# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_0gpa_good
_database_code_depnum_ccdc_archive 'CCDC 2365956'
loop_
_audit_author_name
_audit_author_address
'Maxime Deutsch' 'University of Lorraine'
_audit_update_record             
;
2024-06-26 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-02-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H9 F2 N4)'
_chemical_formula_sum            'C16 H18 F4 I4 N8 Pb'
_chemical_formula_weight         1113.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.9388(4)
_cell_length_b                   30.291(2)
_cell_length_c                   6.6444(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2604.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      25.555
_cell_measurement_theta_min      3.447
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.271
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0815 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.8060.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.839
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.050
_exptl_crystal_description       plate
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 0.406
_diffrn_reflns_Laue_measured_fraction_max 0.386
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            39725
_diffrn_reflns_point_group_measured_fraction_full 0.406
_diffrn_reflns_point_group_measured_fraction_max 0.386
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.048
_diffrn_reflns_theta_min         3.447
_diffrn_ambient_temperature      300(3)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.406
_diffrn_measured_fraction_theta_max 0.386
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON III CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                952
_reflns_number_total             1008
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1008
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0170
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0149P)²+4.7842P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0380
_refine_ls_wR_factor_ref         0.0389
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.33025(2) 0.750000 0.70263(4) 0.0384(5) Uani 1 2 d S T P . .
I1 I 0.33817(3) 0.750000 0.21208(6) 0.0451(7) Uani 1 2 d S T P . .
I2 I 0.08427(3) 0.750000 0.74351(7) 0.0550(7) Uani 1 2 d S T P . .
I3 I 0.31744(3) 0.64561(3) 0.68320(5) 0.0447(6) Uani 1 1 d . . . . .
F2 F 0.4485(3) 0.4173(3) 0.3461(5) 0.050(6) Uani 1 1 d . . . . .
F1 F 0.2680(2) 0.4508(2) 0.4196(4) 0.051(4) Uani 1 1 d . . . . .
N4 N 0.4037(3) 0.5930(4) 0.2127(6) 0.0316(11) Uiso 1 1 d . . . . .
N2 N 0.5021(3) 0.5995(4) 0.1606(5) 0.0327(10) Uiso 1 1 d . . . . .
C3 C 0.5020(3) 0.5309(5) 0.2257(6) 0.0257(11) Uiso 1 1 d . . . . .
C6 C 0.3401(4) 0.4792(5) 0.3510(7) 0.0317(12) Uiso 1 1 d . . . . .
N3 N 0.5649(3) 0.5643(3) 0.1660(5) 0.0326(9) Uiso 1 1 d . . . . .
N1 N 0.6954(3) 0.6424(4) 0.3273(7) 0.0493(12) Uiso 1 1 d . . . . .
H1A H 0.723267 0.654378 0.437002 0.074 Uiso 1 1 calc R U . . .
H1B H 0.738095 0.646032 0.223546 0.074 Uiso 1 1 calc R U . . .
H1C H 0.684810 0.613765 0.347804 0.074 Uiso 1 1 calc R U . . .
C2 C 0.5400(4) 0.6425(5) 0.1086(7) 0.0414(13) Uiso 1 1 d . . . . .
H2A H 0.482581 0.660796 0.065760 0.050 Uiso 1 1 calc R U . . .
H2B H 0.587576 0.639866 -0.003539 0.050 Uiso 1 1 calc R U . . .
C7 C 0.4397(4) 0.4609(6) 0.3142(9) 0.0342(16) Uiso 1 1 d . . . . .
C1 C 0.5945(4) 0.6646(5) 0.2827(7) 0.0468(15) Uiso 1 1 d . . . . .
H1D H 0.606662 0.695385 0.250316 0.056 Uiso 1 1 calc R U . . .
H1E H 0.550685 0.663448 0.401098 0.056 Uiso 1 1 calc R U . . .
C5 C 0.3188(4) 0.5228(5) 0.3241(7) 0.0325(12) Uiso 1 1 d . . . . .
H5 H 0.253606 0.534472 0.348958 0.039 Uiso 1 1 calc R U . . .
C4 C 0.4024(3) 0.5494(4) 0.2559(7) 0.0272(11) Uiso 1 1 d . . . . .
C8 C 0.5207(4) 0.4861(5) 0.2525(7) 0.0306(12) Uiso 1 1 d . . . . .
H8 H 0.585617 0.473992 0.229287 0.037 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.03094(16) 0.0484(16) 0.03582(17) 0.000 -0.00019(9) 0.000
I1 0.0476(3) 0.056(2) 0.0317(3) 0.000 0.00193(17) 0.000
I2 0.0266(2) 0.077(2) 0.0608(3) 0.000 0.0005(2) 0.000
I3 0.0464(2) 0.0490(18) 0.03882(19) -0.0001(3) -0.00016(12) 0.0031(3)
F2 0.057(2) 0.035(19) 0.058(2) -0.002(3) 0.0009(14) -0.002(3)
F1 0.0407(15) 0.053(13) 0.0602(18) 0.006(3) 0.0066(13) -0.011(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
Pb1 I1 3.3866(5) 1_556 ?
Pb1 I1 3.2610(5) . ?
Pb1 I2 3.3060(5) 6_657 ?
Pb1 I2 3.1943(5) . ?
Pb1 I3 3.1690(11) . ?
Pb1 I3 3.1691(11) 7_575 ?
F2 C7 1.342(19) . ?
F1 C6 1.348(11) . ?
N4 N2 1.335(6) . ?
N4 C4 1.349(15) . ?
N2 N3 1.343(12) . ?
N2 C2 1.433(16) . ?
C3 N3 1.358(13) . ?
C3 C4 1.420(10) . ?
C3 C8 1.387(16) . ?
C6 C7 1.424(12) . ?
C6 C5 1.361(18) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.498(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.511(11) . ?
C7 C8 1.361(15) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C5 H5 0.9300 . ?
C5 C4 1.424(13) . ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 176.466(18) . 1_556 ?
I1 Pb1 I2 94.415(13) . 6_657 ?
I2 Pb1 I1 96.679(13) . . ?
I2 Pb1 I1 86.855(13) . 1_556 ?
I2 Pb1 I1 82.052(13) 6_657 1_556 ?
I2 Pb1 I2 168.907(9) . 6_657 ?
I3 Pb1 I1 92.424(7) 7_575 1_556 ?
I3 Pb1 I1 87.760(7) 7_575 . ?
I3 Pb1 I1 92.425(7) . 1_556 ?
I3 Pb1 I1 87.760(7) . . ?
I3 Pb1 I2 93.233(7) . 6_657 ?
I3 Pb1 I2 87.213(7) 7_575 . ?
I3 Pb1 I2 87.212(7) . . ?
I3 Pb1 I2 93.232(8) 7_575 6_657 ?
I3 Pb1 I3 172.399(15) . 7_575 ?
Pb1 I1 Pb1 176.466(18) . 1_554 ?
Pb1 I2 Pb1 178.665(17) . 6_557 ?
N2 N4 C4 102.2(7) . . ?
N4 N2 N3 116.9(9) . . ?
N4 N2 C2 121.6(9) . . ?
N3 N2 C2 121.5(5) . . ?
N3 C3 C4 106.8(11) . . ?
N3 C3 C8 131.3(5) . . ?
C8 C3 C4 121.8(9) . . ?
F1 C6 C7 115.9(13) . . ?
F1 C6 C5 121.5(6) . . ?
C5 C6 C7 122.6(11) . . ?
N2 N3 C3 103.8(5) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N2 C2 H2A 109.2 . . ?
N2 C2 H2B 109.2 . . ?
N2 C2 C1 112.2(6) . . ?
H2A C2 H2B 107.9 . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
F2 C7 C6 115.6(10) . . ?
F2 C7 C8 122.4(9) . . ?
C8 C7 C6 122.0(16) . . ?
N1 C1 C2 111.1(8) . . ?
N1 C1 H1D 109.4 . . ?
N1 C1 H1E 109.4 . . ?
C2 C1 H1D 109.4 . . ?
C2 C1 H1E 109.4 . . ?
H1D C1 H1E 108.0 . . ?
C6 C5 H5 122.0 . . ?
C6 C5 C4 116.0(7) . . ?
C4 C5 H5 122.0 . . ?
N4 C4 C3 110.3(8) . . ?
N4 C4 C5 129.1(8) . . ?
C3 C4 C5 120.6(12) . . ?
C3 C8 H8 121.5 . . ?
C7 C8 C3 117.0(9) . . ?
C7 C8 H8 121.5 . . ?

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
F2 C7 C8 C3 -179.7(7) . . . . ?
F1 C6 C7 F2 2.1(10) . . . . ?
F1 C6 C7 C8 -177.3(5) . . . . ?
F1 C6 C5 C4 178.4(4) . . . . ?
N4 N2 N3 C3 0.6(5) . . . . ?
N4 N2 C2 C1 98.3(6) . . . . ?
N2 N4 C4 C3 -0.6(6) . . . . ?
N2 N4 C4 C5 178.9(5) . . . . ?
N2 C2 C1 N1 70.2(8) . . . . ?
C6 C7 C8 C3 -0.3(10) . . . . ?
C6 C5 C4 N4 178.5(6) . . . . ?
C6 C5 C4 C3 -2.1(8) . . . . ?
N3 N2 C2 C1 -79.3(8) . . . . ?
N3 C3 C4 N4 1.0(6) . . . . ?
N3 C3 C4 C5 -178.5(5) . . . . ?
N3 C3 C8 C7 -179.8(5) . . . . ?
C2 N2 N3 C3 178.3(5) . . . . ?
C7 C6 C5 C4 0.2(9) . . . . ?
C5 C6 C7 F2 -179.6(6) . . . . ?
C5 C6 C7 C8 1.0(11) . . . . ?
C4 N4 N2 N3 0.0(6) . . . . ?
C4 N4 N2 C2 -177.7(5) . . . . ?
C4 C3 N3 N2 -0.9(5) . . . . ?
C4 C3 C8 C7 -1.6(9) . . . . ?
C8 C3 N3 N2 177.5(6) . . . . ?
C8 C3 C4 N4 -177.6(5) . . . . ?
C8 C3 C4 C5 2.9(8) . . . . ?

_shelx_res_file                  
;
TITL mo_DAC24_F2BTa2PbI4_0GPa_0ma_a.res in Pnma
    0gpa_good.res
    created by SHELXL-2019/1 at 11:38:22 on 05-Feb-2024
REM Old TITL __TMP__ in Pnma
REM SHELXT solution in Pnma: R1 0.190, Rweak 0.005, Alpha 0.069
REM <I/s> 2.327 for 104 systematic absences, Orientation as input
REM Formula found by SHELXT: C7 F2 I4 N8 Pb
CELL 0.71073 12.9388 30.2907 6.6444 90 90 90
ZERR 4 0.0004 0.002 0.0002 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H F I N Pb
UNIT 64 72 16 16 32 4

L.S. 30
PLAN  5
TEMP 0
CONF
BOND
LIST 6
MORE -1
BOND $H
fmap 2
acta
OMIT 0 11 7
OMIT 6 9 1
OMIT 10 11 0
OMIT 11 0 5
OMIT 12 0 4
OMIT 13 0 4
OMIT 13 2 4
REM <olex2.extras>
REM <HklSrc "%.\\0GPa_good.hkl">
REM </olex2.extras>

WGHT    0.014900    4.784200
FVAR       0.22275
PB1   6    0.330250    0.750000    0.702626    10.50000    0.03094    0.04839 =
         0.03582    0.00000   -0.00019    0.00000
I1    4    0.338166    0.750000    0.212083    10.50000    0.04761    0.05610 =
         0.03173    0.00000    0.00193    0.00000
I2    4    0.084265    0.750000    0.743514    10.50000    0.02665    0.07750 =
         0.06083    0.00000    0.00050    0.00000
I3    4    0.317443    0.645610    0.683195    11.00000    0.04639    0.04898 =
         0.03882   -0.00005   -0.00016    0.00306
F2    3    0.448513    0.417280    0.346142    11.00000    0.05665    0.03462 =
         0.05766   -0.00199    0.00085   -0.00171
F1    3    0.267983    0.450808    0.419631    11.00000    0.04070    0.05350 =
         0.06025    0.00568    0.00655   -0.01097
N4    5    0.403659    0.592962    0.212699    11.00000    0.03164
N2    5    0.502103    0.599524    0.160580    11.00000    0.03273
C3    1    0.501967    0.530855    0.225666    11.00000    0.02571
C6    1    0.340126    0.479177    0.350965    11.00000    0.03171
N3    5    0.564886    0.564255    0.166012    11.00000    0.03256
N1    5    0.695399    0.642446    0.327286    11.00000    0.04935
AFIX 137
H1A   2    0.723267    0.654378    0.437002    11.00000   -1.50000
H1B   2    0.738095    0.646032    0.223546    11.00000   -1.50000
H1C   2    0.684810    0.613765    0.347804    11.00000   -1.50000
AFIX   0
C2    1    0.539991    0.642477    0.108641    11.00000    0.04142
AFIX  23
H2A   2    0.482581    0.660796    0.065760    11.00000   -1.20000
H2B   2    0.587576    0.639866   -0.003539    11.00000   -1.20000
AFIX   0
C7    1    0.439728    0.460870    0.314167    11.00000    0.03422
C1    1    0.594455    0.664598    0.282693    11.00000    0.04682
AFIX  23
H1D   2    0.606662    0.695385    0.250316    11.00000   -1.20000
H1E   2    0.550685    0.663448    0.401098    11.00000   -1.20000
AFIX   0
C5    1    0.318841    0.522786    0.324148    11.00000    0.03248
AFIX  43
H5    2    0.253606    0.534472    0.348958    11.00000   -1.20000
AFIX   0
C4    1    0.402402    0.549446    0.255851    11.00000    0.02715
C8    1    0.520687    0.486140    0.252455    11.00000    0.03063
AFIX  43
H8    2    0.585617    0.473992    0.229287    11.00000   -1.20000
AFIX   0
HKLF 4




REM  mo_DAC24_F2BTa2PbI4_0GPa_0ma_a.res in Pnma
REM wR2 = 0.0389, GooF = S = 1.102, Restrained GooF = 1.102 for all data
REM R1 = 0.0170 for 952 Fo > 4sig(Fo) and 0.0189 for all 1008 data
REM 95 parameters refined using 0 restraints

END

WGHT      0.0145      4.8563

REM Highest difference peak  0.235,  deepest hole -0.247,  1-sigma level  0.051
Q1    1   0.4246  0.7500  0.0310  10.50000  0.05    0.24
Q2    1   0.4112  0.7500  0.4700  10.50000  0.05    0.23
Q3    1   0.2681  0.7500  0.4506  10.50000  0.05    0.21
Q4    1   0.6875  0.7500  0.2423  10.50000  0.05    0.20
Q5    1   0.5244  0.6605  0.1822  11.00000  0.05    0.19
;
_shelx_res_checksum              81096
_olex2_exptl_crystal_mounting_method 
'Crystal mounted in a Diamond anvil cell of 100 degre opening angle'
_olex2_submission_special_instructions 'No special instructions were received'

_vrf_PLAT029_0gpa_good           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.288 Why?  
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT201_0gpa_good           
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         12 Report
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the available data, preventing from a complete anisotropic refienement. 
;
_vrf_PLAT933_0gpa_good           
;
PROBLEM: Number of HKL-OMIT Records in Embedded .res File          
RESPONSE: Experiment done in a Diamond Anvil Cell some reflections are close 
to gasket ring/shadow or close to diamond peaks and should be deleted.  
;
_vrf_PLAT911_0gpa_good           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT910_0gpa_good           
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT913_0gpa_good           
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
####################################################################### 
# 
# 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_0p60gpa_good
_database_code_depnum_ccdc_archive 'CCDC 2365958'
loop_
_audit_author_name
_audit_author_address
'Maxime Deutsch' 'University of Lorraine'
_audit_update_record             
;
2024-06-26 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-02-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H9 F2 N4)'
_chemical_formula_sum            'C16 H18 F4 I4 N8 Pb'
_chemical_formula_weight         1113.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.8444(5)
_cell_length_b                   29.723(2)
_cell_length_c                   6.5815(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2512.6(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9198
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      25.910
_cell_measurement_theta_min      3.385
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.681
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0924 before and 0.0654 after correction.
The Ratio of minimum to maximum transmission is 0.8006.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.943
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.408
_diffrn_reflns_Laue_measured_fraction_max 0.379
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            28628
_diffrn_reflns_point_group_measured_fraction_full 0.408
_diffrn_reflns_point_group_measured_fraction_max 0.379
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.190
_diffrn_reflns_theta_min         3.478
_diffrn_ambient_temperature      300(3)
_diffrn_ambient_pressure         0.60e+06
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.408
_diffrn_measured_fraction_theta_max 0.379
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON III CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                924
_reflns_number_total             971
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         971
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0167
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0139P)²+5.3498P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0377
_refine_ls_wR_factor_ref         0.0387
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.33638(2) 0.750000 0.70049(4) 0.0347(5) Uani 1 2 d S T P . .
I1 I 0.34375(4) 0.750000 0.20875(6) 0.0386(7) Uani 1 2 d S T P . .
I2 I 0.08818(3) 0.750000 0.74920(7) 0.0456(7) Uani 1 2 d S T P . .
I3 I 0.32000(3) 0.64427(3) 0.67852(5) 0.0395(5) Uani 1 1 d . . . . .
F2 F 0.4459(3) 0.4149(3) 0.3528(6) 0.047(5) Uani 1 1 d . . . . .
F1 F 0.2659(2) 0.4498(2) 0.4272(4) 0.050(4) Uani 1 1 d . . . . .
N4 N 0.4048(3) 0.5931(4) 0.2085(6) 0.0285(11) Uiso 1 1 d . . . . .
N2 N 0.5035(3) 0.5999(4) 0.1550(6) 0.0282(10) Uiso 1 1 d . . . . .
C3 C 0.5027(4) 0.5303(5) 0.2240(7) 0.0235(12) Uiso 1 1 d . . . . .
C6 C 0.3388(4) 0.4781(5) 0.3554(7) 0.0259(12) Uiso 1 1 d . . . . .
N3 N 0.5662(3) 0.5634(3) 0.1612(5) 0.0277(10) Uiso 1 1 d . . . . .
N1 N 0.6949(3) 0.6436(4) 0.3313(7) 0.0413(12) Uiso 1 1 d . . . . .
H1A H 0.742043 0.649096 0.235314 0.062 Uiso 1 1 calc R U . . .
H1B H 0.684447 0.614105 0.340944 0.062 Uiso 1 1 calc R U . . .
H1C H 0.717733 0.654146 0.449774 0.062 Uiso 1 1 calc R U . . .
C2 C 0.5427(4) 0.6431(5) 0.1004(7) 0.0348(13) Uiso 1 1 d . . . . .
H2A H 0.485661 0.661717 0.052384 0.042 Uiso 1 1 calc R U . . .
H2B H 0.592166 0.639881 -0.009869 0.042 Uiso 1 1 calc R U . . .
C7 C 0.4394(5) 0.4587(7) 0.3181(10) 0.0324(18) Uiso 1 1 d . . . . .
C1 C 0.5952(4) 0.6663(5) 0.2774(7) 0.0408(15) Uiso 1 1 d . . . . .
H1D H 0.608931 0.697424 0.242285 0.049 Uiso 1 1 calc R U . . .
H1E H 0.549069 0.665949 0.394010 0.049 Uiso 1 1 calc R U . . .
C5 C 0.3187(4) 0.5227(5) 0.3275(7) 0.0280(12) Uiso 1 1 d . . . . .
H5 H 0.253484 0.534900 0.354641 0.034 Uiso 1 1 calc R U . . .
C4 C 0.4022(3) 0.5495(5) 0.2550(7) 0.0248(12) Uiso 1 1 d . . . . .
C8 C 0.5204(4) 0.4844(5) 0.2537(7) 0.0247(12) Uiso 1 1 d . . . . .
H8 H 0.585637 0.471859 0.230224 0.030 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.02677(16) 0.0466(15) 0.03074(17) 0.000 -0.00023(9) 0.000
I1 0.0410(3) 0.048(2) 0.0268(3) 0.000 0.00113(17) 0.000
I2 0.0230(2) 0.064(2) 0.0501(3) 0.000 0.00082(19) 0.000
I3 0.0396(2) 0.0450(17) 0.03392(19) -0.0004(3) -0.00007(13) 0.0026(3)
F2 0.0463(19) 0.043(18) 0.051(2) -0.005(4) 0.0036(14) -0.002(3)
F1 0.0330(15) 0.066(13) 0.0507(18) -0.001(3) 0.0067(13) -0.006(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
Pb1 I1 3.3465(5) 1_556 ?
Pb1 I1 3.2378(5) . ?
Pb1 I2 3.2511(5) 6_657 ?
Pb1 I2 3.2040(5) . ?
Pb1 I3 3.1531(10) . ?
Pb1 I3 3.1532(10) 7_575 ?
F2 C7 1.323(19) . ?
F1 C6 1.345(11) . ?
N4 N2 1.331(6) . ?
N4 C4 1.334(16) . ?
N2 N3 1.350(12) . ?
N2 C2 1.427(16) . ?
C3 N3 1.345(13) . ?
C3 C4 1.426(10) . ?
C3 C8 1.395(16) . ?
C6 C7 1.436(12) . ?
C6 C5 1.363(18) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.489(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.512(11) . ?
C7 C8 1.359(15) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C5 H5 0.9300 . ?
C5 C4 1.419(13) . ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 176.703(18) . 1_556 ?
I1 Pb1 I2 94.170(14) . 6_657 ?
I2 Pb1 I1 97.418(14) . . ?
I2 Pb1 I1 85.879(13) . 1_556 ?
I2 Pb1 I1 82.533(13) 6_657 1_556 ?
I2 Pb1 I2 168.412(9) . 6_657 ?
I3 Pb1 I1 92.735(7) 7_575 1_556 ?
I3 Pb1 I1 87.485(7) 7_575 . ?
I3 Pb1 I1 92.736(7) . 1_556 ?
I3 Pb1 I1 87.485(7) . . ?
I3 Pb1 I2 94.073(8) . 6_657 ?
I3 Pb1 I2 86.458(8) 7_575 . ?
I3 Pb1 I2 86.458(8) . . ?
I3 Pb1 I2 94.073(8) 7_575 6_657 ?
I3 Pb1 I3 170.715(15) . 7_575 ?
Pb1 I1 Pb1 176.703(18) . 1_554 ?
Pb1 I2 Pb1 179.897(17) . 6_557 ?
N2 N4 C4 103.3(8) . . ?
N4 N2 N3 116.1(9) . . ?
N4 N2 C2 122.5(10) . . ?
N3 N2 C2 121.4(5) . . ?
N3 C3 C4 107.4(11) . . ?
N3 C3 C8 131.3(6) . . ?
C8 C3 C4 121.2(9) . . ?
F1 C6 C7 115.9(12) . . ?
F1 C6 C5 121.5(6) . . ?
C5 C6 C7 122.6(10) . . ?
C3 N3 N2 103.6(5) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N2 C2 H2A 109.2 . . ?
N2 C2 H2B 109.2 . . ?
N2 C2 C1 112.0(6) . . ?
H2A C2 H2B 107.9 . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
F2 C7 C6 114.9(10) . . ?
F2 C7 C8 124.0(9) . . ?
C8 C7 C6 121.1(16) . . ?
N1 C1 C2 111.2(8) . . ?
N1 C1 H1D 109.4 . . ?
N1 C1 H1E 109.4 . . ?
C2 C1 H1D 109.4 . . ?
C2 C1 H1E 109.4 . . ?
H1D C1 H1E 108.0 . . ?
C6 C5 H5 121.7 . . ?
C6 C5 C4 116.6(7) . . ?
C4 C5 H5 121.7 . . ?
N4 C4 C3 109.5(8) . . ?
N4 C4 C5 129.9(8) . . ?
C5 C4 C3 120.5(12) . . ?
C3 C8 H8 121.0 . . ?
C7 C8 C3 117.9(9) . . ?
C7 C8 H8 121.0 . . ?

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
F2 C7 C8 C3 -179.7(7) . . . . ?
F1 C6 C7 F2 2.3(10) . . . . ?
F1 C6 C7 C8 -177.1(6) . . . . ?
F1 C6 C5 C4 178.7(4) . . . . ?
N4 N2 N3 C3 0.0(6) . . . . ?
N4 N2 C2 C1 96.5(6) . . . . ?
N2 N4 C4 C3 -0.9(7) . . . . ?
N2 N4 C4 C5 178.2(5) . . . . ?
N2 C2 C1 N1 69.7(8) . . . . ?
C6 C7 C8 C3 -0.3(10) . . . . ?
C6 C5 C4 N4 177.8(7) . . . . ?
C6 C5 C4 C3 -3.1(8) . . . . ?
N3 N2 C2 C1 -81.3(8) . . . . ?
N3 C3 C4 N4 1.0(7) . . . . ?
N3 C3 C4 C5 -178.2(5) . . . . ?
N3 C3 C8 C7 -179.6(6) . . . . ?
C2 N2 N3 C3 178.0(5) . . . . ?
C7 C6 C5 C4 1.2(10) . . . . ?
C5 C6 C7 F2 179.9(7) . . . . ?
C5 C6 C7 C8 0.5(11) . . . . ?
C4 N4 N2 N3 0.6(6) . . . . ?
C4 N4 N2 C2 -177.4(5) . . . . ?
C4 C3 N3 N2 -0.6(5) . . . . ?
C4 C3 C8 C7 -1.6(9) . . . . ?
C8 C3 N3 N2 177.6(7) . . . . ?
C8 C3 C4 N4 -177.4(5) . . . . ?
C8 C3 C4 C5 3.4(9) . . . . ?

_shelx_res_file                  
;
TITL mo_DAC24_F2BTa2PbI4_0p60GPa_0ma_d.res in Pnma
    0p60gpa_good.res
    created by SHELXL-2019/1 at 11:52:12 on 05-Feb-2024
REM Old TITL __TMP__ in Pnma
REM SHELXT solution in Pnma: R1 0.236, Rweak 0.004, Alpha 0.032
REM <I/s> 2.224 for 105 systematic absences, Orientation as input
REM Formula found by SHELXT: C2 F2 I4 N6 Pb
CELL 0.71073 12.8444 29.7229 6.5815 90 90 90
ZERR 4 0.0005 0.0023 0.0003 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H F I N Pb
UNIT 64 72 16 16 32 4

L.S. 10
PLAN  2
TEMP 0
CONF
BOND
LIST 6
fmap 2
ACTA
MORE -1
BOND $H
OMIT 2 11 7
OMIT 5 8 1
OMIT 6 8 0
OMIT 7 11 6
OMIT 8 0 6
OMIT 8 10 0
OMIT 8 11 3
OMIT 10 11 1
OMIT 14 10 2
OMIT 14 11 1
REM <olex2.extras>
REM <HklSrc "%.\\0p60GPa_good.hkl">
REM </olex2.extras>

WGHT    0.013900    5.349800
FVAR       0.21775
PB1   6    0.336377    0.750000    0.700491    10.50000    0.02677    0.04658 =
         0.03074    0.00000   -0.00023    0.00000
I1    4    0.343748    0.750000    0.208753    10.50000    0.04101    0.04808 =
         0.02675    0.00000    0.00113    0.00000
I2    4    0.088178    0.750000    0.749200    10.50000    0.02298    0.06365 =
         0.05011    0.00000    0.00082    0.00000
I3    4    0.320004    0.644266    0.678521    11.00000    0.03958    0.04496 =
         0.03392   -0.00036   -0.00007    0.00259
F2    3    0.445937    0.414946    0.352806    11.00000    0.04629    0.04340 =
         0.05056   -0.00458    0.00360   -0.00187
F1    3    0.265901    0.449786    0.427224    11.00000    0.03299    0.06595 =
         0.05068   -0.00071    0.00669   -0.00555
N4    5    0.404800    0.593136    0.208463    11.00000    0.02849
N2    5    0.503521    0.599872    0.154965    11.00000    0.02817
C3    1    0.502727    0.530254    0.224037    11.00000    0.02350
C6    1    0.338847    0.478070    0.355377    11.00000    0.02592
N3    5    0.566247    0.563435    0.161246    11.00000    0.02774
N1    5    0.694888    0.643629    0.331272    11.00000    0.04128
AFIX 137
H1A   2    0.742043    0.649096    0.235314    11.00000   -1.50000
H1B   2    0.684447    0.614105    0.340944    11.00000   -1.50000
H1C   2    0.717733    0.654146    0.449774    11.00000   -1.50000
AFIX   0
C2    1    0.542658    0.643140    0.100447    11.00000    0.03476
AFIX  23
H2A   2    0.485661    0.661717    0.052384    11.00000   -1.20000
H2B   2    0.592166    0.639881   -0.009869    11.00000   -1.20000
AFIX   0
C7    1    0.439434    0.458703    0.318096    11.00000    0.03243
C1    1    0.595219    0.666286    0.277359    11.00000    0.04084
AFIX  23
H1D   2    0.608931    0.697424    0.242285    11.00000   -1.20000
H1E   2    0.549069    0.665949    0.394010    11.00000   -1.20000
AFIX   0
C5    1    0.318656    0.522662    0.327523    11.00000    0.02805
AFIX  43
H5    2    0.253484    0.534900    0.354641    11.00000   -1.20000
AFIX   0
C4    1    0.402218    0.549453    0.255001    11.00000    0.02482
C8    1    0.520428    0.484421    0.253740    11.00000    0.02466
AFIX  43
H8    2    0.585637    0.471859    0.230224    11.00000   -1.20000
AFIX   0
HKLF 4




REM  mo_DAC24_F2BTa2PbI4_0p60GPa_0ma_d.res in Pnma
REM wR2 = 0.0387, GooF = S = 1.103, Restrained GooF = 1.103 for all data
REM R1 = 0.0167 for 924 Fo > 4sig(Fo) and 0.0187 for all 971 data
REM 95 parameters refined using 0 restraints

END

WGHT      0.0136      5.3554

REM Highest difference peak  0.261,  deepest hole -0.247,  1-sigma level  0.056
Q1    1   0.4803  0.7500  0.3580  10.50000  0.05    0.26
Q2    1   0.4180  0.7500  0.4622  10.50000  0.05    0.25
;
_shelx_res_checksum              20282
_olex2_submission_special_instructions 'No special instructions were received'
_olex2_exptl_crystal_mounting_method 
'Crystal mounted in a Diamond anvil cell of 100 degre opening angle'

_vrf_PLAT029_0p60gpa_good        
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT201_0p60gpa_good        
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         12 Report
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the available data, preventing from a complete anisotropic refienement. 
;
_vrf_PLAT933_0p60gpa_good        
;
PROBLEM: Number of HKL-OMIT Records in Embedded .res File          
RESPONSE: Experiment done in a Diamond Anvil Cell some reflections are close 
to gasket ring/shadow or close to diamond peaks and should be deleted.  
;
_vrf_PLAT911_0p60gpa_good        
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT910_0p60gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT913_0p60gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
####################################################################### 
# 
# 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_3p90gpa_d_good
_database_code_depnum_ccdc_archive 'CCDC 2365969'
loop_
_audit_author_name
_audit_author_address
'Maxime Deutsch' 'University of Lorraine'
_audit_update_record             
;
2024-06-26 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-02-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H9 F2 N4)'
_chemical_formula_sum            'C16 H18 F4 I4 N8 Pb'
_chemical_formula_weight         1113.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.4841(6)
_cell_length_b                   27.931(2)
_cell_length_c                   6.2972(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2195.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9103
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      25.518
_cell_measurement_theta_min      3.235
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.367
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0825 before and 0.0620 after correction.
The Ratio of minimum to maximum transmission is 0.8182.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.367
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.413
_diffrn_reflns_Laue_measured_fraction_max 0.376
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            23891
_diffrn_reflns_point_group_measured_fraction_full 0.413
_diffrn_reflns_point_group_measured_fraction_max 0.376
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.364
_diffrn_reflns_theta_min         3.264
_diffrn_ambient_temperature      300(3)
_diffrn_ambient_pressure         3.90e+06
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.413
_diffrn_measured_fraction_theta_max 0.376
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON III CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                836
_reflns_number_total             860
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         860
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0165
_refine_ls_R_factor_gt           0.0159
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0091P)²+9.5496P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0355
_refine_ls_wR_factor_ref         0.0358
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.35174(2) 0.750000 0.69460(4) 0.0278(5) Uani 1 2 d S T P . .
I1 I 0.35719(4) 0.750000 0.20112(7) 0.0275(7) Uani 1 2 d S T P . .
I2 I 0.10273(4) 0.750000 0.76260(8) 0.0287(7) Uani 1 2 d S T P . .
I3 I 0.32455(3) 0.64078(4) 0.66543(5) 0.0292(5) Uani 1 1 d . . . . .
F2 F 0.4431(3) 0.4072(4) 0.3683(6) 0.033(6) Uani 1 1 d . . . . .
F1 F 0.2619(2) 0.4465(3) 0.4458(5) 0.027(4) Uani 1 1 d . . . . .
N4 N 0.4070(3) 0.5961(5) 0.1932(7) 0.0189(11) Uiso 1 1 d . . . . .
N2 N 0.5093(3) 0.6018(4) 0.1361(7) 0.0186(11) Uiso 1 1 d . . . . .
C3 C 0.5062(4) 0.5272(5) 0.2208(8) 0.0161(13) Uiso 1 1 d . . . . .
C6 C 0.3373(4) 0.4756(5) 0.3654(9) 0.0167(13) Uiso 1 1 d . . . . .
N3 N 0.5728(3) 0.5631(4) 0.1493(7) 0.0208(11) Uiso 1 1 d . . . . .
N1 N 0.6959(4) 0.6487(4) 0.3402(8) 0.0267(12) Uiso 1 1 d . . . . .
H1A H 0.683420 0.617394 0.351298 0.040 Uiso 1 1 calc R U . . .
H1B H 0.714602 0.660280 0.466457 0.040 Uiso 1 1 calc R U . . .
H1C H 0.748638 0.653624 0.247730 0.040 Uiso 1 1 calc R U . . .
C2 C 0.5489(4) 0.6479(5) 0.0752(8) 0.0233(14) Uiso 1 1 d . . . . .
H2A H 0.490829 0.667043 0.017955 0.028 Uiso 1 1 calc R U . . .
H2B H 0.602806 0.644285 -0.034579 0.028 Uiso 1 1 calc R U . . .
C7 C 0.4383(5) 0.4534(8) 0.3272(11) 0.0215(19) Uiso 1 1 d . . . . .
C1 C 0.5973(4) 0.6732(5) 0.2652(8) 0.0264(15) Uiso 1 1 d . . . . .
H1D H 0.614523 0.705960 0.226877 0.032 Uiso 1 1 calc R U . . .
H1E H 0.545274 0.674115 0.379518 0.032 Uiso 1 1 calc R U . . .
C5 C 0.3166(5) 0.5222(6) 0.3302(8) 0.0185(14) Uiso 1 1 d . . . . .
H5 H 0.249590 0.535527 0.355960 0.022 Uiso 1 1 calc R U . . .
C4 C 0.4041(4) 0.5501(6) 0.2507(9) 0.0167(13) Uiso 1 1 d . . . . .
C8 C 0.5252(4) 0.4792(5) 0.2579(8) 0.0167(13) Uiso 1 1 d . . . . .
H8 H 0.592086 0.465296 0.237394 0.020 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.01944(17) 0.0441(15) 0.01981(17) 0.000 -0.00003(11) 0.000
I1 0.0247(3) 0.040(2) 0.0174(3) 0.000 -0.00017(18) 0.000
I2 0.0164(2) 0.043(2) 0.0264(3) 0.000 0.00007(19) 0.000
I3 0.02466(19) 0.0404(15) 0.02258(19) -0.0002(3) 0.00000(13) 0.0036(3)
F2 0.0279(19) 0.04(2) 0.035(2) -0.001(4) 0.0038(14) 0.001(3)
F1 0.0230(16) 0.025(14) 0.0335(17) 0.006(3) 0.0058(12) -0.002(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.1904(5) 1_556 ?
Pb1 I1 3.1083(5) . ?
Pb1 I2 3.1449(5) 6_657 ?
Pb1 I2 3.1381(5) . ?
Pb1 I3 3.0749(11) . ?
Pb1 I3 3.0749(11) 7_575 ?
F2 C7 1.32(2) . ?
F1 C6 1.343(12) . ?
N4 N2 1.336(6) . ?
N4 C4 1.335(18) . ?
N2 N3 1.344(14) . ?
N2 C2 1.432(18) . ?
C3 N3 1.380(15) . ?
C3 C4 1.439(12) . ?
C3 C8 1.381(19) . ?
C6 C7 1.425(14) . ?
C6 C5 1.346(19) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.485(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.515(12) . ?
C7 C8 1.373(16) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C5 H5 0.9300 . ?
C5 C4 1.432(14) . ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 177.53(2) . 1_556 ?
I1 Pb1 I2 93.663(15) . 6_657 ?
I1 Pb1 I2 99.095(15) . . ?
I2 Pb1 I1 83.377(14) . 1_556 ?
I2 Pb1 I1 83.864(14) 6_657 1_556 ?
I2 Pb1 I2 167.241(10) . 6_657 ?
I3 Pb1 I1 86.714(8) 7_575 . ?
I3 Pb1 I1 93.559(8) 7_575 1_556 ?
I3 Pb1 I1 86.715(8) . . ?
I3 Pb1 I1 93.559(8) . 1_556 ?
I3 Pb1 I2 84.190(9) . . ?
I3 Pb1 I2 96.611(9) . 6_657 ?
I3 Pb1 I2 84.190(9) 7_575 . ?
I3 Pb1 I2 96.611(9) 7_575 6_657 ?
I3 Pb1 I3 165.576(17) . 7_575 ?
Pb1 I1 Pb1 177.53(2) . 1_554 ?
Pb1 I2 Pb1 177.073(18) . 6_557 ?
C4 N4 N2 102.4(9) . . ?
N4 N2 N3 116.8(10) . . ?
N4 N2 C2 120.7(10) . . ?
N3 N2 C2 122.4(6) . . ?
N3 C3 C4 104.6(12) . . ?
C8 C3 N3 131.2(6) . . ?
C8 C3 C4 124.2(10) . . ?
F1 C6 C7 114.8(13) . . ?
F1 C6 C5 120.9(6) . . ?
C5 C6 C7 124.2(11) . . ?
N2 N3 C3 104.5(6) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N2 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
N2 C2 C1 110.2(7) . . ?
H2A C2 H2B 108.1 . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
F2 C7 C6 115.7(11) . . ?
F2 C7 C8 122.7(11) . . ?
C8 C7 C6 121.6(18) . . ?
N1 C1 C2 111.5(9) . . ?
N1 C1 H1D 109.3 . . ?
N1 C1 H1E 109.3 . . ?
C2 C1 H1D 109.3 . . ?
C2 C1 H1E 109.3 . . ?
H1D C1 H1E 108.0 . . ?
C6 C5 H5 122.0 . . ?
C6 C5 C4 115.9(8) . . ?
C4 C5 H5 122.0 . . ?
N4 C4 C3 111.7(8) . . ?
N4 C4 C5 129.7(9) . . ?
C5 C4 C3 118.6(14) . . ?
C3 C8 C7 115.3(10) . . ?
C3 C8 H8 122.4 . . ?
C7 C8 H8 122.4 . . ?

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
F2 C7 C8 C3 179.6(8) . . . . ?
F1 C6 C7 F2 2.3(11) . . . . ?
F1 C6 C7 C8 -175.8(6) . . . . ?
F1 C6 C5 C4 178.1(5) . . . . ?
N4 N2 N3 C3 0.7(7) . . . . ?
N4 N2 C2 C1 93.4(6) . . . . ?
N2 N4 C4 C3 -2.0(8) . . . . ?
N2 N4 C4 C5 179.1(6) . . . . ?
N2 C2 C1 N1 67.1(8) . . . . ?
C6 C7 C8 C3 -2.4(12) . . . . ?
C6 C5 C4 N4 177.0(8) . . . . ?
C6 C5 C4 C3 -1.8(9) . . . . ?
N3 N2 C2 C1 -83.2(9) . . . . ?
N3 C3 C4 N4 2.5(8) . . . . ?
N3 C3 C4 C5 -178.5(5) . . . . ?
N3 C3 C8 C7 -179.2(6) . . . . ?
C2 N2 N3 C3 177.4(6) . . . . ?
C7 C6 C5 C4 -0.5(11) . . . . ?
C5 C6 C7 F2 -179.1(7) . . . . ?
C5 C6 C7 C8 2.8(13) . . . . ?
C4 N4 N2 N3 0.8(8) . . . . ?
C4 N4 N2 C2 -176.0(6) . . . . ?
C4 C3 N3 N2 -1.8(6) . . . . ?
C4 C3 C8 C7 0.1(11) . . . . ?
C8 C3 N3 N2 177.6(8) . . . . ?
C8 C3 C4 N4 -176.9(7) . . . . ?
C8 C3 C4 C5 2.1(10) . . . . ?

_shelx_res_file                  
;
TITL mo_DAC24_F2BTa2PbI4_3p90GPa_d_0ma_e.res in Pnma
    3p90gpa_d_good.res
    created by SHELXL-2019/1 at 17:13:06 on 08-Feb-2024
REM Old TITL __TMP__ in Pnma
REM SHELXT solution in Pnma: R1 0.204, Rweak 0.005, Alpha 0.081
REM <I/s> 2.975 for 96 systematic absences, Orientation as input
REM Formula found by SHELXT: C18 F4 I4 Pb
CELL 0.71073 12.4841 27.9311 6.2972 90 90 90
ZERR 4 0.0006 0.0024 0.0003 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H F I N Pb
UNIT 64 72 16 16 32 4

L.S. 10
PLAN  1
TEMP 0
CONF
BOND
LIST 6
fmap 2
MORE -1
BOND $H
ACTA
OMIT 11 10 4
REM <olex2.extras>
REM <HklSrc "%.\\3p90GPa_d_good.hkl">
REM </olex2.extras>

WGHT    0.009100    9.549600
FVAR       0.11874
PB1   6    0.351744    0.750000    0.694602    10.50000    0.01944    0.04412 =
         0.01981    0.00000   -0.00003    0.00000
I1    4    0.357186    0.750000    0.201125    10.50000    0.02467    0.04050 =
         0.01736    0.00000   -0.00017    0.00000
I2    4    0.102728    0.750000    0.762605    10.50000    0.01639    0.04344 =
         0.02640    0.00000    0.00007    0.00000
I3    4    0.324549    0.640783    0.665434    11.00000    0.02466    0.04036 =
         0.02258   -0.00024    0.00000    0.00365
F2    3    0.443097    0.407232    0.368279    11.00000    0.02788    0.03644 =
         0.03517   -0.00146    0.00377    0.00080
F1    3    0.261914    0.446468    0.445807    11.00000    0.02299    0.02515 =
         0.03353    0.00592    0.00584   -0.00216
N4    5    0.407000    0.596094    0.193207    11.00000    0.01889
N2    5    0.509306    0.601843    0.136141    11.00000    0.01864
C3    1    0.506217    0.527152    0.220803    11.00000    0.01607
C6    1    0.337280    0.475607    0.365440    11.00000    0.01671
N3    5    0.572823    0.563123    0.149343    11.00000    0.02082
N1    5    0.695872    0.648668    0.340190    11.00000    0.02667
AFIX 137
H1A   2    0.683420    0.617394    0.351298    11.00000   -1.50000
H1B   2    0.714602    0.660280    0.466457    11.00000   -1.50000
H1C   2    0.748638    0.653624    0.247730    11.00000   -1.50000
AFIX   0
C2    1    0.548939    0.647946    0.075237    11.00000    0.02335
AFIX  23
H2A   2    0.490829    0.667043    0.017955    11.00000   -1.20000
H2B   2    0.602806    0.644285   -0.034579    11.00000   -1.20000
AFIX   0
C7    1    0.438275    0.453415    0.327165    11.00000    0.02149
C1    1    0.597324    0.673215    0.265223    11.00000    0.02645
AFIX  23
H1D   2    0.614523    0.705960    0.226877    11.00000   -1.20000
H1E   2    0.545274    0.674115    0.379518    11.00000   -1.20000
AFIX   0
C5    1    0.316631    0.522220    0.330206    11.00000    0.01849
AFIX  43
H5    2    0.249590    0.535527    0.355960    11.00000   -1.20000
AFIX   0
C4    1    0.404132    0.550090    0.250663    11.00000    0.01669
C8    1    0.525172    0.479181    0.257890    11.00000    0.01672
AFIX  43
H8    2    0.592086    0.465296    0.237394    11.00000   -1.20000
AFIX   0
HKLF 4




REM  mo_DAC24_F2BTa2PbI4_3p90GPa_d_0ma_e.res in Pnma
REM wR2 = 0.0358, GooF = S = 1.117, Restrained GooF = 1.117 for all data
REM R1 = 0.0159 for 836 Fo > 4sig(Fo) and 0.0165 for all 860 data
REM 95 parameters refined using 0 restraints

END

WGHT      0.0079      9.0298

REM Highest difference peak  0.391,  deepest hole -0.364,  1-sigma level  0.080
Q1    1   0.4399  0.6980  0.5079  11.00000  0.05    0.39
;
_shelx_res_checksum              13791
_olex2_submission_special_instructions 'No special instructions were received'
_olex2_exptl_crystal_mounting_method 
'Crystal mounted in a Diamond anvil cell of 100 degre opening angle'

_vrf_PLAT029_3p90gpa_d_good      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT201_3p90gpa_d_good      
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         12 Report
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the available data, preventing from a complete anisotropic refienement. 
;
_vrf_PLAT933_3p90gpa_d_good      
;
PROBLEM: Number of HKL-OMIT Records in Embedded .res File          
RESPONSE: Experiment done in a Diamond Anvil Cell some reflections are close 
to gasket ring/shadow or close to diamond peaks and should be deleted.  
;
_vrf_PLAT911_3p90gpa_d_good      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT910_3p90gpa_d_good      
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT913_3p90gpa_d_good      
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT088_3p90gpa_d_good      
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space and then number of measured reflections inducing
a low Data / Parameter Ratio despite isotropic refinement done to limit this 
problem
;
####################################################################### 
# 
# 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_4p81gpa_good
_database_code_depnum_ccdc_archive 'CCDC 2365968'
loop_
_audit_author_name
_audit_author_address
'Maxime Deutsch' 'University of Lorraine'
_audit_update_record             
;
2024-06-26 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-02-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H9 F2 N4)'
_chemical_formula_sum            'C16 H18 F4 I4 N8 Pb'
_chemical_formula_weight         1113.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.5017(9)
_cell_length_b                   27.526(4)
_cell_length_c                   6.2872(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2163.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      25.534
_cell_measurement_theta_min      3.259
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.566
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0889 before and 0.0649 after correction.
The Ratio of minimum to maximum transmission is 0.8029.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    3.417
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.424
_diffrn_reflns_Laue_measured_fraction_max 0.394
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            21911
_diffrn_reflns_point_group_measured_fraction_full 0.424
_diffrn_reflns_point_group_measured_fraction_max 0.394
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.069
_diffrn_reflns_theta_min         3.259
_diffrn_ambient_temperature      300(3)
_diffrn_ambient_pressure         4.81e+06
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.424
_diffrn_measured_fraction_theta_max 0.394
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON III CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                830
_reflns_number_total             861
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         861
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0223
_refine_ls_restrained_S_all      1.191
_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)+20.2255P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0459
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.35613(3) 0.750000 0.69605(6) 0.0292(6) Uani 1 2 d S T P . .
I1 I 0.36034(6) 0.750000 0.20278(10) 0.0280(10) Uani 1 2 d S T P . .
I2 I 0.10691(5) 0.750000 0.76702(11) 0.0321(10) Uani 1 2 d S T P . .
I3 I 0.32488(4) 0.63997(5) 0.66533(8) 0.0304(7) Uani 1 1 d . . . . .
F2 F 0.4415(4) 0.4043(5) 0.3734(9) 0.029(8) Uani 1 1 d . . . . .
F1 F 0.2614(3) 0.4458(4) 0.4513(7) 0.025(6) Uani 1 1 d . . . . .
N4 N 0.4087(5) 0.5980(7) 0.1918(10) 0.0184(16) Uiso 1 1 d . . . . .
N2 N 0.5111(5) 0.6024(6) 0.1313(10) 0.0188(16) Uiso 1 1 d . . . . .
C3 C 0.5067(6) 0.5288(8) 0.2217(12) 0.0184(19) Uiso 1 1 d . . . . .
C6 C 0.3372(6) 0.4751(8) 0.3679(12) 0.018(2) Uiso 1 1 d . . . . .
N3 N 0.5736(5) 0.5622(6) 0.1462(9) 0.0200(16) Uiso 1 1 d . . . . .
N1 N 0.6974(5) 0.6490(6) 0.3364(10) 0.0238(17) Uiso 1 1 d . . . . .
H1A H 0.680784 0.618640 0.372565 0.036 Uiso 1 1 calc R U . . .
H1B H 0.723607 0.664513 0.449044 0.036 Uiso 1 1 calc R U . . .
H1C H 0.746196 0.648539 0.233342 0.036 Uiso 1 1 calc R U . . .
C2 C 0.5516(6) 0.6497(7) 0.0706(12) 0.0201(19) Uiso 1 1 d . . . . .
H2A H 0.493732 0.669313 0.014073 0.024 Uiso 1 1 calc R U . . .
H2B H 0.605279 0.646043 -0.039577 0.024 Uiso 1 1 calc R U . . .
C7 C 0.4374(7) 0.4518(11) 0.3315(15) 0.019(3) Uiso 1 1 d . . . . .
C1 C 0.5996(6) 0.6745(7) 0.2597(12) 0.028(2) Uiso 1 1 d . . . . .
H1D H 0.617827 0.707633 0.222166 0.034 Uiso 1 1 calc R U . . .
H1E H 0.547296 0.675587 0.373513 0.034 Uiso 1 1 calc R U . . .
C5 C 0.3175(6) 0.5222(8) 0.3305(12) 0.019(2) Uiso 1 1 d . . . . .
H5 H 0.251233 0.536328 0.356590 0.023 Uiso 1 1 calc R U . . .
C4 C 0.4054(5) 0.5491(8) 0.2481(11) 0.0118(17) Uiso 1 1 d . . . . .
C8 C 0.5228(6) 0.4778(8) 0.2576(12) 0.0164(19) Uiso 1 1 d . . . . .
H8 H 0.588463 0.463127 0.231566 0.020 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0195(2) 0.048(2) 0.0205(2) 0.000 -0.00013(16) 0.000
I1 0.0233(4) 0.042(3) 0.0184(4) 0.000 0.0000(3) 0.000
I2 0.0161(3) 0.055(3) 0.0254(4) 0.000 0.0002(3) 0.000
I3 0.0243(3) 0.044(2) 0.0232(3) 0.0006(5) 0.00019(19) 0.0048(5)
F2 0.027(3) 0.02(3) 0.036(3) -0.003(5) 0.0068(19) 0.001(5)
F1 0.022(2) 0.022(19) 0.033(2) 0.009(4) 0.0058(18) -0.006(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.1863(8) 1_556 ?
Pb1 I1 3.1018(8) . ?
Pb1 I2 3.1475(8) . ?
Pb1 I2 3.1437(8) 6_657 ?
Pb1 I3 3.0598(15) . ?
Pb1 I3 3.0599(15) 7_575 ?
F2 C7 1.34(3) . ?
F1 C6 1.349(16) . ?
N4 N2 1.340(9) . ?
N4 C4 1.39(2) . ?
N2 N3 1.36(2) . ?
N2 C2 1.45(2) . ?
C3 N3 1.33(2) . ?
C3 C4 1.394(16) . ?
C3 C8 1.43(3) . ?
C6 C7 1.43(2) . ?
C6 C5 1.34(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.489(15) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.496(16) . ?
C7 C8 1.37(2) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C5 H5 0.9300 . ?
C5 C4 1.422(19) . ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 178.08(3) . 1_556 ?
I1 Pb1 I2 99.12(2) . . ?
I1 Pb1 I2 93.27(2) . 6_657 ?
I2 Pb1 I1 84.82(2) 6_657 1_556 ?
I2 Pb1 I1 82.79(2) . 1_556 ?
I2 Pb1 I2 167.615(15) 6_657 . ?
I3 Pb1 I1 86.505(12) 7_575 . ?
I3 Pb1 I1 93.740(12) 7_575 1_556 ?
I3 Pb1 I1 86.505(12) . . ?
I3 Pb1 I1 93.740(12) . 1_556 ?
I3 Pb1 I2 97.585(12) . 6_657 ?
I3 Pb1 I2 83.255(12) . . ?
I3 Pb1 I2 97.584(12) 7_575 6_657 ?
I3 Pb1 I2 83.256(12) 7_575 . ?
I3 Pb1 I3 163.62(2) . 7_575 ?
Pb1 I1 Pb1 178.08(3) . 1_554 ?
Pb1 I2 Pb1 176.09(3) 6_557 . ?
N2 N4 C4 100.7(12) . . ?
N4 N2 N3 117.2(14) . . ?
N4 N2 C2 119.2(15) . . ?
N3 N2 C2 123.3(8) . . ?
N3 C3 C4 109.6(18) . . ?
N3 C3 C8 130.1(10) . . ?
C4 C3 C8 120.0(14) . . ?
F1 C6 C7 114.3(19) . . ?
C5 C6 F1 121.1(9) . . ?
C5 C6 C7 124.5(15) . . ?
C3 N3 N2 103.1(9) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N2 C2 H2A 109.7 . . ?
N2 C2 H2B 109.7 . . ?
N2 C2 C1 109.9(10) . . ?
H2A C2 H2B 108.2 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
F2 C7 C6 116.2(14) . . ?
F2 C7 C8 123.4(15) . . ?
C8 C7 C6 120(2) . . ?
N1 C1 C2 111.8(13) . . ?
N1 C1 H1D 109.3 . . ?
N1 C1 H1E 109.3 . . ?
C2 C1 H1D 109.3 . . ?
C2 C1 H1E 109.3 . . ?
H1D C1 H1E 107.9 . . ?
C6 C5 H5 122.4 . . ?
C6 C5 C4 115.2(12) . . ?
C4 C5 H5 122.4 . . ?
N4 C4 C5 128.2(12) . . ?
C3 C4 N4 109.3(12) . . ?
C3 C4 C5 122.5(19) . . ?
C3 C8 H8 121.4 . . ?
C7 C8 C3 117.2(14) . . ?
C7 C8 H8 121.4 . . ?

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
F2 C7 C8 C3 -179.4(11) . . . . ?
F1 C6 C7 F2 3.4(15) . . . . ?
F1 C6 C7 C8 -176.7(9) . . . . ?
F1 C6 C5 C4 178.3(7) . . . . ?
N4 N2 N3 C3 0.3(10) . . . . ?
N4 N2 C2 C1 92.2(9) . . . . ?
N2 N4 C4 C3 1.6(10) . . . . ?
N2 N4 C4 C5 178.6(8) . . . . ?
N2 C2 C1 N1 66.4(12) . . . . ?
C6 C7 C8 C3 0.7(16) . . . . ?
C6 C5 C4 N4 179.1(10) . . . . ?
C6 C5 C4 C3 -4.2(14) . . . . ?
N3 N2 C2 C1 -82.5(12) . . . . ?
N3 C3 C4 N4 -1.6(11) . . . . ?
N3 C3 C4 C5 -178.8(8) . . . . ?
N3 C3 C8 C7 -178.0(9) . . . . ?
C2 N2 N3 C3 175.1(8) . . . . ?
C7 C6 C5 C4 0.3(16) . . . . ?
C5 C6 C7 F2 -178.5(11) . . . . ?
C5 C6 C7 C8 1.4(18) . . . . ?
C4 N4 N2 N3 -1.2(10) . . . . ?
C4 N4 N2 C2 -176.2(8) . . . . ?
C4 C3 N3 N2 0.8(9) . . . . ?
C4 C3 C8 C7 -4.4(15) . . . . ?
C8 C3 N3 N2 174.9(10) . . . . ?
C8 C3 C4 N4 -176.3(9) . . . . ?
C8 C3 C4 C5 6.4(14) . . . . ?

_shelx_res_file                  
;
TITL mo_DAC24_F2BTa2PbI4_4p80GPa_0ma_e.res in Pnma
    4p81gpa_good.res
    created by SHELXL-2019/1 at 16:51:58 on 08-Feb-2024
REM Old TITL __TMP__ in Pnma
REM SHELXT solution in Pnma: R1 0.168, Rweak 0.004, Alpha 0.046
REM <I/s> 3.005 for 93 systematic absences, Orientation as input
REM Formula found by SHELXT: C4 F2 I4 N10 Pb
CELL 0.71073 12.5017 27.5263 6.2872 90 90 90
ZERR 4 0.0009 0.0036 0.0004 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H F I N Pb
UNIT 64 72 16 16 32 4

L.S. 10
PLAN  1
TEMP 0
CONF
BOND
LIST 6
fmap 2
MORE -1
BOND $H
ACTA
OMIT 6 11 5
OMIT 7 9 1
OMIT 7 11 5
OMIT 8 11 5
OMIT 9 10 1
REM <olex2.extras>
REM <HklSrc "%.\\4p81GPa_good.hkl">
REM </olex2.extras>

WGHT    0.000000   20.225500
FVAR       0.11985
PB1   6    0.356134    0.750000    0.696050    10.50000    0.01949    0.04765 =
         0.02048    0.00000   -0.00013    0.00000
I1    4    0.360338    0.750000    0.202776    10.50000    0.02326    0.04249 =
         0.01840    0.00000    0.00002    0.00000
I2    4    0.106910    0.750000    0.767016    10.50000    0.01611    0.05470 =
         0.02536    0.00000    0.00020    0.00000
I3    4    0.324883    0.639973    0.665327    11.00000    0.02430    0.04372 =
         0.02322    0.00059    0.00019    0.00484
F2    3    0.441491    0.404300    0.373426    11.00000    0.02666    0.02288 =
         0.03596   -0.00262    0.00682    0.00115
F1    3    0.261394    0.445832    0.451320    11.00000    0.02160    0.02235 =
         0.03253    0.00917    0.00579   -0.00564
N4    5    0.408711    0.598005    0.191833    11.00000    0.01842
N2    5    0.511074    0.602351    0.131296    11.00000    0.01880
C3    1    0.506716    0.528771    0.221734    11.00000    0.01836
C6    1    0.337164    0.475057    0.367933    11.00000    0.01783
N3    5    0.573575    0.562218    0.146214    11.00000    0.01996
N1    5    0.697391    0.648975    0.336380    11.00000    0.02379
AFIX 137
H1A   2    0.680784    0.618640    0.372565    11.00000   -1.50000
H1B   2    0.723607    0.664513    0.449044    11.00000   -1.50000
H1C   2    0.746196    0.648539    0.233342    11.00000   -1.50000
AFIX   0
C2    1    0.551571    0.649693    0.070615    11.00000    0.02007
AFIX  23
H2A   2    0.493732    0.669313    0.014073    11.00000   -1.20000
H2B   2    0.605279    0.646043   -0.039577    11.00000   -1.20000
AFIX   0
C7    1    0.437432    0.451813    0.331507    11.00000    0.01855
C1    1    0.599628    0.674468    0.259713    11.00000    0.02799
AFIX  23
H1D   2    0.617827    0.707633    0.222166    11.00000   -1.20000
H1E   2    0.547296    0.675587    0.373513    11.00000   -1.20000
AFIX   0
C5    1    0.317543    0.522220    0.330512    11.00000    0.01893
AFIX  43
H5    2    0.251233    0.536328    0.356590    11.00000   -1.20000
AFIX   0
C4    1    0.405441    0.549074    0.248115    11.00000    0.01182
C8    1    0.522771    0.477826    0.257560    11.00000    0.01639
AFIX  43
H8    2    0.588463    0.463127    0.231566    11.00000   -1.20000
AFIX   0
HKLF 4




REM  mo_DAC24_F2BTa2PbI4_4p80GPa_0ma_e.res in Pnma
REM wR2 = 0.0459, GooF = S = 1.191, Restrained GooF = 1.191 for all data
REM R1 = 0.0223 for 830 Fo > 4sig(Fo) and 0.0236 for all 861 data
REM 95 parameters refined using 0 restraints

END

WGHT      0.0000     20.1704

REM Highest difference peak  0.501,  deepest hole -0.551,  1-sigma level  0.107
Q1    1   0.3566  0.7500  0.9375  10.50000  0.05    0.50
;
_shelx_res_checksum              9633
_olex2_submission_special_instructions 'No special instructions were received'
_olex2_exptl_crystal_mounting_method 
'Crystal mounted in a Diamond anvil cell of 100 degre opening angle'

_vrf_PLAT029_4p81gpa_good        
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT342_4p81gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space inducing a lower bond precision.
;
_vrf_PLAT201_4p81gpa_good        
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         12 Report
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the available data, preventing from a complete anisotropic refienement. 
;
_vrf_PLAT933_4p81gpa_good        
;
PROBLEM: Number of HKL-OMIT Records in Embedded .res File          
RESPONSE: Experiment done in a Diamond Anvil Cell some reflections are close 
to gasket ring/shadow or close to diamond peaks and should be deleted.  
;
_vrf_PLAT911_4p81gpa_good        
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT910_4p81gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT913_4p81gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT088_4p81gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space and then number of measured reflections inducing
a low Data / Parameter Ratio despite isotropic refinement done to limit this 
problem
;
####################################################################### 
# 
# 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_1p65gpa_d_good
_database_code_depnum_ccdc_archive 'CCDC 2365970'
loop_
_audit_author_name
_audit_author_address
'Maxime Deutsch' 'University of Lorraine'
_audit_update_record             
;
2024-06-26 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-02-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H9 F2 N4)'
_chemical_formula_sum            'C16 H18 F4 I4 N8 Pb'
_chemical_formula_weight         1113.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.6989(10)
_cell_length_b                   28.912(4)
_cell_length_c                   6.4700(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2375.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9674
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      25.892
_cell_measurement_theta_min      3.227
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.356
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0841 before and 0.0642 after correction.
The Ratio of minimum to maximum transmission is 0.8205.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.113
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.417
_diffrn_reflns_Laue_measured_fraction_max 0.391
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            26755
_diffrn_reflns_point_group_measured_fraction_full 0.417
_diffrn_reflns_point_group_measured_fraction_max 0.391
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.104
_diffrn_reflns_theta_min         3.208
_diffrn_ambient_temperature      300(3)
_diffrn_ambient_pressure         1.61e+06
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.417
_diffrn_measured_fraction_theta_max 0.391
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON III CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                909
_reflns_number_total             938
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         938
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0159
_refine_ls_R_factor_gt           0.0151
_refine_ls_restrained_S_all      1.146
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0139P)²+4.3102P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0352
_refine_ls_wR_factor_ref         0.0355
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.34351(2) 0.750000 0.69763(4) 0.0285(4) Uani 1 2 d S T P . .
I1 I 0.35080(3) 0.750000 0.20481(6) 0.0320(6) Uani 1 2 d S T P . .
I2 I 0.09447(3) 0.750000 0.75569(7) 0.0364(6) Uani 1 2 d S T P . .
I3 I 0.32276(2) 0.64267(3) 0.67267(4) 0.0336(5) Uani 1 1 d . . . . .
F2 F 0.4442(2) 0.4111(3) 0.3605(5) 0.034(5) Uani 1 1 d . . . . .
F1 F 0.26345(18) 0.4482(2) 0.4359(4) 0.037(4) Uani 1 1 d . . . . .
N4 N 0.4063(3) 0.5935(4) 0.2019(6) 0.0240(10) Uiso 1 1 d . . . . .
N2 N 0.5066(3) 0.6001(4) 0.1466(5) 0.0226(9) Uiso 1 1 d . . . . .
C3 C 0.5041(3) 0.5289(5) 0.2232(7) 0.0197(11) Uiso 1 1 d . . . . .
C6 C 0.3378(3) 0.4770(5) 0.3600(7) 0.0214(12) Uiso 1 1 d . . . . .
N3 N 0.5691(3) 0.5627(3) 0.1570(5) 0.0227(9) Uiso 1 1 d . . . . .
N1 N 0.6957(3) 0.6459(3) 0.3361(6) 0.0343(11) Uiso 1 1 d . . . . .
H1A H 0.684534 0.615546 0.345801 0.051 Uiso 1 1 calc R U . . .
H1B H 0.715909 0.656808 0.458359 0.051 Uiso 1 1 calc R U . . .
H1C H 0.745742 0.651241 0.242925 0.051 Uiso 1 1 calc R U . . .
C2 C 0.5458(4) 0.6448(4) 0.0897(7) 0.0284(11) Uiso 1 1 d . . . . .
H2A H 0.488215 0.663462 0.037380 0.034 Uiso 1 1 calc R U . . .
H2B H 0.597155 0.641345 -0.020154 0.034 Uiso 1 1 calc R U . . .
C7 C 0.4377(4) 0.4562(6) 0.3229(9) 0.0245(16) Uiso 1 1 d . . . . .
C1 C 0.5964(4) 0.6693(4) 0.2711(7) 0.0345(13) Uiso 1 1 d . . . . .
H1D H 0.611838 0.701030 0.232932 0.041 Uiso 1 1 calc R U . . .
H1E H 0.547576 0.669853 0.386273 0.041 Uiso 1 1 calc R U . . .
C5 C 0.3173(4) 0.5228(5) 0.3303(7) 0.0232(12) Uiso 1 1 d . . . . .
H5 H 0.251686 0.535675 0.357742 0.028 Uiso 1 1 calc R U . . .
C4 C 0.4029(3) 0.5497(5) 0.2544(7) 0.0212(11) Uiso 1 1 d . . . . .
C8 C 0.5218(4) 0.4821(5) 0.2549(7) 0.0221(11) Uiso 1 1 d . . . . .
H8 H 0.587368 0.468828 0.231213 0.027 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.02274(15) 0.0381(14) 0.02473(16) 0.000 -0.00025(9) 0.000
I1 0.0329(2) 0.042(2) 0.0212(2) 0.000 0.00043(15) 0.000
I2 0.0192(2) 0.053(2) 0.0371(2) 0.000 0.00066(17) 0.000
I3 0.03149(18) 0.0416(15) 0.02787(17) -0.0003(3) -0.00012(11) 0.0034(3)
F2 0.0374(16) 0.023(16) 0.0426(17) 0.000(3) 0.0032(12) -0.001(3)
F1 0.0255(13) 0.045(12) 0.0408(15) 0.005(2) 0.0063(11) -0.008(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
Pb1 I1 3.2828(5) 1_556 ?
Pb1 I1 3.1899(5) . ?
Pb1 I2 3.2012(5) 6_657 ?
Pb1 I2 3.1848(5) . ?
Pb1 I3 3.1185(10) . ?
Pb1 I3 3.1185(10) 7_575 ?
F2 C7 1.330(17) . ?
F1 C6 1.352(10) . ?
N4 N2 1.336(6) . ?
N4 C4 1.313(15) . ?
N2 N3 1.344(12) . ?
N2 C2 1.433(15) . ?
C3 N3 1.348(12) . ?
C3 C4 1.433(10) . ?
C3 C8 1.387(15) . ?
C6 C7 1.425(11) . ?
C6 C5 1.362(16) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.491(9) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.514(10) . ?
C7 C8 1.375(13) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C5 H5 0.9300 . ?
C5 C4 1.423(12) . ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 176.721(17) . 1_556 ?
I1 Pb1 I2 93.752(12) . 6_657 ?
I2 Pb1 I1 98.437(12) . . ?
I2 Pb1 I1 84.842(12) . 1_556 ?
I2 Pb1 I1 82.969(12) 6_657 1_556 ?
I2 Pb1 I2 167.811(8) . 6_657 ?
I3 Pb1 I1 93.103(7) 7_575 1_556 ?
I3 Pb1 I1 87.174(7) 7_575 . ?
I3 Pb1 I1 93.103(7) . 1_556 ?
I3 Pb1 I1 87.174(7) . . ?
I3 Pb1 I2 95.106(7) . 6_657 ?
I3 Pb1 I2 85.539(7) 7_575 . ?
I3 Pb1 I2 85.539(7) . . ?
I3 Pb1 I2 95.105(7) 7_575 6_657 ?
I3 Pb1 I3 168.627(14) . 7_575 ?
Pb1 I1 Pb1 176.722(17) . 1_554 ?
Pb1 I2 Pb1 178.641(15) . 6_557 ?
C4 N4 N2 103.8(7) . . ?
N4 N2 N3 115.8(9) . . ?
N4 N2 C2 121.9(9) . . ?
N3 N2 C2 122.2(5) . . ?
N3 C3 C4 106.9(10) . . ?
N3 C3 C8 130.9(5) . . ?
C8 C3 C4 122.2(8) . . ?
F1 C6 C7 115.0(11) . . ?
F1 C6 C5 121.2(5) . . ?
C5 C6 C7 123.8(9) . . ?
N2 N3 C3 103.7(5) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N2 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
N2 C2 C1 111.8(6) . . ?
H2A C2 H2B 107.9 . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
F2 C7 C6 116.0(9) . . ?
F2 C7 C8 123.0(9) . . ?
C8 C7 C6 121.0(14) . . ?
N1 C1 C2 111.4(8) . . ?
N1 C1 H1D 109.3 . . ?
N1 C1 H1E 109.3 . . ?
C2 C1 H1D 109.3 . . ?
C2 C1 H1E 109.3 . . ?
H1D C1 H1E 108.0 . . ?
C6 C5 H5 122.2 . . ?
C6 C5 C4 115.7(7) . . ?
C4 C5 H5 122.2 . . ?
N4 C4 C3 109.8(7) . . ?
N4 C4 C5 129.9(8) . . ?
C5 C4 C3 120.3(12) . . ?
C3 C8 H8 121.5 . . ?
C7 C8 C3 116.9(8) . . ?
C7 C8 H8 121.5 . . ?

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
F2 C7 C8 C3 -179.6(6) . . . . ?
F1 C6 C7 F2 2.2(9) . . . . ?
F1 C6 C7 C8 -177.0(5) . . . . ?
F1 C6 C5 C4 178.5(4) . . . . ?
N4 N2 N3 C3 0.4(5) . . . . ?
N4 N2 C2 C1 95.0(5) . . . . ?
N2 N4 C4 C3 -1.9(7) . . . . ?
N2 N4 C4 C5 178.7(5) . . . . ?
N2 C2 C1 N1 68.0(7) . . . . ?
C6 C7 C8 C3 -0.4(9) . . . . ?
C6 C5 C4 N4 176.5(7) . . . . ?
C6 C5 C4 C3 -2.9(8) . . . . ?
N3 N2 C2 C1 -81.9(7) . . . . ?
N3 C3 C4 N4 2.2(7) . . . . ?
N3 C3 C4 C5 -178.3(5) . . . . ?
N3 C3 C8 C7 -179.5(5) . . . . ?
C2 N2 N3 C3 177.4(5) . . . . ?
C7 C6 C5 C4 1.1(9) . . . . ?
C5 C6 C7 F2 179.8(6) . . . . ?
C5 C6 C7 C8 0.6(10) . . . . ?
C4 N4 N2 N3 0.9(7) . . . . ?
C4 N4 N2 C2 -176.1(5) . . . . ?
C4 C3 N3 N2 -1.5(5) . . . . ?
C4 C3 C8 C7 -1.5(9) . . . . ?
C8 C3 N3 N2 176.8(6) . . . . ?
C8 C3 C4 N4 -176.2(6) . . . . ?
C8 C3 C4 C5 3.3(8) . . . . ?

_shelx_res_file                  
;
TITL mo_DAC24_F2BTa2PbI4_1p65GPa_d_0ma_d.res in Pnma
    1p65gpa_d_good.res
    created by SHELXL-2019/1 at 17:30:54 on 08-Feb-2024
REM Old TITL __TMP__ in Pnma
REM SHELXT solution in Pnma: R1 0.268, Rweak 0.006, Alpha 0.030
REM <I/s> 2.530 for 101 systematic absences, Orientation as input
REM Formula found by SHELXT: C10 F4 I4 N6 Pb
CELL 0.71073 12.6989 28.9124 6.47 90 90 90
ZERR 4 0.001 0.0043 0.0005 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H F I N Pb
UNIT 64 72 16 16 32 4

L.S. 10
PLAN  1
TEMP 0
CONF
BOND
LIST 6
fmap 2
MORE -1
BOND $H
ACTA
OMIT 0 6 2
OMIT 8 9 0
REM <olex2.extras>
REM <HklSrc "%.\\1p65GPa_d_good.hkl">
REM </olex2.extras>

WGHT    0.013900    4.310200
FVAR       0.11401
PB1   6    0.343512    0.750000    0.697626    10.50000    0.02274    0.03812 =
         0.02473    0.00000   -0.00025    0.00000
I1    4    0.350802    0.750000    0.204805    10.50000    0.03292    0.04187 =
         0.02121    0.00000    0.00043    0.00000
I2    4    0.094472    0.750000    0.755686    10.50000    0.01922    0.05294 =
         0.03711    0.00000    0.00066    0.00000
I3    4    0.322765    0.642671    0.672670    11.00000    0.03149    0.04158 =
         0.02787   -0.00025   -0.00012    0.00336
F2    3    0.444173    0.411105    0.360514    11.00000    0.03742    0.02299 =
         0.04261   -0.00031    0.00320   -0.00119
F1    3    0.263455    0.448156    0.435876    11.00000    0.02549    0.04526 =
         0.04078    0.00542    0.00629   -0.00823
N4    5    0.406340    0.593502    0.201932    11.00000    0.02398
N2    5    0.506557    0.600095    0.146627    11.00000    0.02256
C3    1    0.504114    0.528910    0.223199    11.00000    0.01966
C6    1    0.337764    0.477032    0.360031    11.00000    0.02138
N3    5    0.569091    0.562674    0.157016    11.00000    0.02265
N1    5    0.695656    0.645861    0.336092    11.00000    0.03426
AFIX 137
H1A   2    0.684534    0.615546    0.345801    11.00000   -1.50000
H1B   2    0.715909    0.656808    0.458359    11.00000   -1.50000
H1C   2    0.745742    0.651241    0.242925    11.00000   -1.50000
AFIX   0
C2    1    0.545778    0.644777    0.089723    11.00000    0.02836
AFIX  23
H2A   2    0.488215    0.663462    0.037380    11.00000   -1.20000
H2B   2    0.597155    0.641345   -0.020154    11.00000   -1.20000
AFIX   0
C7    1    0.437731    0.456237    0.322909    11.00000    0.02452
C1    1    0.596444    0.669297    0.271073    11.00000    0.03449
AFIX  23
H1D   2    0.611838    0.701030    0.232932    11.00000   -1.20000
H1E   2    0.547576    0.669853    0.386273    11.00000   -1.20000
AFIX   0
C5    1    0.317330    0.522810    0.330260    11.00000    0.02324
AFIX  43
H5    2    0.251686    0.535675    0.357742    11.00000   -1.20000
AFIX   0
C4    1    0.402907    0.549666    0.254406    11.00000    0.02124
C8    1    0.521762    0.482106    0.254874    11.00000    0.02213
AFIX  43
H8    2    0.587368    0.468828    0.231213    11.00000   -1.20000
AFIX   0
HKLF 4




REM  mo_DAC24_F2BTa2PbI4_1p65GPa_d_0ma_d.res in Pnma
REM wR2 = 0.0355, GooF = S = 1.146, Restrained GooF = 1.146 for all data
REM R1 = 0.0151 for 909 Fo > 4sig(Fo) and 0.0159 for all 938 data
REM 95 parameters refined using 0 restraints

END

WGHT      0.0134      4.3641

REM Highest difference peak  0.341,  deepest hole -0.300,  1-sigma level  0.092
Q1    1  -0.0208  0.7500  0.9452  10.50000  0.05    0.34
;
_shelx_res_checksum              20212
_olex2_submission_special_instructions 'No special instructions were received'
_olex2_exptl_crystal_mounting_method 
'Crystal mounted in a Diamond anvil cell of 100 degre opening angle'

_vrf_PLAT029_1p65gpa_d_good      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT201_1p65gpa_d_good      
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         12 Report
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the available data, preventing from a complete anisotropic refienement. 
;
_vrf_PLAT933_1p65gpa_d_good      
;
PROBLEM: Number of HKL-OMIT Records in Embedded .res File          
RESPONSE: Experiment done in a Diamond Anvil Cell some reflections are close 
to gasket ring/shadow or close to diamond peaks and should be deleted.  
;
_vrf_PLAT911_1p65gpa_d_good      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT910_1p65gpa_d_good      
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT913_1p65gpa_d_good      
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT088_1p65gpa_d_good      
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space and then number of measured reflections inducing
a low Data / Parameter Ratio despite isotropic refinement done to limit this 
problem
;
####################################################################### 
# 
# 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_4p33gpa_good
_database_code_depnum_ccdc_archive 'CCDC 2365967'
loop_
_audit_author_name
_audit_author_address
'Maxime Deutsch' 'University of Lorraine'
_audit_update_record             
;
2024-06-26 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-02-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H9 F2 N4)'
_chemical_formula_sum            'C16 H18 F4 I4 N8 Pb'
_chemical_formula_weight         1113.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.5029(7)
_cell_length_b                   27.709(3)
_cell_length_c                   6.2997(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2182.5(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      25.502
_cell_measurement_theta_min      3.317
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.448
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0862 before and 0.0649 after correction.
The Ratio of minimum to maximum transmission is 0.8084.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.388
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.421
_diffrn_reflns_Laue_measured_fraction_max 0.382
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            23388
_diffrn_reflns_point_group_measured_fraction_full 0.421
_diffrn_reflns_point_group_measured_fraction_max 0.382
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.349
_diffrn_reflns_theta_min         3.259
_diffrn_ambient_temperature      300(3)
_diffrn_ambient_pressure         4.33e+06
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.421
_diffrn_measured_fraction_theta_max 0.382
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON III CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                836
_reflns_number_total             869
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         869
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0185
_refine_ls_restrained_S_all      1.157
_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)+(0.0080P)²+13.3578P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0406
_refine_ls_wR_factor_ref         0.0410
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.35421(3) 0.750000 0.69560(5) 0.0292(6) Uani 1 2 d S T P . .
I1 I 0.35912(5) 0.750000 0.20229(9) 0.0274(8) Uani 1 2 d S T P . .
I2 I 0.10503(4) 0.750000 0.76534(9) 0.0298(8) Uani 1 2 d S T P . .
I3 I 0.32477(3) 0.64025(4) 0.66573(6) 0.0293(6) Uani 1 1 d . . . . .
F2 F 0.4420(3) 0.4055(5) 0.3718(8) 0.035(7) Uani 1 1 d . . . . .
F1 F 0.2616(3) 0.4462(4) 0.4488(6) 0.031(5) Uani 1 1 d . . . . .
N4 N 0.4082(4) 0.5969(6) 0.1931(8) 0.0178(13) Uiso 1 1 d . . . . .
N2 N 0.5106(4) 0.6023(5) 0.1326(8) 0.0191(13) Uiso 1 1 d . . . . .
C3 C 0.5062(5) 0.5281(7) 0.2210(10) 0.0171(16) Uiso 1 1 d . . . . .
C6 C 0.3378(5) 0.4761(6) 0.3672(10) 0.0167(16) Uiso 1 1 d . . . . .
N3 N 0.5733(4) 0.5628(5) 0.1479(8) 0.0215(14) Uiso 1 1 d . . . . .
N1 N 0.6969(4) 0.6488(5) 0.3374(9) 0.0255(14) Uiso 1 1 d . . . . .
H1A H 0.682137 0.617879 0.362661 0.038 Uiso 1 1 calc R U . . .
H1B H 0.719530 0.662734 0.456427 0.038 Uiso 1 1 calc R U . . .
H1C H 0.747769 0.650779 0.238901 0.038 Uiso 1 1 calc R U . . .
C2 C 0.5512(5) 0.6491(6) 0.0724(10) 0.0209(16) Uiso 1 1 d . . . . .
H2A H 0.493442 0.668652 0.016189 0.025 Uiso 1 1 calc R U . . .
H2B H 0.604789 0.645387 -0.037711 0.025 Uiso 1 1 calc R U . . .
C7 C 0.4374(6) 0.4518(9) 0.3291(13) 0.020(2) Uiso 1 1 d . . . . .
C1 C 0.5995(5) 0.6735(6) 0.2612(10) 0.0272(18) Uiso 1 1 d . . . . .
H1D H 0.617229 0.706549 0.224049 0.033 Uiso 1 1 calc R U . . .
H1E H 0.547248 0.674486 0.374979 0.033 Uiso 1 1 calc R U . . .
C5 C 0.3172(5) 0.5223(7) 0.3300(10) 0.0179(16) Uiso 1 1 d . . . . .
H5 H 0.250538 0.536035 0.355071 0.022 Uiso 1 1 calc R U . . .
C4 C 0.4048(4) 0.5492(7) 0.2492(10) 0.0161(15) Uiso 1 1 d . . . . .
C8 C 0.5238(5) 0.4783(6) 0.2571(10) 0.0163(15) Uiso 1 1 d . . . . .
H8 H 0.590141 0.464150 0.233523 0.020 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.01990(19) 0.0472(18) 0.0205(2) 0.000 -0.00006(13) 0.000
I1 0.0241(3) 0.040(3) 0.0183(3) 0.000 0.0000(2) 0.000
I2 0.0166(3) 0.047(3) 0.0261(3) 0.000 0.0000(2) 0.000
I3 0.0250(2) 0.0395(18) 0.0234(2) 0.0000(4) 0.00003(16) 0.0033(4)
F2 0.029(2) 0.04(2) 0.036(3) 0.000(5) 0.0053(17) 0.005(4)
F1 0.0227(19) 0.036(17) 0.034(2) 0.006(3) 0.0052(15) -0.004(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.1926(7) 1_556 ?
Pb1 I1 3.1084(6) . ?
Pb1 I2 3.1464(7) . ?
Pb1 I2 3.1455(7) 6_657 ?
Pb1 I3 3.0691(13) 7_575 ?
Pb1 I3 3.0691(13) . ?
F2 C7 1.31(2) . ?
F1 C6 1.364(14) . ?
N4 N2 1.344(8) . ?
N4 C4 1.37(2) . ?
N2 N3 1.351(17) . ?
N2 C2 1.44(2) . ?
C3 N3 1.356(17) . ?
C3 C4 1.408(14) . ?
C3 C8 1.41(2) . ?
C6 C7 1.434(17) . ?
C6 C5 1.33(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.478(12) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.497(13) . ?
C7 C8 1.383(19) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C5 H5 0.9300 . ?
C5 C4 1.419(16) . ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 177.77(3) . 1_556 ?
I1 Pb1 I2 99.157(18) . . ?
I1 Pb1 I2 93.355(18) . 6_657 ?
I2 Pb1 I1 84.413(18) 6_657 1_556 ?
I2 Pb1 I1 83.075(17) . 1_556 ?
I2 Pb1 I2 167.488(12) 6_657 . ?
I3 Pb1 I1 86.621(10) . . ?
I3 Pb1 I1 93.647(10) . 1_556 ?
I3 Pb1 I1 86.622(10) 7_575 . ?
I3 Pb1 I1 93.647(10) 7_575 1_556 ?
I3 Pb1 I2 97.145(10) 7_575 6_657 ?
I3 Pb1 I2 83.672(10) 7_575 . ?
I3 Pb1 I2 97.144(10) . 6_657 ?
I3 Pb1 I2 83.673(10) . . ?
I3 Pb1 I3 164.52(2) 7_575 . ?
Pb1 I1 Pb1 177.77(3) . 1_554 ?
Pb1 I2 Pb1 176.46(2) 6_557 . ?
N2 N4 C4 102.2(10) . . ?
N4 N2 N3 116.1(12) . . ?
N4 N2 C2 120.7(12) . . ?
N3 N2 C2 122.9(6) . . ?
N3 C3 C4 107.8(15) . . ?
N3 C3 C8 130.5(8) . . ?
C4 C3 C8 121.6(12) . . ?
F1 C6 C7 112.7(15) . . ?
C5 C6 F1 121.2(8) . . ?
C5 C6 C7 126.2(13) . . ?
N2 N3 C3 103.9(7) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N2 C2 H2A 109.7 . . ?
N2 C2 H2B 109.7 . . ?
N2 C2 C1 109.9(8) . . ?
H2A C2 H2B 108.2 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
F2 C7 C6 117.5(12) . . ?
F2 C7 C8 123.5(12) . . ?
C8 C7 C6 119(2) . . ?
N1 C1 C2 112.4(11) . . ?
N1 C1 H1D 109.1 . . ?
N1 C1 H1E 109.1 . . ?
C2 C1 H1D 109.1 . . ?
C2 C1 H1E 109.1 . . ?
H1D C1 H1E 107.9 . . ?
C6 C5 H5 122.6 . . ?
C6 C5 C4 114.9(10) . . ?
C4 C5 H5 122.6 . . ?
N4 C4 C3 109.9(10) . . ?
N4 C4 C5 128.6(11) . . ?
C3 C4 C5 121.4(16) . . ?
C3 C8 H8 121.6 . . ?
C7 C8 C3 116.7(12) . . ?
C7 C8 H8 121.6 . . ?

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
F2 C7 C8 C3 -179.2(9) . . . . ?
F1 C6 C7 F2 1.2(13) . . . . ?
F1 C6 C7 C8 -176.6(7) . . . . ?
F1 C6 C5 C4 178.8(6) . . . . ?
N4 N2 N3 C3 1.2(8) . . . . ?
N4 N2 C2 C1 92.6(7) . . . . ?
N2 N4 C4 C3 0.4(9) . . . . ?
N2 N4 C4 C5 178.9(7) . . . . ?
N2 C2 C1 N1 66.9(10) . . . . ?
C6 C7 C8 C3 -1.5(13) . . . . ?
C6 C5 C4 N4 179.0(9) . . . . ?
C6 C5 C4 C3 -2.7(12) . . . . ?
N3 N2 C2 C1 -82.1(10) . . . . ?
N3 C3 C4 N4 0.3(9) . . . . ?
N3 C3 C4 C5 -178.3(7) . . . . ?
N3 C3 C8 C7 -178.6(7) . . . . ?
C2 N2 N3 C3 176.1(7) . . . . ?
C7 C6 C5 C4 -1.4(14) . . . . ?
C5 C6 C7 F2 -178.6(9) . . . . ?
C5 C6 C7 C8 3.6(15) . . . . ?
C4 N4 N2 N3 -1.0(9) . . . . ?
C4 N4 N2 C2 -176.0(7) . . . . ?
C4 C3 N3 N2 -0.8(8) . . . . ?
C4 C3 C8 C7 -2.4(13) . . . . ?
C8 C3 N3 N2 175.8(9) . . . . ?
C8 C3 C4 N4 -176.7(8) . . . . ?
C8 C3 C4 C5 4.7(12) . . . . ?

_shelx_res_file                  
;
TITL mo_DAC24_F2BTa2PbI4_4p30GPa_0ma_d.res in Pnma
    4p33gpa_good.res
    created by SHELXL-2019/1 at 16:19:38 on 08-Feb-2024
REM Old TITL __TMP__ in Pnma
REM SHELXT solution in Pnma: R1 0.151, Rweak 0.004, Alpha 0.033
REM <I/s> 2.816 for 94 systematic absences, Orientation as input
REM Formula found by SHELXT: C13 F4 I4 N6 Pb
CELL 0.71073 12.5029 27.7091 6.2997 90 90 90
ZERR 4 0.0007 0.0031 0.0004 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H F I N Pb
UNIT 64 72 16 16 32 4

L.S. 10
PLAN  2
TEMP 0
CONF
BOND
LIST 6
fmap 2
MORE -1
BOND $H
ACTA
OMIT 2 0 7
OMIT 5 11 6
OMIT 7 11 5
OMIT 8 11 5
OMIT 9 4 6
OMIT 9 11 4
REM <olex2.extras>
REM <HklSrc "%.\\4p33GPa_good.hkl">
REM </olex2.extras>

WGHT    0.008000   13.357800
FVAR       0.11851
PB1   6    0.354212    0.750000    0.695605    10.50000    0.01990    0.04722 =
         0.02053    0.00000   -0.00006    0.00000
I1    4    0.359118    0.750000    0.202287    10.50000    0.02414    0.03974 =
         0.01833    0.00000   -0.00005    0.00000
I2    4    0.105027    0.750000    0.765344    10.50000    0.01660    0.04665 =
         0.02615    0.00000    0.00000    0.00000
I3    4    0.324770    0.640249    0.665734    11.00000    0.02501    0.03948 =
         0.02341   -0.00005    0.00003    0.00327
F2    3    0.441999    0.405519    0.371844    11.00000    0.02860    0.03917 =
         0.03646    0.00010    0.00531    0.00504
F1    3    0.261578    0.446154    0.448762    11.00000    0.02275    0.03624 =
         0.03361    0.00616    0.00519   -0.00354
N4    5    0.408229    0.596859    0.193119    11.00000    0.01776
N2    5    0.510608    0.602332    0.132565    11.00000    0.01909
C3    1    0.506249    0.528096    0.220952    11.00000    0.01710
C6    1    0.337833    0.476063    0.367235    11.00000    0.01672
N3    5    0.573296    0.562775    0.147942    11.00000    0.02153
N1    5    0.696924    0.648768    0.337379    11.00000    0.02548
AFIX 137
H1A   2    0.682137    0.617879    0.362661    11.00000   -1.50000
H1B   2    0.719530    0.662734    0.456427    11.00000   -1.50000
H1C   2    0.747769    0.650779    0.238901    11.00000   -1.50000
AFIX   0
C2    1    0.551168    0.649062    0.072388    11.00000    0.02088
AFIX  23
H2A   2    0.493442    0.668652    0.016189    11.00000   -1.20000
H2B   2    0.604789    0.645387   -0.037711    11.00000   -1.20000
AFIX   0
C7    1    0.437368    0.451832    0.329120    11.00000    0.02020
C1    1    0.599489    0.673535    0.261219    11.00000    0.02718
AFIX  23
H1D   2    0.617229    0.706549    0.224049    11.00000   -1.20000
H1E   2    0.547248    0.674486    0.374979    11.00000   -1.20000
AFIX   0
C5    1    0.317249    0.522324    0.330037    11.00000    0.01795
AFIX  43
H5    2    0.250538    0.536035    0.355071    11.00000   -1.20000
AFIX   0
C4    1    0.404805    0.549233    0.249189    11.00000    0.01615
C8    1    0.523784    0.478339    0.257065    11.00000    0.01625
AFIX  43
H8    2    0.590141    0.464150    0.233523    11.00000   -1.20000
AFIX   0
HKLF 4




REM  mo_DAC24_F2BTa2PbI4_4p30GPa_0ma_d.res in Pnma
REM wR2 = 0.0410, GooF = S = 1.157, Restrained GooF = 1.157 for all data
REM R1 = 0.0185 for 836 Fo > 4sig(Fo) and 0.0200 for all 869 data
REM 95 parameters refined using 0 restraints

END

WGHT      0.0081     13.5008

REM Highest difference peak  0.409,  deepest hole -0.451,  1-sigma level  0.098
Q1    1   0.3580  0.7500  0.9243  10.50000  0.05    0.41
Q2    1   0.3774  0.7500  0.4773  10.50000  0.05    0.40
;
_shelx_res_checksum              5332
_olex2_submission_special_instructions 'No special instructions were received'
_olex2_exptl_crystal_mounting_method 
'Crystal mounted in a Diamond anvil cell of 100 degre opening angle'

_vrf_PLAT029_4p33gpa_good        
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT201_4p33gpa_good        
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         12 Report
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the available data, preventing from a complete anisotropic refienement. 
;
_vrf_PLAT933_4p33gpa_good        
;
PROBLEM: Number of HKL-OMIT Records in Embedded .res File          
RESPONSE: Experiment done in a Diamond Anvil Cell some reflections are close 
to gasket ring/shadow or close to diamond peaks and should be deleted.  
;
_vrf_PLAT911_4p33gpa_good        
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT910_4p33gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT913_4p33gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT088_4p33gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space and then number of measured reflections inducing
a low Data / Parameter Ratio despite isotropic refinement done to limit this 
problem
;
####################################################################### 
# 
# 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_1p60gpa_good
_database_code_depnum_ccdc_archive 'CCDC 2365961'
loop_
_audit_author_name
_audit_author_address
'Maxime Deutsch' 'University of Lorraine'
_audit_update_record             
;
2024-06-26 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-02-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H9 F2 N4)'
_chemical_formula_sum            'C16 H18 F4 I4 N8 Pb'
_chemical_formula_weight         1113.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.6990(5)
_cell_length_b                   28.928(2)
_cell_length_c                   6.4727(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2377.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9759
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      25.890
_cell_measurement_theta_min      3.225
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.344
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0865 before and 0.0658 after correction.
The Ratio of minimum to maximum transmission is 0.8088.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.110
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.411
_diffrn_reflns_Laue_measured_fraction_max 0.387
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            26600
_diffrn_reflns_point_group_measured_fraction_full 0.411
_diffrn_reflns_point_group_measured_fraction_max 0.387
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.094
_diffrn_reflns_theta_min         3.208
_diffrn_ambient_temperature      300(3)
_diffrn_ambient_pressure         1.60e+06
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.411
_diffrn_measured_fraction_theta_max 0.387
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON III CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                893
_reflns_number_total             928
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         928
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0168
_refine_ls_restrained_S_all      1.153
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0109P)²+7.8039P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0394
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.34331(2) 0.750000 0.69774(4) 0.0291(5) Uani 1 2 d S T P . .
I1 I 0.35059(4) 0.750000 0.20487(7) 0.0315(8) Uani 1 2 d S T P . .
I2 I 0.09422(3) 0.750000 0.75546(8) 0.0372(8) Uani 1 2 d S T P . .
I3 I 0.32268(3) 0.64266(4) 0.67282(5) 0.0340(5) Uani 1 1 d . . . . .
F2 F 0.4442(3) 0.4110(4) 0.3607(6) 0.0395(10) Uiso 1 1 d . . . . .
F1 F 0.2634(2) 0.4485(3) 0.4356(5) 0.040(4) Uani 1 1 d . . . . .
N4 N 0.4063(3) 0.5943(5) 0.2016(7) 0.0261(12) Uiso 1 1 d . . . . .
N2 N 0.5065(3) 0.6006(4) 0.1467(6) 0.0227(11) Uiso 1 1 d . . . . .
C3 C 0.5040(4) 0.5293(6) 0.2225(8) 0.0203(13) Uiso 1 1 d . . . . .
C6 C 0.3378(4) 0.4770(6) 0.3602(9) 0.0235(15) Uiso 1 1 d . . . . .
N3 N 0.5690(3) 0.5629(4) 0.1566(6) 0.0237(11) Uiso 1 1 d . . . . .
N1 N 0.6951(4) 0.6455(4) 0.3362(8) 0.0362(13) Uiso 1 1 d . . . . .
H1A H 0.712892 0.654730 0.462727 0.054 Uiso 1 1 calc R U . . .
H1B H 0.746747 0.652373 0.248497 0.054 Uiso 1 1 calc R U . . .
H1C H 0.684313 0.615139 0.336373 0.054 Uiso 1 1 calc R U . . .
C2 C 0.5457(4) 0.6451(5) 0.0897(8) 0.0263(13) Uiso 1 1 d . . . . .
H2A H 0.488285 0.663695 0.036696 0.032 Uiso 1 1 calc R U . . .
H2B H 0.597295 0.641536 -0.019743 0.032 Uiso 1 1 calc R U . . .
C7 C 0.4379(4) 0.4557(6) 0.3225(9) 0.0256(15) Uiso 1 1 d . . . . .
C1 C 0.5962(4) 0.6698(5) 0.2707(9) 0.0351(16) Uiso 1 1 d . . . . .
H1D H 0.612507 0.701345 0.231856 0.042 Uiso 1 1 calc R U . . .
H1E H 0.547107 0.670686 0.385547 0.042 Uiso 1 1 calc R U . . .
C5 C 0.3181(5) 0.5222(6) 0.3303(8) 0.0245(14) Uiso 1 1 d . . . . .
H5 H 0.252237 0.534739 0.358885 0.029 Uiso 1 1 calc R U . . .
C4 C 0.4028(4) 0.5506(6) 0.2523(8) 0.0193(13) Uiso 1 1 d . . . . .
C8 C 0.5211(4) 0.4827(6) 0.2549(8) 0.0209(13) Uiso 1 1 d . . . . .
H8 H 0.587115 0.469699 0.231823 0.025 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.02280(17) 0.0397(17) 0.02484(18) 0.000 -0.00031(10) 0.000
I1 0.0330(3) 0.040(2) 0.0216(3) 0.000 0.00057(18) 0.000
I2 0.0192(2) 0.055(2) 0.0375(3) 0.000 0.0009(2) 0.000
I3 0.0317(2) 0.0423(17) 0.0279(2) -0.0001(3) -0.00016(13) 0.0027(3)
F1 0.0256(16) 0.054(14) 0.0405(18) 0.006(3) 0.0072(13) -0.009(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.2838(5) 1_556 ?
Pb1 I1 3.1915(5) . ?
Pb1 I2 3.2006(5) 6_657 ?
Pb1 I2 3.1853(5) . ?
Pb1 I3 3.1202(11) 7_575 ?
Pb1 I3 3.1203(11) . ?
F2 C7 1.320(17) . ?
F1 C6 1.346(12) . ?
N4 N2 1.333(7) . ?
N4 C4 1.306(19) . ?
N2 N3 1.351(14) . ?
N2 C2 1.428(18) . ?
C3 N3 1.344(15) . ?
C3 C4 1.440(12) . ?
C3 C8 1.382(19) . ?
C6 C7 1.434(13) . ?
C6 C5 1.34(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.500(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.514(12) . ?
C7 C8 1.385(15) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C5 H5 0.9300 . ?
C5 C4 1.445(15) . ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 176.73(2) . 1_556 ?
I1 Pb1 I2 93.771(15) . 6_657 ?
I2 Pb1 I1 98.396(15) . . ?
I2 Pb1 I1 84.877(14) . 1_556 ?
I2 Pb1 I1 82.956(14) 6_657 1_556 ?
I2 Pb1 I2 167.833(10) . 6_657 ?
I3 Pb1 I1 93.098(8) . 1_556 ?
I3 Pb1 I1 87.178(8) . . ?
I3 Pb1 I1 93.097(8) 7_575 1_556 ?
I3 Pb1 I1 87.178(8) 7_575 . ?
I3 Pb1 I2 95.078(9) 7_575 6_657 ?
I3 Pb1 I2 85.563(9) . . ?
I3 Pb1 I2 85.563(9) 7_575 . ?
I3 Pb1 I2 95.078(9) . 6_657 ?
I3 Pb1 I3 168.679(17) 7_575 . ?
Pb1 I1 Pb1 176.73(2) . 1_554 ?
Pb1 I2 Pb1 178.695(19) . 6_557 ?
C4 N4 N2 103.4(9) . . ?
N4 N2 N3 116.0(11) . . ?
N4 N2 C2 121.7(11) . . ?
N3 N2 C2 122.3(6) . . ?
N3 C3 C4 106.3(13) . . ?
N3 C3 C8 131.1(7) . . ?
C8 C3 C4 122.6(10) . . ?
F1 C6 C7 114.8(13) . . ?
F1 C6 C5 121.1(7) . . ?
C5 C6 C7 124.0(10) . . ?
C3 N3 N2 103.8(6) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N2 C2 H2A 109.2 . . ?
N2 C2 H2B 109.2 . . ?
N2 C2 C1 111.9(7) . . ?
H2A C2 H2B 107.9 . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
F2 C7 C6 116.4(9) . . ?
F2 C7 C8 124.4(9) . . ?
C8 C7 C6 119.2(15) . . ?
N1 C1 C2 110.6(9) . . ?
N1 C1 H1D 109.5 . . ?
N1 C1 H1E 109.5 . . ?
C2 C1 H1D 109.5 . . ?
C2 C1 H1E 109.5 . . ?
H1D C1 H1E 108.1 . . ?
C6 C5 H5 121.2 . . ?
C6 C5 C4 117.7(8) . . ?
C4 C5 H5 121.2 . . ?
N4 C4 C3 110.5(9) . . ?
N4 C4 C5 131.6(9) . . ?
C3 C4 C5 117.9(14) . . ?
C3 C8 H8 120.7 . . ?
C7 C8 C3 118.5(9) . . ?
C7 C8 H8 120.7 . . ?

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
F2 C7 C8 C3 -179.4(7) . . . . ?
F1 C6 C7 F2 1.6(9) . . . . ?
F1 C6 C7 C8 -176.7(5) . . . . ?
F1 C6 C5 C4 179.0(5) . . . . ?
N4 N2 N3 C3 0.3(6) . . . . ?
N4 N2 C2 C1 94.7(6) . . . . ?
N2 N4 C4 C3 -1.4(8) . . . . ?
N2 N4 C4 C5 178.2(6) . . . . ?
N2 C2 C1 N1 67.5(9) . . . . ?
C6 C7 C8 C3 -1.2(9) . . . . ?
C6 C5 C4 N4 177.2(8) . . . . ?
C6 C5 C4 C3 -3.3(10) . . . . ?
N3 N2 C2 C1 -82.4(9) . . . . ?
N3 C3 C4 N4 1.6(8) . . . . ?
N3 C3 C4 C5 -178.0(5) . . . . ?
N3 C3 C8 C7 -179.3(5) . . . . ?
C2 N2 N3 C3 177.6(6) . . . . ?
C7 C6 C5 C4 1.0(11) . . . . ?
C5 C6 C7 F2 179.7(7) . . . . ?
C5 C6 C7 C8 1.3(10) . . . . ?
C4 N4 N2 N3 0.7(8) . . . . ?
C4 N4 N2 C2 -176.6(6) . . . . ?
C4 C3 N3 N2 -1.1(6) . . . . ?
C4 C3 C8 C7 -1.3(10) . . . . ?
C8 C3 N3 N2 177.2(8) . . . . ?
C8 C3 C4 N4 -176.8(7) . . . . ?
C8 C3 C4 C5 3.6(10) . . . . ?

_shelx_res_file                  
;
TITL mo_DAC24_F2BTa2PbI4_1p60GPa_0ma_e.res in Pnma
    1p60gpa_good.res
    created by SHELXL-2019/1 at 17:27:12 on 07-Feb-2024
REM Old TITL __TMP__ in Pnma
REM SHELXT solution in Pnma: R1 0.311, Rweak 0.006, Alpha 0.038
REM <I/s> 2.425 for 101 systematic absences, Orientation as input
REM Formula found by SHELXT: C12 F2 I4 N6 Pb
CELL 0.71073 12.699 28.9279 6.4727 90 90 90
ZERR 4 0.0005 0.0021 0.0003 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H F I N Pb
UNIT 64 72 16 16 32 4

L.S. 10
PLAN  1
TEMP 0
CONF
BOND
LIST 6
MORE -1
BOND $H
fmap 2
acta
OMIT 6 8 0
OMIT 7 11 6
OMIT 8 10 6
REM <olex2.extras>
REM <HklSrc "%.\\1p60GPa_good.hkl">
REM </olex2.extras>

WGHT    0.010900    7.803900
FVAR       0.11364
PB1   6    0.343315    0.750000    0.697737    10.50000    0.02280    0.03973 =
         0.02484    0.00000   -0.00031    0.00000
I1    4    0.350593    0.750000    0.204870    10.50000    0.03303    0.03979 =
         0.02163    0.00000    0.00057    0.00000
I2    4    0.094216    0.750000    0.755462    10.50000    0.01919    0.05502 =
         0.03752    0.00000    0.00093    0.00000
I3    4    0.322675    0.642663    0.672817    11.00000    0.03169    0.04232 =
         0.02792   -0.00012   -0.00016    0.00267
F2    3    0.444198    0.410965    0.360671    11.00000    0.03946
F1    3    0.263357    0.448509    0.435569    11.00000    0.02561    0.05409 =
         0.04054    0.00633    0.00720   -0.00910
N4    5    0.406320    0.594291    0.201640    11.00000    0.02608
N2    5    0.506484    0.600577    0.146655    11.00000    0.02270
C3    1    0.504034    0.529273    0.222494    11.00000    0.02026
C6    1    0.337805    0.477034    0.360216    11.00000    0.02348
N3    5    0.568999    0.562855    0.156590    11.00000    0.02368
N1    5    0.695082    0.645540    0.336242    11.00000    0.03619
AFIX 137
H1A   2    0.712892    0.654730    0.462727    11.00000   -1.50000
H1B   2    0.746747    0.652373    0.248497    11.00000   -1.50000
H1C   2    0.684313    0.615139    0.336373    11.00000   -1.50000
AFIX   0
C2    1    0.545746    0.645058    0.089717    11.00000    0.02631
AFIX  23
H2A   2    0.488285    0.663695    0.036696    11.00000   -1.20000
H2B   2    0.597295    0.641536   -0.019743    11.00000   -1.20000
AFIX   0
C7    1    0.437860    0.455685    0.322468    11.00000    0.02565
C1    1    0.596159    0.669767    0.270743    11.00000    0.03512
AFIX  23
H1D   2    0.612507    0.701345    0.231856    11.00000   -1.20000
H1E   2    0.547107    0.670686    0.385547    11.00000   -1.20000
AFIX   0
C5    1    0.318097    0.522217    0.330318    11.00000    0.02452
AFIX  43
H5    2    0.252237    0.534739    0.358885    11.00000   -1.20000
AFIX   0
C4    1    0.402771    0.550629    0.252294    11.00000    0.01932
C8    1    0.521145    0.482670    0.254881    11.00000    0.02091
AFIX  43
H8    2    0.587115    0.469699    0.231823    11.00000   -1.20000
AFIX   0
HKLF 4




REM  mo_DAC24_F2BTa2PbI4_1p60GPa_0ma_e.res in Pnma
REM wR2 = 0.0394, GooF = S = 1.153, Restrained GooF = 1.153 for all data
REM R1 = 0.0168 for 893 Fo > 4sig(Fo) and 0.0187 for all 928 data
REM 90 parameters refined using 0 restraints

END

WGHT      0.0114      8.1218

REM Highest difference peak  0.398,  deepest hole -0.444,  1-sigma level  0.110
Q1    1   0.4287  0.7500  0.5010  10.50000  0.05    0.40
;
_shelx_res_checksum              42100
_olex2_submission_special_instructions 'No special instructions were received'
_olex2_exptl_crystal_mounting_method 
'Crystal mounted in a Diamond anvil cell of 100 degre opening angle'

_vrf_PLAT029_1p60gpa_good        
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT201_1p60gpa_good        
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         12 Report
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the available data, preventing from a complete anisotropic refienement. 
;
_vrf_PLAT933_1p60gpa_good        
;
PROBLEM: Number of HKL-OMIT Records in Embedded .res File          
RESPONSE: Experiment done in a Diamond Anvil Cell some reflections are close 
to gasket ring/shadow or close to diamond peaks and should be deleted.  
;
_vrf_PLAT911_1p60gpa_good        
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT910_1p60gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT913_1p60gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
####################################################################### 
# 
# 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_0p2gpa_good
_database_code_depnum_ccdc_archive 'CCDC 2365957'
loop_
_audit_author_name
_audit_author_address
'Maxime Deutsch' 'University of Lorraine'
_audit_update_record             
;
2024-06-26 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-02-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H9 F2 N4)'
_chemical_formula_sum            'C16 H18 F4 I4 N8 Pb'
_chemical_formula_weight         1113.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.9028(5)
_cell_length_b                   30.077(3)
_cell_length_c                   6.6218(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2569.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9153
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      25.084
_cell_measurement_theta_min      3.361
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.422
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0902 before and 0.0651 after correction.
The Ratio of minimum to maximum transmission is 0.8009.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.877
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 0.404
_diffrn_reflns_Laue_measured_fraction_max 0.377
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            29522
_diffrn_reflns_point_group_measured_fraction_full 0.404
_diffrn_reflns_point_group_measured_fraction_max 0.377
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.147
_diffrn_reflns_theta_min         3.458
_diffrn_ambient_temperature      300(3)
_diffrn_ambient_pressure         0.20e+06
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.404
_diffrn_measured_fraction_theta_max 0.377
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON III CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                932
_reflns_number_total             983
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         983
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0170
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0144P)²+4.7101P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0383
_refine_ls_wR_factor_ref         0.0390
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.33280(2) 0.750000 0.70183(4) 0.0360(5) Uani 1 2 d S T P . .
I1 I 0.34036(3) 0.750000 0.21078(6) 0.0417(7) Uani 1 2 d S T P . .
I2 I 0.08564(3) 0.750000 0.74588(7) 0.0510(7) Uani 1 2 d S T P . .
I3 I 0.31849(3) 0.64510(3) 0.68131(5) 0.0425(5) Uani 1 1 d . . . . .
F2 F 0.4473(3) 0.4164(3) 0.3489(5) 0.050(6) Uani 1 1 d . . . . .
F1 F 0.2671(2) 0.4504(2) 0.4232(4) 0.051(4) Uani 1 1 d . . . . .
N4 N 0.4041(3) 0.5931(4) 0.2113(6) 0.0310(11) Uiso 1 1 d . . . . .
N2 N 0.5023(3) 0.5995(4) 0.1589(6) 0.0300(10) Uiso 1 1 d . . . . .
C3 C 0.5017(3) 0.5296(5) 0.2247(7) 0.0249(12) Uiso 1 1 d . . . . .
C6 C 0.3397(4) 0.4788(5) 0.3525(7) 0.0297(13) Uiso 1 1 d . . . . .
N3 N 0.5655(3) 0.5641(3) 0.1644(5) 0.0309(10) Uiso 1 1 d . . . . .
N1 N 0.6952(3) 0.6428(4) 0.3291(7) 0.0469(12) Uiso 1 1 d . . . . .
H1A H 0.738990 0.646083 0.226345 0.070 Uiso 1 1 calc R U . . .
H1B H 0.683368 0.613963 0.349393 0.070 Uiso 1 1 calc R U . . .
H1C H 0.722595 0.654631 0.439990 0.070 Uiso 1 1 calc R U . . .
C2 C 0.5412(4) 0.6423(5) 0.1052(7) 0.0377(13) Uiso 1 1 d . . . . .
H2A H 0.484238 0.660655 0.058034 0.045 Uiso 1 1 calc R U . . .
H2B H 0.590021 0.639137 -0.005209 0.045 Uiso 1 1 calc R U . . .
C7 C 0.4393(5) 0.4599(6) 0.3160(9) 0.0341(17) Uiso 1 1 d . . . . .
C1 C 0.5948(4) 0.6658(5) 0.2808(7) 0.0449(15) Uiso 1 1 d . . . . .
H1D H 0.608197 0.696557 0.245242 0.054 Uiso 1 1 calc R U . . .
H1E H 0.550003 0.665438 0.398455 0.054 Uiso 1 1 calc R U . . .
C5 C 0.3189(4) 0.5228(5) 0.3258(7) 0.0313(13) Uiso 1 1 d . . . . .
H5 H 0.253821 0.534786 0.352466 0.038 Uiso 1 1 calc R U . . .
C4 C 0.4022(3) 0.5494(5) 0.2550(7) 0.0256(11) Uiso 1 1 d . . . . .
C8 C 0.5211(4) 0.4856(5) 0.2535(7) 0.0301(12) Uiso 1 1 d . . . . .
H8 H 0.586524 0.473469 0.231831 0.036 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.02943(16) 0.0444(16) 0.03401(18) 0.000 -0.00029(9) 0.000
I1 0.0453(3) 0.050(2) 0.0298(3) 0.000 0.00158(17) 0.000
I2 0.0251(2) 0.071(2) 0.0566(3) 0.000 0.0006(2) 0.000
I3 0.0437(2) 0.0466(18) 0.0371(2) -0.0002(3) -0.00030(13) 0.0029(3)
F2 0.053(2) 0.043(19) 0.054(2) -0.003(4) 0.0014(14) 0.001(3)
F1 0.0379(15) 0.060(13) 0.0567(19) 0.004(3) 0.0066(13) -0.012(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
Pb1 I1 3.3716(5) 1_556 ?
Pb1 I1 3.2531(5) . ?
Pb1 I2 3.2806(5) 6_657 ?
Pb1 I2 3.2024(5) . ?
Pb1 I3 3.1636(11) . ?
Pb1 I3 3.1636(11) 7_575 ?
F2 C7 1.331(19) . ?
F1 C6 1.352(11) . ?
N4 N2 1.328(6) . ?
N4 C4 1.347(15) . ?
N2 N3 1.341(12) . ?
N2 C2 1.428(16) . ?
C3 N3 1.384(13) . ?
C3 C4 1.430(10) . ?
C3 C8 1.361(17) . ?
C6 C7 1.426(12) . ?
C6 C5 1.362(18) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.503(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.526(11) . ?
C7 C8 1.371(15) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C5 H5 0.9300 . ?
C5 C4 1.420(13) . ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 176.625(18) . 1_556 ?
I1 Pb1 I2 94.341(13) . 6_657 ?
I2 Pb1 I1 96.943(14) . . ?
I2 Pb1 I1 86.432(13) . 1_556 ?
I2 Pb1 I1 82.284(13) 6_657 1_556 ?
I2 Pb1 I2 168.715(9) . 6_657 ?
I3 Pb1 I1 92.557(8) 7_575 1_556 ?
I3 Pb1 I1 87.640(8) 7_575 . ?
I3 Pb1 I1 92.557(8) . 1_556 ?
I3 Pb1 I1 87.640(8) . . ?
I3 Pb1 I2 93.588(7) . 6_657 ?
I3 Pb1 I2 86.892(7) 7_575 . ?
I3 Pb1 I2 86.892(7) . . ?
I3 Pb1 I2 93.588(8) 7_575 6_657 ?
I3 Pb1 I3 171.688(15) . 7_575 ?
Pb1 I1 Pb1 176.626(18) . 1_554 ?
Pb1 I2 Pb1 179.167(17) . 6_557 ?
N2 N4 C4 102.4(8) . . ?
N4 N2 N3 117.3(9) . . ?
N4 N2 C2 122.1(10) . . ?
N3 N2 C2 120.6(5) . . ?
N3 C3 C4 105.1(11) . . ?
C8 C3 N3 131.4(5) . . ?
C8 C3 C4 123.5(9) . . ?
F1 C6 C7 115.5(13) . . ?
F1 C6 C5 121.6(6) . . ?
C5 C6 C7 122.9(11) . . ?
N2 N3 C3 104.0(5) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N2 C2 H2A 109.0 . . ?
N2 C2 H2B 109.0 . . ?
N2 C2 C1 112.8(6) . . ?
H2A C2 H2B 107.8 . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
F2 C7 C6 115.7(10) . . ?
F2 C7 C8 122.8(9) . . ?
C8 C7 C6 121.4(16) . . ?
N1 C1 C2 109.8(8) . . ?
N1 C1 H1D 109.7 . . ?
N1 C1 H1E 109.7 . . ?
C2 C1 H1D 109.7 . . ?
C2 C1 H1E 109.7 . . ?
H1D C1 H1E 108.2 . . ?
C6 C5 H5 121.9 . . ?
C6 C5 C4 116.2(7) . . ?
C4 C5 H5 121.9 . . ?
N4 C4 C3 111.2(8) . . ?
N4 C4 C5 129.4(8) . . ?
C5 C4 C3 119.4(12) . . ?
C3 C8 C7 116.6(9) . . ?
C3 C8 H8 121.7 . . ?
C7 C8 H8 121.7 . . ?

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
F2 C7 C8 C3 179.7(7) . . . . ?
F1 C6 C7 F2 2.4(10) . . . . ?
F1 C6 C7 C8 -176.8(6) . . . . ?
F1 C6 C5 C4 178.6(4) . . . . ?
N4 N2 N3 C3 1.1(6) . . . . ?
N4 N2 C2 C1 96.9(6) . . . . ?
N2 N4 C4 C3 -0.8(6) . . . . ?
N2 N4 C4 C5 178.2(5) . . . . ?
N2 C2 C1 N1 70.0(8) . . . . ?
C6 C7 C8 C3 -1.2(10) . . . . ?
C6 C5 C4 N4 178.5(6) . . . . ?
C6 C5 C4 C3 -2.6(8) . . . . ?
N3 N2 C2 C1 -80.8(8) . . . . ?
N3 C3 C4 N4 1.5(6) . . . . ?
N3 C3 C4 C5 -177.6(5) . . . . ?
N3 C3 C8 C7 179.6(6) . . . . ?
C2 N2 N3 C3 179.0(5) . . . . ?
C7 C6 C5 C4 1.1(10) . . . . ?
C5 C6 C7 F2 -180.0(7) . . . . ?
C5 C6 C7 C8 0.8(11) . . . . ?
C4 N4 N2 N3 -0.2(6) . . . . ?
C4 N4 N2 C2 -178.0(5) . . . . ?
C4 C3 N3 N2 -1.4(5) . . . . ?
C4 C3 C8 C7 -0.4(10) . . . . ?
C8 C3 N3 N2 178.6(7) . . . . ?
C8 C3 C4 N4 -178.5(6) . . . . ?
C8 C3 C4 C5 2.4(9) . . . . ?

_shelx_res_file                  
;
TITL mo_DAC24_F2BTa2PbI4_0p15GPa_0ma_a.res in Pnma
    0p2gpa_good.res
    created by SHELXL-2019/1 at 11:39:18 on 05-Feb-2024
REM Old TITL __TMP__ in Pnma
REM SHELXT solution in Pnma: R1 0.208, Rweak 0.005, Alpha 0.038
REM <I/s> 2.003 for 105 systematic absences, Orientation as input
REM Formula found by SHELXT: C8 I4 N4 Pb
CELL 0.71073 12.9028 30.0772 6.6218 90 90 90
ZERR 4 0.0005 0.0025 0.0003 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H F I N Pb
UNIT 64 72 16 16 32 4

L.S. 10
PLAN  3
TEMP 0
CONF
BOND
LIST 6
MORE -1
BOND $H
fmap 2
acta
OMIT 0 11 7
OMIT 6 8 0
OMIT 7 11 6
OMIT 9 11 2
OMIT 10 11 0
OMIT 10 11 1
REM <olex2.extras>
REM <HklSrc "%.\\0p2GPa_good.hkl">
REM </olex2.extras>

WGHT    0.014400    4.710100
FVAR       0.22103
PB1   6    0.332800    0.750000    0.701830    10.50000    0.02943    0.04442 =
         0.03401    0.00000   -0.00029    0.00000
I1    4    0.340356    0.750000    0.210779    10.50000    0.04531    0.05008 =
         0.02982    0.00000    0.00158    0.00000
I2    4    0.085635    0.750000    0.745878    10.50000    0.02508    0.07144 =
         0.05656    0.00000    0.00062    0.00000
I3    4    0.318487    0.645095    0.681311    11.00000    0.04373    0.04660 =
         0.03707   -0.00018   -0.00030    0.00288
F2    3    0.447283    0.416417    0.348851    11.00000    0.05339    0.04284 =
         0.05431   -0.00314    0.00135    0.00064
F1    3    0.267113    0.450377    0.423180    11.00000    0.03785    0.05995 =
         0.05669    0.00410    0.00658   -0.01201
N4    5    0.404084    0.593120    0.211298    11.00000    0.03100
N2    5    0.502273    0.599492    0.158871    11.00000    0.02999
C3    1    0.501726    0.529568    0.224682    11.00000    0.02494
C6    1    0.339655    0.478821    0.352495    11.00000    0.02973
N3    5    0.565469    0.564116    0.164426    11.00000    0.03094
N1    5    0.695172    0.642771    0.329051    11.00000    0.04690
AFIX 137
H1A   2    0.738990    0.646083    0.226345    11.00000   -1.50000
H1B   2    0.683368    0.613963    0.349393    11.00000   -1.50000
H1C   2    0.722595    0.654631    0.439990    11.00000   -1.50000
AFIX   0
C2    1    0.541192    0.642345    0.105212    11.00000    0.03770
AFIX  23
H2A   2    0.484238    0.660655    0.058034    11.00000   -1.20000
H2B   2    0.590021    0.639137   -0.005209    11.00000   -1.20000
AFIX   0
C7    1    0.439260    0.459940    0.315979    11.00000    0.03407
C1    1    0.594769    0.665805    0.280783    11.00000    0.04492
AFIX  23
H1D   2    0.608197    0.696557    0.245242    11.00000   -1.20000
H1E   2    0.550003    0.665438    0.398455    11.00000   -1.20000
AFIX   0
C5    1    0.318874    0.522833    0.325823    11.00000    0.03134
AFIX  43
H5    2    0.253821    0.534786    0.352466    11.00000   -1.20000
AFIX   0
C4    1    0.402224    0.549406    0.255017    11.00000    0.02556
C8    1    0.521118    0.485558    0.253454    11.00000    0.03010
AFIX  43
H8    2    0.586524    0.473469    0.231831    11.00000   -1.20000
AFIX   0
HKLF 4




REM  mo_DAC24_F2BTa2PbI4_0p15GPa_0ma_a.res in Pnma
REM wR2 = 0.0390, GooF = S = 1.113, Restrained GooF = 1.113 for all data
REM R1 = 0.0170 for 932 Fo > 4sig(Fo) and 0.0189 for all 983 data
REM 95 parameters refined using 0 restraints

END

WGHT      0.0144      4.7101

REM Highest difference peak  0.266,  deepest hole -0.253,  1-sigma level  0.057
Q1    1   0.4201  0.7500  0.4527  10.50000  0.05    0.27
Q2    1   0.3213  0.7500  0.9512  10.50000  0.05    0.25
Q3    1   0.3000  0.6973  0.7494  11.00000  0.05    0.22
;
_shelx_res_checksum              37365
_olex2_submission_special_instructions 'No special instructions were received'
_olex2_exptl_crystal_mounting_method 
'Crystal mounted in a Diamond anvil cell of 100 degre opening angle'

_vrf_PLAT029_0p2gpa_good         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT201_0p2gpa_good         
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         12 Report
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the available data, preventing from a complete anisotropic refienement. 
;
_vrf_PLAT933_0p2gpa_good         
;
PROBLEM: Number of HKL-OMIT Records in Embedded .res File          
RESPONSE: Experiment done in a Diamond Anvil Cell some reflections are close 
to gasket ring/shadow or close to diamond peaks and should be deleted.  
;
_vrf_PLAT911_0p2gpa_good         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT910_0p2gpa_good         
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT913_0p2gpa_good         
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
####################################################################### 
# 
# 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_2p82gpa_good
_database_code_depnum_ccdc_archive 'CCDC 2365963'
loop_
_audit_author_name
_audit_author_address
'Maxime Deutsch' 'University of Lorraine'
_audit_update_record             
;
2024-06-26 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-02-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H9 F2 N4)'
_chemical_formula_sum            'C16 H18 F4 I4 N8 Pb'
_chemical_formula_weight         1113.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.5704(5)
_cell_length_b                   28.337(2)
_cell_length_c                   6.3725(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2269.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9759
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      25.64
_cell_measurement_theta_min      3.20
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.930
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0860 before and 0.0649 after correction.
The Ratio of minimum to maximum transmission is 0.8183.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.257
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.419
_diffrn_reflns_Laue_measured_fraction_max 0.384
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            25497
_diffrn_reflns_point_group_measured_fraction_full 0.419
_diffrn_reflns_point_group_measured_fraction_max 0.384
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.239
_diffrn_reflns_theta_min         3.241
_diffrn_ambient_temperature      300(3)
_diffrn_ambient_pressure         2.825e+06
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.419
_diffrn_measured_fraction_theta_max 0.384
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON III CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                869
_reflns_number_total             896
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         896
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0158
_refine_ls_restrained_S_all      1.158
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0119P)²+6.8766P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0361
_refine_ls_wR_factor_ref         0.0376
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.34826(2) 0.750000 0.69568(4) 0.0265(5) Uani 1 2 d S T P . .
I1 I 0.35490(4) 0.750000 0.20238(7) 0.0277(7) Uani 1 2 d S T P . .
I2 I 0.09917(3) 0.750000 0.75990(7) 0.0309(7) Uani 1 2 d S T P . .
I3 I 0.32402(3) 0.64152(4) 0.66833(5) 0.0302(5) Uani 1 1 d . . . . .
F2 F 0.4431(2) 0.4089(3) 0.3656(5) 0.0340(9) Uiso 1 1 d . . . . .
F1 F 0.2627(2) 0.4473(3) 0.4416(5) 0.030(4) Uani 1 1 d . . . . .
N4 N 0.4067(3) 0.5957(5) 0.1968(7) 0.0216(11) Uiso 1 1 d . . . . .
N2 N 0.5079(3) 0.6016(4) 0.1404(6) 0.0186(10) Uiso 1 1 d . . . . .
C3 C 0.5051(4) 0.5282(5) 0.2204(8) 0.0186(12) Uiso 1 1 d . . . . .
C6 C 0.3372(4) 0.4763(5) 0.3632(8) 0.0179(13) Uiso 1 1 d . . . . .
N3 N 0.5712(3) 0.5626(4) 0.1523(6) 0.0206(10) Uiso 1 1 d . . . . .
N1 N 0.6955(3) 0.6475(4) 0.3388(7) 0.0292(12) Uiso 1 1 d . . . . .
H1A H 0.682722 0.616821 0.354308 0.044 Uiso 1 1 calc R U . . .
H1B H 0.716287 0.659644 0.460941 0.044 Uiso 1 1 calc R U . . .
H1C H 0.746616 0.651598 0.243787 0.044 Uiso 1 1 calc R U . . .
C2 C 0.5478(4) 0.6464(5) 0.0804(8) 0.0232(13) Uiso 1 1 d . . . . .
H2A H 0.490435 0.665454 0.023925 0.028 Uiso 1 1 calc R U . . .
H2B H 0.600979 0.642504 -0.028552 0.028 Uiso 1 1 calc R U . . .
C7 C 0.4379(4) 0.4539(6) 0.3243(8) 0.0240(14) Uiso 1 1 d . . . . .
C1 C 0.5973(4) 0.6716(5) 0.2677(8) 0.0292(14) Uiso 1 1 d . . . . .
H1D H 0.613950 0.703898 0.229176 0.035 Uiso 1 1 calc R U . . .
H1E H 0.546377 0.672488 0.382081 0.035 Uiso 1 1 calc R U . . .
C5 C 0.3168(4) 0.5227(5) 0.3294(8) 0.0217(13) Uiso 1 1 d . . . . .
H5 H 0.250491 0.536013 0.355658 0.026 Uiso 1 1 calc R U . . .
C4 C 0.4039(3) 0.5497(5) 0.2509(8) 0.0159(12) Uiso 1 1 d . . . . .
C8 C 0.5231(4) 0.4810(5) 0.2560(8) 0.0182(12) Uiso 1 1 d . . . . .
H8 H 0.589935 0.467783 0.235026 0.022 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.02045(16) 0.0375(15) 0.02170(17) 0.000 -0.00017(10) 0.000
I1 0.0275(3) 0.037(2) 0.0190(3) 0.000 0.00036(17) 0.000
I2 0.0170(2) 0.045(2) 0.0304(3) 0.000 0.00031(18) 0.000
I3 0.0275(2) 0.0385(16) 0.02451(19) 0.0002(3) -0.00010(12) 0.0038(3)
F1 0.0235(15) 0.028(14) 0.0375(17) 0.003(3) 0.0061(12) -0.008(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
Pb1 I1 3.2300(5) 1_556 ?
Pb1 I1 3.1446(5) . ?
Pb1 I2 3.1667(5) 6_657 ?
Pb1 I2 3.1578(5) . ?
Pb1 I3 3.0939(10) . ?
Pb1 I3 3.0940(10) 7_575 ?
F2 C7 1.304(17) . ?
F1 C6 1.343(11) . ?
N4 N2 1.333(6) . ?
N4 C4 1.348(17) . ?
N2 N3 1.365(13) . ?
N2 C2 1.418(16) . ?
C3 N3 1.351(14) . ?
C3 C4 1.423(11) . ?
C3 C8 1.375(18) . ?
C6 C7 1.437(12) . ?
C6 C5 1.358(18) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.483(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.523(11) . ?
C7 C8 1.388(14) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C5 H5 0.9300 . ?
C5 C4 1.426(13) . ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 177.000(19) . 1_556 ?
I1 Pb1 I2 93.607(14) . 6_657 ?
I1 Pb1 I2 98.968(14) . . ?
I2 Pb1 I1 84.033(13) . 1_556 ?
I2 Pb1 I1 83.392(14) 6_657 1_556 ?
I2 Pb1 I2 167.425(9) . 6_657 ?
I3 Pb1 I1 86.922(8) 7_575 . ?
I3 Pb1 I1 93.374(8) 7_575 1_556 ?
I3 Pb1 I1 86.922(8) . . ?
I3 Pb1 I1 93.374(8) . 1_556 ?
I3 Pb1 I2 84.815(8) . . ?
I3 Pb1 I2 95.920(8) . 6_657 ?
I3 Pb1 I2 84.816(8) 7_575 . ?
I3 Pb1 I2 95.920(8) 7_575 6_657 ?
I3 Pb1 I3 166.970(16) . 7_575 ?
Pb1 I1 Pb1 176.999(19) . 1_554 ?
Pb1 I2 Pb1 177.681(17) . 6_557 ?
N2 N4 C4 102.4(8) . . ?
N4 N2 N3 116.1(10) . . ?
N4 N2 C2 121.6(10) . . ?
N3 N2 C2 122.3(5) . . ?
N3 C3 C4 106.6(12) . . ?
N3 C3 C8 130.7(6) . . ?
C8 C3 C4 122.7(9) . . ?
F1 C6 C7 114.2(12) . . ?
F1 C6 C5 121.3(6) . . ?
C5 C6 C7 124.5(9) . . ?
C3 N3 N2 104.0(6) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N2 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
N2 C2 C1 110.7(6) . . ?
H2A C2 H2B 108.1 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
F2 C7 C6 116.1(9) . . ?
F2 C7 C8 124.5(9) . . ?
C8 C7 C6 119.3(14) . . ?
N1 C1 C2 111.3(9) . . ?
N1 C1 H1D 109.4 . . ?
N1 C1 H1E 109.4 . . ?
C2 C1 H1D 109.4 . . ?
C2 C1 H1E 109.4 . . ?
H1D C1 H1E 108.0 . . ?
C6 C5 H5 122.3 . . ?
C6 C5 C4 115.5(8) . . ?
C4 C5 H5 122.3 . . ?
N4 C4 C3 110.8(8) . . ?
N4 C4 C5 128.9(9) . . ?
C3 C4 C5 120.3(13) . . ?
C3 C8 C7 117.6(8) . . ?
C3 C8 H8 121.2 . . ?
C7 C8 H8 121.2 . . ?

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
F2 C7 C8 C3 -179.6(6) . . . . ?
F1 C6 C7 F2 1.3(8) . . . . ?
F1 C6 C7 C8 -175.9(5) . . . . ?
F1 C6 C5 C4 178.4(4) . . . . ?
N4 N2 N3 C3 0.6(6) . . . . ?
N4 N2 C2 C1 93.8(6) . . . . ?
N2 N4 C4 C3 -1.5(7) . . . . ?
N2 N4 C4 C5 178.5(6) . . . . ?
N2 C2 C1 N1 67.9(8) . . . . ?
C6 C7 C8 C3 -2.6(9) . . . . ?
C6 C5 C4 N4 177.7(7) . . . . ?
C6 C5 C4 C3 -2.3(9) . . . . ?
N3 N2 C2 C1 -83.5(8) . . . . ?
N3 C3 C4 N4 1.9(7) . . . . ?
N3 C3 C4 C5 -178.1(5) . . . . ?
N3 C3 C8 C7 -179.1(5) . . . . ?
C2 N2 N3 C3 178.0(5) . . . . ?
C7 C6 C5 C4 -0.3(10) . . . . ?
C5 C6 C7 F2 -179.9(6) . . . . ?
C5 C6 C7 C8 2.9(10) . . . . ?
C4 N4 N2 N3 0.5(7) . . . . ?
C4 N4 N2 C2 -176.8(5) . . . . ?
C4 C3 N3 N2 -1.4(6) . . . . ?
C4 C3 C8 C7 0.0(10) . . . . ?
C8 C3 N3 N2 177.8(7) . . . . ?
C8 C3 C4 N4 -177.4(6) . . . . ?
C8 C3 C4 C5 2.6(10) . . . . ?

_shelx_res_file                  
;
TITL mo_DAC24_F2BTa2PbI4_2p80GPa_0ma_e.res in Pnma
    2p82gpa_good.res
    created by SHELXL-2019/1 at 16:01:02 on 08-Feb-2024
REM Old TITL __TMP__ in Pnma
REM SHELXT solution in Pnma: R1 0.189, Rweak 0.003, Alpha 0.043
REM <I/s> 3.036 for 98 systematic absences, Orientation as input
REM Formula found by SHELXT: C8 F4 I4 N8 Pb
CELL 0.71073 12.5704 28.3372 6.3725 90 90 90
ZERR 4 0.0005 0.0021 0.0003 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H F I N Pb
UNIT 64 72 16 16 32 4

L.S. 10
PLAN  1
TEMP 0
CONF
BOND
LIST 6
MORE -1
BOND $H
fmap 2
ACTA
OMIT 0 3 1
OMIT 8 9 0
OMIT 12 11 1
OMIT 12 11 2
REM <olex2.extras>
REM <HklSrc "%.\\2p82Gpa_good.hkl">
REM </olex2.extras>

WGHT    0.011900    6.876600
FVAR       0.11623
PB1   6    0.348262    0.750000    0.695678    10.50000    0.02045    0.03750 =
         0.02170    0.00000   -0.00017    0.00000
I1    4    0.354901    0.750000    0.202381    10.50000    0.02746    0.03653 =
         0.01901    0.00000    0.00036    0.00000
I2    4    0.099170    0.750000    0.759904    10.50000    0.01705    0.04537 =
         0.03041    0.00000    0.00031    0.00000
I3    4    0.324019    0.641524    0.668331    11.00000    0.02751    0.03852 =
         0.02451    0.00020   -0.00010    0.00376
F2    3    0.443139    0.408939    0.365593    11.00000    0.03400
F1    3    0.262712    0.447283    0.441606    11.00000    0.02351    0.02822 =
         0.03747    0.00324    0.00609   -0.00790
N4    5    0.406656    0.595694    0.196781    11.00000    0.02157
N2    5    0.507870    0.601613    0.140405    11.00000    0.01862
C3    1    0.505082    0.528249    0.220407    11.00000    0.01859
C6    1    0.337232    0.476282    0.363169    11.00000    0.01789
N3    5    0.571188    0.562557    0.152319    11.00000    0.02060
N1    5    0.695543    0.647512    0.338790    11.00000    0.02921
AFIX 137
H1A   2    0.682722    0.616821    0.354308    11.00000   -1.50000
H1B   2    0.716287    0.659644    0.460941    11.00000   -1.50000
H1C   2    0.746616    0.651598    0.243787    11.00000   -1.50000
AFIX   0
C2    1    0.547843    0.646436    0.080433    11.00000    0.02321
AFIX  23
H2A   2    0.490435    0.665454    0.023925    11.00000   -1.20000
H2B   2    0.600979    0.642504   -0.028552    11.00000   -1.20000
AFIX   0
C7    1    0.437948    0.453937    0.324278    11.00000    0.02398
C1    1    0.597263    0.671621    0.267716    11.00000    0.02923
AFIX  23
H1D   2    0.613950    0.703898    0.229176    11.00000   -1.20000
H1E   2    0.546377    0.672488    0.382081    11.00000   -1.20000
AFIX   0
C5    1    0.316805    0.522714    0.329396    11.00000    0.02172
AFIX  43
H5    2    0.250491    0.536013    0.355658    11.00000   -1.20000
AFIX   0
C4    1    0.403901    0.549721    0.250924    11.00000    0.01592
C8    1    0.523103    0.481047    0.255983    11.00000    0.01820
AFIX  43
H8    2    0.589935    0.467783    0.235026    11.00000   -1.20000
AFIX   0
HKLF 4




REM  mo_DAC24_F2BTa2PbI4_2p80GPa_0ma_e.res in Pnma
REM wR2 = 0.0376, GooF = S = 1.158, Restrained GooF = 1.158 for all data
REM R1 = 0.0158 for 869 Fo > 4sig(Fo) and 0.0172 for all 896 data
REM 90 parameters refined using 0 restraints

END

WGHT      0.0119      6.8768

REM Highest difference peak  0.335,  deepest hole -0.316,  1-sigma level  0.090
Q1    1   0.2991  0.7077  0.4619  11.00000  0.05    0.34
;
_shelx_res_checksum              93881
_olex2_submission_special_instructions 'No special instructions were received'
_olex2_exptl_crystal_mounting_method 
'Crystal mounted in a Diamond anvil cell of 100 degre opening angle'

_vrf_PLAT029_2p82gpa_good        
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT201_2p82gpa_good        
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         12 Report
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the available data, preventing from a complete anisotropic refienement. 
;
_vrf_PLAT933_2p82gpa_good        
;
PROBLEM: Number of HKL-OMIT Records in Embedded .res File          
RESPONSE: Experiment done in a Diamond Anvil Cell some reflections are close 
to gasket ring/shadow or close to diamond peaks and should be deleted.  
;
_vrf_PLAT911_2p82gpa_good        
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT910_2p82gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT913_2p82gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT088_2p82gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space and then number of measured reflections inducing
a low Data / Parameter Ratio despite isotropic refinement done to limit this 
problem
;
####################################################################### 
# 
# 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_3p40gpa_good
_database_code_depnum_ccdc_archive 'CCDC 2365964'
loop_
_audit_author_name
_audit_author_address
'Maxime Deutsch' 'University of Lorraine'
_audit_update_record             
;
2024-06-26 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-02-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H9 F2 N4)'
_chemical_formula_sum            'C16 H18 F4 I4 N8 Pb'
_chemical_formula_weight         1113.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.5155(5)
_cell_length_b                   28.112(2)
_cell_length_c                   6.3307(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2227.34(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9585
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      25.788
_cell_measurement_theta_min      3.299
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.178
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0888 before and 0.0648 after correction.
The Ratio of minimum to maximum transmission is 0.8163.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.420
_diffrn_reflns_Laue_measured_fraction_max 0.382
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            24905
_diffrn_reflns_point_group_measured_fraction_full 0.420
_diffrn_reflns_point_group_measured_fraction_max 0.382
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.311
_diffrn_reflns_theta_min         3.255
_diffrn_ambient_temperature      300(3)
_diffrn_ambient_pressure         3.40e+06
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.420
_diffrn_measured_fraction_theta_max 0.382
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON III CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                860
_reflns_number_total             884
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         884
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0170
_refine_ls_restrained_S_all      1.204
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0024P)²+11.4787P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0394
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.34995(3) 0.750000 0.69501(5) 0.0255(5) Uani 1 2 d S T P . .
I1 I 0.35608(4) 0.750000 0.20153(8) 0.0269(8) Uani 1 2 d S T P . .
I2 I 0.10091(4) 0.750000 0.76133(9) 0.0308(8) Uani 1 2 d S T P . .
I3 I 0.32430(3) 0.64112(4) 0.66669(6) 0.0289(5) Uani 1 1 d . . . . .
F2 F 0.4432(3) 0.4077(4) 0.3674(6) 0.0321(11) Uiso 1 1 d . . . . .
F1 F 0.2622(3) 0.4469(3) 0.4440(5) 0.0286(9) Uiso 1 1 d . . . . .
N4 N 0.4068(4) 0.5958(6) 0.1937(8) 0.0229(13) Uiso 1 1 d . . . . .
N2 N 0.5085(4) 0.6025(4) 0.1375(7) 0.0160(11) Uiso 1 1 d . . . . .
C3 C 0.5060(5) 0.5291(6) 0.2201(9) 0.0199(15) Uiso 1 1 d . . . . .
C6 C 0.3376(4) 0.4758(6) 0.3647(9) 0.0158(14) Uiso 1 1 d . . . . .
N3 N 0.5719(4) 0.5627(4) 0.1503(7) 0.0198(12) Uiso 1 1 d . . . . .
N1 N 0.6957(4) 0.6478(5) 0.3379(8) 0.0255(13) Uiso 1 1 d . . . . .
H1A H 0.744209 0.648570 0.235141 0.038 Uiso 1 1 calc R U . . .
H1B H 0.680906 0.617768 0.370547 0.038 Uiso 1 1 calc R U . . .
H1C H 0.721241 0.662714 0.451236 0.038 Uiso 1 1 calc R U . . .
C2 C 0.5489(5) 0.6478(6) 0.0776(9) 0.0208(14) Uiso 1 1 d . . . . .
H2A H 0.491464 0.667190 0.021264 0.025 Uiso 1 1 calc R U . . .
H2B H 0.602552 0.644015 -0.031682 0.025 Uiso 1 1 calc R U . . .
C7 C 0.4383(5) 0.4532(7) 0.3256(10) 0.0219(16) Uiso 1 1 d . . . . .
C1 C 0.5972(5) 0.6719(6) 0.2659(9) 0.0261(16) Uiso 1 1 d . . . . .
H1D H 0.613718 0.704649 0.230120 0.031 Uiso 1 1 calc R U . . .
H1E H 0.545652 0.672218 0.380256 0.031 Uiso 1 1 calc R U . . .
C5 C 0.3163(5) 0.5226(6) 0.3301(9) 0.0207(15) Uiso 1 1 d . . . . .
H5 H 0.249089 0.535384 0.355982 0.025 Uiso 1 1 calc R U . . .
C4 C 0.4041(4) 0.5518(6) 0.2505(9) 0.0143(13) Uiso 1 1 d . . . . .
C8 C 0.5229(4) 0.4808(6) 0.2562(9) 0.0158(14) Uiso 1 1 d . . . . .
H8 H 0.589855 0.467294 0.234055 0.019 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.01975(18) 0.0364(16) 0.02051(19) 0.000 -0.00026(12) 0.000
I1 0.0260(3) 0.037(3) 0.0177(3) 0.000 0.0003(2) 0.000
I2 0.0165(3) 0.048(2) 0.0278(3) 0.000 0.0002(2) 0.000
I3 0.0257(2) 0.0375(17) 0.0235(2) 0.0002(3) -0.00002(15) 0.0039(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.2075(6) 1_556 ?
Pb1 I1 3.1250(6) . ?
Pb1 I2 3.1530(6) 6_657 ?
Pb1 I2 3.1450(6) . ?
Pb1 I3 3.0828(12) 7_575 ?
Pb1 I3 3.0828(12) . ?
F2 C7 1.308(19) . ?
F1 C6 1.342(12) . ?
N4 N2 1.335(7) . ?
N4 C4 1.29(2) . ?
N2 N3 1.372(15) . ?
N2 C2 1.422(19) . ?
C3 N3 1.330(16) . ?
C3 C4 1.440(14) . ?
C3 C8 1.39(2) . ?
C6 C7 1.433(14) . ?
C6 C5 1.36(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.478(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.499(12) . ?
C7 C8 1.385(16) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C5 H5 0.9300 . ?
C5 C4 1.461(16) . ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 177.22(2) . 1_556 ?
I1 Pb1 I2 93.623(17) . 6_657 ?
I1 Pb1 I2 99.079(17) . . ?
I2 Pb1 I1 83.698(16) . 1_556 ?
I2 Pb1 I1 83.601(16) 6_657 1_556 ?
I2 Pb1 I2 167.298(11) . 6_657 ?
I3 Pb1 I1 86.814(9) . . ?
I3 Pb1 I1 93.476(9) . 1_556 ?
I3 Pb1 I1 86.813(9) 7_575 . ?
I3 Pb1 I1 93.476(9) 7_575 1_556 ?
I3 Pb1 I2 84.525(9) 7_575 . ?
I3 Pb1 I2 96.246(9) 7_575 6_657 ?
I3 Pb1 I2 84.525(9) . . ?
I3 Pb1 I2 96.247(9) . 6_657 ?
I3 Pb1 I3 166.302(19) 7_575 . ?
Pb1 I1 Pb1 177.22(2) . 1_554 ?
Pb1 I2 Pb1 177.36(2) . 6_557 ?
C4 N4 N2 103.6(10) . . ?
N4 N2 N3 114.8(11) . . ?
N4 N2 C2 122.5(11) . . ?
N3 N2 C2 122.6(6) . . ?
N3 C3 C4 106.1(14) . . ?
N3 C3 C8 130.8(8) . . ?
C8 C3 C4 123.0(11) . . ?
F1 C6 C7 114.4(13) . . ?
F1 C6 C5 120.6(7) . . ?
C5 C6 C7 125.0(11) . . ?
C3 N3 N2 103.9(7) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N2 C2 H2A 109.7 . . ?
N2 C2 H2B 109.7 . . ?
N2 C2 C1 109.7(7) . . ?
H2A C2 H2B 108.2 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
F2 C7 C6 116.1(10) . . ?
F2 C7 C8 125.2(10) . . ?
C8 C7 C6 118.6(16) . . ?
N1 C1 C2 112.0(10) . . ?
N1 C1 H1D 109.2 . . ?
N1 C1 H1E 109.2 . . ?
C2 C1 H1D 109.2 . . ?
C2 C1 H1E 109.2 . . ?
H1D C1 H1E 107.9 . . ?
C6 C5 H5 121.5 . . ?
C6 C5 C4 116.9(9) . . ?
C4 C5 H5 121.5 . . ?
N4 C4 C3 111.4(9) . . ?
N4 C4 C5 131.0(10) . . ?
C3 C4 C5 117.6(15) . . ?
C3 C8 H8 120.6 . . ?
C7 C8 C3 118.8(9) . . ?
C7 C8 H8 120.6 . . ?

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
F2 C7 C8 C3 -179.3(8) . . . . ?
F1 C6 C7 F2 1.4(9) . . . . ?
F1 C6 C7 C8 -176.0(6) . . . . ?
F1 C6 C5 C4 177.9(5) . . . . ?
N4 N2 N3 C3 -0.4(7) . . . . ?
N4 N2 C2 C1 94.0(7) . . . . ?
N2 N4 C4 C3 -2.8(9) . . . . ?
N2 N4 C4 C5 179.5(7) . . . . ?
N2 C2 C1 N1 68.4(9) . . . . ?
C6 C7 C8 C3 -2.2(10) . . . . ?
C6 C5 C4 N4 176.0(9) . . . . ?
C6 C5 C4 C3 -1.5(10) . . . . ?
N3 N2 C2 C1 -83.2(9) . . . . ?
N3 C3 C4 N4 2.8(9) . . . . ?
N3 C3 C4 C5 -179.3(6) . . . . ?
N3 C3 C8 C7 -178.5(6) . . . . ?
C2 N2 N3 C3 177.0(6) . . . . ?
C7 C6 C5 C4 -1.1(12) . . . . ?
C5 C6 C7 F2 -179.5(7) . . . . ?
C5 C6 C7 C8 3.0(11) . . . . ?
C4 N4 N2 N3 2.1(9) . . . . ?
C4 N4 N2 C2 -175.4(7) . . . . ?
C4 C3 N3 N2 -1.3(7) . . . . ?
C4 C3 C8 C7 -0.4(11) . . . . ?
C8 C3 N3 N2 177.0(8) . . . . ?
C8 C3 C4 N4 -175.7(8) . . . . ?
C8 C3 C4 C5 2.2(11) . . . . ?

_shelx_res_file                  
;
TITL mo_DAC24_F2BTa2PbI4_3p40GPa_0ma_d.res in Pnma
    3p40gpa_good.res
    created by SHELXL-2019/1 at 16:03:56 on 08-Feb-2024
REM Old TITL __TMP__ in Pnma
REM SHELXT solution in Pnma: R1 0.186, Rweak 0.003, Alpha 0.042
REM <I/s> 3.151 for 97 systematic absences, Orientation as input
REM Formula found by SHELXT: C7 F4 I4 N8 Pb
CELL 0.71073 12.5155 28.1117 6.3307 90 90 90
ZERR 4 0.0005 0.002 0.0002 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H F I N Pb
UNIT 64 72 16 16 32 4

L.S. 50
PLAN  1
TEMP 0
CONF
BOND
LIST 6
MORE -1
BOND $H
fmap 2
acta
OMIT 0 6 2
OMIT 3 9 3
OMIT 5 11 5
OMIT 6 11 5
OMIT 7 11 5
OMIT 8 9 0
OMIT 8 11 4
OMIT 9 11 4
OMIT 11 11 3
REM <olex2.extras>
REM <HklSrc "%.\\3p40GPa_good.hkl">
REM </olex2.extras>

WGHT    0.002400   11.478700
FVAR       0.12129
PB1   6    0.349948    0.750000    0.695006    10.50000    0.01975    0.03639 =
         0.02051    0.00000   -0.00026    0.00000
I1    4    0.356078    0.750000    0.201525    10.50000    0.02596    0.03702 =
         0.01772    0.00000    0.00034    0.00000
I2    4    0.100909    0.750000    0.761333    10.50000    0.01649    0.04818 =
         0.02776    0.00000    0.00020    0.00000
I3    4    0.324303    0.641120    0.666687    11.00000    0.02574    0.03747 =
         0.02345    0.00016   -0.00002    0.00386
F2    3    0.443157    0.407666    0.367368    11.00000    0.03206
F1    3    0.262243    0.446867    0.443964    11.00000    0.02859
N4    5    0.406789    0.595761    0.193734    11.00000    0.02288
N2    5    0.508487    0.602476    0.137463    11.00000    0.01605
C3    1    0.506041    0.529084    0.220129    11.00000    0.01992
C6    1    0.337563    0.475785    0.364690    11.00000    0.01581
N3    5    0.571869    0.562745    0.150322    11.00000    0.01979
N1    5    0.695685    0.647848    0.337861    11.00000    0.02546
AFIX 137
H1A   2    0.744209    0.648570    0.235141    11.00000   -1.50000
H1B   2    0.680906    0.617768    0.370547    11.00000   -1.50000
H1C   2    0.721241    0.662714    0.451236    11.00000   -1.50000
AFIX   0
C2    1    0.548903    0.647808    0.077606    11.00000    0.02080
AFIX  23
H2A   2    0.491464    0.667190    0.021264    11.00000   -1.20000
H2B   2    0.602552    0.644015   -0.031682    11.00000   -1.20000
AFIX   0
C7    1    0.438264    0.453179    0.325609    11.00000    0.02192
C1    1    0.597235    0.671911    0.265908    11.00000    0.02610
AFIX  23
H1D   2    0.613718    0.704649    0.230120    11.00000   -1.20000
H1E   2    0.545652    0.672218    0.380256    11.00000   -1.20000
AFIX   0
C5    1    0.316341    0.522573    0.330139    11.00000    0.02068
AFIX  43
H5    2    0.249089    0.535384    0.355982    11.00000   -1.20000
AFIX   0
C4    1    0.404069    0.551796    0.250538    11.00000    0.01427
C8    1    0.522922    0.480770    0.256201    11.00000    0.01583
AFIX  43
H8    2    0.589855    0.467294    0.234055    11.00000   -1.20000
AFIX   0
HKLF 4




REM  mo_DAC24_F2BTa2PbI4_3p40GPa_0ma_d.res in Pnma
REM wR2 = 0.0394, GooF = S = 1.204, Restrained GooF = 1.204 for all data
REM R1 = 0.0170 for 860 Fo > 4sig(Fo) and 0.0188 for all 884 data
REM 85 parameters refined using 0 restraints

END

WGHT      0.0024     11.4788

REM Highest difference peak  0.429,  deepest hole -0.468,  1-sigma level  0.116
Q1    1   0.3030  0.7047  0.4623  11.00000  0.05    0.43
;
_shelx_res_checksum              30310
_olex2_submission_special_instructions 'No special instructions were received'
_olex2_exptl_crystal_mounting_method 
'Crystal mounted in a Diamond anvil cell of 100 degre opening angle'

_vrf_PLAT029_3p40gpa_good        
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT201_3p40gpa_good        
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         12 Report
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the available data, preventing from a complete anisotropic refienement. 
;
_vrf_PLAT933_3p40gpa_good        
;
PROBLEM: Number of HKL-OMIT Records in Embedded .res File          
RESPONSE: Experiment done in a Diamond Anvil Cell some reflections are close 
to gasket ring/shadow or close to diamond peaks and should be deleted.  
;
_vrf_PLAT911_3p40gpa_good        
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT910_3p40gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT913_3p40gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT934_3p40gpa_good        
;
PROBLEM: 
RESPONSE: Very low intensity reflection 
;
####################################################################### 
# 
# 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_2p2gpa_good
_database_code_depnum_ccdc_archive 'CCDC 2365962'
loop_
_audit_author_name
_audit_author_address
'Maxime Deutsch' 'University of Lorraine'
_audit_update_record             
;
2024-06-26 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-06-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H9 F2 N4)'
_chemical_formula_sum            'C16 H18 F4 I4 N8 Pb'
_chemical_formula_weight         1113.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.6346(5)
_cell_length_b                   28.617(2)
_cell_length_c                   6.4221(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2322.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      26.040
_cell_measurement_theta_min      3.251
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.640
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0863 before and 0.0645 after correction.
The Ratio of minimum to maximum transmission is 0.8049.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.184
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.414
_diffrn_reflns_Laue_measured_fraction_max 0.387
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            26144
_diffrn_reflns_point_group_measured_fraction_full 0.414
_diffrn_reflns_point_group_measured_fraction_max 0.387
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.158
_diffrn_reflns_theta_min         3.225
_diffrn_ambient_temperature      300(3)
_diffrn_ambient_pressure         2.22e+06
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.414
_diffrn_measured_fraction_theta_max 0.387
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON III CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                888
_reflns_number_total             914
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         914
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0159
_refine_ls_R_factor_gt           0.0151
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0096P)²+4.4327P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0316
_refine_ls_wR_factor_ref         0.0319
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.34599(2) 0.750000 0.69662(3) 0.0277(4) Uani 1 2 d S T P . .
I1 I 0.35309(3) 0.750000 0.20344(5) 0.0298(6) Uani 1 2 d S T P . .
I2 I 0.09689(3) 0.750000 0.75794(6) 0.0335(6) Uani 1 2 d S T P . .
I3 I 0.32350(2) 0.64203(3) 0.67046(4) 0.0319(4) Uani 1 1 d . . . . .
F2 F 0.4435(2) 0.4094(3) 0.3623(5) 0.026(4) Uani 1 1 d . . . . .
F1 F 0.26278(17) 0.4477(2) 0.4391(4) 0.030(3) Uani 1 1 d . . . . .
N4 N 0.4064(3) 0.5946(4) 0.1997(5) 0.0231(9) Uiso 1 1 d . . . . .
N2 N 0.5071(3) 0.6010(3) 0.1432(5) 0.0207(8) Uiso 1 1 d . . . . .
C3 C 0.5044(3) 0.5285(4) 0.2216(6) 0.0187(10) Uiso 1 1 d . . . . .
C6 C 0.3376(3) 0.4762(4) 0.3617(7) 0.0199(11) Uiso 1 1 d . . . . .
N3 N 0.5701(3) 0.5623(3) 0.1545(5) 0.0212(9) Uiso 1 1 d . . . . .
N1 N 0.6955(3) 0.6466(3) 0.3379(6) 0.0311(10) Uiso 1 1 d . . . . .
H1A H 0.684262 0.615951 0.342949 0.047 Uiso 1 1 calc R U . . .
H1B H 0.713652 0.656896 0.463709 0.047 Uiso 1 1 calc R U . . .
H1C H 0.747363 0.652700 0.248147 0.047 Uiso 1 1 calc R U . . .
C2 C 0.5469(3) 0.6453(4) 0.0851(6) 0.0253(11) Uiso 1 1 d . . . . .
H2A H 0.489659 0.664137 0.029623 0.030 Uiso 1 1 calc R U . . .
H2B H 0.599352 0.641411 -0.023809 0.030 Uiso 1 1 calc R U . . .
C7 C 0.4378(4) 0.4562(6) 0.3250(8) 0.0232(15) Uiso 1 1 d . . . . .
C1 C 0.5970(3) 0.6706(4) 0.2690(7) 0.0315(12) Uiso 1 1 d . . . . .
H1D H 0.613469 0.702526 0.229223 0.038 Uiso 1 1 calc R U . . .
H1E H 0.547035 0.671717 0.383583 0.038 Uiso 1 1 calc R U . . .
C5 C 0.3175(4) 0.5227(4) 0.3305(6) 0.0217(11) Uiso 1 1 d . . . . .
H5 H 0.251705 0.535846 0.358356 0.026 Uiso 1 1 calc R U . . .
C4 C 0.4033(3) 0.5495(5) 0.2528(7) 0.0187(10) Uiso 1 1 d . . . . .
C8 C 0.5225(3) 0.4815(4) 0.2561(7) 0.0201(11) Uiso 1 1 d . . . . .
H8 H 0.588392 0.467963 0.233797 0.024 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.02138(14) 0.0386(13) 0.02308(15) 0.000 -0.00015(8) 0.000
I1 0.0298(2) 0.040(2) 0.0198(2) 0.000 0.00026(14) 0.000
I2 0.0180(2) 0.0493(19) 0.0332(2) 0.000 0.00062(16) 0.000
I3 0.02912(17) 0.0406(13) 0.02595(16) -0.0002(3) -0.00017(11) 0.0033(3)
F2 0.0341(15) 0.002(14) 0.0421(16) -0.001(3) 0.0037(11) -0.002(3)
F1 0.0246(13) 0.028(11) 0.0381(14) 0.004(2) 0.0065(10) -0.007(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
Pb1 I1 3.2561(4) 1_556 ?
Pb1 I1 3.1685(4) . ?
Pb1 I2 3.1835(4) 6_657 ?
Pb1 I2 3.1718(4) . ?
Pb1 I3 3.1075(9) . ?
Pb1 I3 3.1075(9) 7_575 ?
F2 C7 1.360(15) . ?
F1 C6 1.344(9) . ?
N4 N2 1.336(5) . ?
N4 C4 1.335(15) . ?
N2 N3 1.365(11) . ?
N2 C2 1.414(14) . ?
C3 N3 1.346(11) . ?
C3 C4 1.426(10) . ?
C3 C8 1.382(14) . ?
C6 C7 1.410(11) . ?
C6 C5 1.370(15) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.489(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.523(9) . ?
C7 C8 1.366(12) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C5 H5 0.9300 . ?
C5 C4 1.419(11) . ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 176.803(16) . 1_556 ?
I1 Pb1 I2 93.639(12) . 6_657 ?
I1 Pb1 I2 98.752(12) . . ?
I2 Pb1 I1 84.445(11) . 1_556 ?
I2 Pb1 I1 83.164(11) 6_657 1_556 ?
I2 Pb1 I2 167.609(8) . 6_657 ?
I3 Pb1 I1 87.050(7) 7_575 . ?
I3 Pb1 I1 93.243(7) 7_575 1_556 ?
I3 Pb1 I1 87.050(7) . . ?
I3 Pb1 I1 93.243(7) . 1_556 ?
I3 Pb1 I2 85.180(7) . . ?
I3 Pb1 I2 95.510(7) . 6_657 ?
I3 Pb1 I2 85.180(7) 7_575 . ?
I3 Pb1 I2 95.509(7) 7_575 6_657 ?
I3 Pb1 I3 167.803(14) . 7_575 ?
Pb1 I1 Pb1 176.803(16) . 1_554 ?
Pb1 I2 Pb1 178.128(15) . 6_557 ?
C4 N4 N2 103.3(7) . . ?
N4 N2 N3 115.4(8) . . ?
N4 N2 C2 122.3(8) . . ?
N3 N2 C2 122.3(4) . . ?
N3 C3 C4 107.2(10) . . ?
N3 C3 C8 130.4(5) . . ?
C8 C3 C4 122.4(8) . . ?
F1 C6 C7 116.6(11) . . ?
F1 C6 C5 120.9(5) . . ?
C5 C6 C7 122.5(9) . . ?
C3 N3 N2 103.9(5) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N2 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
N2 C2 C1 111.7(5) . . ?
H2A C2 H2B 107.9 . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
F2 C7 C6 114.7(8) . . ?
F2 C7 C8 122.6(8) . . ?
C8 C7 C6 122.8(13) . . ?
N1 C1 C2 111.0(7) . . ?
N1 C1 H1D 109.4 . . ?
N1 C1 H1E 109.4 . . ?
C2 C1 H1D 109.4 . . ?
C2 C1 H1E 109.4 . . ?
H1D C1 H1E 108.0 . . ?
C6 C5 H5 122.1 . . ?
C6 C5 C4 115.8(7) . . ?
C4 C5 H5 122.1 . . ?
N4 C4 C3 110.1(7) . . ?
N4 C4 C5 129.4(7) . . ?
C5 C4 C3 120.4(11) . . ?
C3 C8 H8 122.0 . . ?
C7 C8 C3 116.1(8) . . ?
C7 C8 H8 122.0 . . ?

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
F2 C7 C8 C3 178.9(6) . . . . ?
F1 C6 C7 F2 3.6(8) . . . . ?
F1 C6 C7 C8 -176.8(5) . . . . ?
F1 C6 C5 C4 178.5(4) . . . . ?
N4 N2 N3 C3 0.6(5) . . . . ?
N4 N2 C2 C1 93.9(5) . . . . ?
N2 N4 C4 C3 -1.5(6) . . . . ?
N2 N4 C4 C5 178.4(5) . . . . ?
N2 C2 C1 N1 67.8(7) . . . . ?
C6 C7 C8 C3 -0.7(9) . . . . ?
C6 C5 C4 N4 177.0(6) . . . . ?
C6 C5 C4 C3 -3.1(8) . . . . ?
N3 N2 C2 C1 -83.1(7) . . . . ?
N3 C3 C4 N4 2.0(6) . . . . ?
N3 C3 C4 C5 -178.0(4) . . . . ?
N3 C3 C8 C7 -179.9(5) . . . . ?
C2 N2 N3 C3 177.7(5) . . . . ?
C7 C6 C5 C4 1.7(8) . . . . ?
C5 C6 C7 F2 -179.4(5) . . . . ?
C5 C6 C7 C8 0.2(10) . . . . ?
C4 N4 N2 N3 0.6(6) . . . . ?
C4 N4 N2 C2 -176.5(5) . . . . ?
C4 C3 N3 N2 -1.5(5) . . . . ?
C4 C3 C8 C7 -0.8(9) . . . . ?
C8 C3 N3 N2 177.7(6) . . . . ?
C8 C3 C4 N4 -177.3(5) . . . . ?
C8 C3 C4 C5 2.8(8) . . . . ?

_shelx_res_file                  
;
TITL mo_DAC24_F2BTa2PbI4_2p20GPa_0ma_d.res in Pnma
    2p2gpa_good.res
    created by SHELXL-2019/1 at 16:18:53 on 26-Jun-2024
REM Old TITL __TMP__ in Pnma
REM SHELXT solution in Pnma: R1 0.207, Rweak 0.004, Alpha 0.038
REM <I/s> 2.787 for 99 systematic absences, Orientation as input
REM Formula found by SHELXT: C10 F4 I4 N6 Pb
CELL 0.71073 12.6346 28.6171 6.4221 90 90 90
ZERR 4 0.0005 0.0021 0.0003 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H F I N Pb
UNIT 64 72 16 16 32 4

L.S. 30
PLAN  2
TEMP 0
CONF
BOND
LIST 6
MORE -1
BOND $H
fmap 2
acta
OMIT 0 3 1
OMIT 2 11 6
OMIT 3 11 6
OMIT 8 9 0
OMIT 12 11 0
OMIT 12 11 3
REM <olex2.extras>
REM <HklSrc "%.\\2p2Gpa_good.hkl">
REM </olex2.extras>

WGHT    0.009600    4.432700
FVAR       0.11486
PB1   6    0.345994    0.750000    0.696623    10.50000    0.02138    0.03857 =
         0.02308    0.00000   -0.00015    0.00000
I1    4    0.353086    0.750000    0.203444    10.50000    0.02982    0.03977 =
         0.01978    0.00000    0.00026    0.00000
I2    4    0.096894    0.750000    0.757938    10.50000    0.01799    0.04935 =
         0.03324    0.00000    0.00062    0.00000
I3    4    0.323503    0.642027    0.670455    11.00000    0.02912    0.04057 =
         0.02595   -0.00020   -0.00017    0.00332
F2    3    0.443513    0.409438    0.362288    11.00000    0.03409    0.00208 =
         0.04214   -0.00091    0.00368   -0.00247
F1    3    0.262776    0.447676    0.439088    11.00000    0.02455    0.02839 =
         0.03810    0.00420    0.00652   -0.00715
N4    5    0.406425    0.594569    0.199742    11.00000    0.02305
N2    5    0.507130    0.600995    0.143237    11.00000    0.02068
C3    1    0.504360    0.528509    0.221580    11.00000    0.01874
C6    1    0.337608    0.476179    0.361726    11.00000    0.01985
N3    5    0.570134    0.562315    0.154542    11.00000    0.02118
N1    5    0.695467    0.646634    0.337873    11.00000    0.03111
AFIX 137
H1A   2    0.684262    0.615951    0.342949    11.00000   -1.50000
H1B   2    0.713652    0.656896    0.463709    11.00000   -1.50000
H1C   2    0.747363    0.652700    0.248147    11.00000   -1.50000
AFIX   0
C2    1    0.546915    0.645304    0.085140    11.00000    0.02534
AFIX  23
H2A   2    0.489659    0.664137    0.029623    11.00000   -1.20000
H2B   2    0.599352    0.641411   -0.023809    11.00000   -1.20000
AFIX   0
C7    1    0.437847    0.456163    0.324991    11.00000    0.02320
C1    1    0.596986    0.670645    0.268983    11.00000    0.03148
AFIX  23
H1D   2    0.613469    0.702526    0.229223    11.00000   -1.20000
H1E   2    0.547035    0.671717    0.383583    11.00000   -1.20000
AFIX   0
C5    1    0.317487    0.522678    0.330455    11.00000    0.02173
AFIX  43
H5    2    0.251705    0.535846    0.358356    11.00000   -1.20000
AFIX   0
C4    1    0.403274    0.549495    0.252838    11.00000    0.01866
C8    1    0.522465    0.481520    0.256127    11.00000    0.02011
AFIX  43
H8    2    0.588392    0.467963    0.233797    11.00000   -1.20000
AFIX   0
HKLF 4




REM  mo_DAC24_F2BTa2PbI4_2p20GPa_0ma_d.res in Pnma
REM wR2 = 0.0319, GooF = S = 1.154, Restrained GooF = 1.154 for all data
REM R1 = 0.0151 for 888 Fo > 4sig(Fo) and 0.0159 for all 914 data
REM 95 parameters refined using 0 restraints

END

WGHT      0.0096      4.4361

REM Highest difference peak  0.366,  deepest hole -0.310,  1-sigma level  0.084
Q1    1   0.3991  0.7500 -0.0289  10.50000  0.05    0.37
Q2    1   0.0355  0.7500  1.0325  10.50000  0.05    0.32
;
_shelx_res_checksum              20513
_olex2_submission_special_instructions 'No special instructions were received'
_olex2_exptl_crystal_mounting_method 
'Crystal mounted in a Diamond anvil cell of 100 degre opening angle'

_vrf_PLAT029_2p2gpa_good         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT201_2p2gpa_good         
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         12 Report
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the available data, preventing from a complete anisotropic refienement. 
;
_vrf_PLAT933_2p2gpa_good         
;
PROBLEM: Number of HKL-OMIT Records in Embedded .res File          
RESPONSE: Experiment done in a Diamond Anvil Cell some reflections are close 
to gasket ring/shadow or close to diamond peaks and should be deleted.  
;
_vrf_PLAT911_2p2gpa_good         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT910_2p2gpa_good         
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT913_2p2gpa_good         
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT088_2p2gpa_good         
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space and then number of measured reflections inducing
a low Data / Parameter Ratio despite isotropic refinement done to limit this 
problem
;
_vrf_PLAT213_2p2gpa_good         
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space may introduce some atrefact on ADPs
;
####################################################################### 
# 
# 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_1p10gpa_good
_database_code_depnum_ccdc_archive 'CCDC 2365959'
loop_
_audit_author_name
_audit_author_address
'Maxime Deutsch' 'University of Lorraine'
_audit_update_record             
;
2024-06-26 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-02-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H9 F2 N4)'
_chemical_formula_sum            'C16 H18 F4 I4 N8 Pb'
_chemical_formula_weight         1113.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.7582(5)
_cell_length_b                   29.234(2)
_cell_length_c                   6.5183(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2431.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5696
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      25.59
_cell_measurement_theta_min      3.20
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.073
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0847 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.8023.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.041
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.409
_diffrn_reflns_Laue_measured_fraction_max 0.375
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            32734
_diffrn_reflns_point_group_measured_fraction_full 0.409
_diffrn_reflns_point_group_measured_fraction_max 0.375
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.351
_diffrn_reflns_theta_min         3.193
_diffrn_ambient_temperature      300(3)
_diffrn_ambient_pressure         1.10e+06
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.409
_diffrn_measured_fraction_theta_max 0.375
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON III CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                908
_reflns_number_total             944
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         944
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0166
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0066P)²+7.3037P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0339
_refine_ls_wR_factor_ref         0.0350
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.34073(2) 0.750000 0.69877(4) 0.0310(5) Uani 1 2 d S T P . .
I1 I 0.34806(4) 0.750000 0.20634(6) 0.0342(7) Uani 1 2 d S T P . .
I2 I 0.09180(3) 0.750000 0.75313(8) 0.0411(7) Uani 1 2 d S T P . .
I3 I 0.32177(3) 0.64328(4) 0.67499(5) 0.0365(5) Uani 1 1 d . . . . .
F2 F 0.4448(2) 0.4124(3) 0.3579(6) 0.034(5) Uani 1 1 d . . . . .
F1 F 0.2644(2) 0.4489(3) 0.4327(4) 0.039(4) Uani 1 1 d . . . . .
N4 N 0.4055(3) 0.5938(4) 0.2046(6) 0.0255(11) Uiso 1 1 d . . . . .
N2 N 0.5055(3) 0.5999(4) 0.1494(6) 0.0249(10) Uiso 1 1 d . . . . .
C3 C 0.5029(4) 0.5300(5) 0.2239(7) 0.0214(12) Uiso 1 1 d . . . . .
C6 C 0.3381(4) 0.4769(5) 0.3578(8) 0.0261(14) Uiso 1 1 d . . . . .
N3 N 0.5682(3) 0.5629(3) 0.1586(6) 0.0252(10) Uiso 1 1 d . . . . .
N1 N 0.6951(3) 0.6450(4) 0.3337(7) 0.0371(12) Uiso 1 1 d . . . . .
H1A H 0.743329 0.649711 0.237345 0.056 Uiso 1 1 calc R U . . .
H1B H 0.684055 0.615072 0.347440 0.056 Uiso 1 1 calc R U . . .
H1C H 0.717454 0.656445 0.452373 0.056 Uiso 1 1 calc R U . . .
C2 C 0.5445(4) 0.6441(5) 0.0937(8) 0.0312(13) Uiso 1 1 d . . . . .
H2A H 0.487108 0.662662 0.042988 0.037 Uiso 1 1 calc R U . . .
H2B H 0.595257 0.640769 -0.016074 0.037 Uiso 1 1 calc R U . . .
C7 C 0.4385(5) 0.4570(7) 0.3212(10) 0.0274(18) Uiso 1 1 d . . . . .
C1 C 0.5954(4) 0.6679(5) 0.2733(8) 0.0365(15) Uiso 1 1 d . . . . .
H1D H 0.609791 0.699477 0.236983 0.044 Uiso 1 1 calc R U . . .
H1E H 0.547596 0.667902 0.388952 0.044 Uiso 1 1 calc R U . . .
C5 C 0.3184(4) 0.5222(5) 0.3295(7) 0.0247(13) Uiso 1 1 d . . . . .
H5 H 0.252920 0.534732 0.357942 0.030 Uiso 1 1 calc R U . . .
C4 C 0.4027(3) 0.5499(5) 0.2539(8) 0.0230(12) Uiso 1 1 d . . . . .
C8 C 0.5209(4) 0.4832(5) 0.2539(7) 0.0218(12) Uiso 1 1 d . . . . .
H8 H 0.586376 0.470297 0.228996 0.026 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.02405(16) 0.0420(15) 0.02705(17) 0.000 -0.00027(10) 0.000
I1 0.0358(3) 0.043(2) 0.0235(3) 0.000 0.00076(17) 0.000
I2 0.0204(2) 0.061(2) 0.0419(3) 0.000 0.00071(19) 0.000
I3 0.03443(19) 0.0447(16) 0.03030(19) -0.0001(3) -0.00007(13) 0.0030(3)
F2 0.0415(19) 0.014(18) 0.048(2) -0.002(4) 0.0041(14) -0.005(3)
F1 0.0289(15) 0.043(13) 0.0449(17) 0.002(3) 0.0077(12) -0.005(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
Pb1 I1 3.3098(5) 1_556 ?
Pb1 I1 3.2112(5) . ?
Pb1 I2 3.2186(5) 6_657 ?
Pb1 I2 3.1955(5) . ?
Pb1 I3 3.1330(11) 7_575 ?
Pb1 I3 3.1330(11) . ?
F2 C7 1.329(19) . ?
F1 C6 1.338(11) . ?
N4 N2 1.339(6) . ?
N4 C4 1.322(17) . ?
N2 N3 1.347(13) . ?
N2 C2 1.429(16) . ?
C3 N3 1.340(13) . ?
C3 C4 1.419(11) . ?
C3 C8 1.403(17) . ?
C6 C7 1.427(13) . ?
C6 C5 1.363(18) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.491(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.510(11) . ?
C7 C8 1.373(15) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C5 H5 0.9300 . ?
C5 C4 1.433(14) . ?
C8 H8 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 176.709(19) . 1_556 ?
I1 Pb1 I2 93.919(14) . 6_657 ?
I2 Pb1 I1 98.037(14) . . ?
I2 Pb1 I1 85.255(13) . 1_556 ?
I2 Pb1 I1 82.790(13) 6_657 1_556 ?
I2 Pb1 I2 168.044(9) . 6_657 ?
I3 Pb1 I1 92.960(8) . 1_556 ?
I3 Pb1 I1 87.294(8) . . ?
I3 Pb1 I1 92.960(8) 7_575 1_556 ?
I3 Pb1 I1 87.294(8) 7_575 . ?
I3 Pb1 I2 94.684(8) 7_575 6_657 ?
I3 Pb1 I2 85.914(8) . . ?
I3 Pb1 I2 85.914(8) 7_575 . ?
I3 Pb1 I2 94.684(8) . 6_657 ?
I3 Pb1 I3 169.477(16) 7_575 . ?
Pb1 I1 Pb1 176.708(19) . 1_554 ?
Pb1 I2 Pb1 179.224(18) . 6_557 ?
C4 N4 N2 102.8(8) . . ?
N4 N2 N3 116.4(10) . . ?
N4 N2 C2 121.5(10) . . ?
N3 N2 C2 122.1(5) . . ?
N3 C3 C4 108.1(12) . . ?
N3 C3 C8 130.0(6) . . ?
C8 C3 C4 121.9(9) . . ?
F1 C6 C7 116.2(13) . . ?
F1 C6 C5 121.0(6) . . ?
C5 C6 C7 122.7(11) . . ?
C3 N3 N2 102.8(5) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N2 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
N2 C2 C1 111.7(6) . . ?
H2A C2 H2B 107.9 . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
F2 C7 C6 115.1(10) . . ?
F2 C7 C8 124.0(10) . . ?
C8 C7 C6 121.0(16) . . ?
N1 C1 C2 111.4(8) . . ?
N1 C1 H1D 109.4 . . ?
N1 C1 H1E 109.4 . . ?
C2 C1 H1D 109.4 . . ?
C2 C1 H1E 109.4 . . ?
H1D C1 H1E 108.0 . . ?
C6 C5 H5 121.4 . . ?
C6 C5 C4 117.2(8) . . ?
C4 C5 H5 121.4 . . ?
N4 C4 C3 109.8(8) . . ?
N4 C4 C5 130.6(8) . . ?
C3 C4 C5 119.5(13) . . ?
C3 C8 H8 121.2 . . ?
C7 C8 C3 117.6(9) . . ?
C7 C8 H8 121.2 . . ?

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
F2 C7 C8 C3 -179.3(7) . . . . ?
F1 C6 C7 F2 2.9(10) . . . . ?
F1 C6 C7 C8 -176.9(6) . . . . ?
F1 C6 C5 C4 178.3(4) . . . . ?
N4 N2 N3 C3 0.4(6) . . . . ?
N4 N2 C2 C1 95.2(6) . . . . ?
N2 N4 C4 C3 -0.9(7) . . . . ?
N2 N4 C4 C5 178.6(6) . . . . ?
N2 C2 C1 N1 68.9(8) . . . . ?
C6 C7 C8 C3 0.4(10) . . . . ?
C6 C5 C4 N4 176.9(7) . . . . ?
C6 C5 C4 C3 -3.7(9) . . . . ?
N3 N2 C2 C1 -81.6(8) . . . . ?
N3 C3 C4 N4 1.2(7) . . . . ?
N3 C3 C4 C5 -178.3(5) . . . . ?
N3 C3 C8 C7 -179.4(6) . . . . ?
C2 N2 N3 C3 177.4(5) . . . . ?
C7 C6 C5 C4 1.9(10) . . . . ?
C5 C6 C7 F2 179.5(7) . . . . ?
C5 C6 C7 C8 -0.3(11) . . . . ?
C4 N4 N2 N3 0.3(7) . . . . ?
C4 N4 N2 C2 -176.7(5) . . . . ?
C4 C3 N3 N2 -0.9(5) . . . . ?
C4 C3 C8 C7 -2.4(10) . . . . ?
C8 C3 N3 N2 176.5(7) . . . . ?
C8 C3 C4 N4 -176.4(6) . . . . ?
C8 C3 C4 C5 4.0(9) . . . . ?

_shelx_res_file                  
;
TITL mo_DAC24_F2BTa2PbI4_1p10GPa_0ma_d.res in Pnma
    1p10gpa_good.res
    created by SHELXL-2019/1 at 17:10:46 on 07-Feb-2024
REM Old TITL __TMP__ in Pnma
REM SHELXT solution in Pnma: R1 0.194, Rweak 0.003, Alpha 0.037
REM <I/s> 2.588 for 103 systematic absences, Orientation as input
REM Formula found by SHELXT: C11 F4 I4 N4 Pb
CELL 0.71073 12.7582 29.2337 6.5183 90 90 90
ZERR 4 0.0005 0.0021 0.0003 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H F I N Pb
UNIT 64 72 16 16 32 4

L.S. 10
PLAN  1
TEMP 0
CONF
BOND
LIST 6
fmap 2
MORE -1
BOND $H
ACTA
OMIT 2 10 4
OMIT 2 11 7
OMIT 3 9 3
OMIT 4 7 1
OMIT 4 11 6
OMIT 5 11 6
OMIT 6 8 0
OMIT 7 0 6
OMIT 7 11 6
OMIT 8 11 4
OMIT 12 10 4
REM <olex2.extras>
REM <HklSrc "%.\\1p10GPa_good.hkl">
REM </olex2.extras>

WGHT    0.006600    7.303700
FVAR       0.19852
PB1   6    0.340726    0.750000    0.698774    10.50000    0.02405    0.04204 =
         0.02705    0.00000   -0.00027    0.00000
I1    4    0.348065    0.750000    0.206343    10.50000    0.03581    0.04326 =
         0.02352    0.00000    0.00076    0.00000
I2    4    0.091805    0.750000    0.753131    10.50000    0.02040    0.06094 =
         0.04186    0.00000    0.00071    0.00000
I3    4    0.321765    0.643279    0.674991    11.00000    0.03443    0.04472 =
         0.03030   -0.00015   -0.00007    0.00296
F2    3    0.444774    0.412371    0.357898    11.00000    0.04154    0.01373 =
         0.04751   -0.00191    0.00409   -0.00520
F1    3    0.264437    0.448868    0.432695    11.00000    0.02888    0.04306 =
         0.04492    0.00210    0.00766   -0.00515
N4    5    0.405459    0.593763    0.204567    11.00000    0.02553
N2    5    0.505544    0.599949    0.149423    11.00000    0.02488
C3    1    0.502939    0.530042    0.223949    11.00000    0.02144
C6    1    0.338086    0.476871    0.357811    11.00000    0.02614
N3    5    0.568156    0.562891    0.158613    11.00000    0.02519
N1    5    0.695109    0.644975    0.333698    11.00000    0.03712
AFIX 137
H1A   2    0.743329    0.649711    0.237345    11.00000   -1.50000
H1B   2    0.684055    0.615072    0.347440    11.00000   -1.50000
H1C   2    0.717454    0.656445    0.452373    11.00000   -1.50000
AFIX   0
C2    1    0.544484    0.644059    0.093706    11.00000    0.03122
AFIX  23
H2A   2    0.487108    0.662662    0.042988    11.00000   -1.20000
H2B   2    0.595257    0.640769   -0.016074    11.00000   -1.20000
AFIX   0
C7    1    0.438488    0.456994    0.321229    11.00000    0.02740
C1    1    0.595442    0.667915    0.273301    11.00000    0.03649
AFIX  23
H1D   2    0.609791    0.699477    0.236983    11.00000   -1.20000
H1E   2    0.547596    0.667902    0.388952    11.00000   -1.20000
AFIX   0
C5    1    0.318367    0.522245    0.329463    11.00000    0.02466
AFIX  43
H5    2    0.252920    0.534732    0.357942    11.00000   -1.20000
AFIX   0
C4    1    0.402673    0.549927    0.253936    11.00000    0.02300
C8    1    0.520942    0.483172    0.253880    11.00000    0.02181
AFIX  43
H8    2    0.586376    0.470297    0.228996    11.00000   -1.20000
AFIX   0
HKLF 4




REM  mo_DAC24_F2BTa2PbI4_1p10GPa_0ma_d.res in Pnma
REM wR2 = 0.0350, GooF = S = 1.118, Restrained GooF = 1.118 for all data
REM R1 = 0.0166 for 908 Fo > 4sig(Fo) and 0.0181 for all 944 data
REM 95 parameters refined using 0 restraints

END

WGHT      0.0074      6.8837

REM Highest difference peak  0.317,  deepest hole -0.337,  1-sigma level  0.077
Q1    1   0.4255  0.7500  0.0186  10.50000  0.05    0.32
;
_shelx_res_checksum              27736
_olex2_submission_special_instructions 'No special instructions were received'
_olex2_exptl_crystal_mounting_method 
'Crystal mounted in a Diamond anvil cell of 100 degre opening angle'

_vrf_PLAT029_1p10gpa_good        
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT201_1p10gpa_good        
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         12 Report
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the available data, preventing from a complete anisotropic refienement. 
;
_vrf_PLAT933_1p10gpa_good        
;
PROBLEM: Number of HKL-OMIT Records in Embedded .res File          
RESPONSE: Experiment done in a Diamond Anvil Cell some reflections are close 
to gasket ring/shadow or close to diamond peaks and should be deleted.  
;
_vrf_PLAT911_1p10gpa_good        
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT910_1p10gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT913_1p10gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space 
;
_vrf_PLAT088_1p10gpa_good        
;
PROBLEM: 
RESPONSE: Experiment done under pressure in a Diamond Anvil Cell limitting 
the access to reciprocal space and then number of measured reflections inducing
a low Data / Parameter Ratio despite isotropic refinement done to limit this 
problem
;
