# Electronic Supplementary Material (ESI) for Materials Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

####################################################################### 
# 
# 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_3cl-pea_cc
_database_code_depnum_ccdc_archive 'CCDC 1986784'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2020-02-27 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT109_3cl-pea_cc          
;
PROBLEM: Twinning Matrix is inverted Laue group operation ? Check
RESPONSE:   After reduction the symmetry by removing centrosymmetry, the R1 
dropped from 4.5% in C2/c to 2.9% in Cc.  Refining the structure 
with this with a twin law (an inverted Laue group 
operation) gives the lower symmetry twinned structure and 
revealed that the PbI2 framework is slightly disordered 
and with the goodness of fit and residuals that are considerably better. 
The organic ligand is no longer disordered in the non-centrosymmetric 
structure. 
;
# end Validation Reply Form

_audit_creation_date             2020-02-19
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6020)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
mtremblay6@gatech.edu
john.bacsa@emory.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C8 H11 Cl N), I8 Pb2'
_chemical_formula_sum            'C32 H44 Cl4 I8 N4 Pb2'
_chemical_formula_weight         2056.09
_chemical_absolute_configuration unk
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C64  H88  Cl8  I16  N8  Pb4  '
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   34.0078(5)
_cell_length_b                   8.54937(11)
_cell_length_c                   8.82309(13)
_cell_angle_alpha                90
_cell_angle_beta                 94.8607(14)
_cell_angle_gamma                90
_cell_volume                     2556.04(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    29553
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      38.1530
_cell_measurement_theta_min      2.3790
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.645
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.046
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'orangish yellow'
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.671
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1840
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0461
-1 0 0 0.0461
3 5 -5 0.1574
-3 -5 5 0.1574
-3 5 5 0.0950
3 -5 -5 0.0950
-4 1 -5 0.1609
5 1 -4 0.1722
-5 1 1 0.0917
-5 3 0 0.1510
4 -5 1 0.1734
5 -1 -1 0.0895

_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.092
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9996 0.0006 -0.0003 0.0006 0.0129 0.0165
-0.9996 -0.0006 0.0003 -0.0006 -0.0129 -0.0165
2.9108 4.9956 -4.9824 0.3108 -0.3707 0.3144
-2.9108 -4.9956 4.9824 -0.3108 0.3707 -0.3144
-2.9818 4.9922 4.9975 0.4951 0.2064 -0.2138
2.9818 -4.9922 -4.9975 -0.4951 -0.2064 0.2138
-4.0580 0.9966 -4.9862 -0.0156 -0.3951 0.1587
4.9489 1.0016 -3.9913 0.0084 -0.2138 0.2642
-4.9946 0.9960 1.0009 0.0965 -0.0154 -0.1153
-5.0192 2.9935 0.0061 0.2389 -0.1137 -0.0523
4.0443 -4.9916 0.9890 -0.3819 0.1991 -0.0272
4.9946 -0.9960 -1.0009 -0.0965 0.0154 0.1153

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43854
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.318
_diffrn_reflns_theta_min         2.317
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(5)
_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 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      6.00  48.00   0.50    1.48    --   25.84  77.00  30.00   84
  2  ω     69.00  97.00   0.50    1.48    --   25.84  77.00  30.00   56
  3  ω     53.00  79.00   0.50    1.48    --   25.84 156.00   6.00   52
  4  ω      2.00  97.00   0.50    1.48    --   25.84  77.00 -90.00  190
  5  ω     46.00  85.00   0.50    1.48    --   25.84 178.00 -30.00   78
  6  ω     39.00  90.00   0.50    1.48    --   25.84 178.00  90.00  102
  7  ω    -89.00 -63.00   0.50    1.48    --  -25.84 -77.00  90.00   52
  8  ω    -43.00  -7.00   0.50    3.00    --  -25.84 -77.00  90.00   72
  9  ω      8.00  51.00   0.50    3.00    --   25.84-120.00 126.00   86
 10  ω     64.00  91.00   0.50    3.00    --   25.84-156.00 -29.00   54
 11  ω     20.00  60.00   0.50    3.00    --   25.84 -99.00-180.00   80
 12  ω    -15.00  11.00   0.50    3.00    --   25.84 -99.00-180.00   52
 13  ω     40.00  66.00   0.50    3.00    --   25.84-156.00 -29.00   52
 14  ω    -66.00  -2.00   0.50    3.00    --  -25.84 -77.00-180.00  128
 15  ω    -53.00 -14.00   0.50    3.00    --  -25.84 -38.00 -60.00   78
 16  ω    -40.00  11.00   0.50    3.00    --  -25.84  38.00 150.00  102
 17  ω    -96.00 -44.00   0.50    3.00    --  -25.84 -57.00 120.00  104
 18  ω    -98.00 -72.00   0.50    3.00    --  -25.84 -38.00 -60.00   52
 19  ω     39.00  97.00   0.50    3.00    --   25.84 178.00  60.00  116
 20  ω     64.00  96.00   0.50    3.00    --   25.84 178.00  30.00   64
 21  ω     55.00  90.00   0.50    3.00    --   25.84 178.00 150.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0005378000
_diffrn_orient_matrix_UB_12      0.0806711000
_diffrn_orient_matrix_UB_13      0.0188150000
_diffrn_orient_matrix_UB_21      0.0129144000
_diffrn_orient_matrix_UB_22      -0.0164492000
_diffrn_orient_matrix_UB_23      0.0654461000
_diffrn_orient_matrix_UB_31      0.0164788000
_diffrn_orient_matrix_UB_32      0.0102532000
_diffrn_orient_matrix_UB_33      -0.0431914000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.955
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                11597
_reflns_number_total             12144
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_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       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.573
_refine_diff_density_min         -1.861
_refine_diff_density_rms         0.207
_refine_ls_abs_structure_details 
;
 Flack x determined using 5185 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(5)
_refine_ls_extinction_coef       0.00077(4)
_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   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         12144
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0291
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0328P)²+9.8765P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0714
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.497(6)
 0.503(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3. Restrained planarity
 I4_4, Pb1_4, I1_4, I3_4, I2_4
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(Pb1_4) = Uanis(Pb1_3)
Uanis(I1_3) = Uanis(I4_4)
Uanis(I2_3) = Uanis(I2_4)
Uanis(I4_3) = Uanis(I1_4)
Uanis(I3_4) = Uanis(I2_3)
Uanis(I3_3) = Uanis(I2_4)
5. Rigid body (RIGU) restrains
 C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1, Cl1_1, N9_1
 C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2, Cl1_2, N9_2
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0004
6. Same fragment restrains
{I1_4, I2_4, I3_4, I4_4, Pb1_4}
as
{I1_3, I2_3, I3_3, I4_3, Pb1_3} sigma for 1-2: 0.0002 1-3: 0.0004
{C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2, Cl1_2, N9_2}
as
{C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1, Cl1_1, N9_1} sigma for 1-2:
0.0002 1-3: 0.0004
7. Others
 Sof(I1)=Sof(I2)=Sof(I3)=Sof(I4)=Sof(Pb1)=1-FVAR(1)
 Sof(I1)=Sof(I2)=Sof(I3)=Sof(I4)=Sof(Pb1)=FVAR(1)
8.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B)
8.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C2(H2), C4(H4), C5(H5), C6(H6)
8.c Idealised Me refined as rotating group:
 N9(H9A,H9B,H9C), N9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1_1 C 0.23963(14) 0.9165(4) 0.2268(5) 0.0172(8) Uani 1 1 d D . . A 1
C2_1 C 0.26559(14) 0.8937(5) 0.3540(5) 0.0173(8) Uani 1 1 d D . . A 1
H2_1 H 0.273723 0.978223 0.415226 0.021 Uiso 1 1 calc R U . A 1
C3_1 C 0.27948(14) 0.7452(5) 0.3901(5) 0.0156(10) Uani 1 1 d D . . A 1
C4_1 C 0.26775(16) 0.6195(5) 0.2941(5) 0.0196(9) Uani 1 1 d D . . A 1
H4_1 H 0.276746 0.518979 0.317678 0.024 Uiso 1 1 calc R U . A 1
C5_1 C 0.24272(16) 0.6456(5) 0.1641(6) 0.0212(9) Uani 1 1 d D . . A 1
H5_1 H 0.235443 0.562400 0.099904 0.025 Uiso 1 1 calc R U . A 1
C6_1 C 0.22846(17) 0.7938(5) 0.1288(5) 0.0216(9) Uani 1 1 d D . . A 1
H6_1 H 0.211757 0.811139 0.041405 0.026 Uiso 1 1 calc R U . A 1
C7_1 C 0.30709(12) 0.7209(5) 0.5323(4) 0.0200(9) Uani 1 1 d D . . A 1
H7A_1 H 0.306835 0.611285 0.560705 0.024 Uiso 1 1 calc R U . A 1
H7B_1 H 0.297580 0.780958 0.615029 0.024 Uiso 1 1 calc R U . A 1
C8_1 C 0.34938(12) 0.7700(7) 0.5104(6) 0.0187(10) Uani 1 1 d D . . A 1
H8A_1 H 0.349714 0.878890 0.479757 0.022 Uiso 1 1 calc R U . A 1
H8B_1 H 0.365455 0.759813 0.606096 0.022 Uiso 1 1 calc R U . A 1
Cl1_1 Cl 0.21959(6) 1.10210(19) 0.1918(2) 0.0235(3) Uani 1 1 d D . . A 1
N9_1 N 0.36640(13) 0.6715(7) 0.3925(6) 0.0157(10) Uani 1 1 d D . . A 1
H9A_1 H 0.354990 0.696045 0.301109 0.019 Uiso 1 1 calc R U . A 1
H9B_1 H 0.362120 0.570987 0.411601 0.019 Uiso 1 1 calc R U . A 1
H9C_1 H 0.392253 0.688735 0.394540 0.019 Uiso 1 1 calc R U . A 1
C1_2 C 0.64682(14) 0.0864(4) 0.2809(5) 0.0173(8) Uani 1 1 d D . . B 1
C2_2 C 0.62087(14) 0.1073(5) 0.1534(5) 0.0170(8) Uani 1 1 d D . . B 1
H2_2 H 0.613200 0.022270 0.092138 0.020 Uiso 1 1 calc R U . B 1
C3_2 C 0.60629(14) 0.2548(5) 0.1169(5) 0.0168(10) Uani 1 1 d D . . B 1
C4_2 C 0.61778(16) 0.3817(5) 0.2117(5) 0.0209(9) Uani 1 1 d D . . B 1
H4_2 H 0.608388 0.481599 0.187674 0.025 Uiso 1 1 calc R U . B 1
C5_2 C 0.64315(16) 0.3577(5) 0.3411(6) 0.0214(9) Uani 1 1 d D . . B 1
H5_2 H 0.650414 0.441900 0.404204 0.026 Uiso 1 1 calc R U . B 1
C6_2 C 0.65778(16) 0.2104(5) 0.3777(6) 0.0206(9) Uani 1 1 d D . . B 1
H6_2 H 0.674586 0.194388 0.465036 0.025 Uiso 1 1 calc R U . B 1
C7_2 C 0.57797(12) 0.2764(5) -0.0238(4) 0.0204(9) Uani 1 1 d D . . B 1
H7A_2 H 0.578591 0.183756 -0.086927 0.024 Uiso 1 1 calc R U . B 1
H7B_2 H 0.586622 0.364361 -0.081962 0.024 Uiso 1 1 calc R U . B 1
C8_2 C 0.53568(12) 0.3053(6) 0.0150(6) 0.0192(10) Uani 1 1 d D . . B 1
H8A_2 H 0.534426 0.403368 0.069588 0.023 Uiso 1 1 calc R U . B 1
H8B_2 H 0.518509 0.313483 -0.078208 0.023 Uiso 1 1 calc R U . B 1
Cl1_2 Cl 0.66706(6) -0.09847(19) 0.3181(2) 0.0251(3) Uani 1 1 d D . . B 1
N9_2 N 0.52165(15) 0.1757(6) 0.1102(6) 0.0163(10) Uani 1 1 d D . . B 1
H9A_2 H 0.496031 0.187915 0.120618 0.020 Uiso 1 1 calc R U . B 1
H9B_2 H 0.534999 0.177465 0.201416 0.020 Uiso 1 1 calc R U . B 1
H9C_2 H 0.525559 0.084425 0.065323 0.020 Uiso 1 1 calc R U . B 1
I1_3 I 0.35013(4) 0.26039(6) 0.48453(15) 0.01401(9) Uani 0.9804(8) 1 d D . P C
1
I2_3 I 0.44374(4) 0.43942(5) 0.19645(14) 0.01249(6) Uani 0.9804(8) 1 d D . P C
1
I3_3 I 0.53953(4) 0.22931(6) 0.52004(14) 0.01249(6) Uani 0.9804(8) 1 d D . P C
1
I4_3 I 0.44499(4) 0.06533(5) 0.81578(14) 0.01330(8) Uani 0.9804(8) 1 d D . P C
1
Pb1_3 Pb 0.44498(4) 0.24798(3) 0.50393(15) 0.00915(4) Uani 0.9804(8) 1 d D . P
C 1
I1_4 I 0.4498(2) -0.0519(6) 0.6974(6) 0.01330(8) Uani 0.0196(8) 1 d D . P C 2
I2_4 I 0.54173(11) 0.2693(10) 0.5288(7) 0.01249(6) Uani 0.0196(8) 1 d D . P C 2
I3_4 I 0.4467(2) 0.5876(6) 0.3134(6) 0.01249(6) Uani 0.0196(8) 1 d D . P C 2
I4_4 I 0.35500(11) 0.2625(10) 0.4844(7) 0.01401(9) Uani 0.0196(8) 1 d D . P C 2
Pb1_4 Pb 0.44832(11) 0.2682(4) 0.5052(3) 0.00915(4) Uani 0.0196(8) 1 d D . P C
2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1_1 C2_1 1.382(5) . ?
C1_1 C6_1 1.392(5) . ?
C1_1 Cl1_1 1.744(4) . ?
C2_1 H2_1 0.9300 . ?
C2_1 C3_1 1.383(5) . ?
C3_1 C4_1 1.405(5) . ?
C3_1 C7_1 1.516(5) . ?
C4_1 H4_1 0.9300 . ?
C4_1 C5_1 1.387(6) . ?
C5_1 H5_1 0.9300 . ?
C5_1 C6_1 1.383(6) . ?
C6_1 H6_1 0.9300 . ?
C7_1 H7A_1 0.9700 . ?
C7_1 H7B_1 0.9700 . ?
C7_1 C8_1 1.526(5) . ?
C8_1 H8A_1 0.9700 . ?
C8_1 H8B_1 0.9700 . ?
C8_1 N9_1 1.493(5) . ?
N9_1 H9A_1 0.8900 . ?
N9_1 H9B_1 0.8900 . ?
N9_1 H9C_1 0.8900 . ?
C1_2 C2_2 1.382(5) . ?
C1_2 C6_2 1.392(5) . ?
C1_2 Cl1_2 1.744(4) . ?
C2_2 H2_2 0.9300 . ?
C2_2 C3_2 1.383(5) . ?
C3_2 C4_2 1.405(5) . ?
C3_2 C7_2 1.516(5) . ?
C4_2 H4_2 0.9300 . ?
C4_2 C5_2 1.387(6) . ?
C5_2 H5_2 0.9300 . ?
C5_2 C6_2 1.383(6) . ?
C6_2 H6_2 0.9300 . ?
C7_2 H7A_2 0.9700 . ?
C7_2 H7B_2 0.9700 . ?
C7_2 C8_2 1.526(5) . ?
C8_2 H8A_2 0.9700 . ?
C8_2 H8B_2 0.9700 . ?
C8_2 N9_2 1.493(5) . ?
N9_2 H9A_2 0.8900 . ?
N9_2 H9B_2 0.8900 . ?
N9_2 H9C_2 0.8900 . ?
I1_3 Pb1_3 3.2175(7) . ?
I2_3 Pb1_3 3.1688(6) 2_564 ?
I2_3 Pb1_3 3.1656(7) . ?
I3_3 Pb1_3 3.2105(8) . ?
I4_3 Pb1_3 3.1514(6) 2 ?
I4_3 Pb1_3 3.1637(7) . ?
I1_4 Pb1_4 3.2175(8) . ?
I1_4 Pb1_4 3.289(5) 2 ?
I2_4 Pb1_4 3.1656(8) . ?
I3_4 Pb1_4 2.991(5) 2_564 ?
I3_4 Pb1_4 3.2105(8) . ?
I4_4 Pb1_4 3.1637(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2_1 C1_1 C6_1 121.4(4) . . ?
C2_1 C1_1 Cl1_1 119.0(3) . . ?
C6_1 C1_1 Cl1_1 119.6(3) . . ?
C1_1 C2_1 H2_1 120.0 . . ?
C1_1 C2_1 C3_1 119.9(3) . . ?
C3_1 C2_1 H2_1 120.0 . . ?
C2_1 C3_1 C4_1 119.3(3) . . ?
C2_1 C3_1 C7_1 119.5(3) . . ?
C4_1 C3_1 C7_1 121.2(4) . . ?
C3_1 C4_1 H4_1 120.0 . . ?
C5_1 C4_1 C3_1 119.9(4) . . ?
C5_1 C4_1 H4_1 120.0 . . ?
C4_1 C5_1 H5_1 119.6 . . ?
C6_1 C5_1 C4_1 120.8(4) . . ?
C6_1 C5_1 H5_1 119.6 . . ?
C1_1 C6_1 H6_1 120.7 . . ?
C5_1 C6_1 C1_1 118.6(4) . . ?
C5_1 C6_1 H6_1 120.7 . . ?
C3_1 C7_1 H7A_1 109.1 . . ?
C3_1 C7_1 H7B_1 109.1 . . ?
C3_1 C7_1 C8_1 112.4(3) . . ?
H7A_1 C7_1 H7B_1 107.8 . . ?
C8_1 C7_1 H7A_1 109.1 . . ?
C8_1 C7_1 H7B_1 109.1 . . ?
C7_1 C8_1 H8A_1 109.4 . . ?
C7_1 C8_1 H8B_1 109.4 . . ?
H8A_1 C8_1 H8B_1 108.0 . . ?
N9_1 C8_1 C7_1 111.0(3) . . ?
N9_1 C8_1 H8A_1 109.4 . . ?
N9_1 C8_1 H8B_1 109.4 . . ?
C8_1 N9_1 H9A_1 109.5 . . ?
C8_1 N9_1 H9B_1 109.5 . . ?
C8_1 N9_1 H9C_1 109.5 . . ?
H9A_1 N9_1 H9B_1 109.5 . . ?
H9A_1 N9_1 H9C_1 109.5 . . ?
H9B_1 N9_1 H9C_1 109.5 . . ?
C2_2 C1_2 C6_2 121.4(4) . . ?
C2_2 C1_2 Cl1_2 119.0(3) . . ?
C6_2 C1_2 Cl1_2 119.6(3) . . ?
C1_2 C2_2 H2_2 120.0 . . ?
C1_2 C2_2 C3_2 120.0(3) . . ?
C3_2 C2_2 H2_2 120.0 . . ?
C2_2 C3_2 C4_2 119.3(3) . . ?
C2_2 C3_2 C7_2 119.5(3) . . ?
C4_2 C3_2 C7_2 121.2(4) . . ?
C3_2 C4_2 H4_2 120.0 . . ?
C5_2 C4_2 C3_2 119.9(4) . . ?
C5_2 C4_2 H4_2 120.0 . . ?
C4_2 C5_2 H5_2 119.6 . . ?
C6_2 C5_2 C4_2 120.8(4) . . ?
C6_2 C5_2 H5_2 119.6 . . ?
C1_2 C6_2 H6_2 120.7 . . ?
C5_2 C6_2 C1_2 118.6(4) . . ?
C5_2 C6_2 H6_2 120.7 . . ?
C3_2 C7_2 H7A_2 109.1 . . ?
C3_2 C7_2 H7B_2 109.1 . . ?
C3_2 C7_2 C8_2 112.4(3) . . ?
H7A_2 C7_2 H7B_2 107.8 . . ?
C8_2 C7_2 H7A_2 109.1 . . ?
C8_2 C7_2 H7B_2 109.1 . . ?
C7_2 C8_2 H8A_2 109.4 . . ?
C7_2 C8_2 H8B_2 109.4 . . ?
H8A_2 C8_2 H8B_2 108.0 . . ?
N9_2 C8_2 C7_2 111.0(3) . . ?
N9_2 C8_2 H8A_2 109.4 . . ?
N9_2 C8_2 H8B_2 109.4 . . ?
C8_2 N9_2 H9A_2 109.5 . . ?
C8_2 N9_2 H9B_2 109.5 . . ?
C8_2 N9_2 H9C_2 109.5 . . ?
H9A_2 N9_2 H9B_2 109.5 . . ?
H9A_2 N9_2 H9C_2 109.5 . . ?
H9B_2 N9_2 H9C_2 109.5 . . ?
Pb1_3 I2_3 Pb1_3 153.59(2) . 2_564 ?
Pb1_3 I4_3 Pb1_3 151.37(2) 2 . ?
I2_3 Pb1_3 I1_3 89.82(2) . . ?
I2_3 Pb1_3 I1_3 86.669(19) 2_565 . ?
I2_3 Pb1_3 I2_3 91.348(9) . 2_565 ?
I2_3 Pb1_3 I3_3 90.240(19) . . ?
I2_3 Pb1_3 I3_3 94.415(19) 2_565 . ?
I3_3 Pb1_3 I1_3 178.91(2) . . ?
I4_3 Pb1_3 I1_3 89.36(2) . . ?
I4_3 Pb1_3 I1_3 92.573(18) 2_554 . ?
I4_3 Pb1_3 I2_3 178.97(3) 2_554 2_565 ?
I4_3 Pb1_3 I2_3 178.27(2) . . ?
I4_3 Pb1_3 I2_3 87.09(2) . 2_565 ?
I4_3 Pb1_3 I2_3 89.34(2) 2_554 . ?
I4_3 Pb1_3 I3_3 86.342(19) 2_554 . ?
I4_3 Pb1_3 I3_3 90.61(2) . . ?
I4_3 Pb1_3 I4_3 92.212(9) 2_554 . ?
Pb1_4 I1_4 Pb1_4 155.9(2) . 2 ?
Pb1_4 I3_4 Pb1_4 146.0(2) 2_564 . ?
I2_4 Pb1_4 I1_4 89.82(2) . . ?
I2_4 Pb1_4 I3_4 90.23(2) . . ?
I3_4 Pb1_4 I1_4 82.66(13) 2_565 . ?
I3_4 Pb1_4 I1_4 179.95(4) . . ?
I3_4 Pb1_4 I2_4 91.96(16) 2_565 . ?
I3_4 Pb1_4 I3_4 97.34(13) 2_565 . ?
I3_4 Pb1_4 I4_4 87.93(16) 2_565 . ?
I4_4 Pb1_4 I1_4 89.35(2) . . ?
I4_4 Pb1_4 I2_4 179.17(3) . . ?
I4_4 Pb1_4 I3_4 90.60(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
C1_1 C2_1 C3_1 C4_1 1.7(8) . . . . ?
C1_1 C2_1 C3_1 C7_1 -178.4(4) . . . . ?
C2_1 C1_1 C6_1 C5_1 2.5(8) . . . . ?
C2_1 C3_1 C4_1 C5_1 0.5(8) . . . . ?
C2_1 C3_1 C7_1 C8_1 -78.3(6) . . . . ?
C3_1 C4_1 C5_1 C6_1 -1.2(9) . . . . ?
C3_1 C7_1 C8_1 N9_1 -63.4(5) . . . . ?
C4_1 C3_1 C7_1 C8_1 101.6(5) . . . . ?
C4_1 C5_1 C6_1 C1_1 -0.2(9) . . . . ?
C6_1 C1_1 C2_1 C3_1 -3.2(8) . . . . ?
C7_1 C3_1 C4_1 C5_1 -179.5(5) . . . . ?
Cl1_1 C1_1 C2_1 C3_1 175.1(4) . . . . ?
Cl1_1 C1_1 C6_1 C5_1 -175.8(5) . . . . ?
C1_2 C2_2 C3_2 C4_2 -0.8(8) . . . . ?
C1_2 C2_2 C3_2 C7_2 179.7(4) . . . . ?
C2_2 C1_2 C6_2 C5_2 -2.1(8) . . . . ?
C2_2 C3_2 C4_2 C5_2 -0.7(9) . . . . ?
C2_2 C3_2 C7_2 C8_2 106.8(5) . . . . ?
C3_2 C4_2 C5_2 C6_2 0.8(9) . . . . ?
C3_2 C7_2 C8_2 N9_2 -56.5(6) . . . . ?
C4_2 C3_2 C7_2 C8_2 -72.6(7) . . . . ?
C4_2 C5_2 C6_2 C1_2 0.6(9) . . . . ?
C6_2 C1_2 C2_2 C3_2 2.3(8) . . . . ?
C7_2 C3_2 C4_2 C5_2 178.8(5) . . . . ?
Cl1_2 C1_2 C2_2 C3_2 -176.2(4) . . . . ?
Cl1_2 C1_2 C6_2 C5_2 176.3(4) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id 3Cl-PEA
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.282
_oxdiff_exptl_absorpt_empirical_full_min 0.789
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.497(6)
2 0.503(6)

####################################################################### 
# 
# 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_3br-pea
_database_code_depnum_ccdc_archive 'CCDC 1987208'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2020-02-28 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT112_3br-pea             
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem C 91 %Fit
RESPONSE: The diffraction patterns have weak satellite
reflections. An larger cell with C2 symmetry element was 
foundbut the non-modulated structure provides the essential
features of the structure.
;
# end Validation Reply Form

_audit_creation_date             2020-02-27
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6020)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
mtremblay6@gatech.edu
john.bacsa@emory.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H11 Br N)'
_chemical_formula_sum            'C16 H22 Br2 I4 N2 Pb'
_chemical_formula_weight         1116.96
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33  H44  Br4  I8  N3  Pb2  '
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'
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      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   8.65320(10)
_cell_length_b                   8.65570(10)
_cell_length_c                   17.9336(2)
_cell_angle_alpha                86.6110(10)
_cell_angle_beta                 79.4250(10)
_cell_angle_gamma                89.7100(10)
_cell_volume                     1318.07(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15113
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4580
_cell_measurement_theta_min      3.3330
_shelx_estimated_absorpt_T_max   0.438
_shelx_estimated_absorpt_T_min   0.148
_exptl_absorpt_coefficient_mu    14.120
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.112
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.814
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0350
0 1 0 0.1132
3 2 0 0.0754
0 0 1 0.0350
-3 -2 0 0.0946
0 -1 0 0.1132
-1 4 2 0.1280
-1 -1 2 0.0832
-1 1 3 0.0673
2 2 4 0.0843
1 -1 2 0.0579
0 -1 0 0.1224
1 1 -2 0.0639
-3 2 -1 0.1052
-3 2 4 0.0885
0 1 3 0.0391
0 -2 -3 0.1184

_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.07
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0011 -0.0008 -0.5004 -0.0013 -0.0136 0.0148
-0.4967 0.5033 -0.2460 0.0562 -0.0062 0.0200
3.0002 1.9681 -0.0265 -0.1043 0.1772 0.2144
0.0011 0.0008 0.5004 0.0013 0.0136 -0.0148
-2.5046 -2.4723 -0.2279 0.0467 -0.1846 -0.2196
0.4967 -0.5033 0.2460 -0.0562 0.0062 -0.0200
-0.9736 4.0051 2.0091 0.2612 0.1641 0.1401
-0.9971 -0.9856 2.0103 0.0242 -0.0166 -0.1500
-0.9854 1.0123 3.0105 0.1216 0.0829 -0.0635
1.5156 2.4873 3.7390 0.0288 0.2450 0.0833
0.5012 -0.5001 2.2474 -0.0510 0.0607 -0.0792
0.4956 -0.5041 -0.2544 -0.0575 -0.0074 -0.0052
0.9971 0.9856 -2.0103 -0.0242 0.0166 0.1500
-2.9836 2.0227 -0.9752 0.2913 -0.0599 0.0473
-2.9735 2.0300 3.5280 0.3030 0.0628 -0.0859
-0.4899 0.5082 2.7561 0.0641 0.0755 -0.0688
0.4841 -1.5071 -3.2563 -0.1128 -0.1253 0.0255

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24825
_diffrn_reflns_point_group_measured_fraction_full 0.761
_diffrn_reflns_point_group_measured_fraction_max 0.680
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.482
_diffrn_reflns_theta_min         2.357
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_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 0.956
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -24.00   2.00   0.25    1.00    --   -0.16 -56.00  13.00  104
  2  ω    -25.00  33.00   0.25    5.00    --  -40.66 -99.00 -30.00  232
  3  ω    -26.00  33.00   0.25    5.00    --  -40.66 -99.00 -60.00  236
  4  ω    -43.00  45.00   0.25    5.00    --   40.35 -56.00  13.00  352
  5  ω      0.00  39.00   0.25    5.00    --   40.35 -38.00-120.00  156
  6  ω    -26.00  68.00   0.25    5.00    --   40.35 -99.00-120.00  376
  7  ω    -26.00  77.00   0.25    5.00    --   40.35 -99.00-180.00  412
  8  ω     62.00  88.00   0.25    5.00    --   40.35  77.00  30.00  104
  9  ω     88.00 113.00   0.25    5.00    --   40.35 125.00 -30.00  100
 10  ω     71.00 127.00   0.25    5.00    --   40.35 125.00  30.00  224
 11  ω     71.00 123.00   0.25    5.00    --   40.35 125.00 120.00  208
 12  ω     21.00  47.00   0.25    1.00    --   -0.16  56.00 155.00  104
 13  ω      7.00  32.00   0.25    5.00    --   40.35  56.00 155.00  100
 14  ω      5.00  31.00   0.25    5.00    --   40.35  77.00  30.00  104
 15  ω    -44.00 -19.00   0.25    5.00    --  -40.66  56.00 155.00  100
 16  ω    -63.00 -36.00   0.25    1.00    --   -0.16 -56.00  13.00  108
 17  ω    -75.00 -49.00   0.25    5.00    --   40.35 -56.00  13.00  104
 18  ω    -75.00  39.00   0.25    5.00    --   40.35 -38.00 -90.00  456
 19  ω     37.00  87.00   0.25    1.00    --   -0.16-178.00 150.00  200
 20  ω    -22.00  62.00   0.25    5.00    --   40.35 -99.00 150.00  336
 21  ω    -55.00  38.00   0.25    5.00    --   40.35 -38.00 150.00  372
 22  ω    -73.00 -10.00   0.25    5.00    --  -40.66 -56.00  13.00  252
 23  ω    -70.00  -6.00   0.25    5.00    --   40.35 -38.00-120.00  256
 24  ω   -100.00 -69.00   0.25    1.00    --   -0.16 -56.00  13.00  124
 25  ω   -115.00  35.00   0.25    1.00    --   -0.16 -38.00-150.00  600
 26  ω     71.00 122.00   0.25    5.00    --   40.35 125.00-120.00  204
 27  ω   -115.00 -90.00   0.25    1.00    --   -0.16-178.00 150.00  100
 28  ω   -145.00-109.00   0.25    5.00    --  -40.66 -99.00 120.00  144
 29  ω   -149.00-108.00   0.25    5.00    --  -40.66 -99.00 -30.00  164
 30  ω   -129.00-104.00   0.25    5.00    --  -40.66 -99.00-150.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0660923000
_diffrn_orient_matrix_UB_12      0.0478105000
_diffrn_orient_matrix_UB_13      0.0026783000
_diffrn_orient_matrix_UB_21      0.0356578000
_diffrn_orient_matrix_UB_22      0.0360614000
_diffrn_orient_matrix_UB_23      0.0270919000
_diffrn_orient_matrix_UB_31      0.0331719000
_diffrn_orient_matrix_UB_32      0.0579696000
_diffrn_orient_matrix_UB_33      -0.0297416000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.423
_reflns_Friedel_fraction_full    0.522
_reflns_Friedel_fraction_max     0.405
_reflns_number_gt                10851
_reflns_number_total             11923
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.108
_refine_diff_density_min         -3.059
_refine_diff_density_rms         0.262
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.021(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         11923
_refine_ls_number_restraints     255
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0391
_refine_ls_restrained_S_all      1.158
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0584P)²+4.5953P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1146
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.979(4)
 0.021(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1A,H1B,H1C} of N1, {H1A,H1B,H1C} of N1, {H1A,H1B,H1C} of
  N1, All C(H,H) groups
 At 1.5 times of:
  {H1A,H1B,H1C} of N1
3. Uiso/Uaniso restraints and constraints
Uanis(I2) = Uanis(I1)
4. Rigid body (RIGU) restrains
 Br1_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1, N1_1
 Br1_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2, N1_2
 Br1_3, C1_3, C2_3, C3_3, C4_3, C5_3, C6_3, C7_3, C8_3, N1_3
 Br1_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4, C7_4, C8_4, N1_4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Br1_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4, C7_4, C8_4, H1A_4, H1B_4, H1C_4,
 H2_4, H4_4, H5_4, H6_4, H7A_4, H7B_4, H8A_4, H8B_4, N1_4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(I2)=Sof(I4)=Sof(I10)=Sof(I12)=1-FVAR(1)
 Sof(I1)=Sof(I3)=Sof(I5)=Sof(I6)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B),
 C7(H7A,H7B), C8(H8A,H8B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C2(H2), C4(H4), C5(H5), C6(H6), C2(H2),
 C4(H4), C5(H5), C6(H6), C2(H2), C4(H4), C5(H5), C6(H6)
6.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N1(H1A,H1B,H1C), N1(H1A,H1B,H1C), N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.19879(15) 0.60502(15) 0.50011(8) 0.01398(16) Uani 0.7534(10) 1 d . . P A
1
I2 I 0.0717(5) 0.4770(6) 0.4960(3) 0.01398(16) Uani 0.2466(10) 1 d . . P A 2
I3 I 0.06715(14) 1.09681(14) 0.50070(7) 0.01134(16) Uani 0.7534(10) 1 d . . P A
1
I4 I 0.6995(6) 0.1048(7) 0.4956(3) 0.0237(8) Uani 0.2466(10) 1 d . . P A 2
I5 I 0.69076(14) 0.47381(14) 0.49981(7) 0.01145(16) Uani 0.7534(10) 1 d . . P A
1
I6 I 0.57178(14) -0.02185(14) 0.50015(7) 0.00993(16) Uani 0.7534(10) 1 d . . P
A 1
I7 I 0.32300(8) 0.25688(9) 0.68177(4) 0.0188(2) Uani 1 1 d . . . . .
I8 I 0.46152(9) 0.32200(8) 0.31656(4) 0.0185(2) Uani 1 1 d . . . . .
I9 I -0.17511(8) 0.77549(9) 0.68225(4) 0.0188(2) Uani 1 1 d . . . . .
I10 I 0.5676(6) 0.5967(6) 0.4962(3) 0.0189(6) Uani 0.2466(10) 1 d . . P A 2
I11 I -0.05833(9) 0.82050(9) 0.31702(4) 0.0187(2) Uani 1 1 d . . . . .
I12 I 0.1915(6) 0.9729(6) 0.4951(3) 0.0186(6) Uani 0.2466(10) 1 d . . P A 2
Pb1 Pb 0.37852(5) 0.28787(5) 0.49913(3) 0.01083(9) Uani 1 1 d . . . . .
Pb2 Pb -0.11804(5) 0.78440(5) 0.49957(3) 0.01109(9) Uani 1 1 d . . . . .
Br1_1 Br -0.27946(16) 0.06577(17) 0.05484(8) 0.0301(3) Uani 1 1 d . . . B 1
C1_1 C 0.0033(14) 0.2699(13) 0.1855(6) 0.0210(18) Uani 1 1 d . . . B 1
C2_1 C -0.1278(13) 0.2270(13) 0.1540(6) 0.0188(17) Uani 1 1 d . . . B 1
H2_1 H -0.227201 0.274284 0.168541 0.023 Uiso 1 1 calc R U . B 1
C3_1 C -0.1072(15) 0.1148(13) 0.1016(7) 0.0221(19) Uani 1 1 d . . . B 1
C4_1 C 0.0343(16) 0.0399(14) 0.0789(6) 0.025(2) Uani 1 1 d . . . B 1
H4_1 H 0.044278 -0.036981 0.042630 0.030 Uiso 1 1 calc R U . B 1
C5_1 C 0.1623(16) 0.0824(15) 0.1117(7) 0.026(2) Uani 1 1 d . . . B 1
H5_1 H 0.260089 0.031456 0.098260 0.032 Uiso 1 1 calc R U . B 1
C6_1 C 0.1486(16) 0.1980(16) 0.1636(8) 0.026(2) Uani 1 1 d . . . B 1
H6_1 H 0.237260 0.227669 0.183951 0.031 Uiso 1 1 calc R U . B 1
C7_1 C -0.0119(15) 0.3971(14) 0.2407(7) 0.025(2) Uani 1 1 d . . . B 1
H7A_1 H -0.111194 0.453461 0.239143 0.030 Uiso 1 1 calc R U . B 1
H7B_1 H 0.076036 0.471444 0.224492 0.030 Uiso 1 1 calc R U . B 1
C8_1 C -0.0108(19) 0.3353(18) 0.3229(7) 0.035(3) Uani 1 1 d . . . B 1
H8A_1 H 0.091223 0.284759 0.325069 0.042 Uiso 1 1 calc R U . B 1
H8B_1 H -0.020668 0.423498 0.356160 0.042 Uiso 1 1 calc R U . B 1
N1_1 N -0.1373(17) 0.2251(16) 0.3516(7) 0.043(3) Uani 1 1 d . . . B 1
H1A_1 H -0.107609 0.129261 0.336262 0.052 Uiso 1 1 calc R U . B 1
H1B_1 H -0.224974 0.254309 0.333202 0.052 Uiso 1 1 calc R U . B 1
H1C_1 H -0.158457 0.222664 0.403265 0.052 Uiso 1 1 calc R U . B 1
Br1_2 Br 0.21603(16) 0.56568(16) 0.05458(7) 0.0291(3) Uani 1 1 d . . . C 1
C1_2 C 0.5012(14) 0.7686(12) 0.1832(6) 0.0186(17) Uani 1 1 d . . . C 1
C2_2 C 0.3720(13) 0.7247(13) 0.1535(6) 0.0188(18) Uani 1 1 d . . . C 1
H2_2 H 0.272519 0.770974 0.169237 0.023 Uiso 1 1 calc R U . C 1
C3_2 C 0.3897(14) 0.6132(13) 0.1009(6) 0.0207(18) Uani 1 1 d . . . C 1
C4_2 C 0.5330(15) 0.5383(14) 0.0783(6) 0.023(2) Uani 1 1 d . . . C 1
H4_2 H 0.542895 0.461188 0.042153 0.028 Uiso 1 1 calc R U . C 1
C5_2 C 0.6589(15) 0.5797(14) 0.1098(7) 0.024(2) Uani 1 1 d . . . C 1
H5_2 H 0.756135 0.527692 0.096603 0.029 Uiso 1 1 calc R U . C 1
C6_2 C 0.6467(15) 0.6969(15) 0.1611(7) 0.022(2) Uani 1 1 d . . . C 1
H6_2 H 0.735970 0.727503 0.180696 0.026 Uiso 1 1 calc R U . C 1
C7_2 C 0.4847(16) 0.8947(14) 0.2380(7) 0.027(2) Uani 1 1 d . . . C 1
H7A_2 H 0.417510 0.977335 0.220756 0.032 Uiso 1 1 calc R U . C 1
H7B_2 H 0.589602 0.940204 0.237446 0.032 Uiso 1 1 calc R U . C 1
C8_2 C 0.413(2) 0.8383(19) 0.3195(8) 0.035(3) Uani 1 1 d . . . C 1
H8A_2 H 0.398734 0.927459 0.352139 0.042 Uiso 1 1 calc R U . C 1
H8B_2 H 0.308654 0.791521 0.320397 0.042 Uiso 1 1 calc R U . C 1
N1_2 N 0.5142(18) 0.7246(15) 0.3493(7) 0.037(3) Uani 1 1 d . . . C 1
H1A_2 H 0.514808 0.636307 0.324033 0.056 Uiso 1 1 calc R U . C 1
H1B_2 H 0.477212 0.703125 0.399652 0.056 Uiso 1 1 calc R U . C 1
H1C_2 H 0.613732 0.763117 0.342726 0.056 Uiso 1 1 calc R U . C 1
Br1_3 Br 0.43846(16) -0.09695(17) 0.94479(8) 0.0305(3) Uani 1 1 d . . . . .
C1_3 C 0.7044(12) 0.2505(14) 0.8140(6) 0.0180(17) Uani 1 1 d . . . . .
C2_3 C 0.6477(12) 0.1063(14) 0.8452(6) 0.0189(18) Uani 1 1 d . . . . .
H2_3 H 0.703368 0.014723 0.830715 0.023 Uiso 1 1 calc R U . . .
C3_3 C 0.5085(13) 0.0987(15) 0.8979(7) 0.0226(19) Uani 1 1 d . . . . .
C4_3 C 0.4242(13) 0.2322(16) 0.9197(6) 0.024(2) Uani 1 1 d . . . . .
H4_3 H 0.329051 0.224858 0.955872 0.029 Uiso 1 1 calc R U . . .
C5_3 C 0.4803(14) 0.3728(16) 0.8883(7) 0.026(2) Uani 1 1 d . . . . .
H5_3 H 0.423570 0.464221 0.902084 0.031 Uiso 1 1 calc R U . . .
C6_3 C 0.6230(14) 0.3825(16) 0.8354(7) 0.022(2) Uani 1 1 d . . . . .
H6_3 H 0.663063 0.480744 0.814349 0.026 Uiso 1 1 calc R U . . .
C7_3 C 0.8608(13) 0.2623(16) 0.7588(7) 0.025(2) Uani 1 1 d . . . . .
H7A_3 H 0.926838 0.342968 0.774512 0.030 Uiso 1 1 calc R U . . .
H7B_3 H 0.916721 0.162473 0.760825 0.030 Uiso 1 1 calc R U . . .
C8_3 C 0.8387(16) 0.3020(19) 0.6777(7) 0.033(3) Uani 1 1 d . . . . .
H8A_3 H 0.789092 0.405010 0.675363 0.040 Uiso 1 1 calc R U . . .
H8B_3 H 0.943251 0.308823 0.644148 0.040 Uiso 1 1 calc R U . . .
N1_3 N 0.7432(14) 0.1906(17) 0.6490(7) 0.039(3) Uani 1 1 d . . . . .
H1A_3 H 0.755343 0.205544 0.597635 0.047 Uiso 1 1 calc R U . . .
H1B_3 H 0.640334 0.203343 0.670252 0.047 Uiso 1 1 calc R U . . .
H1C_3 H 0.773750 0.093089 0.661252 0.047 Uiso 1 1 calc R U . . .
Br1_4 Br -0.06334(16) 0.40088(17) 0.94307(7) 0.0295(3) Uani 1 1 d . . . . .
C1_4 C 0.2058(13) 0.7500(15) 0.8149(7) 0.0205(18) Uani 1 1 d . . . . .
C2_4 C 0.1462(13) 0.6075(14) 0.8444(6) 0.0196(18) Uani 1 1 d . . . . .
H2_4 H 0.200764 0.515926 0.828896 0.024 Uiso 1 1 calc R U . . .
C3_4 C 0.0069(13) 0.5977(16) 0.8968(6) 0.0228(19) Uani 1 1 d . . . . .
C4_4 C -0.0767(14) 0.7300(17) 0.9205(7) 0.026(2) Uani 1 1 d . . . . .
H4_4 H -0.170673 0.721796 0.957454 0.031 Uiso 1 1 calc R U . . .
C5_4 C -0.0200(14) 0.8731(17) 0.8893(7) 0.026(2) Uani 1 1 d . . . . .
H5_4 H -0.077760 0.964062 0.902795 0.031 Uiso 1 1 calc R U . . .
C6_4 C 0.1244(15) 0.8837(16) 0.8373(7) 0.023(2) Uani 1 1 d . . . . .
H6_4 H 0.165932 0.982284 0.817699 0.028 Uiso 1 1 calc R U . . .
C7_4 C 0.3604(13) 0.7638(16) 0.7613(7) 0.024(2) Uani 1 1 d . . . . .
H7A_4 H 0.436200 0.690414 0.778816 0.029 Uiso 1 1 calc R U . . .
H7B_4 H 0.402929 0.869839 0.760883 0.029 Uiso 1 1 calc R U . . .
C8_4 C 0.3408(18) 0.728(2) 0.6795(9) 0.038(3) Uani 1 1 d . . . . .
H8A_4 H 0.445426 0.724676 0.646259 0.045 Uiso 1 1 calc R U . . .
H8B_4 H 0.289764 0.625776 0.680542 0.045 Uiso 1 1 calc R U . . .
N1_4 N 0.2442(15) 0.849(2) 0.6488(8) 0.045(3) Uani 1 1 d . . . . .
H1A_4 H 0.244170 0.833940 0.598947 0.054 Uiso 1 1 calc R U . . .
H1B_4 H 0.284879 0.943578 0.653165 0.054 Uiso 1 1 calc R U . . .
H1C_4 H 0.143884 0.842186 0.675309 0.054 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
I1 Pb1 3.1476(15) . ?
I1 Pb2 3.1452(15) . ?
I2 Pb1 3.120(4) . ?
I2 Pb2 3.117(4) . ?
I3 Pb1 3.1634(15) 1_565 ?
I3 Pb2 3.1533(15) . ?
I4 Pb1 3.183(5) . ?
I4 Pb2 3.188(5) 1_645 ?
I5 Pb1 3.1542(14) . ?
I5 Pb2 3.1631(15) 1_655 ?
I6 Pb1 3.1535(15) . ?
I6 Pb2 3.1564(15) 1_645 ?
I7 Pb1 3.2174(8) . ?
I8 Pb1 3.2167(8) . ?
I9 Pb2 3.2186(8) . ?
I10 Pb1 3.134(5) . ?
I10 Pb2 3.188(5) 1_655 ?
I11 Pb2 3.2159(8) . ?
I12 Pb1 3.189(5) 1_565 ?
I12 Pb2 3.129(5) . ?
Br1_1 C3_1 1.901(13) . ?
C1_1 C2_1 1.417(17) . ?
C1_1 C6_1 1.401(18) . ?
C1_1 C7_1 1.513(17) . ?
C2_1 H2_1 0.9500 . ?
C2_1 C3_1 1.379(15) . ?
C3_1 C4_1 1.388(17) . ?
C4_1 H4_1 0.9500 . ?
C4_1 C5_1 1.41(2) . ?
C5_1 H5_1 0.9500 . ?
C5_1 C6_1 1.397(19) . ?
C6_1 H6_1 0.9500 . ?
C7_1 H7A_1 0.9900 . ?
C7_1 H7B_1 0.9900 . ?
C7_1 C8_1 1.539(19) . ?
C8_1 H8A_1 0.9900 . ?
C8_1 H8B_1 0.9900 . ?
C8_1 N1_1 1.456(19) . ?
N1_1 H1A_1 0.9100 . ?
N1_1 H1B_1 0.9100 . ?
N1_1 H1C_1 0.9100 . ?
Br1_2 C3_2 1.903(12) . ?
C1_2 C2_2 1.387(16) . ?
C1_2 C6_2 1.402(17) . ?
C1_2 C7_2 1.499(16) . ?
C2_2 H2_2 0.9500 . ?
C2_2 C3_2 1.378(15) . ?
C3_2 C4_2 1.399(17) . ?
C4_2 H4_2 0.9500 . ?
C4_2 C5_2 1.375(19) . ?
C5_2 H5_2 0.9500 . ?
C5_2 C6_2 1.400(18) . ?
C6_2 H6_2 0.9500 . ?
C7_2 H7A_2 0.9900 . ?
C7_2 H7B_2 0.9900 . ?
C7_2 C8_2 1.531(19) . ?
C8_2 H8A_2 0.9900 . ?
C8_2 H8B_2 0.9900 . ?
C8_2 N1_2 1.46(2) . ?
N1_2 H1A_2 0.9100 . ?
N1_2 H1B_2 0.9100 . ?
N1_2 H1C_2 0.9100 . ?
Br1_3 C3_3 1.897(13) . ?
C1_3 C2_3 1.391(16) . ?
C1_3 C6_3 1.375(17) . ?
C1_3 C7_3 1.523(15) . ?
C2_3 H2_3 0.9500 . ?
C2_3 C3_3 1.387(15) . ?
C3_3 C4_3 1.401(17) . ?
C4_3 H4_3 0.9500 . ?
C4_3 C5_3 1.363(19) . ?
C5_3 H5_3 0.9500 . ?
C5_3 C6_3 1.413(16) . ?
C6_3 H6_3 0.9500 . ?
C7_3 H7A_3 0.9900 . ?
C7_3 H7B_3 0.9900 . ?
C7_3 C8_3 1.521(18) . ?
C8_3 H8A_3 0.9900 . ?
C8_3 H8B_3 0.9900 . ?
C8_3 N1_3 1.449(19) . ?
N1_3 H1A_3 0.9100 . ?
N1_3 H1B_3 0.9100 . ?
N1_3 H1C_3 0.9100 . ?
Br1_4 C3_4 1.902(13) . ?
C1_4 C2_4 1.377(16) . ?
C1_4 C6_4 1.393(18) . ?
C1_4 C7_4 1.498(15) . ?
C2_4 H2_4 0.9500 . ?
C2_4 C3_4 1.385(14) . ?
C3_4 C4_4 1.398(18) . ?
C4_4 H4_4 0.9500 . ?
C4_4 C5_4 1.38(2) . ?
C5_4 H5_4 0.9500 . ?
C5_4 C6_4 1.415(17) . ?
C6_4 H6_4 0.9500 . ?
C7_4 H7A_4 0.9900 . ?
C7_4 H7B_4 0.9900 . ?
C7_4 C8_4 1.56(2) . ?
C8_4 H8A_4 0.9900 . ?
C8_4 H8B_4 0.9900 . ?
C8_4 N1_4 1.48(2) . ?
N1_4 H1A_4 0.9100 . ?
N1_4 H1B_4 0.9100 . ?
N1_4 H1C_4 0.9100 . ?

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
Pb2 I1 Pb1 148.82(5) . . ?
Pb2 I2 Pb1 152.76(17) . . ?
Pb2 I3 Pb1 152.39(5) . 1_565 ?
Pb1 I4 Pb2 149.52(19) . 1_645 ?
Pb1 I5 Pb2 152.50(5) . 1_655 ?
Pb1 I6 Pb2 153.91(5) . 1_645 ?
Pb1 I10 Pb2 152.20(17) . 1_655 ?
Pb2 I12 Pb1 152.28(17) . 1_565 ?
I1 Pb1 I3 92.23(4) . 1_545 ?
I1 Pb1 I5 88.56(4) . . ?
I1 Pb1 I6 177.36(5) . . ?
I1 Pb1 I7 91.93(3) . . ?
I1 Pb1 I8 89.72(3) . . ?
I1 Pb1 I12 119.67(8) . 1_545 ?
I2 Pb1 I4 177.31(17) . . ?
I2 Pb1 I7 93.55(8) . . ?
I2 Pb1 I8 89.82(8) . . ?
I2 Pb1 I10 89.94(13) . . ?
I3 Pb1 I7 90.59(3) 1_545 . ?
I3 Pb1 I8 93.29(3) 1_545 . ?
I3 Pb1 I12 27.50(10) 1_545 1_545 ?
I4 Pb1 I7 88.57(9) . . ?
I4 Pb1 I8 87.99(9) . . ?
I5 Pb1 I3 178.93(5) . 1_545 ?
I5 Pb1 I7 88.66(3) . . ?
I5 Pb1 I8 87.44(3) . . ?
I5 Pb1 I12 151.75(8) . 1_545 ?
I6 Pb1 I3 90.32(4) . 1_545 ?
I6 Pb1 I5 88.89(4) . . ?
I6 Pb1 I7 87.38(3) . . ?
I6 Pb1 I8 90.80(3) . . ?
I6 Pb1 I12 62.90(10) . 1_545 ?
I8 Pb1 I7 175.73(3) . . ?
I10 Pb1 I4 88.37(13) . . ?
I10 Pb1 I7 91.01(9) . . ?
I10 Pb1 I8 86.35(9) . . ?
I12 Pb1 I7 91.18(9) 1_545 . ?
I12 Pb1 I8 91.43(9) 1_545 . ?
I1 Pb2 I3 88.65(4) . . ?
I1 Pb2 I4 149.23(9) . 1_465 ?
I1 Pb2 I5 92.24(4) . 1_455 ?
I1 Pb2 I6 177.44(5) . 1_465 ?
I1 Pb2 I9 89.17(3) . . ?
I1 Pb2 I10 119.71(9) . 1_455 ?
I1 Pb2 I11 92.53(3) . . ?
I2 Pb2 I9 91.89(8) . . ?
I2 Pb2 I11 91.47(8) . . ?
I2 Pb2 I12 90.05(12) . . ?
I3 Pb2 I4 60.60(11) . 1_465 ?
I3 Pb2 I5 179.00(5) . 1_455 ?
I3 Pb2 I6 88.80(4) . 1_465 ?
I3 Pb2 I9 86.92(3) . . ?
I3 Pb2 I10 151.62(8) . 1_455 ?
I3 Pb2 I11 89.25(3) . . ?
I4 Pb2 I9 90.43(9) 1_465 . ?
I4 Pb2 I11 86.14(9) 1_465 . ?
I5 Pb2 I4 118.51(10) 1_455 1_465 ?
I5 Pb2 I9 92.65(3) 1_455 . ?
I5 Pb2 I10 27.49(11) 1_455 1_455 ?
I5 Pb2 I11 91.15(3) 1_455 . ?
I6 Pb2 I4 28.25(11) 1_465 1_465 ?
I6 Pb2 I5 90.30(4) 1_465 1_455 ?
I6 Pb2 I9 90.35(3) 1_465 . ?
I6 Pb2 I10 62.83(10) 1_465 1_455 ?
I6 Pb2 I11 87.78(3) 1_465 . ?
I10 Pb2 I9 93.74(8) 1_455 . ?
I10 Pb2 I11 88.77(9) 1_455 . ?
I11 Pb2 I9 175.78(3) . . ?
I12 Pb2 I9 88.76(9) . . ?
I12 Pb2 I11 88.69(9) . . ?
C2_1 C1_1 C7_1 120.2(10) . . ?
C6_1 C1_1 C2_1 120.0(11) . . ?
C6_1 C1_1 C7_1 119.9(12) . . ?
C1_1 C2_1 H2_1 120.9 . . ?
C3_1 C2_1 C1_1 118.3(11) . . ?
C3_1 C2_1 H2_1 120.9 . . ?
C2_1 C3_1 Br1_1 118.3(9) . . ?
C2_1 C3_1 C4_1 123.6(12) . . ?
C4_1 C3_1 Br1_1 118.0(9) . . ?
C3_1 C4_1 H4_1 121.4 . . ?
C3_1 C4_1 C5_1 117.2(11) . . ?
C5_1 C4_1 H4_1 121.4 . . ?
C4_1 C5_1 H5_1 119.3 . . ?
C6_1 C5_1 C4_1 121.4(12) . . ?
C6_1 C5_1 H5_1 119.3 . . ?
C1_1 C6_1 H6_1 120.2 . . ?
C5_1 C6_1 C1_1 119.5(13) . . ?
C5_1 C6_1 H6_1 120.2 . . ?
C1_1 C7_1 H7A_1 109.0 . . ?
C1_1 C7_1 H7B_1 109.0 . . ?
C1_1 C7_1 C8_1 112.8(11) . . ?
H7A_1 C7_1 H7B_1 107.8 . . ?
C8_1 C7_1 H7A_1 109.0 . . ?
C8_1 C7_1 H7B_1 109.0 . . ?
C7_1 C8_1 H8A_1 109.0 . . ?
C7_1 C8_1 H8B_1 109.0 . . ?
H8A_1 C8_1 H8B_1 107.8 . . ?
N1_1 C8_1 C7_1 112.8(12) . . ?
N1_1 C8_1 H8A_1 109.0 . . ?
N1_1 C8_1 H8B_1 109.0 . . ?
C8_1 N1_1 H1A_1 109.5 . . ?
C8_1 N1_1 H1B_1 109.5 . . ?
C8_1 N1_1 H1C_1 109.5 . . ?
H1A_1 N1_1 H1B_1 109.5 . . ?
H1A_1 N1_1 H1C_1 109.5 . . ?
H1B_1 N1_1 H1C_1 109.5 . . ?
C2_2 C1_2 C6_2 120.0(11) . . ?
C2_2 C1_2 C7_2 119.6(11) . . ?
C6_2 C1_2 C7_2 120.4(11) . . ?
C1_2 C2_2 H2_2 120.4 . . ?
C3_2 C2_2 C1_2 119.3(11) . . ?
C3_2 C2_2 H2_2 120.4 . . ?
C2_2 C3_2 Br1_2 118.8(9) . . ?
C2_2 C3_2 C4_2 122.1(11) . . ?
C4_2 C3_2 Br1_2 119.0(9) . . ?
C3_2 C4_2 H4_2 121.0 . . ?
C5_2 C4_2 C3_2 118.1(11) . . ?
C5_2 C4_2 H4_2 121.0 . . ?
C4_2 C5_2 H5_2 119.3 . . ?
C4_2 C5_2 C6_2 121.3(11) . . ?
C6_2 C5_2 H5_2 119.3 . . ?
C1_2 C6_2 H6_2 120.4 . . ?
C5_2 C6_2 C1_2 119.2(12) . . ?
C5_2 C6_2 H6_2 120.4 . . ?
C1_2 C7_2 H7A_2 108.9 . . ?
C1_2 C7_2 H7B_2 108.9 . . ?
C1_2 C7_2 C8_2 113.2(11) . . ?
H7A_2 C7_2 H7B_2 107.8 . . ?
C8_2 C7_2 H7A_2 108.9 . . ?
C8_2 C7_2 H7B_2 108.9 . . ?
C7_2 C8_2 H8A_2 109.5 . . ?
C7_2 C8_2 H8B_2 109.5 . . ?
H8A_2 C8_2 H8B_2 108.0 . . ?
N1_2 C8_2 C7_2 110.9(13) . . ?
N1_2 C8_2 H8A_2 109.5 . . ?
N1_2 C8_2 H8B_2 109.5 . . ?
C8_2 N1_2 H1A_2 109.5 . . ?
C8_2 N1_2 H1B_2 109.5 . . ?
C8_2 N1_2 H1C_2 109.5 . . ?
H1A_2 N1_2 H1B_2 109.5 . . ?
H1A_2 N1_2 H1C_2 109.5 . . ?
H1B_2 N1_2 H1C_2 109.5 . . ?
C2_3 C1_3 C7_3 119.7(10) . . ?
C6_3 C1_3 C2_3 120.2(11) . . ?
C6_3 C1_3 C7_3 120.1(11) . . ?
C1_3 C2_3 H2_3 120.6 . . ?
C3_3 C2_3 C1_3 118.8(11) . . ?
C3_3 C2_3 H2_3 120.6 . . ?
C2_3 C3_3 Br1_3 118.6(9) . . ?
C2_3 C3_3 C4_3 121.5(11) . . ?
C4_3 C3_3 Br1_3 119.8(8) . . ?
C3_3 C4_3 H4_3 120.4 . . ?
C5_3 C4_3 C3_3 119.2(11) . . ?
C5_3 C4_3 H4_3 120.4 . . ?
C4_3 C5_3 H5_3 120.0 . . ?
C4_3 C5_3 C6_3 119.9(12) . . ?
C6_3 C5_3 H5_3 120.0 . . ?
C1_3 C6_3 C5_3 120.4(12) . . ?
C1_3 C6_3 H6_3 119.8 . . ?
C5_3 C6_3 H6_3 119.8 . . ?
C1_3 C7_3 H7A_3 109.2 . . ?
C1_3 C7_3 H7B_3 109.2 . . ?
H7A_3 C7_3 H7B_3 107.9 . . ?
C8_3 C7_3 C1_3 111.9(10) . . ?
C8_3 C7_3 H7A_3 109.2 . . ?
C8_3 C7_3 H7B_3 109.2 . . ?
C7_3 C8_3 H8A_3 108.8 . . ?
C7_3 C8_3 H8B_3 108.8 . . ?
H8A_3 C8_3 H8B_3 107.7 . . ?
N1_3 C8_3 C7_3 113.7(12) . . ?
N1_3 C8_3 H8A_3 108.8 . . ?
N1_3 C8_3 H8B_3 108.8 . . ?
C8_3 N1_3 H1A_3 109.5 . . ?
C8_3 N1_3 H1B_3 109.5 . . ?
C8_3 N1_3 H1C_3 109.5 . . ?
H1A_3 N1_3 H1B_3 109.5 . . ?
H1A_3 N1_3 H1C_3 109.5 . . ?
H1B_3 N1_3 H1C_3 109.5 . . ?
C2_4 C1_4 C6_4 119.7(11) . . ?
C2_4 C1_4 C7_4 120.9(11) . . ?
C6_4 C1_4 C7_4 119.4(11) . . ?
C1_4 C2_4 H2_4 120.0 . . ?
C1_4 C2_4 C3_4 120.0(11) . . ?
C3_4 C2_4 H2_4 120.0 . . ?
C2_4 C3_4 Br1_4 119.1(10) . . ?
C2_4 C3_4 C4_4 121.5(12) . . ?
C4_4 C3_4 Br1_4 119.2(8) . . ?
C3_4 C4_4 H4_4 120.6 . . ?
C5_4 C4_4 C3_4 118.8(11) . . ?
C5_4 C4_4 H4_4 120.6 . . ?
C4_4 C5_4 H5_4 120.1 . . ?
C4_4 C5_4 C6_4 119.8(12) . . ?
C6_4 C5_4 H5_4 120.1 . . ?
C1_4 C6_4 C5_4 120.2(13) . . ?
C1_4 C6_4 H6_4 119.9 . . ?
C5_4 C6_4 H6_4 119.9 . . ?
C1_4 C7_4 H7A_4 109.5 . . ?
C1_4 C7_4 H7B_4 109.5 . . ?
C1_4 C7_4 C8_4 110.6(11) . . ?
H7A_4 C7_4 H7B_4 108.1 . . ?
C8_4 C7_4 H7A_4 109.5 . . ?
C8_4 C7_4 H7B_4 109.5 . . ?
C7_4 C8_4 H8A_4 109.6 . . ?
C7_4 C8_4 H8B_4 109.6 . . ?
H8A_4 C8_4 H8B_4 108.1 . . ?
N1_4 C8_4 C7_4 110.2(13) . . ?
N1_4 C8_4 H8A_4 109.6 . . ?
N1_4 C8_4 H8B_4 109.6 . . ?
C8_4 N1_4 H1A_4 109.5 . . ?
C8_4 N1_4 H1B_4 109.5 . . ?
C8_4 N1_4 H1C_4 109.5 . . ?
H1A_4 N1_4 H1B_4 109.5 . . ?
H1A_4 N1_4 H1C_4 109.5 . . ?
H1B_4 N1_4 H1C_4 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1_1 C3_1 C4_1 C5_1 177.3(9) . . . . ?
C1_1 C2_1 C3_1 Br1_1 -176.4(8) . . . . ?
C1_1 C2_1 C3_1 C4_1 1.0(17) . . . . ?
C1_1 C7_1 C8_1 N1_1 -59.0(16) . . . . ?
C2_1 C1_1 C6_1 C5_1 -1.1(19) . . . . ?
C2_1 C1_1 C7_1 C8_1 108.1(13) . . . . ?
C2_1 C3_1 C4_1 C5_1 0.0(18) . . . . ?
C3_1 C4_1 C5_1 C6_1 -1.5(18) . . . . ?
C4_1 C5_1 C6_1 C1_1 2(2) . . . . ?
C6_1 C1_1 C2_1 C3_1 -0.4(17) . . . . ?
C6_1 C1_1 C7_1 C8_1 -74.0(15) . . . . ?
C7_1 C1_1 C2_1 C3_1 177.5(10) . . . . ?
C7_1 C1_1 C6_1 C5_1 -179.0(11) . . . . ?
Br1_2 C3_2 C4_2 C5_2 177.0(9) . . . . ?
C1_2 C2_2 C3_2 Br1_2 -175.1(8) . . . . ?
C1_2 C2_2 C3_2 C4_2 2.3(17) . . . . ?
C1_2 C7_2 C8_2 N1_2 62.9(17) . . . . ?
C2_2 C1_2 C6_2 C5_2 -0.9(18) . . . . ?
C2_2 C1_2 C7_2 C8_2 81.2(15) . . . . ?
C2_2 C3_2 C4_2 C5_2 -0.4(17) . . . . ?
C3_2 C4_2 C5_2 C6_2 -2.2(18) . . . . ?
C4_2 C5_2 C6_2 C1_2 2.9(19) . . . . ?
C6_2 C1_2 C2_2 C3_2 -1.6(17) . . . . ?
C6_2 C1_2 C7_2 C8_2 -99.7(15) . . . . ?
C7_2 C1_2 C2_2 C3_2 177.4(10) . . . . ?
C7_2 C1_2 C6_2 C5_2 -179.9(11) . . . . ?
Br1_3 C3_3 C4_3 C5_3 176.6(9) . . . . ?
C1_3 C2_3 C3_3 Br1_3 -176.2(8) . . . . ?
C1_3 C2_3 C3_3 C4_3 0.4(17) . . . . ?
C1_3 C7_3 C8_3 N1_3 -58.9(16) . . . . ?
C2_3 C1_3 C6_3 C5_3 -0.8(18) . . . . ?
C2_3 C1_3 C7_3 C8_3 108.0(13) . . . . ?
C2_3 C3_3 C4_3 C5_3 0.1(18) . . . . ?
C3_3 C4_3 C5_3 C6_3 -0.9(18) . . . . ?
C4_3 C5_3 C6_3 C1_3 1.3(19) . . . . ?
C6_3 C1_3 C2_3 C3_3 0.0(17) . . . . ?
C6_3 C1_3 C7_3 C8_3 -74.7(15) . . . . ?
C7_3 C1_3 C2_3 C3_3 177.2(11) . . . . ?
C7_3 C1_3 C6_3 C5_3 -178.1(11) . . . . ?
Br1_4 C3_4 C4_4 C5_4 176.7(9) . . . . ?
C1_4 C2_4 C3_4 Br1_4 -174.7(9) . . . . ?
C1_4 C2_4 C3_4 C4_4 0.3(17) . . . . ?
C1_4 C7_4 C8_4 N1_4 66.4(17) . . . . ?
C2_4 C1_4 C6_4 C5_4 -1.0(19) . . . . ?
C2_4 C1_4 C7_4 C8_4 80.0(15) . . . . ?
C2_4 C3_4 C4_4 C5_4 1.6(18) . . . . ?
C3_4 C4_4 C5_4 C6_4 -3.2(18) . . . . ?
C4_4 C5_4 C6_4 C1_4 2.9(19) . . . . ?
C6_4 C1_4 C2_4 C3_4 -0.6(17) . . . . ?
C6_4 C1_4 C7_4 C8_4 -102.5(15) . . . . ?
C7_4 C1_4 C2_4 C3_4 176.8(11) . . . . ?
C7_4 C1_4 C6_4 C5_4 -178.5(11) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder with paratone oil'
_olex2_submission_original_sample_id 3Br-PEA
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.347
_oxdiff_exptl_absorpt_empirical_full_min 0.800
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.979(4)
2 0.021(4)

####################################################################### 
# 
# 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_mht-b007-3
_database_code_depnum_ccdc_archive 'CCDC 1986788'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2020-02-27 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
_audit_creation_date             2019-08-19
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled 2019.08.16 svn.r3652 for OlexSys, GUI svn.r5895)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
mtremblay6@gatech.edu
john.bacsa@emory.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, C20 H32 N2'
_chemical_formula_sum            'C20 H32 I4 N2 Pb'
_chemical_formula_weight         1015.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40  H64  I8  N4  Pb2  '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.0599(2)
_cell_length_b                   8.74908(10)
_cell_length_c                   8.89838(11)
_cell_angle_alpha                90
_cell_angle_beta                 98.8141(12)
_cell_angle_gamma                90
_cell_volume                     1389.41(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    30839
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      38.1240
_cell_measurement_theta_min      2.2750
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.524
_exptl_absorpt_correction_T_max  0.398
_exptl_absorpt_correction_T_min  0.230
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.427
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 -12 1 0.1042
20 0 -9 0.0777
25 -3 0 0.0676
-24 1 -2 0.0831
19 -8 0 0.0756
0 -4 12 0.1090
9 -12 0 0.0895
1 -12 0 0.0964
18 4 -9 0.0839
-15 -10 0 0.1046
24 2 -5 0.0755
-2 -7 -10 0.0846
-25 -2 0 0.0813
-21 -1 -5 0.0857
25 -2 1 0.0698
18 -3 7 0.1009
-11 10 5 0.1176
0 8 9 0.0866
12 11 0 0.0970
1 0 -12 0.0606
-13 7 -7 0.0940
-13 8 8 0.1105
1 9 -9 0.0692
25 0 0 0.0605
-12 0 12 0.1228
2 -2 12 0.1056
1 6 11 0.0856

_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.147
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-7.4190 -11.7956 0.6242 -0.3160 -0.8933 0.3195
20.2583 -0.4816 -9.0412 0.0113 0.5222 0.8528
24.7310 -2.6243 -0.4790 -0.6753 0.5156 0.5274
-24.1419 1.3788 -1.8788 0.7485 -0.5722 -0.3351
18.6766 -8.3144 -0.2869 -0.7613 0.0176 0.6481
0.4786 -4.4645 11.5094 -0.8503 -0.2517 -0.4622
8.5213 -11.6111 -0.1388 -0.6519 -0.4508 0.6098
1.0376 -12.3103 0.4309 -0.5303 -0.6946 0.4861
17.8371 4.0370 -9.2167 0.2565 0.7219 0.6427
-14.7189 -9.9866 -0.1356 -0.0243 -0.9846 0.1731
24.3713 2.2523 -4.6697 -0.2343 0.7930 0.5623
-2.3352 -7.2609 -9.7775 0.3380 -0.4872 0.8052
-25.0826 -1.5299 0.3614 0.5285 -0.7689 -0.3598
-21.0686 -0.6607 -5.3358 0.7939 -0.6079 -0.0093
24.6210 -2.0613 0.5582 -0.7105 0.5454 0.4446
18.1573 -2.6774 6.8855 -0.9429 0.3328 0.0093
-10.6027 10.4038 5.0190 0.3735 0.3225 -0.8697
0.4177 8.3818 9.0597 -0.2063 0.5012 -0.8404
11.7033 10.8899 0.2849 0.1242 0.9560 -0.2659
0.9261 0.4675 -12.4444 0.7143 0.0553 0.6977
-12.8861 7.2671 -6.8247 0.9905 0.0792 -0.1126
-12.9799 7.9673 8.0369 0.1620 0.1144 -0.9801
1.2605 8.9406 -8.6022 0.8149 0.5608 0.1465
25.2082 0.2218 -0.1230 -0.5964 0.6955 0.4008
-12.2224 0.0727 11.8019 -0.3818 -0.3293 -0.8636
2.0354 -1.9862 12.0336 -0.8217 -0.0642 -0.5663
0.5631 6.1032 10.7246 -0.3948 0.3711 -0.8405

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43561
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.075
_diffrn_reflns_theta_min         2.282
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(6)
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00  -2.00   0.50    3.00    --  -25.84  82.00 117.00   50
  2  ω     31.00  56.00   0.50    3.00    --   25.84  82.00 117.00   50
  3  ω     65.00  99.00   0.50    3.00    --   25.84  82.00 117.00   68
  4  ω     40.00  97.00   0.50    3.00    --   25.84 178.00 120.00  114
  5  ω     49.00  97.00   0.50    3.00    --   25.84 178.00   0.00   96
  6  ω     39.00  98.00   0.50    3.00    --   25.84 178.00-120.00  118
  7  ω     13.00  39.00   0.50    3.00    --  -25.84  38.00 -90.00   52
  8  ω    -16.00   9.00   0.50    3.00    --  -25.84  38.00 -90.00   50
  9  ω     20.00  97.00   0.50    3.00    --   25.84  19.00   0.00  154
 10  ω     11.00  99.00   0.50    3.00    --   25.84  38.00 120.00  176
 11  ω    -25.00   3.00   0.50    3.00    --   25.84 -82.00  -4.00   56
 12  ω    -50.00   0.00   0.50    3.00    --  -25.84 -82.00  -4.00  100
 13  ω     49.00  98.00   0.50    3.00    --   25.84-178.00  30.00   98
 14  ω     36.00  91.00   0.50    3.00    --   25.84-178.00  90.00  110
 15  ω     39.00  97.00   0.50    3.00    --   25.84-178.00 150.00  116
 16  ω    -97.00 -14.00   0.50    3.00    --  -25.84 -38.00-150.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0242833000
_diffrn_orient_matrix_UB_12      0.0390113000
_diffrn_orient_matrix_UB_13      -0.0577398000
_diffrn_orient_matrix_UB_21      0.0270716000
_diffrn_orient_matrix_UB_22      0.0586959000
_diffrn_orient_matrix_UB_23      -0.0002254000
_diffrn_orient_matrix_UB_31      0.0159778000
_diffrn_orient_matrix_UB_32      -0.0401171000
_diffrn_orient_matrix_UB_33      -0.0563804000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6889
_reflns_number_total             7239
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/3 (Sheldrick, 2015)'
_refine_diff_density_max         1.762
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       0.00410(10)
_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   1.115
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         7239
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0202
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0161P)²+1.6099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0464
_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 C(H,H,H) groups, All N(H,H,H) groups
2. Restrained distances
 C11-H11B
 0.995 with sigma of 0.005
 C10-H10A
 0.995 with sigma of 0.003
 C14-H14B
 0.995 with sigma of 0.005
 C5-H5
 0.975 with sigma of 0.005
 N12-H12C
 0.975 with sigma of 0.005
 C9-H9 \\sim C5-H5 \\sim C7-H7
 with sigma of 0.002
 C13-H13A \\sim C13-H13B \\sim C13-H13C \\sim C14-H14B \\sim C14-H14A \\sim
C14-H14C
 with sigma of 0.002
 H11B-H11A \\sim H10B-H10A \\sim H14C-H14A \\sim H14B-H14A \\sim H14C-H14B
\\sim H13B-H13A \\sim H13C-
 H13A \\sim H13C-H13B
 with sigma of 0.002
 C11-H11A \\sim C11-H11B \\sim C10-H10A \\sim C10-H10B
 with sigma of 0.002
 N12-H12C \\sim N12-H12A \\sim N12-H12B
 with sigma of 0.002
 H12C-H12A \\sim H12C-H12B \\sim H12B-H12A
 with sigma of 0.002
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.500000 1.000000 0.500000 0.00983(2) Uani 1 2 d S . P . .
I1 I 0.49452(2) 0.70243(2) 0.70198(2) 0.01355(3) Uani 1 1 d . . . . .
I2 I 0.32133(2) 1.03614(2) 0.42542(2) 0.01452(3) Uani 1 1 d . . . . .
N12 N 0.35609(10) 0.4325(2) 0.5331(2) 0.0163(3) Uani 1 1 d D . . . .
H12A H 0.3514(13) 0.3247(10) 0.509(3) 0.025 Uiso 1 1 d D U . . .
H12B H 0.3311(12) 0.448(3) 0.6208(19) 0.025 Uiso 1 1 d D U . . .
H12C H 0.4089(4) 0.451(3) 0.568(3) 0.025 Uiso 1 1 d D U . . .
C11 C 0.33296(12) 0.5379(2) 0.4014(2) 0.0176(3) Uani 1 1 d D . . . .
H11A H 0.3699(12) 0.526(3) 0.330(3) 0.021 Uiso 1 1 d D U . . .
H11B H 0.3371(15) 0.6449(11) 0.439(3) 0.021 Uiso 1 1 d D U . . .
C10 C 0.25270(13) 0.5046(3) 0.3284(3) 0.0206(4) Uani 1 1 d D . . . .
H10A H 0.2459(19) 0.566(2) 0.2336(16) 0.025 Uiso 1 1 d D U . . .
H10B H 0.2531(19) 0.3955(8) 0.298(3) 0.025 Uiso 1 1 d D U . . .
C4 C 0.19580(11) 0.5391(2) 0.4323(2) 0.0154(3) Uani 1 1 d . . . . .
C8 C 0.11892(11) 0.7229(2) 0.5406(2) 0.0162(3) Uani 1 1 d . . . . .
C9 C 0.17249(11) 0.6889(2) 0.4493(2) 0.0161(3) Uani 1 1 d D . . . .
H9 H 0.1913(16) 0.771(2) 0.391(3) 0.019 Uiso 1 1 d D U . . .
C5 C 0.16608(11) 0.4221(2) 0.5119(2) 0.0162(3) Uani 1 1 d D . . . .
H5 H 0.1845(17) 0.3187(14) 0.502(4) 0.019 Uiso 1 1 d D U . . .
C6 C 0.11213(11) 0.4534(2) 0.6046(2) 0.0167(3) Uani 1 1 d . . . . .
C14 C 0.09165(13) 0.8853(3) 0.5525(3) 0.0227(4) Uani 1 1 d D . . . .
H14A H 0.1243(12) 0.963(2) 0.515(2) 0.034 Uiso 1 1 d D U . . .
H14B H 0.0860(12) 0.915(3) 0.6579(12) 0.034 Uiso 1 1 d D U . . .
H14C H 0.0414(6) 0.895(4) 0.490(2) 0.034 Uiso 1 1 d D U . . .
C7 C 0.08860(11) 0.6039(2) 0.6168(2) 0.0168(3) Uani 1 1 d D . . . .
H7 H 0.0485(12) 0.621(4) 0.676(3) 0.020 Uiso 1 1 d D U . . .
C13 C 0.07928(14) 0.3270(3) 0.6891(3) 0.0250(4) Uani 1 1 d D . . . .
H13A H 0.0939(14) 0.2254(16) 0.653(3) 0.038 Uiso 1 1 d D U . . .
H13B H 0.0236(3) 0.330(3) 0.673(3) 0.038 Uiso 1 1 d D U . . .
H13C H 0.0961(14) 0.330(3) 0.8008(8) 0.038 Uiso 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 I1 3.17372(11) 3_676 ?
Pb1 I1 3.17373(11) . ?
Pb1 I1 3.17784(11) 2_656 ?
Pb1 I1 3.17784(11) 4_575 ?
Pb1 I2 3.20876(13) . ?
Pb1 I2 3.20881(13) 3_676 ?
N12 H12A 0.969(5) . ?
N12 H12B 0.969(5) . ?
N12 H12C 0.970(5) . ?
N12 C11 1.500(3) . ?
C11 H11A 0.993(3) . ?
C11 H11B 0.993(3) . ?
C11 C10 1.523(3) . ?
C10 H10A 0.993(3) . ?
C10 H10B 0.993(3) . ?
C10 C4 1.515(3) . ?
C4 C9 1.392(3) . ?
C4 C5 1.397(3) . ?
C8 C9 1.388(3) . ?
C8 C14 1.512(3) . ?
C8 C7 1.399(3) . ?
C9 H9 0.972(5) . ?
C5 H5 0.972(5) . ?
C5 C6 1.397(3) . ?
C6 C7 1.393(3) . ?
C6 C13 1.509(3) . ?
C14 H14A 0.994(5) . ?
C14 H14B 0.994(4) . ?
C14 H14C 0.994(5) . ?
C7 H7 0.972(5) . ?
C13 H13A 0.994(5) . ?
C13 H13B 0.994(5) . ?
C13 H13C 0.994(5) . ?

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 180.0 3_676 . ?
I1 Pb1 I1 90.900(1) . 4_575 ?
I1 Pb1 I1 89.100(2) 3_676 4_575 ?
I1 Pb1 I1 89.100(1) . 2_656 ?
I1 Pb1 I1 90.900(1) 3_676 2_656 ?
I1 Pb1 I1 180.0 4_575 2_656 ?
I1 Pb1 I2 91.111(4) 2_656 . ?
I1 Pb1 I2 88.889(4) 4_575 . ?
I1 Pb1 I2 91.112(3) 4_575 3_676 ?
I1 Pb1 I2 94.610(3) 3_676 3_676 ?
I1 Pb1 I2 85.390(3) 3_676 . ?
I1 Pb1 I2 94.609(3) . . ?
I1 Pb1 I2 88.888(3) 2_656 3_676 ?
I1 Pb1 I2 85.391(3) . 3_676 ?
I2 Pb1 I2 180.0 . 3_676 ?
Pb1 I1 Pb1 158.446(4) . 2_646 ?
H12A N12 H12B 106.2(12) . . ?
H12A N12 H12C 106.2(12) . . ?
H12B N12 H12C 106.2(12) . . ?
C11 N12 H12A 114.7(18) . . ?
C11 N12 H12B 115.9(18) . . ?
C11 N12 H12C 106.9(19) . . ?
N12 C11 H11A 107.4(17) . . ?
N12 C11 H11B 108.6(17) . . ?
N12 C11 C10 110.41(17) . . ?
H11A C11 H11B 107.1(10) . . ?
C10 C11 H11A 113.3(17) . . ?
C10 C11 H11B 109.9(17) . . ?
C11 C10 H10A 104.1(19) . . ?
C11 C10 H10B 104.8(19) . . ?
H10A C10 H10B 107.1(10) . . ?
C4 C10 C11 113.07(18) . . ?
C4 C10 H10A 113.8(18) . . ?
C4 C10 H10B 113.2(17) . . ?
C9 C4 C10 119.90(19) . . ?
C9 C4 C5 119.25(18) . . ?
C5 C4 C10 120.85(18) . . ?
C9 C8 C14 120.42(19) . . ?
C9 C8 C7 118.91(18) . . ?
C7 C8 C14 120.63(18) . . ?
C4 C9 H9 119.9(18) . . ?
C8 C9 C4 121.02(18) . . ?
C8 C9 H9 118.9(18) . . ?
C4 C5 H5 118.2(18) . . ?
C6 C5 C4 120.83(18) . . ?
C6 C5 H5 120.9(18) . . ?
C5 C6 C13 120.91(19) . . ?
C7 C6 C5 118.68(19) . . ?
C7 C6 C13 120.40(19) . . ?
C8 C14 H14A 114.0(17) . . ?
C8 C14 H14B 113.1(18) . . ?
C8 C14 H14C 108.5(18) . . ?
H14A C14 H14B 107.0(9) . . ?
H14A C14 H14C 107.0(9) . . ?
H14B C14 H14C 107.0(9) . . ?
C8 C7 H7 122(2) . . ?
C6 C7 C8 121.28(18) . . ?
C6 C7 H7 117(2) . . ?
C6 C13 H13A 110.6(17) . . ?
C6 C13 H13B 111.9(18) . . ?
C6 C13 H13C 113.2(18) . . ?
H13A C13 H13B 107.0(9) . . ?
H13A C13 H13C 107.0(9) . . ?
H13B C13 H13C 107.0(9) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C5 H5 N12 0.972(5) 3.23(3) 3.409(3) 92.4(19) . yes

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
N12 C11 C10 C4 65.5(2) . . . . ?
C11 C10 C4 C9 80.0(2) . . . . ?
C11 C10 C4 C5 -100.0(2) . . . . ?
C10 C4 C9 C8 178.24(19) . . . . ?
C10 C4 C5 C6 -178.29(19) . . . . ?
C4 C5 C6 C7 -0.2(3) . . . . ?
C4 C5 C6 C13 179.3(2) . . . . ?
C9 C4 C5 C6 1.6(3) . . . . ?
C9 C8 C7 C6 1.2(3) . . . . ?
C5 C4 C9 C8 -1.7(3) . . . . ?
C5 C6 C7 C8 -1.2(3) . . . . ?
C14 C8 C9 C4 -177.30(19) . . . . ?
C14 C8 C7 C6 178.77(19) . . . . ?
C7 C8 C9 C4 0.3(3) . . . . ?
C13 C6 C7 C8 179.3(2) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id MHT-B007-3
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.269
_oxdiff_exptl_absorpt_empirical_full_min 0.887
####################################################################### 
# 
# 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_dbr-pea_twin1_hklf5
_database_code_depnum_ccdc_archive 'CCDC 1986786'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2020-02-27 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT342_dbr-pea_twin1_hklf5 
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.03 Ang.
RESPONSE: The crystal was twinned, and the twinning could 
only be partly resolved.  The twinning, strong  scatterers 
(Pb, I and Br) and strong absorption contributed to the low 
precision of the lighter scatterers.
;
# end Validation Reply Form
_audit_creation_date             2020-02-26
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6020)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
mtremblay6@gatech.edu
john.bacsa@emory.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H10 Br2 N)'
_chemical_formula_sum            'C16 H20 Br4 I4 N2 Pb'
_chemical_formula_weight         1274.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         C16H20Br4I4N2Pb
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.1147(7)
_cell_length_b                   8.7853(3)
_cell_length_c                   8.8694(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.314(4)
_cell_angle_gamma                90
_cell_volume                     1405.42(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12066
_cell_measurement_temperature    106(9)
_cell_measurement_theta_max      33.7250
_cell_measurement_theta_min      2.2870
_shelx_estimated_absorpt_T_max   0.739
_shelx_estimated_absorpt_T_min   0.083
_exptl_absorpt_coefficient_mu    16.088
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.186
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.012
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 0 -2 0.0500
1 0 0 0.0100
-1 5 0 0.1543
4 -5 -3 0.0970
4 1 -5 0.0758
-4 2 5 0.0644
1 -4 -5 0.1018
-1 0 0 0.0100
7 0 -12 0.0762
3 -5 1 0.1437
-5 0 -4 0.0673
22 1 -7 0.0419
18 9 0 0.1027
-7 11 5 0.1278
12 1 10 0.0546
-16 0 10 0.0545

_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.02
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.9931 0.0070 -2.0016 -0.0491 -0.1585 -0.1760
0.9997 0.0037 -0.0006 -0.0302 -0.0218 -0.0124
-1.0530 4.9864 -0.0181 0.1501 -0.2801 0.2509
4.0442 -4.9926 -2.9814 -0.0878 0.1406 -0.4589
3.9749 0.9841 -5.0024 0.1581 -0.2709 -0.2866
-4.0069 2.0099 4.9911 -0.0861 0.0898 0.4297
1.0293 -4.0170 -4.9817 0.1288 0.0965 -0.4878
-0.9997 -0.0037 0.0006 0.0302 0.0218 0.0124
6.9663 -0.0429 -11.9951 0.4003 -0.4486 -0.7700
3.0550 -4.9734 1.0161 -0.2615 0.2610 -0.2188
-5.0088 -0.0413 -3.9937 0.3550 0.0106 -0.1655
21.8327 1.2946 -7.3344 -0.2573 -0.7340 -0.6285
17.8133 8.8642 -0.1033 -0.3268 -0.9249 0.1945
-7.1902 10.7459 5.4261 0.1935 -0.3602 0.9126
12.2768 1.0587 10.3047 -0.8739 -0.0711 0.4808
-15.8965 0.3368 10.4655 -0.0444 0.5853 0.8096

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4218
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.674
_diffrn_reflns_theta_min         2.258
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      106(9)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -33.00  -8.00   0.50   14.00    --   15.69 -72.00  46.00   50
  2  ω    -23.00  20.00   0.50   14.00    --  -15.84 -99.00 -60.00   86
  3  ω    -14.00  11.00   0.50   14.00    --  -15.84 -99.00-150.00   50
  4  ω    -88.00   4.00   0.50   14.00    --  -15.84 -72.00  46.00  184
  5  ω     36.00  74.00   0.50   14.00    --   15.69-178.00 150.00   76
  6  ω     -3.00  81.00   0.50   14.00    --   15.69  57.00 -60.00  168
  7  ω     39.00  64.00   0.50   14.00    --   15.69 178.00  60.00   50
  8  ω     39.00  90.00   0.50   14.00    --   15.69 178.00   0.00  102
  9  ω     41.00  84.00   0.50   14.00    --   15.69 178.00  90.00   86
 10  ω     16.00  41.00   0.50   14.00    --   15.69  72.00 176.00   50
 11  ω    -34.00  43.00   0.50   14.00    --  -15.84  72.00 176.00  154
 12  ω    -34.00  56.00   0.50   14.00    --  -15.84  57.00 150.00  180
 13  ω    -85.00 -76.00   0.50   14.00    --  -15.84 -57.00  60.00   18
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0303391000
_diffrn_orient_matrix_UB_12      0.0235041000
_diffrn_orient_matrix_UB_13      -0.0510799000
_diffrn_orient_matrix_UB_21      -0.0216022000
_diffrn_orient_matrix_UB_22      -0.0606335000
_diffrn_orient_matrix_UB_23      0.0250662000
_diffrn_orient_matrix_UB_31      -0.0125736000
_diffrn_orient_matrix_UB_32      0.0478688000
_diffrn_orient_matrix_UB_33      0.0567192000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3967
_reflns_number_total             4218
_reflns_special_details          
;
 _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       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         5.381
_refine_diff_density_min         -1.906
_refine_diff_density_rms         0.434
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         4218
_refine_ls_number_restraints     69
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0654
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1200P)²+46.6203P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.1879
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.582(2)
 0.418(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3. Rigid body (RIGU) restrains
 C4, Br1, C1, C2, C6, C3, C5, Br2, C7, C8, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C4(H4)
4.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.000000 0.500000 0.500000 0.0180(3) Uani 1 2 d S . P . .
I1 I -0.00401(7) 0.20170(12) 0.29651(13) 0.0204(3) Uani 1 1 d . . . . .
I2 I 0.17696(8) 0.46527(13) 0.51516(14) 0.0224(3) Uani 1 1 d . . . . .
Br1 Br 0.42032(12) 0.9104(2) 0.2823(2) 0.0264(5) Uani 1 1 d . . . . .
Br2 Br 0.40999(12) 0.2868(2) 0.4355(2) 0.0260(5) Uani 1 1 d . . . . .
N1 N 0.1407(10) 0.4330(18) 0.1032(17) 0.024(4) Uani 1 1 d . . . . .
H1A H 0.145722 0.339022 0.068212 0.028 Uiso 1 1 calc R U . . .
H1B H 0.093332 0.449882 0.116974 0.028 Uiso 1 1 calc R U . . .
H1C H 0.168294 0.443524 0.190928 0.028 Uiso 1 1 calc R U . . .
C2 C 0.4074(10) 0.593(2) 0.344(2) 0.019(3) Uani 1 1 d . . . . .
H2 H 0.442425 0.608757 0.425409 0.023 Uiso 1 1 calc R U . . .
C6 C 0.3279(11) 0.689(2) 0.124(2) 0.021(3) Uani 1 1 d . . . . .
H6 H 0.310725 0.770325 0.062970 0.026 Uiso 1 1 calc R U . . .
C1 C 0.3806(12) 0.713(2) 0.243(2) 0.024(4) Uani 1 1 d . . . . .
C8 C 0.1651(11) 0.544(2) -0.007(2) 0.022(4) Uani 1 1 d . . . . .
H8A H 0.161153 0.645721 0.033120 0.026 Uiso 1 1 calc R U . . .
H8B H 0.132333 0.537329 -0.099932 0.026 Uiso 1 1 calc R U . . .
C3 C 0.3782(11) 0.455(2) 0.311(2) 0.024(4) Uani 1 1 d . . . . .
C4 C 0.3251(11) 0.422(2) 0.190(2) 0.022(3) Uani 1 1 d . . . . .
H4 H 0.307092 0.323314 0.174181 0.026 Uiso 1 1 calc R U . . .
C5 C 0.3001(11) 0.542(2) 0.095(2) 0.021(3) Uani 1 1 d . . . . .
C7 C 0.2451(12) 0.516(2) -0.044(2) 0.025(4) Uani 1 1 d . . . . .
H7A H 0.249877 0.412867 -0.080034 0.029 Uiso 1 1 calc R U . . .
H7B H 0.256708 0.584931 -0.124233 0.029 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 Pb1 6.24193(14) 2 ?
Pb1 Pb1 6.24193(14) 4_566 ?
Pb1 Pb1 6.24193(15) 2_545 ?
Pb1 I1 3.1790(11) . ?
Pb1 I1 3.1775(11) 2 ?
Pb1 I1 3.1790(11) 3_566 ?
Pb1 I1 3.1775(11) 4_566 ?
Pb1 I2 3.2104(14) 3_566 ?
Pb1 I2 3.2104(14) . ?
Br1 C1 1.896(19) . ?
Br2 C3 1.90(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C8 1.48(2) . ?
C2 H2 0.9300 . ?
C2 C1 1.44(3) . ?
C2 C3 1.34(3) . ?
C6 H6 0.9300 . ?
C6 C1 1.38(3) . ?
C6 C5 1.41(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.53(3) . ?
C3 C4 1.40(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.40(3) . ?
C5 C7 1.53(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 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
Pb1 Pb1 Pb1 180.0 2 4_566 ?
Pb1 Pb1 Pb1 89.454(4) 2_545 2 ?
Pb1 Pb1 Pb1 90.546(3) 2_545 4_566 ?
I1 Pb1 Pb1 169.10(2) 4_566 2 ?
I1 Pb1 Pb1 101.37(2) 4_566 2_545 ?
I1 Pb1 Pb1 100.27(2) 3_566 4_566 ?
I1 Pb1 Pb1 79.73(2) . 4_566 ?
I1 Pb1 Pb1 79.73(2) 3_566 2 ?
I1 Pb1 Pb1 10.89(2) . 2_545 ?
I1 Pb1 Pb1 10.90(2) 2 2 ?
I1 Pb1 Pb1 169.11(2) 3_566 2_545 ?
I1 Pb1 Pb1 169.10(2) 2 4_566 ?
I1 Pb1 Pb1 10.90(2) 4_566 4_566 ?
I1 Pb1 Pb1 78.63(2) 2 2_545 ?
I1 Pb1 Pb1 100.27(2) . 2 ?
I1 Pb1 I1 180.0 4_566 2 ?
I1 Pb1 I1 90.521(8) 4_566 . ?
I1 Pb1 I1 89.479(8) 4_566 3_566 ?
I1 Pb1 I1 180.0 3_566 . ?
I1 Pb1 I1 89.479(8) 2 . ?
I1 Pb1 I1 90.521(8) 2 3_566 ?
I1 Pb1 I2 94.84(3) 3_566 . ?
I1 Pb1 I2 85.16(3) 3_566 3_566 ?
I1 Pb1 I2 85.16(3) . . ?
I1 Pb1 I2 89.33(3) 2 . ?
I1 Pb1 I2 94.84(3) . 3_566 ?
I1 Pb1 I2 89.33(3) 4_566 3_566 ?
I1 Pb1 I2 90.67(3) 4_566 . ?
I1 Pb1 I2 90.67(3) 2 3_566 ?
I2 Pb1 Pb1 95.90(2) 3_566 2_545 ?
I2 Pb1 Pb1 84.10(2) . 2_545 ?
I2 Pb1 Pb1 88.23(2) . 4_566 ?
I2 Pb1 Pb1 88.23(2) 3_566 2 ?
I2 Pb1 Pb1 91.77(2) 3_566 4_566 ?
I2 Pb1 Pb1 91.77(2) . 2 ?
I2 Pb1 I2 180.0 3_566 . ?
Pb1 I1 Pb1 158.21(4) 2_545 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C8 N1 H1A 109.5 . . ?
C8 N1 H1B 109.5 . . ?
C8 N1 H1C 109.5 . . ?
C1 C2 H2 122.4 . . ?
C3 C2 H2 122.4 . . ?
C3 C2 C1 115.2(19) . . ?
C1 C6 H6 120.2 . . ?
C1 C6 C5 119.6(18) . . ?
C5 C6 H6 120.2 . . ?
C2 C1 Br1 117.5(15) . . ?
C6 C1 Br1 120.3(15) . . ?
C6 C1 C2 122.3(18) . . ?
N1 C8 H8A 109.1 . . ?
N1 C8 H8B 109.1 . . ?
N1 C8 C7 112.6(16) . . ?
H8A C8 H8B 107.8 . . ?
C7 C8 H8A 109.1 . . ?
C7 C8 H8B 109.1 . . ?
C2 C3 Br2 118.7(16) . . ?
C2 C3 C4 126(2) . . ?
C4 C3 Br2 115.5(15) . . ?
C3 C4 H4 121.2 . . ?
C3 C4 C5 117.7(18) . . ?
C5 C4 H4 121.2 . . ?
C6 C5 C7 118.7(17) . . ?
C4 C5 C6 119.5(19) . . ?
C4 C5 C7 121.9(17) . . ?
C8 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
C5 C7 C8 111.3(16) . . ?
C5 C7 H7A 109.4 . . ?
C5 C7 H7B 109.4 . . ?
H7A C7 H7B 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
Br2 C3 C4 C5 -179.9(13) . . . . ?
N1 C8 C7 C5 -65(2) . . . . ?
C2 C3 C4 C5 0(3) . . . . ?
C6 C5 C7 C8 -88(2) . . . . ?
C1 C2 C3 Br2 179.8(14) . . . . ?
C1 C2 C3 C4 0(3) . . . . ?
C1 C6 C5 C4 2(3) . . . . ?
C1 C6 C5 C7 -176.3(18) . . . . ?
C3 C2 C1 Br1 -179.4(14) . . . . ?
C3 C2 C1 C6 1(3) . . . . ?
C3 C4 C5 C6 -1(3) . . . . ?
C3 C4 C5 C7 177.0(17) . . . . ?
C4 C5 C7 C8 94(2) . . . . ?
C5 C6 C1 Br1 178.7(14) . . . . ?
C5 C6 C1 C2 -2(3) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id dBr-PEA
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.216
_oxdiff_exptl_absorpt_empirical_full_min 0.384
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.582(2) 5079 16629 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.418(2) 5050 16629 nmt 0.9997 -0.0037 0.3810 -0.0008 -1.0000 0.0002 -0.0004
-0.0003 -1.0000

_twin_special_details            
;
Component 2 rotated by -179.9834° 
 around [1.00 -0.00 -0.00] (reciprocal) or [0.98 -0.01 0.19] (direct)
;
####################################################################### 
# 
# 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_5-dcpea2pbi4
_database_code_depnum_ccdc_archive 'CCDC 1986789'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2020-02-27 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
_audit_creation_date             2018-10-01
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(I8 Pb2), 2(C8 H10 Cl2 N)'
_chemical_formula_sum            'C16 H20 Cl4 I4 N2 Pb'
_chemical_formula_weight         1096.93
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32  H40  Cl8  I8  N4  Pb2  '
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.0323(4)
_cell_length_b                   8.64280(10)
_cell_length_c                   8.8430(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.226(2)
_cell_angle_gamma                90
_cell_volume                     1356.29(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17275
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      38.3070
_cell_measurement_theta_min      2.6050
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.173
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.033
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.15a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.686
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 1 0.2729
1 -2 -2 0.0934
-7 -11 3 0.1291
12 0 -12 0.1546
4 -10 -7 0.0829
11 -11 1 0.1093
19 6 4 0.0770
-22 3 -4 0.0917
-3 10 6 0.0988
25 0 -1 0.0191
-25 2 1 0.0419
-25 -2 1 0.0453

_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by ---'
_exptl_crystal_size_max          0.539
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.063
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0024 0.0017 1.0008 0.0194 0.0819 0.0043
1.0182 -2.0061 -1.9977 -0.0228 -0.1465 -0.1759
-7.0861 -11.4206 3.1687 0.0859 0.3499 -0.9328
11.8734 -0.1923 -11.8800 -0.2317 -0.9706 -0.0647
4.0038 -9.8324 -7.3265 -0.1224 -0.5216 -0.8444
10.6144 -10.8600 1.2176 -0.5669 0.1331 -0.8130
18.7158 6.3889 3.6335 -0.7389 0.1783 0.6498
-21.9245 2.7500 -3.6607 0.9700 -0.2315 0.0737
-2.9918 10.4463 6.4015 0.1081 0.4414 0.8908
25.3545 -0.1526 -1.2391 -0.9773 -0.1820 0.1088
-25.0723 1.9013 1.4195 0.9824 0.1833 0.0360
-25.1338 -1.5061 1.0607 0.9533 0.1785 -0.2438

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            41439
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.313
_diffrn_reflns_theta_min         2.295
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      106(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -26.00   0.00   0.50    8.00    --   25.84 -12.00  63.00   52
  2  ω     18.00  98.00   0.50    8.00    --   25.84  57.00  30.00  160
  3  ω     45.00  93.00   0.50    8.00    --   25.84  12.00-124.00   96
  4  ω     10.00  97.00   0.50    8.00    --   25.84  57.00 -60.00  174
  5  ω      8.00  49.00   0.50    8.00    --  -25.84  12.00-124.00   82
  6  ω    -38.00 -11.00   0.50    8.00    --  -25.84 -38.00-180.00   54
  7  ω    -80.00 -53.00   0.50    8.00    --  -25.84 -77.00 -60.00   54
  8  ω    -47.00  -6.00   0.50    8.00    --  -25.84 -77.00 -60.00   82
  9  ω    -82.00 -40.00   0.50    8.00    --  -25.84 -12.00  63.00   84
 10  ω    -65.00 -40.00   0.50    8.00    --  -25.84 108.00 -45.20   50
 11  ω    -72.00 -30.00   0.50    8.00    --  -25.84 120.00 -54.65   84
 12  ω    -72.00 -28.00   0.50    8.00    --  -25.84 120.00 -67.18   88
 13  ω    -73.00 -44.00   0.50    8.00    --  -25.84 122.00-127.83   58
 14  ω    -73.00 -39.00   0.50    8.00    --  -25.84 122.00-103.39   68
 15  ω     39.00  96.00   0.50    8.00    --   25.84 178.00 -90.00  114
 16  ω     40.00  91.00   0.50    8.00    --   25.84 178.00-120.00  102
 17  ω     39.00  90.00   0.50    8.00    --   25.84 178.00-180.00  102
 18  ω    -82.00 -57.00   0.50    8.00    --  -25.84 -38.00-180.00   50
 19  ω     49.00  98.00   0.50    8.00    --   25.84-178.00  30.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0394585000
_diffrn_orient_matrix_UB_12      0.0113768000
_diffrn_orient_matrix_UB_13      -0.0201186000
_diffrn_orient_matrix_UB_21      -0.0033859000
_diffrn_orient_matrix_UB_22      -0.0067735000
_diffrn_orient_matrix_UB_23      0.0784290000
_diffrn_orient_matrix_UB_31      0.0052386000
_diffrn_orient_matrix_UB_32      0.0810300000
_diffrn_orient_matrix_UB_33      0.0093683000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5576
_reflns_number_total             6585
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.15a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         11.374
_refine_diff_density_min         -3.182
_refine_diff_density_rms         0.438
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         6585
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0521
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0970P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1403
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C8(H8)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.500000 0.000000 0.500000 0.01436(7) Uani 1 2 d S T P . .
I1 I 0.50303(2) 0.30470(3) 0.30409(3) 0.01824(8) Uani 1 1 d . . . . .
I2 I 0.31980(2) 0.02704(4) 0.41898(4) 0.01866(8) Uani 1 1 d . . . . .
Cl2 Cl 0.08161(8) 0.90060(16) 0.55100(16) 0.0272(3) Uani 1 1 d . . . . .
Cl1 Cl 0.07793(9) 0.29838(18) 0.70622(19) 0.0315(3) Uani 1 1 d . . . . .
N1 N 0.3541(3) 0.4293(5) 0.5272(5) 0.0195(8) Uani 1 1 d . . . . .
H1A H 0.347546 0.331434 0.496605 0.023 Uiso 1 1 calc GR . . . .
H1B H 0.327968 0.447462 0.601803 0.023 Uiso 1 1 calc GR . . . .
H1C H 0.402823 0.446403 0.562226 0.023 Uiso 1 1 calc GR . . . .
C1 C 0.3273(4) 0.5348(7) 0.3946(7) 0.0253(10) Uani 1 1 d . . . . .
H1D H 0.359193 0.522910 0.317866 0.030 Uiso 1 1 calc R . . . .
H1E H 0.330745 0.641321 0.429604 0.030 Uiso 1 1 calc R . . . .
C6 C 0.0842(3) 0.5967(5) 0.6172(6) 0.0174(8) Uani 1 1 d . . . . .
H6 H 0.047494 0.617383 0.676215 0.021 Uiso 1 1 calc R . . . .
C3 C 0.1909(3) 0.5309(7) 0.4304(6) 0.0197(9) Uani 1 1 d . . . . .
C5 C 0.1134(3) 0.7119(6) 0.5384(6) 0.0191(8) Uani 1 1 d . . . . .
C4 C 0.1665(3) 0.6833(6) 0.4452(6) 0.0211(9) Uani 1 1 d . . . . .
H4 H 0.185517 0.763839 0.393683 0.025 Uiso 1 1 calc R . . . .
C2 C 0.2453(4) 0.4972(7) 0.3228(7) 0.0262(12) Uani 1 1 d . . . . .
H2A H 0.231073 0.557577 0.229753 0.031 Uiso 1 1 calc R . . . .
H2B H 0.241665 0.388630 0.294560 0.031 Uiso 1 1 calc R . . . .
C8 C 0.1632(3) 0.4127(6) 0.5111(6) 0.0210(9) Uani 1 1 d . . . . .
H8 H 0.178944 0.311134 0.502339 0.025 Uiso 1 1 calc R . . . .
C7 C 0.1116(3) 0.4488(6) 0.6053(6) 0.0214(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.1580(3) . ?
Pb1 I1 3.1672(3) 4_566 ?
Pb1 I1 3.1672(3) 2_645 ?
Pb1 I1 3.1580(3) 3_656 ?
Pb1 I2 3.2094(4) 3_656 ?
Pb1 I2 3.2094(4) . ?
Cl2 C5 1.739(5) . ?
Cl1 C7 1.745(6) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.496(7) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.537(9) . ?
C6 H6 0.9300 . ?
C6 C5 1.373(7) . ?
C6 C7 1.381(7) . ?
C3 C4 1.402(7) . ?
C3 C2 1.510(9) . ?
C3 C8 1.389(8) . ?
C5 C4 1.392(8) . ?
C4 H4 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C8 H8 0.9300 . ?
C8 C7 1.390(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 180.0 . 3_656 ?
I1 Pb1 I1 88.741(3) 3_656 4_566 ?
I1 Pb1 I1 91.260(2) . 4_566 ?
I1 Pb1 I1 91.259(3) 3_656 2_645 ?
I1 Pb1 I1 88.740(2) . 2_645 ?
I1 Pb1 I1 180.0 4_566 2_645 ?
I1 Pb1 I2 93.884(9) 3_656 . ?
I1 Pb1 I2 90.855(9) 4_566 . ?
I1 Pb1 I2 86.116(9) 3_656 3_656 ?
I1 Pb1 I2 86.116(9) . . ?
I1 Pb1 I2 89.145(9) 4_566 3_656 ?
I1 Pb1 I2 90.855(9) 2_645 3_656 ?
I1 Pb1 I2 89.145(9) 2_645 . ?
I1 Pb1 I2 93.884(9) . 3_656 ?
I2 Pb1 I2 180.0 3_656 . ?
Pb1 I1 Pb1 155.620(11) . 2_655 ?
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 . . ?
N1 C1 H1D 109.6 . . ?
N1 C1 H1E 109.6 . . ?
N1 C1 C2 110.4(5) . . ?
H1D C1 H1E 108.1 . . ?
C2 C1 H1D 109.6 . . ?
C2 C1 H1E 109.6 . . ?
C5 C6 H6 121.4 . . ?
C5 C6 C7 117.2(5) . . ?
C7 C6 H6 121.4 . . ?
C4 C3 C2 119.3(5) . . ?
C8 C3 C4 119.7(5) . . ?
C8 C3 C2 121.0(5) . . ?
C6 C5 Cl2 119.1(4) . . ?
C6 C5 C4 122.5(4) . . ?
C4 C5 Cl2 118.3(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.9(5) . . ?
C5 C4 H4 120.6 . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C3 C2 C1 112.5(5) . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C3 C8 H8 120.5 . . ?
C3 C8 C7 118.9(5) . . ?
C7 C8 H8 120.5 . . ?
C6 C7 Cl1 119.3(4) . . ?
C6 C7 C8 122.7(5) . . ?
C8 C7 Cl1 118.0(4) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 'The crystal was mounted on a None'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.774
_oxdiff_exptl_absorpt_empirical_full_min 0.389
####################################################################### 
# 
# 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_3-5-dfpea2pbi4
_database_code_depnum_ccdc_archive 'CCDC 1986787'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2020-02-27 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
_audit_creation_date             2018-11-12
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.92(I8 Pb2), C16 H21 F4 I0.64 N2 Pb0.16, 2(C8 H10 F2 N)'
_chemical_formula_sum            'C32 H41 F8 I8 N4 Pb2'
_chemical_formula_weight         2063.27
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C64  H96  I16  N8  O16  Pb4  '
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.21680(19)
_cell_length_b                   12.27147(16)
_cell_length_c                   16.8535(3)
_cell_angle_alpha                100.4107(13)
_cell_angle_beta                 95.9(10)
_cell_angle_gamma                90.0024(12)
_cell_volume                     2471(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    24050
_cell_measurement_temperature    109(4)
_cell_measurement_theta_max      38.0630
_cell_measurement_theta_min      2.6040
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.858
_exptl_absorpt_correction_T_max  0.650
_exptl_absorpt_correction_T_min  0.222
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.15a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.773
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1842
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0605
-10 -1 20 0.0398
13 3 -18 0.0476
3 4 -24 0.0443
-4 -6 23 0.0410
1 1 23 0.0256
-14 4 -10 0.0470
5 -3 22 0.0283
-4 3 -22 0.0446
5 17 -6 0.0919
13 -11 -2 0.0614
15 0 9 0.0498
-5 4 21 0.0351
10 6 -20 0.0533
-1 1 -2 0.0598
6 -2 -22 0.0370
-2 2 1 0.0651
-2 0 -1 0.0553
2 2 1 0.0735
1 -1 2 0.0538
-1 1 2 0.0485
1 -1 -2 0.0511
1 0 -1 0.0495
-15 0 13 0.0533
-12 -1 -15 0.0533
-13 -8 -6 0.0724
-4 -17 5 0.0946

_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by ---'
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.073
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0031 0.0009 -0.0017 0.0272 -0.0436 0.0281
-9.9738 -0.9174 19.9499 -0.1437 -0.9289 -0.2739
12.9764 2.9303 -17.9757 0.1083 1.0108 0.0469
2.9696 3.8949 -23.9889 0.5323 0.7253 0.4654
-3.9711 -5.9015 23.0153 -0.5697 -0.7451 -0.3245
1.0295 1.1068 22.9335 -0.4144 -0.5242 -0.7556
-14.0111 3.9447 -10.0478 0.7315 -0.3588 0.5257
5.0273 -2.8967 21.9928 -0.6701 -0.3279 -0.6722
-4.0274 2.8976 -21.9913 0.6430 0.3713 0.6441
4.9945 16.9868 -6.1950 0.6824 0.3744 -0.6673
12.9948 -11.0046 -1.8356 -0.7713 0.6081 0.1509
15.0104 0.0540 9.0006 -0.5738 0.4291 -0.6901
-4.9721 4.0944 20.8911 -0.0901 -0.7338 -0.6519
9.9745 5.9204 -20.0136 0.3513 0.9315 0.0663
-1.0023 0.9906 -2.0094 0.1059 0.0065 0.0462
5.9711 -2.0969 -21.9128 0.1647 0.8030 0.5706
-1.9983 2.0041 0.9691 0.1185 -0.1105 -0.0566
-2.0011 -0.0063 -1.0006 0.0728 -0.0622 0.0860
2.0014 2.0074 0.9751 0.0103 0.0632 -0.1691
1.0023 -0.9906 2.0094 -0.1059 -0.0065 -0.0462
-0.9972 1.0089 1.9810 0.0313 -0.0923 -0.0731
0.9972 -1.0089 -1.9810 -0.0313 0.0923 0.0731
0.9986 -0.0037 -0.9961 -0.0084 0.0681 0.0017
-15.3330 0.1833 12.7177 0.1831 -0.9821 0.0448
-12.0184 -1.0795 -14.9690 0.5629 -0.1511 0.8262
-13.0079 -8.0432 -5.9029 0.1316 -0.4206 0.8765
-3.9958 -16.9905 5.1988 -0.6908 -0.3063 0.6691

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81072
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.981
_diffrn_reflns_theta_min         1.676
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      109(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -1.00  39.00   0.50    9.94    --   25.84 -62.00 163.00   80
  2  ω    -52.00 -26.00   0.50    9.94    --  -25.84 -62.00 163.00   52
  3  ω    -47.00  -2.00   0.50    9.94    --  -25.84 -77.00 120.00   90
  4  ω    -64.00 -11.00   0.50    9.94    --  -25.84 -38.00  30.00  106
  5  ω    -93.00 -62.00   0.50    9.94    --  -25.84 -62.00 163.00   62
  6  ω    -84.00 -57.00   0.50    9.94    --  -25.84 -77.00 120.00   54
  7  ω    -98.00 -72.00   0.50    9.94    --  -25.84 -38.00  30.00   52
  8  ω      8.00  99.00   0.50    9.94    --   25.84  62.00 -58.00  182
  9  ω     40.00  89.00   0.50   16.00    --   25.84 178.00 -30.00   98
 10  ω     72.00  98.00   0.50   16.00    --   25.84 178.00 -60.00   52
 11  ω     39.00  97.00   0.50   16.00    --   25.84 178.00  90.00  116
 12  ω     66.00  92.00   0.50   16.00    --   25.84 178.00 120.00   52
 13  ω     10.00  98.00   0.50   16.00    --   25.84  77.00 -30.00  176
 14  ω      3.00  96.00   0.50   16.00    --   25.84  77.00-180.00  186
 15  ω      5.00  98.00   0.50   16.00    --   25.84  77.00  60.00  186
 16  ω     13.00  59.00   0.50   16.00    --   25.84  77.00  90.00   92
 17  ω    -41.00 -16.00   0.50   16.00    --  -25.84  62.00 -58.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0270762000
_diffrn_orient_matrix_UB_12      0.0412591000
_diffrn_orient_matrix_UB_13      -0.0188436000
_diffrn_orient_matrix_UB_21      0.0434670000
_diffrn_orient_matrix_UB_22      0.0002083000
_diffrn_orient_matrix_UB_23      -0.0248187000
_diffrn_orient_matrix_UB_31      -0.0280320000
_diffrn_orient_matrix_UB_32      -0.0418641000
_diffrn_orient_matrix_UB_33      -0.0296700000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                19354
_reflns_number_total             25236
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.15a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.501
_refine_diff_density_min         -3.170
_refine_diff_density_rms         0.277
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         25236
_refine_ls_number_restraints     328
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0387
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0384P)²+1.1493P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0904
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All F(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Pb1_1) = Uanis(Pb1_2)
Uanis(I1_2) = Uanis(I1_1)
Uanis(I6_2) = Uanis(I6_1)
Uanis(I3_1) = Uanis(I3_2)
Uanis(I4_2) = Uanis(I4_1)
Uanis(I7_1) = Uanis(I7_2)
Uanis(I8_2) = Uanis(I8_1)
Uanis(I5_1) = Uanis(I5_2)
Uanis(Pb2_2) = Uanis(Pb2_1)
3. Rigid body (RIGU) restrains
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 Pb1_1, Pb2_1, I1_1, I2_1, I3_1, I4_1, I5_1, I6_1, I7_1, I8_1
 Pb1_2, Pb2_2, I1_2, I2_2, I3_2, I4_2, I5_2, I6_2, I7_2, I8_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{F1_4, F2_4, N1_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4, C7_4, C8_4}
{F1_5, F2_5, N1_5, C1_5, C2_5, C3_5, C4_5, C5_5, C6_5, C7_5, C8_5}
{F1_6, F2_6, N1_6, C1_6, C2_6, C3_6, C4_6, C5_6, C6_6, C7_6, C8_6}
as
{F1_3, F2_3, N1_3, C1_3, C2_3, C3_3, C4_3, C5_3, C6_3, C7_3, C8_3} sigma for
1-2: 0.002 1-3: 0.004
{Pb1_2, Pb2_2, I1_2, I2_2, I3_2, I4_2, I5_2, I6_2, I7_2, I8_2}
as
{Pb1_1, Pb2_1, I1_1, I2_1, I3_1, I4_1, I5_1, I6_1, I7_1, I8_1} sigma for 1-2:
0.02 1-3: 0.04
5. Others
 Sof(Pb1)=Sof(Pb2)=Sof(I1)=Sof(I2)=Sof(I3)=Sof(I4)=Sof(I5)=Sof(I6)=Sof(I7)=
 Sof(I8)=1-FVAR(1)
 Sof(Pb1)=Sof(Pb2)=Sof(I1)=Sof(I2)=Sof(I3)=Sof(I4)=Sof(I5)=Sof(I6)=Sof(I7)=
 Sof(I8)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B),
 C7(H7A,H7B), C8(H8A,H8B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C2(H2), C4(H4), C6(H6), C2(H2), C4(H4), C6(H6),
 C2(H2), C4(H4), C6(H6)
6.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N1(H1A,H1B,H1C), N1(H1A,H1B,H1C), N1(H1A,H1B,H1C)
6.d Idealised tetrahedral OH refined as rotating group:
 F1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1_1 Pb 0.25115(2) 0.24730(2) 1.01289(2) 0.01040(3) Uani 0.9201(4) 1 d D U P A
1
Pb2_1 Pb 0.24892(2) -0.25918(2) 0.98721(2) 0.01033(3) Uani 0.9201(4) 1 d D U P
A 1
I1_1 I 0.49836(2) 0.31446(2) 0.99728(2) 0.01331(5) Uani 0.9201(4) 1 d D U P A 1
I2_1 I 0.18612(2) 0.49544(2) 1.00136(2) 0.01390(5) Uani 0.9201(4) 1 d D U P A 1
I3_1 I -0.00164(2) 0.18448(2) 0.99715(2) 0.01337(5) Uani 0.9201(4) 1 d D U P A
1
I4_1 I 0.21590(7) 0.19028(6) 0.80630(4) 0.01335(8) Uani 0.9201(4) 1 d D U P A 1
I5_1 I 0.28298(11) 0.30078(9) 1.19879(4) 0.01593(8) Uani 0.9201(4) 1 d D U P A
1
I6_1 I 0.31387(2) -0.00516(2) 0.99876(2) 0.01376(5) Uani 0.9201(4) 1 d D U P A
1
I7_1 I 0.28392(6) -0.21351(3) 1.19376(3) 0.01341(7) Uani 0.9201(4) 1 d D U P A
1
I8_1 I 0.21766(5) -0.29740(3) 0.80166(3) 0.01539(7) Uani 0.9201(4) 1 d D U P A
1
Pb1_2 Pb 0.24952(17) 0.24028(16) 0.98599(12) 0.01040(3) Uani 0.0799(4) 1 d D U
P A 2
Pb2_2 Pb 0.25078(17) -0.25275(16) 1.01393(12) 0.01033(3) Uani 0.0799(4) 1 d D U
P A 2
I1_2 I 0.5018(2) 0.1859(2) 1.00243(16) 0.01331(5) Uani 0.0799(4) 1 d D U P A 2
I2_2 I 0.3138(2) 0.4949(2) 0.99890(18) 0.0173(5) Uani 0.0799(4) 1 d D U P A 2
I3_2 I 0.0017(2) 0.3160(2) 1.00223(16) 0.01337(5) Uani 0.0799(4) 1 d D U P A 2
I4_2 I 0.2168(10) 0.1992(9) 0.7975(5) 0.01335(8) Uani 0.0799(4) 1 d D U P A 2
I5_2 I 0.2831(14) 0.2935(12) 1.1890(6) 0.01593(8) Uani 0.0799(4) 1 d D U P A 2
I6_2 I 0.1856(2) -0.0051(2) 1.00090(17) 0.01376(5) Uani 0.0799(4) 1 d D U P A 2
I7_2 I 0.2810(8) -0.1957(6) 1.2017(4) 0.01341(7) Uani 0.0799(4) 1 d D U P A 2
I8_2 I 0.2159(7) -0.3146(5) 0.8085(4) 0.01539(7) Uani 0.0799(4) 1 d D U P A 2
F1_3 F 0.4500(2) 0.70559(19) 0.57102(16) 0.0359(7) Uani 1 1 d D . . . .
F2_3 F 0.73944(19) 0.4547(3) 0.56376(17) 0.0397(7) Uani 1 1 d D . . . .
N1_3 N 0.5613(2) 0.4667(3) 0.84001(18) 0.0197(6) Uani 1 1 d D . . . .
H1A_3 H 0.596755 0.511982 0.815257 0.024 Uiso 1 1 calc GR . . . .
H1B_3 H 0.592483 0.400579 0.833014 0.024 Uiso 1 1 calc GR . . . .
H1C_3 H 0.564637 0.494616 0.892772 0.024 Uiso 1 1 calc GR . . . .
C1_3 C 0.4901(2) 0.4624(2) 0.66329(18) 0.0190(7) Uani 1 1 d D . . . .
C2_3 C 0.4436(3) 0.5576(2) 0.6411(2) 0.0195(7) Uani 1 1 d D . . . .
H2_3 H 0.376336 0.582080 0.658179 0.023 Uiso 1 1 calc R . . . .
C3_3 C 0.4981(3) 0.6148(3) 0.5938(2) 0.0237(8) Uani 1 1 d D . . . .
C4_3 C 0.5981(3) 0.5839(3) 0.5669(2) 0.0250(8) Uani 1 1 d D . . . .
H4_3 H 0.633955 0.624109 0.535178 0.030 Uiso 1 1 calc R . . . .
C5_3 C 0.6416(2) 0.4899(3) 0.5899(2) 0.0248(8) Uani 1 1 d D . . . .
C6_3 C 0.5908(3) 0.4283(3) 0.6369(2) 0.0209(7) Uani 1 1 d D . . . .
H6_3 H 0.623474 0.364911 0.650677 0.025 Uiso 1 1 calc R . . . .
C7_3 C 0.4332(3) 0.3985(3) 0.71640(17) 0.0250(8) Uani 1 1 d D . . . .
H7A_3 H 0.464597 0.325324 0.712540 0.030 Uiso 1 1 calc R . . . .
H7B_3 H 0.355876 0.389180 0.696303 0.030 Uiso 1 1 calc R . . . .
C8_3 C 0.4433(3) 0.4547(3) 0.80467(17) 0.0222(7) Uani 1 1 d D . . . .
H8A_3 H 0.410797 0.527356 0.809071 0.027 Uiso 1 1 calc R . . . .
H8B_3 H 0.403101 0.411428 0.835275 0.027 Uiso 1 1 calc R . . . .
F1_4 F 0.24013(19) 0.8264(3) 0.56548(18) 0.0429(8) Uani 1 1 d D . . . .
F2_4 F -0.0507(2) 0.57989(18) 0.57010(16) 0.0377(7) Uani 1 1 d D . . . .
N1_4 N 0.0617(2) 0.9534(3) 0.84074(18) 0.0206(6) Uani 1 1 d D . . . .
H1A_4 H 0.095763 0.892520 0.819725 0.025 Uiso 1 1 calc GR . . . .
H1B_4 H 0.064957 0.958855 0.894315 0.025 Uiso 1 1 calc GR . . . .
H1C_4 H 0.094361 1.012584 0.829165 0.025 Uiso 1 1 calc GR . . . .
C1_4 C -0.0096(2) 0.8684(2) 0.66409(17) 0.0193(7) Uani 1 1 d D . . . .
C2_4 C 0.0917(3) 0.8891(2) 0.6380(2) 0.0229(8) Uani 1 1 d D . . . .
H2_4 H 0.124565 0.959223 0.652106 0.028 Uiso 1 1 calc R . . . .
C3_4 C 0.1423(2) 0.8045(3) 0.5912(2) 0.0259(9) Uani 1 1 d D . . . .
C4_4 C 0.0986(3) 0.6987(2) 0.5680(2) 0.0265(9) Uani 1 1 d D . . . .
H4_4 H 0.134680 0.642552 0.536696 0.032 Uiso 1 1 calc R . . . .
C5_4 C -0.0017(3) 0.6817(2) 0.5940(2) 0.0233(8) Uani 1 1 d D . . . .
C6_4 C -0.0566(3) 0.7627(2) 0.6413(2) 0.0205(7) Uani 1 1 d D . . . .
H6_4 H -0.124307 0.746905 0.657741 0.025 Uiso 1 1 calc R . . . .
C7_4 C -0.0669(3) 0.9586(3) 0.71698(17) 0.0258(9) Uani 1 1 d D . . . .
H7A_4 H -0.144383 0.957170 0.696995 0.031 Uiso 1 1 calc R . . . .
H7B_4 H -0.036238 1.029942 0.712664 0.031 Uiso 1 1 calc R . . . .
C8_4 C -0.0563(3) 0.9471(3) 0.80542(17) 0.0231(8) Uani 1 1 d D . . . .
H8A_4 H -0.096665 1.005677 0.835813 0.028 Uiso 1 1 calc R . . . .
H8B_4 H -0.088495 0.876708 0.810279 0.028 Uiso 1 1 calc R . . . .
F1_5 F 0.26752(19) 1.0387(3) 0.43274(17) 0.0414(8) Uani 1 1 d D . . . .
F2_5 F 0.5581(2) 0.78998(19) 0.43866(16) 0.0351(7) Uani 1 1 d D . . . .
N1_5 N 0.5197(3) 0.9457(2) 0.15807(17) 0.0198(6) Uani 1 1 d D . . . .
H1A_5 H 0.501261 0.938490 0.104868 0.024 Uiso 1 1 calc GR . . . .
H1B_5 H 0.469884 0.910669 0.179764 0.024 Uiso 1 1 calc GR . . . .
H1C_5 H 0.585479 0.916542 0.167139 0.024 Uiso 1 1 calc GR . . . .
C1_5 C 0.5196(2) 1.0245(2) 0.33661(18) 0.0200(7) Uani 1 1 d D . . . .
C2_5 C 0.4176(3) 1.0594(3) 0.3604(2) 0.0238(8) Uani 1 1 d D . . . .
H2_5 H 0.385076 1.121231 0.343756 0.029 Uiso 1 1 calc R . . . .
C3_5 C 0.3655(2) 1.0016(3) 0.4086(2) 0.0268(9) Uani 1 1 d D . . . .
C4_5 C 0.4087(3) 0.9097(3) 0.4356(2) 0.0281(9) Uani 1 1 d D . . . .
H4_5 H 0.372015 0.871646 0.468278 0.034 Uiso 1 1 calc R . . . .
C5_5 C 0.5095(3) 0.8777(3) 0.4114(2) 0.0251(8) Uani 1 1 d D . . . .
C6_5 C 0.5663(3) 0.9326(3) 0.3635(2) 0.0219(7) Uani 1 1 d D . . . .
H6_5 H 0.635038 0.908453 0.349330 0.026 Uiso 1 1 calc R . . . .
C7_5 C 0.5785(3) 1.0845(3) 0.28217(17) 0.0233(8) Uani 1 1 d D . . . .
H7A_5 H 0.653763 1.059486 0.281822 0.028 Uiso 1 1 calc R . . . .
H7B_5 H 0.580731 1.163292 0.304203 0.028 Uiso 1 1 calc R . . . .
C8_5 C 0.5239(3) 1.0661(2) 0.19579(17) 0.0223(8) Uani 1 1 d D . . . .
H8A_5 H 0.449634 1.094126 0.195559 0.027 Uiso 1 1 calc R . . . .
H8B_5 H 0.564433 1.106999 0.163838 0.027 Uiso 1 1 calc R . . . .
F1_6 F 1.0563(2) 0.92805(18) 0.43725(16) 0.0358(7) Uani 1 1 d D . . . .
H1_6 H 1.013309 0.975395 0.425551 0.054 Uiso 1 1 calc GR . . . .
F2_6 F 0.76820(19) 0.6751(3) 0.43441(17) 0.0400(7) Uani 1 1 d D . . . .
N1_6 N 1.0201(3) 0.6327(2) 0.15838(17) 0.0190(6) Uani 1 1 d D . . . .
H1A_6 H 0.998878 0.613950 0.105518 0.023 Uiso 1 1 calc GR . . . .
H1B_6 H 1.086573 0.664750 0.165683 0.023 Uiso 1 1 calc GR . . . .
H1C_6 H 0.972350 0.679746 0.181592 0.023 Uiso 1 1 calc GR . . . .
C1_6 C 1.0197(2) 0.6421(2) 0.33695(17) 0.0187(7) Uani 1 1 d D . . . .
C2_6 C 1.0650(3) 0.7483(2) 0.36233(19) 0.0200(7) Uani 1 1 d D . . . .
H2_6 H 1.132312 0.766425 0.346420 0.024 Uiso 1 1 calc R . . . .
C3_6 C 1.0090(3) 0.8261(2) 0.4112(2) 0.0240(8) Uani 1 1 d D . . . .
C4_6 C 0.9081(3) 0.8060(2) 0.4357(2) 0.0252(8) Uani 1 1 d D . . . .
H4_6 H 0.870796 0.860388 0.467716 0.030 Uiso 1 1 calc R . . . .
C5_6 C 0.8661(2) 0.7004(3) 0.4097(2) 0.0261(9) Uani 1 1 d D . . . .
C6_6 C 0.9180(3) 0.6186(2) 0.3609(2) 0.0233(8) Uani 1 1 d D . . . .
H6_6 H 0.885535 0.548516 0.344223 0.028 Uiso 1 1 calc R . . . .
C7_6 C 1.0782(3) 0.5548(3) 0.28246(17) 0.0226(8) Uani 1 1 d D . . . .
H7A_6 H 1.079822 0.486818 0.304301 0.027 Uiso 1 1 calc R . . . .
H7B_6 H 1.153738 0.579187 0.282392 0.027 Uiso 1 1 calc R . . . .
C8_6 C 1.0241(3) 0.5310(2) 0.19598(17) 0.0221(7) Uani 1 1 d D . . . .
H8A_6 H 1.064874 0.474330 0.164030 0.026 Uiso 1 1 calc R . . . .
H8B_6 H 0.949876 0.502682 0.195440 0.026 Uiso 1 1 calc R . . . .


_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_1 I1_1 3.180(4) . ?
Pb1_1 I2_1 3.1817(9) . ?
Pb1_1 I3_1 3.156(5) . ?
Pb1_1 I4_1 3.407(8) . ?
Pb1_1 I5_1 3.067(7) . ?
Pb1_1 I6_1 3.1643(10) . ?
Pb2_1 I1_1 3.156(4) 2_657 ?
Pb2_1 I2_1 3.1638(10) 1_545 ?
Pb2_1 I3_1 3.180(4) 2_557 ?
Pb2_1 I6_1 3.1833(9) . ?
Pb2_1 I7_1 3.406(8) . ?
Pb2_1 I8_1 3.061(7) . ?
Pb1_2 I1_2 3.148(6) . ?
Pb1_2 I2_2 3.186(4) . ?
Pb1_2 I3_2 3.191(6) . ?
Pb1_2 I4_2 3.109(11) . ?
Pb1_2 I5_2 3.347(12) . ?
Pb1_2 I6_2 3.171(3) . ?
Pb2_2 I1_2 3.184(6) 2_657 ?
Pb2_2 I2_2 3.162(4) 1_545 ?
Pb2_2 I3_2 3.153(6) 2_557 ?
Pb2_2 I6_2 3.182(3) . ?
Pb2_2 I7_2 3.098(10) . ?
Pb2_2 I8_2 3.390(10) . ?
F1_3 C3_3 1.357(4) . ?
F2_3 C5_3 1.360(7) . ?
N1_3 H1A_3 0.8900 . ?
N1_3 H1B_3 0.8900 . ?
N1_3 H1C_3 0.8900 . ?
N1_3 C8_3 1.498(10) . ?
C1_3 C2_3 1.393(4) . ?
C1_3 C6_3 1.391(7) . ?
C1_3 C7_3 1.510(8) . ?
C2_3 H2_3 0.9300 . ?
C2_3 C3_3 1.373(7) . ?
C3_3 C4_3 1.377(8) . ?
C4_3 H4_3 0.9300 . ?
C4_3 C5_3 1.372(4) . ?
C5_3 C6_3 1.378(7) . ?
C6_3 H6_3 0.9300 . ?
C7_3 H7A_3 0.9700 . ?
C7_3 H7B_3 0.9700 . ?
C7_3 C8_3 1.515(4) . ?
C8_3 H8A_3 0.9700 . ?
C8_3 H8B_3 0.9700 . ?
F1_4 C3_4 1.356(7) . ?
F2_4 C5_4 1.360(4) . ?
N1_4 H1A_4 0.8900 . ?
N1_4 H1B_4 0.8900 . ?
N1_4 H1C_4 0.8900 . ?
N1_4 C8_4 1.498(10) . ?
C1_4 C2_4 1.393(7) . ?
C1_4 C6_4 1.391(4) . ?
C1_4 C7_4 1.511(8) . ?
C2_4 H2_4 0.9300 . ?
C2_4 C3_4 1.374(7) . ?
C3_4 C4_4 1.377(4) . ?
C4_4 H4_4 0.9300 . ?
C4_4 C5_4 1.371(8) . ?
C5_4 C6_4 1.377(7) . ?
C6_4 H6_4 0.9300 . ?
C7_4 H7A_4 0.9700 . ?
C7_4 H7B_4 0.9700 . ?
C7_4 C8_4 1.515(4) . ?
C8_4 H8A_4 0.9700 . ?
C8_4 H8B_4 0.9700 . ?
F1_5 C3_5 1.356(7) . ?
F2_5 C5_5 1.359(4) . ?
N1_5 H1A_5 0.8900 . ?
N1_5 H1B_5 0.8900 . ?
N1_5 H1C_5 0.8900 . ?
N1_5 C8_5 1.497(3) . ?
C1_5 C2_5 1.393(7) . ?
C1_5 C6_5 1.391(4) . ?
C1_5 C7_5 1.511(8) . ?
C2_5 H2_5 0.9300 . ?
C2_5 C3_5 1.373(7) . ?
C3_5 C4_5 1.377(5) . ?
C4_5 H4_5 0.9300 . ?
C4_5 C5_5 1.371(7) . ?
C5_5 C6_5 1.378(8) . ?
C6_5 H6_5 0.9300 . ?
C7_5 H7A_5 0.9700 . ?
C7_5 H7B_5 0.9700 . ?
C7_5 C8_5 1.515(12) . ?
C8_5 H8A_5 0.9700 . ?
C8_5 H8B_5 0.9700 . ?
F1_6 H1_6 0.8200 . ?
F1_6 C3_6 1.356(4) . ?
F2_6 C5_6 1.360(7) . ?
N1_6 H1A_6 0.8900 . ?
N1_6 H1B_6 0.8900 . ?
N1_6 H1C_6 0.8900 . ?
N1_6 C8_6 1.497(3) . ?
C1_6 C2_6 1.392(4) . ?
C1_6 C6_6 1.391(7) . ?
C1_6 C7_6 1.511(8) . ?
C2_6 H2_6 0.9300 . ?
C2_6 C3_6 1.374(8) . ?
C3_6 C4_6 1.377(7) . ?
C4_6 H4_6 0.9300 . ?
C4_6 C5_6 1.372(4) . ?
C5_6 C6_6 1.378(7) . ?
C6_6 H6_6 0.9300 . ?
C7_6 H7A_6 0.9700 . ?
C7_6 H7B_6 0.9700 . ?
C7_6 C8_6 1.515(11) . ?
C8_6 H8A_6 0.9700 . ?
C8_6 H8B_6 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
I1_1 Pb1_1 I2_1 87.89(4) . . ?
I1_1 Pb1_1 I4_1 86.8(10) . . ?
I2_1 Pb1_1 I4_1 87.4(3) . . ?
I3_1 Pb1_1 I1_1 170.27(3) . . ?
I3_1 Pb1_1 I2_1 88.90(8) . . ?
I3_1 Pb1_1 I4_1 83.8(10) . . ?
I3_1 Pb1_1 I6_1 90.87(5) . . ?
I5_1 Pb1_1 I1_1 93.0(10) . . ?
I5_1 Pb1_1 I2_1 92.1(3) . . ?
I5_1 Pb1_1 I3_1 96.3(10) . . ?
I5_1 Pb1_1 I4_1 179.50(2) . . ?
I5_1 Pb1_1 I6_1 95.5(3) . . ?
I6_1 Pb1_1 I1_1 91.10(9) . . ?
I6_1 Pb1_1 I2_1 172.345(12) . . ?
I6_1 Pb1_1 I4_1 84.9(2) . . ?
I1_1 Pb2_1 I2_1 90.84(6) 2_657 1_545 ?
I1_1 Pb2_1 I3_1 170.35(3) 2_657 2_557 ?
I1_1 Pb2_1 I6_1 88.98(8) 2_657 . ?
I1_1 Pb2_1 I7_1 84.0(10) 2_657 . ?
I2_1 Pb2_1 I3_1 91.03(9) 1_545 2_557 ?
I2_1 Pb2_1 I6_1 172.330(11) 1_545 . ?
I2_1 Pb2_1 I7_1 84.9(2) 1_545 . ?
I3_1 Pb2_1 I6_1 87.90(4) 2_557 . ?
I3_1 Pb2_1 I7_1 86.8(10) 2_557 . ?
I6_1 Pb2_1 I7_1 87.4(3) . . ?
I8_1 Pb2_1 I1_1 96.1(10) . 2_657 ?
I8_1 Pb2_1 I2_1 95.7(3) . 1_545 ?
I8_1 Pb2_1 I3_1 93.1(10) . 2_557 ?
I8_1 Pb2_1 I6_1 92.0(3) . . ?
I8_1 Pb2_1 I7_1 179.354(12) . . ?
Pb2_1 I1_1 Pb1_1 149.292(12) 2_657 . ?
Pb2_1 I2_1 Pb1_1 151.408(17) 1_565 . ?
Pb1_1 I3_1 Pb2_1 149.364(13) . 2_557 ?
Pb1_1 I6_1 Pb2_1 151.457(17) . . ?
I1_2 Pb1_2 I2_2 89.00(12) . . ?
I1_2 Pb1_2 I3_2 169.84(11) . . ?
I1_2 Pb1_2 I5_2 84.2(10) . . ?
I1_2 Pb1_2 I6_2 91.17(10) . . ?
I2_2 Pb1_2 I3_2 87.52(10) . . ?
I2_2 Pb1_2 I5_2 85.3(4) . . ?
I3_2 Pb1_2 I5_2 86.0(10) . . ?
I4_2 Pb1_2 I1_2 96.5(10) . . ?
I4_2 Pb1_2 I2_2 92.9(3) . . ?
I4_2 Pb1_2 I3_2 93.2(10) . . ?
I4_2 Pb1_2 I5_2 178.1(3) . . ?
I4_2 Pb1_2 I6_2 95.4(3) . . ?
I6_2 Pb1_2 I2_2 171.67(10) . . ?
I6_2 Pb1_2 I3_2 90.90(13) . . ?
I6_2 Pb1_2 I5_2 86.4(4) . . ?
I1_2 Pb2_2 I8_2 86.9(10) 2_657 . ?
I2_2 Pb2_2 I6_2 171.62(10) 1_545 . ?
I2_2 Pb2_2 I8_2 83.6(3) 1_545 . ?
I3_2 Pb2_2 I6_2 88.95(12) 2_557 . ?
I3_2 Pb2_2 I8_2 83.5(10) 2_557 . ?
I6_2 Pb2_2 I8_2 88.0(3) . . ?
I7_2 Pb2_2 I3_2 96.2(10) . 2_557 ?
I7_2 Pb2_2 I6_2 91.8(3) . . ?
I7_2 Pb2_2 I8_2 179.6(2) . . ?
Pb2_2 I2_2 Pb1_2 151.54(12) 1_565 . ?
Pb2_2 I3_2 Pb1_2 149.04(11) 2_557 . ?
Pb1_2 I6_2 Pb2_2 151.18(12) . . ?
H1A_3 N1_3 H1B_3 109.5 . . ?
H1A_3 N1_3 H1C_3 109.5 . . ?
H1B_3 N1_3 H1C_3 109.5 . . ?
C8_3 N1_3 H1A_3 109.5 . . ?
C8_3 N1_3 H1B_3 109.5 . . ?
C8_3 N1_3 H1C_3 109.5 . . ?
C2_3 C1_3 C7_3 120.6(3) . . ?
C6_3 C1_3 C2_3 118.9(3) . . ?
C6_3 C1_3 C7_3 120.5(5) . . ?
C1_3 C2_3 H2_3 120.4 . . ?
C3_3 C2_3 C1_3 119.2(3) . . ?
C3_3 C2_3 H2_3 120.4 . . ?
F1_3 C3_3 C2_3 118.3(3) . . ?
F1_3 C3_3 C4_3 118.1(3) . . ?
C2_3 C3_3 C4_3 123.5(5) . . ?
C3_3 C4_3 H4_3 122.1 . . ?
C5_3 C4_3 C3_3 115.7(3) . . ?
C5_3 C4_3 H4_3 122.1 . . ?
F2_3 C5_3 C4_3 118.1(3) . . ?
F2_3 C5_3 C6_3 118.3(5) . . ?
C4_3 C5_3 C6_3 123.7(3) . . ?
C1_3 C6_3 H6_3 120.5 . . ?
C5_3 C6_3 C1_3 119.0(5) . . ?
C5_3 C6_3 H6_3 120.5 . . ?
C1_3 C7_3 H7A_3 109.0 . . ?
C1_3 C7_3 H7B_3 109.0 . . ?
C1_3 C7_3 C8_3 113.1(4) . . ?
H7A_3 C7_3 H7B_3 107.8 . . ?
C8_3 C7_3 H7A_3 109.0 . . ?
C8_3 C7_3 H7B_3 109.0 . . ?
N1_3 C8_3 C7_3 111.3(9) . . ?
N1_3 C8_3 H8A_3 109.4 . . ?
N1_3 C8_3 H8B_3 109.4 . . ?
C7_3 C8_3 H8A_3 109.4 . . ?
C7_3 C8_3 H8B_3 109.4 . . ?
H8A_3 C8_3 H8B_3 108.0 . . ?
H1A_4 N1_4 H1B_4 109.5 . . ?
H1A_4 N1_4 H1C_4 109.5 . . ?
H1B_4 N1_4 H1C_4 109.5 . . ?
C8_4 N1_4 H1A_4 109.5 . . ?
C8_4 N1_4 H1B_4 109.5 . . ?
C8_4 N1_4 H1C_4 109.5 . . ?
C2_4 C1_4 C7_4 120.7(5) . . ?
C6_4 C1_4 C2_4 118.8(3) . . ?
C6_4 C1_4 C7_4 120.5(3) . . ?
C1_4 C2_4 H2_4 120.5 . . ?
C3_4 C2_4 C1_4 119.1(5) . . ?
C3_4 C2_4 H2_4 120.5 . . ?
F1_4 C3_4 C2_4 118.3(5) . . ?
F1_4 C3_4 C4_4 118.0(3) . . ?
C2_4 C3_4 C4_4 123.7(3) . . ?
C3_4 C4_4 H4_4 122.2 . . ?
C5_4 C4_4 C3_4 115.6(3) . . ?
C5_4 C4_4 H4_4 122.2 . . ?
F2_4 C5_4 C4_4 118.1(3) . . ?
F2_4 C5_4 C6_4 118.3(3) . . ?
C4_4 C5_4 C6_4 123.6(5) . . ?
C1_4 C6_4 H6_4 120.4 . . ?
C5_4 C6_4 C1_4 119.2(3) . . ?
C5_4 C6_4 H6_4 120.4 . . ?
C1_4 C7_4 H7A_4 108.9 . . ?
C1_4 C7_4 H7B_4 108.9 . . ?
C1_4 C7_4 C8_4 113.2(4) . . ?
H7A_4 C7_4 H7B_4 107.8 . . ?
C8_4 C7_4 H7A_4 108.9 . . ?
C8_4 C7_4 H7B_4 108.9 . . ?
N1_4 C8_4 C7_4 111.4(9) . . ?
N1_4 C8_4 H8A_4 109.3 . . ?
N1_4 C8_4 H8B_4 109.3 . . ?
C7_4 C8_4 H8A_4 109.3 . . ?
C7_4 C8_4 H8B_4 109.3 . . ?
H8A_4 C8_4 H8B_4 108.0 . . ?
H1A_5 N1_5 H1B_5 109.5 . . ?
H1A_5 N1_5 H1C_5 109.5 . . ?
H1B_5 N1_5 H1C_5 109.5 . . ?
C8_5 N1_5 H1A_5 109.5 . . ?
C8_5 N1_5 H1B_5 109.5 . . ?
C8_5 N1_5 H1C_5 109.5 . . ?
C2_5 C1_5 C7_5 120.8(5) . . ?
C6_5 C1_5 C2_5 118.8(3) . . ?
C6_5 C1_5 C7_5 120.4(3) . . ?
C1_5 C2_5 H2_5 120.4 . . ?
C3_5 C2_5 C1_5 119.2(5) . . ?
C3_5 C2_5 H2_5 120.4 . . ?
F1_5 C3_5 C2_5 118.2(5) . . ?
F1_5 C3_5 C4_5 118.2(4) . . ?
C2_5 C3_5 C4_5 123.6(3) . . ?
C3_5 C4_5 H4_5 122.1 . . ?
C5_5 C4_5 C3_5 115.7(4) . . ?
C5_5 C4_5 H4_5 122.1 . . ?
F2_5 C5_5 C4_5 118.3(4) . . ?
F2_5 C5_5 C6_5 118.0(3) . . ?
C4_5 C5_5 C6_5 123.6(5) . . ?
C1_5 C6_5 H6_5 120.4 . . ?
C5_5 C6_5 C1_5 119.1(3) . . ?
C5_5 C6_5 H6_5 120.4 . . ?
C1_5 C7_5 H7A_5 109.0 . . ?
C1_5 C7_5 H7B_5 109.0 . . ?
C1_5 C7_5 C8_5 112.9(3) . . ?
H7A_5 C7_5 H7B_5 107.8 . . ?
C8_5 C7_5 H7A_5 109.0 . . ?
C8_5 C7_5 H7B_5 109.0 . . ?
N1_5 C8_5 C7_5 111.4(2) . . ?
N1_5 C8_5 H8A_5 109.3 . . ?
N1_5 C8_5 H8B_5 109.3 . . ?
C7_5 C8_5 H8A_5 109.3 . . ?
C7_5 C8_5 H8B_5 109.3 . . ?
H8A_5 C8_5 H8B_5 108.0 . . ?
C3_6 F1_6 H1_6 109.5 . . ?
H1A_6 N1_6 H1B_6 109.5 . . ?
H1A_6 N1_6 H1C_6 109.5 . . ?
H1B_6 N1_6 H1C_6 109.5 . . ?
C8_6 N1_6 H1A_6 109.5 . . ?
C8_6 N1_6 H1B_6 109.5 . . ?
C8_6 N1_6 H1C_6 109.5 . . ?
C2_6 C1_6 C7_6 120.7(3) . . ?
C6_6 C1_6 C2_6 118.8(3) . . ?
C6_6 C1_6 C7_6 120.5(5) . . ?
C1_6 C2_6 H2_6 120.4 . . ?
C3_6 C2_6 C1_6 119.2(3) . . ?
C3_6 C2_6 H2_6 120.4 . . ?
F1_6 C3_6 C2_6 118.2(3) . . ?
F1_6 C3_6 C4_6 118.2(3) . . ?
C2_6 C3_6 C4_6 123.6(5) . . ?
C3_6 C4_6 H4_6 122.2 . . ?
C5_6 C4_6 C3_6 115.6(3) . . ?
C5_6 C4_6 H4_6 122.2 . . ?
F2_6 C5_6 C4_6 118.0(4) . . ?
F2_6 C5_6 C6_6 118.3(5) . . ?
C4_6 C5_6 C6_6 123.7(3) . . ?
C1_6 C6_6 H6_6 120.5 . . ?
C5_6 C6_6 C1_6 119.1(5) . . ?
C5_6 C6_6 H6_6 120.5 . . ?
C1_6 C7_6 H7A_6 109.0 . . ?
C1_6 C7_6 H7B_6 109.0 . . ?
C1_6 C7_6 C8_6 113.0(3) . . ?
H7A_6 C7_6 H7B_6 107.8 . . ?
C8_6 C7_6 H7A_6 109.0 . . ?
C8_6 C7_6 H7B_6 109.0 . . ?
N1_6 C8_6 C7_6 111.7(2) . . ?
N1_6 C8_6 H8A_6 109.3 . . ?
N1_6 C8_6 H8B_6 109.3 . . ?
C7_6 C8_6 H8A_6 109.3 . . ?
C7_6 C8_6 H8B_6 109.3 . . ?
H8A_6 C8_6 H8B_6 107.9 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 'The crystal was mounted on a None'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.770
_oxdiff_exptl_absorpt_empirical_full_min 0.600
_oxdiff_exptl_absorpt_spherical_max 0.403
_oxdiff_exptl_absorpt_spherical_min 0.381
####################################################################### 
# 
# 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_3me-pea
_database_code_depnum_ccdc_archive 'CCDC 1986785'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2020-02-27 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
_audit_creation_date             2020-02-21
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6020)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
mtremblay6@gatech.edu
john.bacsa@emory.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4.008 Pb, 2(C9 H14 N)'
_chemical_formula_sum            'C18 H28 I4.01 N2 Pb'
_chemical_formula_weight         988.16
_chemical_melting_point          ?
_chemical_oxdiff_formula         C18H28I4N2Pb2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.32860(10)
_cell_length_b                   19.0688(2)
_cell_length_c                   24.3751(2)
_cell_angle_alpha                67.7520(10)
_cell_angle_beta                 89.9860(10)
_cell_angle_gamma                80.6850(10)
_cell_volume                     5222.14(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    45885
_cell_measurement_temperature    104(7)
_cell_measurement_theta_max      38.1030
_cell_measurement_theta_min      2.3320
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.205
_exptl_absorpt_correction_T_max  0.399
_exptl_absorpt_correction_T_min  0.029
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.514
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3555
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 -3 -2 0.1567
5 3 2 0.1700
-5 0 -3 0.1458
5 0 3 0.1600
0 0 -1 0.0639
0 -24 -25 0.0500
-17 0 2 0.1525
0 -24 1 0.0400
0 24 -1 0.0444
0 -7 -34 0.0587
-17 -8 4 0.1549
0 1 32 0.0635
0 16 33 0.0513
2 8 -26 0.0629
11 23 7 0.1178

_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.084
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.9964 -2.9874 -2.0006 -0.0087 -0.0101 0.2967
4.9964 2.9874 2.0006 0.0087 0.0101 -0.2967
-4.9944 0.0168 -2.9895 0.1234 -0.0462 0.2837
4.9944 -0.0168 2.9895 -0.1234 0.0462 -0.2837
0.0005 0.0024 -0.9978 0.0244 0.0192 0.0051
-0.0015 -23.9562 -25.0180 -0.2507 0.9212 0.2731
-16.9864 0.0285 2.0096 0.1216 -0.3908 0.9020
-0.0134 -24.0174 0.9261 -0.8861 0.4228 0.1400
0.0134 24.0174 -0.9261 0.8861 -0.4228 -0.1400
0.0118 -6.9244 -33.9478 0.5795 0.7807 0.2164
-16.9917 -7.9812 3.9814 -0.2145 -0.2818 0.9401
-0.0141 0.9253 31.9342 -0.7461 -0.6319 -0.1699
-0.0065 15.9324 32.9769 -0.2320 -0.9273 -0.2656
2.0145 8.0623 -25.9218 0.9025 0.3926 -0.0226
10.9998 22.9764 7.0447 0.5444 -0.3297 -0.7651

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.0774
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            69618
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         1.174
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      104(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -45.00  38.00   0.50    7.00    --   25.84 -38.00 -90.00  166
  2  ω     10.00  98.00   0.50    7.00    --   25.84  57.00-150.00  176
  3  ω      3.00  93.00   0.50    7.00    --   25.84  77.00 -30.00  180
  4  ω     46.00  71.00   0.50    7.00    --   25.84 171.00  44.00   50
  5  ω     39.00  81.00   0.50    7.00    --   25.84 178.00  90.00   84
  6  ω      4.00  96.00   0.50    7.00    --   25.84  77.00  90.00  184
  7  ω     26.00  98.00   0.50    7.00    --   25.84  57.00  60.00  144
  8  ω     54.00  97.00   0.50    7.00    --   25.84 178.00 -90.00   86
  9  ω      2.00   5.50   0.50    7.00    --   25.84  77.00-120.00    7
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0099840000
_diffrn_orient_matrix_UB_12      0.0359585000
_diffrn_orient_matrix_UB_13      -0.0244092000
_diffrn_orient_matrix_UB_21      0.0206989000
_diffrn_orient_matrix_UB_22      -0.0183583000
_diffrn_orient_matrix_UB_23      -0.0192452000
_diffrn_orient_matrix_UB_31      -0.0537233000
_diffrn_orient_matrix_UB_32      -0.0059969000
_diffrn_orient_matrix_UB_33      -0.0051688000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                21681
_reflns_number_total             25770
_reflns_odcompleteness_completeness 97.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.365
_refine_diff_density_min         -1.888
_refine_diff_density_rms         0.344
_refine_ls_extinction_coef       0.000182(12)
_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   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         25770
_refine_ls_number_restraints     924
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0434
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0471P)²+2.3327P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1144
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(I8B) = Uanis(I2_8)
Uanis(I2_8) = Uanis(I8B)
Uanis(I3_8) = Uanis(I6B)
Uanis(I5B) = Uanis(I1_8)
Uanis(I1) = Uanis(I2_8)
Uanis(I2B) = Uanis(I6_8)
Uanis(I1B) = Uanis(I1_8)
Uanis(I3B) = Uanis(I3_8)
Uanis(I4_8) = Uanis(I4B)
Uanis(Pb2B) = Uanis(Pb2A_8)
Uanis(Pb3A) = Uanis(Pb3B_8)
Uanis(I14B) = Uanis(I9_8)
3. Rigid body (RIGU) restrains
 N6_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1, C9_1
 N6_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2, C9_2
 N6_3, C1_3, C2_3, C3_3, C4_3, C5_3, C6_3, C7_3, C8_3, C9_3
 N6_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4, C7_4, C8_4, C9_4
 N6_5, C1_5, C2_5, C3_5, C4_5, C5_5, C6_5, C7_5, C8_5, C9_5
 N6_6, C1_6, C2_6, C3_6, C4_6, C5_6, C6_6, C7_6, C8_6, C9_6
 N6_7, C1_7, C2_7, C3_7, C4_7, C5_7, C6_7, C7_7, C8_7, C9_7
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{N6_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2, C9_2}
{N6_3, C1_3, C2_3, C3_3, C4_3, C5_3, C6_3, C7_3, C8_3, C9_3}
{N6_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4, C7_4, C8_4, C9_4}
{N6_5, C1_5, C2_5, C3_5, C4_5, C5_5, C6_5, C7_5, C8_5, C9_5}
{N6_6, C1_6, C2_6, C3_6, C4_6, C5_6, C6_6, C7_6, C8_6, C9_6}
{N6_7, C1_7, C2_7, C3_7, C4_7, C5_7, C6_7, C7_7, C8_7, C9_7}
as
{N6_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1, C9_1} sigma for 1-2:
0.002 1-3: 0.004
5. Others
 Sof(Pb2B)=Sof(I1)=Sof(I1B)=Sof(I2B)=Sof(I3B)=Sof(I4B)=Sof(I5B)=Sof(I6B)=
 Sof(I8B)=Sof(I14B)=Sof(Pb3B)=1-FVAR(1)
 Sof(Pb3A)=Sof(Pb2A)=Sof(I1)=Sof(I2)=Sof(I3)=Sof(I4)=Sof(I5)=Sof(I6)=Sof(I7)=
 Sof(I9)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B),
 C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B),
 C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C2(H2), C4(H4), C5(H5), C6(H6), C2(H2),
 C4(H4), C5(H5), C6(H6), C2(H2), C4(H4), C5(H5), C6(H6), C2(H2), C4(H4), C5(H5),
  C6(H6), C2(H2), C4(H4), C5(H5), C6(H6), C2(H2), C4(H4), C5(H5), C6(H6),
 C2(H2), C4(H4), C5(H5), C6(H6)
6.c Idealised Me refined as rotating group:
 N6(H6A,H6B,H6C), C9(H9A,H9B,H9C), N6(H6A,H6B,H6C), C9(H9A,H9B,H9C), N6(H6A,
 H6B,H6C), C9(H9A,H9B,H9C), N6(H6A,H6B,H6C), C9(H9A,H9B,H9C), N6(H6A,H6B,H6C),
 C9(H9A,H9B,H9C), N6(H6A,H6B,H6C), C9(H9A,H9B,H9C), N6(H6A,H6B,H6C), C9(H9A,H9B,
 H9C), N6(H6A,H6B,H6C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb2B Pb 0.4968(7) 0.4869(5) 0.7528(4) 0.01158(6) Uani 0.0318(5) 1 d . . P A 2
Pb3A Pb 1.00912(2) 0.51151(2) 0.24696(2) 0.01165(6) Uani 0.9682(5) 1 d . . P A
1
I1 I 0.7486(7) 0.5012(5) -0.0311(4) 0.01411(8) Uani 0.0318(5) 1 d . . P A 2
I1B I 0.5553(8) 0.5013(5) 0.6249(4) 0.01434(8) Uani 0.0318(5) 1 d . . P A 2
I2B I 0.7367(8) 0.4989(5) 0.7810(4) 0.01427(8) Uani 0.0318(5) 1 d . . P A 2
I3B I 0.9283(8) 0.4989(5) 0.6243(4) 0.01458(8) Uani 0.0318(5) 1 d . . P A 2
I4B I 0.7509(7) 0.5010(5) 0.4684(4) 0.01436(8) Uani 0.0318(5) 1 d . . P A 2
I5B I 0.4286(8) 0.5013(5) 0.8745(4) 0.01434(8) Uani 0.0318(5) 1 d . . P A 2
I6B I 1.0551(8) 0.4992(5) 0.8744(4) 0.01458(8) Uani 0.0318(5) 1 d . . P A 2
I8B I 1.2355(8) 0.5004(5) 0.7200(4) 0.01411(8) Uani 0.0318(5) 1 d . . P A 2
I14B I 0.451(2) 0.6867(16) 0.4537(11) 0.01475(11) Uani 0.0318(5) 1 d . . P A 2
N6 N 0.7010(3) 0.6521(2) 0.78960(19) 0.0195(9) Uani 1 1 d . . . . .
H6A H 0.639404 0.674571 0.764619 0.023 Uiso 1 1 calc R U . . .
H6B H 0.703555 0.600272 0.806110 0.023 Uiso 1 1 calc R U . . .
H6C H 0.761741 0.662557 0.768872 0.023 Uiso 1 1 calc R U . . .
C1 C 0.6348(4) 0.8198(3) 0.7650(2) 0.0183(10) Uani 1 1 d . . . . .
C2 C 0.5337(4) 0.8495(3) 0.7794(2) 0.0235(11) Uani 1 1 d . . . . .
H2 H 0.518191 0.834392 0.819992 0.028 Uiso 1 1 calc R U . . .
C3 C 0.4537(4) 0.9011(3) 0.7360(3) 0.0245(11) Uani 1 1 d . . . . .
C4 C 0.4775(4) 0.9199(3) 0.6770(2) 0.0283(12) Uani 1 1 d . . . . .
H4 H 0.424041 0.953881 0.646596 0.034 Uiso 1 1 calc R U . . .
C5 C 0.5768(5) 0.8907(3) 0.6616(2) 0.0300(12) Uani 1 1 d . . . . .
H5 H 0.591245 0.904655 0.620852 0.036 Uiso 1 1 calc R U . . .
C6 C 0.6560(5) 0.8406(3) 0.7053(2) 0.0239(11) Uani 1 1 d . . . . .
H6 H 0.724588 0.820581 0.694536 0.029 Uiso 1 1 calc R U . . .
C7 C 0.7199(4) 0.7652(3) 0.8131(2) 0.0227(11) Uani 1 1 d . . . . .
H7A H 0.720594 0.783404 0.846150 0.027 Uiso 1 1 calc R U . . .
H7B H 0.793595 0.765956 0.797013 0.027 Uiso 1 1 calc R U . . .
C8 C 0.6981(5) 0.6829(3) 0.8373(2) 0.0231(11) Uani 1 1 d . . . . .
H8A H 0.754523 0.650063 0.869512 0.028 Uiso 1 1 calc R U . . .
H8B H 0.625079 0.681589 0.854149 0.028 Uiso 1 1 calc R U . . .
C9 C 0.3484(4) 0.9373(3) 0.7529(3) 0.0334(13) Uani 1 1 d . . . . .
H9A H 0.333909 0.905450 0.793446 0.050 Uiso 1 1 calc R U . . .
H9B H 0.287446 0.941435 0.725405 0.050 Uiso 1 1 calc R U . . .
H9C H 0.355217 0.988795 0.750723 0.050 Uiso 1 1 calc R U . . .
N6_1 N 0.7226(3) 0.6521(2) 0.28986(17) 0.0200(9) Uani 1 1 d D . . . .
H6A_1 H 0.770850 0.676127 0.264117 0.024 Uiso 1 1 calc R U . . .
H6B_1 H 0.656251 0.660557 0.269976 0.024 Uiso 1 1 calc R U . . .
H6C_1 H 0.748943 0.600651 0.306367 0.024 Uiso 1 1 calc R U . . .
C1_1 C 0.7038(3) 0.8195(2) 0.26472(15) 0.0198(9) Uani 1 1 d D . . . .
C2_1 C 0.7905(3) 0.8492(2) 0.27910(14) 0.0216(10) Uani 1 1 d D . . . .
H2_1 H 0.813586 0.834592 0.319681 0.026 Uiso 1 1 calc R U . . .
C3_1 C 0.8447(3) 0.9004(2) 0.23508(16) 0.0252(10) Uani 1 1 d D . . . .
C4_1 C 0.8113(4) 0.9193(3) 0.17612(16) 0.0315(12) Uani 1 1 d D . . . .
H4_1 H 0.847848 0.952981 0.145533 0.038 Uiso 1 1 calc R U . . .
C5_1 C 0.7255(4) 0.8898(3) 0.16121(14) 0.0277(11) Uani 1 1 d D . . . .
H5_1 H 0.704324 0.903062 0.120569 0.033 Uiso 1 1 calc R U . . .
C6_1 C 0.6702(3) 0.8410(3) 0.20503(18) 0.0246(11) Uani 1 1 d D . . . .
H6_1 H 0.609833 0.822260 0.194508 0.030 Uiso 1 1 calc R U . . .
C7_1 C 0.6466(3) 0.76542(18) 0.31349(16) 0.0246(11) Uani 1 1 d D . . . .
H7A_1 H 0.572023 0.766234 0.297897 0.030 Uiso 1 1 calc R U . . .
H7B_1 H 0.637883 0.783900 0.346379 0.030 Uiso 1 1 calc R U . . .
C8_1 C 0.7090(4) 0.6832(2) 0.33756(16) 0.0226(11) Uani 1 1 d D . . . .
H8A_1 H 0.782445 0.681695 0.354813 0.027 Uiso 1 1 calc R U . . .
H8B_1 H 0.668499 0.650448 0.369582 0.027 Uiso 1 1 calc R U . . .
C9_1 C 0.9317(4) 0.9373(3) 0.2520(2) 0.0368(14) Uani 1 1 d D . . . .
H9A_1 H 0.899949 0.990066 0.247029 0.055 Uiso 1 1 calc R U . . .
H9B_1 H 0.993233 0.938163 0.226449 0.055 Uiso 1 1 calc R U . . .
H9C_1 H 0.958352 0.907614 0.293584 0.055 Uiso 1 1 calc R U . . .
N6_2 N 0.7902(3) 0.3476(2) 0.46050(18) 0.0204(9) Uani 1 1 d D . . . .
H6A_2 H 0.764565 0.399136 0.444316 0.024 Uiso 1 1 calc R U . . .
H6B_2 H 0.855920 0.338359 0.481173 0.024 Uiso 1 1 calc R U . . .
H6C_2 H 0.740894 0.323586 0.485457 0.024 Uiso 1 1 calc R U . . .
C1_2 C 0.8185(3) 0.1798(2) 0.48410(15) 0.0186(9) Uani 1 1 d D . . . .
C2_2 C 0.7337(3) 0.1485(2) 0.46965(14) 0.0198(9) Uani 1 1 d D . . . .
H2_2 H 0.711597 0.162416 0.429041 0.024 Uiso 1 1 calc R U . . .
C3_2 C 0.6802(3) 0.0969(2) 0.51369(15) 0.0249(10) Uani 1 1 d D . . . .
C4_2 C 0.7134(3) 0.0783(2) 0.57261(15) 0.0257(10) Uani 1 1 d D . . . .
H4_2 H 0.677605 0.043966 0.603183 0.031 Uiso 1 1 calc R U . . .
C5_2 C 0.7978(4) 0.1089(2) 0.58757(14) 0.0250(10) Uani 1 1 d D . . . .
H5_2 H 0.819004 0.095551 0.628222 0.030 Uiso 1 1 calc R U . . .
C6_2 C 0.8518(4) 0.1588(3) 0.54377(18) 0.0229(10) Uani 1 1 d D . . . .
H6_2 H 0.911077 0.178497 0.554298 0.028 Uiso 1 1 calc R U . . .
C7_2 C 0.8725(3) 0.23661(18) 0.43537(16) 0.0235(10) Uani 1 1 d D . . . .
H7A_2 H 0.882777 0.218993 0.402076 0.028 Uiso 1 1 calc R U . . .
H7B_2 H 0.946219 0.237773 0.450743 0.028 Uiso 1 1 calc R U . . .
C8_2 C 0.8054(4) 0.3175(2) 0.41226(16) 0.0225(11) Uani 1 1 d D . . . .
H8A_2 H 0.843372 0.352003 0.379943 0.027 Uiso 1 1 calc R U . . .
H8B_2 H 0.732405 0.316961 0.395619 0.027 Uiso 1 1 calc R U . . .
C9_2 C 0.5931(4) 0.0601(3) 0.4968(2) 0.0338(14) Uani 1 1 d D . . . .
H9A_2 H 0.560505 0.092853 0.456747 0.051 Uiso 1 1 calc R U . . .
H9B_2 H 0.535529 0.053956 0.525134 0.051 Uiso 1 1 calc R U . . .
H9C_2 H 0.626629 0.009510 0.497421 0.051 Uiso 1 1 calc R U . . .
N6_3 N 0.6377(3) 0.6517(2) 0.08040(18) 0.0202(9) Uani 1 1 d D . . . .
H6A_3 H 0.589633 0.678457 0.048142 0.024 Uiso 1 1 calc R U . . .
H6B_3 H 0.610673 0.660173 0.112525 0.024 Uiso 1 1 calc R U . . .
H6C_3 H 0.646667 0.600590 0.087760 0.024 Uiso 1 1 calc R U . . .
C1_3 C 0.6570(3) 0.8173(2) 0.01558(15) 0.0182(9) Uani 1 1 d D . . . .
C2_3 C 0.5575(3) 0.8503(2) 0.02963(14) 0.0211(10) Uani 1 1 d D . . . .
H2_3 H 0.541895 0.836684 0.070173 0.025 Uiso 1 1 calc R U . . .
C3_3 C 0.4795(3) 0.9033(2) -0.01459(15) 0.0211(9) Uani 1 1 d D . . . .
C4_3 C 0.5041(3) 0.9217(2) -0.07339(15) 0.0252(10) Uani 1 1 d D . . . .
H4_3 H 0.451939 0.956620 -0.104144 0.030 Uiso 1 1 calc R U . . .
C5_3 C 0.6034(3) 0.8900(2) -0.08800(14) 0.0261(11) Uani 1 1 d D . . . .
H5_3 H 0.619445 0.904479 -0.128533 0.031 Uiso 1 1 calc R U . . .
C6_3 C 0.6798(3) 0.8372(3) -0.04404(18) 0.0223(10) Uani 1 1 d D . . . .
H6_3 H 0.747173 0.814828 -0.054399 0.027 Uiso 1 1 calc R U . . .
C7_3 C 0.7384(3) 0.76001(17) 0.06451(16) 0.0227(10) Uani 1 1 d D . . . .
H7A_3 H 0.716611 0.762376 0.102940 0.027 Uiso 1 1 calc R U . . .
H7B_3 H 0.812139 0.774788 0.057559 0.027 Uiso 1 1 calc R U . . .
C8_3 C 0.7460(3) 0.67791(19) 0.0686(2) 0.0217(10) Uani 1 1 d D . . . .
H8A_3 H 0.770909 0.674699 0.030822 0.026 Uiso 1 1 calc R U . . .
H8B_3 H 0.801345 0.643397 0.100827 0.026 Uiso 1 1 calc R U . . .
C9_3 C 0.3743(3) 0.9408(3) 0.0021(2) 0.0300(12) Uani 1 1 d D . . . .
H9A_3 H 0.356550 0.907576 0.041646 0.045 Uiso 1 1 calc R U . . .
H9B_3 H 0.314120 0.948587 -0.026985 0.045 Uiso 1 1 calc R U . . .
H9C_3 H 0.383883 0.990650 0.002527 0.045 Uiso 1 1 calc R U . . .
N6_4 N 0.8798(3) 0.3482(2) 0.17350(18) 0.0211(9) Uani 1 1 d D . . . .
H6A_4 H 0.909979 0.339351 0.142135 0.025 Uiso 1 1 calc R U . . .
H6B_4 H 0.925786 0.321952 0.206694 0.025 Uiso 1 1 calc R U . . .
H6C_4 H 0.869685 0.399417 0.165817 0.025 Uiso 1 1 calc R U . . .
C1_4 C 0.8641(3) 0.1830(2) 0.23600(15) 0.0187(9) Uani 1 1 d D . . . .
C2_4 C 0.9643(3) 0.1505(2) 0.22216(14) 0.0226(10) Uani 1 1 d D . . . .
H2_4 H 0.980173 0.164209 0.181665 0.027 Uiso 1 1 calc R U . . .
C3_4 C 1.0424(3) 0.0981(2) 0.26652(15) 0.0221(10) Uani 1 1 d D . . . .
C4_4 C 1.0175(3) 0.0794(2) 0.32531(15) 0.0272(11) Uani 1 1 d D . . . .
H4_4 H 1.069450 0.044462 0.356120 0.033 Uiso 1 1 calc R U . . .
C5_4 C 0.9179(3) 0.1111(3) 0.33973(14) 0.0274(11) Uani 1 1 d D . . . .
H5_4 H 0.901974 0.097101 0.380245 0.033 Uiso 1 1 calc R U . . .
C6_4 C 0.8411(3) 0.1631(3) 0.29560(18) 0.0233(11) Uani 1 1 d D . . . .
H6_4 H 0.773209 0.184935 0.305855 0.028 Uiso 1 1 calc R U . . .
C7_4 C 0.7819(3) 0.23928(18) 0.18699(16) 0.0242(11) Uani 1 1 d D . . . .
H7A_4 H 0.708907 0.223362 0.193807 0.029 Uiso 1 1 calc R U . . .
H7B_4 H 0.804630 0.237312 0.148564 0.029 Uiso 1 1 calc R U . . .
C8_4 C 0.7715(3) 0.32151(19) 0.1831(2) 0.0220(10) Uani 1 1 d D . . . .
H8A_4 H 0.717802 0.355737 0.149907 0.026 Uiso 1 1 calc R U . . .
H8B_4 H 0.743452 0.324637 0.220319 0.026 Uiso 1 1 calc R U . . .
C9_4 C 1.1473(3) 0.0600(3) 0.2500(2) 0.0327(13) Uani 1 1 d D . . . .
H9A_4 H 1.139383 0.008315 0.253127 0.049 Uiso 1 1 calc R U . . .
H9B_4 H 1.208797 0.056185 0.277033 0.049 Uiso 1 1 calc R U . . .
H9C_4 H 1.161837 0.090724 0.209115 0.049 Uiso 1 1 calc R U . . .
N6_5 N 0.7867(3) 0.6525(2) 0.57979(18) 0.0208(9) Uani 1 1 d D . . . .
H6A_5 H 0.820798 0.676481 0.546399 0.025 Uiso 1 1 calc R U . . .
H6B_5 H 0.803021 0.600664 0.590063 0.025 Uiso 1 1 calc R U . . .
H6C_5 H 0.810590 0.664491 0.609944 0.025 Uiso 1 1 calc R U . . .
C1_5 C 0.6853(3) 0.8175(2) 0.51557(15) 0.0196(9) Uani 1 1 d D . . . .
C2_5 C 0.7682(3) 0.8507(2) 0.52951(14) 0.0203(9) Uani 1 1 d D . . . .
H2_5 H 0.790806 0.836998 0.570017 0.024 Uiso 1 1 calc R U . . .
C3_5 C 0.8192(3) 0.9039(2) 0.48521(15) 0.0230(10) Uani 1 1 d D . . . .
C4_5 C 0.7851(4) 0.9225(2) 0.42640(15) 0.0272(11) Uani 1 1 d D . . . .
H4_5 H 0.819162 0.957834 0.395623 0.033 Uiso 1 1 calc R U . . .
C5_5 C 0.7022(4) 0.8902(2) 0.41194(14) 0.0255(11) Uani 1 1 d D . . . .
H5_5 H 0.679636 0.904059 0.371403 0.031 Uiso 1 1 calc R U . . .
C6_5 C 0.6517(3) 0.8379(3) 0.45598(18) 0.0215(10) Uani 1 1 d D . . . .
H6_5 H 0.594717 0.816150 0.445696 0.026 Uiso 1 1 calc R U . . .
C7_5 C 0.6318(3) 0.76051(18) 0.56436(16) 0.0251(11) Uani 1 1 d D . . . .
H7A_5 H 0.550716 0.775465 0.557225 0.030 Uiso 1 1 calc R U . . .
H7B_5 H 0.652164 0.762787 0.602858 0.030 Uiso 1 1 calc R U . . .
C8_5 C 0.6652(3) 0.67844(19) 0.5683(2) 0.0229(10) Uani 1 1 d D . . . .
H8A_5 H 0.627486 0.643820 0.600666 0.028 Uiso 1 1 calc R U . . .
H8B_5 H 0.641645 0.675266 0.530590 0.028 Uiso 1 1 calc R U . . .
C9_5 C 0.9055(4) 0.9416(3) 0.5017(2) 0.0301(12) Uani 1 1 d D . . . .
H9A_5 H 0.870860 0.991563 0.501873 0.045 Uiso 1 1 calc R U . . .
H9B_5 H 0.961911 0.949178 0.472680 0.045 Uiso 1 1 calc R U . . .
H9C_5 H 0.939752 0.908633 0.541331 0.045 Uiso 1 1 calc R U . . .
N6_6 N 0.6957(3) 0.3484(2) 0.67338(18) 0.0207(9) Uani 1 1 d D . . . .
H6A_6 H 0.670214 0.340141 0.641707 0.025 Uiso 1 1 calc R U . . .
H6B_6 H 0.680602 0.399604 0.666001 0.025 Uiso 1 1 calc R U . . .
H6C_6 H 0.662243 0.322124 0.706306 0.025 Uiso 1 1 calc R U . . .
C1_6 C 0.7924(3) 0.1831(2) 0.73581(15) 0.0194(9) Uani 1 1 d D . . . .
C2_6 C 0.7093(3) 0.1502(2) 0.72176(14) 0.0215(10) Uani 1 1 d D . . . .
H2_6 H 0.686883 0.163855 0.681221 0.026 Uiso 1 1 calc R U . . .
C3_6 C 0.6577(3) 0.0973(2) 0.76598(15) 0.0244(10) Uani 1 1 d D . . . .
C4_6 C 0.6908(4) 0.0791(2) 0.82485(15) 0.0271(11) Uani 1 1 d D . . . .
H4_6 H 0.655694 0.044470 0.855581 0.032 Uiso 1 1 calc R U . . .
C5_6 C 0.7742(4) 0.1109(2) 0.83941(14) 0.0260(11) Uani 1 1 d D . . . .
H5_6 H 0.796545 0.097070 0.879972 0.031 Uiso 1 1 calc R U . . .
C6_6 C 0.8255(3) 0.1627(3) 0.79547(18) 0.0222(10) Uani 1 1 d D . . . .
H6_6 H 0.882866 0.184110 0.805861 0.027 Uiso 1 1 calc R U . . .
C7_6 C 0.8474(3) 0.23900(18) 0.68699(16) 0.0242(11) Uani 1 1 d D . . . .
H7A_6 H 0.825752 0.237297 0.648465 0.029 Uiso 1 1 calc R U . . .
H7B_6 H 0.928294 0.222687 0.693989 0.029 Uiso 1 1 calc R U . . .
C8_6 C 0.8172(3) 0.32117(19) 0.6834(2) 0.0226(10) Uani 1 1 d D . . . .
H8A_6 H 0.843339 0.323905 0.720810 0.027 Uiso 1 1 calc R U . . .
H8B_6 H 0.854405 0.355336 0.650464 0.027 Uiso 1 1 calc R U . . .
C9_6 C 0.5719(4) 0.0593(3) 0.7493(2) 0.0355(14) Uani 1 1 d D . . . .
H9A_6 H 0.534830 0.093480 0.710662 0.053 Uiso 1 1 calc R U . . .
H9B_6 H 0.517637 0.048849 0.779493 0.053 Uiso 1 1 calc R U . . .
H9C_6 H 0.607597 0.010764 0.746963 0.053 Uiso 1 1 calc R U . . .
N6_7 N 0.7866(3) 0.3477(2) 0.96033(18) 0.0202(9) Uani 1 1 d D . . . .
H6A_7 H 0.785018 0.399416 0.943859 0.024 Uiso 1 1 calc R U . . .
H6B_7 H 0.848672 0.324590 0.984843 0.024 Uiso 1 1 calc R U . . .
H6C_7 H 0.726286 0.337756 0.981557 0.024 Uiso 1 1 calc R U . . .
C1_7 C 0.8425(3) 0.1794(2) 0.98415(15) 0.0190(9) Uani 1 1 d D . . . .
C2_7 C 0.9433(3) 0.1488(2) 0.96946(14) 0.0221(10) Uani 1 1 d D . . . .
H2_7 H 0.958824 0.163854 0.928832 0.026 Uiso 1 1 calc R U . . .
C3_7 C 1.0225(3) 0.0964(2) 1.01322(15) 0.0230(10) Uani 1 1 d D . . . .
C4_7 C 0.9989(3) 0.0773(2) 1.07224(15) 0.0255(10) Uani 1 1 d D . . . .
H4_7 H 1.051856 0.042573 1.102656 0.031 Uiso 1 1 calc R U . . .
C5_7 C 0.8995(3) 0.1079(2) 1.08752(14) 0.0261(11) Uani 1 1 d D . . . .
H5_7 H 0.885088 0.094059 1.128220 0.031 Uiso 1 1 calc R U . . .
C6_7 C 0.8208(3) 0.1587(3) 1.04396(18) 0.0239(11) Uani 1 1 d D . . . .
H6_7 H 0.752551 0.179310 1.054754 0.029 Uiso 1 1 calc R U . . .
C7_7 C 0.7596(3) 0.23627(17) 0.93578(16) 0.0219(10) Uani 1 1 d D . . . .
H7A_7 H 0.685633 0.237522 0.951534 0.026 Uiso 1 1 calc R U . . .
H7B_7 H 0.757329 0.218649 0.902527 0.026 Uiso 1 1 calc R U . . .
C8_7 C 0.7864(4) 0.31711(19) 0.91239(16) 0.0223(10) Uani 1 1 d D . . . .
H8A_7 H 0.859689 0.316386 0.895761 0.027 Uiso 1 1 calc R U . . .
H8B_7 H 0.731238 0.351501 0.880008 0.027 Uiso 1 1 calc R U . . .
C9_7 C 1.1283(3) 0.0603(3) 0.9960(2) 0.0309(13) Uani 1 1 d D . . . .
H9A_7 H 1.188762 0.053998 1.024489 0.046 Uiso 1 1 calc R U . . .
H9B_7 H 1.144390 0.093677 0.956114 0.046 Uiso 1 1 calc R U . . .
H9C_7 H 1.120520 0.009924 0.996131 0.046 Uiso 1 1 calc R U . . .
Pb1_8 Pb 0.500000 0.500000 0.500000 0.01121(6) Uani 1 2 d S . P . .
Pb2A_8 Pb 0.51485(2) 0.48854(2) 0.25307(2) 0.01158(6) Uani 0.9682(5) 1 d . . P
A 1
Pb3B_8 Pb 0.9873(7) 0.5135(5) 0.7468(4) 0.01165(6) Uani 0.0318(5) 1 d . . P A 2
Pb4_8 Pb 1.000000 0.500000 0.500000 0.01129(6) Uani 1 2 d S . P . .
Pb5_8 Pb 0.500000 0.500000 0.000000 0.01131(6) Uani 1 2 d S . P . .
Pb6_8 Pb 1.000000 0.500000 0.000000 0.01113(6) Uani 1 2 d S . P . .
I1_8 I 0.56901(3) 0.50080(2) 0.37524(2) 0.01434(8) Uani 0.9682(5) 1 d . . P A 1
I2_8 I 0.76122(3) 0.50095(2) 0.22003(2) 0.01411(8) Uani 0.9682(5) 1 d . . P A 1
I3_8 I 0.94341(3) 0.49916(2) 0.37471(2) 0.01458(8) Uani 0.9682(5) 1 d . . P A 1
I4_8 I 0.75016(2) 0.49851(2) 0.53150(2) 0.01436(8) Uani 0.9682(5) 1 d . . P A 1
I5_8 I 0.44288(3) 0.50088(2) 0.12532(2) 0.01459(8) Uani 0.9682(5) 1 d . . P A 1
I6_8 I 0.75068(2) 0.49850(2) 0.03140(2) 0.01427(8) Uani 0.9682(5) 1 d . . P A 1
I7_8 I 1.06937(3) 0.49938(2) 0.12474(2) 0.01447(8) Uani 0.9682(5) 1 d . . P A 1
I8_8 I 1.26177(3) 0.49895(2) 0.28021(2) 0.01600(8) Uani 1 1 d . . . A 1
I9_8 I 0.43811(6) 0.68518(4) 0.44465(3) 0.01475(11) Uani 0.9682(5) 1 d . . P A
1
I10_8 I 0.47301(3) 0.68396(2) 0.19805(2) 0.01491(7) Uani 1 1 d . . . A 1
I11_8 I 0.54832(3) 0.31211(2) 0.30258(2) 0.01628(7) Uani 1 1 d . . . A 1
I12_8 I 1.06525(3) 0.31591(2) 0.30183(2) 0.01484(7) Uani 1 1 d . . . A 1
I13_8 I 0.95455(3) 0.68793(2) 0.19772(2) 0.01640(7) Uani 1 1 d . . . A 1
I14_8 I 0.95260(3) 0.68481(2) 0.45220(2) 0.01596(7) Uani 1 1 d . . . B 1
I15_8 I 0.45504(3) 0.68481(2) -0.04766(2) 0.01600(7) Uani 1 1 d . . . C 1
I16_8 I 0.96888(3) 0.68517(2) -0.05536(2) 0.01554(7) Uani 1 1 d . . . D 1

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
Pb2B 0.00855(10) 0.01582(10) 0.01078(10) -0.00523(9) 0.00076(7) -0.00296(8)
Pb3A 0.00812(9) 0.01582(10) 0.01091(10) -0.00509(9) 0.00043(7) -0.00189(9)
I1 0.00786(15) 0.01780(15) 0.01762(16) -0.00755(13) 0.00114(12) -0.00298(11)
I1B 0.01517(16) 0.01810(15) 0.00945(15) -0.00551(12) 0.00017(12) -0.00148(12)
I2B 0.00743(15) 0.01806(15) 0.01799(16) -0.00764(13) 0.00089(12) -0.00226(11)
I3B 0.01562(17) 0.01826(15) 0.00935(15) -0.00521(12) -0.00004(12) -0.00174(12)
I4B 0.00830(15) 0.01829(15) 0.01780(16) -0.00771(13) 0.00138(12) -0.00401(11)
I5B 0.01517(16) 0.01810(15) 0.00945(15) -0.00551(12) 0.00017(12) -0.00148(12)
I6B 0.01562(17) 0.01826(15) 0.00935(15) -0.00521(12) -0.00004(12) -0.00174(12)
I8B 0.00786(15) 0.01780(15) 0.01762(16) -0.00755(13) 0.00114(12) -0.00298(11)
I14B 0.0143(3) 0.01425(15) 0.0152(3) -0.00438(18) 0.00039(18) -0.00415(15)
N6 0.016(2) 0.018(2) 0.023(2) -0.0071(18) -0.0002(17) -0.0033(16)
C1 0.021(3) 0.011(2) 0.021(2) -0.0051(19) -0.005(2) -0.0010(18)
C2 0.028(3) 0.014(2) 0.029(3) -0.009(2) 0.000(2) -0.0042(19)
C3 0.018(3) 0.014(2) 0.044(3) -0.014(2) -0.004(2) -0.0028(18)
C4 0.030(3) 0.017(2) 0.033(3) -0.006(2) -0.007(2) 0.000(2)
C5 0.042(4) 0.021(3) 0.026(3) -0.008(2) -0.001(2) -0.004(2)
C6 0.032(3) 0.016(2) 0.023(3) -0.006(2) 0.000(2) -0.005(2)
C7 0.022(3) 0.022(2) 0.025(3) -0.013(2) -0.010(2) 0.0021(19)
C8 0.025(3) 0.019(2) 0.020(3) -0.005(2) -0.002(2) 0.003(2)
C9 0.025(3) 0.026(3) 0.052(4) -0.019(3) 0.001(3) -0.001(2)
N6_1 0.021(2) 0.0162(19) 0.021(2) -0.0057(17) -0.0019(17) -0.0027(16)
C1_1 0.020(2) 0.015(2) 0.025(2) -0.0088(18) 0.0080(18) -0.0014(17)
C2_1 0.026(2) 0.015(2) 0.023(2) -0.0083(18) 0.0009(18) 0.0004(17)
C3_1 0.023(3) 0.014(2) 0.041(3) -0.013(2) 0.0092(19) -0.0026(17)
C4_1 0.039(3) 0.016(2) 0.038(3) -0.006(2) 0.011(2) -0.007(2)
C5_1 0.037(3) 0.017(2) 0.024(3) -0.005(2) 0.005(2) -0.0007(19)
C6_1 0.029(3) 0.016(2) 0.026(2) -0.0058(19) 0.0027(19) -0.0029(19)
C7_1 0.031(3) 0.019(2) 0.024(3) -0.0072(19) 0.012(2) -0.0078(18)
C8_1 0.026(3) 0.021(2) 0.021(2) -0.0079(19) 0.004(2) -0.0070(19)
C9_1 0.028(3) 0.024(3) 0.065(4) -0.023(3) 0.007(3) -0.008(2)
N6_2 0.020(2) 0.016(2) 0.023(2) -0.0058(17) -0.0023(17) -0.0027(16)
C1_2 0.019(2) 0.015(2) 0.020(2) -0.0043(17) 0.0044(17) -0.0030(17)
C2_2 0.021(2) 0.015(2) 0.022(2) -0.0071(18) -0.0010(18) -0.0002(16)
C3_2 0.021(2) 0.017(2) 0.035(2) -0.008(2) 0.0025(19) -0.0047(18)
C4_2 0.023(3) 0.017(2) 0.032(2) -0.004(2) 0.0116(19) -0.0024(18)
C5_2 0.032(3) 0.016(2) 0.022(2) -0.0030(19) 0.004(2) 0.0000(18)
C6_2 0.028(3) 0.019(2) 0.024(2) -0.0098(19) 0.0001(19) -0.007(2)
C7_2 0.027(3) 0.019(2) 0.024(3) -0.0067(19) 0.006(2) -0.0056(18)
C8_2 0.028(3) 0.018(2) 0.020(2) -0.0039(18) 0.003(2) -0.0071(19)
C9_2 0.029(3) 0.024(3) 0.053(4) -0.017(3) 0.004(3) -0.008(2)
N6_3 0.020(2) 0.019(2) 0.018(2) -0.0042(17) -0.0006(16) -0.0029(16)
C1_3 0.022(2) 0.013(2) 0.018(2) -0.0038(17) -0.0016(16) -0.0066(16)
C2_3 0.023(2) 0.018(2) 0.023(2) -0.0073(19) 0.0016(17) -0.0072(17)
C3_3 0.018(2) 0.013(2) 0.033(2) -0.0081(18) -0.0016(17) -0.0060(16)
C4_3 0.028(3) 0.016(2) 0.025(2) -0.0020(19) -0.0078(19) -0.0014(18)
C5_3 0.034(3) 0.020(2) 0.022(2) -0.006(2) -0.0056(19) -0.0037(19)
C6_3 0.027(3) 0.018(2) 0.021(2) -0.0049(19) 0.0019(18) -0.0041(19)
C7_3 0.022(3) 0.019(2) 0.026(3) -0.0067(19) -0.009(2) -0.0047(18)
C8_3 0.019(2) 0.020(2) 0.026(3) -0.007(2) -0.005(2) -0.0050(18)
C9_3 0.022(3) 0.024(3) 0.045(4) -0.015(3) 0.004(2) -0.004(2)
N6_4 0.023(2) 0.019(2) 0.021(2) -0.0073(17) 0.0006(17) -0.0038(16)
C1_4 0.021(2) 0.014(2) 0.019(2) -0.0021(17) -0.0040(17) -0.0057(16)
C2_4 0.028(2) 0.017(2) 0.022(2) -0.0054(19) 0.0004(18) -0.0066(17)
C3_4 0.019(2) 0.016(2) 0.035(2) -0.0122(19) 0.0006(18) -0.0051(17)
C4_4 0.031(3) 0.017(2) 0.029(2) -0.006(2) -0.008(2) 0.0011(19)
C5_4 0.039(3) 0.020(2) 0.020(2) -0.006(2) -0.0055(19) 0.0011(19)
C6_4 0.027(3) 0.016(2) 0.022(2) -0.0030(19) -0.0012(19) -0.0022(19)
C7_4 0.025(3) 0.021(2) 0.023(2) -0.0044(19) -0.007(2) -0.0046(18)
C8_4 0.021(2) 0.018(2) 0.022(3) -0.0023(19) -0.001(2) -0.0013(18)
C9_4 0.027(3) 0.027(3) 0.045(4) -0.017(3) 0.006(2) -0.001(2)
N6_5 0.024(2) 0.020(2) 0.018(2) -0.0073(17) 0.0028(17) -0.0031(16)
C1_5 0.022(2) 0.014(2) 0.018(2) -0.0021(17) 0.0060(17) 0.0013(16)
C2_5 0.023(2) 0.017(2) 0.020(2) -0.0069(18) 0.0018(18) 0.0013(17)
C3_5 0.023(2) 0.017(2) 0.030(2) -0.0102(19) 0.0060(18) -0.0018(17)
C4_5 0.031(3) 0.017(2) 0.028(2) -0.003(2) 0.004(2) -0.0039(19)
C5_5 0.031(3) 0.019(2) 0.020(2) -0.0025(19) 0.002(2) -0.0015(19)
C6_5 0.024(3) 0.020(2) 0.022(2) -0.0097(19) 0.0032(19) -0.0054(19)
C7_5 0.024(3) 0.019(2) 0.026(3) -0.0021(19) 0.007(2) -0.0023(18)
C8_5 0.023(2) 0.019(2) 0.024(3) -0.006(2) 0.005(2) -0.0022(18)
C9_5 0.024(3) 0.023(3) 0.044(3) -0.014(3) 0.001(2) -0.002(2)
N6_6 0.020(2) 0.021(2) 0.024(2) -0.0099(18) 0.0007(17) -0.0049(15)
C1_6 0.021(2) 0.012(2) 0.019(2) -0.0013(17) 0.0038(17) 0.0013(16)
C2_6 0.023(2) 0.016(2) 0.023(2) -0.0062(18) 0.0011(18) 0.0025(17)
C3_6 0.022(3) 0.017(2) 0.033(2) -0.0091(19) 0.0052(19) -0.0015(18)
C4_6 0.033(3) 0.016(2) 0.028(2) -0.004(2) 0.011(2) -0.0051(19)
C5_6 0.037(3) 0.017(2) 0.021(2) -0.0037(19) 0.003(2) -0.0024(19)
C6_6 0.028(3) 0.018(2) 0.019(2) -0.0067(18) 0.0008(18) -0.0032(19)
C7_6 0.024(3) 0.019(2) 0.023(2) -0.0028(19) 0.009(2) -0.0008(18)
C8_6 0.019(2) 0.016(2) 0.027(3) -0.003(2) 0.002(2) -0.0011(17)
C9_6 0.028(3) 0.024(3) 0.058(4) -0.019(3) 0.002(3) -0.005(2)
N6_7 0.017(2) 0.017(2) 0.028(2) -0.0105(18) -0.0017(18) -0.0011(16)
C1_7 0.022(2) 0.014(2) 0.020(2) -0.0052(17) -0.0041(17) -0.0037(16)
C2_7 0.023(2) 0.013(2) 0.027(2) -0.0043(19) -0.0014(18) -0.0039(16)
C3_7 0.018(2) 0.016(2) 0.032(2) -0.0062(19) -0.0026(18) -0.0037(17)
C4_7 0.027(3) 0.018(2) 0.028(2) -0.006(2) -0.0078(19) -0.0027(18)
C5_7 0.037(3) 0.020(2) 0.021(2) -0.007(2) 0.0003(19) -0.0062(19)
C6_7 0.030(3) 0.017(2) 0.023(2) -0.0047(19) 0.0048(19) -0.0051(19)
C7_7 0.018(2) 0.021(2) 0.027(3) -0.0111(19) -0.0080(19) 0.0000(17)
C8_7 0.024(3) 0.021(2) 0.018(2) -0.0070(19) 0.001(2) 0.0034(19)
C9_7 0.022(3) 0.024(3) 0.046(4) -0.014(3) 0.001(2) -0.001(2)
Pb1_8 0.00818(12) 0.01460(12) 0.01017(12) -0.00409(10) 0.00079(9) -0.00180(9)
Pb2A_8 0.00855(10) 0.01582(10) 0.01078(10) -0.00523(9) 0.00076(7) -0.00296(8)
Pb3B_8 0.00812(9) 0.01582(10) 0.01091(10) -0.00509(9) 0.00043(7) -0.00189(9)
Pb4_8 0.00910(12) 0.01455(12) 0.01079(12) -0.00497(10) 0.00104(9) -0.00338(9)
Pb5_8 0.00835(12) 0.01470(12) 0.01080(12) -0.00499(10) 0.00041(9) -0.00155(9)
Pb6_8 0.00853(12) 0.01454(12) 0.01022(12) -0.00422(10) 0.00055(9) -0.00301(9)
I1_8 0.01517(16) 0.01810(15) 0.00945(15) -0.00551(12) 0.00017(12) -0.00148(12)
I2_8 0.00786(15) 0.01780(15) 0.01762(16) -0.00755(13) 0.00114(12) -0.00298(11)
I3_8 0.01562(17) 0.01826(15) 0.00935(15) -0.00521(12) -0.00004(12) -0.00174(12)
I4_8 0.00830(15) 0.01829(15) 0.01780(16) -0.00771(13) 0.00138(12) -0.00401(11)
I5_8 0.01660(17) 0.01833(15) 0.00919(15) -0.00519(12) 0.00092(12) -0.00424(12)
I6_8 0.00743(15) 0.01806(15) 0.01799(16) -0.00764(13) 0.00089(12) -0.00226(11)
I7_8 0.01604(16) 0.01845(15) 0.00971(15) -0.00576(12) 0.00108(12) -0.00434(12)
I8_8 0.00975(15) 0.01944(15) 0.01985(16) -0.00836(13) 0.00111(12) -0.00342(11)
I9_8 0.0143(3) 0.01425(15) 0.0152(3) -0.00438(18) 0.00039(18) -0.00415(15)
I10_8 0.01461(16) 0.01466(14) 0.01401(15) -0.00410(12) 0.00008(12) -0.00209(11)
I11_8 0.01435(16) 0.01446(15) 0.01737(16) -0.00348(12) -0.00003(12)
-0.00166(11)
I12_8 0.01463(16) 0.01495(14) 0.01369(15) -0.00407(12) 0.00102(12) -0.00267(11)
I13_8 0.01525(16) 0.01445(15) 0.01735(16) -0.00354(12) 0.00074(12) -0.00299(12)
I14_8 0.01548(16) 0.01441(15) 0.01595(15) -0.00327(12) 0.00011(12) -0.00330(11)
I15_8 0.01511(16) 0.01452(15) 0.01591(15) -0.00348(12) 0.00088(12) -0.00166(11)
I16_8 0.01387(16) 0.01411(14) 0.01660(15) -0.00440(12) -0.00037(12)
-0.00052(11)

_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
Pb2B I1B 3.118(13) . ?
Pb2B I2B 3.100(13) . ?
Pb2B I5B 3.182(13) . ?
Pb2B I8B 3.265(13) 1_455 ?
Pb3A I2_8 3.1800(4) . ?
Pb3A I3_8 3.1486(4) . ?
Pb3A I7_8 3.1535(4) . ?
Pb3A I8_8 3.1669(4) . ?
Pb3A I12_8 3.4010(4) . ?
Pb3A I13_8 3.0694(4) . ?
I1 Pb5_8 3.158(9) . ?
I1 Pb6_8 3.186(9) . ?
I1B Pb1_8 3.130(9) . ?
I2B Pb3B_8 3.228(13) . ?
I3B Pb3B_8 3.196(13) . ?
I3B Pb4_8 3.150(10) . ?
I4B Pb1_8 3.189(9) . ?
I4B Pb4_8 3.162(9) . ?
I5B Pb5_8 3.173(9) 1_556 ?
I6B Pb3B_8 3.121(13) . ?
I6B Pb6_8 3.140(9) 1_556 ?
I8B Pb3B_8 3.118(13) . ?
I14B Pb1_8 3.25(3) . ?
N6 H6A 0.9100 . ?
N6 H6B 0.9100 . ?
N6 H6C 0.9100 . ?
N6 C8 1.485(6) . ?
C1 C2 1.386(7) . ?
C1 C6 1.391(7) . ?
C1 C7 1.511(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.399(7) . ?
C3 C4 1.387(7) . ?
C3 C9 1.502(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.374(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.390(7) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.523(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
N6_1 H6A_1 0.9100 . ?
N6_1 H6B_1 0.9100 . ?
N6_1 H6C_1 0.9100 . ?
N6_1 C8_1 1.490(3) . ?
C1_1 C2_1 1.391(3) . ?
C1_1 C6_1 1.397(4) . ?
C1_1 C7_1 1.511(3) . ?
C2_1 H2_1 0.9500 . ?
C2_1 C3_1 1.402(3) . ?
C3_1 C4_1 1.388(3) . ?
C3_1 C9_1 1.510(3) . ?
C4_1 H4_1 0.9500 . ?
C4_1 C5_1 1.384(3) . ?
C5_1 H5_1 0.9500 . ?
C5_1 C6_1 1.387(4) . ?
C6_1 H6_1 0.9500 . ?
C7_1 H7A_1 0.9900 . ?
C7_1 H7B_1 0.9900 . ?
C7_1 C8_1 1.519(3) . ?
C8_1 H8A_1 0.9900 . ?
C8_1 H8B_1 0.9900 . ?
C9_1 H9A_1 0.9800 . ?
C9_1 H9B_1 0.9800 . ?
C9_1 H9C_1 0.9800 . ?
N6_2 H6A_2 0.9100 . ?
N6_2 H6B_2 0.9100 . ?
N6_2 H6C_2 0.9100 . ?
N6_2 C8_2 1.491(3) . ?
C1_2 C2_2 1.391(3) . ?
C1_2 C6_2 1.397(4) . ?
C1_2 C7_2 1.512(3) . ?
C2_2 H2_2 0.9500 . ?
C2_2 C3_2 1.402(3) . ?
C3_2 C4_2 1.387(3) . ?
C3_2 C9_2 1.510(3) . ?
C4_2 H4_2 0.9500 . ?
C4_2 C5_2 1.384(3) . ?
C5_2 H5_2 0.9500 . ?
C5_2 C6_2 1.387(4) . ?
C6_2 H6_2 0.9500 . ?
C7_2 H7A_2 0.9900 . ?
C7_2 H7B_2 0.9900 . ?
C7_2 C8_2 1.520(3) . ?
C8_2 H8A_2 0.9900 . ?
C8_2 H8B_2 0.9900 . ?
C9_2 H9A_2 0.9800 . ?
C9_2 H9B_2 0.9800 . ?
C9_2 H9C_2 0.9800 . ?
N6_3 H6A_3 0.9100 . ?
N6_3 H6B_3 0.9100 . ?
N6_3 H6C_3 0.9100 . ?
N6_3 C8_3 1.491(3) . ?
C1_3 C2_3 1.390(3) . ?
C1_3 C6_3 1.397(4) . ?
C1_3 C7_3 1.511(3) . ?
C2_3 H2_3 0.9500 . ?
C2_3 C3_3 1.403(3) . ?
C3_3 C4_3 1.387(3) . ?
C3_3 C9_3 1.510(3) . ?
C4_3 H4_3 0.9500 . ?
C4_3 C5_3 1.384(3) . ?
C5_3 H5_3 0.9500 . ?
C5_3 C6_3 1.387(4) . ?
C6_3 H6_3 0.9500 . ?
C7_3 H7A_3 0.9900 . ?
C7_3 H7B_3 0.9900 . ?
C7_3 C8_3 1.518(3) . ?
C8_3 H8A_3 0.9900 . ?
C8_3 H8B_3 0.9900 . ?
C9_3 H9A_3 0.9800 . ?
C9_3 H9B_3 0.9800 . ?
C9_3 H9C_3 0.9800 . ?
N6_4 H6A_4 0.9100 . ?
N6_4 H6B_4 0.9100 . ?
N6_4 H6C_4 0.9100 . ?
N6_4 C8_4 1.491(3) . ?
C1_4 C2_4 1.390(3) . ?
C1_4 C6_4 1.397(4) . ?
C1_4 C7_4 1.511(3) . ?
C2_4 H2_4 0.9500 . ?
C2_4 C3_4 1.403(3) . ?
C3_4 C4_4 1.387(3) . ?
C3_4 C9_4 1.510(3) . ?
C4_4 H4_4 0.9500 . ?
C4_4 C5_4 1.384(3) . ?
C5_4 H5_4 0.9500 . ?
C5_4 C6_4 1.388(4) . ?
C6_4 H6_4 0.9500 . ?
C7_4 H7A_4 0.9900 . ?
C7_4 H7B_4 0.9900 . ?
C7_4 C8_4 1.519(3) . ?
C8_4 H8A_4 0.9900 . ?
C8_4 H8B_4 0.9900 . ?
C9_4 H9A_4 0.9800 . ?
C9_4 H9B_4 0.9800 . ?
C9_4 H9C_4 0.9800 . ?
N6_5 H6A_5 0.9100 . ?
N6_5 H6B_5 0.9100 . ?
N6_5 H6C_5 0.9100 . ?
N6_5 C8_5 1.491(3) . ?
C1_5 C2_5 1.390(3) . ?
C1_5 C6_5 1.397(4) . ?
C1_5 C7_5 1.511(3) . ?
C2_5 H2_5 0.9500 . ?
C2_5 C3_5 1.403(3) . ?
C3_5 C4_5 1.387(3) . ?
C3_5 C9_5 1.510(3) . ?
C4_5 H4_5 0.9500 . ?
C4_5 C5_5 1.383(3) . ?
C5_5 H5_5 0.9500 . ?
C5_5 C6_5 1.387(4) . ?
C6_5 H6_5 0.9500 . ?
C7_5 H7A_5 0.9900 . ?
C7_5 H7B_5 0.9900 . ?
C7_5 C8_5 1.519(3) . ?
C8_5 H8A_5 0.9900 . ?
C8_5 H8B_5 0.9900 . ?
C9_5 H9A_5 0.9800 . ?
C9_5 H9B_5 0.9800 . ?
C9_5 H9C_5 0.9800 . ?
N6_6 H6A_6 0.9100 . ?
N6_6 H6B_6 0.9100 . ?
N6_6 H6C_6 0.9100 . ?
N6_6 C8_6 1.491(3) . ?
C1_6 C2_6 1.390(3) . ?
C1_6 C6_6 1.397(4) . ?
C1_6 C7_6 1.511(3) . ?
C2_6 H2_6 0.9500 . ?
C2_6 C3_6 1.403(3) . ?
C3_6 C4_6 1.387(3) . ?
C3_6 C9_6 1.510(3) . ?
C4_6 H4_6 0.9500 . ?
C4_6 C5_6 1.384(3) . ?
C5_6 H5_6 0.9500 . ?
C5_6 C6_6 1.387(4) . ?
C6_6 H6_6 0.9500 . ?
C7_6 H7A_6 0.9900 . ?
C7_6 H7B_6 0.9900 . ?
C7_6 C8_6 1.520(3) . ?
C8_6 H8A_6 0.9900 . ?
C8_6 H8B_6 0.9900 . ?
C9_6 H9A_6 0.9800 . ?
C9_6 H9B_6 0.9800 . ?
C9_6 H9C_6 0.9800 . ?
N6_7 H6A_7 0.9100 . ?
N6_7 H6B_7 0.9100 . ?
N6_7 H6C_7 0.9100 . ?
N6_7 C8_7 1.491(3) . ?
C1_7 C2_7 1.391(3) . ?
C1_7 C6_7 1.397(4) . ?
C1_7 C7_7 1.511(3) . ?
C2_7 H2_7 0.9500 . ?
C2_7 C3_7 1.403(3) . ?
C3_7 C4_7 1.387(3) . ?
C3_7 C9_7 1.510(3) . ?
C4_7 H4_7 0.9500 . ?
C4_7 C5_7 1.383(3) . ?
C5_7 H5_7 0.9500 . ?
C5_7 C6_7 1.388(4) . ?
C6_7 H6_7 0.9500 . ?
C7_7 H7A_7 0.9900 . ?
C7_7 H7B_7 0.9900 . ?
C7_7 C8_7 1.520(3) . ?
C8_7 H8A_7 0.9900 . ?
C8_7 H8B_7 0.9900 . ?
C9_7 H9A_7 0.9800 . ?
C9_7 H9B_7 0.9800 . ?
C9_7 H9C_7 0.9800 . ?
Pb1_8 I1_8 3.1529(3) 2_666 ?
Pb1_8 I1_8 3.1529(3) . ?
Pb1_8 I4_8 3.1715(3) . ?
Pb1_8 I4_8 3.1715(3) 2_666 ?
Pb1_8 I9_8 3.2237(8) . ?
Pb1_8 I9_8 3.2237(8) 2_666 ?
Pb2A_8 I1_8 3.1538(4) . ?
Pb2A_8 I2_8 3.1651(4) . ?
Pb2A_8 I5_8 3.1492(4) . ?
Pb2A_8 I8_8 3.1797(4) 1_455 ?
Pb2A_8 I10_8 3.3978(4) . ?
Pb2A_8 I11_8 3.0694(4) . ?
Pb4_8 I3_8 3.1394(3) . ?
Pb4_8 I3_8 3.1394(3) 2_766 ?
Pb4_8 I4_8 3.1762(3) . ?
Pb4_8 I4_8 3.1762(3) 2_766 ?
Pb4_8 I14_8 3.2159(3) 2_766 ?
Pb4_8 I14_8 3.2159(3) . ?
Pb5_8 I5_8 3.1403(3) . ?
Pb5_8 I5_8 3.1404(3) 2_665 ?
Pb5_8 I6_8 3.1771(3) 2_665 ?
Pb5_8 I6_8 3.1771(3) . ?
Pb5_8 I15_8 3.2161(3) . ?
Pb5_8 I15_8 3.2161(3) 2_665 ?
Pb6_8 I6_8 3.1695(3) 2_765 ?
Pb6_8 I6_8 3.1695(3) . ?
Pb6_8 I7_8 3.1540(3) 2_765 ?
Pb6_8 I7_8 3.1540(3) . ?
Pb6_8 I16_8 3.2233(3) . ?
Pb6_8 I16_8 3.2234(3) 2_765 ?

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
I1B Pb2B I5B 170.9(4) . . ?
I2B Pb2B I1B 89.9(3) . . ?
I2B Pb2B I5B 89.7(3) . . ?
I2_8 Pb3A I12_8 87.857(9) . . ?
I3_8 Pb3A I2_8 87.471(10) . . ?
I3_8 Pb3A I7_8 171.801(11) . . ?
I3_8 Pb3A I8_8 92.199(10) . . ?
I3_8 Pb3A I12_8 87.703(10) . . ?
I7_8 Pb3A I2_8 89.381(10) . . ?
I7_8 Pb3A I8_8 89.966(10) . . ?
I7_8 Pb3A I12_8 84.614(9) . . ?
I8_8 Pb3A I2_8 172.738(11) . . ?
I8_8 Pb3A I12_8 84.881(9) . . ?
I13_8 Pb3A I2_8 91.287(10) . . ?
I13_8 Pb3A I3_8 91.936(11) . . ?
I13_8 Pb3A I7_8 95.704(11) . . ?
I13_8 Pb3A I8_8 95.975(10) . . ?
I13_8 Pb3A I12_8 179.084(11) . . ?
Pb5_8 I1 Pb6_8 152.7(3) . . ?
Pb2B I1B Pb1_8 152.6(4) . . ?
Pb2B I2B Pb3B_8 152.5(4) . . ?
Pb4_8 I3B Pb3B_8 149.2(4) . . ?
Pb4_8 I4B Pb1_8 152.1(3) . . ?
Pb5_8 I5B Pb2B 149.1(4) 1_556 . ?
H6A N6 H6B 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
C8 N6 H6A 109.5 . . ?
C8 N6 H6B 109.5 . . ?
C8 N6 H6C 109.5 . . ?
C2 C1 C6 118.6(5) . . ?
C2 C1 C7 120.6(5) . . ?
C6 C1 C7 120.7(5) . . ?
C1 C2 H2 118.9 . . ?
C1 C2 C3 122.2(5) . . ?
C3 C2 H2 118.9 . . ?
C2 C3 C9 121.1(5) . . ?
C4 C3 C2 117.4(5) . . ?
C4 C3 C9 121.5(5) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 C3 121.6(5) . . ?
C5 C4 H4 119.2 . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.1(5) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 H6 120.0 . . ?
C5 C6 C1 120.1(5) . . ?
C5 C6 H6 120.0 . . ?
C1 C7 H7A 109.0 . . ?
C1 C7 H7B 109.0 . . ?
C1 C7 C8 112.8(4) . . ?
H7A C7 H7B 107.8 . . ?
C8 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
N6 C8 C7 110.9(4) . . ?
N6 C8 H8A 109.5 . . ?
N6 C8 H8B 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C3 C9 H9A 109.5 . . ?
C3 C9 H9B 109.5 . . ?
C3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
H6A_1 N6_1 H6B_1 109.5 . . ?
H6A_1 N6_1 H6C_1 109.5 . . ?
H6B_1 N6_1 H6C_1 109.5 . . ?
C8_1 N6_1 H6A_1 109.5 . . ?
C8_1 N6_1 H6B_1 109.5 . . ?
C8_1 N6_1 H6C_1 109.5 . . ?
C2_1 C1_1 C6_1 119.2(3) . . ?
C2_1 C1_1 C7_1 119.9(3) . . ?
C6_1 C1_1 C7_1 120.9(3) . . ?
C1_1 C2_1 H2_1 119.2 . . ?
C1_1 C2_1 C3_1 121.5(3) . . ?
C3_1 C2_1 H2_1 119.2 . . ?
C2_1 C3_1 C9_1 120.4(3) . . ?
C4_1 C3_1 C2_1 118.0(2) . . ?
C4_1 C3_1 C9_1 121.4(3) . . ?
C3_1 C4_1 H4_1 119.5 . . ?
C5_1 C4_1 C3_1 121.0(3) . . ?
C5_1 C4_1 H4_1 119.5 . . ?
C4_1 C5_1 H5_1 119.7 . . ?
C4_1 C5_1 C6_1 120.6(3) . . ?
C6_1 C5_1 H5_1 119.7 . . ?
C1_1 C6_1 H6_1 120.2 . . ?
C5_1 C6_1 C1_1 119.6(3) . . ?
C5_1 C6_1 H6_1 120.2 . . ?
C1_1 C7_1 H7A_1 109.0 . . ?
C1_1 C7_1 H7B_1 109.0 . . ?
C1_1 C7_1 C8_1 112.7(3) . . ?
H7A_1 C7_1 H7B_1 107.8 . . ?
C8_1 C7_1 H7A_1 109.0 . . ?
C8_1 C7_1 H7B_1 109.0 . . ?
N6_1 C8_1 C7_1 111.2(3) . . ?
N6_1 C8_1 H8A_1 109.4 . . ?
N6_1 C8_1 H8B_1 109.4 . . ?
C7_1 C8_1 H8A_1 109.4 . . ?
C7_1 C8_1 H8B_1 109.4 . . ?
H8A_1 C8_1 H8B_1 108.0 . . ?
C3_1 C9_1 H9A_1 109.5 . . ?
C3_1 C9_1 H9B_1 109.5 . . ?
C3_1 C9_1 H9C_1 109.5 . . ?
H9A_1 C9_1 H9B_1 109.5 . . ?
H9A_1 C9_1 H9C_1 109.5 . . ?
H9B_1 C9_1 H9C_1 109.5 . . ?
H6A_2 N6_2 H6B_2 109.5 . . ?
H6A_2 N6_2 H6C_2 109.5 . . ?
H6B_2 N6_2 H6C_2 109.5 . . ?
C8_2 N6_2 H6A_2 109.5 . . ?
C8_2 N6_2 H6B_2 109.5 . . ?
C8_2 N6_2 H6C_2 109.5 . . ?
C2_2 C1_2 C6_2 119.3(3) . . ?
C2_2 C1_2 C7_2 119.9(3) . . ?
C6_2 C1_2 C7_2 120.9(3) . . ?
C1_2 C2_2 H2_2 119.3 . . ?
C1_2 C2_2 C3_2 121.5(3) . . ?
C3_2 C2_2 H2_2 119.3 . . ?
C2_2 C3_2 C9_2 120.4(3) . . ?
C4_2 C3_2 C2_2 118.0(2) . . ?
C4_2 C3_2 C9_2 121.5(3) . . ?
C3_2 C4_2 H4_2 119.5 . . ?
C5_2 C4_2 C3_2 121.1(3) . . ?
C5_2 C4_2 H4_2 119.5 . . ?
C4_2 C5_2 H5_2 119.7 . . ?
C4_2 C5_2 C6_2 120.6(3) . . ?
C6_2 C5_2 H5_2 119.7 . . ?
C1_2 C6_2 H6_2 120.2 . . ?
C5_2 C6_2 C1_2 119.5(3) . . ?
C5_2 C6_2 H6_2 120.2 . . ?
C1_2 C7_2 H7A_2 109.1 . . ?
C1_2 C7_2 H7B_2 109.1 . . ?
C1_2 C7_2 C8_2 112.7(3) . . ?
H7A_2 C7_2 H7B_2 107.8 . . ?
C8_2 C7_2 H7A_2 109.1 . . ?
C8_2 C7_2 H7B_2 109.1 . . ?
N6_2 C8_2 C7_2 111.2(3) . . ?
N6_2 C8_2 H8A_2 109.4 . . ?
N6_2 C8_2 H8B_2 109.4 . . ?
C7_2 C8_2 H8A_2 109.4 . . ?
C7_2 C8_2 H8B_2 109.4 . . ?
H8A_2 C8_2 H8B_2 108.0 . . ?
C3_2 C9_2 H9A_2 109.5 . . ?
C3_2 C9_2 H9B_2 109.5 . . ?
C3_2 C9_2 H9C_2 109.5 . . ?
H9A_2 C9_2 H9B_2 109.5 . . ?
H9A_2 C9_2 H9C_2 109.5 . . ?
H9B_2 C9_2 H9C_2 109.5 . . ?
H6A_3 N6_3 H6B_3 109.5 . . ?
H6A_3 N6_3 H6C_3 109.5 . . ?
H6B_3 N6_3 H6C_3 109.5 . . ?
C8_3 N6_3 H6A_3 109.5 . . ?
C8_3 N6_3 H6B_3 109.5 . . ?
C8_3 N6_3 H6C_3 109.5 . . ?
C2_3 C1_3 C6_3 119.2(3) . . ?
C2_3 C1_3 C7_3 120.0(3) . . ?
C6_3 C1_3 C7_3 120.8(3) . . ?
C1_3 C2_3 H2_3 119.2 . . ?
C1_3 C2_3 C3_3 121.6(3) . . ?
C3_3 C2_3 H2_3 119.2 . . ?
C2_3 C3_3 C9_3 120.4(3) . . ?
C4_3 C3_3 C2_3 117.9(2) . . ?
C4_3 C3_3 C9_3 121.6(3) . . ?
C3_3 C4_3 H4_3 119.5 . . ?
C5_3 C4_3 C3_3 121.1(3) . . ?
C5_3 C4_3 H4_3 119.5 . . ?
C4_3 C5_3 H5_3 119.7 . . ?
C4_3 C5_3 C6_3 120.7(3) . . ?
C6_3 C5_3 H5_3 119.7 . . ?
C1_3 C6_3 H6_3 120.2 . . ?
C5_3 C6_3 C1_3 119.5(3) . . ?
C5_3 C6_3 H6_3 120.2 . . ?
C1_3 C7_3 H7A_3 108.9 . . ?
C1_3 C7_3 H7B_3 108.9 . . ?
C1_3 C7_3 C8_3 113.2(2) . . ?
H7A_3 C7_3 H7B_3 107.8 . . ?
C8_3 C7_3 H7A_3 108.9 . . ?
C8_3 C7_3 H7B_3 108.9 . . ?
N6_3 C8_3 C7_3 111.4(3) . . ?
N6_3 C8_3 H8A_3 109.3 . . ?
N6_3 C8_3 H8B_3 109.3 . . ?
C7_3 C8_3 H8A_3 109.3 . . ?
C7_3 C8_3 H8B_3 109.3 . . ?
H8A_3 C8_3 H8B_3 108.0 . . ?
C3_3 C9_3 H9A_3 109.5 . . ?
C3_3 C9_3 H9B_3 109.5 . . ?
C3_3 C9_3 H9C_3 109.5 . . ?
H9A_3 C9_3 H9B_3 109.5 . . ?
H9A_3 C9_3 H9C_3 109.5 . . ?
H9B_3 C9_3 H9C_3 109.5 . . ?
H6A_4 N6_4 H6B_4 109.5 . . ?
H6A_4 N6_4 H6C_4 109.5 . . ?
H6B_4 N6_4 H6C_4 109.5 . . ?
C8_4 N6_4 H6A_4 109.5 . . ?
C8_4 N6_4 H6B_4 109.5 . . ?
C8_4 N6_4 H6C_4 109.5 . . ?
C2_4 C1_4 C6_4 119.1(2) . . ?
C2_4 C1_4 C7_4 120.1(3) . . ?
C6_4 C1_4 C7_4 120.8(3) . . ?
C1_4 C2_4 H2_4 119.2 . . ?
C1_4 C2_4 C3_4 121.6(3) . . ?
C3_4 C2_4 H2_4 119.2 . . ?
C2_4 C3_4 C9_4 120.4(3) . . ?
C4_4 C3_4 C2_4 118.0(2) . . ?
C4_4 C3_4 C9_4 121.5(3) . . ?
C3_4 C4_4 H4_4 119.5 . . ?
C5_4 C4_4 C3_4 121.0(3) . . ?
C5_4 C4_4 H4_4 119.5 . . ?
C4_4 C5_4 H5_4 119.7 . . ?
C4_4 C5_4 C6_4 120.7(3) . . ?
C6_4 C5_4 H5_4 119.7 . . ?
C1_4 C6_4 H6_4 120.2 . . ?
C5_4 C6_4 C1_4 119.6(3) . . ?
C5_4 C6_4 H6_4 120.2 . . ?
C1_4 C7_4 H7A_4 109.0 . . ?
C1_4 C7_4 H7B_4 109.0 . . ?
C1_4 C7_4 C8_4 113.0(2) . . ?
H7A_4 C7_4 H7B_4 107.8 . . ?
C8_4 C7_4 H7A_4 109.0 . . ?
C8_4 C7_4 H7B_4 109.0 . . ?
N6_4 C8_4 C7_4 111.2(3) . . ?
N6_4 C8_4 H8A_4 109.4 . . ?
N6_4 C8_4 H8B_4 109.4 . . ?
C7_4 C8_4 H8A_4 109.4 . . ?
C7_4 C8_4 H8B_4 109.4 . . ?
H8A_4 C8_4 H8B_4 108.0 . . ?
C3_4 C9_4 H9A_4 109.5 . . ?
C3_4 C9_4 H9B_4 109.5 . . ?
C3_4 C9_4 H9C_4 109.5 . . ?
H9A_4 C9_4 H9B_4 109.5 . . ?
H9A_4 C9_4 H9C_4 109.5 . . ?
H9B_4 C9_4 H9C_4 109.5 . . ?
H6A_5 N6_5 H6B_5 109.5 . . ?
H6A_5 N6_5 H6C_5 109.5 . . ?
H6B_5 N6_5 H6C_5 109.5 . . ?
C8_5 N6_5 H6A_5 109.5 . . ?
C8_5 N6_5 H6B_5 109.5 . . ?
C8_5 N6_5 H6C_5 109.5 . . ?
C2_5 C1_5 C6_5 119.1(3) . . ?
C2_5 C1_5 C7_5 120.3(3) . . ?
C6_5 C1_5 C7_5 120.6(3) . . ?
C1_5 C2_5 H2_5 119.2 . . ?
C1_5 C2_5 C3_5 121.6(3) . . ?
C3_5 C2_5 H2_5 119.2 . . ?
C2_5 C3_5 C9_5 120.4(3) . . ?
C4_5 C3_5 C2_5 118.0(2) . . ?
C4_5 C3_5 C9_5 121.5(3) . . ?
C3_5 C4_5 H4_5 119.5 . . ?
C5_5 C4_5 C3_5 120.9(3) . . ?
C5_5 C4_5 H4_5 119.5 . . ?
C4_5 C5_5 H5_5 119.6 . . ?
C4_5 C5_5 C6_5 120.7(3) . . ?
C6_5 C5_5 H5_5 119.6 . . ?
C1_5 C6_5 H6_5 120.2 . . ?
C5_5 C6_5 C1_5 119.5(3) . . ?
C5_5 C6_5 H6_5 120.2 . . ?
C1_5 C7_5 H7A_5 109.0 . . ?
C1_5 C7_5 H7B_5 109.0 . . ?
C1_5 C7_5 C8_5 112.9(2) . . ?
H7A_5 C7_5 H7B_5 107.8 . . ?
C8_5 C7_5 H7A_5 109.0 . . ?
C8_5 C7_5 H7B_5 109.0 . . ?
N6_5 C8_5 C7_5 111.3(3) . . ?
N6_5 C8_5 H8A_5 109.4 . . ?
N6_5 C8_5 H8B_5 109.4 . . ?
C7_5 C8_5 H8A_5 109.4 . . ?
C7_5 C8_5 H8B_5 109.4 . . ?
H8A_5 C8_5 H8B_5 108.0 . . ?
C3_5 C9_5 H9A_5 109.5 . . ?
C3_5 C9_5 H9B_5 109.5 . . ?
C3_5 C9_5 H9C_5 109.5 . . ?
H9A_5 C9_5 H9B_5 109.5 . . ?
H9A_5 C9_5 H9C_5 109.5 . . ?
H9B_5 C9_5 H9C_5 109.5 . . ?
H6A_6 N6_6 H6B_6 109.5 . . ?
H6A_6 N6_6 H6C_6 109.5 . . ?
H6B_6 N6_6 H6C_6 109.5 . . ?
C8_6 N6_6 H6A_6 109.5 . . ?
C8_6 N6_6 H6B_6 109.5 . . ?
C8_6 N6_6 H6C_6 109.5 . . ?
C2_6 C1_6 C6_6 119.1(2) . . ?
C2_6 C1_6 C7_6 120.2(3) . . ?
C6_6 C1_6 C7_6 120.7(3) . . ?
C1_6 C2_6 H2_6 119.2 . . ?
C1_6 C2_6 C3_6 121.6(3) . . ?
C3_6 C2_6 H2_6 119.2 . . ?
C2_6 C3_6 C9_6 120.4(3) . . ?
C4_6 C3_6 C2_6 118.1(2) . . ?
C4_6 C3_6 C9_6 121.5(3) . . ?
C3_6 C4_6 H4_6 119.6 . . ?
C5_6 C4_6 C3_6 120.9(3) . . ?
C5_6 C4_6 H4_6 119.6 . . ?
C4_6 C5_6 H5_6 119.6 . . ?
C4_6 C5_6 C6_6 120.8(3) . . ?
C6_6 C5_6 H5_6 119.6 . . ?
C1_6 C6_6 H6_6 120.2 . . ?
C5_6 C6_6 C1_6 119.6(3) . . ?
C5_6 C6_6 H6_6 120.2 . . ?
C1_6 C7_6 H7A_6 109.0 . . ?
C1_6 C7_6 H7B_6 109.0 . . ?
C1_6 C7_6 C8_6 112.7(2) . . ?
H7A_6 C7_6 H7B_6 107.8 . . ?
C8_6 C7_6 H7A_6 109.0 . . ?
C8_6 C7_6 H7B_6 109.0 . . ?
N6_6 C8_6 C7_6 111.2(3) . . ?
N6_6 C8_6 H8A_6 109.4 . . ?
N6_6 C8_6 H8B_6 109.4 . . ?
C7_6 C8_6 H8A_6 109.4 . . ?
C7_6 C8_6 H8B_6 109.4 . . ?
H8A_6 C8_6 H8B_6 108.0 . . ?
C3_6 C9_6 H9A_6 109.5 . . ?
C3_6 C9_6 H9B_6 109.5 . . ?
C3_6 C9_6 H9C_6 109.5 . . ?
H9A_6 C9_6 H9B_6 109.5 . . ?
H9A_6 C9_6 H9C_6 109.5 . . ?
H9B_6 C9_6 H9C_6 109.5 . . ?
H6A_7 N6_7 H6B_7 109.5 . . ?
H6A_7 N6_7 H6C_7 109.5 . . ?
H6B_7 N6_7 H6C_7 109.5 . . ?
C8_7 N6_7 H6A_7 109.5 . . ?
C8_7 N6_7 H6B_7 109.5 . . ?
C8_7 N6_7 H6C_7 109.5 . . ?
C2_7 C1_7 C6_7 119.2(2) . . ?
C2_7 C1_7 C7_7 120.0(3) . . ?
C6_7 C1_7 C7_7 120.8(3) . . ?
C1_7 C2_7 H2_7 119.2 . . ?
C1_7 C2_7 C3_7 121.6(3) . . ?
C3_7 C2_7 H2_7 119.2 . . ?
C2_7 C3_7 C9_7 120.5(3) . . ?
C4_7 C3_7 C2_7 118.0(2) . . ?
C4_7 C3_7 C9_7 121.5(3) . . ?
C3_7 C4_7 H4_7 119.5 . . ?
C5_7 C4_7 C3_7 121.1(3) . . ?
C5_7 C4_7 H4_7 119.5 . . ?
C4_7 C5_7 H5_7 119.7 . . ?
C4_7 C5_7 C6_7 120.6(3) . . ?
C6_7 C5_7 H5_7 119.7 . . ?
C1_7 C6_7 H6_7 120.2 . . ?
C5_7 C6_7 C1_7 119.6(3) . . ?
C5_7 C6_7 H6_7 120.2 . . ?
C1_7 C7_7 H7A_7 109.0 . . ?
C1_7 C7_7 H7B_7 109.0 . . ?
C1_7 C7_7 C8_7 112.7(2) . . ?
H7A_7 C7_7 H7B_7 107.8 . . ?
C8_7 C7_7 H7A_7 109.0 . . ?
C8_7 C7_7 H7B_7 109.0 . . ?
N6_7 C8_7 C7_7 111.3(3) . . ?
N6_7 C8_7 H8A_7 109.4 . . ?
N6_7 C8_7 H8B_7 109.4 . . ?
C7_7 C8_7 H8A_7 109.4 . . ?
C7_7 C8_7 H8B_7 109.4 . . ?
H8A_7 C8_7 H8B_7 108.0 . . ?
C3_7 C9_7 H9A_7 109.5 . . ?
C3_7 C9_7 H9B_7 109.5 . . ?
C3_7 C9_7 H9C_7 109.5 . . ?
H9A_7 C9_7 H9B_7 109.5 . . ?
H9A_7 C9_7 H9C_7 109.5 . . ?
H9B_7 C9_7 H9C_7 109.5 . . ?
I1B Pb1_8 I4B 91.2(2) . . ?
I1B Pb1_8 I4B 88.8(2) 2_666 . ?
I1B Pb1_8 I14B 85.9(4) . . ?
I1B Pb1_8 I14B 94.1(4) 2_666 . ?
I4B Pb1_8 I4B 180.0 2_666 . ?
I4B Pb1_8 I14B 88.9(5) 2_666 . ?
I4B Pb1_8 I14B 91.1(5) . . ?
I14B Pb1_8 I14B 180.0 2_666 . ?
I1_8 Pb1_8 I4B 119.56(17) . 2_666 ?
I1_8 Pb1_8 I4B 60.44(17) 2_666 2_666 ?
I1_8 Pb1_8 I14B 86.4(5) . 2_666 ?
I1_8 Pb1_8 I14B 93.6(5) 2_666 2_666 ?
I1_8 Pb1_8 I1_8 179.999(12) . 2_666 ?
I1_8 Pb1_8 I4_8 88.122(8) 2_666 2_666 ?
I1_8 Pb1_8 I4_8 88.122(9) . . ?
I1_8 Pb1_8 I4_8 91.879(8) 2_666 . ?
I1_8 Pb1_8 I4_8 91.877(8) . 2_666 ?
I1_8 Pb1_8 I9_8 89.542(14) 2_666 . ?
I1_8 Pb1_8 I9_8 90.459(14) . . ?
I1_8 Pb1_8 I9_8 89.542(14) . 2_666 ?
I1_8 Pb1_8 I9_8 90.458(14) 2_666 2_666 ?
I4_8 Pb1_8 I4B 27.69(17) 2_666 2_666 ?
I4_8 Pb1_8 I4B 152.31(17) . 2_666 ?
I4_8 Pb1_8 I14B 90.0(4) . 2_666 ?
I4_8 Pb1_8 I14B 90.0(4) 2_666 2_666 ?
I4_8 Pb1_8 I4_8 180.0 . 2_666 ?
I4_8 Pb1_8 I9_8 86.169(12) 2_666 . ?
I4_8 Pb1_8 I9_8 93.832(12) . . ?
I4_8 Pb1_8 I9_8 86.167(12) . 2_666 ?
I4_8 Pb1_8 I9_8 93.832(12) 2_666 2_666 ?
I9_8 Pb1_8 I14B 5.1(4) 2_666 2_666 ?
I9_8 Pb1_8 I14B 175.0(4) . 2_666 ?
I9_8 Pb1_8 I9_8 180.0 . 2_666 ?
I1_8 Pb2A_8 I2_8 89.864(10) . . ?
I1_8 Pb2A_8 I8_8 89.334(10) . 1_455 ?
I1_8 Pb2A_8 I10_8 84.653(9) . . ?
I2_8 Pb2A_8 I8_8 172.826(11) . 1_455 ?
I2_8 Pb2A_8 I10_8 84.932(9) . . ?
I5_8 Pb2A_8 I1_8 171.758(11) . . ?
I5_8 Pb2A_8 I2_8 92.316(11) . . ?
I5_8 Pb2A_8 I8_8 87.512(10) . 1_455 ?
I5_8 Pb2A_8 I10_8 87.623(10) . . ?
I8_8 Pb2A_8 I10_8 87.895(9) 1_455 . ?
I11_8 Pb2A_8 I1_8 95.639(11) . . ?
I11_8 Pb2A_8 I2_8 96.016(10) . . ?
I11_8 Pb2A_8 I5_8 92.037(10) . . ?
I11_8 Pb2A_8 I8_8 91.157(10) . 1_455 ?
I11_8 Pb2A_8 I10_8 179.005(11) . . ?
I3B Pb3B_8 I2B 88.7(3) . . ?
I6B Pb3B_8 I2B 91.3(3) . . ?
I6B Pb3B_8 I3B 170.9(4) . . ?
I8B Pb3B_8 I2B 171.3(4) . . ?
I8B Pb3B_8 I3B 89.8(3) . . ?
I8B Pb3B_8 I6B 88.8(3) . . ?
I3B Pb4_8 I3B 180.0 2_766 . ?
I3B Pb4_8 I4B 92.4(2) 2_766 . ?
I3B Pb4_8 I4B 87.6(3) . . ?
I3_8 Pb4_8 I3B 150.74(18) 2_766 2_766 ?
I3_8 Pb4_8 I3B 29.26(18) . 2_766 ?
I3_8 Pb4_8 I4B 63.11(18) 2_766 2_766 ?
I3_8 Pb4_8 I4B 116.89(18) . 2_766 ?
I3_8 Pb4_8 I3_8 180.0 2_766 . ?
I3_8 Pb4_8 I4_8 90.883(9) . . ?
I3_8 Pb4_8 I4_8 89.116(8) 2_766 . ?
I3_8 Pb4_8 I4_8 90.885(8) 2_766 2_766 ?
I3_8 Pb4_8 I4_8 89.116(8) . 2_766 ?
I3_8 Pb4_8 I14_8 86.855(8) . 2_766 ?
I3_8 Pb4_8 I14_8 93.146(8) . . ?
I3_8 Pb4_8 I14_8 86.854(8) 2_766 . ?
I3_8 Pb4_8 I14_8 93.145(8) 2_766 2_766 ?
I4_8 Pb4_8 I4_8 180.0 . 2_766 ?
I4_8 Pb4_8 I14_8 90.498(8) . 2_766 ?
I4_8 Pb4_8 I14_8 90.498(8) 2_766 . ?
I4_8 Pb4_8 I14_8 89.501(8) 2_766 2_766 ?
I4_8 Pb4_8 I14_8 89.503(8) . . ?
I14_8 Pb4_8 I14_8 180.0 2_766 . ?
I1 Pb5_8 I1 180.0 2_665 . ?
I5_8 Pb5_8 I1 116.62(17) 2_665 2_665 ?
I5_8 Pb5_8 I1 63.38(17) . 2_665 ?
I5_8 Pb5_8 I5B 28.94(18) . 2_666 ?
I5_8 Pb5_8 I5B 151.06(18) . 1_554 ?
I5_8 Pb5_8 I5B 28.94(18) 2_665 1_554 ?
I5_8 Pb5_8 I5B 151.06(18) 2_665 2_666 ?
I5_8 Pb5_8 I5_8 180.0 . 2_665 ?
I5_8 Pb5_8 I6_8 90.846(8) . 2_665 ?
I5_8 Pb5_8 I6_8 89.154(8) . . ?
I5_8 Pb5_8 I6_8 89.154(9) 2_665 2_665 ?
I5_8 Pb5_8 I6_8 90.845(8) 2_665 . ?
I5_8 Pb5_8 I15_8 93.212(8) . 2_665 ?
I5_8 Pb5_8 I15_8 93.214(8) 2_665 . ?
I5_8 Pb5_8 I15_8 86.787(8) . . ?
I5_8 Pb5_8 I15_8 86.787(8) 2_665 2_665 ?
I6_8 Pb5_8 I6_8 180.0 2_665 . ?
I6_8 Pb5_8 I15_8 90.533(8) 2_665 . ?
I6_8 Pb5_8 I15_8 90.534(8) . 2_665 ?
I6_8 Pb5_8 I15_8 89.467(8) 2_665 2_665 ?
I6_8 Pb5_8 I15_8 89.466(8) . . ?
I15_8 Pb5_8 I15_8 180.0 2_665 . ?
I1 Pb6_8 I16_8 87.20(17) . 2_765 ?
I1 Pb6_8 I16_8 92.80(17) 2_765 2_765 ?
I6B Pb6_8 I1 88.8(2) 1_554 . ?
I6B Pb6_8 I1 91.2(2) 2_766 . ?
I6B Pb6_8 I16_8 90.68(17) 1_554 2_765 ?
I6B Pb6_8 I16_8 89.32(17) 2_766 2_765 ?
I6_8 Pb6_8 I1 152.61(18) . 2_765 ?
I6_8 Pb6_8 I1 27.40(18) 2_765 2_765 ?
I6_8 Pb6_8 I6_8 180.0 . 2_765 ?
I6_8 Pb6_8 I16_8 93.765(8) 2_765 2_765 ?
I6_8 Pb6_8 I16_8 86.236(8) . 2_765 ?
I6_8 Pb6_8 I16_8 86.234(8) 2_765 . ?
I6_8 Pb6_8 I16_8 93.765(8) . . ?
I7_8 Pb6_8 I1 60.68(18) . 2_765 ?
I7_8 Pb6_8 I1 119.32(18) 2_765 2_765 ?
I7_8 Pb6_8 I6_8 88.065(8) 2_765 . ?
I7_8 Pb6_8 I6_8 91.935(8) 2_765 2_765 ?
I7_8 Pb6_8 I6_8 88.065(8) . 2_765 ?
I7_8 Pb6_8 I6_8 91.936(8) . . ?
I7_8 Pb6_8 I7_8 180.0 . 2_765 ?
I7_8 Pb6_8 I16_8 89.507(8) . . ?
I7_8 Pb6_8 I16_8 90.494(8) . 2_765 ?
I7_8 Pb6_8 I16_8 89.506(8) 2_765 2_765 ?
I7_8 Pb6_8 I16_8 90.493(8) 2_765 . ?
I16_8 Pb6_8 I16_8 180.0 . 2_765 ?
Pb1_8 I1_8 Pb2A_8 151.065(12) . . ?
Pb2A_8 I2_8 Pb3A 153.607(13) . . ?
Pb4_8 I3_8 Pb3A 151.163(12) . . ?
Pb1_8 I4_8 Pb4_8 152.388(12) . . ?
Pb5_8 I5_8 Pb2A_8 151.129(12) . . ?
Pb6_8 I6_8 Pb5_8 152.469(11) . . ?
Pb3A I7_8 Pb6_8 151.086(12) . . ?
Pb3A I8_8 Pb2A_8 153.452(13) . 1_655 ?

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
C1 C2 C3 C4 2.1(7) . . . . ?
C1 C2 C3 C9 -175.1(5) . . . . ?
C1 C7 C8 N6 61.1(6) . . . . ?
C2 C1 C6 C5 0.4(7) . . . . ?
C2 C1 C7 C8 80.5(6) . . . . ?
C2 C3 C4 C5 -1.5(7) . . . . ?
C3 C4 C5 C6 0.3(8) . . . . ?
C4 C5 C6 C1 0.2(8) . . . . ?
C6 C1 C2 C3 -1.6(7) . . . . ?
C6 C1 C7 C8 -98.9(6) . . . . ?
C7 C1 C2 C3 179.0(4) . . . . ?
C7 C1 C6 C5 179.8(5) . . . . ?
C9 C3 C4 C5 175.7(5) . . . . ?
C1_1 C2_1 C3_1 C4_1 -1.6(7) . . . . ?
C1_1 C2_1 C3_1 C9_1 174.5(4) . . . . ?
C1_1 C7_1 C8_1 N6_1 -59.7(4) . . . . ?
C2_1 C1_1 C6_1 C5_1 1.7(7) . . . . ?
C2_1 C1_1 C7_1 C8_1 -81.0(5) . . . . ?
C2_1 C3_1 C4_1 C5_1 1.3(8) . . . . ?
C3_1 C4_1 C5_1 C6_1 0.6(8) . . . . ?
C4_1 C5_1 C6_1 C1_1 -2.1(8) . . . . ?
C6_1 C1_1 C2_1 C3_1 0.1(7) . . . . ?
C6_1 C1_1 C7_1 C8_1 99.7(4) . . . . ?
C7_1 C1_1 C2_1 C3_1 -179.1(4) . . . . ?
C7_1 C1_1 C6_1 C5_1 -179.0(4) . . . . ?
C9_1 C3_1 C4_1 C5_1 -174.8(5) . . . . ?
C1_2 C2_2 C3_2 C4_2 0.6(7) . . . . ?
C1_2 C2_2 C3_2 C9_2 -176.3(5) . . . . ?
C1_2 C7_2 C8_2 N6_2 60.3(4) . . . . ?
C2_2 C1_2 C6_2 C5_2 -1.8(7) . . . . ?
C2_2 C1_2 C7_2 C8_2 80.1(5) . . . . ?
C2_2 C3_2 C4_2 C5_2 -0.8(7) . . . . ?
C3_2 C4_2 C5_2 C6_2 -0.4(8) . . . . ?
C4_2 C5_2 C6_2 C1_2 1.7(8) . . . . ?
C6_2 C1_2 C2_2 C3_2 0.7(7) . . . . ?
C6_2 C1_2 C7_2 C8_2 -99.2(5) . . . . ?
C7_2 C1_2 C2_2 C3_2 -178.6(4) . . . . ?
C7_2 C1_2 C6_2 C5_2 177.5(4) . . . . ?
C9_2 C3_2 C4_2 C5_2 176.1(5) . . . . ?
C1_3 C2_3 C3_3 C4_3 0.5(7) . . . . ?
C1_3 C2_3 C3_3 C9_3 -177.4(4) . . . . ?
C1_3 C7_3 C8_3 N6_3 -59.9(4) . . . . ?
C2_3 C1_3 C6_3 C5_3 0.5(7) . . . . ?
C2_3 C1_3 C7_3 C8_3 107.7(4) . . . . ?
C2_3 C3_3 C4_3 C5_3 -1.3(7) . . . . ?
C3_3 C4_3 C5_3 C6_3 1.8(8) . . . . ?
C4_3 C5_3 C6_3 C1_3 -1.4(8) . . . . ?
C6_3 C1_3 C2_3 C3_3 -0.1(7) . . . . ?
C6_3 C1_3 C7_3 C8_3 -71.7(5) . . . . ?
C7_3 C1_3 C2_3 C3_3 -179.6(4) . . . . ?
C7_3 C1_3 C6_3 C5_3 180.0(4) . . . . ?
C9_3 C3_3 C4_3 C5_3 176.5(5) . . . . ?
C1_4 C2_4 C3_4 C4_4 -0.4(7) . . . . ?
C1_4 C2_4 C3_4 C9_4 176.1(4) . . . . ?
C1_4 C7_4 C8_4 N6_4 58.0(5) . . . . ?
C2_4 C1_4 C6_4 C5_4 -0.4(7) . . . . ?
C2_4 C1_4 C7_4 C8_4 -108.5(4) . . . . ?
C2_4 C3_4 C4_4 C5_4 0.7(7) . . . . ?
C3_4 C4_4 C5_4 C6_4 -0.8(8) . . . . ?
C4_4 C5_4 C6_4 C1_4 0.6(8) . . . . ?
C6_4 C1_4 C2_4 C3_4 0.3(7) . . . . ?
C6_4 C1_4 C7_4 C8_4 71.2(5) . . . . ?
C7_4 C1_4 C2_4 C3_4 -180.0(4) . . . . ?
C7_4 C1_4 C6_4 C5_4 179.8(4) . . . . ?
C9_4 C3_4 C4_4 C5_4 -175.8(5) . . . . ?
C1_5 C2_5 C3_5 C4_5 -0.4(7) . . . . ?
C1_5 C2_5 C3_5 C9_5 177.3(4) . . . . ?
C1_5 C7_5 C8_5 N6_5 59.4(4) . . . . ?
C2_5 C1_5 C6_5 C5_5 0.6(7) . . . . ?
C2_5 C1_5 C7_5 C8_5 -107.9(4) . . . . ?
C2_5 C3_5 C4_5 C5_5 0.8(8) . . . . ?
C3_5 C4_5 C5_5 C6_5 -0.5(8) . . . . ?
C4_5 C5_5 C6_5 C1_5 -0.2(8) . . . . ?
C6_5 C1_5 C2_5 C3_5 -0.3(7) . . . . ?
C6_5 C1_5 C7_5 C8_5 72.5(5) . . . . ?
C7_5 C1_5 C2_5 C3_5 -179.9(4) . . . . ?
C7_5 C1_5 C6_5 C5_5 -179.8(4) . . . . ?
C9_5 C3_5 C4_5 C5_5 -176.8(5) . . . . ?
C1_6 C2_6 C3_6 C4_6 0.9(7) . . . . ?
C1_6 C2_6 C3_6 C9_6 -176.7(4) . . . . ?
C1_6 C7_6 C8_6 N6_6 -58.3(5) . . . . ?
C2_6 C1_6 C6_6 C5_6 -0.8(7) . . . . ?
C2_6 C1_6 C7_6 C8_6 109.6(4) . . . . ?
C2_6 C3_6 C4_6 C5_6 -1.6(7) . . . . ?
C3_6 C4_6 C5_6 C6_6 1.1(8) . . . . ?
C4_6 C5_6 C6_6 C1_6 0.1(8) . . . . ?
C6_6 C1_6 C2_6 C3_6 0.3(7) . . . . ?
C6_6 C1_6 C7_6 C8_6 -71.6(5) . . . . ?
C7_6 C1_6 C2_6 C3_6 179.1(4) . . . . ?
C7_6 C1_6 C6_6 C5_6 -179.6(4) . . . . ?
C9_6 C3_6 C4_6 C5_6 176.0(5) . . . . ?
C1_7 C2_7 C3_7 C4_7 -1.9(7) . . . . ?
C1_7 C2_7 C3_7 C9_7 176.2(4) . . . . ?
C1_7 C7_7 C8_7 N6_7 -61.0(4) . . . . ?
C2_7 C1_7 C6_7 C5_7 -0.4(7) . . . . ?
C2_7 C1_7 C7_7 C8_7 -79.0(5) . . . . ?
C2_7 C3_7 C4_7 C5_7 1.1(7) . . . . ?
C3_7 C4_7 C5_7 C6_7 0.0(8) . . . . ?
C4_7 C5_7 C6_7 C1_7 -0.4(8) . . . . ?
C6_7 C1_7 C2_7 C3_7 1.5(7) . . . . ?
C6_7 C1_7 C7_7 C8_7 98.9(4) . . . . ?
C7_7 C1_7 C2_7 C3_7 179.5(4) . . . . ?
C7_7 C1_7 C6_7 C5_7 -178.3(4) . . . . ?
C9_7 C3_7 C4_7 C5_7 -177.0(5) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id 3ME-PEA
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.580
_oxdiff_exptl_absorpt_empirical_full_min 0.706
