# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_2011145536_2_0m_pl
_database_code_depnum_ccdc_archive 'CCDC 2101286'
loop_
_audit_author_name
_audit_author_address
'Dianxing Ju'
;Qingdao University of Science and Technology
China
;
_audit_update_record             
;
2021-08-04 deposited with the CCDC.	2022-07-31 downloaded from the CCDC.
;
_audit_creation_date             2020-11-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H8 Br2 N2 Pb'
_chemical_formula_sum            'C10 H8 Br2 N2 Pb'
_chemical_formula_weight         523.19
_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 0.0148 0.0070 '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 -0.9502 1.0410 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.4950 6.8412 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.1000(7)
_cell_length_b                   12.4041(7)
_cell_length_c                   4.2095(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.555(4)
_cell_angle_gamma                90
_cell_volume                     627.67(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3773
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.941
_cell_measurement_theta_min      8.943
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.552
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.2670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 6399 reflections, Rint = 0.0556
 (3625 with I > 3sig(I), Rint = 0.0488)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.768
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            1147
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.025
_diffrn_reflns_theta_min         8.939
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1146
_reflns_number_total             1147
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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         4.677
_refine_diff_density_min         -2.914
_refine_diff_density_rms         0.418
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         1147
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0492
_refine_ls_restrained_S_all      1.157
_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)+(0.1078P)²+1.8009P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1382
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.982(11)
 0.018(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb -0.500000 0.000000 -0.500000 0.0266(4) Uani 1 4 d S T P . .
Br1 Br -0.67714(11) 0.000000 -0.0582(4) 0.0344(5) Uani 1 2 d S T P . .
N1 N -0.500000 0.2122(11) -0.500000 0.047(3) Uani 1 2 d S T P . .
C1 C -0.5825(10) 0.2697(10) -0.394(4) 0.057(3) Uani 1 1 d . . . . .
H1 H -0.642762 0.231248 -0.321756 0.069 Uiso 1 1 calc R . . . .
C2 C -0.5855(8) 0.3821(10) -0.382(4) 0.054(3) Uani 1 1 d . . . . .
H2 H -0.644515 0.418264 -0.295357 0.064 Uiso 1 1 calc R . . . .
C3 C -0.500000 0.4405(12) -0.500000 0.038(3) Uani 1 2 d S T P . .


_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 Br1 2.9937(14) 5_454 ?
Pb1 Br1 2.9944(14) 1_554 ?
Pb1 Br1 2.9944(14) 5_455 ?
Pb1 Br1 2.9937(14) . ?
Pb1 N1 2.632(13) 5_454 ?
Pb1 N1 2.632(13) . ?
N1 C1 1.344(14) 2_454 ?
N1 C1 1.344(14) . ?
C1 H1 0.9500 . ?
C1 C2 1.395(17) . ?
C2 H2 0.9500 . ?
C2 C3 1.400(13) . ?
C3 C3 1.48(3) 5_464 ?

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
Br1 Pb1 Br1 180.00(3) 5_454 . ?
Br1 Pb1 Br1 89.33(4) 5_454 5_455 ?
Br1 Pb1 Br1 90.67(4) 5_454 1_554 ?
Br1 Pb1 Br1 180.00(4) 1_554 5_455 ?
Br1 Pb1 Br1 90.67(4) . 5_455 ?
Br1 Pb1 Br1 89.33(4) . 1_554 ?
N1 Pb1 Br1 90.0 . 5_455 ?
N1 Pb1 Br1 90.0 . . ?
N1 Pb1 Br1 90.0 5_454 1_554 ?
N1 Pb1 Br1 90.0 5_454 5_455 ?
N1 Pb1 Br1 90.0 . 5_454 ?
N1 Pb1 Br1 90.0 5_454 . ?
N1 Pb1 Br1 90.0 . 1_554 ?
N1 Pb1 Br1 90.0 5_454 5_454 ?
N1 Pb1 N1 180.0 . 5_454 ?
Pb1 Br1 Pb1 89.33(4) . 1_556 ?
C1 N1 Pb1 122.1(7) . . ?
C1 N1 Pb1 122.1(7) 2_454 . ?
C1 N1 C1 115.9(14) 2_454 . ?
N1 C1 H1 117.8 . . ?
N1 C1 C2 124.5(11) . . ?
C2 C1 H1 117.8 . . ?
C1 C2 H2 120.7 . . ?
C1 C2 C3 118.7(11) . . ?
C3 C2 H2 120.7 . . ?
C2 C3 C2 117.7(14) 2_454 . ?
C2 C3 C3 121.1(7) 2_454 5_464 ?
C2 C3 C3 121.1(7) . 5_464 ?

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
Pb1 N1 C1 C2 178.6(12) . . . . ?
N1 C1 C2 C3 3(2) . . . . ?
C1 N1 C1 C2 -1.4(12) 2_454 . . . ?
C1 C2 C3 C2 -1.3(10) . . . 2_454 ?
C1 C2 C3 C3 178.7(10) . . . 5_464 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.982(11)
2 0.018(11)

####################################################################### 
# 
# 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_2011145536_3_0m
_database_code_depnum_ccdc_archive 'CCDC 2101289'
loop_
_audit_author_name
_audit_author_address
'Dianxing Ju'
;Qingdao University of Science and Technology
China
;
_audit_update_record             
;
2021-08-04 deposited with the CCDC.	2022-07-31 downloaded from the CCDC.
;
_audit_creation_date             2020-11-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H8 I2 N2 Pb'
_chemical_formula_sum            'C10 H8 I2 N2 Pb'
_chemical_formula_weight         617.17
_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 0.0148 0.0070 '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 0.0969 5.4976 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.4950 6.8412 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.6647(5)
_cell_length_b                   12.4402(5)
_cell_length_c                   4.4277(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.211(3)
_cell_angle_gamma                90
_cell_volume                     692.07(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1892
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.00
_cell_measurement_theta_min      6.13
_shelx_estimated_absorpt_T_max   0.507
_shelx_estimated_absorpt_T_min   0.386
_exptl_absorpt_coefficient_mu    39.257
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.3920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 4275 reflections, Rint = 0.0977
 (2564 with I > 3sig(I), Rint = 0.0874)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.962
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            676
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.970
_diffrn_reflns_theta_min         6.129
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                596
_reflns_number_total             676
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.062
_refine_diff_density_min         -3.851
_refine_diff_density_rms         0.405
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         676
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0566
_refine_ls_restrained_S_all      1.098
_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)+(0.0751P)²+11.3371P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1505
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.996(3)
 0.004(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.500000 0.500000 0.500000 0.0357(4) Uani 1 4 d S T P . .
I1 I 0.68221(7) 0.500000 0.0613(2) 0.0402(5) Uani 1 2 d S T P . .
N1 N 0.500000 0.7143(16) 0.500000 0.059(4) Uani 1 2 d S T P . .
C3 C 0.500000 0.9418(16) 0.500000 0.043(4) Uani 1 2 d S T P . .
C2 C 0.5786(11) 0.8776(15) 0.395(4) 0.079(6) Uani 1 1 d . . . . .
H2 H 0.637631 0.912259 0.323898 0.095 Uiso 1 1 calc R . . . .
C1 C 0.5751(13) 0.7713(16) 0.388(5) 0.086(6) Uani 1 1 d . . . . .
H1 H 0.628810 0.733785 0.299146 0.103 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.1720(9) 5_665 ?
Pb1 I1 3.1976(9) . ?
Pb1 I1 3.1976(9) 5_666 ?
Pb1 I1 3.1720(9) 1_556 ?
Pb1 N1 2.67(2) . ?
Pb1 N1 2.67(2) 5_666 ?
N1 C1 1.330(19) . ?
N1 C1 1.330(19) 2_656 ?
C3 C3 1.45(4) 5_676 ?
C3 C2 1.401(18) . ?
C3 C2 1.401(18) 2_656 ?
C2 H2 0.9500 . ?
C2 C1 1.32(3) . ?
C1 H1 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 180.0 5_665 1_556 ?
I1 Pb1 I1 88.07(2) 5_665 5_666 ?
I1 Pb1 I1 91.93(2) 1_556 5_666 ?
I1 Pb1 I1 180.0 5_666 . ?
I1 Pb1 I1 91.93(2) 5_665 . ?
I1 Pb1 I1 88.07(2) 1_556 . ?
N1 Pb1 I1 90.000(1) 5_666 1_556 ?
N1 Pb1 I1 90.0 5_666 5_666 ?
N1 Pb1 I1 90.0 . 5_665 ?
N1 Pb1 I1 90.000(1) 5_666 5_665 ?
N1 Pb1 I1 90.000(1) . . ?
N1 Pb1 I1 90.0 . 1_556 ?
N1 Pb1 I1 90.000(1) . 5_666 ?
N1 Pb1 I1 90.0 5_666 . ?
N1 Pb1 N1 180.0 5_666 . ?
Pb1 I1 Pb1 88.07(2) 1_554 . ?
C1 N1 Pb1 122.2(10) . . ?
C1 N1 Pb1 122.2(10) 2_656 . ?
C1 N1 C1 116(2) 2_656 . ?
C2 C3 C3 124.8(9) . 5_676 ?
C2 C3 C3 124.8(9) 2_656 5_676 ?
C2 C3 C2 110.4(18) 2_656 . ?
C3 C2 H2 118.2 . . ?
C1 C2 C3 123.7(14) . . ?
C1 C2 H2 118.2 . . ?
N1 C1 H1 118.4 . . ?
C2 C1 N1 123.2(15) . . ?
C2 C1 H1 118.4 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.996(3)
2 0.004(3)

####################################################################### 
# 
# 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_2011145536_1
_database_code_depnum_ccdc_archive 'CCDC 2101288'
loop_
_audit_author_name
_audit_author_address
'Dianxing Ju'
;Qingdao University of Science and Technology
China
;
_audit_update_record             
;
2021-08-04 deposited with the CCDC.	2022-07-31 downloaded from the CCDC.
;
_audit_creation_date             2020-11-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H8 Cl2 N2 Pb'
_chemical_formula_sum            'C10 H8 Cl2 N2 Pb'
_chemical_formula_weight         434.27
_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 0.0148 0.0070 '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 0.3294 0.5404 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.2614 7.2057 '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                   3.9454(2)
_cell_length_b                   11.8482(13)
_cell_length_c                   12.3247(6)
_cell_angle_alpha                94.232(4)
_cell_angle_beta                 93.267(2)
_cell_angle_gamma                93.132(3)
_cell_volume                     572.62(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7632
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.89
_cell_measurement_theta_min      3.26
_shelx_estimated_absorpt_T_max   0.805
_shelx_estimated_absorpt_T_min   0.805
_exptl_absorpt_coefficient_mu    22.683
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 17540 reflections, Rint = 0.0996
 (14626 with I > 3sig(I), Rint = 0.0967)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.519
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2053
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.950
_diffrn_reflns_theta_min         3.134
_diffrn_ambient_temperature      172.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1854
_reflns_number_total             2053
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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         5.317
_refine_diff_density_min         -4.557
_refine_diff_density_rms         0.601
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2053
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.1063
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1172P)²+32.5576P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2770
_refine_ls_wR_factor_ref         0.2834
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.428(13)
 0.572(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid bond restraints
 C3, C6, C7, C8
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10)
;
_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 0.2245(3) 0.28856(9) 0.74819(9) 0.0370(5) Uani 1 1 d . . . . .
Cl1 Cl 0.691(2) 0.2670(7) 0.9135(5) 0.0431(17) Uani 1 1 d . . . . .
Cl2 Cl 0.629(2) 0.2410(6) 0.5791(6) 0.0451(17) Uani 1 1 d . . . . .
N1 N 0.156(7) 0.071(2) 0.749(2) 0.041(6) Uani 1 1 d . . . . .
N2 N -0.363(10) -0.507(3) 0.744(2) 0.063(8) Uani 1 1 d . . . . .
C1 C 0.190(9) 0.015(2) 0.839(2) 0.043(7) Uani 1 1 d . . . . .
H1 H 0.278870 0.056691 0.903821 0.052 Uiso 1 1 calc R . . . .
C2 C 0.109(10) -0.095(3) 0.843(2) 0.049(8) Uani 1 1 d . . . . .
H2 H 0.136268 -0.130903 0.909251 0.059 Uiso 1 1 calc R . . . .
C3 C -0.016(8) -0.155(2) 0.749(2) 0.037(6) Uani 1 1 d . U . . .
C4 C -0.050(9) -0.097(3) 0.656(3) 0.047(7) Uani 1 1 d . . . . .
H4 H -0.143552 -0.136294 0.589786 0.056 Uiso 1 1 calc R . . . .
C5 C 0.046(10) 0.012(3) 0.659(2) 0.047(8) Uani 1 1 d . . . . .
H5 H 0.036186 0.048481 0.592494 0.056 Uiso 1 1 calc R . . . .
C6 C -0.152(7) -0.283(2) 0.742(2) 0.033(5) Uani 1 1 d . U . . .
C7 C -0.249(7) -0.312(2) 0.840(2) 0.037(6) Uani 1 1 d . U . . .
H7 H -0.253797 -0.261106 0.903242 0.045 Uiso 1 1 calc R . . . .
C8 C -0.352(13) -0.442(3) 0.834(3) 0.066(12) Uani 1 1 d . U . . .
H8 H -0.408123 -0.475486 0.898760 0.079 Uiso 1 1 calc R . . . .
C9 C -0.233(7) -0.462(2) 0.653(3) 0.040(7) Uani 1 1 d . . . . .
H9 H -0.215407 -0.509258 0.588773 0.048 Uiso 1 1 calc R . . . .
C10 C -0.131(8) -0.351(3) 0.655(2) 0.039(6) Uani 1 1 d . U . . .
H10 H -0.041255 -0.322588 0.592182 0.047 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Cl1 2.703(8) . ?
Pb1 Cl1 3.025(7) 1_455 ?
Pb1 Cl2 2.742(8) . ?
Pb1 Cl2 3.050(8) 1_455 ?
Pb1 N1 2.57(2) . ?
N1 C1 1.33(4) . ?
N1 C5 1.32(4) . ?
N2 C8 1.30(5) . ?
N2 C9 1.38(4) . ?
C1 C2 1.34(4) . ?
C2 C3 1.36(4) . ?
C3 C4 1.38(4) . ?
C3 C6 1.58(4) . ?
C4 C5 1.33(5) . ?
C6 C7 1.35(4) . ?
C6 C10 1.30(4) . ?
C7 C8 1.57(4) . ?
C9 C10 1.35(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pb1 Cl1 86.88(17) . 1_455 ?
Cl1 Pb1 Cl2 85.0(2) 1_455 1_455 ?
Cl1 Pb1 Cl2 97.8(2) . . ?
Cl1 Pb1 Cl2 162.6(2) . 1_455 ?
Cl2 Pb1 Cl1 162.2(2) . 1_455 ?
Cl2 Pb1 Cl2 85.7(2) . 1_455 ?
N1 Pb1 Cl1 82.9(6) . . ?
N1 Pb1 Cl1 79.8(6) . 1_455 ?
N1 Pb1 Cl2 83.7(6) . . ?
N1 Pb1 Cl2 80.5(6) . 1_455 ?
Pb1 Cl1 Pb1 86.88(17) . 1_655 ?
Pb1 Cl2 Pb1 85.7(2) . 1_655 ?
C1 N1 Pb1 124.2(19) . . ?
C5 N1 Pb1 118(2) . . ?
C5 N1 C1 117(2) . . ?
C8 N2 C9 118(3) . . ?
N1 C1 C2 125(3) . . ?
C1 C2 C3 118(3) . . ?
C2 C3 C4 118(3) . . ?
C2 C3 C6 124(2) . . ?
C4 C3 C6 118(3) . . ?
C5 C4 C3 120(3) . . ?
N1 C5 C4 122(3) . . ?
C7 C6 C3 111(2) . . ?
C10 C6 C3 122(3) . . ?
C10 C6 C7 126(3) . . ?
C6 C7 C8 110(3) . . ?
N2 C8 C7 123(3) . . ?
C10 C9 N2 121(3) . . ?
C6 C10 C9 121(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.428(13)
2 0.572(13)

####################################################################### 
# 
# 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_2011145536_4_0m
_database_code_depnum_ccdc_archive 'CCDC 2101287'
loop_
_audit_author_name
_audit_author_address
'Dianxing Ju'
;Qingdao University of Science and Technology
China
;
_audit_update_record             
;
2021-08-04 deposited with the CCDC.	2022-07-31 downloaded from the CCDC.
;
_audit_creation_date             2020-11-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C20 H16 I4 N4 Pb2)'
_chemical_formula_sum            'C10 H8 I2 N2 Pb'
_chemical_formula_weight         617.17
_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 0.0148 0.0070 '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 0.0969 5.4976 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.4950 6.8412 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.3113(13)
_cell_length_b                   10.3816(7)
_cell_length_c                   8.2206(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.375(3)
_cell_angle_gamma                90
_cell_volume                     1359.71(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1665
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.73
_cell_measurement_theta_min      8.16
_shelx_estimated_absorpt_T_max   0.240
_shelx_estimated_absorpt_T_min   0.198
_exptl_absorpt_coefficient_mu    39.963
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.1353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1717 before and 0.0982 after correction. The Ratio of minimum to maximum transmission is 0.1802. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.015
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6716
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.902
_diffrn_reflns_theta_min         6.133
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1190
_reflns_number_total             1244
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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         4.438
_refine_diff_density_min         -3.373
_refine_diff_density_rms         0.432
_refine_ls_extinction_coef       0.00056(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1244
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0461
_refine_ls_restrained_S_all      1.044
_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)+(0.0686P)²+2.5246P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1119
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C5 \\sim N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.01
Uanis(C5) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C3(H3), C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.500000 0.92475(5) 0.250000 0.0105(3) Uani 1 2 d S T P . .
I1 I 0.62771(3) 0.88214(7) 0.00856(6) 0.0188(3) Uani 1 1 d . . . . .
N1 N 0.4344(4) 0.7198(8) 0.1185(8) 0.0115(12) Uani 1 1 d . U . . .
C5 C 0.4626(4) 0.6050(9) 0.1811(9) 0.0096(13) Uani 1 1 d . U . . .
C2 C 0.3241(5) 0.6165(10) -0.0774(11) 0.0220(15) Uani 1 1 d . U . . .
H2 H 0.276044 0.622844 -0.165725 0.026 Uiso 1 1 calc R . . . .
C4 C 0.4236(5) 0.4914(9) 0.1148(9) 0.0174(14) Uani 1 1 d . U . . .
H4 H 0.444477 0.410036 0.157718 0.021 Uiso 1 1 calc R . . . .
C3 C 0.3540(5) 0.4994(10) -0.0146(10) 0.0200(15) Uani 1 1 d . U . . .
H3 H 0.326543 0.422786 -0.060355 0.024 Uiso 1 1 calc R . . . .
C1 C 0.3664(5) 0.7247(11) -0.0079(10) 0.0177(14) Uani 1 1 d . U . . .
H1 H 0.346790 0.806641 -0.051053 0.021 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.2010(5) 2_655 ?
Pb1 I1 3.2010(5) . ?
Pb1 I1 3.3133(6) 5_675 ?
Pb1 I1 3.3133(6) 6_576 ?
Pb1 N1 2.519(7) 2_655 ?
Pb1 N1 2.519(7) . ?
N1 C5 1.340(12) . ?
N1 C1 1.349(10) . ?
C5 C5 1.476(14) 2_655 ?
C5 C4 1.395(12) . ?
C2 H2 0.9500 . ?
C2 C3 1.369(14) . ?
C2 C1 1.377(14) . ?
C4 H4 0.9500 . ?
C4 C3 1.382(12) . ?
C3 H3 0.9500 . ?
C1 H1 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 164.11(3) 2_655 . ?
I1 Pb1 I1 94.484(16) 2_655 5_675 ?
I1 Pb1 I1 94.484(16) . 6_576 ?
I1 Pb1 I1 105.53(2) 6_576 5_675 ?
I1 Pb1 I1 95.109(14) . 5_675 ?
I1 Pb1 I1 95.109(14) 2_655 6_576 ?
N1 Pb1 I1 94.87(16) . 5_675 ?
N1 Pb1 I1 83.70(14) 2_655 2_655 ?
N1 Pb1 I1 82.89(14) 2_655 . ?
N1 Pb1 I1 83.70(14) . . ?
N1 Pb1 I1 159.60(16) 2_655 5_675 ?
N1 Pb1 I1 159.59(16) . 6_576 ?
N1 Pb1 I1 94.87(16) 2_655 6_576 ?
N1 Pb1 I1 82.89(14) . 2_655 ?
N1 Pb1 N1 64.7(3) 2_655 . ?
Pb1 I1 Pb1 84.890(14) . 5_675 ?
C5 N1 Pb1 120.5(5) . . ?
C5 N1 C1 119.2(8) . . ?
C1 N1 Pb1 120.2(6) . . ?
N1 C5 C5 117.0(4) . 2_655 ?
N1 C5 C4 120.8(6) . . ?
C4 C5 C5 122.2(5) . 2_655 ?
C3 C2 H2 121.2 . . ?
C3 C2 C1 117.5(8) . . ?
C1 C2 H2 121.2 . . ?
C5 C4 H4 120.6 . . ?
C3 C4 C5 118.7(9) . . ?
C3 C4 H4 120.6 . . ?
C2 C3 C4 120.7(9) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
N1 C1 C2 123.0(9) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
