# Supplementary Information (SI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_(DMP)PbBr3_333K
_database_code_depnum_ccdc_archive 'CCDC 2366481'
loop_
_audit_author_name
_audit_author_address
'zhilong li'
;southeast university
China
;
_audit_update_record             
;
2024-07-25 deposited with the CCDC.	2024-08-04 downloaded from the CCDC.
;
_audit_creation_date             2024-06-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb1, 2(C3 N0.5)'
_chemical_formula_sum            'C6 Br3 N Pb'
_chemical_formula_weight         532.99
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-y, -x, -z+1/2'
'x-y, -y, -z'
'x, x-y, -z+1/2'
'y, x, -z'
'-x+y, y, -z+1/2'
'-x, -x+y, -z'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'y, x, z-1/2'
'-x+y, y, z'
'-x, -x+y, z-1/2'
'-y, -x, z'
'x-y, -y, z-1/2'
'x, x-y, z'

_cell_length_a                   9.613
_cell_length_b                   9.613
_cell_length_c                   7.840
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     627.4
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1695
_cell_measurement_temperature    333.0
_cell_measurement_theta_max      19.47
_cell_measurement_theta_min      2.45
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.947
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.3782
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1286 before and 0.0683 after correction.
The Ratio of minimum to maximum transmission is 0.5074.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.821
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1724
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11236
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.941
_diffrn_reflns_theta_max         24.941
_diffrn_reflns_theta_min         2.446
_diffrn_ambient_temperature      333.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                171
_reflns_number_total             240
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     19
_refine_ls_number_reflns         240
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0432
_refine_ls_restrained_S_all      0.977
_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)+(0.0450P)²+6.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1211
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.006 and sigma for
terminal atoms of 0.006
2. Others
 Fixed Sof: C2(0.25) N1(0.08333)
 Fixed X: C1(0.13811)
 Fixed Y: C1(-0.43094)
 Fixed Z: C1(0.75)
;
_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 0.000000 0.000000 1.000000 0.1032(8) Uani 1 12 d S T P . .
Br1 Br -0.13882(19) -0.2776(4) 0.750000 0.1493(14) Uani 1 4 d S T P . .
C2 C 0.247(8) -0.376(4) 0.959(7) 0.256(13) Uani 0.5 2 d S TU P . .
C1 C 0.138110 -0.430940 0.750000 0.626(14) Uani 1 4 d S TU P . .
N1 N 0.333333 -0.333333 0.803(5) 0.120(18) Uani 0.5 6 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 3.030(2) 14_557 ?
Pb1 Br1 3.030(2) 3 ?
Pb1 Br1 3.030(2) 15_557 ?
Pb1 Br1 3.030(2) 2 ?
Pb1 Br1 3.030(2) . ?
Pb1 Br1 3.030(2) 13_557 ?
C2 C2 1.24(12) 5_655 ?
C2 C2 1.24(12) 3_545 ?
C2 C1 1.87(6) . ?
C2 N1 1.41(6) . ?
C1 N1 1.678(9) 14_657 ?
C1 N1 1.678(9) . ?
N1 N1 0.84(7) 14_657 ?

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 180.0 14_557 2 ?
Br1 Pb1 Br1 97.32(6) . 15_557 ?
Br1 Pb1 Br1 97.32(6) 13_557 3 ?
Br1 Pb1 Br1 82.68(6) 14_557 . ?
Br1 Pb1 Br1 82.68(6) 14_557 3 ?
Br1 Pb1 Br1 97.32(6) 2 . ?
Br1 Pb1 Br1 82.68(6) 2 15_557 ?
Br1 Pb1 Br1 97.32(6) 14_557 13_557 ?
Br1 Pb1 Br1 82.68(6) 13_557 15_557 ?
Br1 Pb1 Br1 82.68(6) 2 13_557 ?
Br1 Pb1 Br1 97.32(6) 2 3 ?
Br1 Pb1 Br1 180.0 . 13_557 ?
Br1 Pb1 Br1 180.0 15_557 3 ?
Br1 Pb1 Br1 97.32(6) 14_557 15_557 ?
Br1 Pb1 Br1 82.68(6) . 3 ?
Pb1 Br1 Pb1 80.60(8) . 2_554 ?
C2 C2 C2 60.00(2) 3_545 5_655 ?
C2 C2 C1 114.8(17) 3_545 . ?
C2 C2 C1 114.8(17) 5_655 . ?
C2 C2 N1 64(2) 3_545 . ?
C2 C2 N1 64(2) 5_655 . ?
N1 C2 C1 59(2) . . ?
C2 C1 C2 122(4) 16_557 . ?
N1 C1 C2 75(3) 14_657 . ?
N1 C1 C2 47(2) . . ?
N1 C1 C2 75(3) . 16_557 ?
N1 C1 C2 47(2) 14_657 16_557 ?
N1 C1 N1 29(2) . 14_657 ?
C2 N1 C2 52(5) 5_655 3_545 ?
C2 N1 C2 52(5) 5_655 . ?
C2 N1 C2 52(5) . 3_545 ?
C2 N1 C1 117.4(16) 3_545 14_657 ?
C2 N1 C1 74(3) 5_655 14_657 ?
C2 N1 C1 117.4(16) . 14_657 ?
C2 N1 C1 117.4(16) . 3_545 ?
C2 N1 C1 117.4(16) 5_655 3_545 ?
C2 N1 C1 117.4(16) 5_655 . ?
C2 N1 C1 74(3) 3_545 3_545 ?
C2 N1 C1 74(3) . . ?
C2 N1 C1 117.4(16) 3_545 . ?
C1 N1 C1 114.0(10) 14_657 3_545 ?
C1 N1 C1 114.0(10) . 3_545 ?
C1 N1 C1 114.0(10) . 14_657 ?
N1 N1 C2 150(3) 14_657 3_545 ?
N1 N1 C2 150(3) 14_657 5_655 ?
N1 N1 C2 150(3) 14_657 . ?
N1 N1 C1 75.6(12) 14_657 14_657 ?
N1 N1 C1 75.6(12) 14_657 3_545 ?
N1 N1 C1 75.6(12) 14_657 . ?

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
C2 C2 C1 C2 33.4(5) 5_655 . . 16_557 ?
C2 C2 C1 C2 -33.4(5) 3_545 . . 16_557 ?
C2 C2 C1 N1 -33.4(5) 3_545 . . . ?
C2 C2 C1 N1 33.4(5) 5_655 . . . ?
C2 C2 C1 N1 -33.4(5) 3_545 . . 14_657 ?
C2 C2 C1 N1 33.4(5) 5_655 . . 14_657 ?
C2 C2 N1 C2 67.6(15) 5_655 . . 3_545 ?
C2 C2 N1 C2 -67.6(15) 3_545 . . 5_655 ?
C2 C2 N1 C1 146.2(8) 3_545 . . . ?
C2 C2 N1 C1 105(2) 5_655 . . 3_545 ?
C2 C2 N1 C1 37.0(11) 3_545 . . 3_545 ?
C2 C2 N1 C1 -105(2) 3_545 . . 14_657 ?
C2 C2 N1 C1 -37.0(11) 5_655 . . 14_657 ?
C2 C2 N1 C1 -146.2(8) 5_655 . . . ?
C2 C2 N1 N1 -146.2(8) 5_655 . . 14_657 ?
C2 C2 N1 N1 146.2(8) 3_545 . . 14_657 ?
C2 C1 N1 C2 30(3) . . . 3_545 ?
C2 C1 N1 C2 -150(3) 16_557 . . 3_545 ?
C2 C1 N1 C2 150(3) 16_557 . . 5_655 ?
C2 C1 N1 C2 180.001(7) 16_557 . . . ?
C2 C1 N1 C2 -30(3) . . . 5_655 ?
C2 C1 N1 C1 -113.3(17) . . . 14_657 ?
C2 C1 N1 C1 66.7(17) 16_557 . . 14_657 ?
C2 C1 N1 C1 113.3(17) . . . 3_545 ?
C2 C1 N1 C1 -66.7(17) 16_557 . . 3_545 ?
C2 C1 N1 N1 0.000(5) 16_557 . . 14_657 ?
C2 C1 N1 N1 179.999(9) . . . 14_657 ?
C1 C2 N1 C2 146.2(8) . . . 5_655 ?
C1 C2 N1 C2 -146.2(8) . . . 3_545 ?
C1 C2 N1 C1 109.2(18) . . . 14_657 ?
C1 C2 N1 C1 -109.2(17) . . . 3_545 ?
C1 C2 N1 N1 -0.002(18) . . . 14_657 ?
N1 C2 C1 C2 0.001(9) . . . 16_557 ?
N1 C2 C1 N1 0.000(7) . . . 14_657 ?
N1 C1 N1 C2 -150(3) 14_657 . . 3_545 ?
N1 C1 N1 C2 150(3) 14_657 . . 5_655 ?
N1 C1 N1 C2 180.001(8) 14_657 . . . ?
N1 C1 N1 C1 66.7(17) 14_657 . . 14_657 ?
N1 C1 N1 C1 -66.7(17) 14_657 . . 3_545 ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT260_DMPPbBr3_333K       
;
PROBLEM: Large Average Ueq of Residue Including        N1      0.334 Check 
RESPONSE:  It could be due to disorder
;
# end Validation Reply Form
####################################################################### 
# 
# 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_(EMP)PbBr3_423K
_database_code_depnum_ccdc_archive 'CCDC 2366486'
loop_
_audit_author_name
_audit_author_address
'zhilong li'
;Southeast University
China
;
_audit_update_record             
;
2024-06-28 deposited with the CCDC.	2024-08-04 downloaded from the CCDC.
;
_audit_creation_date             2024-06-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb1, 2(C3.499 N0.5)'
_chemical_formula_sum            'C7 Br3 N Pb'
_chemical_formula_weight         545.00
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   10.073
_cell_length_b                   10.073
_cell_length_c                   7.910
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     695.0
_cell_formula_units_Z            2
_cell_measurement_reflns_used    694
_cell_measurement_temperature    423.0
_cell_measurement_theta_max      12.82
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.719
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.2701
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1918 before and 0.0895 after correction.
The Ratio of minimum to maximum transmission is 0.3625.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.604
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             472
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2449
_diffrn_reflns_av_unetI/netI     0.1215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11673
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.335
_diffrn_ambient_temperature      423.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                95
_reflns_number_total             273
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.025(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     23
_refine_ls_number_reflns         273
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0457
_refine_ls_restrained_S_all      0.934
_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)+(0.0526P)²+0.9687P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1697
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: -9(10)
 10(10)
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Fixed Sof: C1(0.2916) C2(0.2916)
;
_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 1.000000 1.000000 0.500000 0.212(2) Uani 1 12 d S TU P . .
Br1 Br 0.8674(2) 0.7347(4) 0.250000 0.287(3) Uani 1 4 d S TU P . .
N1 N 1.333333 0.666667 0.250000 0.361(12) Uani 1 12 d S TU P . .
C1 C 1.404(5) 0.808(9) 0.409(6) 0.38(2) Uani 0.5832 2 d S TU P . .
C2 C 1.381(5) 0.762(9) 0.534(5) 0.39(3) Uani 0.5832 2 d S TU 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 3.044(3) 13_776 ?
Pb1 Br1 3.044(3) 14_566 ?
Pb1 Br1 3.044(3) 2_765 ?
Pb1 Br1 3.044(3) 15_656 ?
Pb1 Br1 3.044(3) 3_675 ?
Pb1 Br1 3.044(3) . ?
N1 C1 1.76(6) . ?
N1 C1 1.76(6) 3_775 ?
N1 C1 1.76(6) 18_776 ?
N1 C1 1.76(6) 16_556 ?
N1 C1 1.76(6) 2_755 ?
N1 C1 1.76(6) 17_756 ?
C1 C2 1.07(7) . ?
C2 C2 1.44(14) 3_775 ?
C2 C2 1.44(14) 2_755 ?

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 82.35(7) 13_776 15_656 ?
Br1 Pb1 Br1 97.65(7) 3_675 14_566 ?
Br1 Pb1 Br1 82.35(7) 3_675 . ?
Br1 Pb1 Br1 97.65(7) 13_776 3_675 ?
Br1 Pb1 Br1 180.0 13_776 . ?
Br1 Pb1 Br1 180.0 15_656 3_675 ?
Br1 Pb1 Br1 82.35(7) 15_656 14_566 ?
Br1 Pb1 Br1 97.65(7) 13_776 2_765 ?
Br1 Pb1 Br1 180.0 2_765 14_566 ?
Br1 Pb1 Br1 97.65(7) 15_656 2_765 ?
Br1 Pb1 Br1 97.65(7) 15_656 . ?
Br1 Pb1 Br1 82.35(7) 3_675 2_765 ?
Br1 Pb1 Br1 82.35(7) 2_765 . ?
Br1 Pb1 Br1 82.35(7) 13_776 14_566 ?
Br1 Pb1 Br1 97.65(7) 14_566 . ?
Pb1 Br1 Pb1 81.04(9) . 4_774 ?
C1 N1 C1 75(3) 16_556 18_776 ?
C1 N1 C1 139.0(17) 16_556 3_775 ?
C1 N1 C1 139.0(17) . 17_756 ?
C1 N1 C1 75(3) . 3_775 ?
C1 N1 C1 75(3) 17_756 16_556 ?
C1 N1 C1 91(4) 18_776 3_775 ?
C1 N1 C1 75(3) . 2_755 ?
C1 N1 C1 139.0(17) 2_755 18_776 ?
C1 N1 C1 91(4) 17_756 2_755 ?
C1 N1 C1 139.0(17) 17_756 3_775 ?
C1 N1 C1 139.0(17) 16_556 2_755 ?
C1 N1 C1 75(3) 2_755 3_775 ?
C1 N1 C1 139.0(17) . 18_776 ?
C1 N1 C1 75(3) 17_756 18_776 ?
C1 N1 C1 91(4) . 16_556 ?
C2 C1 N1 114(8) . . ?
C1 C2 C2 109(6) . 3_775 ?
C1 C2 C2 109(6) . 2_755 ?
C2 C2 C2 60.000(5) 2_755 3_775 ?

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
N1 C1 C2 C2 31.9(12) . . . 3_775 ?
N1 C1 C2 C2 -31.9(12) . . . 2_755 ?
C1 N1 C1 C2 -38.9(10) 3_775 . . . ?
C1 N1 C1 C2 180.000(16) 16_556 . . . ?
C1 N1 C1 C2 112.4(8) 17_756 . . . ?
C1 N1 C1 C2 38.9(11) 2_755 . . . ?
C1 N1 C1 C2 -112.4(8) 18_776 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 -9(10)
2 10(10)
# start Validation Reply Form
_vrf_RINTA01_EMPPbBr3_423K       
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The high Rint value is caused by the poor crystal data quality.
;
_vrf_PLAT260_EMPPbBr3_423K       
;
PROBLEM: Large Average Ueq of Residue Including        C1      0.385 Check 
RESPONSE: It could be due to disorder.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_(DMP)PbBr3_300K
_database_code_depnum_ccdc_archive 'CCDC 2366482'
loop_
_audit_author_name
_audit_author_address
'zhilong li'
;Southeast University
China
;
_audit_update_record             
;
2024-06-28 deposited with the CCDC.	2024-08-04 downloaded from the CCDC.
;
_audit_creation_date             2024-06-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C6 H12 N'
_chemical_formula_sum            'C6 H12 Br3 N Pb'
_chemical_formula_weight         545.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N Pb Br'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.6477(10)
_cell_length_b                   7.9361(7)
_cell_length_c                   16.0202(19)
_cell_angle_alpha                90
_cell_angle_beta                 92.416(9)
_cell_angle_gamma                90
_cell_volume                     1225.5(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3122
_cell_measurement_temperature    300.91(10)
_cell_measurement_theta_max      27.8810
_cell_measurement_theta_min      2.4150
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.499
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.954
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9017
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.420
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.91(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -2.00  36.00   0.50    1.00    --    4.83 -99.00 -60.00   76
  2  ω    -55.00  17.00   0.50    1.00    --    4.83 -23.00 -24.00  144
  3  ω     -7.00  64.00   0.50    1.00    --    4.83  38.00   0.00  142
  4  ω      2.00  50.00   0.50    1.00    --    4.83  23.00 140.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0628631000
_diffrn_orient_matrix_UB_12      0.0150011000
_diffrn_orient_matrix_UB_13      0.0202280000
_diffrn_orient_matrix_UB_21      -0.0325743000
_diffrn_orient_matrix_UB_22      0.0235515000
_diffrn_orient_matrix_UB_23      -0.0387625000
_diffrn_orient_matrix_UB_31      -0.0201832000
_diffrn_orient_matrix_UB_32      -0.0848592000
_diffrn_orient_matrix_UB_33      -0.0072007000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1972
_reflns_number_total             2737
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         4.753
_refine_diff_density_min         -2.786
_refine_diff_density_rms         0.383
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2737
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0748
_refine_ls_restrained_S_all      1.087
_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)+(0.1220P)²+0.9465P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1932
_refine_ls_wR_factor_ref         0.2076
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C5
 1.38 with sigma of 0.01
 C3-C4
 1.45 with sigma of 0.01
 N1-C6
 1.51 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C3(H3A,H3B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4)
4.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb -0.25118(6) 0.04262(7) 0.75171(4) 0.0390(3) Uani 1 1 d . . . . .
Br1 Br -0.05539(18) -0.1606(2) 0.66746(11) 0.0464(4) Uani 1 1 d . . . . .
Br3 Br -0.2869(2) 0.2761(2) 0.60787(11) 0.0498(5) Uani 1 1 d . . . . .
Br2 Br -0.03490(19) 0.2694(2) 0.81897(13) 0.0530(5) Uani 1 1 d . . . . .
N1 N 0.2559(13) 0.2150(16) 0.5908(9) 0.046(3) Uani 1 1 d D . . . .
C5 C 0.0947(18) 0.432(2) 0.5942(12) 0.058(5) Uani 1 1 d D . . . .
H5 H 0.012099 0.486613 0.604877 0.069 Uiso 1 1 calc R U . . .
C6 C 0.1039(15) 0.254(2) 0.5785(14) 0.063(5) Uani 1 1 d D . . . .
H6A H 0.071025 0.227241 0.522017 0.076 Uiso 1 1 calc R U . . .
H6B H 0.049928 0.190564 0.617505 0.076 Uiso 1 1 calc R U . . .
C4 C 0.2199(17) 0.512(2) 0.5919(14) 0.070(6) Uani 1 1 d D . . . .
H4 H 0.235107 0.627301 0.597727 0.084 Uiso 1 1 calc R U . . .
C2 C 0.280(3) 0.159(3) 0.6788(14) 0.083(7) Uani 1 1 d . . . . .
H2A H 0.263906 0.251079 0.715879 0.125 Uiso 1 1 calc R U . . .
H2B H 0.374738 0.121488 0.686950 0.125 Uiso 1 1 calc R U . . .
H2C H 0.218717 0.067776 0.690422 0.125 Uiso 1 1 calc R U . . .
C1 C 0.295(3) 0.078(3) 0.5360(16) 0.095(8) Uani 1 1 d . U . . .
H1A H 0.262738 -0.027068 0.557631 0.142 Uiso 1 1 calc R U . . .
H1B H 0.394295 0.074626 0.533181 0.142 Uiso 1 1 calc R U . . .
H1C H 0.254200 0.096065 0.481069 0.142 Uiso 1 1 calc R U . . .
C3 C 0.325(2) 0.384(3) 0.5788(19) 0.099(9) Uani 1 1 d D . . . .
H3A H 0.402390 0.398357 0.618651 0.119 Uiso 1 1 calc R U . . .
H3B H 0.358663 0.393157 0.522824 0.119 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.8648(17) . ?
Pb1 Br1 3.3028(17) 2_456 ?
Pb1 Br3 3.0982(19) 2_446 ?
Pb1 Br3 2.9659(18) . ?
Pb1 Br2 2.9264(19) . ?
Pb1 Br2 3.1698(19) 2_446 ?
N1 C6 1.503(9) . ?
N1 C2 1.49(2) . ?
N1 C1 1.46(2) . ?
N1 C3 1.52(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.44(2) . ?
C5 C4 1.367(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C4 H4 0.9300 . ?
C4 C3 1.454(10) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 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
Br1 Pb1 Br1 168.78(5) . 2_456 ?
Br1 Pb1 Br3 92.48(5) . . ?
Br1 Pb1 Br3 84.10(5) . 2_446 ?
Br1 Pb1 Br2 83.04(5) . 2_446 ?
Br1 Pb1 Br2 92.61(5) . . ?
Br3 Pb1 Br1 79.05(5) . 2_456 ?
Br3 Pb1 Br1 104.70(5) 2_446 2_456 ?
Br3 Pb1 Br3 175.58(5) . 2_446 ?
Br3 Pb1 Br2 95.58(5) . 2_446 ?
Br3 Pb1 Br2 81.25(5) 2_446 2_446 ?
Br2 Pb1 Br1 79.81(5) . 2_456 ?
Br2 Pb1 Br1 104.93(5) 2_446 2_456 ?
Br2 Pb1 Br3 95.24(6) . 2_446 ?
Br2 Pb1 Br3 87.69(6) . . ?
Br2 Pb1 Br2 174.66(5) . 2_446 ?
Pb1 Br3 Pb1 81.72(4) . 2_456 ?
Pb1 Br2 Pb1 81.13(4) . 2_456 ?
C6 N1 C3 103.4(13) . . ?
C2 N1 C6 107.5(16) . . ?
C2 N1 C3 109.5(18) . . ?
C1 N1 C6 110.5(16) . . ?
C1 N1 C2 108.2(16) . . ?
C1 N1 C3 117.3(18) . . ?
C6 C5 H5 123.5 . . ?
C4 C5 H5 123.5 . . ?
C4 C5 C6 113.1(16) . . ?
N1 C6 H6A 110.9 . . ?
N1 C6 H6B 110.9 . . ?
C5 C6 N1 104.2(13) . . ?
C5 C6 H6A 110.9 . . ?
C5 C6 H6B 110.9 . . ?
H6A C6 H6B 108.9 . . ?
C5 C4 H4 126.3 . . ?
C5 C4 C3 107.4(18) . . ?
C3 C4 H4 126.3 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C3 H3A 110.4 . . ?
N1 C3 H3B 110.4 . . ?
C4 C3 N1 106.8(17) . . ?
C4 C3 H3A 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?

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
C5 C4 C3 N1 -11(3) . . . . ?
C6 N1 C3 C4 21(3) . . . . ?
C6 C5 C4 C3 -3(3) . . . . ?
C4 C5 C6 N1 17(2) . . . . ?
C2 N1 C6 C5 93.9(19) . . . . ?
C2 N1 C3 C4 -94(2) . . . . ?
C1 N1 C6 C5 -148.2(18) . . . . ?
C1 N1 C3 C4 142(2) . . . . ?
C3 N1 C6 C5 -22(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 24.839
_oxdiff_exptl_absorpt_empirical_full_min 0.445
# start Validation Reply Form
_vrf_PLAT971_DMPPbBr3_300K       
;
PROBLEM: Check Calcd Resid. Dens.  1.13Ang From Pb1             4.49 eA-3  
RESPONSE:This density residual is very close to the heavy metal that 
has a high electron density.
;
_vrf_PLAT342_DMPPbBr3_300K       
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02333 Ang.  
RESPONSE: The quality of this crystal was poor.
;
_vrf_PLAT972_DMPPbBr3_300K       
;
PROBLEM: Check Calcd Resid. Dens.  0.99Ang From Pb1            -2.64 eA-3  
RESPONSE: This density residual is very close to the heavy metal that 
has a high electron density.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_(DMP)PbBr3_303Kcooling
_database_code_depnum_ccdc_archive 'CCDC 2366483'
loop_
_audit_author_name
_audit_author_address
'zhilong li'
;southeast university
China
;
_audit_update_record             
;
2024-07-25 deposited with the CCDC.	2024-08-04 downloaded from the CCDC.
;
_audit_creation_date             2024-03-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb1, 2(C3 N0.5)'
_chemical_formula_sum            'C6 Br3 N Pb'
_chemical_formula_weight         532.99
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-y, -x, -z+1/2'
'x-y, -y, -z'
'x, x-y, -z+1/2'
'y, x, -z'
'-x+y, y, -z+1/2'
'-x, -x+y, -z'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'y, x, z-1/2'
'-x+y, y, z'
'-x, -x+y, z-1/2'
'-y, -x, z'
'x-y, -y, z-1/2'
'x, x-y, z'

_cell_length_a                   9.503
_cell_length_b                   9.503
_cell_length_c                   7.812
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     611.0
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1346
_cell_measurement_temperature    303.0
_cell_measurement_theta_max      21.99
_cell_measurement_theta_min      4.93
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.566
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3660
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1226 before and 0.0613 after correction.
The Ratio of minimum to maximum transmission is 0.4911.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.897
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.3367
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_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       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7184
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        24.951
_diffrn_reflns_theta_max         24.951
_diffrn_reflns_theta_min         3.596
_diffrn_ambient_temperature      303.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                193
_reflns_number_total             229
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.629
_refine_diff_density_min         -3.584
_refine_diff_density_rms         0.419
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         229
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1879
_refine_ls_R_factor_gt           0.1735
_refine_ls_restrained_S_all      1.024
_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)+(0.0010P)²+130.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3366
_refine_ls_wR_factor_ref         0.3415
_refine_special_details          ?
_olex2_refinement_description    
;
1. Rigid body (RIGU) restrains
 N1, C1, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
2. Others
 Fixed Sof: C1(0.25) C2(0.25)
 Fixed U11: N1(0.036057) C1(0.036733) C2(0.03426)
 Fixed U12: N1(-0.000006) C1(-0.011697) C2(0.004307)
 Fixed U13: N1(0) C1(0.006859) C2(0)
 Fixed U22: N1(0.03605) C1(0.05024) C2(0.08026)
 Fixed U23: N1(0) C1(0.00396) C2(0)
 Fixed U33: N1(0.03851) C1(0.02854) C2(0.02889)
 Fixed X: N1(0.66667) C1(0.557281) C2(0.50556)
 Fixed Y: N1(0.33333) C1(0.27864) C2(0.361961)
 Fixed Z: N1(0.25) C1(0.118281) C2(0.25)
;
_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 0.000000 0.000000 0.000000 0.088(3) Uani 1 12 d S T P . .
Br1 Br 0.1384(6) 0.2767(13) 0.250000 0.147(5) Uani 1 4 d S T P . .
N1 N 0.666670 0.333330 0.250000 0.037 Uani 1 12 d S T P . .
C1 C 0.557281 0.278640 0.118281 0.039 Uani 0.5 2 d S T P . .
C2 C 0.505560 0.361961 0.250000 0.048 Uani 0.5 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 3.000(8) . ?
Pb1 Br1 3.000(8) 15 ?
Pb1 Br1 3.000(8) 2_554 ?
Pb1 Br1 3.000(8) 13 ?
Pb1 Br1 3.000(8) 14_556 ?
Pb1 Br1 3.000(8) 3 ?
N1 C1 1.3672 18_656 ?
N1 C1 1.3672 5_665 ?
N1 C1 1.3672 14_666 ?
N1 C1 1.3672 3_655 ?
N1 C1 1.3672 . ?
N1 C1 1.3672 16_556 ?
N1 C2 1.6835 3_655 ?
N1 C2 1.6836 7_665 ?
N1 C2 1.6836 14_666 ?
N1 C2 1.6835 20_655 ?
N1 C2 1.6836 9 ?
N1 C2 1.6836 . ?
C1 C1 1.5592 5_665 ?
C1 C1 1.5592 3_655 ?
C1 C2 1.5220 . ?
C1 C2 1.5220 9 ?
C2 C2 1.2589 7_665 ?

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 180.0 . 13 ?
Br1 Pb1 Br1 97.8(2) 14_556 15 ?
Br1 Pb1 Br1 82.2(2) 14_556 3 ?
Br1 Pb1 Br1 82.2(2) . 14_556 ?
Br1 Pb1 Br1 82.2(2) . 3 ?
Br1 Pb1 Br1 97.8(2) 13 14_556 ?
Br1 Pb1 Br1 82.2(2) 13 15 ?
Br1 Pb1 Br1 97.8(2) . 2_554 ?
Br1 Pb1 Br1 82.2(2) 2_554 15 ?
Br1 Pb1 Br1 82.2(2) 13 2_554 ?
Br1 Pb1 Br1 97.8(2) 13 3 ?
Br1 Pb1 Br1 180.0 14_556 2_554 ?
Br1 Pb1 Br1 97.8(2) 2_554 3 ?
Br1 Pb1 Br1 97.8(2) . 15 ?
Br1 Pb1 Br1 180.0 15 3 ?
Pb1 Br1 Pb1 81.2(3) . 2 ?
C1 N1 C1 69.5 3_655 5_665 ?
C1 N1 C1 141.6 3_655 16_556 ?
C1 N1 C1 97.6 18_656 3_655 ?
C1 N1 C1 97.6 14_666 5_665 ?
C1 N1 C1 141.6 18_656 . ?
C1 N1 C1 69.5 14_666 16_556 ?
C1 N1 C1 69.5 3_655 . ?
C1 N1 C1 69.5 . 5_665 ?
C1 N1 C1 69.5 18_656 14_666 ?
C1 N1 C1 69.5 18_656 16_556 ?
C1 N1 C1 141.6 3_655 14_666 ?
C1 N1 C1 97.6 . 16_556 ?
C1 N1 C1 141.6 . 14_666 ?
C1 N1 C1 141.6 18_656 5_665 ?
C1 N1 C1 141.6 5_665 16_556 ?
C1 N1 C2 58.8 . . ?
C1 N1 C2 58.8 16_556 9 ?
C1 N1 C2 127.6 3_655 7_665 ?
C1 N1 C2 84.7 5_665 . ?
C1 N1 C2 58.8 14_666 14_666 ?
C1 N1 C2 84.7 . 3_655 ?
C1 N1 C2 84.7 16_556 7_665 ?
C1 N1 C2 127.6 14_666 3_655 ?
C1 N1 C2 84.7 3_655 14_666 ?
C1 N1 C2 127.6 5_665 3_655 ?
C1 N1 C2 127.6 16_556 14_666 ?
C1 N1 C2 84.7 16_556 3_655 ?
C1 N1 C2 58.8 14_666 7_665 ?
C1 N1 C2 58.8 18_656 20_655 ?
C1 N1 C2 127.6 3_655 . ?
C1 N1 C2 58.8 3_655 20_655 ?
C1 N1 C2 84.7 18_656 14_666 ?
C1 N1 C2 127.6 . 20_655 ?
C1 N1 C2 127.6 . 14_666 ?
C1 N1 C2 84.7 14_666 20_655 ?
C1 N1 C2 58.8 5_665 14_666 ?
C1 N1 C2 84.7 5_665 20_655 ?
C1 N1 C2 127.6 18_656 7_665 ?
C1 N1 C2 127.6 16_556 20_655 ?
C1 N1 C2 84.7 . 7_665 ?
C1 N1 C2 84.7 18_656 9 ?
C1 N1 C2 58.8 5_665 7_665 ?
C1 N1 C2 84.7 3_655 9 ?
C1 N1 C2 127.6 18_656 . ?
C1 N1 C2 58.8 . 9 ?
C1 N1 C2 127.6 14_666 9 ?
C1 N1 C2 84.7 14_666 . ?
C1 N1 C2 58.8 18_656 3_655 ?
C1 N1 C2 58.8 16_556 . ?
C1 N1 C2 58.8 3_655 3_655 ?
C1 N1 C2 127.6 5_665 9 ?
C2 N1 C2 163.9 3_655 7_665 ?
C2 N1 C2 120.0 3_655 . ?
C2 N1 C2 43.9 7_665 . ?
C2 N1 C2 120.0 20_655 7_665 ?
C2 N1 C2 76.1 9 . ?
C2 N1 C2 120.0 9 7_665 ?
C2 N1 C2 76.1 3_655 20_655 ?
C2 N1 C2 76.1 14_666 7_665 ?
C2 N1 C2 163.9 20_655 . ?
C2 N1 C2 163.9 9 14_666 ?
C2 N1 C2 120.0 14_666 . ?
C2 N1 C2 43.9 3_655 9 ?
C2 N1 C2 43.9 20_655 14_666 ?
C2 N1 C2 120.0 20_655 9 ?
C2 N1 C2 120.0 3_655 14_666 ?
N1 C1 C1 55.2 . 5_665 ?
N1 C1 C1 55.2 . 3_655 ?
N1 C1 C2 71.1 . . ?
N1 C1 C2 71.1 . 9 ?
C1 C1 C1 60.0 3_655 5_665 ?
C2 C1 C1 125.7 . 3_655 ?
C2 C1 C1 84.3 9 3_655 ?
C2 C1 C1 125.7 9 5_665 ?
C2 C1 C1 84.3 . 5_665 ?
C2 C1 C2 86.0 9 . ?
C1 C2 N1 50.2 . . ?
C1 C2 N1 50.2 16_556 . ?
C1 C2 C1 85.1 . 16_556 ?
C2 C2 N1 68.0 7_665 . ?
C2 C2 C1 95.7 7_665 . ?
C2 C2 C1 95.7 7_665 16_556 ?

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
N1 C1 C2 C1 -40.1 . . . 16_556 ?
N1 C1 C2 C2 55.1 . . . 7_665 ?
C1 N1 C1 C1 75.0 5_665 . . 3_655 ?
C1 N1 C1 C1 151.0 14_666 . . 3_655 ?
C1 N1 C1 C1 76.0 14_666 . . 5_665 ?
C1 N1 C1 C1 142.5 16_556 . . 5_665 ?
C1 N1 C1 C1 -76.0 18_656 . . 3_655 ?
C1 N1 C1 C1 -151.0 18_656 . . 5_665 ?
C1 N1 C1 C1 -75.0 3_655 . . 5_665 ?
C1 N1 C1 C1 -142.5 16_556 . . 3_655 ?
C1 N1 C1 C2 20.4 18_656 . . 9 ?
C1 N1 C1 C2 -96.4 5_665 . . . ?
C1 N1 C1 C2 -171.4 3_655 . . . ?
C1 N1 C1 C2 96.4 3_655 . . 9 ?
C1 N1 C1 C2 112.6 18_656 . . . ?
C1 N1 C1 C2 -112.6 14_666 . . 9 ?
C1 N1 C1 C2 -20.4 14_666 . . . ?
C1 N1 C1 C2 171.4 5_665 . . 9 ?
C1 N1 C1 C2 46.1 16_556 . . . ?
C1 N1 C1 C2 -46.1 16_556 . . 9 ?
C1 N1 C2 C1 -167.4 5_665 . . 16_556 ?
C1 N1 C2 C1 123.3 . . . 16_556 ?
C1 N1 C2 C1 -10.2 18_656 . . 16_556 ?
C1 N1 C2 C1 -69.2 14_666 . . 16_556 ?
C1 N1 C2 C1 -123.3 16_556 . . . ?
C1 N1 C2 C1 10.2 3_655 . . . ?
C1 N1 C2 C1 133.6 3_655 . . 16_556 ?
C1 N1 C2 C1 167.4 14_666 . . . ?
C1 N1 C2 C1 69.2 5_665 . . . ?
C1 N1 C2 C1 -133.6 18_656 . . . ?
C1 N1 C2 C2 -108.1 3_655 . . 7_665 ?
C1 N1 C2 C2 118.3 16_556 . . 7_665 ?
C1 N1 C2 C2 108.1 18_656 . . 7_665 ?
C1 N1 C2 C2 -118.3 . . . 7_665 ?
C1 N1 C2 C2 49.1 14_666 . . 7_665 ?
C1 N1 C2 C2 -49.1 5_665 . . 7_665 ?
C1 C1 C2 N1 -8.7 3_655 . . . ?
C1 C1 C2 N1 -55.1 5_665 . . . ?
C1 C1 C2 C1 -95.2 5_665 . . 16_556 ?
C1 C1 C2 C1 -48.8 3_655 . . 16_556 ?
C1 C1 C2 C2 0.0 5_665 . . 7_665 ?
C1 C1 C2 C2 46.4 3_655 . . 7_665 ?
C2 N1 C1 C1 58.6 7_665 . . 5_665 ?
C2 N1 C1 C1 -58.6 3_655 . . 3_655 ?
C2 N1 C1 C1 -133.6 3_655 . . 5_665 ?
C2 N1 C1 C1 96.4 . . . 5_665 ?
C2 N1 C1 C1 -9.3 14_666 . . 5_665 ?
C2 N1 C1 C1 65.7 14_666 . . 3_655 ?
C2 N1 C1 C1 -171.4 9 . . 5_665 ?
C2 N1 C1 C1 9.3 20_655 . . 3_655 ?
C2 N1 C1 C1 171.4 . . . 3_655 ?
C2 N1 C1 C1 -96.4 9 . . 3_655 ?
C2 N1 C1 C1 133.6 7_665 . . 3_655 ?
C2 N1 C1 C1 -65.7 20_655 . . 5_665 ?
C2 N1 C1 C2 162.1 14_666 . . 9 ?
C2 N1 C1 C2 37.8 3_655 . . 9 ?
C2 N1 C1 C2 -105.7 14_666 . . . ?
C2 N1 C1 C2 -130.0 7_665 . . 9 ?
C2 N1 C1 C2 92.2 9 . . . ?
C2 N1 C1 C2 -92.2 . . . 9 ?
C2 N1 C1 C2 -37.8 7_665 . . . ?
C2 N1 C1 C2 130.0 3_655 . . . ?
C2 N1 C1 C2 -162.1 20_655 . . . ?
C2 N1 C1 C2 105.7 20_655 . . 9 ?
C2 N1 C2 C1 118.3 7_665 . . . ?
C2 N1 C2 C1 118.3 20_655 . . . ?
C2 N1 C2 C1 118.3 14_666 . . . ?
C2 N1 C2 C1 -118.3 20_655 . . 16_556 ?
C2 N1 C2 C1 61.7 3_655 . . 16_556 ?
C2 N1 C2 C1 61.7 9 . . 16_556 ?
C2 N1 C2 C1 -61.7 3_655 . . . ?
C2 N1 C2 C1 -61.7 9 . . . ?
C2 N1 C2 C1 -118.3 14_666 . . 16_556 ?
C2 N1 C2 C1 -118.3 7_665 . . 16_556 ?
C2 N1 C2 C2 180.0 9 . . 7_665 ?
C2 N1 C2 C2 0.0 20_655 . . 7_665 ?
C2 N1 C2 C2 180.0 3_655 . . 7_665 ?
C2 N1 C2 C2 0.0 14_666 . . 7_665 ?
C2 C1 C2 N1 71.3 9 . . . ?
C2 C1 C2 C1 31.2 9 . . 16_556 ?
C2 C1 C2 C2 126.5 9 . . 7_665 ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_RINTA01_DMPPbBr3_303Kcooling 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The low-temperature phase of the crystal is too close to the high-temperature 
phase, and the intermediate phase is extremely unstable and heavily disordered.
;
_vrf_PLAT020_DMPPbBr3_303Kcooling 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.337 Report
RESPONSE: The low-temperature phase of the crystal is too close to the high-temperature 
phase, and the intermediate phase is extremely unstable and heavily disordered.
;
_vrf_PLAT972_DMPPbBr3_303Kcooling 
;
PROBLEM: Check Calcd Resid. Dens.  1.47Ang From Pb1            -4.78 eA-3  
RESPONSE: This density residual is very close to the heavy metal(Pb) that 
has a high electron density.
The low-temperature phase of the crystal is too close to the high-temperature 
phase, and the intermediate phase is extremely unstable and heavily disordered.
;
_vrf_PLAT082_DMPPbBr3_303Kcooling 
;
PROBLEM: High R1 Value ..................................       0.17 Report
RESPONSE: The low-temperature phase of the crystal is too close to the high-temperature 
phase, and the intermediate phase is extremely unstable and heavily disordered.
;
_vrf_PLAT976_DMPPbBr3_303Kcooling 
;
PROBLEM: Check Calcd Resid. Dens.  0.83Ang From C2      .      -1.83 eA-3  
RESPONSE: The low-temperature phase of the crystal is too close to the high-temperature 
phase, and the intermediate phase is extremely unstable and heavily disordered.
;
# end Validation Reply Form



####################################################################### 
# 
# 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_(DMP)PbBr3_273K
_database_code_depnum_ccdc_archive 'CCDC 2366484'
loop_
_audit_author_name
_audit_author_address
'zhilong li'
;Southeast University
China
;
_audit_update_record             
;
2024-06-28 deposited with the CCDC.	2024-08-04 downloaded from the CCDC.
;
_audit_creation_date             2024-06-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C6 H12 N'
_chemical_formula_sum            'C6 H12 Br3 N Pb'
_chemical_formula_weight         545.09
_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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.657(4)
_cell_length_b                   7.966(3)
_cell_length_c                   16.008(7)
_cell_angle_alpha                90
_cell_angle_beta                 92.539(9)
_cell_angle_gamma                90
_cell_volume                     1230.3(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1002
_cell_measurement_temperature    273.0
_cell_measurement_theta_max      23.70
_cell_measurement_theta_min      2.42
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.407
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4483
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1352 before and 0.0844 after correction.
The Ratio of minimum to maximum transmission is 0.6014.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.943
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1554
_diffrn_reflns_av_unetI/netI     0.1562
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9061
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.434
_diffrn_reflns_theta_min         2.417
_diffrn_ambient_temperature      273.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1358
_reflns_number_total             2504
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.546
_refine_diff_density_min         -2.757
_refine_diff_density_rms         0.467
_refine_ls_extinction_coef       0.0033(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2504
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1486
_refine_ls_R_factor_gt           0.0892
_refine_ls_restrained_S_all      1.068
_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)+(0.1059P)²+3.0575P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2629
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C5, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.25155(11) 0.54418(12) 0.24830(6) 0.0404(5) Uani 1 1 d . . . . .
Br3 Br 0.0542(3) 0.3417(3) 0.33190(19) 0.0489(8) Uani 1 1 d . . . . .
Br1 Br 0.2881(3) 0.7758(3) 0.39260(18) 0.0507(8) Uani 1 1 d . . . . .
Br2 Br 0.0351(3) 0.7710(3) 0.1799(2) 0.0534(9) Uani 1 1 d . . . . .
N1 N 0.741(2) 0.717(3) 0.4063(14) 0.042(6) Uani 1 1 d . . . . .
C4 C 0.900(3) 0.935(4) 0.4087(19) 0.059(8) Uani 1 1 d . U . . .
H4 H 0.981079 0.994154 0.401184 0.071 Uiso 1 1 calc R U . . .
C2 C 0.720(3) 0.664(4) 0.319(2) 0.063(9) Uani 1 1 d . . . . .
H2A H 0.623962 0.640487 0.306919 0.094 Uiso 1 1 calc R U . . .
H2B H 0.773634 0.563931 0.309534 0.094 Uiso 1 1 calc R U . . .
H2C H 0.750097 0.751290 0.282525 0.094 Uiso 1 1 calc R U . . .
C5 C 0.786(4) 1.004(4) 0.407(2) 0.064(10) Uani 1 1 d . U . . .
H5 H 0.772724 1.117780 0.396385 0.077 Uiso 1 1 calc R U . . .
C6 C 0.669(3) 0.881(4) 0.426(3) 0.073(11) Uani 1 1 d . . . . .
H6A H 0.643758 0.886139 0.483670 0.088 Uiso 1 1 calc R U . . .
H6B H 0.587560 0.898737 0.389319 0.088 Uiso 1 1 calc R U . . .
C3 C 0.899(3) 0.750(3) 0.423(2) 0.062(10) Uani 1 1 d . . . . .
H3A H 0.929785 0.720805 0.479887 0.074 Uiso 1 1 calc R U . . .
H3B H 0.955269 0.690278 0.383843 0.074 Uiso 1 1 calc R U . . .
C1 C 0.700(5) 0.583(5) 0.463(3) 0.108(16) Uani 1 1 d . . . . .
H1A H 0.601892 0.563772 0.455225 0.162 Uiso 1 1 calc R U . . .
H1B H 0.721862 0.614720 0.519422 0.162 Uiso 1 1 calc R U . . .
H1C H 0.748685 0.481450 0.449919 0.162 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br3 2.872(3) . ?
Pb1 Br1 2.965(3) . ?
Pb1 Br1 3.119(3) 2_545 ?
Pb1 Br2 2.938(3) . ?
Pb1 Br2 3.177(3) 2_545 ?
N1 C2 1.47(4) . ?
N1 C6 1.52(4) . ?
N1 C3 1.56(4) . ?
N1 C1 1.46(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.22(4) . ?
C4 C3 1.49(4) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C5 H5 0.9300 . ?
C5 C6 1.54(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br3 Pb1 Br1 83.64(9) . 2_545 ?
Br3 Pb1 Br1 92.57(9) . . ?
Br3 Pb1 Br2 92.48(10) . . ?
Br3 Pb1 Br2 83.10(9) . 2_545 ?
Br1 Pb1 Br1 175.15(8) . 2_545 ?
Br1 Pb1 Br2 81.31(8) 2_545 2_545 ?
Br1 Pb1 Br2 95.25(9) . 2_545 ?
Br2 Pb1 Br1 88.03(9) . . ?
Br2 Pb1 Br1 95.15(9) . 2_545 ?
Br2 Pb1 Br2 174.59(8) . 2_545 ?
Pb1 Br3 Pb1 79.79(8) . 2_545 ?
Pb1 Br1 Pb1 81.76(8) . 2 ?
Pb1 Br2 Pb1 81.20(8) . 2 ?
C2 N1 C6 114(2) . . ?
C2 N1 C3 108(2) . . ?
C6 N1 C3 106.0(19) . . ?
C1 N1 C2 110(2) . . ?
C1 N1 C6 111(3) . . ?
C1 N1 C3 108(3) . . ?
C5 C4 H4 121.9 . . ?
C5 C4 C3 116(3) . . ?
C3 C4 H4 121.9 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C5 H5 124.1 . . ?
C4 C5 C6 112(3) . . ?
C6 C5 H5 124.1 . . ?
N1 C6 C5 99(2) . . ?
N1 C6 H6A 111.9 . . ?
N1 C6 H6B 111.9 . . ?
C5 C6 H6A 111.9 . . ?
C5 C6 H6B 111.9 . . ?
H6A C6 H6B 109.6 . . ?
N1 C3 H3A 112.1 . . ?
N1 C3 H3B 112.1 . . ?
C4 C3 N1 98(2) . . ?
C4 C3 H3A 112.1 . . ?
C4 C3 H3B 112.1 . . ?
H3A C3 H3B 109.7 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 C5 C6 N1 -20(4) . . . . ?
C2 N1 C6 C5 -90(3) . . . . ?
C2 N1 C3 C4 96(3) . . . . ?
C5 C4 C3 N1 15(4) . . . . ?
C6 N1 C3 C4 -26(3) . . . . ?
C3 N1 C6 C5 28(3) . . . . ?
C3 C4 C5 C6 3(5) . . . . ?
C1 N1 C6 C5 145(3) . . . . ?
C1 N1 C3 C4 -145(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT971_DMPPbBr3_273K       
;
PROBLEM: Check Calcd Resid. Dens.  0.84Ang From Pb1             3.65 eA-3  
RESPONSE: This density residual is very close to the heavy metal that 
has a high electron density.
;
_vrf_PLAT973_DMPPbBr3_273K       
;
PROBLEM: Check Calcd Positive Resid. Density on       Pb1       4.53 eA-3  
RESPONSE: This density residual is very close to the heavy metal that 
has a high electron density.
;
_vrf_PLAT342_DMPPbBr3_273K       
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04667 Ang.  
RESPONSE: The quality of this crystal was poor.
;
_vrf_PLAT972_DMPPbBr3_273K       
;
PROBLEM: Check Calcd Resid. Dens.  0.90Ang From Pb1            -2.66 eA-3  
RESPONSE: This density residual is very close to the heavy metal that 
has a high electron density.
;
# end Validation Reply Form
####################################################################### 
# 
# 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__(EMP)PbBr3_300K
_database_code_depnum_ccdc_archive 'CCDC 2366487'
loop_
_audit_author_name
_audit_author_address
'zhilong li'
;Southeast University
China
;
_audit_update_record             
;
2024-06-28 deposited with the CCDC.	2024-08-04 downloaded from the CCDC.
;
_audit_creation_date             2024-06-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C7 H14 N'
_chemical_formula_sum            'C7 H14 Br3 N Pb'
_chemical_formula_weight         559.11
_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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.8938(6)
_cell_length_b                   16.7828(10)
_cell_length_c                   7.8993(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.698(3)
_cell_angle_gamma                90
_cell_volume                     1308.91(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4548
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.39
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.006
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.3832
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1613 before and 0.0743 after correction.
The Ratio of minimum to maximum transmission is 0.5131.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.837
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1119
_diffrn_reflns_av_unetI/netI     0.1095
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            35260
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.429
_diffrn_reflns_theta_min         2.063
_diffrn_ambient_temperature      300.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2295
_reflns_number_total             5508
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.384
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.218
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         5508
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1518
_refine_ls_R_factor_gt           0.0395
_refine_ls_restrained_S_all      0.967
_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)+(0.0157P)²+0.6121P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0876
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-C1 \\sim C2-C1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C1A) = Uanis(C1)
4. Rigid body (RIGU) restrains
 C2, C1A, C1
 with sigma for 1-2 distances of 0.006 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H2AA(0.5) H2AB(0.5) H2BC(0.5) H2BD(0.5) C1(0.5) H1A(0.5) H1B(0.5)
 H1C(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2AA,H2AB), C2(H2BC,H2BD), C4(H4A,H4B), C7(H7A,H7B)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6)
6.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC)
;
_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 0.77365(2) -0.25084(2) 0.38367(2) 0.04165(9) Uani 1 1 d . . . . .
Br1 Br 0.78638(8) -0.11223(4) 0.60683(8) 0.05880(19) Uani 1 1 d . . . . .
Br2 Br 0.97624(7) -0.18043(4) 0.15498(8) 0.05665(18) Uani 1 1 d . . . . .
Br3 Br 0.56965(7) -0.18215(5) 0.12562(8) 0.0608(2) Uani 1 1 d . . . . .
N1 N 0.7497(5) 0.0929(3) 0.2744(6) 0.0469(12) Uani 1 1 d . . . . .
C2 C 0.8280(10) 0.0342(5) 0.1802(9) 0.093(3) Uani 1 1 d D U . . .
H2AA H 0.825823 -0.015792 0.241648 0.112 Uiso 0.5 1 calc R U P A 1
H2AB H 0.921470 0.051932 0.187000 0.112 Uiso 0.5 1 calc R U P A 1
H2BC H 0.840479 -0.015016 0.243719 0.112 Uiso 0.5 1 calc R U P B 2
H2BD H 0.915938 0.055299 0.156047 0.112 Uiso 0.5 1 calc R U P B 2
C4 C 0.8222(8) 0.1018(5) 0.4524(9) 0.074(2) Uani 1 1 d . . . . .
H4A H 0.869352 0.053264 0.487179 0.089 Uiso 1 1 calc R U . . .
H4B H 0.886072 0.145718 0.455988 0.089 Uiso 1 1 calc R U . . .
C5 C 0.7079(10) 0.1180(5) 0.5595(9) 0.073(2) Uani 1 1 d . . . . .
H5 H 0.717333 0.139109 0.668504 0.088 Uiso 1 1 calc R U . . .
C6 C 0.5966(9) 0.0996(5) 0.4840(11) 0.085(3) Uani 1 1 d . . . . .
H6 H 0.513583 0.104801 0.531820 0.103 Uiso 1 1 calc R U . . .
C7 C 0.6119(8) 0.0688(5) 0.3100(10) 0.085(3) Uani 1 1 d . . . . .
H7A H 0.602335 0.011253 0.306300 0.102 Uiso 1 1 calc R U . . .
H7B H 0.545504 0.092394 0.229377 0.102 Uiso 1 1 calc R U . . .
C3 C 0.7458(8) 0.1718(4) 0.1880(8) 0.0662(19) Uani 1 1 d . . . . .
H3A H 0.836606 0.190171 0.176048 0.099 Uiso 1 1 calc R U . . .
H3B H 0.698735 0.209421 0.254449 0.099 Uiso 1 1 calc R U . . .
H3C H 0.699558 0.166787 0.077939 0.099 Uiso 1 1 calc R U . . .
C1 C 0.7903(19) 0.0164(16) -0.0001(17) 0.074(4) Uani 0.5 1 d D U P C 1
H1A H 0.695034 0.005404 -0.014036 0.111 Uiso 0.5 1 calc R U P C 1
H1B H 0.840224 -0.029171 -0.034821 0.111 Uiso 0.5 1 calc R U P C 1
H1C H 0.811271 0.061474 -0.068577 0.111 Uiso 0.5 1 calc R U P C 1
C1A C 0.7392(18) 0.0209(17) 0.0167(18) 0.074(4) Uani 0.5 1 d D U P C 2
H1AA H 0.645621 0.020717 0.041982 0.111 Uiso 0.5 1 calc R U P C 2
H1AB H 0.761787 -0.029243 -0.032522 0.111 Uiso 0.5 1 calc R U P C 2
H1AC H 0.754620 0.063072 -0.062027 0.111 Uiso 0.5 1 calc R U P C 2


_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 2.9165(7) . ?
Pb1 Br1 3.1803(7) 4 ?
Pb1 Br2 3.0637(7) 4_556 ?
Pb1 Br2 3.0239(7) . ?
Pb1 Br3 3.0045(7) . ?
Pb1 Br3 3.0803(7) 4_556 ?
N1 C2 1.483(9) . ?
N1 C4 1.544(8) . ?
N1 C7 1.467(9) . ?
N1 C3 1.489(7) . ?
C2 H2AA 0.9700 . ?
C2 H2AB 0.9700 . ?
C2 H2BC 0.9700 . ?
C2 H2BD 0.9700 . ?
C2 C1 1.480(14) . ?
C2 C1A 1.531(14) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.480(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.257(11) . ?
C6 H6 0.9300 . ?
C6 C7 1.485(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1A H1AA 0.9600 . ?
C1A H1AB 0.9600 . ?
C1A H1AC 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 171.83(2) . 4 ?
Br1 Pb1 Br2 82.91(2) . 4_556 ?
Br1 Pb1 Br2 92.58(2) . . ?
Br1 Pb1 Br3 96.03(2) . . ?
Br1 Pb1 Br3 85.45(2) . 4_556 ?
Br2 Pb1 Br1 79.304(18) . 4 ?
Br2 Pb1 Br1 98.966(19) 4_556 4 ?
Br2 Pb1 Br2 97.82(2) . 4_556 ?
Br2 Pb1 Br3 177.992(19) . 4_556 ?
Br2 Pb1 Br3 81.594(19) 4_556 4_556 ?
Br3 Pb1 Br1 102.677(19) 4_556 4 ?
Br3 Pb1 Br1 82.264(19) . 4 ?
Br3 Pb1 Br2 83.51(2) . . ?
Br3 Pb1 Br2 178.327(18) . 4_556 ?
Br3 Pb1 Br3 97.05(2) . 4_556 ?
Pb1 Br1 Pb1 80.631(17) . 4_556 ?
Pb1 Br2 Pb1 80.900(17) . 4 ?
Pb1 Br3 Pb1 80.938(17) . 4 ?
C2 N1 C4 107.1(6) . . ?
C2 N1 C3 111.1(5) . . ?
C7 N1 C2 115.7(6) . . ?
C7 N1 C4 103.6(5) . . ?
C7 N1 C3 109.7(6) . . ?
C3 N1 C4 109.2(5) . . ?
N1 C2 H2AA 107.2 . . ?
N1 C2 H2AB 107.2 . . ?
N1 C2 H2BC 111.1 . . ?
N1 C2 H2BD 111.1 . . ?
N1 C2 C1 120.7(11) . . ?
N1 C2 C1A 103.3(11) . . ?
H2AA C2 H2AB 106.8 . . ?
H2BC C2 H2BD 109.1 . . ?
C1 C2 H2AA 107.2 . . ?
C1 C2 H2AB 107.2 . . ?
C1A C2 H2BC 111.1 . . ?
C1A C2 H2BD 111.1 . . ?
N1 C4 H4A 111.3 . . ?
N1 C4 H4B 111.3 . . ?
H4A C4 H4B 109.2 . . ?
C5 C4 N1 102.2(6) . . ?
C5 C4 H4A 111.3 . . ?
C5 C4 H4B 111.3 . . ?
C4 C5 H5 124.4 . . ?
C6 C5 C4 111.2(7) . . ?
C6 C5 H5 124.4 . . ?
C5 C6 H6 123.6 . . ?
C5 C6 C7 112.7(7) . . ?
C7 C6 H6 123.6 . . ?
N1 C7 C6 103.5(6) . . ?
N1 C7 H7A 111.1 . . ?
N1 C7 H7B 111.1 . . ?
C6 C7 H7A 111.1 . . ?
C6 C7 H7B 111.1 . . ?
H7A C7 H7B 109.0 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1A H1AA 109.5 . . ?
C2 C1A H1AB 109.5 . . ?
C2 C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C4 C5 C6 16.5(9) . . . . ?
C2 N1 C4 C5 -147.7(6) . . . . ?
C2 N1 C7 C6 141.2(7) . . . . ?
C4 N1 C2 C1 -175.6(13) . . . . ?
C4 N1 C2 C1A 172.6(11) . . . . ?
C4 N1 C7 C6 24.3(8) . . . . ?
C4 C5 C6 C7 -1.1(11) . . . . ?
C5 C6 C7 N1 -15.7(10) . . . . ?
C7 N1 C2 C1 69.5(14) . . . . ?
C7 N1 C2 C1A 57.8(12) . . . . ?
C7 N1 C4 C5 -24.9(8) . . . . ?
C3 N1 C2 C1 -56.5(14) . . . . ?
C3 N1 C2 C1A -68.2(12) . . . . ?
C3 N1 C4 C5 91.9(6) . . . . ?
C3 N1 C7 C6 -92.1(7) . . . . ?

_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_(EMP)PbBr3_273K
_database_code_depnum_ccdc_archive 'CCDC 2366488'
loop_
_audit_author_name
_audit_author_address
'zhilong li'
;Southeast University
China
;
_audit_update_record             
;
2024-06-28 deposited with the CCDC.	2024-08-04 downloaded from the CCDC.
;
_audit_creation_date             2024-02-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C7 H14 N'
_chemical_formula_sum            'C7 H14 Br3 N Pb'
_chemical_formula_weight         559.11
_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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.761(2)
_cell_length_b                   7.9767(14)
_cell_length_c                   16.706(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.053(6)
_cell_angle_gamma                90
_cell_volume                     1299.9(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5437
_cell_measurement_temperature    273.0
_cell_measurement_theta_max      26.76
_cell_measurement_theta_min      2.38
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.158
_exptl_absorpt_correction_T_max  0.7477
_exptl_absorpt_correction_T_min  0.3500
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1417 before and 0.0802 after correction.
The Ratio of minimum to maximum transmission is 0.4681.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.857
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28797
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         2.380
_diffrn_ambient_temperature      273.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2185
_reflns_number_total             2836
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.880
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.222
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2836
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0388
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0599P)²+14.7416P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1272
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C2(H2A,H2B), C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.25218(4) 1.11064(5) 0.74900(2) 0.03417(16) Uani 1 1 d . . . . .
Br3 Br 0.46575(11) 1.33315(15) 0.81111(7) 0.0452(3) Uani 1 1 d . . . . .
Br1 Br 0.28293(13) 0.87992(15) 0.88720(7) 0.0476(3) Uani 1 1 d . . . . .
Br2 Br 0.44340(12) 0.89578(14) 0.67063(8) 0.0477(3) Uani 1 1 d . . . . .
N1 N 0.7671(9) 0.2868(12) 0.5939(5) 0.038(2) Uani 1 1 d . . . . .
C6 C 0.7098(14) 0.5707(15) 0.6173(8) 0.052(3) Uani 1 1 d . . . . .
H6 H 0.715187 0.679888 0.636619 0.062 Uiso 1 1 calc R U . . .
C5 C 0.5946(13) 0.4896(17) 0.6009(8) 0.057(3) Uani 1 1 d . . . . .
H5 H 0.508286 0.537050 0.605920 0.068 Uiso 1 1 calc R U . . .
C3 C 0.7796(14) 0.2029(16) 0.6740(7) 0.052(3) Uani 1 1 d . . . . .
H3A H 0.874682 0.183847 0.687835 0.078 Uiso 1 1 calc R U . . .
H3B H 0.732028 0.097556 0.671822 0.078 Uiso 1 1 calc R U . . .
H3C H 0.740289 0.273321 0.713701 0.078 Uiso 1 1 calc R U . . .
C7 C 0.8293(11) 0.4638(16) 0.6007(8) 0.049(3) Uani 1 1 d . . . . .
H7A H 0.897929 0.469732 0.644057 0.059 Uiso 1 1 calc R U . . .
H7B H 0.870697 0.496566 0.551143 0.059 Uiso 1 1 calc R U . . .
C2 C 0.8411(15) 0.1869(18) 0.5322(8) 0.064(4) Uani 1 1 d . . . . .
H2A H 0.835246 0.246804 0.481658 0.077 Uiso 1 1 calc R U . . .
H2B H 0.937223 0.179599 0.548658 0.077 Uiso 1 1 calc R U . . .
C1 C 0.7865(18) 0.0130(19) 0.5192(9) 0.078(5) Uani 1 1 d . . . . .
H1A H 0.820162 -0.031369 0.470267 0.117 Uiso 1 1 calc R U . . .
H1B H 0.688142 0.016156 0.515963 0.117 Uiso 1 1 calc R U . . .
H1C H 0.816233 -0.057246 0.563179 0.117 Uiso 1 1 calc R U . . .
C4 C 0.6163(12) 0.3161(17) 0.5738(9) 0.055(3) Uani 1 1 d . . . . .
H4A H 0.596645 0.305218 0.516688 0.066 Uiso 1 1 calc R U . . .
H4B H 0.559379 0.238076 0.602205 0.066 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br3 2.9014(12) . ?
Pb1 Br3 3.2062(13) 2_546 ?
Pb1 Br1 3.1390(13) 2_556 ?
Pb1 Br1 2.9593(13) . ?
Pb1 Br2 2.8828(12) . ?
N1 C3 1.497(13) . ?
N1 C7 1.539(15) . ?
N1 C2 1.508(14) . ?
N1 C4 1.516(14) . ?
C6 H6 0.9300 . ?
C6 C5 1.317(18) . ?
C6 C7 1.479(17) . ?
C5 H5 0.9300 . ?
C5 C4 1.474(19) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.50(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 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
Br3 Pb1 Br3 173.99(4) . 2_546 ?
Br3 Pb1 Br1 92.86(4) . . ?
Br3 Pb1 Br1 84.20(4) . 2_556 ?
Br1 Pb1 Br3 82.11(4) . 2_546 ?
Br1 Pb1 Br3 101.03(3) 2_556 2_546 ?
Br1 Pb1 Br1 175.19(4) . 2_556 ?
Br2 Pb1 Br3 93.30(4) . . ?
Br2 Pb1 Br3 83.13(4) . 2_546 ?
Br2 Pb1 Br1 97.66(4) . 2_556 ?
Br2 Pb1 Br1 86.30(4) . . ?
Pb1 Br3 Pb1 81.38(3) . 2_556 ?
Pb1 Br1 Pb1 81.64(3) . 2_546 ?
C3 N1 C7 109.0(9) . . ?
C3 N1 C2 110.4(10) . . ?
C3 N1 C4 108.4(9) . . ?
C2 N1 C7 109.7(9) . . ?
C2 N1 C4 114.5(10) . . ?
C4 N1 C7 104.6(9) . . ?
C5 C6 H6 124.7 . . ?
C5 C6 C7 110.6(11) . . ?
C7 C6 H6 124.7 . . ?
C6 C5 H5 123.4 . . ?
C6 C5 C4 113.2(11) . . ?
C4 C5 H5 123.4 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C7 H7A 111.1 . . ?
N1 C7 H7B 111.1 . . ?
C6 C7 N1 103.3(9) . . ?
C6 C7 H7A 111.1 . . ?
C6 C7 H7B 111.1 . . ?
H7A C7 H7B 109.1 . . ?
N1 C2 H2A 108.7 . . ?
N1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C1 C2 N1 114.3(12) . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C4 H4A 111.2 . . ?
N1 C4 H4B 111.2 . . ?
C5 C4 N1 103.1(10) . . ?
C5 C4 H4A 111.2 . . ?
C5 C4 H4B 111.2 . . ?
H4A C4 H4B 109.1 . . ?

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
C6 C5 C4 N1 12.6(15) . . . . ?
C5 C6 C7 N1 -15.5(14) . . . . ?
C3 N1 C7 C6 -93.5(11) . . . . ?
C3 N1 C2 C1 61.2(15) . . . . ?
C3 N1 C4 C5 95.1(12) . . . . ?
C7 N1 C2 C1 -178.6(11) . . . . ?
C7 N1 C4 C5 -21.0(12) . . . . ?
C7 C6 C5 C4 2.0(16) . . . . ?
C2 N1 C7 C6 145.6(11) . . . . ?
C2 N1 C4 C5 -141.2(11) . . . . ?
C4 N1 C7 C6 22.3(12) . . . . ?
C4 N1 C2 C1 -61.4(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_(EMP)PbBr3_373K
_database_code_depnum_ccdc_archive 'CCDC 2366485'
loop_
_audit_author_name
_audit_author_address
'zhilong li'
;Southeast University
China
;
_audit_update_record             
;
2024-06-28 deposited with the CCDC.	2024-08-04 downloaded from the CCDC.
;
_audit_creation_date             2024-06-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C7 N'
_chemical_formula_sum            'C7 Br3 N Pb'
_chemical_formula_weight         545.00
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.897(12)
_cell_length_b                   17.309(19)
_cell_length_c                   7.897(8)
_cell_angle_alpha                90
_cell_angle_beta                 94.10(2)
_cell_angle_gamma                90
_cell_volume                     1349(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1404
_cell_measurement_temperature    373.0
_cell_measurement_theta_max      17.89
_cell_measurement_theta_min      2.41
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    21.344
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3657
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1618 before and 0.0906 after correction.
The Ratio of minimum to maximum transmission is 0.4907.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.683
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             944
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1975
_diffrn_reflns_av_unetI/netI     0.1035
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18812
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.370
_diffrn_reflns_theta_min         2.063
_diffrn_ambient_temperature      373.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                974
_reflns_number_total             2406
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.296
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       0.0071(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2406
_refine_ls_number_restraints     435
_refine_ls_R_factor_all          0.1597
_refine_ls_R_factor_gt           0.0715
_refine_ls_restrained_S_all      0.909
_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)+(0.1127P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.2417
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N1-C4 \\sim N1A-C7A
 with sigma of 0.02
 N1-C3 \\sim N1A-C3A
 with sigma of 0.02
 N1-C7 \\sim N1A-C4A
 with sigma of 0.02
 N1-C2 \\sim N1A-C2A
 with sigma of 0.02
 C4-C7 \\sim C7A-C4A
 with sigma of 0.04
 C6-C7 \\sim C5A-C4A
 with sigma of 0.02
 C1-C2 \\sim C1A-C2A
 with sigma of 0.02
 C3-C2 \\sim C3A-C2A
 with sigma of 0.04
 C7-C2 \\sim C4A-C2A
 with sigma of 0.04
 C6-C4 \\sim C5A-C7A
 with sigma of 0.04
 C4-C3 \\sim C7A-C3A
 with sigma of 0.04
 C4-C2 \\sim C7A-C2A
 with sigma of 0.04
 N1-C5 \\sim N1A-C6A
 with sigma of 0.04
 N1-C6 \\sim N1A-C5A
 with sigma of 0.04
 N1-C1 \\sim N1A-C1A
 with sigma of 0.04
 C3-C7 \\sim C3A-C4A
 with sigma of 0.04
 C5-C6 \\sim C6A-C5A
 with sigma of 0.04
 C5-C4 \\sim C6A-C7A
 with sigma of 0.04
 C5-C7 \\sim C6A-C4A
 with sigma of 0.04
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C5, N1, C4, C3, C7, C2, C6, C1, C4A, N1A, C3A, C7A, C2A, C5A, C6A, C1A
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
5. Others
 Sof(N1A)=Sof(C3A)=Sof(C4A)=Sof(C5A)=Sof(C6A)=Sof(C7A)=Sof(C2A)=Sof(C1A)=1-
 FVAR(1)
 Sof(N1)=Sof(C5)=Sof(C6)=Sof(C4)=Sof(C1)=Sof(C3)=Sof(C7)=Sof(C2)=FVAR(1)
;
_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 0.26444(9) 0.24982(5) 0.41376(11) 0.0969(6) Uani 1 1 d . U . . .
Br3 Br 0.2667(3) 0.38291(18) 0.6486(3) 0.1385(12) Uani 1 1 d . U . . .
Br1 Br 0.4680(3) 0.3149(2) 0.1838(4) 0.1433(12) Uani 1 1 d . U . . .
Br2 Br 0.0629(3) 0.3163(2) 0.1451(4) 0.1400(12) Uani 1 1 d . U . . .
N1 N 0.248(6) 0.586(2) 0.271(9) 0.146(8) Uani 0.599(18) 1 d D U P A 1
C5 C 0.182(7) 0.639(4) 0.507(7) 0.174(12) Uani 0.599(18) 1 d D U P A 1
C6 C 0.114(6) 0.593(3) 0.460(7) 0.169(11) Uani 0.599(18) 1 d D U P A 1
C4 C 0.326(6) 0.605(3) 0.441(7) 0.159(9) Uani 0.599(18) 1 d D U P A 1
C1 C 0.309(5) 0.516(3) 0.035(6) 0.156(14) Uani 0.599(18) 1 d D U P A 1
C3 C 0.263(5) 0.653(3) 0.165(7) 0.169(13) Uani 0.599(18) 1 d D U P A 1
C7 C 0.118(5) 0.581(3) 0.300(7) 0.159(9) Uani 0.599(18) 1 d D U P A 1
C2 C 0.335(5) 0.525(3) 0.235(6) 0.161(9) Uani 0.599(18) 1 d D U P A 1
N1A N 0.263(7) 0.592(3) 0.256(10) 0.147(8) Uani 0.401(18) 1 d D U P A 2
C3A C 0.200(8) 0.666(4) 0.277(10) 0.162(13) Uani 0.401(18) 1 d D U P A 2
C4A C 0.323(7) 0.596(4) 0.110(8) 0.157(10) Uani 0.401(18) 1 d D U P A 2
C5A C 0.233(8) 0.564(4) 0.007(8) 0.166(13) Uani 0.401(18) 1 d D U P A 2
C6A C 0.199(7) 0.508(4) 0.052(9) 0.159(12) Uani 0.401(18) 1 d D U P A 2
C7A C 0.154(6) 0.530(3) 0.239(8) 0.155(10) Uani 0.401(18) 1 d D U P A 2
C2A C 0.327(7) 0.561(4) 0.407(8) 0.155(10) Uani 0.401(18) 1 d D U P A 2
C1A C 0.238(8) 0.600(5) 0.546(8) 0.155(17) Uani 0.401(18) 1 d D U P A 2


_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 Br3 2.956(4) . ?
Pb1 Br3 3.110(4) 4_565 ?
Pb1 Br1 3.025(4) . ?
Pb1 Br1 3.041(4) 4_566 ?
Pb1 Br2 3.033(4) . ?
Pb1 Br2 3.025(3) 4_566 ?
N1 C4 1.53(8) . ?
N1 C3 1.44(6) . ?
N1 C7 1.32(7) . ?
N1 C2 1.41(6) . ?
C5 C6 1.09(6) . ?
C5 C4 1.66(7) . ?
C6 C7 1.29(6) . ?
C1 C2 1.59(6) . ?
N1A C3A 1.44(6) . ?
N1A C4A 1.33(7) . ?
N1A C7A 1.51(8) . ?
N1A C2A 1.41(6) . ?
C4A C5A 1.29(6) . ?
C5A C6A 1.10(7) . ?
C6A C7A 1.62(8) . ?
C2A C1A 1.61(6) . ?

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
Br3 Pb1 Br3 176.34(9) . 4_565 ?
Br3 Pb1 Br1 96.37(11) . . ?
Br3 Pb1 Br1 82.66(10) . 4_566 ?
Br3 Pb1 Br2 83.80(11) . 4_566 ?
Br3 Pb1 Br2 96.77(11) . . ?
Br1 Pb1 Br3 80.42(10) . 4_565 ?
Br1 Pb1 Br3 99.43(10) 4_566 4_565 ?
Br1 Pb1 Br1 97.00(13) . 4_566 ?
Br1 Pb1 Br2 82.62(12) . . ?
Br2 Pb1 Br3 81.11(10) . 4_565 ?
Br2 Pb1 Br3 99.43(10) 4_566 4_565 ?
Br2 Pb1 Br1 179.45(9) 4_566 . ?
Br2 Pb1 Br1 82.49(12) 4_566 4_566 ?
Br2 Pb1 Br1 179.29(9) . 4_566 ?
Br2 Pb1 Br2 97.89(13) 4_566 . ?
Pb1 Br3 Pb1 81.17(11) . 4_566 ?
Pb1 Br1 Pb1 81.23(10) . 4_565 ?
Pb1 Br2 Pb1 81.35(10) 4_565 . ?
C3 N1 C4 106(5) . . ?
C7 N1 C4 108(6) . . ?
C7 N1 C3 107(4) . . ?
C7 N1 C2 126(5) . . ?
C2 N1 C4 94(4) . . ?
C2 N1 C3 113(6) . . ?
C6 C5 C4 99(5) . . ?
C5 C6 C7 113(7) . . ?
N1 C4 C5 88(4) . . ?
C6 C7 N1 105(6) . . ?
N1 C2 C1 103(4) . . ?
C3A N1A C7A 109(5) . . ?
C4A N1A C3A 106(4) . . ?
C4A N1A C7A 109(6) . . ?
C4A N1A C2A 123(5) . . ?
C2A N1A C3A 114(6) . . ?
C2A N1A C7A 95(4) . . ?
C5A C4A N1A 101(6) . . ?
C6A C5A C4A 112(7) . . ?
C5A C6A C7A 102(6) . . ?
N1A C7A C6A 90(4) . . ?
N1A C2A C1A 101(4) . . ?

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
C5 C6 C7 N1 40(8) . . . . ?
C6 C5 C4 N1 44(6) . . . . ?
C4 N1 C7 C6 -1(6) . . . . ?
C4 N1 C2 C1 -159(4) . . . . ?
C4 C5 C6 C7 -55(7) . . . . ?
C3 N1 C4 C5 92(5) . . . . ?
C3 N1 C7 C6 -114(7) . . . . ?
C3 N1 C2 C1 -50(6) . . . . ?
C7 N1 C4 C5 -22(5) . . . . ?
C7 N1 C2 C1 86(7) . . . . ?
C2 N1 C4 C5 -152(5) . . . . ?
C2 N1 C7 C6 108(7) . . . . ?
N1A C4A C5A C6A -51(8) . . . . ?
C3A N1A C4A C5A -97(7) . . . . ?
C3A N1A C7A C6A 119(6) . . . . ?
C3A N1A C2A C1A 28(8) . . . . ?
C4A N1A C7A C6A 4(6) . . . . ?
C4A N1A C2A C1A 159(7) . . . . ?
C4A C5A C6A C7A 54(8) . . . . ?
C5A C6A C7A N1A -32(7) . . . . ?
C7A N1A C4A C5A 20(6) . . . . ?
C7A N1A C2A C1A -85(6) . . . . ?
C2A N1A C4A C5A 129(8) . . . . ?
C2A N1A C7A C6A -123(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_RINTA01_EMPPbBr3_373K       
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The high Rint value is caused by the poor crystal data quality.
;
_vrf_PLAT020_EMPPbBr3_373K       
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.198 Report
RESPONSE: The high Rint value is caused by the poor crystal data quality.
;
# end Validation Reply Form
