5 C6 1.35(4) . ?
C6 N1 1.32(3) . ?
C7 C9 1.36(3) . ?
C7 N2 1.41(3) . ?
C8 O1 1.21(3) . ?
C8 N2 1.37(3) 3_676 ?
C8 C9 1.48(3) . ?
C9 C9 1.44(5) 3_676 ?
C10 N3 1.44(5) . ?
C11 N3 1.48(4) . ?
C12 O2 1.19(4) . ?
C12 N3 1.33(4) . ?
I1 Pb1 3.1049(16) . ?
I1 Pb1 3.3683(17) 2_556 ?
I2 Pb1 3.1827(17) . ?
I2 Pb1 3.3080(17) 2_546 ?
I3 Pb1 3.079(2) . ?
I3 Pb1 3.429(2) 2_546 ?

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
C3 C2 N1 120(2) . . ?
C4 C3 C2 121(3) . . ?
C3 C4 C5 119(2) . . ?
C3 C4 C7 120(2) . . ?
C5 C4 C7 121(2) . . ?
C6 C5 C4 119(2) . . ?
N1 C6 C5 121(2) . . ?
C9 C7 N2 107(2) . . ?
C9 C7 C4 130(2) . . ?
N2 C7 C4 123(2) . . ?
O1 C8 N2 124(2) . 3_676 ?
O1 C8 C9 131(3) . . ?
N2 C8 C9 105(2) 3_676 . ?
C7 C9 C9 110(3) . 3_676 ?
C7 C9 C8 144(2) . . ?
C9 C9 C8 106(2) 3_676 . ?
O2 C12 N3 128(3) . . ?
C6 N1 C2 120(2) . . ?
C6 N1 C1 122(3) . . ?
C2 N1 C1 118(3) . . ?
C8 N2 C7 112(2) 3_676 . ?
C12 N3 C10 121(3) . . ?
C12 N3 C11 121(3) . . ?
C10 N3 C11 118(3) . . ?
Pb1 I1 Pb1 78.59(3) . 2_556 ?
Pb1 I2 Pb1 78.43(3) . 2_546 ?
Pb1 I3 Pb1 78.00(4) . 2_546 ?
I3 Pb1 I1 91.27(5) . . ?
I3 Pb1 I2 87.67(5) . . ?
I1 Pb1 I2 92.29(5) . . ?
I3 Pb1 I2 94.02(5) . 2_556 ?
I1 Pb1 I2 86.14(5) . 2_556 ?
I2 Pb1 I2 177.71(5) . 2_556 ?
I3 Pb1 I1 84.91(5) . 2_546 ?
I1 Pb1 I1 174.71(5) . 2_546 ?
I2 Pb1 I1 83.91(4) . 2_546 ?
I2 Pb1 I1 97.76(4) 2_556 2_546 ?
I3 Pb1 I3 172.39(6) . 2_556 ?
I1 Pb1 I3 83.51(5) . 2_556 ?
I2 Pb1 I3 98.03(5) . 2_556 ?
I2 Pb1 I3 80.15(5) 2_556 2_556 ?
I1 Pb1 I3 100.64(5) 2_546 2_556 ?

_refine_diff_density_max         3.763
_refine_diff_density_min         -3.271
_refine_diff_density_rms         0.482


# start Validation Reply Form
_vrf_PLAT413_shelx               
;
PROBLEM: Short Inter XH3 .. XHn     H10B     ..H10B     .       1.68 Ang.  
RESPONSE: This is due to a possible unaccounted disorder on the DMF solvent molecule.
;
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  1.27Ang From Pb1             3.99 eA-3  
RESPONSE: This residual density peak near the heavy atom is due to the use 
of Cu X-ray diffraction source and can not be assigned to 
unaccounted atom type or twinning error.
;
_vrf_PLAT972_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  1.63Ang From Pb1            -3.53 eA-3  
RESPONSE: This residual density peak near the heavy atom is due to the use 
of Cu X-ray diffraction source and can not be assigned to 
unaccounted atom type or twinning error.
;
_vrf_PLAT973_shelx               
;
PROBLEM: Check Calcd Positive Resid. Density on       Pb1       2.57 eA-3  
RESPONSE: This residual density peak near the heavy atom is due to the use 
of Cu X-ray diffraction source and can not be assigned to 
unaccounted atom type or twinning error.
;
_vrf_PLAT342_shelx               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03625 Ang.  
RESPONSE: This is due to a possible unaccounted disorder on the DMF solvent molecule.
;
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2494689'
loop_
_audit_author_name
_audit_author_address
'Alexandre Abherve' 'Laboratoire MOLTECH Anjou, CNRS, Univ Angers'
_audit_update_record             
;
2025-10-11 deposited with the CCDC.	2026-04-02 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         'C36 H32 Br9 N8 O4 Pb2, H3O, 3 H2O'
_chemical_formula_sum            'C36 H41 Br9 N8 O8 Pb2'
_chemical_formula_weight         1847.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'I 2/m'
_space_group_name_Hall           '-I 2y'

_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'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   18.4120(7)
_cell_length_b                   6.3623(3)
_cell_length_c                   22.4728(8)
_cell_angle_alpha                90
_cell_angle_beta                 108.424(4)
_cell_angle_gamma                90
_cell_volume                     2497.59(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    200.00(10)
_cell_measurement_reflns_used    4204
_cell_measurement_theta_min      5.0560
_cell_measurement_theta_max      76.0630

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.456
_exptl_crystal_F_000             1712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    21.851
_shelx_estimated_absorpt_T_min   0.111
_shelx_estimated_absorpt_T_max   0.408
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.058
_exptl_absorpt_correction_T_max  0.320
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.400
_oxdiff_exptl_absorpt_empirical_full_max 2.818
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            6290
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.717
_diffrn_reflns_theta_max         76.231
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             2774
_reflns_number_gt                2587
_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       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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)+(0.1408P)²+42.9048P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2774
_refine_ls_number_parameters     191
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0709
_refine_ls_wR_factor_ref         0.2084
_refine_ls_wR_factor_gt          0.2041
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_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
C1 C 0.1891(8) 0.500000 0.8355(6) 0.040(3) Uani 1 2 d S T P . .
H1A H 0.245180 0.500000 0.849563 0.061 Uiso 1 2 calc R U P . .
H1B H 0.170652 0.625767 0.851414 0.061 Uiso 0.5 1 calc R U P . .
H1C H 0.170652 0.374233 0.851414 0.061 Uiso 0.5 1 calc R U P . .
C2 C 0.2110(7) 0.500000 0.7340(6) 0.033(2) Uani 1 2 d S T P . .
H2 H 0.264430 0.500000 0.755827 0.040 Uiso 1 2 calc R U P . .
C3 C 0.1856(7) 0.500000 0.6694(6) 0.032(2) Uani 1 2 d S T P . .
H3 H 0.220932 0.500000 0.646461 0.039 Uiso 1 2 calc R U P . .
C4 C 0.1067(7) 0.500000 0.6384(6) 0.031(2) Uani 1 2 d S T P . .
C5 C 0.0570(7) 0.500000 0.6730(6) 0.031(2) Uani 1 2 d S T P . .
H5 H 0.003312 0.500000 0.652335 0.037 Uiso 1 2 calc R U P . .
C6 C 0.0848(7) 0.500000 0.7377(6) 0.033(2) Uani 1 2 d S T P . .
H6 H 0.050389 0.500000 0.761514 0.040 Uiso 1 2 calc R U P . .
C7 C 0.0767(7) 0.500000 0.5699(5) 0.027(2) Uani 1 2 d S T P . .
C8 C 0.0012(7) 0.500000 0.5321(5) 0.026(2) Uani 1 2 d S T P . .
C9 C -0.0784(7) 0.500000 0.5331(6) 0.027(2) Uani 1 2 d S T P . .
C10 C 0.1439(11) 0.500000 0.0759(11) 0.078(7) Uani 1 2 d S T P . .
H10A H 0.149565 0.500000 0.120758 0.118 Uiso 1 2 calc R U P . .
H10B H 0.115717 0.625767 0.056216 0.118 Uiso 0.5 1 calc R U P . .
H10C H 0.115717 0.374233 0.056216 0.118 Uiso 0.5 1 calc R U P . .
C11 C 0.2850(11) 0.500000 0.1207(9) 0.068(6) Uani 1 2 d S T P . .
H11 H 0.279187 0.500000 0.161245 0.082 Uiso 1 2 calc R U P . .
C12 C 0.3565(10) 0.500000 0.1149(8) 0.058(4) Uani 1 2 d S T P . .
H12 H 0.400261 0.500000 0.151327 0.070 Uiso 1 2 calc R U P . .
C13 C 0.3658(7) 0.500000 0.0556(5) 0.029(2) Uani 1 2 d S T P . .
C14 C 0.2993(8) 0.500000 0.0040(7) 0.037(3) Uani 1 2 d S T P . .
H14 H 0.303207 0.500000 -0.037106 0.045 Uiso 1 2 calc R U P . .
C15 C 0.2284(8) 0.500000 0.0118(8) 0.044(3) Uani 1 2 d S T P . .
H15 H 0.184080 0.500000 -0.024171 0.053 Uiso 1 2 calc R U P . .
C16 C 0.4388(7) 0.500000 0.0464(5) 0.025(2) Uani 1 2 d S T P . .
C17 C 0.4595(6) 0.500000 -0.0084(5) 0.025(2) Uani 1 2 d S T P . .
C18 C 0.4294(6) 0.500000 -0.0753(6) 0.027(2) Uani 1 2 d S T P . .
N1 N 0.1602(6) 0.500000 0.7666(5) 0.032(2) Uani 1 2 d S T P . .
N2 N 0.1219(6) 0.500000 0.5321(5) 0.029(2) Uani 1 2 d S T P . .
H2A H 0.172233 0.500000 0.546285 0.035 Uiso 1 2 calc R U P . .
N3 N 0.2205(8) 0.500000 0.0677(7) 0.054(3) Uani 1 2 d S T P . .
N4 N 0.5067(6) 0.500000 0.0961(4) 0.0285(19) Uani 1 2 d S T P . .
H4 H 0.509197 0.500000 0.135800 0.034 Uiso 1 2 calc R U P . .
O1 O -0.1062(5) 0.500000 0.5745(4) 0.0356(19) Uani 1 2 d S T P . .
O2 O 0.3614(5) 0.500000 -0.1124(4) 0.037(2) Uani 1 2 d S T P . .
O3 O 0.7444(15) 0.500000 0.6091(13) 0.128(8) Uani 1 2 d S T P . .
O4 O 0.885(3) 0.500000 0.722(2) 0.212(17) Uani 1 2 d S TU P . .
Br1 Br 0.500000 0.500000 0.500000 0.122(2) Uani 1 4 d S T P . .
Br2 Br 0.35857(18) 0.500000 0.29398(17) 0.1207(14) Uani 1 2 d S T P . .
Br3 Br 0.56754(12) 0.500000 0.25545(7) 0.0507(4) Uani 1 2 d S T P . .
Br4 Br 0.69225(8) 0.500000 0.44269(8) 0.0473(4) Uani 1 2 d S T P . .
Br5 Br 0.51914(11) 0.000000 0.37995(11) 0.1005(12) Uani 1 2 d S T P . .
Pb1 Pb 0.52292(3) 0.500000 0.37535(3) 0.0440(3) Uani 1 2 d S T P . .


_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 N1 1.470(17) . ?
C2 N1 1.359(17) . ?
C2 C3 1.375(18) . ?
C3 C4 1.398(17) . ?
C4 C5 1.378(19) . ?
C4 C7 1.461(17) . ?
C5 C6 1.379(18) . ?
C6 N1 1.335(17) . ?
C7 N2 1.363(15) . ?
C7 C8 1.381(17) . ?
C8 C8 1.43(2) 5_566 ?
C8 C9 1.473(16) . ?
C9 O1 1.195(15) . ?
C9 N2 1.431(15) 5_566 ?
C10 N3 1.48(2) . ?
C11 C12 1.36(2) . ?
C11 N3 1.39(2) . ?
C12 C13 1.40(2) . ?
C13 C14 1.394(19) . ?
C13 C16 1.424(17) . ?
C14 C15 1.37(2) . ?
C15 N3 1.31(2) . ?
C16 N4 1.388(15) . ?
C16 C17 1.400(15) . ?
C17 C17 1.42(2) 5_665 ?
C17 C18 1.428(17) . ?
C18 O2 1.266(15) . ?
C18 N4 1.395(16) 5_665 ?
Br1 Pb1 2.9618(5) . ?
Br1 Pb1 2.9619(5) 5_666 ?
Br2 Pb1 3.000(3) . ?
Br3 Pb1 3.0552(16) . ?
Br4 Pb1 3.0047(15) . ?
Br5 Pb1 3.18431(17) . ?
Br5 Pb1 3.18431(18) 1_545 ?

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
N1 C2 C3 120.4(12) . . ?
C2 C3 C4 118.7(12) . . ?
C5 C4 C3 119.2(12) . . ?
C5 C4 C7 119.8(11) . . ?
C3 C4 C7 120.9(12) . . ?
C6 C5 C4 120.3(11) . . ?
N1 C6 C5 119.7(12) . . ?
N2 C7 C8 108.1(10) . . ?
N2 C7 C4 123.6(11) . . ?
C8 C7 C4 128.3(11) . . ?
C7 C8 C8 108.9(13) . 5_566 ?
C7 C8 C9 143.5(11) . . ?
C8 C8 C9 107.5(12) 5_566 . ?
O1 C9 N2 123.9(11) . 5_566 ?
O1 C9 C8 133.2(12) . . ?
N2 C9 C8 102.8(9) 5_566 . ?
C12 C11 N3 120.4(16) . . ?
C11 C12 C13 120.3(16) . . ?
C14 C13 C12 116.9(13) . . ?
C14 C13 C16 120.1(11) . . ?
C12 C13 C16 123.0(12) . . ?
C15 C14 C13 121.1(13) . . ?
N3 C15 C14 121.4(14) . . ?
N4 C16 C17 106.3(10) . . ?
N4 C16 C13 122.3(10) . . ?
C17 C16 C13 131.3(11) . . ?
C16 C17 C17 108.7(12) . 5_665 ?
C16 C17 C18 143.4(10) . . ?
C17 C17 C18 108.0(11) 5_665 . ?
O2 C18 N4 122.9(11) . 5_665 ?
O2 C18 C17 131.9(11) . . ?
N4 C18 C17 105.2(9) 5_665 . ?
C6 N1 C2 121.7(11) . . ?
C6 N1 C1 119.1(11) . . ?
C2 N1 C1 119.2(11) . . ?
C7 N2 C9 112.6(9) . 5_566 ?
C15 N3 C11 119.9(13) . . ?
C15 N3 C10 121.3(16) . . ?
C11 N3 C10 118.8(16) . . ?
C16 N4 C18 111.8(9) . 5_665 ?
Pb1 Br1 Pb1 180.0 . 5_666 ?
Pb1 Br5 Pb1 174.90(8) . 1_545 ?
Br1 Pb1 Br2 99.13(8) . . ?
Br1 Pb1 Br4 87.65(4) . . ?
Br2 Pb1 Br4 173.22(8) . . ?
Br1 Pb1 Br3 172.99(4) . . ?
Br2 Pb1 Br3 87.88(8) . . ?
Br4 Pb1 Br3 85.34(5) . . ?
Br1 Pb1 Br5 87.60(4) . 1_565 ?
Br2 Pb1 Br5 89.52(4) . 1_565 ?
Br4 Pb1 Br5 90.77(4) . 1_565 ?
Br3 Pb1 Br5 92.49(4) . 1_565 ?
Br1 Pb1 Br5 87.60(4) . . ?
Br2 Pb1 Br5 89.52(4) . . ?
Br4 Pb1 Br5 90.77(4) . . ?
Br3 Pb1 Br5 92.49(4) . . ?
Br5 Pb1 Br5 174.90(7) 1_565 . ?

_refine_diff_density_max         3.611
_refine_diff_density_min         -2.722
_refine_diff_density_rms         0.299


# start Validation Reply Form
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  0.83Ang From Br3             3.58 eA-3  
RESPONSE: This residual density peak near the heavy atom is due to the use 
of Cu X-ray diffraction source and can not be assigned to 
unaccounted atom type or twinning error.
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O3 Check 
RESPONSE: The hydrogen atoms belonging to the hydronium cluster couldn't be modeled.
;
_vrf_PLAT972_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  0.57Ang From Br2            -2.81 eA-3  
RESPONSE: This residual density peak near the heavy atom is due to the use 
of Cu X-ray diffraction source and can not be assigned to 
unaccounted atom type or twinning error.
;
# 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_DPPPy-BiBr5
_database_code_depnum_ccdc_archive 'CCDC 2494692'
loop_
_audit_author_name
_audit_author_address
'Alexandre Abherve' 'Laboratoire MOLTECH Anjou, CNRS, Univ Angers'
_audit_update_record             
;
2025-10-11 deposited with the CCDC.	2026-04-02 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         'C18 H16 Bi Br5 N4 O2'
_chemical_formula_sum            'C18 H16 Bi Br5 N4 O2'
_chemical_formula_weight         928.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.0111 8.9310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.1538(10)
_cell_length_b                   20.3764(13)
_cell_length_c                   9.0431(7)
_cell_angle_alpha                90
_cell_angle_beta                 100.093(7)
_cell_angle_gamma                90
_cell_volume                     2386.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    230.00(10)
_cell_measurement_reflns_used    1804
_cell_measurement_theta_min      4.0430
_cell_measurement_theta_max      71.5590

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.586
_exptl_crystal_F_000             1704
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    24.512
_shelx_estimated_absorpt_T_min   0.216
_shelx_estimated_absorpt_T_max   0.640
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.744
_oxdiff_exptl_absorpt_empirical_full_max 1.410
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      230.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            4990
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         4.045
_diffrn_reflns_theta_max         72.147
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2291
_reflns_number_gt                1850
_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       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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)+(0.0598P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2291
_refine_ls_number_parameters     138
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0535
_refine_ls_wR_factor_ref         0.1356
_refine_ls_wR_factor_gt          0.1260
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
C1 C 0.3168(12) 0.7405(8) 0.1990(17) 0.054(3) Uani 1 1 d . . . . .
H1A H 0.282570 0.781287 0.215935 0.080 Uiso 1 1 calc R U . . .
H1B H 0.386199 0.740504 0.256971 0.080 Uiso 1 1 calc R U . . .
H1C H 0.320030 0.736298 0.093091 0.080 Uiso 1 1 calc R U . . .
C2 C 0.2900(10) 0.6227(7) 0.2340(16) 0.046(3) Uani 1 1 d . . . . .
H2 H 0.349884 0.614150 0.193701 0.056 Uiso 1 1 calc R U . . .
C3 C 0.2356(9) 0.5721(6) 0.2799(13) 0.039(3) Uani 1 1 d . . . . .
H3 H 0.256407 0.528767 0.265987 0.047 Uiso 1 1 calc R U . . .
C4 C 0.1505(9) 0.5832(6) 0.3465(13) 0.035(2) Uani 1 1 d . . . . .
C5 C 0.1209(9) 0.6484(6) 0.3606(13) 0.036(2) Uani 1 1 d . . . . .
H5 H 0.063179 0.657948 0.405144 0.043 Uiso 1 1 calc R U . . .
C6 C 0.1741(9) 0.6975(6) 0.3111(14) 0.038(3) Uani 1 1 d . . . . .
H6 H 0.153150 0.741126 0.321413 0.045 Uiso 1 1 calc R U . . .
C7 C 0.0944(9) 0.5304(6) 0.4069(13) 0.036(2) Uani 1 1 d . . . . .
C8 C 0.0124(8) 0.5320(6) 0.4834(12) 0.030(2) Uani 1 1 d . . . . .
C9 C -0.0562(9) 0.5771(6) 0.5435(13) 0.037(2) Uani 1 1 d . . . . .
N1 N 0.2585(8) 0.6850(5) 0.2460(11) 0.037(2) Uani 1 1 d . . . . .
N2 N 0.1194(8) 0.4656(5) 0.3886(11) 0.036(2) Uani 1 1 d . . . . .
H2A H 0.167972 0.452555 0.341290 0.043 Uiso 1 1 calc R U . . .
O1 O -0.0664(7) 0.6369(4) 0.5402(11) 0.047(2) Uani 1 1 d . . . . .
Br1 Br 0.99766(11) 0.80846(7) 0.03811(15) 0.0482(4) Uani 1 1 d . . . . .
Br2 Br 1.21762(9) 0.89632(7) 0.30341(15) 0.0414(3) Uani 1 1 d . . . . .
Br3 Br 1.000000 1.000000 0.500000 0.148(2) Uani 1 2 d S . P . .
Bi1 Bi 1.000000 0.90381(3) 0.250000 0.0277(2) Uani 1 2 d S T P . .


_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 N1 1.470(18) . ?
C2 N1 1.345(18) . ?
C2 C3 1.36(2) . ?
C3 C4 1.380(18) . ?
C4 C5 1.396(17) . ?
C4 C7 1.463(18) . ?
C5 C6 1.343(18) . ?
C6 N1 1.368(16) . ?
C7 N2 1.377(16) . ?
C7 C8 1.380(17) . ?
C8 C8 1.39(2) 5_566 ?
C8 C9 1.459(17) . ?
C9 O1 1.225(16) . ?
C9 N2 1.416(16) 5_566 ?
Br1 Bi1 2.7252(13) . ?
Br2 Bi1 2.8224(12) . ?
Br3 Bi1 2.9921(4) 5_776 ?
Br3 Bi1 2.9921(4) . ?

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
N1 C2 C3 120.2(12) . . ?
C2 C3 C4 121.3(12) . . ?
C3 C4 C5 117.1(12) . . ?
C3 C4 C7 122.9(11) . . ?
C5 C4 C7 119.9(11) . . ?
C6 C5 C4 120.6(11) . . ?
C5 C6 N1 121.0(11) . . ?
N2 C7 C8 107.9(11) . . ?
N2 C7 C4 120.9(10) . . ?
C8 C7 C4 131.2(11) . . ?
C7 C8 C8 108.6(13) . 5_566 ?
C7 C8 C9 142.3(11) . . ?
C8 C8 C9 109.0(12) 5_566 . ?
O1 C9 N2 123.5(11) . 5_566 ?
O1 C9 C8 133.5(11) . . ?
N2 C9 C8 102.9(10) 5_566 . ?
C2 N1 C6 119.7(11) . . ?
C2 N1 C1 121.2(11) . . ?
C6 N1 C1 119.0(11) . . ?
C7 N2 C9 111.5(10) . 5_566 ?
Bi1 Br3 Bi1 180.000(16) 5_776 . ?
Br1 Bi1 Br1 89.05(7) 2_755 . ?
Br1 Bi1 Br2 88.16(4) 2_755 2_755 ?
Br1 Bi1 Br2 87.42(4) . 2_755 ?
Br1 Bi1 Br2 87.42(4) 2_755 . ?
Br1 Bi1 Br2 88.16(4) . . ?
Br2 Bi1 Br2 173.80(6) 2_755 . ?
Br1 Bi1 Br3 86.40(3) 2_755 . ?
Br1 Bi1 Br3 175.40(4) . . ?
Br2 Bi1 Br3 91.74(3) 2_755 . ?
Br2 Bi1 Br3 92.31(3) . . ?
Br1 Bi1 Br3 175.40(4) 2_755 2_755 ?
Br1 Bi1 Br3 86.40(3) . 2_755 ?
Br2 Bi1 Br3 92.31(3) 2_755 2_755 ?
Br2 Bi1 Br3 91.74(3) . 2_755 ?
Br3 Bi1 Br3 98.151(17) . 2_755 ?

_refine_diff_density_max         2.044
_refine_diff_density_min         -1.704
_refine_diff_density_rms         0.250


# start Validation Reply Form
_vrf_PLAT242_DPPPy-BiBr5         
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Bi1 Check 
RESPONSE: One of the three bromide anions linked to the metal center presents
a relatively high Ueq which couldn't be improved, possibly because this
bromide anion is located on a special position.
;
_vrf_PLAT973_DPPPy-BiBr5         
;
PROBLEM: Check Calcd Positive Resid. Density on       Bi1       1.55 eA-3  
RESPONSE: This residual density peak near the heavy atom is due to the use 
of Cu X-ray diffraction source and can not be assigned to 
unaccounted atom type or twinning error.
;
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2494691'
loop_
_audit_author_name
_audit_author_address
'Alexandre Abherve' 'Laboratoire MOLTECH Anjou, CNRS, Univ Angers'
_audit_update_record             
;
2025-10-11 deposited with the CCDC.	2026-04-02 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         'C22 H28 I6 N4 O4 Pb2 S2'
_chemical_formula_sum            'C22 H28 I6 N4 O4 Pb2 S2'
_chemical_formula_weight         1652.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'
'-x, -y, -z'

_cell_length_a                   8.1967(4)
_cell_length_b                   9.1368(4)
_cell_length_c                   13.2153(6)
_cell_angle_alpha                102.695(4)
_cell_angle_beta                 95.518(4)
_cell_angle_gamma                93.869(4)
_cell_volume                     957.04(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    200.01(10)
_cell_measurement_reflns_used    4604
_cell_measurement_theta_min      3.3560
_cell_measurement_theta_max      71.7930

_exptl_crystal_description       platelet
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.867
_exptl_crystal_F_000             734
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    56.178
_shelx_estimated_absorpt_T_min   0.033
_shelx_estimated_absorpt_T_max   0.134
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.235
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.398
_oxdiff_exptl_absorpt_empirical_full_max 2.838
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200.01(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            6755
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.451
_diffrn_reflns_theta_max         72.169
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             3603
_reflns_number_gt                3344
_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       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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)+(0.1566P)²+7.0166P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3603
_refine_ls_number_parameters     183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0789
_refine_ls_wR_factor_ref         0.2101
_refine_ls_wR_factor_gt          0.2055
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_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
C1 C 0.4471(19) 0.5081(15) 0.6390(12) 0.033(3) Uani 1 1 d . . . . .
H1A H 0.560159 0.555132 0.657423 0.049 Uiso 1 1 calc R U . . .
H1B H 0.442811 0.404521 0.648511 0.049 Uiso 1 1 calc R U . . .
H1C H 0.410899 0.506917 0.565946 0.049 Uiso 1 1 calc R U . . .
C2 C 0.1806(15) 0.5495(15) 0.6945(10) 0.025(2) Uani 1 1 d . . . . .
H2 H 0.137094 0.463634 0.641801 0.030 Uiso 1 1 calc R U . . .
C3 C 0.0764(15) 0.6290(13) 0.7596(9) 0.020(2) Uani 1 1 d . . . . .
H3 H -0.037388 0.595860 0.751915 0.024 Uiso 1 1 calc R U . . .
C4 C 0.1385(14) 0.7560(12) 0.8353(8) 0.015(2) Uani 1 1 d . . . . .
C5 C 0.3074(15) 0.8011(12) 0.8430(9) 0.020(2) Uani 1 1 d . . . . .
H5 H 0.354724 0.889209 0.892380 0.024 Uiso 1 1 calc R U . . .
C6 C 0.4019(15) 0.7156(13) 0.7780(9) 0.020(2) Uani 1 1 d . . . . .
H6 H 0.516639 0.744380 0.784416 0.024 Uiso 1 1 calc R U . . .
C7 C 0.0357(13) 0.8424(12) 0.9067(8) 0.015(2) Uani 1 1 d . . . . .
C8 C 0.0728(13) 0.9816(12) 0.9747(8) 0.014(2) Uani 1 1 d . . . . .
C9 C 0.2016(14) 1.1053(13) 1.0163(9) 0.019(2) Uani 1 1 d . . . . .
C10 C 0.043(5) 0.702(4) 0.154(3) 0.103(11) Uani 1 1 d . . . . .
H10A H -0.002042 0.778021 0.119611 0.154 Uiso 1 1 calc R U . A 1
H10B H -0.045068 0.624051 0.154294 0.154 Uiso 1 1 calc R U . A 1
H10C H 0.087158 0.750482 0.226104 0.154 Uiso 1 1 calc R U . A 1
C11 C 0.339(5) 0.786(3) 0.132(3) 0.100(11) Uani 1 1 d . . . . .
H11A H 0.306872 0.863274 0.094809 0.150 Uiso 1 1 calc R U . B 1
H11B H 0.336544 0.823773 0.206895 0.150 Uiso 1 1 calc R U . B 1
H11C H 0.450564 0.761061 0.118278 0.150 Uiso 1 1 calc R U . B 1
N1 N 0.3396(14) 0.5932(11) 0.7058(8) 0.022(2) Uani 1 1 d . . . . .
N2 N -0.1249(12) 0.7911(10) 0.9131(7) 0.0173(18) Uani 1 1 d . . . . .
H2A H -0.173212 0.703767 0.877048 0.021 Uiso 1 1 calc R U . . .
O1 O 0.3438(12) 1.1229(10) 1.0004(8) 0.0285(19) Uani 1 1 d . . . . .
O2 O 0.264(2) 0.4946(13) 0.1542(13) 0.061(4) Uani 1 1 d . . . . .
I1 I 0.23898(10) 0.14661(11) 0.36248(7) 0.0333(3) Uani 1 1 d . . . . .
I4 I 0.28178(11) 0.12175(10) 0.69022(7) 0.0347(3) Uani 1 1 d . . . . .
I5 I 0.21696(10) -0.28278(8) 0.45458(7) 0.0290(3) Uani 1 1 d . . . . .
Pb1 Pb 0.500000 0.000000 0.500000 0.0236(3) Uani 1 2 d S . P . .
Pb2 Pb 0.000000 0.000000 0.500000 0.0197(2) Uani 1 2 d S . P . .
S1A S 0.1992(10) 0.6212(9) 0.0867(6) 0.0595(16) Uiso 0.7 1 d . . P C 1
S1B S 0.295(2) 0.658(2) 0.1820(14) 0.060(4) Uiso 0.3 1 d . . P C 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
C1 N1 1.449(15) . ?
C2 N1 1.321(18) . ?
C2 C3 1.395(15) . ?
C3 C4 1.385(16) . ?
C4 C5 1.405(17) . ?
C4 C7 1.463(15) . ?
C5 C6 1.365(16) . ?
C6 N1 1.335(17) . ?
C7 C8 1.382(16) . ?
C7 N2 1.384(15) . ?
C8 C8 1.45(2) 2_577 ?
C8 C9 1.466(16) . ?
C9 O1 1.211(16) . ?
C9 N2 1.402(15) 2_577 ?
C10 S1A 1.75(4) . ?
C10 S1B 2.15(4) . ?
C11 S1B 1.51(4) . ?
C11 S1A 1.78(3) . ?
O2 S1B 1.45(2) . ?
O2 S1A 1.690(19) . ?
I1 Pb2 3.2148(8) . ?
I1 Pb1 3.2224(8) . ?
I4 Pb2 3.1936(8) . ?
I4 Pb1 3.2650(10) . ?
I5 Pb2 3.2159(7) . ?
I5 Pb1 3.2649(8) . ?

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
N1 C2 C3 120.3(12) . . ?
C4 C3 C2 120.2(11) . . ?
C3 C4 C5 117.8(10) . . ?
C3 C4 C7 122.6(10) . . ?
C5 C4 C7 119.6(10) . . ?
C6 C5 C4 118.5(11) . . ?
N1 C6 C5 122.7(12) . . ?
C8 C7 N2 108.8(9) . . ?
C8 C7 C4 129.2(10) . . ?
N2 C7 C4 121.9(10) . . ?
C7 C8 C8 107.3(12) . 2_577 ?
C7 C8 C9 144.7(10) . . ?
C8 C8 C9 108.0(12) 2_577 . ?
O1 C9 N2 124.1(11) . 2_577 ?
O1 C9 C8 132.1(11) . . ?
N2 C9 C8 103.9(9) 2_577 . ?
C2 N1 C6 120.5(11) . . ?
C2 N1 C1 119.8(12) . . ?
C6 N1 C1 119.7(12) . . ?
C7 N2 C9 112.0(9) . 2_577 ?
Pb2 I1 Pb1 79.087(18) . . ?
Pb2 I4 Pb1 78.766(19) . . ?
Pb2 I5 Pb1 78.448(17) . . ?
I1 Pb1 I1 180.00(3) 2_656 . ?
I1 Pb1 I5 84.29(2) 2_656 2_656 ?
I1 Pb1 I5 95.71(2) . 2_656 ?
I1 Pb1 I5 95.71(2) 2_656 . ?
I1 Pb1 I5 84.29(2) . . ?
I5 Pb1 I5 180.0 2_656 . ?
I1 Pb1 I4 84.66(2) 2_656 2_656 ?
I1 Pb1 I4 95.34(2) . 2_656 ?
I5 Pb1 I4 81.04(2) 2_656 2_656 ?
I5 Pb1 I4 98.96(2) . 2_656 ?
I1 Pb1 I4 95.34(2) 2_656 . ?
I1 Pb1 I4 84.66(2) . . ?
I5 Pb1 I4 98.96(2) 2_656 . ?
I5 Pb1 I4 81.04(2) . . ?
I4 Pb1 I4 180.0 2_656 . ?
I4 Pb2 I4 180.0 2_556 . ?
I4 Pb2 I1 85.95(2) 2_556 2_556 ?
I4 Pb2 I1 94.05(2) . 2_556 ?
I4 Pb2 I1 94.05(2) 2_556 . ?
I4 Pb2 I1 85.95(2) . . ?
I1 Pb2 I1 180.0 2_556 . ?
I4 Pb2 I5 82.89(2) 2_556 2_556 ?
I4 Pb2 I5 97.11(2) . 2_556 ?
I1 Pb2 I5 85.21(2) 2_556 2_556 ?
I1 Pb2 I5 94.79(2) . 2_556 ?
I4 Pb2 I5 97.11(2) 2_556 . ?
I4 Pb2 I5 82.89(2) . . ?
I1 Pb2 I5 94.79(2) 2_556 . ?
I1 Pb2 I5 85.21(2) . . ?
I5 Pb2 I5 180.00(2) 2_556 . ?
O2 S1A C10 104.2(13) . . ?
O2 S1A C11 106.2(12) . . ?
C10 S1A C11 93.1(19) . . ?
O2 S1B C11 139(2) . . ?
O2 S1B C10 95.7(16) . . ?
C11 S1B C10 87.0(19) . . ?

_refine_diff_density_max         5.307
_refine_diff_density_min         -6.736
_refine_diff_density_rms         0.654


# start Validation Reply Form
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  0.87Ang From S1A             5.03 eA-3  
RESPONSE: This residual density peak near the heavy atom is due to the use 
of Cu X-ray diffraction source and can not be assigned to 
unaccounted atom type or twinning error.
;
_vrf_PLAT972_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  0.86Ang From Pb2            -6.49 eA-3  
RESPONSE: This residual density peak near the heavy atom is due to the use 
of Cu X-ray diffraction source and can not be assigned to 
unaccounted atom type or twinning error.
;
_vrf_PLAT973_shelx               
;
PROBLEM: Check Calcd Positive Resid. Density on       Pb2       1.83 eA-3  
RESPONSE: This residual density peak near the heavy atom is due to the use 
of Cu X-ray diffraction source and can not be assigned to 
unaccounted atom type or twinning error.
;
# 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_DPPPy2-Pb2Br9-P1
_database_code_depnum_ccdc_archive 'CCDC 2494688'
loop_
_audit_author_name
_audit_author_address
'Alexandre Abherve' 'Laboratoire MOLTECH Anjou, CNRS, Univ Angers'
_audit_update_record             
;
2025-10-11 deposited with the CCDC.	2026-04-02 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         'C36 H32 Br9 N8 O4 Pb2, H3O, 5 H2O'
_chemical_formula_sum            'C36 H45 Br9 N8 O10 Pb2'
_chemical_formula_weight         1883.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'
'-x, -y, -z'

_cell_length_a                   9.9282(2)
_cell_length_b                   10.0715(3)
_cell_length_c                   13.1792(3)
_cell_angle_alpha                78.571(2)
_cell_angle_beta                 89.853(2)
_cell_angle_gamma                85.428(2)
_cell_volume                     1287.45(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    200.00(10)
_cell_measurement_reflns_used    15838
_cell_measurement_theta_min      3.3840
_cell_measurement_theta_max      76.0920

_exptl_crystal_description       platelet
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.429
_exptl_crystal_F_000             876
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    21.243
_shelx_estimated_absorpt_T_min   0.155
_shelx_estimated_absorpt_T_max   0.362
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.039
_exptl_absorpt_correction_T_max  0.222
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.397
_oxdiff_exptl_absorpt_empirical_full_max 3.376
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            21357
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.422
_diffrn_reflns_theta_max         76.284
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             5203
_reflns_number_gt                5132
_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       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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)+(0.0894P)²+1.0534P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5203
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1150
_refine_ls_wR_factor_gt          0.1145
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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
C1 C 0.1404(6) 0.5935(6) 0.1135(5) 0.0413(12) Uani 1 1 d . . . . .
H1A H 0.110097 0.631754 0.042216 0.062 Uiso 1 1 calc R U . . .
H1B H 0.234092 0.554671 0.113295 0.062 Uiso 1 1 calc R U . . .
H1C H 0.082524 0.522108 0.144268 0.062 Uiso 1 1 calc R U . . .
C2 C 0.1681(6) 0.6743(6) 0.2744(4) 0.0375(11) Uani 1 1 d . . . . .
H2 H 0.195577 0.583242 0.306807 0.045 Uiso 1 1 calc R U . . .
C3 C 0.1663(6) 0.7759(5) 0.3315(4) 0.0367(11) Uani 1 1 d . . . . .
H3 H 0.190869 0.755045 0.402840 0.044 Uiso 1 1 calc R U . . .
C4 C 0.1278(5) 0.9092(5) 0.2827(4) 0.0297(9) Uani 1 1 d . . . . .
C5 C 0.0876(5) 0.9358(5) 0.1792(4) 0.0328(10) Uani 1 1 d . . . . .
H5 H 0.058283 1.025702 0.145208 0.039 Uiso 1 1 calc R U . . .
C6 C 0.0907(5) 0.8300(6) 0.1266(4) 0.0361(10) Uani 1 1 d . . . . .
H6 H 0.063544 0.847305 0.055796 0.043 Uiso 1 1 calc R U . . .
C7 C 0.1290(5) 1.0175(5) 0.3417(4) 0.0302(9) Uani 1 1 d . . . . .
C8 C 0.1536(5) 1.0105(5) 0.4458(4) 0.0307(9) Uani 1 1 d . . . . .
C9 C 0.1832(5) 0.9164(5) 0.5436(4) 0.0315(9) Uani 1 1 d . . . . .
C10 C 0.1775(5) 1.1378(5) 0.5678(4) 0.0297(9) Uani 1 1 d . . . . .
C11 C 0.1491(5) 1.1452(5) 0.4641(4) 0.0321(10) Uani 1 1 d . . . . .
C12 C 0.1197(5) 1.2386(5) 0.3656(4) 0.0330(10) Uani 1 1 d . . . . .
C13 C 0.1881(5) 1.2467(5) 0.6243(4) 0.0314(9) Uani 1 1 d . . . . .
C14 C 0.2220(6) 1.2210(6) 0.7282(4) 0.0379(11) Uani 1 1 d . . . . .
H14 H 0.241339 1.130172 0.764574 0.046 Uiso 1 1 calc R U . . .
C15 C 0.2279(6) 1.3285(6) 0.7793(4) 0.0377(11) Uani 1 1 d . . . . .
H15 H 0.250761 1.310610 0.850898 0.045 Uiso 1 1 calc R U . . .
C16 C 0.1708(6) 1.4840(6) 0.6280(5) 0.0401(12) Uani 1 1 d . . . . .
H16 H 0.153548 1.575952 0.593345 0.048 Uiso 1 1 calc R U . . .
C17 C 0.1637(6) 1.3814(6) 0.5739(4) 0.0399(11) Uani 1 1 d . . . . .
H17 H 0.142181 1.402404 0.502060 0.048 Uiso 1 1 calc R U . . .
C18 C 0.2037(7) 1.5688(6) 0.7873(5) 0.0460(13) Uani 1 1 d . . . . .
H18A H 0.182644 1.655725 0.739471 0.069 Uiso 1 1 calc R U . . .
H18B H 0.136028 1.557221 0.841936 0.069 Uiso 1 1 calc R U . . .
H18C H 0.293436 1.567707 0.818324 0.069 Uiso 1 1 calc R U . . .
N1 N 0.1320(4) 0.7021(4) 0.1749(4) 0.0330(9) Uani 1 1 d . . . . .
N2 N 0.1047(4) 1.1535(4) 0.2954(3) 0.0318(8) Uani 1 1 d . . . . .
H2A H 0.082476 1.182614 0.229713 0.038 Uiso 1 1 calc R U . . .
N3 N 0.1975(4) 1.0016(4) 0.6147(3) 0.0325(8) Uani 1 1 d . . . . .
H3A H 0.216768 0.972118 0.680842 0.039 Uiso 1 1 calc R U . . .
N4 N 0.2020(4) 1.4553(4) 0.7294(3) 0.0340(9) Uani 1 1 d . . . . .
O1 O 0.1928(4) 0.7922(4) 0.5671(3) 0.0401(8) Uani 1 1 d . . . . .
O2 O 0.1065(4) 1.3631(4) 0.3422(3) 0.0387(8) Uani 1 1 d . . . . .
O3 O 0.5053(6) 1.1705(6) 0.5650(4) 0.0632(13) Uani 1 1 d . . . . .
O4 O 0.5509(8) 1.4182(6) 0.5707(5) 0.0785(18) Uani 1 1 d . . . . .
O5 O 0.4538(8) 1.4935(7) 0.2566(5) 0.0785(18) Uani 1 1 d . . . . .
Br1 Br 0.77226(5) 1.13495(6) 0.12602(4) 0.03544(14) Uani 1 1 d . . . . .
Br2 Br 0.45913(6) 0.87256(6) 0.13440(5) 0.04168(15) Uani 1 1 d . . . . .
Br3 Br 0.17544(6) 0.26421(6) 0.04878(4) 0.03839(15) Uani 1 1 d . . . . .
Br4 Br 0.45993(6) 1.16090(7) 0.31464(5) 0.04695(17) Uani 1 1 d . . . . .
Br5 Br 0.500000 0.500000 0.000000 0.0478(2) Uani 1 2 d S . P . .
Pb1 Pb 0.48234(2) 1.17229(2) 0.08333(2) 0.03389(10) Uani 1 1 d . . . . .


_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 N1 1.482(6) . ?
C2 N1 1.330(7) . ?
C2 C3 1.384(7) . ?
C3 C4 1.393(7) . ?
C4 C5 1.389(7) . ?
C4 C7 1.461(6) . ?
C5 C6 1.381(7) . ?
C6 N1 1.351(7) . ?
C7 C8 1.381(7) . ?
C7 N2 1.387(7) . ?
C8 C11 1.421(7) . ?
C8 C9 1.456(7) . ?
C9 O1 1.224(6) . ?
C9 N3 1.404(6) . ?
C10 C11 1.382(7) . ?
C10 N3 1.387(7) . ?
C10 C13 1.454(6) . ?
C11 C12 1.459(8) . ?
C12 O2 1.227(7) . ?
C12 N2 1.396(6) . ?
C13 C14 1.379(7) . ?
C13 C17 1.389(8) . ?
C14 C15 1.388(7) . ?
C15 N4 1.321(7) . ?
C16 N4 1.342(7) . ?
C16 C17 1.373(7) . ?
C18 N4 1.495(6) . ?
Br1 Pb1 2.9146(5) . ?
Br2 Pb1 2.9873(7) . ?
Br2 Pb1 3.0397(6) 2_675 ?
Br3 Pb1 3.1207(6) 1_545 ?
Br4 Pb1 3.0361(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
N1 C2 C3 121.0(5) . . ?
C2 C3 C4 118.9(5) . . ?
C5 C4 C3 119.2(4) . . ?
C5 C4 C7 121.5(5) . . ?
C3 C4 C7 119.3(5) . . ?
C6 C5 C4 119.1(5) . . ?
N1 C6 C5 120.5(5) . . ?
C8 C7 N2 107.7(4) . . ?
C8 C7 C4 130.2(5) . . ?
N2 C7 C4 122.1(5) . . ?
C7 C8 C11 108.4(5) . . ?
C7 C8 C9 143.3(5) . . ?
C11 C8 C9 108.3(4) . . ?
O1 C9 N3 123.8(5) . . ?
O1 C9 C8 132.3(5) . . ?
N3 C9 C8 103.9(4) . . ?
C11 C10 N3 108.0(4) . . ?
C11 C10 C13 129.4(5) . . ?
N3 C10 C13 122.6(5) . . ?
C10 C11 C8 108.1(5) . . ?
C10 C11 C12 144.0(5) . . ?
C8 C11 C12 107.9(4) . . ?
O2 C12 N2 123.8(5) . . ?
O2 C12 C11 132.1(5) . . ?
N2 C12 C11 104.1(4) . . ?
C14 C13 C17 118.0(5) . . ?
C14 C13 C10 121.9(5) . . ?
C17 C13 C10 120.1(5) . . ?
C13 C14 C15 119.7(5) . . ?
N4 C15 C14 120.8(5) . . ?
N4 C16 C17 120.4(5) . . ?
C16 C17 C13 120.1(5) . . ?
C2 N1 C6 121.2(4) . . ?
C2 N1 C1 120.4(5) . . ?
C6 N1 C1 118.4(5) . . ?
C7 N2 C12 111.8(4) . . ?
C10 N3 C9 111.7(4) . . ?
C15 N4 C16 121.1(5) . . ?
C15 N4 C18 119.6(5) . . ?
C16 N4 C18 119.3(5) . . ?
Pb1 Br2 Pb1 95.218(18) . 2_675 ?
Br1 Pb1 Br2 91.430(17) . . ?
Br1 Pb1 Br4 84.292(17) . . ?
Br2 Pb1 Br4 85.802(19) . . ?
Br1 Pb1 Br2 88.381(16) . 2_675 ?
Br2 Pb1 Br2 84.781(18) . 2_675 ?
Br4 Pb1 Br2 167.91(2) . 2_675 ?
Br1 Pb1 Br3 169.441(18) . 1_565 ?
Br2 Pb1 Br3 97.965(17) . 1_565 ?
Br4 Pb1 Br3 91.566(17) . 1_565 ?
Br2 Pb1 Br3 97.227(16) 2_675 1_565 ?

_refine_diff_density_max         2.899
_refine_diff_density_min         -1.815
_refine_diff_density_rms         0.215


# start Validation Reply Form
_vrf_PLAT430_DPPPy2-Pb2Br9-P1    
;
PROBLEM: Short Inter D...A Contact  O4       ..O4       .       2.39 Ang.  
RESPONSE: The hydrogen atoms belonging to the hydronium cluster couldn't be modeled.
;
_vrf_PLAT306_DPPPy2-Pb2Br9-P1    
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O3 Check 
RESPONSE: The hydrogen atoms belonging to the hydronium cluster couldn't be modeled.
;
_vrf_PLAT780_DPPPy2-Pb2Br9-P1    
;
PROBLEM: Coordinates do not Form a Properly Connected Set     Please Do !  
RESPONSE: The isolated oxygen atoms belong to the hydronium cluster 
for which the hydrogen atoms couldn't be modeled.
;
_vrf_PLAT971_DPPPy2-Pb2Br9-P1    
;
PROBLEM: Check Calcd Resid. Dens.  0.78Ang From Pb1             2.68 eA-3  
RESPONSE: This residual density peak near the heavy atom is due to the use 
of Cu X-ray diffraction source and can not be assigned to unaccounted 
atom type or twinning error. 
;
# end Validation Reply Form


