# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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 1935993'
loop_
_audit_author_name
_audit_author_address
'Wenjuan Wei'
;Jiangxi University of Science and Technology
China
;
_audit_update_record             
;
2019-06-24 deposited with the CCDC.	2019-09-09 downloaded from the CCDC.
;
_audit_creation_date             2019-06-21
_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(Br8 Pb2), 2(C5 H11 N S)'
_chemical_formula_sum            'C10 H16 Br4 N2 Pb S2'
_chemical_formula_weight         755.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 '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           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   8.4013(3)
_cell_length_b                   8.2000(3)
_cell_length_c                   29.0071(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1998.32(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7806
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.4600
_cell_measurement_theta_min      2.4520
_shelx_estimated_absorpt_T_max   0.287
_shelx_estimated_absorpt_T_min   0.082
_exptl_absorpt_coefficient_mu    16.640
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.510
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            18793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.609
_diffrn_reflns_theta_min         2.802
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2142
_reflns_number_total             2868
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.447
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         2868
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0433
_refine_ls_restrained_S_all      1.124
_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)+(0.0348P)²+9.1846P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0965
_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:
 C3(H3A,H3B), C5(H5A,H5B), C1(H1D,H1E), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.0000 0.5000 0.5000 0.03284(10) Uani 1 2 d S T P . .
Br2 Br 0.19531(8) 0.80629(8) 0.50286(2) 0.04626(18) Uani 1 1 d . . . . .
Br1 Br 0.03635(9) 0.47884(8) 0.39710(3) 0.05193(18) Uani 1 1 d . . . . .
S1 S 0.4556(5) 0.3633(5) 0.30749(11) 0.1214(12) Uani 1 1 d . . . . .
N1 N 0.4244(7) 0.5712(7) 0.4140(2) 0.0516(14) Uani 1 1 d . . . . .
H1A H 0.3292 0.5484 0.4022 0.062 Uiso 1 1 calc GR . . . .
H1B H 0.4511 0.6730 0.4067 0.062 Uiso 1 1 calc GR . . . .
H1C H 0.4211 0.5607 0.4445 0.062 Uiso 1 1 calc GR . . . .
C3 C 0.6770(10) 0.5893(11) 0.3211(3) 0.063(2) Uani 1 1 d . . . . .
H3A H 0.6519 0.7014 0.3288 0.076 Uiso 1 1 calc R . . . .
H3B H 0.7858 0.5663 0.3302 0.076 Uiso 1 1 calc R . . . .
C4 C 0.5636(9) 0.4741(9) 0.3438(3) 0.0546(17) Uani 1 1 d . . . . .
C5 C 0.5447(11) 0.4564(10) 0.3947(3) 0.0604(19) Uani 1 1 d . . . . .
H5A H 0.5128 0.3455 0.4017 0.072 Uiso 1 1 calc R . . . .
H5B H 0.6464 0.4761 0.4095 0.072 Uiso 1 1 calc R . . . .
C1 C 0.5485(17) 0.4432(17) 0.2615(4) 0.113(5) Uani 1 1 d . . . . .
H1D H 0.6044 0.3578 0.2450 0.136 Uiso 1 1 calc R . . . .
H1E H 0.4707 0.4910 0.2408 0.136 Uiso 1 1 calc R . . . .
C2 C 0.6550(14) 0.5608(17) 0.2754(7) 0.141(7) Uani 1 1 d . . . . .
H2A H 0.7578 0.5328 0.2624 0.169 Uiso 1 1 calc R . . . .
H2B H 0.6225 0.6629 0.2613 0.169 Uiso 1 1 calc R . . . .

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
Pb1 0.02565(15) 0.02384(15) 0.04902(19) 0.00013(12) -0.00096(12) 0.00000(9)
Br2 0.0399(3) 0.0366(3) 0.0623(4) -0.0026(3) 0.0077(3) -0.0144(3)
Br1 0.0537(4) 0.0465(3) 0.0555(4) 0.0058(3) -0.0104(3) -0.0002(3)
S1 0.136(3) 0.153(3) 0.0755(19) -0.017(2) -0.0106(19) -0.040(3)
N1 0.050(3) 0.044(3) 0.060(4) 0.000(3) -0.005(3) -0.007(3)
C3 0.056(5) 0.083(6) 0.050(4) 0.006(4) 0.002(4) 0.000(4)
C4 0.050(4) 0.052(4) 0.062(5) -0.002(3) -0.004(4) 0.008(3)
C5 0.069(5) 0.055(4) 0.058(5) -0.005(4) -0.013(4) 0.008(4)
C1 0.125(10) 0.160(12) 0.055(6) 0.009(7) 0.015(6) 0.071(10)
C2 0.068(7) 0.115(10) 0.24(2) 0.095(12) 0.028(10) 0.012(7)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 3.0012(6) . ?
Pb1 Br2 3.0137(6) 4_466 ?
Pb1 Br2 3.0013(6) 5_566 ?
Pb1 Br2 3.0137(6) 8_655 ?
Pb1 Br1 3.0053(8) 5_566 ?
Pb1 Br1 3.0054(8) . ?
Br2 Pb1 3.0137(6) 4_566 ?
S1 C4 1.661(8) . ?
S1 C1 1.679(12) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C5 1.489(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.495(11) . ?
C3 C2 1.360(19) . ?
C4 C5 1.490(11) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.376(18) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br2 180.0 . 5_566 ?
Br2 Pb1 Br2 91.379(5) 5_566 8_655 ?
Br2 Pb1 Br2 88.621(5) . 8_655 ?
Br2 Pb1 Br2 91.379(5) . 4_466 ?
Br2 Pb1 Br2 180.0 4_466 8_655 ?
Br2 Pb1 Br2 88.621(5) 5_566 4_466 ?
Br2 Pb1 Br1 91.159(18) 5_566 5_566 ?
Br2 Pb1 Br1 88.842(18) 5_566 . ?
Br2 Pb1 Br1 88.842(18) . 5_566 ?
Br2 Pb1 Br1 91.158(18) . . ?
Br1 Pb1 Br2 95.129(19) . 4_466 ?
Br1 Pb1 Br2 84.871(19) 5_566 4_466 ?
Br1 Pb1 Br2 84.871(19) . 8_655 ?
Br1 Pb1 Br2 95.129(19) 5_566 8_655 ?
Br1 Pb1 Br1 180.0 5_566 . ?
Pb1 Br2 Pb1 154.78(3) . 4_566 ?
C4 S1 C1 92.1(6) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C5 N1 H1A 109.5 . . ?
C5 N1 H1B 109.5 . . ?
C5 N1 H1C 109.5 . . ?
H3A C3 H3B 109.0 . . ?
C4 C3 H3A 111.0 . . ?
C4 C3 H3B 111.0 . . ?
C2 C3 H3A 111.0 . . ?
C2 C3 H3B 111.0 . . ?
C2 C3 C4 103.6(8) . . ?
C3 C4 S1 114.4(6) . . ?
C5 C4 S1 121.1(6) . . ?
C5 C4 C3 124.5(7) . . ?
N1 C5 C4 112.5(6) . . ?
N1 C5 H5A 109.1 . . ?
N1 C5 H5B 109.1 . . ?
C4 C5 H5A 109.1 . . ?
C4 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
S1 C1 H1D 109.6 . . ?
S1 C1 H1E 109.6 . . ?
H1D C1 H1E 108.2 . . ?
C2 C1 S1 110.1(10) . . ?
C2 C1 H1D 109.6 . . ?
C2 C1 H1E 109.6 . . ?
C3 C2 C1 119.6(11) . . ?
C3 C2 H2A 107.4 . . ?
C3 C2 H2B 107.4 . . ?
C1 C2 H2A 107.4 . . ?
C1 C2 H2B 107.4 . . ?
H2A C2 H2B 107.0 . . ?

_shelx_res_file                  
;
    1.res created by SHELXL-2014/7

TITL 1_a.res in Pbca
REM Old TITL 1_a.res in Pbca
REM SHELXT solution in Pbca
REM R1 0.149, Rweak 0.002, Alpha 0.018, Orientation as input
REM Formula found by SHELXT: C2 S2 Br4 Pb
CELL 0.71073 8.4013 8.2 29.0071 90 90 90
ZERR 4 0.0003 0.0003 0.0012 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Br N Pb S
UNIT 40 64 16 8 4 8

L.S. 4 0 0
PLAN  20
SIZE 0.1 0.2 0.3
BOND $H
list 4
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\1.hkl">
REM </olex2.extras>

WGHT    0.034800    9.184600
FVAR       0.13895
PB1   5    0.000000    0.500000    0.500000    10.50000    0.02565    0.02384 =
         0.04902    0.00013   -0.00096    0.00000
BR2   3    0.195312    0.806292    0.502858    11.00000    0.03986    0.03659 =
         0.06231   -0.00258    0.00772   -0.01438
BR1   3    0.036346    0.478837    0.397101    11.00000    0.05370    0.04655 =
         0.05553    0.00580   -0.01041   -0.00021
S1    6    0.455578    0.363337    0.307492    11.00000    0.13550    0.15309 =
         0.07550   -0.01674   -0.01064   -0.03983
N1    4    0.424429    0.571159    0.413951    11.00000    0.04981    0.04449 =
         0.06047    0.00035   -0.00534   -0.00693
AFIX 137
H1A   2    0.329162    0.548361    0.402181    11.00000   -1.20000
H1B   2    0.451133    0.673022    0.406714    11.00000   -1.20000
H1C   2    0.421135    0.560653    0.444475    11.00000   -1.20000
AFIX   0
C3    1    0.676957    0.589253    0.321106    11.00000    0.05581    0.08337 =
         0.05001    0.00558    0.00172   -0.00035
AFIX  23
H3A   2    0.651906    0.701440    0.328839    11.00000   -1.20000
H3B   2    0.785823    0.566317    0.330162    11.00000   -1.20000
AFIX   0
C4    1    0.563574    0.474082    0.343840    11.00000    0.05020    0.05155 =
         0.06206   -0.00158   -0.00423    0.00834
C5    1    0.544658    0.456445    0.394683    11.00000    0.06886    0.05477 =
         0.05753   -0.00453   -0.01342    0.00767
AFIX  23
H5A   2    0.512827    0.345457    0.401672    11.00000   -1.20000
H5B   2    0.646440    0.476079    0.409463    11.00000   -1.20000
AFIX   0
C1    1    0.548512    0.443204    0.261498    11.00000    0.12545    0.16015 =
         0.05474    0.00875    0.01549    0.07147
AFIX  23
H1D   2    0.604381    0.357777    0.244969    11.00000   -1.20000
H1E   2    0.470734    0.490965    0.240799    11.00000   -1.20000
AFIX   0
C2    1    0.655005    0.560810    0.275369    11.00000    0.06770    0.11541 =
         0.23938    0.09462    0.02758    0.01175
AFIX  23
H2A   2    0.757801    0.532819    0.262360    11.00000   -1.20000
H2B   2    0.622520    0.662906    0.261342    11.00000   -1.20000
AFIX   0
HKLF 4

REM  1_a.res in Pbca
REM R1 =  0.0433 for    2142 Fo > 4sig(Fo)  and  0.0655 for all    2868 data
REM     89 parameters refined using      0 restraints

END

WGHT      0.0348      9.1795

REM Highest difference peak  1.447,  deepest hole -1.393,  1-sigma level  0.200
Q1    1  -0.0013  0.4029  0.5004  11.00000  0.05    1.45
Q2    1   0.1822  0.9084  0.4994  11.00000  0.05    0.90
Q3    1   0.0607  0.7219  0.4997  11.00000  0.05    0.85
Q4    1   0.4193  0.7827  0.5008  11.00000  0.05    0.80
Q5    1   0.7131  0.6217  0.3369  11.00000  0.05    0.74
Q6    1   0.1027  0.8165  0.5011  11.00000  0.05    0.65
Q7    1   0.2222  0.6767  0.5013  11.00000  0.05    0.65
Q8    1   0.0675  0.3806  0.4008  11.00000  0.05    0.64
Q9    1   0.0589  0.8817  0.4996  11.00000  0.05    0.63
Q10   1   0.1912  0.4804  0.4992  11.00000  0.05    0.60
Q11   1   0.2970  0.8764  0.5005  11.00000  0.05    0.59
Q12   1  -0.0048  0.8009  0.5000  11.00000  0.05    0.55
Q13   1   0.6665  0.5174  0.3276  11.00000  0.05    0.53
Q14   1   0.0695  0.5836  0.3997  11.00000  0.05    0.52
Q15   1   0.5358  0.2437  0.4002  11.00000  0.05    0.49
Q16   1  -0.2360  0.4401  0.4997  11.00000  0.05    0.49
Q17   1   0.1906  0.4284  0.4024  11.00000  0.05    0.48
Q18   1   0.5155  0.5207  0.2623  11.00000  0.05    0.46
Q19   1   0.4198  0.6029  0.4991  11.00000  0.05    0.45
Q20   1   0.5357  0.8042  0.3430  11.00000  0.05    0.43
;
_shelx_res_checksum              59636
_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_123
_database_code_depnum_ccdc_archive 'CCDC 1935994'
loop_
_audit_author_name
_audit_author_address
'Wenjuan Wei'
;Jiangxi University of Science and Technology
China
;
_audit_update_record             
;
2019-06-24 deposited with the CCDC.	2019-09-09 downloaded from the CCDC.
;
_audit_creation_date             2019-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.13(Cl8 Pb2), 0.53(C5 H9 N S)'
_chemical_formula_sum            'C2.67 H4.80 Cl1.07 N0.53 Pb0.27 S0.53'
_chemical_formula_weight         154.50
_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'
Cl Cl 0.1484 0.1585 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z'
4 '-x, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x-1/2, y, -z-1/2'
7 '-x-1/2, y-1/2, z'
8 'x, -y-1/2, z-1/2'

_cell_length_a                   7.6733(4)
_cell_length_b                   7.6733(4)
_cell_length_c                   32.330(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1903.6(2)
_cell_formula_units_Z            15
_cell_measurement_reflns_used    17753
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.8660
_cell_measurement_theta_min      2.4720
_exptl_absorpt_coefficient_mu    9.633
_exptl_absorpt_correction_T_max  0.4459
_exptl_absorpt_correction_T_min  0.1602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.022
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            40616
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.52
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                1480
_reflns_number_total             1678
_reflns_threshold_expression     >2sigma(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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1678
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0337
_refine_ls_restrained_S_all      1.195
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0164P)²+13.3205P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0719
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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:
 C3(H3A,H3B), C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pb1 Pb 0.0000 0.0000 0.5000 0.03028(12) Uani 1 d . . 2 S T P
Cl2 Cl -0.3212(2) 0.1769(2) 0.51196(6) 0.0491(4) Uani 1 d . . 1 . . .
Cl1 Cl 0.0591(3) 0.0280(2) 0.58762(6) 0.0487(4) Uani 1 d . . 1 . . .
C4 C 0.5119(9) 0.0086(10) 0.6553(3) 0.0516(19) Uani 1 d . . 1 . . .
C3 C 0.3741(10) 0.1037(11) 0.6759(2) 0.054(2) Uani 1 d . . 1 . . .
H3A H 0.2663 0.0963 0.6603 0.065 Uiso 1 calc . . 1 R . .
H3B H 0.4053 0.2255 0.6790 0.065 Uiso 1 calc . . 1 R . .
C2 C 0.3553(14) 0.0209(14) 0.7159(3) 0.081(3) Uani 1 d . . 1 . . .
H2 H 0.2729 0.0589 0.7350 0.097 Uiso 1 calc . . 1 R . .
S1 S 0.5971(4) -0.1561(4) 0.68499(9) 0.0977(9) Uani 1 d . . 1 . . .
N1 N 0.4677(8) -0.0503(8) 0.58105(19) 0.0500(15) Uani 1 d . . 1 . . .
H1A H 0.5092 -0.0280 0.5559 0.060 Uiso 1 calc . . 1 GR . .
H1B H 0.3572 -0.0159 0.5826 0.060 Uiso 1 calc . . 1 GR . .
H1C H 0.4739 -0.1643 0.5860 0.060 Uiso 1 calc . . 1 GR . .
C5 C 0.5744(10) 0.0465(11) 0.6128(2) 0.0529(19) Uani 1 d . . 1 . . .
H5A H 0.6957 0.0126 0.6104 0.063 Uiso 1 calc . . 1 R . .
H5B H 0.5665 0.1708 0.6076 0.063 Uiso 1 calc . . 1 R . .
C1 C 0.4600(15) -0.1107(15) 0.7240(3) 0.083(3) Uani 1 d . . 1 . . .
H1 H 0.4582 -0.1722 0.7488 0.100 Uiso 1 calc . . 1 R . .

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
Pb1 0.02519(18) 0.02822(18) 0.0374(2) -0.00133(15) -0.00036(13) -0.00099(13)
Cl2 0.0430(9) 0.0439(9) 0.0604(10) 0.0081(8) 0.0089(8) 0.0180(8)
Cl1 0.0459(9) 0.0524(10) 0.0478(10) -0.0010(8) -0.0041(8) 0.0002(8)
C4 0.048(4) 0.055(5) 0.052(4) 0.002(4) -0.015(3) -0.014(4)
C3 0.050(4) 0.081(6) 0.030(4) -0.016(4) 0.004(3) -0.014(4)
C2 0.080(7) 0.094(8) 0.070(6) -0.014(6) 0.002(5) -0.007(6)
S1 0.103(2) 0.104(2) 0.0869(19) 0.0147(17) -0.0185(17) 0.0269(19)
N1 0.047(4) 0.059(4) 0.045(3) -0.001(3) 0.000(3) -0.001(3)
C5 0.045(4) 0.061(5) 0.053(4) -0.002(4) -0.001(4) -0.012(4)
C1 0.111(8) 0.093(8) 0.045(5) 0.006(5) -0.007(5) -0.019(7)

_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 Cl2 2.8400(16) . ?
Pb1 Cl2 2.8600(17) 3_556 ?
Pb1 Cl2 2.8400(16) 5_556 ?
Pb1 Cl2 2.8600(17) 7 ?
Pb1 Cl1 2.8770(18) 5_556 ?
Pb1 Cl1 2.8770(18) . ?
Cl2 Pb1 2.8600(16) 3_456 ?
C4 C3 1.448(11) . ?
C4 S1 1.717(8) . ?
C4 C5 1.483(11) . ?
C3 C2 1.448(12) . ?
C2 C1 1.317(14) . ?
S1 C1 1.679(11) . ?
N1 C5 1.509(9) . ?

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
Cl2 Pb1 Cl2 180.00(8) . 5_556 ?
Cl2 Pb1 Cl2 88.83(2) 5_556 3_556 ?
Cl2 Pb1 Cl2 91.17(2) . 3_556 ?
Cl2 Pb1 Cl2 88.83(2) . 7 ?
Cl2 Pb1 Cl2 91.17(2) 5_556 7 ?
Cl2 Pb1 Cl2 180.00(8) 7 3_556 ?
Cl2 Pb1 Cl1 89.58(5) 3_556 . ?
Cl2 Pb1 Cl1 88.11(5) . . ?
Cl2 Pb1 Cl1 90.42(5) 3_556 5_556 ?
Cl2 Pb1 Cl1 88.11(5) 5_556 5_556 ?
Cl2 Pb1 Cl1 90.42(5) 7 . ?
Cl2 Pb1 Cl1 89.58(5) 7 5_556 ?
Cl2 Pb1 Cl1 91.89(5) . 5_556 ?
Cl2 Pb1 Cl1 91.89(5) 5_556 . ?
Cl1 Pb1 Cl1 180.0 5_556 . ?
Pb1 Cl2 Pb1 144.32(7) . 3_456 ?
C3 C4 S1 113.0(6) . . ?
C3 C4 C5 124.3(7) . . ?
C5 C4 S1 122.7(6) . . ?
C4 C3 C2 105.2(8) . . ?
C1 C2 C3 117.0(9) . . ?
C1 S1 C4 91.7(5) . . ?
C4 C5 N1 111.0(6) . . ?
C2 C1 S1 113.0(8) . . ?

_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_qq
_database_code_depnum_ccdc_archive 'CCDC 1935996'
loop_
_audit_author_name
_audit_author_address
'Wenjuan Wei'
;Jiangxi University of Science and Technology
China
;
_audit_update_record             
;
2019-06-24 deposited with the CCDC.	2019-09-09 downloaded from the CCDC.
;
_audit_creation_date             2019-06-21
_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         'I8 Pb2, 4(C7.86 N2 S0.14)'
_chemical_formula_sum            'C31.45 I8 N8 Pb2 S0.55'
_chemical_formula_weight         1937.01
_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'
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'
S S 0.1246 0.1234 '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           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   29.051(2)
_cell_length_b                   8.6982(6)
_cell_length_c                   8.7096(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2200.8(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6192
_cell_measurement_temperature    212
_cell_measurement_theta_max      27.307
_cell_measurement_theta_min      2.804
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.309
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.923
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1683
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   0.788
_exptl_transmission_factor_min   0.729
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11081
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         2.805
_diffrn_ambient_temperature      212.01
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1180
_reflns_number_total             1281
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.336
_refine_diff_density_min         -1.939
_refine_diff_density_rms         0.234
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.291
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1281
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0408
_refine_ls_restrained_S_all      1.286
_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)+90.2935P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0813
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{C1, S1}
{C2AA, S2}
2. Rigid bond restraints
 C5, S2, S1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C5) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(S2) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C1) = Uanis(S1)
Uanis(C2AA) = Uanis(S2)
4. Others
 Sof(S1)=1-FVAR(1)
 Sof(C1)=FVAR(1)
 Sof(S2)=1-FVAR(2)
 Sof(C2AA)=FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_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 0.5000 0.5000 0.5000 0.01936(17) Uani 1 4 d S T P . .
I002 I 0.5000 0.81500(10) 0.31490(10) 0.0275(2) Uani 1 2 d S T P . .
I003 I 0.60977(3) 0.5000 0.5000 0.0429(3) Uani 1 2 d S T P . .
C1 C 0.6962(4) 0.471(2) 0.1573(16) 0.071(7) Uani 0.96(2) 1 d . . . A 1
C2AA C 0.6961(4) 0.3426(17) 0.026(2) 0.075(7) Uani 0.97(2) 1 d . . . A 3
C5 C 0.7452(5) 0.456(3) 0.043(3) 0.123(8) Uani 1 1 d . U . . .
C0AA C 0.6665(6) 0.5000 0.0000 0.064(6) Uani 1 2 d S T P . .
N3 N 0.5923(7) 0.420(2) -0.080(2) 0.134(7) Uani 1 1 d . . . . .
C1AA C 0.6168(9) 0.5000 0.0000 0.115(12) Uani 1 2 d S T P A .
S1 S 0.6962(4) 0.471(2) 0.1573(16) 0.071(7) Uani 0.04(2) 1 d . U . A 2
S2 S 0.6961(4) 0.3426(17) 0.026(2) 0.075(7) Uani 0.03(2) 1 d . U . A 4

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 0.0234(3) 0.0168(3) 0.0179(3) 0.0000(3) 0.000 0.000
I002 0.0371(5) 0.0221(4) 0.0234(4) 0.0097(4) 0.000 0.000
I003 0.0230(5) 0.0537(7) 0.0519(6) -0.0027(5) 0.000 0.000
C1 0.032(7) 0.115(15) 0.065(9) 0.008(8) -0.011(5) -0.005(7)
C2AA 0.045(8) 0.064(10) 0.115(15) 0.013(9) 0.001(8) 0.019(6)
C5 0.024(6) 0.17(2) 0.17(2) 0.096(16) 0.005(8) 0.004(8)
C0AA 0.029(9) 0.091(16) 0.072(13) 0.015(12) 0.000 0.000
N3 0.128(17) 0.133(18) 0.140(18) -0.039(14) 0.014(14) 0.010(14)
C1AA 0.036(14) 0.14(3) 0.17(4) 0.00(3) 0.000 0.000
S1 0.032(7) 0.115(15) 0.065(9) 0.008(8) -0.011(5) -0.005(7)
S2 0.045(8) 0.064(10) 0.115(15) 0.013(9) 0.001(8) 0.019(6)

_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 3.1790(8) . ?
Pb01 I002 3.1799(8) 2_665 ?
Pb01 I002 3.1790(8) 9_666 ?
Pb01 I002 3.1799(8) 10_556 ?
Pb01 I003 3.1890(10) . ?
Pb01 I003 3.1890(10) 9_666 ?
I002 Pb01 3.1799(8) 2_664 ?
C1 C5 1.74(2) . ?
C1 C0AA 1.638(15) . ?
C2AA C5 1.74(2) . ?
C2AA C0AA 1.632(15) . ?
C5 C5 1.07(3) 4_565 ?
C5 S1 1.74(2) . ?
C5 S2 1.74(2) . ?
C0AA C1 1.638(15) 4_565 ?
C0AA C2AA 1.632(15) 4_565 ?
C0AA C1AA 1.44(3) . ?
C0AA S1 1.638(15) 4_565 ?
C0AA S1 1.638(15) . ?
C0AA S2 1.632(15) . ?
C0AA S2 1.632(15) 4_565 ?
N3 C1AA 1.21(2) . ?
C1AA N3 1.21(2) 4_565 ?

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 . 9_666 ?
I002 Pb01 I002 89.929(9) 9_666 2_665 ?
I002 Pb01 I002 90.072(9) . 2_665 ?
I002 Pb01 I002 89.928(9) . 10_556 ?
I002 Pb01 I002 90.071(9) 9_666 10_556 ?
I002 Pb01 I002 180.000(15) 10_556 2_665 ?
I002 Pb01 I003 90.0 2_665 9_666 ?
I002 Pb01 I003 90.0 9_666 9_666 ?
I002 Pb01 I003 90.0 . 9_666 ?
I002 Pb01 I003 90.0 9_666 . ?
I002 Pb01 I003 90.0 10_556 9_666 ?
I002 Pb01 I003 90.0 10_556 . ?
I002 Pb01 I003 90.0 . . ?
I002 Pb01 I003 90.0 2_665 . ?
I003 Pb01 I003 180.0 . 9_666 ?
Pb01 I002 Pb01 150.87(3) . 2_664 ?
C0AA C1 C5 88.0(11) . . ?
C0AA C2AA C5 88.2(11) . . ?
C5 C5 C1 110(2) 4_565 . ?
C5 C5 C2AA 110(2) 4_565 . ?
C5 C5 S1 110(2) 4_565 . ?
C5 C5 S2 110(2) 4_565 . ?
C1 C0AA C1 116.5(13) 4_565 . ?
C2AA C0AA C2AA 116.4(14) . 4_565 ?
C1AA C0AA C1 121.8(7) . . ?
C1AA C0AA C1 121.8(7) . 4_565 ?
C1AA C0AA C2AA 121.8(7) . 4_565 ?
C1AA C0AA C2AA 121.8(7) . . ?
C1AA C0AA S1 121.8(7) . 4_565 ?
C1AA C0AA S1 121.8(7) . . ?
C1AA C0AA S2 121.8(7) . . ?
C1AA C0AA S2 121.8(7) . 4_565 ?
S1 C0AA S1 116.5(13) 4_565 . ?
S2 C0AA S2 116.4(14) . 4_565 ?
N3 C1AA C0AA 125.8(14) . . ?
N3 C1AA C0AA 125.8(14) 4_565 . ?
N3 C1AA N3 108(3) 4_565 . ?
C0AA S1 C5 88.0(11) . . ?
C0AA S2 C5 88.2(11) . . ?

_shelx_res_file                  
;
    qq.res created by SHELXL-2014/7

TITL qq_a.res in Cmca
REM Old TITL qq in Cmce #64
REM SHELXT solution in Cmca
REM R1 0.162, Rweak 0.010, Alpha 0.030, Orientation as input
REM Formula found by SHELXT: C4 I4 Pb
CELL 0.71073 29.0506 8.6982 8.7096 90 90 90
ZERR 2 0.002 0.0006 0.0006 0 0 0
LATT 7
SYMM -X,0.5-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM +X,-Y,-Z
SFAC C I N Pb S
UNIT 62.9 16 16 4 1.1
DELU C5 S2 S1
ISOR C5
ISOR C5 S1 S2
EADP C1 S1
EADP C2AA S2
EXYZ C1 S1
EXYZ C2AA S2

L.S. 99
PLAN  10
TEMP -61.14
BOND $H
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\qq.hkl">
REM </olex2.extras>

WGHT    0.000000   90.293495
FVAR       0.10808   0.96402   0.96694
PB01  4    0.500000    0.500000    0.500000    10.25000    0.02337    0.01679 =
         0.01790    0.00002    0.00000    0.00000
I002  2    0.500000    0.814998    0.314902    10.50000    0.03705    0.02209 =
         0.02345    0.00966    0.00000    0.00000
I003  2    0.609772    0.500000    0.500000    10.50000    0.02296    0.05369 =
         0.05190   -0.00267    0.00000    0.00000
PART 1
C1    1    0.696166    0.471302    0.157328    21.00000    0.03247    0.11509 =
         0.06475    0.00816   -0.01115   -0.00515
PART 0
PART 3
C2AA  1    0.696078    0.342647    0.025564    31.00000    0.04549    0.06424 =
         0.11479    0.01337    0.00147    0.01867
PART 0
C5    1    0.745155    0.455922    0.043119    11.00000    0.02436    0.17245 =
         0.17322    0.09596    0.00514    0.00400
C0AA  1    0.666471    0.500000    0.000000    10.50000    0.02948    0.09058 =
         0.07182    0.01478    0.00000    0.00000
N3    3    0.592299    0.419764   -0.079628    11.00000    0.12814    0.13335 =
         0.13980   -0.03938    0.01424    0.00989
C1AA  1    0.616765    0.500000    0.000000    10.50000    0.03646    0.13653 =
         0.17218   -0.00280    0.00000    0.00000
PART 2
S1    5    0.696166    0.471302    0.157328   -21.00000    0.03247    0.11509 =
         0.06475    0.00816   -0.01115   -0.00515
PART 0
PART 4
S2    5    0.696078    0.342647    0.025564   -31.00000    0.04549    0.06424 =
         0.11479    0.01337    0.00147    0.01867
HKLF 4

REM  qq_a.res in Cmca
REM R1 =  0.0408 for    1180 Fo > 4sig(Fo)  and  0.0456 for all    1281 data
REM     64 parameters refined using     20 restraints

END

WGHT      0.0000     90.2972

REM Highest difference peak  2.336,  deepest hole -1.939,  1-sigma level  0.234
Q1    1   0.5000  0.9424  0.1898  10.50000  0.05    2.34
Q2    1   0.5000  0.6911  0.4463  10.50000  0.05    1.99
Q3    1   0.5000  0.6862  0.0968  10.50000  0.05    1.64
Q4    1   0.7219  0.3143 -0.1876  11.00000  0.05    1.53
Q5    1   0.5000  1.0517  0.2899  10.50000  0.05    0.87
Q6    1   0.5000  0.5890  0.1937  10.50000  0.05    0.80
Q7    1   0.6200  0.5719  0.4640  11.00000  0.05    0.75
Q8    1   0.7760  0.5545  0.1787  11.00000  0.05    0.70
Q9    1   0.5197  0.7485  0.3390  11.00000  0.05    0.64
Q10   1   0.5525  0.5000  0.5000  10.50000  0.05    0.64
;
_shelx_res_checksum              16127
_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_mo_ly18_2415k_0m
_database_code_depnum_ccdc_archive 'CCDC 1935995'
loop_
_audit_author_name
_audit_author_address
'Wenjuan Wei'
;Jiangxi University of Science and Technology
China
;
_audit_update_record             
;
2019-06-24 deposited with the CCDC.	2019-09-09 downloaded from the CCDC.
;
_audit_creation_date             2019-06-21
_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         'Cl8 Pb2, 4(C5.32 N S0.68)'
_chemical_formula_sum            'C21.28 Cl8 N4 Pb2 S2.72'
_chemical_formula_weight         1096.80
_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'
Cl Cl 0.1484 0.1585 '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'
S S 0.1246 0.1234 '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           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   32.397(7)
_cell_length_b                   7.7997(13)
_cell_length_c                   7.7943(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1969.5(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2448
_cell_measurement_temperature    415
_cell_measurement_theta_max      27.430
_cell_measurement_theta_min      2.514
_shelx_estimated_absorpt_T_max   0.458
_shelx_estimated_absorpt_T_min   0.168
_exptl_absorpt_coefficient_mu    9.240
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6234
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.586
_diffrn_reflns_theta_min         3.749
_diffrn_ambient_temperature      415
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                787
_reflns_number_total             1160
_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 (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         0.688
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1160
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0291
_refine_ls_restrained_S_all      1.141
_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)+(0.0374P)²+1.1929P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0767
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{S10, C0AA}
2. Uiso/Uaniso restraints and constraints
Uanis(S10) = Uanis(C0AA)
3. Rigid body (RIGU) restrains
 C2, S10, C1, C3, C0AA, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C0AA)=1-FVAR(1)
 Sof(S10)=FVAR(1)
 Fixed Sof: N1(0.5)
;
_atom_sites_solution_hydrogens   .
_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 0.5000 0.5000 0.5000 0.06120(17) Uani 1 4 d S T P . .
Cl2 Cl 0.5000 0.1812(2) 0.3190(3) 0.0903(6) Uani 1 2 d S T P . .
Cl1 Cl 0.58767(10) 0.5000 0.5000 0.1172(10) Uani 1 2 d S T P . .
S10 S 0.6742(2) -0.1164(12) 0.6167(12) 0.238(6) Uani 0.340(17) 1 d . U . A 1
C2 C 0.6475(6) 0.0000 0.5000 0.166(5) Uani 1 2 d S TU P . .
C1 C 0.7142(6) -0.067(4) 0.559(3) 0.265(9) Uani 1 1 d . U . . .
N1 N 0.5800(4) 0.0738(16) 0.5762(18) 0.109(3) Uani 0.5 1 d . U . A -1
C3 C 0.6019(7) 0.0000 0.5000 0.149(4) Uani 1 2 d S TU P A .
C0AA C 0.6742(2) -0.1164(12) 0.6167(12) 0.238(6) Uani 0.660(17) 1 d . U . A 2

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
Pb1 0.1006(3) 0.0420(2) 0.0410(2) 0.00001(14) 0.000 0.000
Cl2 0.1431(18) 0.0640(9) 0.0637(11) -0.0231(10) 0.000 0.000
Cl1 0.1054(19) 0.126(3) 0.120(3) -0.0007(14) 0.000 0.000
S10 0.182(5) 0.289(11) 0.245(10) 0.070(9) -0.016(4) 0.039(4)
C2 0.146(6) 0.187(10) 0.165(9) 0.009(6) 0.000 0.000
C1 0.182(6) 0.346(17) 0.268(15) 0.071(13) -0.011(4) 0.026(4)
N1 0.133(6) 0.089(7) 0.104(8) 0.048(6) -0.009(4) -0.016(4)
C3 0.152(6) 0.144(9) 0.150(9) 0.018(6) 0.000 0.000
C0AA 0.182(5) 0.289(11) 0.245(10) 0.070(9) -0.016(4) 0.039(4)

_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 Cl2 2.8586(17) 9_666 ?
Pb1 Cl2 2.8601(18) 10_566 ?
Pb1 Cl2 2.8601(18) 2_655 ?
Pb1 Cl2 2.8586(17) . ?
Pb1 Cl1 2.840(3) . ?
Pb1 Cl1 2.840(3) 9_666 ?
Cl2 Pb1 2.8601(18) 2_654 ?
S10 C2 1.550(12) . ?
S10 C1 1.425(18) . ?
C2 S10 1.550(12) 4_556 ?
C2 C3 1.48(3) . ?
C2 C0AA 1.550(12) . ?
C2 C0AA 1.550(12) 4_556 ?
C1 C1 1.38(4) 4_556 ?
C1 C0AA 1.425(18) . ?
N1 C3 1.090(16) . ?

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
Cl2 Pb1 Cl2 180.0 9_666 . ?
Cl2 Pb1 Cl2 180.0 2_655 10_566 ?
Cl2 Pb1 Cl2 90.05(2) . 10_566 ?
Cl2 Pb1 Cl2 89.95(2) . 2_655 ?
Cl2 Pb1 Cl2 89.95(2) 9_666 10_566 ?
Cl2 Pb1 Cl2 90.05(2) 9_666 2_655 ?
Cl1 Pb1 Cl2 90.0 9_666 2_655 ?
Cl1 Pb1 Cl2 90.0 . 9_666 ?
Cl1 Pb1 Cl2 90.0 . . ?
Cl1 Pb1 Cl2 90.0 . 2_655 ?
Cl1 Pb1 Cl2 90.0 9_666 . ?
Cl1 Pb1 Cl2 90.0 9_666 9_666 ?
Cl1 Pb1 Cl2 90.0 9_666 10_566 ?
Cl1 Pb1 Cl2 90.0 . 10_566 ?
Cl1 Pb1 Cl1 180.0 9_666 . ?
Pb1 Cl2 Pb1 149.20(8) . 2_654 ?
C1 S10 C2 99.3(11) . . ?
S10 C2 S10 112.0(14) 4_556 . ?
C3 C2 S10 124.0(7) . . ?
C3 C2 S10 124.0(7) . 4_556 ?
C3 C2 C0AA 124.0(7) . 4_556 ?
C3 C2 C0AA 124.0(7) . . ?
C0AA C2 C0AA 112.0(14) . 4_556 ?
C1 C1 S10 114.5(9) 4_556 . ?
C1 C1 C0AA 114.5(9) 4_556 . ?
N1 C3 C2 130.6(12) . . ?
C1 C0AA C2 99.3(11) . . ?

_shelx_res_file                  
;
    mo_ly18_2415k_0m.res created by SHELXL-2014/7

TITL mo_ly18_2415k_0m_a.res in Cmca
REM Old TITL mo_ly18_2415k_0m_b.res in Cmmm
REM SHELXT solution in Cmca
REM R1 0.278, Rweak 0.001, Alpha 0.016, Orientation as input
REM Formula found by SHELXT: C2 Cl4 Pb
CELL 0.71073 32.3975 7.7997 7.7943 90 90 90
ZERR 2 0.0067 0.0013 0.0014 0 0 0
LATT 7
SYMM -X,0.5-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM +X,-Y,-Z
SFAC C Cl N Pb S
UNIT 42.56 16 8 4 5.44
EQIV $1 +X,-Y,1-Z
RIGU 0.001 0.001 C2 S10 C1 C3 C0AA N1
EADP S10 C0AA
EXYZ S10 C0AA

L.S. 10
PLAN  20
SIZE 0.1 0.2 0.3
TEMP 141.85
FREE S10 S10_$1
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\mo_LY18_2415K_0m.hkl">
REM </olex2.extras>

WGHT    0.037400    1.192900
FVAR       0.23468   0.33974
PB1   4    0.500000    0.500000    0.500000    10.25000    0.10056    0.04199 =
         0.04103    0.00001    0.00000    0.00000
CL2   2    0.500000    0.181244    0.318987    10.50000    0.14310    0.06404 =
         0.06368   -0.02314    0.00000    0.00000
CL1   2    0.587670    0.500000    0.500000    10.50000    0.10542    0.12643 =
         0.11978   -0.00066    0.00000    0.00000
PART 1
S10   5    0.674229   -0.116366    0.616661    21.00000    0.18189    0.28875 =
         0.24477    0.07013   -0.01614    0.03936
PART 0
C2    1    0.647482    0.000000    0.500000    10.50000    0.14612    0.18683 =
         0.16538    0.00874    0.00000    0.00000
C1    1    0.714185   -0.066608    0.558505    11.00000    0.18200    0.34629 =
         0.26779    0.07109   -0.01092    0.02585
PART -1
N1    3    0.580017    0.073834    0.576164    10.50000    0.13349    0.08864 =
         0.10416    0.04814   -0.00895   -0.01551
PART 0
C3    1    0.601929    0.000000    0.500000    10.50000    0.15243    0.14433 =
         0.14982    0.01764    0.00000    0.00000
PART 2
C0AA  1    0.674229   -0.116366    0.616661   -21.00000    0.18189    0.28875 =
         0.24477    0.07013   -0.01614    0.03936
HKLF 4

REM  mo_ly18_2415k_0m_a.res in Cmca
REM R1 =  0.0291 for     787 Fo > 4sig(Fo)  and  0.0488 for all    1160 data
REM     54 parameters refined using     30 restraints

END

WGHT      0.0418      2.2481

REM Highest difference peak  0.688,  deepest hole -1.221,  1-sigma level  0.097
Q1    1   0.5384  0.5000  0.5000  10.50000  0.05    0.61
Q2    1   0.5822  0.1236  0.5258  11.00000  0.05    0.41
Q3    1   0.5888  0.0125  0.6497  11.00000  0.05    0.37
Q4    1   0.7297 -0.0258  0.4713  11.00000  0.05    0.34
Q5    1   0.6825 -0.1487  0.4895  11.00000  0.05    0.33
Q6    1   0.5669  0.0188  0.5852  11.00000  0.05    0.32
Q7    1   0.6083  0.1013  0.5222  11.00000  0.05    0.29
Q8    1   0.6554 -0.1809  0.6657  11.00000  0.05    0.26
Q9    1   0.7088 -0.1751  0.6590  11.00000  0.05    0.22
Q10   1   0.6884 -0.0452  0.6276  11.00000  0.05    0.21
Q11   1   0.5000  0.4748  0.5779  10.50000  0.05    0.21
Q12   1   0.5325  0.2368  0.2730  11.00000  0.05    0.21
Q13   1   0.6718  0.0044  0.6715  11.00000  0.05    0.20
Q14   1   0.5956  0.1968  0.4003  11.00000  0.05    0.19
Q15   1   0.5412  0.3705  0.3037  11.00000  0.05    0.19
Q16   1   0.4541  0.2468  0.2511  11.00000  0.05    0.19
Q17   1   0.5784  0.2643  0.5072  11.00000  0.05    0.18
Q18   1   0.5000  0.2071  0.4919  10.50000  0.05    0.18
Q19   1   0.7219 -0.2362  0.6665  11.00000  0.05    0.18
Q20   1   0.5491  0.4814  0.6988  11.00000  0.05    0.18
;
_shelx_res_checksum              46052
_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_t20180930lc_e16_0m
_database_code_depnum_ccdc_archive 'CCDC 1935997'
loop_
_audit_author_name
_audit_author_address
'Wenjuan Wei'
;Jiangxi University of Science and Technology
China
;
_audit_update_record             
;
2019-06-24 deposited with the CCDC.	2019-09-09 downloaded from the CCDC.
;
_audit_creation_date             2019-05-31
_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(I8 Pb2), 2(C5.26 H9 N S0.74)'
_chemical_formula_sum            'C10.71 H24.71 I4 N2 Pb S1.29'
_chemical_formula_weight         937.65
_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'
S S 0.1246 0.1234 '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           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.810(2)
_cell_length_b                   8.6780(19)
_cell_length_c                   28.972(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2215.0(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7821
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.547
_cell_measurement_theta_min      2.812
_shelx_estimated_absorpt_T_max   0.350
_shelx_estimated_absorpt_T_min   0.109
_exptl_absorpt_coefficient_mu    13.306
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.812
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1670
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            22805
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         27.614
_diffrn_reflns_theta_min         2.706
_diffrn_ambient_temperature      298
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1923
_reflns_number_total             2566
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.916
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.282
_refine_ls_extinction_coef       0.00079(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         2566
_refine_ls_number_restraints     129
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0620
_refine_ls_restrained_S_all      1.225
_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)+(0.0346P)²+45.3005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1412
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Shared sites
{C7, S7}
{C4, S4}
3. Rigid bond restraints
 S7, C0AA, C2AA, S4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C5 \\sim C1AA \\sim C7 \\sim C4 \\sim C0AA \\sim C2AA: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02
S7 \\sim C0AA \\sim C2AA \\sim S4 \\sim C5: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C0AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C7) = Uanis(S7)
Uanis(C4) = Uanis(S4)
5. Others
 Sof(H0AC)=Sof(H0AD)=Sof(S7)=1-FVAR(1)
 Sof(C7)=Sof(H0AA)=Sof(H0AB)=FVAR(1)
 Sof(H2AF)=Sof(H2AG)=Sof(S4)=1-FVAR(2)
 Sof(C4)=Sof(H2AD)=Sof(H2AE)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB), C0AA(H0AA,H0AB), C0AA(H0AC,H0AD), C2AA(H2AD,H2AE), C2AA(H2AF,
 H2AG)
6.b Idealised Me refined as rotating group:
 N2AA(H2AA,H2AB,H2AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.5000 0.0000 0.5000 0.0322(2) Uani 1 2 d S T P . .
I2 I 0.19215(10) 0.19111(10) 0.50292(3) 0.0452(3) Uani 1 1 d . . . . .
I3 I 0.46787(12) 0.01584(11) 0.38986(3) 0.0511(3) Uani 1 1 d . . . . .
C5 C 0.942(3) 0.020(3) 0.3371(8) 0.102(4) Uani 1 1 d . U . . .
N2AA N 1.0698(16) -0.0711(17) 0.4079(5) 0.067(4) Uani 1 1 d . . . . .
H2AA H 1.1591 -0.0518 0.3947 0.080 Uiso 1 1 calc GR . . . .
H2AB H 1.0435 -0.1685 0.4025 0.080 Uiso 1 1 calc GR . . . .
H2AC H 1.0769 -0.0558 0.4382 0.080 Uiso 1 1 calc GR . . . .
C1AA C 0.953(3) 0.034(3) 0.3883(8) 0.103(4) Uani 1 1 d . U . . .
H1AA H 0.9780 0.1392 0.3964 0.124 Uiso 1 1 calc R . . . .
H1AB H 0.8552 0.0096 0.4020 0.124 Uiso 1 1 calc R . . . .
C7 C 0.8310(19) -0.099(2) 0.3128(5) 0.110(4) Uani 0.76(2) 1 d . U . A 4
C4 C 1.0356(14) 0.1221(14) 0.3028(3) 0.109(3) Uani 0.50(3) 1 d . U . A 6
C0AA C 0.869(3) -0.048(3) 0.2639(8) 0.109(4) Uani 1 1 d . U . . .
H0AA H 0.9035 -0.1382 0.2472 0.131 Uiso 0.76(2) 1 calc R . . A 4
H0AB H 0.7751 -0.0150 0.2496 0.131 Uiso 0.76(2) 1 calc R . . A 4
H0AC H 0.9035 -0.1382 0.2472 0.131 Uiso 0.24(2) 1 calc R . . A 5
H0AD H 0.7751 -0.0150 0.2496 0.131 Uiso 0.24(2) 1 calc R . . A 5
C2AA C 0.966(3) 0.058(3) 0.2569(8) 0.110(4) Uani 1 1 d . U . . .
H2AD H 0.9179 0.1413 0.2402 0.132 Uiso 0.50(3) 1 calc R . . A 6
H2AE H 1.0470 0.0172 0.2377 0.132 Uiso 0.50(3) 1 calc R . . A 6
H2AF H 0.9179 0.1413 0.2402 0.132 Uiso 0.50(3) 1 calc R . . A 7
H2AG H 1.0470 0.0172 0.2377 0.132 Uiso 0.50(3) 1 calc R . . A 7
S7 S 0.8310(19) -0.099(2) 0.3128(5) 0.110(4) Uani 0.24(2) 1 d . U . A 5
S4 S 1.0356(14) 0.1221(14) 0.3028(3) 0.109(3) Uani 0.50(3) 1 d . U . A 7

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
Pb1 0.0268(3) 0.0271(3) 0.0428(4) -0.0012(3) 0.0019(3) -0.0001(2)
I2 0.0376(5) 0.0380(5) 0.0601(6) 0.0035(4) 0.0086(4) 0.0164(4)
I3 0.0588(6) 0.0556(6) 0.0390(6) -0.0041(5) 0.0060(4) 0.0025(5)
C5 0.115(7) 0.124(8) 0.068(5) 0.004(6) 0.002(5) -0.012(6)
N2AA 0.058(10) 0.066(9) 0.077(10) 0.006(8) 0.002(8) -0.013(8)
C1AA 0.116(8) 0.126(8) 0.067(6) 0.008(6) 0.000(6) -0.012(7)
C7 0.119(7) 0.132(8) 0.078(5) 0.003(5) -0.002(5) -0.016(6)
C4 0.127(7) 0.135(7) 0.066(5) 0.010(5) 0.004(4) -0.020(5)
C0AA 0.121(7) 0.132(8) 0.074(6) 0.000(6) -0.002(6) -0.011(6)
C2AA 0.123(8) 0.134(8) 0.072(6) 0.003(6) 0.003(6) -0.010(6)
S7 0.119(7) 0.132(8) 0.078(5) 0.003(5) -0.002(5) -0.016(6)
S4 0.127(7) 0.135(7) 0.066(5) 0.010(5) 0.004(4) -0.020(5)

_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 I2 3.1715(10) 7_655 ?
Pb1 I2 3.1801(10) . ?
Pb1 I2 3.1715(10) 3_556 ?
Pb1 I2 3.1801(10) 5_656 ?
Pb1 I3 3.2064(12) 5_656 ?
Pb1 I3 3.2065(12) . ?
I2 Pb1 3.1715(10) 3_456 ?
C5 C1AA 1.49(3) . ?
C5 C7 1.59(3) . ?
C5 C4 1.57(3) . ?
C5 S7 1.59(3) . ?
C5 S4 1.57(3) . ?
N2AA C1AA 1.49(3) . ?
C7 C0AA 1.52(3) . ?
C4 C2AA 1.57(3) . ?
C0AA C2AA 1.27(3) . ?
C0AA S7 1.52(3) . ?
C2AA S4 1.57(3) . ?

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
I2 Pb1 I2 180.0 7_655 3_556 ?
I2 Pb1 I2 90.868(17) 3_556 . ?
I2 Pb1 I2 89.132(18) 7_655 . ?
I2 Pb1 I2 90.868(18) 7_655 5_656 ?
I2 Pb1 I2 89.132(18) 3_556 5_656 ?
I2 Pb1 I2 180.0 5_656 . ?
I2 Pb1 I3 94.08(3) 5_656 . ?
I2 Pb1 I3 90.90(3) 7_655 . ?
I2 Pb1 I3 94.08(3) . 5_656 ?
I2 Pb1 I3 90.90(3) 3_556 5_656 ?
I2 Pb1 I3 89.10(3) 3_556 . ?
I2 Pb1 I3 85.92(3) 5_656 5_656 ?
I2 Pb1 I3 85.92(3) . . ?
I2 Pb1 I3 89.10(3) 7_655 5_656 ?
I3 Pb1 I3 180.00(4) 5_656 . ?
Pb1 I2 Pb1 153.54(3) 3_456 . ?
C1AA C5 C7 122(2) . . ?
C1AA C5 C4 123(2) . . ?
C1AA C5 S7 122(2) . . ?
C1AA C5 S4 123(2) . . ?
N2AA C1AA C5 112(2) . . ?
C0AA C7 C5 94.8(16) . . ?
C2AA C4 C5 97.4(15) . . ?
C2AA C0AA C7 121(2) . . ?
C2AA C0AA S7 121(2) . . ?
C0AA C2AA C4 113(2) . . ?
C0AA C2AA S4 113(2) . . ?
C0AA S7 C5 94.8(16) . . ?
C2AA S4 C5 97.4(15) . . ?

_shelx_res_file                  
;
    t20180930lc_e16_0m.res created by SHELXL-2014/7

TITL T20180930LC_E16_0m in Pbca #61
REM reset to Pbca #61
CELL 0.71076 8.8099 8.678 28.9722 90 90 90
ZERR 4 0.002 0.0019 0.0061 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
SFAC C H I N Pb S
UNIT 42.85 98.85 16 8 4 5.15
DELU S7 C0AA C2AA S4 C5
SIMU 0.01 0.02 3.8 $C
SIMU S7 C0AA C2AA S4 C5
ISOR C0AA C2AA
EADP C7 S7
EADP C4 S4
EXYZ C7 S7
EXYZ C4 S4

L.S. 24
PLAN  10
SIZE 0.1 0.2 0.3
TEMP 24.85
BOND
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\T20180930LC_E16_0m.hkl">
REM </olex2.extras>

WGHT    0.034600   45.300499
EXTI    0.000787
FVAR       0.13159   0.76052   0.50259
PB1   5    0.500000    0.000000    0.500000    10.50000    0.02682    0.02713 =
         0.04278   -0.00115    0.00191   -0.00013
I2    3    0.192148    0.191107    0.502924    11.00000    0.03759    0.03796 =
         0.06011    0.00354    0.00860    0.01636
I3    3    0.467873    0.015841    0.389861    11.00000    0.05878    0.05563 =
         0.03903   -0.00410    0.00600    0.00245
C5    1    0.941568    0.019952    0.337083    11.00000    0.11474    0.12431 =
         0.06834    0.00362    0.00173   -0.01152
N2AA  4    1.069836   -0.071134    0.407904    11.00000    0.05813    0.06633 =
         0.07654    0.00573    0.00161   -0.01286
AFIX 137
H2AA  2    1.159076   -0.051835    0.394718    11.00000   -1.20000
H2AB  2    1.043527   -0.168502    0.402510    11.00000   -1.20000
H2AC  2    1.076914   -0.055804    0.438202    11.00000   -1.20000
AFIX   0
C1AA  1    0.952915    0.033646    0.388335    11.00000    0.11582    0.12612 =
         0.06722    0.00768    0.00009   -0.01195
AFIX  23
H1AA  2    0.977958    0.139153    0.396351    11.00000   -1.20000
H1AB  2    0.855174    0.009642    0.401969    11.00000   -1.20000
AFIX   0
PART 4
C7    1    0.830966   -0.099374    0.312821    21.00000    0.11943    0.13237 =
         0.07783    0.00254   -0.00235   -0.01581
PART 0
PART 6
C4    1    1.035642    0.122108    0.302787    31.00000    0.12715    0.13478 =
         0.06551    0.01002    0.00417   -0.01992
PART 0
C0AA  1    0.869257   -0.047800    0.263916    11.00000    0.12137    0.13197 =
         0.07442    0.00036   -0.00177   -0.01070
PART 4
AFIX  23
H0AA  2    0.903485   -0.138238    0.247218    21.00000   -1.20000
H0AB  2    0.775132   -0.015043    0.249582    21.00000   -1.20000
AFIX  23
PART 0
PART 5
H0AC  2    0.903485   -0.138238    0.247218   -21.00000   -1.20000
H0AD  2    0.775132   -0.015043    0.249582   -21.00000   -1.20000
AFIX   0
PART 0
C2AA  1    0.966008    0.057590    0.256895    11.00000    0.12305    0.13367 =
         0.07219    0.00336    0.00311   -0.01044
PART 6
AFIX  23
H2AD  2    0.917908    0.141264    0.240196    31.00000   -1.20000
H2AE  2    1.047044    0.017244    0.237720    31.00000   -1.20000
AFIX  23
PART 0
PART 7
H2AF  2    0.917908    0.141264    0.240196   -31.00000   -1.20000
H2AG  2    1.047044    0.017244    0.237720   -31.00000   -1.20000
AFIX   0
PART 0
PART 5
S7    6    0.830966   -0.099374    0.312821   -21.00000    0.11943    0.13237 =
         0.07783    0.00254   -0.00235   -0.01581
PART 0
PART 7
S4    6    1.035642    0.122108    0.302787   -31.00000    0.12715    0.13478 =
         0.06551    0.01002    0.00417   -0.01992
HKLF 4

REM  T20180930LC_E16_0m in Pbca #61
REM R1 =  0.0620 for    1923 Fo > 4sig(Fo)  and  0.0889 for all    2566 data
REM     92 parameters refined using    129 restraints

END

WGHT      0.0346     45.3121

REM Highest difference peak  1.916,  deepest hole -1.352,  1-sigma level  0.282
Q1    1   1.1122  0.0442  0.3007  11.00000  0.05    1.68
Q2    1   0.9044 -0.1592  0.3008  11.00000  0.05    1.26
Q3    1   0.4673  0.0023  0.4202  11.00000  0.05    1.02
Q4    1   0.8080 -0.0235  0.3030  11.00000  0.05    0.98
Q5    1   0.4914  0.0181  0.3632  11.00000  0.05    0.96
Q6    1   0.2038  0.1958  0.5387  11.00000  0.05    0.93
Q7    1   0.8337  0.1409  0.4400  11.00000  0.05    0.92
Q8    1   0.5818 -0.0612  0.3859  11.00000  0.05    0.91
Q9    1   0.3829 -0.0013  0.4199  11.00000  0.05    0.88
Q10   1   0.4217 -0.0957  0.3990  11.00000  0.05    0.86
;
_shelx_res_checksum              40984
_olex2_submission_special_instructions 'No special instructions were received'
