# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2063222'
loop_
_audit_author_name
_audit_author_address
wangdi
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2021-02-16 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
_audit_creation_date             2020-10-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I10 Pb3, 2(C8 H14 N2), 4(C3 H7 N O)'
_chemical_formula_sum            'C28 H56 I10 N8 O4 Pb3'
_chemical_formula_weight         2459.37
_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'
O O 0.0106 0.0060 '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                   11.1291(7)
_cell_length_b                   11.7689(6)
_cell_length_c                   13.0217(8)
_cell_angle_alpha                68.354(2)
_cell_angle_beta                 70.907(2)
_cell_angle_gamma                74.918(2)
_cell_volume                     1479.04(15)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9766
_cell_measurement_temperature    289.99
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.50
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.769
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1398 before and 0.0799 after correction.
The Ratio of minimum to maximum transmission is 0.4186.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.761
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_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  0.0656
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            60023
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.611
_diffrn_reflns_theta_min         2.496
_diffrn_ambient_temperature      289.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_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_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6075
_reflns_number_total             6805
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.162
_refine_diff_density_min         -2.637
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.00409(11)
_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   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         6805
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0268
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0156P)²+4.4818P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0612
_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.a Secondary CH2 refined with riding coordinates:
 C00I(H00H,H00I), C00K(H00J,H00K)
2.b Aromatic/amide H refined with riding coordinates:
 C00E(H00G), C00O(H00P), C00M(H00O), C00L(H00L), C00H(H00M), C00G(H00N)
2.c Idealised Me refined as rotating group:
 N008(H00A,H00B,H00C), N00A(H00D,H00E,H00F), C00N(H00Q,H00R,H00S), C1(H1A,H1B,
 H1C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.60036(2) 0.31487(2) -0.02619(2) 0.03643(7) Uani 1 1 d . . . . .
Pb02 Pb 0.500000 0.000000 0.000000 0.03864(8) Uani 1 2 d S . P . .
I003 I 0.50443(3) 0.41529(3) 0.19155(3) 0.04121(9) Uani 1 1 d . . . . .
I004 I 0.30939(3) 0.23811(3) 0.05554(3) 0.04223(9) Uani 1 1 d . . . . .
I005 I 0.64170(4) 0.20191(3) -0.22874(3) 0.04647(10) Uani 1 1 d . . . . .
I006 I 0.68710(4) 0.03996(3) 0.12184(3) 0.04895(10) Uani 1 1 d . . . . .
I007 I 0.87304(4) 0.39092(4) -0.08757(4) 0.06111(13) Uani 1 1 d . . . . .
N008 N 0.1756(4) 0.3222(4) 0.3154(4) 0.0428(10) Uani 1 1 d . . . . .
H00A H 0.135843 0.315693 0.269025 0.051 Uiso 1 1 calc R U . . .
H00B H 0.213425 0.247534 0.350012 0.051 Uiso 1 1 calc R U . . .
H00C H 0.234796 0.371285 0.274821 0.051 Uiso 1 1 calc R U . . .
O009 O 0.2680(4) 0.0927(4) 0.4338(4) 0.0609(11) Uani 1 1 d . . . . .
O00B O 0.0587(4) 0.7114(4) 0.7342(4) 0.0553(10) Uani 1 1 d . . . . .
N00A N 0.1951(5) 0.4787(5) 0.8158(4) 0.0485(11) Uani 1 1 d . . . . .
H00D H 0.160932 0.554792 0.780400 0.058 Uiso 1 1 calc R U . . .
H00E H 0.229646 0.481544 0.867317 0.058 Uiso 1 1 calc R U . . .
H00F H 0.133949 0.431047 0.850553 0.058 Uiso 1 1 calc R U . . .
N00C N 0.4013(4) -0.0882(4) 0.4793(4) 0.0466(11) Uani 1 1 d . . . . .
N00D N -0.0011(4) 0.8982(5) 0.7641(4) 0.0460(11) Uani 1 1 d . . . . .
C00E C 0.1242(6) 0.3046(5) 0.5946(5) 0.0449(13) Uani 1 1 d . . . . .
H00G H 0.078277 0.240356 0.615603 0.054 Uiso 1 1 calc R U . . .
C00O C 0.0426(6) 0.7798(6) 0.7925(5) 0.0500(14) Uani 1 1 d . . . . .
H00P H 0.063475 0.743417 0.862333 0.060 Uiso 1 1 calc R U . . .
C00M C 0.3654(6) 0.0187(6) 0.4094(5) 0.0528(14) Uani 1 1 d . . . . .
H00O H 0.417539 0.040927 0.335211 0.063 Uiso 1 1 calc R U . . .
C00J C 0.2423(5) 0.4125(5) 0.6447(5) 0.0454(13) Uani 1 1 d . . . . .
C00I C 0.2969(6) 0.4261(8) 0.7303(6) 0.067(2) Uani 1 1 d . . . . .
H00H H 0.338369 0.345744 0.769725 0.081 Uiso 1 1 calc R U . . .
H00I H 0.361754 0.479910 0.690517 0.081 Uiso 1 1 calc R U . . .
C00N C -0.0376(8) 0.9633(7) 0.6581(6) 0.073(2) Uani 1 1 d . . . . .
H00Q H -0.009347 0.910576 0.610550 0.110 Uiso 1 1 calc R U . . .
H00R H 0.001900 1.036510 0.619402 0.110 Uiso 1 1 calc R U . . .
H00S H -0.129525 0.986052 0.673830 0.110 Uiso 1 1 calc R U . . .
C00L C 0.1760(6) 0.3162(5) 0.6736(5) 0.0492(14) Uani 1 1 d . . . . .
H00L H 0.165906 0.258606 0.746296 0.059 Uiso 1 1 calc R U . . .
C00F C 0.1403(5) 0.3874(5) 0.4856(4) 0.0374(11) Uani 1 1 d . . . . .
C00K C 0.0803(6) 0.3756(6) 0.4023(5) 0.0490(14) Uani 1 1 d . . . . .
H00J H 0.014177 0.323410 0.444186 0.059 Uiso 1 1 calc R U . . .
H00K H 0.039179 0.456746 0.364046 0.059 Uiso 1 1 calc R U . . .
C00H C 0.2591(6) 0.4953(6) 0.5338(5) 0.0515(14) Uani 1 1 d . . . . .
H00M H 0.304807 0.559874 0.512046 0.062 Uiso 1 1 calc R U . . .
C00G C 0.2081(6) 0.4819(5) 0.4560(5) 0.0474(13) Uani 1 1 d . . . . .
H00N H 0.219921 0.537785 0.382418 0.057 Uiso 1 1 calc R U . . .
C1 C -0.0241(7) 0.9683(7) 0.8435(7) 0.071(2) Uani 1 1 d . . . . .
H1A H -0.114852 0.995742 0.868137 0.107 Uiso 1 1 calc R U . . .
H1B H 0.019830 1.038710 0.805611 0.107 Uiso 1 1 calc R U . . .
H1C H 0.007637 0.916086 0.908748 0.107 Uiso 1 1 calc R U . . .
C3 C 0.5161(7) -0.1734(7) 0.4464(6) 0.0674(19) Uani 1 1 d . . . . .
H3A H 0.491611 -0.247685 0.450568 0.101 Uiso 1 1 calc R U . . .
H3B H 0.569689 -0.193327 0.497319 0.101 Uiso 1 1 calc R U . . .
H3C H 0.562730 -0.135302 0.369588 0.101 Uiso 1 1 calc R U . . .
C2 C 0.3239(11) -0.1279(10) 0.5933(8) 0.149(6) Uani 1 1 d . . . . .
H2A H 0.261761 -0.059165 0.610174 0.223 Uiso 1 1 calc R U . . .
H2B H 0.377632 -0.159135 0.645465 0.223 Uiso 1 1 calc R U . . .
H2C H 0.280125 -0.192072 0.601036 0.223 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
Pb01 I003 3.2791(4) 2_665 ?
Pb01 I003 3.2266(4) . ?
Pb01 I004 3.3156(4) . ?
Pb01 I005 3.2265(4) . ?
Pb01 I006 3.1790(4) . ?
Pb01 I007 3.1540(5) . ?
Pb02 I004 3.2053(4) 2_655 ?
Pb02 I004 3.2053(4) . ?
Pb02 I005 3.2651(4) . ?
Pb02 I005 3.2651(4) 2_655 ?
Pb02 I006 3.2087(4) 2_655 ?
Pb02 I006 3.2086(4) . ?
N008 H00A 0.8900 . ?
N008 H00B 0.8900 . ?
N008 H00C 0.8900 . ?
N008 C00K 1.481(7) . ?
O009 C00M 1.233(7) . ?
O00B C00O 1.241(7) . ?
N00A H00D 0.8900 . ?
N00A H00E 0.8900 . ?
N00A H00F 0.8900 . ?
N00A C00I 1.491(7) . ?
N00C C00M 1.305(7) . ?
N00C C3 1.453(7) . ?
N00C C2 1.422(9) . ?
N00D C00O 1.304(8) . ?
N00D C00N 1.443(8) . ?
N00D C1 1.470(8) . ?
C00E H00G 0.9300 . ?
C00E C00L 1.393(8) . ?
C00E C00F 1.378(7) . ?
C00O H00P 0.9300 . ?
C00M H00O 0.9300 . ?
C00J C00I 1.505(8) . ?
C00J C00L 1.383(8) . ?
C00J C00H 1.397(8) . ?
C00I H00H 0.9700 . ?
C00I H00I 0.9700 . ?
C00N H00Q 0.9600 . ?
C00N H00R 0.9600 . ?
C00N H00S 0.9600 . ?
C00L H00L 0.9300 . ?
C00F C00K 1.508(7) . ?
C00F C00G 1.373(8) . ?
C00K H00J 0.9700 . ?
C00K H00K 0.9700 . ?
C00H H00M 0.9300 . ?
C00H C00G 1.384(8) . ?
C00G H00N 0.9300 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 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
I003 Pb01 I003 91.596(11) . 2_665 ?
I003 Pb01 I004 89.718(11) 2_665 . ?
I003 Pb01 I004 85.676(10) . . ?
I005 Pb01 I003 169.088(12) . . ?
I005 Pb01 I003 88.088(11) . 2_665 ?
I005 Pb01 I004 83.415(11) . . ?
I006 Pb01 I003 173.581(11) . 2_665 ?
I006 Pb01 I003 92.877(11) . . ?
I006 Pb01 I004 86.033(11) . . ?
I006 Pb01 I005 86.648(12) . . ?
I007 Pb01 I003 91.216(11) . 2_665 ?
I007 Pb01 I003 90.464(13) . . ?
I007 Pb01 I004 176.052(13) . . ?
I007 Pb01 I005 100.448(13) . . ?
I007 Pb01 I006 93.348(12) . . ?
I004 Pb02 I004 180.0 . 2_655 ?
I004 Pb02 I005 84.559(10) . . ?
I004 Pb02 I005 95.441(10) 2_655 . ?
I004 Pb02 I005 84.559(10) 2_655 2_655 ?
I004 Pb02 I005 95.442(10) . 2_655 ?
I004 Pb02 I006 87.414(10) 2_655 2_655 ?
I004 Pb02 I006 87.414(10) . . ?
I004 Pb02 I006 92.586(10) 2_655 . ?
I004 Pb02 I006 92.586(10) . 2_655 ?
I005 Pb02 I005 180.0 2_655 . ?
I006 Pb02 I005 85.513(11) . . ?
I006 Pb02 I005 85.511(11) 2_655 2_655 ?
I006 Pb02 I005 94.488(11) . 2_655 ?
I006 Pb02 I005 94.488(11) 2_655 . ?
I006 Pb02 I006 180.0 . 2_655 ?
Pb01 I003 Pb01 88.404(11) . 2_665 ?
Pb02 I004 Pb01 75.841(9) . . ?
Pb01 I005 Pb02 76.263(9) . . ?
Pb01 I006 Pb02 77.736(9) . . ?
H00A N008 H00B 109.5 . . ?
H00A N008 H00C 109.5 . . ?
H00B N008 H00C 109.5 . . ?
C00K N008 H00A 109.5 . . ?
C00K N008 H00B 109.5 . . ?
C00K N008 H00C 109.5 . . ?
H00D N00A H00E 109.5 . . ?
H00D N00A H00F 109.5 . . ?
H00E N00A H00F 109.5 . . ?
C00I N00A H00D 109.5 . . ?
C00I N00A H00E 109.5 . . ?
C00I N00A H00F 109.5 . . ?
C00M N00C C3 123.5(5) . . ?
C00M N00C C2 119.7(6) . . ?
C2 N00C C3 116.9(6) . . ?
C00O N00D C00N 121.6(6) . . ?
C00O N00D C1 120.8(5) . . ?
C00N N00D C1 117.5(6) . . ?
C00L C00E H00G 119.6 . . ?
C00F C00E H00G 119.6 . . ?
C00F C00E C00L 120.7(5) . . ?
O00B C00O N00D 125.7(6) . . ?
O00B C00O H00P 117.2 . . ?
N00D C00O H00P 117.2 . . ?
O009 C00M N00C 125.4(6) . . ?
O009 C00M H00O 117.3 . . ?
N00C C00M H00O 117.3 . . ?
C00L C00J C00I 120.6(6) . . ?
C00L C00J C00H 118.4(5) . . ?
C00H C00J C00I 121.0(6) . . ?
N00A C00I C00J 111.7(5) . . ?
N00A C00I H00H 109.3 . . ?
N00A C00I H00I 109.3 . . ?
C00J C00I H00H 109.3 . . ?
C00J C00I H00I 109.3 . . ?
H00H C00I H00I 107.9 . . ?
N00D C00N H00Q 109.5 . . ?
N00D C00N H00R 109.5 . . ?
N00D C00N H00S 109.5 . . ?
H00Q C00N H00R 109.5 . . ?
H00Q C00N H00S 109.5 . . ?
H00R C00N H00S 109.5 . . ?
C00E C00L H00L 119.7 . . ?
C00J C00L C00E 120.5(5) . . ?
C00J C00L H00L 119.7 . . ?
C00E C00F C00K 120.0(5) . . ?
C00G C00F C00E 118.9(5) . . ?
C00G C00F C00K 121.1(5) . . ?
N008 C00K C00F 112.6(4) . . ?
N008 C00K H00J 109.1 . . ?
N008 C00K H00K 109.1 . . ?
C00F C00K H00J 109.1 . . ?
C00F C00K H00K 109.1 . . ?
H00J C00K H00K 107.8 . . ?
C00J C00H H00M 119.8 . . ?
C00G C00H C00J 120.4(5) . . ?
C00G C00H H00M 119.8 . . ?
C00F C00G C00H 121.1(5) . . ?
C00F C00G H00N 119.5 . . ?
C00H C00G H00N 119.5 . . ?
N00D C1 H1A 109.5 . . ?
N00D C1 H1B 109.5 . . ?
N00D C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N00C C3 H3A 109.5 . . ?
N00C C3 H3B 109.5 . . ?
N00C C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N00C C2 H2A 109.5 . . ?
N00C C2 H2B 109.5 . . ?
N00C C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 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
C00E C00F C00K N008 -104.1(6) . . . . ?
C00E C00F C00G C00H -0.5(8) . . . . ?
C00J C00H C00G C00F -0.1(9) . . . . ?
C00I C00J C00L C00E 179.2(5) . . . . ?
C00I C00J C00H C00G -179.8(5) . . . . ?
C00N N00D C00O O00B 0.6(10) . . . . ?
C00L C00E C00F C00K -178.2(5) . . . . ?
C00L C00E C00F C00G -0.2(8) . . . . ?
C00L C00J C00I N00A -77.0(7) . . . . ?
C00L C00J C00H C00G 1.2(8) . . . . ?
C00F C00E C00L C00J 1.3(9) . . . . ?
C00K C00F C00G C00H 177.6(5) . . . . ?
C00H C00J C00I N00A 104.1(7) . . . . ?
C00H C00J C00L C00E -1.8(8) . . . . ?
C00G C00F C00K N008 77.9(6) . . . . ?
C1 N00D C00O O00B 176.0(6) . . . . ?
C3 N00C C00M O009 179.1(7) . . . . ?
C2 N00C C00M O009 1.2(12) . . . . ?

_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_2fabs
_database_code_depnum_ccdc_archive 'CCDC 2063260'
loop_
_audit_author_name
_audit_author_address
'wang di'
;ShanghaiTech University
China
;
_audit_update_record             
;
2021-02-16 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
_audit_creation_date             2021-02-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, C8 H10 F4 N2'
_chemical_formula_sum            'C8 H10 F4 I4 N2 Pb'
_chemical_formula_weight         924.97
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32  N8  F16  I16  Pb4  H1  '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 '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                   13.0472(4)
_cell_length_b                   8.5023(3)
_cell_length_c                   8.4976(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.989(3)
_cell_angle_gamma                90
_cell_volume                     933.50(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5383
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      74.8490
_cell_measurement_theta_min      3.3670
_shelx_estimated_absorpt_T_max   0.229
_shelx_estimated_absorpt_T_min   0.167
_exptl_absorpt_coefficient_mu    69.773
_exptl_absorpt_correction_T_max  0.03322
_exptl_absorpt_correction_T_min  0.00092
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.65a (Rigaku Oxford Diffraction, 2020)
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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.291
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_size_rad          0.400
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.768
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5772
_diffrn_reflns_point_group_measured_fraction_full 0.768
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         6.231
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3468
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.768
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -17.00   1.00    1.00    --  -41.41 -38.00 -30.00   99
  2  ω    -66.00  33.00   1.00    1.00    --  -41.41  38.00 -30.00   99
  3  ω     27.00  97.00   1.00    1.00    --   41.41-125.00-180.00   70
  4  ω     35.00 134.00   1.00    1.00    --  108.23 -45.00 120.00   99
  5  ω     80.00 178.00   1.00    1.00    --  108.23  30.00 -60.00   98
  6  ω     53.00 144.00   1.00    1.00    --  108.23-170.00 135.00   91
  7  ω     32.00 109.00   1.00    1.00    --  108.23-111.00 -30.00   77
  8  ω     82.00 178.00   1.00    1.00    --  108.23  45.00-150.00   96
  9  ω     26.00 106.00   1.00    1.00    --  108.23 -94.00 150.00   80
 10  ω   -114.00 -13.00   1.00    1.00    --  -41.41 -57.00  90.00  101
 11  ω   -114.00 -13.00   1.00    1.00    --  -41.41 -57.00-180.00  101
 12  ω   -114.00 -13.00   1.00    1.00    --  -41.41 -57.00 -90.00  101
 13  ω     35.00  60.00   1.00    1.00    --  108.23 -45.00 -30.00   25
 14  ω     56.00 178.00   1.00    1.00    --  108.23  15.00  60.00  122
 15  ω     79.00 178.00   1.00    1.00    --  108.23  61.00 120.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0934704000
_diffrn_orient_matrix_UB_12      0.0337500000
_diffrn_orient_matrix_UB_13      -0.0872787000
_diffrn_orient_matrix_UB_21      -0.0713093000
_diffrn_orient_matrix_UB_22      -0.0049240000
_diffrn_orient_matrix_UB_23      -0.1605060000
_diffrn_orient_matrix_UB_31      -0.0199279000
_diffrn_orient_matrix_UB_32      0.1779094000
_diffrn_orient_matrix_UB_33      0.0122315000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1509
_reflns_number_total             1584
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.65a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.65a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.65a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.883
_refine_diff_density_min         -2.368
_refine_diff_density_rms         0.385
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1584
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0627
_refine_ls_restrained_S_all      1.084
_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)+(0.1297P)²+1.2057P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1702
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C009(H00D,H00E)
2.b Idealised Me refined as rotating group:
 N006(H00A,H00B,H00C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.000000 1.000000 1.000000 0.0401(3) Uani 1 2 d S . P . .
I002 I 0.03814(5) 1.18111(9) 0.68914(8) 0.0433(3) Uani 1 1 d . . . . .
I003 I 0.24449(5) 0.93931(10) 1.06377(9) 0.0454(4) Uani 1 1 d . . . . .
F004 F 0.6217(6) 0.7805(10) 0.6601(9) 0.0522(17) Uani 1 1 d . . . . .
F005 F 0.4364(5) 0.8381(10) 0.7456(9) 0.0510(16) Uani 1 1 d . . . . .
N006 N 0.2151(7) 0.9704(14) 0.4790(14) 0.047(2) Uani 1 1 d . . . . .
H00A H 0.229121 0.976570 0.377165 0.057 Uiso 1 1 calc R U . . .
H00B H 0.151290 1.011383 0.484506 0.057 Uiso 1 1 calc R U . . .
H00C H 0.216594 0.867992 0.510198 0.057 Uiso 1 1 calc R U . . .
C007 C 0.5614(9) 0.8898(15) 0.5807(15) 0.044(3) Uani 1 1 d . . . . .
C008 C 0.4006(9) 1.0269(16) 0.5431(15) 0.044(2) Uani 1 1 d . . . . .
C009 C 0.2946(9) 1.0614(17) 0.5857(16) 0.048(3) Uani 1 1 d . . . . .
H00D H 0.291931 1.031748 0.697740 0.058 Uiso 1 1 calc R U . . .
H00E H 0.279947 1.175349 0.574121 0.058 Uiso 1 1 calc R U . . .
C00A C 0.4654(9) 0.9177(16) 0.6221(16) 0.045(3) 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
Pb01 I002 3.1559(7) 4_586 ?
Pb01 I002 3.1563(7) . ?
Pb01 I002 3.1559(7) 2_546 ?
Pb01 I002 3.1563(7) 3_577 ?
Pb01 I003 3.2024(7) . ?
Pb01 I003 3.2024(7) 3_577 ?
F004 C007 1.337(15) . ?
F005 C00A 1.346(15) . ?
N006 H00A 0.9100 . ?
N006 H00B 0.9100 . ?
N006 H00C 0.9100 . ?
N006 C009 1.495(16) . ?
C007 C008 1.414(19) 3_676 ?
C007 C00A 1.369(17) . ?
C008 C009 1.506(17) . ?
C008 C00A 1.367(19) . ?
C009 H00D 0.9900 . ?
C009 H00E 0.9900 . ?

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
I002 Pb01 I002 180.0 4_586 2_546 ?
I002 Pb01 I002 88.570(8) 4_586 . ?
I002 Pb01 I002 91.430(8) 2_546 . ?
I002 Pb01 I002 88.570(8) 2_546 3_577 ?
I002 Pb01 I002 91.430(8) 4_586 3_577 ?
I002 Pb01 I002 180.0 3_577 . ?
I002 Pb01 I003 91.753(19) 4_586 3_577 ?
I002 Pb01 I003 92.807(18) 3_577 . ?
I002 Pb01 I003 88.247(19) 4_586 . ?
I002 Pb01 I003 87.193(18) . . ?
I002 Pb01 I003 92.807(18) . 3_577 ?
I002 Pb01 I003 88.247(19) 2_546 3_577 ?
I002 Pb01 I003 91.753(19) 2_546 . ?
I002 Pb01 I003 87.193(18) 3_577 3_577 ?
I003 Pb01 I003 180.0 . 3_577 ?
Pb01 I002 Pb01 144.42(2) 2_556 . ?
H00A N006 H00B 109.5 . . ?
H00A N006 H00C 109.5 . . ?
H00B N006 H00C 109.5 . . ?
C009 N006 H00A 109.5 . . ?
C009 N006 H00B 109.5 . . ?
C009 N006 H00C 109.5 . . ?
F004 C007 C008 118.8(11) . 3_676 ?
F004 C007 C00A 119.1(12) . . ?
C00A C007 C008 122.2(12) . 3_676 ?
C007 C008 C009 120.6(12) 3_676 . ?
C00A C008 C007 116.7(11) . 3_676 ?
C00A C008 C009 122.7(12) . . ?
N006 C009 C008 109.6(11) . . ?
N006 C009 H00D 109.7 . . ?
N006 C009 H00E 109.7 . . ?
C008 C009 H00D 109.7 . . ?
C008 C009 H00E 109.7 . . ?
H00D C009 H00E 108.2 . . ?
F005 C00A C007 118.6(11) . . ?
F005 C00A C008 120.2(11) . . ?
C008 C00A C007 121.2(12) . . ?

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
F004 C007 C00A F005 2.4(17) . . . . ?
F004 C007 C00A C008 -179.2(11) . . . . ?
C007 C008 C009 N006 84.5(15) 3_676 . . . ?
C007 C008 C00A F005 177.3(11) 3_676 . . . ?
C007 C008 C00A C007 -1(2) 3_676 . . . ?
C008 C007 C00A F005 -177.3(11) 3_676 . . . ?
C008 C007 C00A C008 1(2) 3_676 . . . ?
C009 C008 C00A F005 -1.4(19) . . . . ?
C009 C008 C00A C007 -179.7(12) . . . . ?
C00A C008 C009 N006 -96.9(14) . . . . ?

_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 2.812
_oxdiff_exptl_absorpt_empirical_full_min 0.501
