# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_(R_3_FPD)PbBr3
_database_code_depnum_ccdc_archive 'CCDC 2272053'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2023-06-24 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_audit_creation_date             2022-01-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C5 H11 F N'
_chemical_formula_sum            'C5 H11 Br3 F N Pb'
_chemical_formula_weight         551.07
_chemical_absolute_configuration rmad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C N H F Pb Br'
_chemical_oxdiff_usercomment     \
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'
Br Br -0.2901 2.4595 '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'
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           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   7.8341(5)
_cell_length_b                   10.1533(6)
_cell_length_c                   14.2642(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1134.60(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3683
_cell_measurement_temperature    293(10)
_cell_measurement_theta_max      29.5290
_cell_measurement_theta_min      2.4510
_shelx_estimated_absorpt_T_max   0.785
_shelx_estimated_absorpt_T_min   0.516
_exptl_absorpt_coefficient_mu    25.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic brownish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.226
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.824
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6359
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.778
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.639
_diffrn_reflns_theta_min         2.462
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00 -12.00   0.50    0.62    --   -5.29 103.00  29.00   52
  2  ω     15.00  78.00   0.50    0.62    --    5.13  38.00 177.00  126
  3  ω    -14.00  25.00   0.50    0.62    --   -5.29 -99.00   0.00   78
  4  ω    -15.00  28.00   0.50    0.62    --   -5.29 -99.00  30.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0811532000
_diffrn_orient_matrix_UB_12      -0.0056989000
_diffrn_orient_matrix_UB_13      0.0217428000
_diffrn_orient_matrix_UB_21      -0.0317865000
_diffrn_orient_matrix_UB_22      0.0328989000
_diffrn_orient_matrix_UB_23      0.0402054000
_diffrn_orient_matrix_UB_31      -0.0246218000
_diffrn_orient_matrix_UB_32      -0.0613601000
_diffrn_orient_matrix_UB_33      0.0195492000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.644
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.717
_reflns_number_gt                2186
_reflns_number_total             2731
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         3.537
_refine_diff_density_min         -5.231
_refine_diff_density_rms         0.492
_refine_ls_abs_structure_details 
;
 Flack x determined using 695 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_coef       0.0138(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2731
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0658
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1101P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1687
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Ternary CH refined with riding coordinates:
 C8(H8)
1.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2A,H2B), N1(H1A,H1B), C5(H5A,H5B), C6(H6A,H6B)
;
_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 -0.47768(6) 0.75639(5) 0.50270(4) 0.02733(12) Uani 1 1 d . . . . .
Br2 Br -0.1968(2) 0.69898(16) 0.66035(10) 0.0364(4) Uani 1 1 d . . . . .
Br3 Br -0.2000(2) 0.96430(14) 0.44479(10) 0.0312(3) Uani 1 1 d . . . . .
Br4 Br -0.27531(17) 0.57727(14) 0.39430(11) 0.0312(3) Uani 1 1 d . . . . .
F3 F -0.3348(15) 1.2787(10) 0.5134(6) 0.053(3) Uani 1 1 d . . . . .
C4 C -0.126(2) 1.3100(13) 0.6283(11) 0.035(4) Uani 1 1 d . . . . .
H4A H -0.099760 1.350439 0.688239 0.042 Uiso 1 1 calc R U . . .
H4B H -0.057055 1.352770 0.580665 0.042 Uiso 1 1 calc R U . . .
C2 C -0.194(2) 1.0905(16) 0.7003(10) 0.037(4) Uani 1 1 d . . . . .
H2A H -0.165459 0.997543 0.698215 0.044 Uiso 1 1 calc R U . . .
H2B H -0.172804 1.122045 0.763514 0.044 Uiso 1 1 calc R U . . .
N1 N -0.0824(15) 1.1653(10) 0.6319(9) 0.029(3) Uani 1 1 d . . . . .
H1A H 0.026488 1.156012 0.648530 0.034 Uiso 1 1 calc R U . . .
H1B H -0.094870 1.130720 0.574996 0.034 Uiso 1 1 calc R U . . .
C8 C -0.308(2) 1.3282(15) 0.6067(12) 0.042(4) Uani 1 1 d . . . . .
H8 H -0.336160 1.422237 0.608475 0.051 Uiso 1 1 calc R U . . .
C5 C -0.423(2) 1.2558(17) 0.6704(12) 0.048(4) Uani 1 1 d . . . . .
H5A H -0.540046 1.265163 0.648667 0.057 Uiso 1 1 calc R U . . .
H5B H -0.416249 1.293929 0.732638 0.057 Uiso 1 1 calc R U . . .
C6 C -0.378(2) 1.1095(16) 0.6758(11) 0.040(4) Uani 1 1 d . . . . .
H6A H -0.449077 1.067183 0.722782 0.048 Uiso 1 1 calc R U . . .
H6B H -0.401759 1.068124 0.615843 0.048 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 2.9258(16) 3_466 ?
Pb1 Br2 3.1999(16) . ?
Pb1 Br3 2.9351(16) 3_466 ?
Pb1 Br3 3.1419(16) . ?
Pb1 Br4 3.2323(15) 3_466 ?
Pb1 Br4 2.8657(15) . ?
F3 C8 1.437(19) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 N1 1.509(17) . ?
C4 C8 1.47(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 N1 1.513(18) . ?
C2 C6 1.50(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C8 H8 0.9800 . ?
C8 C5 1.48(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.53(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

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
Br2 Pb1 Br2 172.00(5) 3_466 . ?
Br2 Pb1 Br3 95.34(4) 3_466 . ?
Br2 Pb1 Br3 88.45(5) 3_466 3_466 ?
Br2 Pb1 Br4 81.79(4) 3_466 3_466 ?
Br2 Pb1 Br4 105.78(4) . 3_466 ?
Br3 Pb1 Br2 80.27(4) . . ?
Br3 Pb1 Br2 95.15(4) 3_466 . ?
Br3 Pb1 Br3 172.25(5) 3_466 . ?
Br3 Pb1 Br4 105.54(4) . 3_466 ?
Br3 Pb1 Br4 81.66(4) 3_466 3_466 ?
Br4 Pb1 Br2 83.29(4) . . ?
Br4 Pb1 Br2 89.65(5) . 3_466 ?
Br4 Pb1 Br3 88.94(4) . 3_466 ?
Br4 Pb1 Br3 84.34(4) . . ?
Br4 Pb1 Br4 167.41(4) . 3_466 ?
Pb1 Br2 Pb1 79.43(4) 3_566 . ?
Pb1 Br3 Pb1 80.26(3) 3_566 . ?
Pb1 Br4 Pb1 79.76(4) . 3_566 ?
H4A C4 H4B 108.1 . . ?
N1 C4 H4A 109.6 . . ?
N1 C4 H4B 109.6 . . ?
C8 C4 H4A 109.6 . . ?
C8 C4 H4B 109.6 . . ?
C8 C4 N1 110.4(11) . . ?
H2A C2 H2B 108.2 . . ?
N1 C2 H2A 109.7 . . ?
N1 C2 H2B 109.7 . . ?
C6 C2 H2A 109.7 . . ?
C6 C2 H2B 109.7 . . ?
C6 C2 N1 109.9(12) . . ?
C4 N1 C2 112.4(11) . . ?
C4 N1 H1A 109.1 . . ?
C4 N1 H1B 109.1 . . ?
C2 N1 H1A 109.1 . . ?
C2 N1 H1B 109.1 . . ?
H1A N1 H1B 107.9 . . ?
F3 C8 C4 106.9(14) . . ?
F3 C8 H8 109.4 . . ?
F3 C8 C5 107.9(13) . . ?
C4 C8 H8 109.4 . . ?
C4 C8 C5 113.6(14) . . ?
C5 C8 H8 109.4 . . ?
C8 C5 H5A 109.2 . . ?
C8 C5 H5B 109.2 . . ?
C8 C5 C6 111.9(13) . . ?
H5A C5 H5B 107.9 . . ?
C6 C5 H5A 109.2 . . ?
C6 C5 H5B 109.2 . . ?
C2 C6 C5 111.0(13) . . ?
C2 C6 H6A 109.4 . . ?
C2 C6 H6B 109.4 . . ?
C5 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?

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
F3 C8 C5 C6 64.8(17) . . . . ?
C4 C8 C5 C6 -53.5(19) . . . . ?
N1 C4 C8 F3 -65.1(16) . . . . ?
N1 C4 C8 C5 53.8(18) . . . . ?
N1 C2 C6 C5 -54.6(17) . . . . ?
C8 C4 N1 C2 -55.3(17) . . . . ?
C8 C5 C6 C2 53.5(19) . . . . ?
C6 C2 N1 C4 56.5(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 11.935
_oxdiff_exptl_absorpt_empirical_full_min 0.353
####################################################################### 
# 
# 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_(3_3_DFPD)2PbBr4
_database_code_depnum_ccdc_archive 'CCDC 2272054'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2023-06-24 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_audit_creation_date             2021-12-27
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br8 Pb2, 4(C5 H10 F2 N)'
_chemical_formula_sum            'C20 H40 Br8 F8 N4 Pb2'
_chemical_formula_weight         1542.22
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
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      tetragonal
_space_group_IT_number           92
_space_group_name_H-M_alt        'P 41 21 2'
_space_group_name_Hall           'P 4abw 2nw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x+1/2, z+1/4'
'-x, -y, z+1/2'
'y+1/2, -x+1/2, z+3/4'
'x+1/2, -y+1/2, -z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   12.2050(3)
_cell_length_b                   12.2050(3)
_cell_length_c                   51.295(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7641.0(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    8032
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.4200
_cell_measurement_theta_min      2.3830
_shelx_estimated_absorpt_T_max   0.847
_shelx_estimated_absorpt_T_min   0.626
_exptl_absorpt_coefficient_mu    17.228
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic brownish colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.681
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5632
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            34696
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.715
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.703
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5695
_reflns_number_total             7503
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.575
_refine_diff_density_min         -1.476
_refine_diff_density_rms         0.381
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.504(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         7503
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0710
_refine_ls_restrained_S_all      1.090
_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)+(0.0648P)²+90.4424P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1575
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.496(14)
 0.504(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
3. Restrained distances
 C77-C18 = C77-C45 = C54-C45 = C7-C54
 1.54 with sigma of 0.02
 C2-H2A = N15-C18
 1.5 with sigma of 0.02
4. Rigid bond restraints
 C77
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
F74 \\sim C77: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
Uanis(C77) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C18) = Uanis(N15) = Uanis(C7) = Uanis(C54) = Uanis(C45) = Uanis(C77)
6.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), C2(H2A,H2B), N1(H1A,H1B), C5(H5A,H5B), C1(H1C,H1D), C8(H8A,H8B),
 C10(H10A,H10B), C13(H13A,H13B), C17(H17A,H17B), C22(H22A,H22B), N4(H4A,H4B),
 C6(H6A,H6B), C3(H3C,H3D), N15(H15A,H15B), C14(H14A,H14B), C18(H18A,H18B),
 C7(H7A,H7B), C19(H19A,H19B), C45(H45A,H45B), C54(H54A,H54B)
;
_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 0.44538(3) -0.25461(4) -0.12438(2) 0.03035(10) Uani 1 1 d . . . . .
Pb2 Pb 0.49761(4) -0.75499(4) -0.12292(2) 0.02893(10) Uani 1 1 d . . . . .
Br3 Br 0.44408(11) -0.25113(13) -0.18267(3) 0.0472(4) Uani 1 1 d . . . . .
Br4 Br 0.50221(11) -0.75570(12) -0.17984(3) 0.0422(3) Uani 1 1 d . . . . .
Br5 Br 0.73820(11) -0.78004(13) -0.12438(3) 0.0552(4) Uani 1 1 d . . . . .
Br6 Br 0.20440(11) -0.27467(15) -0.12485(3) 0.0617(5) Uani 1 1 d . . . . .
Br7 Br 0.41181(11) -0.26287(12) -0.06661(3) 0.0433(4) Uani 1 1 d . . . . .
Br8 Br 0.53294(11) -0.76930(11) -0.06366(3) 0.0423(4) Uani 1 1 d . . . . .
Br9 Br 0.47617(13) -0.98939(11) -0.12425(3) 0.0536(5) Uani 1 1 d . . . . .
Br10 Br 0.46272(14) -0.48941(11) -0.12415(3) 0.0599(5) Uani 1 1 d . . . . .
F2 F 0.6421(8) 0.1806(8) 0.0298(2) 0.073(3) Uani 1 1 d . . . . .
F8 F 0.5310(10) 0.0431(9) 0.0273(2) 0.099(4) Uani 1 1 d . . . . .
C9 C 0.8001(11) 0.0254(12) -0.0342(3) 0.044(4) Uani 1 1 d . . . . .
C11 C 0.5398(12) 0.1458(12) 0.0349(3) 0.048(4) Uani 1 1 d . . . . .
F18 F 0.7628(8) 0.1300(7) -0.02759(18) 0.078(3) Uani 1 1 d . . . . .
F21 F 0.9081(9) 0.0217(10) -0.0266(2) 0.092(4) Uani 1 1 d . . . . .
N3 N 0.5062(11) 0.2489(11) 0.0749(2) 0.098(4) Uani 1 1 d . . . . .
H3A H 0.569362 0.285300 0.074834 0.117 Uiso 1 1 calc R U . . .
H3B H 0.486167 0.241408 0.091472 0.117 Uiso 1 1 calc R U . . .
C2 C 0.7367(13) -0.0562(13) -0.0217(3) 0.061(5) Uani 1 1 d D . . . .
H2A H 0.730039 -0.039924 -0.003292 0.074 Uiso 1 1 calc DR U . . .
H2B H 0.771782 -0.127042 -0.023594 0.074 Uiso 1 1 calc R U . . .
N1 N 0.6930(10) 0.0161(10) -0.0743(2) 0.052(4) Uani 1 1 d . . . . .
H1A H 0.660094 0.079134 -0.070421 0.063 Uiso 1 1 calc R U . . .
H1B H 0.693202 0.009480 -0.091583 0.063 Uiso 1 1 calc R U . . .
C5 C 0.4577(15) 0.2202(14) 0.0210(3) 0.077(6) Uani 1 1 d . . . . .
H5A H 0.482380 0.231449 0.003244 0.092 Uiso 1 1 calc R U . . .
H5B H 0.387570 0.182919 0.020238 0.092 Uiso 1 1 calc R U . . .
C1 C 0.6214(12) -0.0586(14) -0.0346(3) 0.054(5) Uani 1 1 d . . . . .
H1C H 0.578846 -0.117881 -0.027102 0.064 Uiso 1 1 calc R U . . .
H1D H 0.583639 0.009627 -0.030876 0.064 Uiso 1 1 calc R U . . .
C8 C 0.8108(12) 0.0208(12) -0.0647(3) 0.045(4) Uani 1 1 d . . . . .
H8A H 0.847700 0.085523 -0.071347 0.054 Uiso 1 1 calc R U . . .
H8B H 0.851191 -0.043702 -0.070176 0.054 Uiso 1 1 calc R U . . .
C10 C 0.4422(15) 0.3239(14) 0.0329(3) 0.072(6) Uani 1 1 d . . . . .
H10A H 0.379890 0.359465 0.024773 0.086 Uiso 1 1 calc R U . . .
H10B H 0.506261 0.368727 0.029517 0.086 Uiso 1 1 calc R U . . .
C13 C 0.6291(12) -0.0738(11) -0.0632(3) 0.051(4) Uani 1 1 d . . . . .
H13A H 0.664189 -0.143223 -0.067078 0.061 Uiso 1 1 calc R U . . .
H13B H 0.556252 -0.074616 -0.070784 0.061 Uiso 1 1 calc R U . . .
C17 C 0.4233(14) 0.3194(14) 0.0619(3) 0.067(5) Uani 1 1 d . . . . .
H17A H 0.427184 0.392832 0.069100 0.080 Uiso 1 1 calc R U . . .
H17B H 0.350588 0.290689 0.065382 0.080 Uiso 1 1 calc R U . . .
C22 C 0.5271(13) 0.1426(13) 0.0649(3) 0.054(5) Uani 1 1 d . . . . .
H22A H 0.467220 0.094122 0.069564 0.065 Uiso 1 1 calc R U . . .
H22B H 0.593673 0.113863 0.072699 0.065 Uiso 1 1 calc R U . . .
F4 F 0.5326(10) -0.7256(10) -0.2477(2) 0.106(4) Uani 1 1 d . . . . .
F3 F 0.4552(10) -0.8482(8) -0.2714(2) 0.099(4) Uani 1 1 d . . . . .
N4 N 0.3850(10) -0.6809(9) -0.3087(3) 0.060(4) Uani 1 1 d . . . . .
H4A H 0.347447 -0.743104 -0.310152 0.072 Uiso 1 1 calc R U . . .
H4B H 0.341407 -0.626621 -0.313939 0.072 Uiso 1 1 calc R U . . .
C6 C 0.4134(13) -0.6633(15) -0.2808(3) 0.061(5) Uani 1 1 d . . . . .
H6A H 0.348922 -0.672911 -0.269960 0.073 Uiso 1 1 calc R U . . .
H6B H 0.440896 -0.589507 -0.278225 0.073 Uiso 1 1 calc R U . . .
C3 C 0.5969(12) -0.7539(15) -0.2898(3) 0.069(5) Uani 1 1 d . . . . .
H3C H 0.643365 -0.813723 -0.284106 0.082 Uiso 1 1 calc R U . . .
H3D H 0.638667 -0.686496 -0.288509 0.082 Uiso 1 1 calc R U . . .
N15 N 0.7696(15) -0.6089(15) -0.0609(2) 0.111(3) Uani 1 1 d D . . . .
H15A H 0.709394 -0.650043 -0.061173 0.133 Uiso 1 1 calc R U . . .
H15B H 0.823783 -0.649334 -0.067399 0.133 Uiso 1 1 calc R U . . .
C12 C 0.5016(12) -0.7472(15) -0.2732(3) 0.062(5) Uani 1 1 d . . . . .
F16 F 0.6070(12) -0.5494(15) -0.0212(3) 0.182(7) Uani 1 1 d . . . . .
C14 C 0.5642(12) -0.7719(12) -0.3173(2) 0.050(4) Uani 1 1 d . U . . .
H14A H 0.532678 -0.844481 -0.319103 0.060 Uiso 1 1 calc R U . . .
H14B H 0.628480 -0.768083 -0.328395 0.060 Uiso 1 1 calc R U . . .
C18 C 0.7958(13) -0.5854(14) -0.0335(2) 0.111(3) Uani 1 1 d D . . . .
H18A H 0.867550 -0.551708 -0.032257 0.133 Uiso 1 1 calc R U . . .
H18B H 0.796503 -0.652795 -0.023493 0.133 Uiso 1 1 calc R U . . .
C7 C 0.7520(13) -0.5157(14) -0.0786(4) 0.111(3) Uani 1 1 d D . . . .
H7A H 0.730861 -0.542229 -0.095652 0.133 Uiso 1 1 calc R U . . .
H7B H 0.819554 -0.474440 -0.080389 0.133 Uiso 1 1 calc R U . . .
C19 C 0.4804(14) -0.6859(16) -0.3262(3) 0.065(5) Uani 1 1 d . U . . .
H19A H 0.515411 -0.614631 -0.326764 0.078 Uiso 1 1 calc R U . . .
H19B H 0.455901 -0.703559 -0.343699 0.078 Uiso 1 1 calc R U . . .
C45 C 0.6880(18) -0.4078(12) -0.0395(2) 0.111(3) Uani 1 1 d D . . . .
H45A H 0.752222 -0.361034 -0.039261 0.133 Uiso 1 1 calc R U . . .
H45B H 0.627058 -0.366660 -0.032287 0.133 Uiso 1 1 calc R U . . .
C54 C 0.6618(13) -0.4410(14) -0.0676(2) 0.111(3) Uani 1 1 d D . . . .
H54A H 0.655600 -0.375861 -0.078368 0.133 Uiso 1 1 calc R U . . .
H54B H 0.592071 -0.479151 -0.068128 0.133 Uiso 1 1 calc R U . . .
F74 F 0.7317(11) -0.4813(12) -0.0001(3) 0.131(3) Uani 1 1 d . U . . .
C77 C 0.7088(14) -0.5080(11) -0.0229(3) 0.111(3) Uani 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br3 2.9906(15) . ?
Pb1 Br6 2.9514(14) . ?
Pb1 Br6 3.1817(15) 5_544 ?
Pb1 Br7 2.9931(15) . ?
Pb1 Br10 2.8735(14) . ?
Pb2 Br4 2.9207(14) . ?
Pb2 Br5 3.1978(14) 5_434 ?
Pb2 Br5 2.9533(14) . ?
Pb2 Br8 3.0749(15) . ?
Pb2 Br9 2.8736(14) . ?
Pb2 Br10 3.2699(14) . ?
F2 C11 1.344(17) . ?
F8 C11 1.319(18) . ?
C9 F18 1.397(16) . ?
C9 F21 1.376(17) . ?
C9 C2 1.41(2) . ?
C9 C8 1.574(19) . ?
C11 C5 1.53(2) . ?
C11 C22 1.55(2) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C17 1.48(2) . ?
N3 C22 1.42(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.55(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C8 1.521(18) . ?
N1 C13 1.462(18) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C10 1.42(2) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C13 1.483(19) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C17 1.51(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
F4 C12 1.385(18) . ?
F3 C12 1.36(2) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 C6 1.49(2) . ?
N4 C19 1.47(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C12 1.54(2) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C3 C12 1.45(2) . ?
C3 C14 1.48(2) . ?
N15 H15A 0.8900 . ?
N15 H15B 0.8900 . ?
N15 C18 1.468(15) . ?
N15 C7 1.47(2) . ?
F16 C77 1.34(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C19 1.53(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C77 1.521(18) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C54 1.536(18) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C45 C54 1.534(16) . ?
C45 C77 1.511(17) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
F74 C77 1.25(2) . ?

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
Br3 Pb1 Br6 89.50(4) . 5_544 ?
Br3 Pb1 Br7 171.75(4) . . ?
Br6 Pb1 Br3 89.29(4) . . ?
Br6 Pb1 Br6 177.934(18) . 5_544 ?
Br6 Pb1 Br7 82.47(4) . . ?
Br7 Pb1 Br6 98.75(4) . 5_544 ?
Br10 Pb1 Br3 91.07(5) . . ?
Br10 Pb1 Br6 89.47(5) . . ?
Br10 Pb1 Br6 92.23(5) . 5_544 ?
Br10 Pb1 Br7 88.42(5) . . ?
Br4 Pb2 Br5 88.63(4) . 5_434 ?
Br4 Pb2 Br5 87.43(4) . . ?
Br4 Pb2 Br8 170.21(4) . . ?
Br4 Pb2 Br10 89.20(4) . . ?
Br5 Pb2 Br5 175.689(17) . 5_434 ?
Br5 Pb2 Br8 83.09(4) . . ?
Br5 Pb2 Br10 74.80(4) 5_434 . ?
Br5 Pb2 Br10 103.39(5) . . ?
Br8 Pb2 Br5 100.92(4) . 5_434 ?
Br8 Pb2 Br10 95.38(4) . . ?
Br9 Pb2 Br4 88.57(5) . . ?
Br9 Pb2 Br5 89.25(5) . . ?
Br9 Pb2 Br5 92.40(4) . 5_434 ?
Br9 Pb2 Br8 88.84(4) . . ?
Br9 Pb2 Br10 167.05(5) . . ?
Pb2 Br5 Pb2 166.33(6) . 5_534 ?
Pb1 Br6 Pb1 168.79(7) . 5_444 ?
Pb1 Br10 Pb2 176.63(7) . . ?
F18 C9 C2 110.9(12) . . ?
F18 C9 C8 107.5(11) . . ?
F21 C9 F18 105.9(11) . . ?
F21 C9 C2 111.9(13) . . ?
F21 C9 C8 101.7(11) . . ?
C2 C9 C8 118.0(12) . . ?
F2 C11 C5 109.4(13) . . ?
F2 C11 C22 107.0(12) . . ?
F8 C11 F2 108.5(12) . . ?
F8 C11 C5 111.9(13) . . ?
F8 C11 C22 105.3(12) . . ?
C5 C11 C22 114.5(13) . . ?
H3A N3 H3B 107.0 . . ?
C17 N3 H3A 107.4 . . ?
C17 N3 H3B 107.4 . . ?
C22 N3 H3A 107.4 . . ?
C22 N3 H3B 107.4 . . ?
C22 N3 C17 119.5(13) . . ?
C9 C2 H2A 110.0 . . ?
C9 C2 H2B 110.0 . . ?
C9 C2 C1 108.5(12) . . ?
H2A C2 H2B 108.4 . . ?
C1 C2 H2A 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H1A N1 H1B 107.6 . . ?
C8 N1 H1A 108.7 . . ?
C8 N1 H1B 108.7 . . ?
C13 N1 H1A 108.7 . . ?
C13 N1 H1B 108.7 . . ?
C13 N1 C8 114.0(11) . . ?
C11 C5 H5A 108.6 . . ?
C11 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
C10 C5 C11 114.7(14) . . ?
C10 C5 H5A 108.6 . . ?
C10 C5 H5B 108.6 . . ?
C2 C1 H1C 109.3 . . ?
C2 C1 H1D 109.3 . . ?
H1C C1 H1D 108.0 . . ?
C13 C1 C2 111.4(12) . . ?
C13 C1 H1C 109.3 . . ?
C13 C1 H1D 109.3 . . ?
C9 C8 H8A 110.9 . . ?
C9 C8 H8B 110.9 . . ?
N1 C8 C9 104.1(10) . . ?
N1 C8 H8A 110.9 . . ?
N1 C8 H8B 110.9 . . ?
H8A C8 H8B 109.0 . . ?
C5 C10 H10A 108.7 . . ?
C5 C10 H10B 108.7 . . ?
C5 C10 C17 114.4(14) . . ?
H10A C10 H10B 107.6 . . ?
C17 C10 H10A 108.7 . . ?
C17 C10 H10B 108.7 . . ?
N1 C13 C1 109.0(12) . . ?
N1 C13 H13A 109.9 . . ?
N1 C13 H13B 109.9 . . ?
C1 C13 H13A 109.9 . . ?
C1 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
N3 C17 C10 111.0(13) . . ?
N3 C17 H17A 109.4 . . ?
N3 C17 H17B 109.4 . . ?
C10 C17 H17A 109.4 . . ?
C10 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
C11 C22 H22A 109.5 . . ?
C11 C22 H22B 109.5 . . ?
N3 C22 C11 110.6(12) . . ?
N3 C22 H22A 109.5 . . ?
N3 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
H4A N4 H4B 107.6 . . ?
C6 N4 H4A 108.7 . . ?
C6 N4 H4B 108.7 . . ?
C19 N4 H4A 108.7 . . ?
C19 N4 H4B 108.7 . . ?
C19 N4 C6 114.1(12) . . ?
N4 C6 H6A 110.1 . . ?
N4 C6 H6B 110.1 . . ?
N4 C6 C12 108.2(13) . . ?
H6A C6 H6B 108.4 . . ?
C12 C6 H6A 110.1 . . ?
C12 C6 H6B 110.1 . . ?
H3C C3 H3D 108.1 . . ?
C12 C3 H3C 109.5 . . ?
C12 C3 H3D 109.5 . . ?
C12 C3 C14 110.7(13) . . ?
C14 C3 H3C 109.5 . . ?
C14 C3 H3D 109.5 . . ?
H15A N15 H15B 107.1 . . ?
C18 N15 H15A 107.8 . . ?
C18 N15 H15B 107.8 . . ?
C18 N15 C7 118.0(16) . . ?
C7 N15 H15A 107.8 . . ?
C7 N15 H15B 107.8 . . ?
F4 C12 C6 107.7(13) . . ?
F4 C12 C3 110.4(13) . . ?
F3 C12 F4 103.0(13) . . ?
F3 C12 C6 109.2(13) . . ?
F3 C12 C3 108.8(15) . . ?
C3 C12 C6 116.8(14) . . ?
C3 C14 H14A 109.4 . . ?
C3 C14 H14B 109.4 . . ?
C3 C14 C19 111.2(12) . . ?
H14A C14 H14B 108.0 . . ?
C19 C14 H14A 109.4 . . ?
C19 C14 H14B 109.4 . . ?
N15 C18 H18A 110.1 . . ?
N15 C18 H18B 110.1 . . ?
N15 C18 C77 108.1(14) . . ?
H18A C18 H18B 108.4 . . ?
C77 C18 H18A 110.1 . . ?
C77 C18 H18B 110.1 . . ?
N15 C7 H7A 109.7 . . ?
N15 C7 H7B 109.7 . . ?
N15 C7 C54 109.8(15) . . ?
H7A C7 H7B 108.2 . . ?
C54 C7 H7A 109.7 . . ?
C54 C7 H7B 109.7 . . ?
N4 C19 C14 112.1(12) . . ?
N4 C19 H19A 109.2 . . ?
N4 C19 H19B 109.2 . . ?
C14 C19 H19A 109.2 . . ?
C14 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
H45A C45 H45B 108.1 . . ?
C54 C45 H45A 109.5 . . ?
C54 C45 H45B 109.5 . . ?
C77 C45 H45A 109.5 . . ?
C77 C45 H45B 109.5 . . ?
C77 C45 C54 110.5(13) . . ?
C7 C54 H54A 109.5 . . ?
C7 C54 H54B 109.5 . . ?
C45 C54 C7 110.5(14) . . ?
C45 C54 H54A 109.5 . . ?
C45 C54 H54B 109.5 . . ?
H54A C54 H54B 108.1 . . ?
F16 C77 C18 115.8(14) . . ?
F16 C77 C45 100.8(15) . . ?
C45 C77 C18 114.8(14) . . ?
F74 C77 F16 104.1(15) . . ?
F74 C77 C18 110.0(14) . . ?
F74 C77 C45 110.7(13) . . ?

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 C11 C5 C10 -75.6(18) . . . . ?
F2 C11 C22 N3 80.0(15) . . . . ?
F8 C11 C5 C10 164.1(15) . . . . ?
F8 C11 C22 N3 -164.6(13) . . . . ?
C9 C2 C1 C13 54.8(18) . . . . ?
C11 C5 C10 C17 -48(2) . . . . ?
F18 C9 C2 C1 71.0(15) . . . . ?
F18 C9 C8 N1 -73.1(13) . . . . ?
F21 C9 C2 C1 -171.0(12) . . . . ?
F21 C9 C8 N1 175.9(11) . . . . ?
C2 C9 C8 N1 53.1(16) . . . . ?
C2 C1 C13 N1 -59.2(17) . . . . ?
C5 C11 C22 N3 -41.3(18) . . . . ?
C5 C10 C17 N3 48(2) . . . . ?
C8 C9 C2 C1 -53.6(17) . . . . ?
C8 N1 C13 C1 62.7(15) . . . . ?
C13 N1 C8 C9 -55.3(14) . . . . ?
C17 N3 C22 C11 46.1(19) . . . . ?
C22 C11 C5 C10 44(2) . . . . ?
C22 N3 C17 C10 -50(2) . . . . ?
N4 C6 C12 F4 176.2(12) . . . . ?
N4 C6 C12 F3 -72.7(16) . . . . ?
N4 C6 C12 C3 51.3(19) . . . . ?
C6 N4 C19 C14 54.1(18) . . . . ?
C3 C14 C19 N4 -54.0(18) . . . . ?
N15 C18 C77 F16 66(2) . . . . ?
N15 C18 C77 C45 -51(2) . . . . ?
N15 C18 C77 F74 -176.3(15) . . . . ?
N15 C7 C54 C45 53.4(19) . . . . ?
C12 C3 C14 C19 52.8(19) . . . . ?
C14 C3 C12 F4 -177.4(14) . . . . ?
C14 C3 C12 F3 70.3(18) . . . . ?
C14 C3 C12 C6 -54(2) . . . . ?
C18 N15 C7 C54 -56(2) . . . . ?
C7 N15 C18 C77 53(2) . . . . ?
C19 N4 C6 C12 -50.2(18) . . . . ?
C54 C45 C77 F16 -71.3(18) . . . . ?
C54 C45 C77 C18 54(2) . . . . ?
C54 C45 C77 F74 179.0(15) . . . . ?
C77 C45 C54 C7 -54(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.496(14)
2 0.504(14)

