# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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_yuyi_1_0ma
_database_code_depnum_ccdc_archive 'CCDC 2051854'
loop_
_audit_author_name
_audit_author_address
'Yiwei Zhang'
;Beijing University of Technology
China
;
_audit_update_record             
;
2020-12-22 deposited with the CCDC.	2021-01-25 downloaded from the CCDC.
;
_audit_creation_date             2020-09-27
_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         'I4 Pb, 0.5(C8 H24 N4)'
_chemical_formula_sum            'C4 H12 I4 N2 Pb'
_chemical_formula_weight         802.95
_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      orthorhombic
_space_group_IT_number           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   15.295(15)
_cell_length_b                   6.482(6)
_cell_length_c                   15.084(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1496(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1898
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.66
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.501
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1317 before and 0.0550 after correction.
The Ratio of minimum to maximum transmission is 0.2283.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_colour_primary    .
_exptl_crystal_density_diffrn    3.566
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3436
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.439
_diffrn_reflns_theta_min         1.896
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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           30.0
_diffrn_source_power             1.5
_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                801
_reflns_number_total             871
_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 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 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.495
_refine_diff_density_min         -8.180
_refine_diff_density_rms         1.313
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         871
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0727
_refine_ls_restrained_S_all      1.143
_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)+(0.1324P)²+27.1219P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1890
_refine_ls_wR_factor_ref         0.1926
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C006) = Uanis(N005) = Uanis(C1)
3. Others
 Fixed Sof: H00A(0.5) H00B(0.5) H1A(0.5) H1B(0.5) H1C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C006(H00A,H00B)
4.b Aromatic/amide H refined with riding coordinates:
 N005(H005)
4.c Idealised Me refined as rotating group:
 C1(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
Pb01 Pb 0.500000 0.750000 0.38276(6) 0.0317(4) Uani 1 4 d S T P . .
I002 I 0.500000 0.250000 0.38918(11) 0.0389(6) Uani 1 4 d S T P . .
I003 I 0.70562(11) 0.750000 0.39551(10) 0.0465(5) Uani 1 2 d S T P . .
I004 I 0.500000 0.750000 0.18041(13) 0.0501(6) Uani 1 4 d S T P . .
N005 N 0.7843(15) 0.250000 0.3675(14) 0.049(3) Uani 1 2 d S T P . .
H005 H 0.734099 0.250000 0.393128 0.059 Uiso 1 2 calc R U P . .
C006 C 0.7957(15) 0.250000 0.2751(15) 0.049(3) Uani 1 2 d S T P . .
H00A H 0.828893 0.128945 0.257846 0.059 Uiso 0.5 1 calc R U P . .
H00B H 0.828894 0.371055 0.257846 0.059 Uiso 0.5 1 calc R U P . .
C1 C 0.8718(16) 0.250000 0.4177(16) 0.049(3) Uani 1 2 d S T P . .
H1A H 0.905017 0.130202 0.401263 0.074 Uiso 0.5 1 calc R U P A -1
H1B H 0.860951 0.247787 0.480327 0.074 Uiso 0.5 1 calc R U P A -1
H1C H 0.904218 0.372011 0.402698 0.074 Uiso 0.5 1 calc R U P A -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
Pb01 0.0359(6) 0.0365(7) 0.0229(6) 0.000 0.000 0.000
I002 0.0552(13) 0.0336(10) 0.0280(9) 0.000 0.000 0.000
I003 0.0405(9) 0.0498(9) 0.0492(9) 0.000 -0.0041(6) 0.000
I004 0.0662(14) 0.0591(13) 0.0250(10) 0.000 0.000 0.000
N005 0.048(7) 0.057(7) 0.043(8) 0.000 0.008(6) 0.000
C006 0.048(7) 0.057(7) 0.043(8) 0.000 0.008(6) 0.000
C1 0.048(7) 0.057(7) 0.043(8) 0.000 0.008(6) 0.000

_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 3.243(3) . ?
Pb01 I002 3.243(3) 1_565 ?
Pb01 I003 3.151(3) . ?
Pb01 I003 3.151(3) 2_665 ?
Pb01 I004 3.052(4) . ?
N005 H005 0.8600 . ?
N005 C006 1.40(3) . ?
N005 C1 1.54(3) . ?
C006 C006 1.59(5) 13_655 ?
C006 H00A 0.9700 . ?
C006 H00B 0.9700 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 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
I002 Pb01 I002 176.58(7) 1_565 . ?
I003 Pb01 I002 89.896(2) . . ?
I003 Pb01 I002 89.896(2) 2_665 1_565 ?
I003 Pb01 I002 89.896(2) 2_665 . ?
I003 Pb01 I002 89.896(2) . 1_565 ?
I003 Pb01 I003 173.00(7) 2_665 . ?
I004 Pb01 I002 91.71(3) . . ?
I004 Pb01 I002 91.71(3) . 1_565 ?
I004 Pb01 I003 93.50(3) . 2_665 ?
I004 Pb01 I003 93.50(3) . . ?
Pb01 I002 Pb01 176.58(7) . 1_545 ?
C006 N005 H005 123.8 . . ?
C006 N005 C1 112.3(19) . . ?
C1 N005 H005 123.8 . . ?
N005 C006 C006 111(2) . 13_655 ?
N005 C006 H00A 109.4 . . ?
N005 C006 H00B 109.4 . . ?
C006 C006 H00A 109.4 13_655 . ?
C006 C006 H00B 109.4 13_655 . ?
H00A C006 H00B 108.0 . . ?
N005 C1 H1A 109.5 . . ?
N005 C1 H1B 109.5 . . ?
N005 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 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
C1 N005 C006 C006 180.000(2) . . . 13_655 ?

_shelx_res_file                  
;
TITL yuyi_1_0ma_a.res in Imma
    yuyi_1_0ma.res
    created by SHELXL-2018/3 at 10:36:38 on 27-Sep-2020
REM Old TITL YUYI_1_0ma in Imma
REM SHELXT solution in Imma: R1 0.141, Rweak 0.009, Alpha 0.035
REM <I/s> 1.583 for 30 systematic absences, Orientation as input
REM Formula found by SHELXT: C4 I4 Pb
CELL 0.71073 15.2948 6.4823 15.0845 90 90 90
ZERR 4 0.015 0.0064 0.015 0 0 0
LATT 2
SYMM -X,0.5-Y,+Z
SYMM -X,0.5+Y,-Z
SYMM +X,-Y,-Z
SFAC C H I N Pb
UNIT 16 48 16 8 4
EADP C006 N005 C1

L.S. 100
PLAN  4 0 0
TEMP 23
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\YUYI_1_0ma.hkl">
REM </olex2.extras>

WGHT    0.132400   27.121901
FVAR       0.12563
PB01  5    0.500000    0.750000    0.382765    10.25000    0.03588    0.03645 =
         0.02291    0.00000    0.00000    0.00000
I002  3    0.500000    0.250000    0.389175    10.25000    0.05515    0.03360 =
         0.02796    0.00000    0.00000    0.00000
I003  3    0.705619    0.750000    0.395511    10.50000    0.04055    0.04985 =
         0.04923    0.00000   -0.00408    0.00000
I004  3    0.500000    0.750000    0.180407    10.25000    0.06622    0.05909 =
         0.02504    0.00000    0.00000    0.00000
N005  4    0.784333    0.250000    0.367514    10.50000    0.04767    0.05687 =
         0.04339    0.00000    0.00788    0.00000
AFIX  43
H005  2    0.734099    0.250000    0.393128    10.50000   -1.20000
AFIX   0
C006  1    0.795738    0.250000    0.275128    10.50000    0.04767    0.05687 =
         0.04339    0.00000    0.00788    0.00000
AFIX  23
H00A  2    0.828893    0.128945    0.257846    10.50000   -1.20000
H00B  2    0.828894    0.371055    0.257846    10.50000   -1.20000
AFIX   0
C1    1    0.871847    0.250000    0.417659    10.50000    0.04767    0.05687 =
         0.04339    0.00000    0.00788    0.00000
PART -1
AFIX 137
H1A   2    0.905017    0.130202    0.401263    10.50000   -1.50000
H1B   2    0.860951    0.247787    0.480327    10.50000   -1.50000
H1C   2    0.904218    0.372011    0.402698    10.50000   -1.50000
AFIX   0
HKLF 4




REM  yuyi_1_0ma_a.res in Imma
REM wR2 = 0.1926, GooF = S = 1.143, Restrained GooF = 1.143 for all data
REM R1 = 0.0727 for 801 Fo > 4sig(Fo) and 0.0756 for all 871 data
REM 30 parameters refined using 0 restraints

END

WGHT      0.1325     27.3097

REM Highest difference peak  3.495,  deepest hole -8.180,  1-sigma level  1.313
Q1    1   0.5000  0.8991  0.3527  10.50000  0.05    3.49
Q2    1   0.5000  0.8873  0.4142  10.50000  0.05    3.35
Q3    1   0.5000  0.0929  0.3594  10.50000  0.05    2.98
Q4    1   0.5000  0.0978  0.4187  10.50000  0.05    2.97
;
_shelx_res_checksum              93919
_olex2_submission_special_instructions 'No special instructions were received'
