# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 2033297'
loop_
_audit_author_name
_audit_author_address
lidong
;FJRISM
China
;
_audit_update_record             
;
2020-09-22 deposited with the CCDC.	2021-01-04 downloaded from the CCDC.
;
_audit_creation_date             2020-08-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(I20 Pb6), C2 H12 N2, C8 H22 I2 N2'
_chemical_formula_sum            'C10 H34 I12 N4 Pb3'
_chemical_formula_weight         2354.78
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   8.909(2)
_cell_length_b                   9.012(3)
_cell_length_c                   27.896(8)
_cell_angle_alpha                90
_cell_angle_beta                 92.832(10)
_cell_angle_gamma                90
_cell_volume                     2237.1(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8253
_cell_measurement_temperature    385(2)
_cell_measurement_theta_max      27.76
_cell_measurement_theta_min      2.37
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.550
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.496
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            17421
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.991
_diffrn_reflns_theta_max         24.991
_diffrn_reflns_theta_min         2.193
_diffrn_ambient_temperature      385.05
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1684
_reflns_number_total             2111
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         6.355
_refine_diff_density_min         -3.712
_refine_diff_density_rms         0.460
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2111
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0948
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1452P)²+146.3748P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2620
_refine_ls_wR_factor_ref         0.2731
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: H6C(0.5) H6D(0.5) H6E(0.5) H8A(0.5) H8B(0.5) H8C(0.5) H5A(0.5)
 H5B(0.5) H5C(0.5) C6(0.5) H6A(0.5) H6B(0.5) C15(0.5) H15A(0.5) H15B(0.5)
 H27A(0.5) H27B(0.5) H60A(0.5) H60B(0.5) I29(0.5)
 Fixed U11: Pb00(0.047846) Pb1(0.051974) I003(0.087806) I004(0.115715)
 I005(0.171714) I006(0.218042) N6(0.410025) C8(0.41103) N5(0.713406)
 C6(0.727327) C15(0.730745) C27(0.73204) C60(0.732263) I29(0.2829)
 Fixed U12: Pb00(0) Pb1(0) I003(0.048207) I004(-0.078194) I005(0) I006(0)
 N6(0) C8(0) N5(0) C6(0.000148) C15(0.002151) C27(0) C60(0) I29(-0.054264)
 Fixed U13: Pb00(0.001482) Pb1(0.000085) I003(-0.002739) I004(0.000477)
 I005(0.006278) I006(0.00393) N6(-0.000257) C8(-0.000307) N5(-0.141744) C6(-
 0.150706) C15(-0.155008) C27(-0.168172) C60(-0.160409) I29(-0.015491)
 Fixed U22: Pb00(0.043) Pb1(0.046) I003(0.082) I004(0.108) I005(0.269)
 I006(0.474) N6(0.41) C8(0.411) N5(0.271) C6(0.279) C15(0.284) C27(0.284)
 C60(0.288) I29(0.244)
 Fixed U23: Pb00(0) Pb1(0) I003(-0.003) I004(0.002) I005(0) I006(0) N6(0)
 C8(0) N5(0) C6(-0.003) C15(-0.003) C27(0) C60(0) I29(0.004)
 Fixed U33: Pb00(0.051) Pb1(0.059) I003(0.278) I004(0.213) I005(0.035)
 I006(0.042) N6(0.41) C8(0.411) N5(0.133) C6(0.132) C15(0.138) C27(0.141)
 C60(0.146) I29(0.131)
 Fixed Uiso: Pb00(0.047) Pb1(0.052) I003(0.15) I004(0.145) I005(0.159)
 I006(0.245) N6(0.41) H6C(0.492) H6D(0.492) H6E(0.492) C8(0.411) H8A(0.616)
 H8B(0.616) H8C(0.616) N5(0.372) H5A(0.447) H5B(0.447) H5C(0.447) C6(0.379)
 H6A(0.455) H6B(0.455) C15(0.384) H15A(0.461) H15B(0.461) C27(0.385)
 H27A(0.462) H27B(0.462) C60(0.389) H60A(0.466) H60B(0.466) I29(0.22)
 Fixed X: Pb00(0.5) I004(0.25) H6C(0.593) H6D(0.5182) H6E(0.5368) H8A(0.2955)
 H8B(0.3514) H8C(0.3778) H5A(0.4954) H5B(0.367) H5C(0.518) H6A(0.5776)
 H6B(0.4547) H15A(0.4292) H15B(0.3145) H27A(0.4127) H27B(0.2943) H60A(0.2555)
 H60B(0.1633)
 Fixed Y: Pb00(0.5) Pb1(0.5) I004(0.25) I005(0.5) I006(0.5) N6(0) H6C(0.0223)
 H6D(0.0671) H6E(-0.0894) C8(0) H8A(-0.0316) H8B(0.0983) H8C(-0.0668) N5(0)
 H5A(-0.0826) H5B(0.0153) H5C(0.0765) H6A(0.0068) H6B(-0.1177) H15A(0.1502)
 H15B(0.1427) C27(0) H27A(-0.0206) H27B(0.1018) C60(0) H60A(-0.1018)
 H60B(0.0443)
 Fixed Z: Pb00(0.5) I004(0.5) H6C(0.4064) H6D(0.3613) H6E(0.3725) H8A(0.385)
 H8B(0.4187) H8C(0.4347) H5A(0.2064) H5B(0.1984) H5C(0.2025) H6A(0.1308)
 H6B(0.1297) H15A(0.0914) H15B(0.1322) H27A(0.0273) H27B(0.0153) H60A(0.0883)
 H60B(0.0789)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb00 Pb 0.5000 0.5000 0.5000 0.047 Uani 1 4 d S T P . .
Pb1 Pb 0.53713(2) 0.5000 0.73152(2) 0.052 Uani 1 2 d S T P . .
I003 I 0.28402(2) 0.74737(2) 0.72876(2) 0.150 Uani 1 1 d . . . . .
I004 I 0.2500 0.2500 0.5000 0.145 Uani 1 2 d S T P . .
I005 I 0.51790(2) 0.5000 0.61365(2) 0.159 Uani 1 2 d DS T P . .
I006 I 0.56463(2) 0.5000 0.84054(2) 0.245 Uani 1 2 d S T P . .
N6 N 0.52004(2) 0.0000 0.38470(2) 0.410 Uani 1 2 d DS TU P . .
H6C H 0.5930 0.0223 0.4064 0.492 Uiso 0.5 1 calc GR . . A -1
H6D H 0.5182 0.0671 0.3613 0.492 Uiso 0.5 1 calc GR . . A -1
H6E H 0.5368 -0.0894 0.3725 0.492 Uiso 0.5 1 calc GR . . A -1
C8 C 0.37315(2) 0.0000 0.40782(2) 0.411 Uani 1 2 d DS TU P . .
H8A H 0.2955 -0.0316 0.3850 0.616 Uiso 0.5 1 calc GR . . B -1
H8B H 0.3514 0.0983 0.4187 0.616 Uiso 0.5 1 calc GR . . B -1
H8C H 0.3778 -0.0668 0.4347 0.616 Uiso 0.5 1 calc GR . . B -1
N5 N 0.46264(2) 0.0000 0.19192(2) 0.372 Uani 1 2 d DS TU P . .
H5A H 0.4954 -0.0826 0.2064 0.447 Uiso 0.5 1 calc GR . . C -1
H5B H 0.3670 0.0153 0.1984 0.447 Uiso 0.5 1 calc GR . . C -1
H5C H 0.5180 0.0765 0.2025 0.447 Uiso 0.5 1 calc GR . . C -1
C6 C 0.47524(2) -0.01554(2) 0.13877(2) 0.379 Uani 0.5 1 d D U . D -1
H6A H 0.5776 0.0068 0.1308 0.455 Uiso 0.5 1 calc R . . D -1
H6B H 0.4547 -0.1177 0.1297 0.455 Uiso 0.5 1 calc R . . D -1
C15 C 0.37078(2) 0.08318(2) 0.11030(2) 0.384 Uani 0.5 1 d D U . D -1
H15A H 0.4292 0.1502 0.0914 0.461 Uiso 0.5 1 calc R . . D -1
H15B H 0.3145 0.1427 0.1322 0.461 Uiso 0.5 1 calc R . . D -1
C27 C 0.30573(2) 0.0000 0.02615(2) 0.385 Uani 1 2 d DS TU P . .
H27A H 0.4127 -0.0206 0.0273 0.462 Uiso 0.5 1 calc R . . E .
H27B H 0.2943 0.1018 0.0153 0.462 Uiso 0.5 1 calc R . . . .
C60 C 0.26211(2) 0.0000 0.07724(2) 0.389 Uani 1 2 d DS TU P D .
H60A H 0.2555 -0.1018 0.0883 0.466 Uiso 0.5 1 calc R . . . .
H60B H 0.1633 0.0443 0.0789 0.466 Uiso 0.5 1 calc R . . . .
I29 I 0.21601(2) -0.12596(2) -0.02724(2) 0.220 Uani 0.5 1 d D U . E -1


_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
Pb00 I004 3.1681(6) . ?
Pb00 I004 3.1681(6) 2_656 ?
Pb00 I004 3.1681(6) 4_556 ?
Pb00 I004 3.1681(6) 3 ?
Pb00 I005 3.1666(9) . ?
Pb00 I005 3.1665(10) 5_666 ?
Pb1 I003 3.1693(6) 3_545 ?
Pb1 I003 3.1692(6) . ?
Pb1 I003 3.1692(6) 6_565 ?
Pb1 I003 3.1693(6) 8_565 ?
Pb1 I005 3.2842(10) . ?
Pb1 I006 3.0390(9) . ?
I003 Pb1 3.1693(6) 3_455 ?
I004 Pb00 3.1681(6) 3_445 ?
N6 C8 1.4873(3) . ?
N5 C6 1.4990(4) . ?
C6 C15 1.4884(3) . ?
C15 C60 1.5039(3) . ?
C27 C60 1.4957(4) . ?
C27 I29 2.0070(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I004 Pb00 I004 180.0 . 3 ?
I004 Pb00 I004 180.0 2_656 4_556 ?
I004 Pb00 I004 89.34(2) 3 4_556 ?
I004 Pb00 I004 89.34(2) . 2_656 ?
I004 Pb00 I004 90.66(2) . 4_556 ?
I004 Pb00 I004 90.66(2) 3 2_656 ?
I005 Pb00 I004 89.964(7) 5_666 . ?
I005 Pb00 I004 89.964(7) 5_666 4_556 ?
I005 Pb00 I004 90.036(7) 5_666 3 ?
I005 Pb00 I004 90.036(7) . . ?
I005 Pb00 I004 89.964(7) . 2_656 ?
I005 Pb00 I004 90.036(7) 5_666 2_656 ?
I005 Pb00 I004 90.036(7) . 4_556 ?
I005 Pb00 I004 89.964(7) . 3 ?
I005 Pb00 I005 180.0 5_666 . ?
I003 Pb1 I003 89.31(2) . 8_565 ?
I003 Pb1 I003 177.0 6_565 8_565 ?
I003 Pb1 I003 177.0 . 3_545 ?
I003 Pb1 I003 91.84(2) 8_565 3_545 ?
I003 Pb1 I003 89.31(2) 6_565 3_545 ?
I003 Pb1 I003 89.41(2) 6_565 . ?
I003 Pb1 I005 88.717(7) 3_545 . ?
I003 Pb1 I005 88.717(7) 8_565 . ?
I003 Pb1 I005 88.500(7) . . ?
I003 Pb1 I005 88.500(7) 6_565 . ?
I006 Pb1 I003 92.659(7) . 6_565 ?
I006 Pb1 I003 90.148(8) . 8_565 ?
I006 Pb1 I003 92.659(7) . . ?
I006 Pb1 I003 90.148(7) . 3_545 ?
I006 Pb1 I005 178.368(1) . . ?
Pb1 I003 Pb1 176.964(1) . 3_455 ?
Pb00 I004 Pb00 180.0 3_445 . ?
Pb00 I005 Pb1 179.9 . . ?
C15 C6 N5 113.362(13) . . ?
C6 C15 C60 113.321(19) . . ?
C60 C27 I29 126.472(14) . . ?
C27 C60 C15 113.245(15) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_b
_database_code_depnum_ccdc_archive 'CCDC 2033299'
loop_
_audit_author_name
_audit_author_address
lidong
;FJRISM
China
;
_audit_update_record             
;
2020-09-22 deposited with the CCDC.	2021-01-04 downloaded from the CCDC.
;
_audit_creation_date             2020-09-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I10 Pb3, 2(C4 H11 I N), 2(C H6 N)'
_chemical_formula_sum            'C10 H34 I12 N4 Pb3'
_chemical_formula_weight         2354.78
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   27.3848(12)
_cell_length_b                   9.0015(4)
_cell_length_c                   8.8216(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.9990(10)
_cell_angle_gamma                90
_cell_volume                     2162.65(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.38
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.223
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.616
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            36105
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.420
_diffrn_reflns_theta_min         2.243
_diffrn_ambient_temperature      290.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                6463
_reflns_number_total             8192
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         5.668
_refine_diff_density_min         -3.495
_refine_diff_density_rms         0.514
_refine_ls_abs_structure_details 
;
 Flack x determined using 2407 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         8192
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0627
_refine_ls_restrained_S_all      1.033
_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)+(0.0955P)²+44.0087P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.1831
_refine_special_details          ?
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.512(10)
 0.488(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2-C3 = C3-C4 = C5-C4 = C5-C6
 1.49 with sigma of 0.02
 C8-C9 = C8-C7
 1.49 with sigma of 0.02
 N1-C10 = C9-C10 = C8-C7 = C8-C9
 1.49 with sigma of 0.02
 N3-C2 = N4-C1
 1.49 with sigma of 0.02
4. Rigid bond restraints
 C1, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C2, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N1, C10, C9, C8, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C6, C5, C4, C3, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C1 \\sim N4: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C2 \\sim N3: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C6 \\sim C5 \\sim C4 \\sim C3 \\sim N2: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C10 \\sim C9 \\sim C8 \\sim C7 \\sim N1: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C5(H5A,H5B), C4(H4A,H4B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B)
6.b Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N1(H1A,H1B,H1C), N4(H4C,H4D,H4E), N3(H3C,H3D,H3E), C1(H1D,
 H1E,H1F), C2(H2D,H2E,H2F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.19075(2) 0.74926(4) 0.45604(3) 0.03140(11) Uani 1 1 d . . . . .
Pb2 Pb 0.42531(4) 0.75024(7) 0.53715(9) 0.03182(8) Uani 1 1 d . . . . .
Pb3 Pb 0.66112(2) 0.75080(4) 0.61337(3) 0.03047(11) Uani 1 1 d . . . . .
I1 I 0.08085(3) 0.68146(11) 0.44628(11) 0.0572(3) Uani 1 1 d . . . . .
I10 I 0.77075(3) 0.81667(11) 0.62927(13) 0.0699(4) Uani 1 1 d . . . . .
I3 I 0.20799(4) 0.49718(10) 0.21224(11) 0.0711(3) Uani 1 1 d . . . . .
I9 I 0.67396(5) 0.50938(10) 0.87517(10) 0.0709(3) Uani 1 1 d . . . . .
I7 I 0.53971(3) 0.70395(16) 0.57179(14) 0.0819(4) Uani 1 1 d . . . . .
I8 I 0.64475(5) 0.99253(10) 0.86191(10) 0.0621(3) Uani 1 1 d . . . . .
I2 I 0.17667(5) 0.98714(11) 0.18662(12) 0.0753(4) Uani 1 1 d . . . . .
I11 I 0.89034(4) 0.96029(16) 0.45445(12) 0.0763(4) Uani 1 1 d . . . . .
I12 I 0.96070(4) 0.54684(14) 0.60437(14) 0.0779(4) Uani 1 1 d . . . . .
I4 I 0.30957(4) 0.79502(18) 0.49903(14) 0.0869(5) Uani 1 1 d . . . . .
I5 I 0.43648(5) 0.98879(13) 0.80117(12) 0.0975(4) Uani 1 1 d . . . . .
I6 I 0.41479(7) 0.47848(13) 0.75992(15) 0.1097(5) Uani 1 1 d . . . . .
N2 N 0.7368(3) 0.2114(14) 0.6475(14) 0.064(3) Uani 1 1 d D U . . .
H2A H 0.7124 0.2582 0.5923 0.077 Uiso 1 1 calc GR . . . .
H2B H 0.7368 0.2363 0.7451 0.077 Uiso 1 1 calc GR . . . .
H2C H 0.7327 0.1137 0.6374 0.077 Uiso 1 1 calc GR . . . .
C6 C 0.8922(5) 0.4984(13) 0.6963(14) 0.065(3) Uani 1 1 d D U . . .
H6A H 0.8997 0.4578 0.7979 0.078 Uiso 1 1 calc R . . . .
H6B H 0.8748 0.5912 0.7065 0.078 Uiso 1 1 calc R . . . .
C5 C 0.8586(3) 0.3941(13) 0.6072(12) 0.063(2) Uani 1 1 d D U . . .
H5A H 0.8752 0.3000 0.5964 0.076 Uiso 1 1 calc R . . . .
H5B H 0.8496 0.4343 0.5061 0.076 Uiso 1 1 calc R . . . .
C4 C 0.8133(3) 0.3697(13) 0.6851(13) 0.064(2) Uani 1 1 d D U . . .
H4A H 0.8219 0.3355 0.7888 0.077 Uiso 1 1 calc R . . . .
H4B H 0.7947 0.4612 0.6880 0.077 Uiso 1 1 calc R . . . .
C3 C 0.7839(3) 0.2543(12) 0.5941(14) 0.065(2) Uani 1 1 d D U . . .
H3A H 0.7775 0.2901 0.4902 0.078 Uiso 1 1 calc R . . . .
H3B H 0.8040 0.1657 0.5913 0.078 Uiso 1 1 calc R . . . .
C7 C 0.9647(4) 0.9496(9) 0.400(2) 0.068(3) Uani 1 1 d D U . . .
H7A H 0.9835 0.8798 0.4660 0.081 Uiso 1 1 calc R . . . .
H7B H 0.9657 0.9180 0.2948 0.081 Uiso 1 1 calc R . . . .
C8 C 0.9851(3) 1.1020(9) 0.4219(17) 0.0661(19) Uani 1 1 d D U . . .
H8A H 0.9826 1.1319 0.5265 0.079 Uiso 1 1 calc R . . . .
H8B H 0.9650 1.1697 0.3564 0.079 Uiso 1 1 calc R . . . .
C9 C 1.0376(3) 1.1180(11) 0.3891(18) 0.070(2) Uani 1 1 d D U . . .
H9A H 1.0574 1.0446 0.4480 0.084 Uiso 1 1 calc R . . . .
H9B H 1.0397 1.0972 0.2820 0.084 Uiso 1 1 calc R . . . .
N1 N 1.1072(3) 1.2879(13) 0.3694(14) 0.063(3) Uani 1 1 d D U . . .
H1A H 1.1052 1.3570 0.2968 0.076 Uiso 1 1 calc GR . . . .
H1B H 1.1169 1.2025 0.3317 0.076 Uiso 1 1 calc GR . . . .
H1C H 1.1288 1.3165 0.4463 0.076 Uiso 1 1 calc GR . . . .
C10 C 1.0582(3) 1.2677(11) 0.4252(19) 0.072(2) Uani 1 1 d D U . . .
H10A H 1.0612 1.2824 0.5347 0.086 Uiso 1 1 calc R . . . .
H10B H 1.0358 1.3423 0.3790 0.086 Uiso 1 1 calc R . . . .
N4 N 0.3380(4) 0.220(2) 0.507(3) 0.161(5) Uani 1 1 d D U . . .
H4C H 0.3553 0.2096 0.4275 0.193 Uiso 1 1 calc GR . . . .
H4D H 0.3420 0.1407 0.5664 0.193 Uiso 1 1 calc GR . . . .
H4E H 0.3482 0.3009 0.5592 0.193 Uiso 1 1 calc GR . . . .
N3 N 0.5491(9) 0.7009(15) 1.012(2) 0.18849(9) Uani 1 1 d D U . . .
H3C H 0.5589 0.6283 1.0771 0.226 Uiso 1 1 calc GR . . . .
H3D H 0.5730 0.7219 0.9546 0.226 Uiso 1 1 calc GR . . . .
H3E H 0.5225 0.6720 0.9534 0.226 Uiso 1 1 calc GR . . . .
C1 C 0.2856(4) 0.237(2) 0.451(3) 0.160(5) Uani 1 1 d D U . . .
H1D H 0.2804 0.2077 0.3460 0.240 Uiso 1 1 calc GR . . . .
H1E H 0.2759 0.3385 0.4610 0.240 Uiso 1 1 calc GR . . . .
H1F H 0.2663 0.1747 0.5104 0.240 Uiso 1 1 calc GR . . . .
C2 C 0.5376(10) 0.8346(15) 1.099(2) 0.18023(9) Uani 1 1 d D U . . .
H2D H 0.5221 0.8055 1.1871 0.270 Uiso 1 1 calc GR . . . .
H2E H 0.5158 0.8976 1.0355 0.270 Uiso 1 1 calc GR . . . .
H2F H 0.5673 0.8876 1.1306 0.270 Uiso 1 1 calc GR . . . .


_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 3.0634(10) . ?
Pb1 I3 3.1668(10) 2_565 ?
Pb1 I3 3.1952(10) . ?
Pb1 I2 3.1924(11) . ?
Pb1 I2 3.1749(11) 2_575 ?
Pb1 I4 3.2622(11) . ?
Pb2 I7 3.1434(14) . ?
Pb2 I4 3.1780(14) . ?
Pb2 I5 3.1746(13) 2_574 ?
Pb2 I5 3.1592(13) . ?
Pb2 I6 3.1867(14) 2_564 ?
Pb2 I6 3.1698(14) . ?
Pb3 I10 3.0490(10) . ?
Pb3 I9 3.1639(9) . ?
Pb3 I9 3.1904(10) 2_564 ?
Pb3 I7 3.3334(11) . ?
Pb3 I8 3.2019(9) 2_574 ?
Pb3 I8 3.1541(10) . ?
I3 Pb1 3.1668(10) 2_564 ?
I9 Pb3 3.1905(10) 2_565 ?
I8 Pb3 3.2019(9) 2_575 ?
I2 Pb1 3.1749(11) 2_574 ?
I11 C7 2.144(13) . ?
I12 C6 2.166(13) . ?
I5 Pb2 3.1747(13) 2_575 ?
I6 Pb2 3.1867(14) 2_565 ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C3 1.471(13) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.481(14) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 1.496(13) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.495(14) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.487(10) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.503(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.484(13) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C10 1.488(14) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
N4 H4C 0.8900 . ?
N4 H4D 0.8900 . ?
N4 H4E 0.8900 . ?
N4 C1 1.474(16) . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N3 H3E 0.8900 . ?
N3 C2 1.477(18) . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 H1F 0.9600 . ?
C2 H2D 0.9600 . ?
C2 H2E 0.9600 . ?
C2 H2F 0.9600 . ?

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 I3 87.32(3) . 2_565 ?
I1 Pb1 I3 93.06(3) . . ?
I1 Pb1 I2 94.06(3) . . ?
I1 Pb1 I2 88.97(3) . 2_575 ?
I1 Pb1 I4 173.45(3) . . ?
I3 Pb1 I3 87.790(11) 2_565 . ?
I3 Pb1 I2 94.89(3) 2_565 2_575 ?
I3 Pb1 I2 176.96(3) 2_565 . ?
I3 Pb1 I4 87.26(3) . . ?
I3 Pb1 I4 86.16(3) 2_565 . ?
I2 Pb1 I3 176.71(3) 2_575 . ?
I2 Pb1 I3 89.43(3) . . ?
I2 Pb1 I2 87.844(11) 2_575 . ?
I2 Pb1 I4 92.48(4) . . ?
I2 Pb1 I4 91.01(4) 2_575 . ?
I7 Pb2 I4 179.41(5) . . ?
I7 Pb2 I5 89.91(4) . 2_574 ?
I7 Pb2 I5 89.98(4) . . ?
I7 Pb2 I6 89.52(5) . . ?
I7 Pb2 I6 89.90(5) . 2_564 ?
I4 Pb2 I6 89.52(5) . 2_564 ?
I5 Pb2 I4 90.60(4) . . ?
I5 Pb2 I4 90.01(4) 2_574 . ?
I5 Pb2 I5 88.392(18) . 2_574 ?
I5 Pb2 I6 88.97(4) 2_574 2_564 ?
I5 Pb2 I6 94.33(4) . . ?
I5 Pb2 I6 177.36(4) . 2_564 ?
I6 Pb2 I4 90.53(5) . . ?
I6 Pb2 I5 177.22(4) . 2_574 ?
I6 Pb2 I6 88.305(18) . 2_564 ?
I10 Pb3 I9 93.80(3) . . ?
I10 Pb3 I9 89.85(3) . 2_564 ?
I10 Pb3 I7 174.65(3) . . ?
I10 Pb3 I8 87.56(3) . 2_574 ?
I10 Pb3 I8 92.56(3) . . ?
I9 Pb3 I9 87.998(11) . 2_564 ?
I9 Pb3 I7 90.68(3) 2_564 . ?
I9 Pb3 I7 91.54(3) . . ?
I9 Pb3 I8 176.54(3) . 2_574 ?
I9 Pb3 I8 95.19(2) 2_564 2_574 ?
I8 Pb3 I9 176.13(3) . 2_564 ?
I8 Pb3 I9 88.82(2) . . ?
I8 Pb3 I7 87.09(3) 2_574 . ?
I8 Pb3 I7 87.20(3) . . ?
I8 Pb3 I8 87.939(11) . 2_574 ?
Pb1 I3 Pb1 163.00(4) 2_564 . ?
Pb3 I9 Pb3 166.78(5) . 2_565 ?
Pb2 I7 Pb3 165.10(5) . . ?
Pb3 I8 Pb3 163.66(5) . 2_575 ?
Pb1 I2 Pb1 164.78(5) 2_574 . ?
Pb2 I4 Pb1 165.45(6) . . ?
Pb2 I5 Pb2 167.92(6) . 2_575 ?
Pb2 I6 Pb2 165.37(6) . 2_565 ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C3 N2 H2A 109.5 . . ?
C3 N2 H2B 109.5 . . ?
C3 N2 H2C 109.5 . . ?
I12 C6 H6A 108.2 . . ?
I12 C6 H6B 108.2 . . ?
H6A C6 H6B 107.4 . . ?
C5 C6 I12 116.3(8) . . ?
C5 C6 H6A 108.2 . . ?
C5 C6 H6B 108.2 . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
C6 C5 C4 110.3(10) . . ?
H5A C5 H5B 108.1 . . ?
C4 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
C5 C4 H4A 110.5 . . ?
C5 C4 H4B 110.5 . . ?
H4A C4 H4B 108.7 . . ?
C3 C4 C5 106.3(9) . . ?
C3 C4 H4A 110.5 . . ?
C3 C4 H4B 110.5 . . ?
N2 C3 C4 116.8(10) . . ?
N2 C3 H3A 108.1 . . ?
N2 C3 H3B 108.1 . . ?
C4 C3 H3A 108.1 . . ?
C4 C3 H3B 108.1 . . ?
H3A C3 H3B 107.3 . . ?
I11 C7 H7A 110.5 . . ?
I11 C7 H7B 110.5 . . ?
H7A C7 H7B 108.7 . . ?
C8 C7 I11 106.3(7) . . ?
C8 C7 H7A 110.5 . . ?
C8 C7 H7B 110.5 . . ?
C7 C8 H8A 108.6 . . ?
C7 C8 H8B 108.6 . . ?
C7 C8 C9 114.6(9) . . ?
H8A C8 H8B 107.6 . . ?
C9 C8 H8A 108.6 . . ?
C9 C8 H8B 108.6 . . ?
C8 C9 H9A 108.9 . . ?
C8 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C10 C9 C8 113.3(9) . . ?
C10 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C10 N1 H1A 109.5 . . ?
C10 N1 H1B 109.5 . . ?
C10 N1 H1C 109.5 . . ?
C9 C10 N1 112.1(10) . . ?
C9 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
N1 C10 H10A 109.2 . . ?
N1 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
H4C N4 H4D 109.5 . . ?
H4C N4 H4E 109.5 . . ?
H4D N4 H4E 109.5 . . ?
C1 N4 H4C 109.5 . . ?
C1 N4 H4D 109.5 . . ?
C1 N4 H4E 109.5 . . ?
H3C N3 H3D 109.5 . . ?
H3C N3 H3E 109.5 . . ?
H3D N3 H3E 109.5 . . ?
C2 N3 H3C 109.5 . . ?
C2 N3 H3D 109.5 . . ?
C2 N3 H3E 109.5 . . ?
N4 C1 H1D 109.5 . . ?
N4 C1 H1E 109.5 . . ?
N4 C1 H1F 109.5 . . ?
H1D C1 H1E 109.5 . . ?
H1D C1 H1F 109.5 . . ?
H1E C1 H1F 109.5 . . ?
N3 C2 H2D 109.5 . . ?
N3 C2 H2E 109.5 . . ?
N3 C2 H2F 109.5 . . ?
H2D C2 H2E 109.5 . . ?
H2D C2 H2F 109.5 . . ?
H2E C2 H2F 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.512(10)
2 0.488(10)

