# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_cmp1
_database_code_depnum_ccdc_archive 'CCDC 2296329'
loop_
_audit_author_name
_audit_author_address
'Guang-Ning Liu'
;University of Jinan
China
;
_audit_update_record             
;
2023-09-21 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_audit_creation_date             2023-09-20
_chemical_oxdiff_formula         'C H N S Br Pb'
_diffrn_orient_matrix_UB_11      0.0766429000
_diffrn_orient_matrix_UB_12      -0.0300414000
_diffrn_orient_matrix_UB_13      0.0119650000
_diffrn_orient_matrix_UB_21      0.0443052000
_diffrn_orient_matrix_UB_22      0.0267179000
_diffrn_orient_matrix_UB_23      -0.0366035000
_diffrn_orient_matrix_UB_31      0.0239828000
_diffrn_orient_matrix_UB_32      0.0462200000
_diffrn_orient_matrix_UB_33      0.0288766000
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_audit_creation_method           
;
FinalCif V106 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C8 H8 Br3 N Pb S'
_chemical_formula_moiety         'Br3 Pb, C8 H8 N S'
_chemical_formula_weight         597.13
_chemical_melting_point          ?
_exptl_crystal_colour_primary    colourless
_chemical_absolute_configuration ?
_space_group_crystal_system      orthorhombic
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_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 6.163
_oxdiff_exptl_absorpt_empirical_full_min 0.451
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   7.7383(4)
_cell_length_b                   11.5787(7)
_cell_length_c                   14.7269(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1319.52(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1992
_cell_measurement_theta_min      3.2240
_cell_measurement_theta_max      28.5100
_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.006
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    21.992
_vrf_PLAT342_19                  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04667 Ang.  
RESPONSE: The presence of the heavy atom of Pb in the asymmetric unit distorts
the positions of lighter atoms, hereby lowering the precision of C-C bonds.
;
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.09374
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_ambient_temperature_device_make ?
_diffrn_radiation_probe          x-ray
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0355
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00  88.00   1.00   20.00    --   15.86 178.00  90.00   53
  2  ω     41.00  88.00   1.00   20.00    --   15.86 178.00 -90.00   47
  3  ω     35.00  80.00   1.00   20.00    --   15.86 178.00-180.00   45
  4  ω    -24.00  13.00   1.00   20.00    --  -16.95 -99.00 -90.00   37
  5  ω     15.00  55.00   1.00   20.00    --   15.70 -99.00  30.00   40
  6  ω    -11.00  42.00   1.00   20.00    --   15.70  77.00-180.00   53
;
_diffrn_reflns_number            6548
_diffrn_reflns_av_unetI/netI     0.1140
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_theta_min         3.166
_diffrn_reflns_theta_max         25.338
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2397
_reflns_number_gt                1541
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.995
_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.
;
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0394P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         2397
_refine_ls_number_parameters     128
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1111
_refine_ls_wR_factor_gt          0.1027
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_restrained_S_all      0.914
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         4.290
_refine_diff_density_min         -1.914
_refine_diff_density_rms         0.280
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_Flack   -0.012(19)
_refine_ls_abs_structure_details 
;
 Flack x determined using 468 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;

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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_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 0.07595(11) 0.75031(12) 0.50113(8) 0.0322(3) Uani 1 1 d . . . . .
Br1 Br 0.3080(5) 0.6881(2) 0.34934(16) 0.0428(8) Uani 1 1 d . . . . .
Br2 Br 0.3058(5) 0.6100(2) 0.61862(18) 0.0461(8) Uani 1 1 d . . . . .
Br3 Br -0.1525(4) 0.5520(2) 0.46380(19) 0.0423(7) Uani 1 1 d . . . . .
S1 S 0.9885(12) 0.7479(12) 0.1756(6) 0.076(3) Uani 1 1 d . . . . .
N1 N 0.753(4) 0.604(3) 0.1998(18) 0.061(8) Uani 1 1 d . . . . .
C1 C 0.676(5) 0.685(2) 0.1520(16) 0.039(7) Uani 1 1 d . . . . .
C2 C 0.504(4) 0.691(3) 0.1245(19) 0.044(8) Uani 1 1 d . U . . .
H2 H 0.4275 0.6308 0.1364 0.052 Uiso 1 1 calc R . . . .
C3 C 0.452(4) 0.790(3) 0.0786(19) 0.045(8) Uani 1 1 d . . . . .
H3 H 0.3388 0.7929 0.0580 0.054 Uiso 1 1 calc R . . . .
C4 C 0.551(5) 0.877(3) 0.063(2) 0.070(11) Uani 1 1 d . U . . .
H4 H 0.5056 0.9443 0.0368 0.085 Uiso 1 1 calc R . . . .
C5 C 0.731(5) 0.870(3) 0.085(2) 0.059(10) Uani 1 1 d . . . . .
H5 H 0.8073 0.9272 0.0670 0.071 Uiso 1 1 calc R . . . .
C6 C 0.788(4) 0.775(2) 0.1349(19) 0.045(8) Uani 1 1 d . . . . .
C7 C 0.915(5) 0.618(3) 0.218(2) 0.057(10) Uani 1 1 d . . . . .
H7 H 0.9828 0.5657 0.2498 0.069 Uiso 1 1 calc R . . . .
C8 C 0.667(5) 0.492(2) 0.229(2) 0.076(11) Uani 1 1 d . . . . .
H8A H 0.7524 0.4403 0.2537 0.113 Uiso 1 1 calc GR . . . .
H8B H 0.6136 0.4559 0.1771 0.113 Uiso 1 1 calc GR . . . .
H8C H 0.5810 0.5076 0.2740 0.113 Uiso 1 1 calc GR . . . .


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 2.957(3) . ?
Pb1 Br1 3.107(3) 4_466 ?
Pb1 Br2 3.177(3) 4_466 ?
Pb1 Br2 2.966(3) . ?
Pb1 Br3 3.150(3) 4_566 ?
Pb1 Br3 2.950(3) . ?
Br1 Pb1 3.108(3) 4_566 ?
Br2 Pb1 3.177(3) 4_566 ?
Br3 Pb1 3.150(3) 4_466 ?
S1 C6 1.69(3) . ?
S1 C7 1.72(4) . ?
N1 C1 1.32(4) . ?
N1 C7 1.29(4) . ?
N1 C8 1.52(4) . ?
C1 C2 1.39(4) . ?
C1 C6 1.38(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.39(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.29(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.43(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.39(4) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 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 175.56(11) . 4_466 ?
Br1 Pb1 Br2 80.65(8) 4_466 4_466 ?
Br1 Pb1 Br2 86.76(9) . . ?
Br1 Pb1 Br2 95.97(9) . 4_466 ?
Br1 Pb1 Br3 99.33(8) 4_466 4_566 ?
Br1 Pb1 Br3 84.02(8) . 4_566 ?
Br2 Pb1 Br1 96.45(9) . 4_466 ?
Br2 Pb1 Br2 175.68(11) . 4_466 ?
Br2 Pb1 Br3 84.39(8) . 4_566 ?
Br3 Pb1 Br1 84.89(8) . 4_466 ?
Br3 Pb1 Br1 91.92(9) . . ?
Br3 Pb1 Br2 92.39(9) . . ?
Br3 Pb1 Br2 84.18(8) . 4_466 ?
Br3 Pb1 Br2 99.21(8) 4_566 4_466 ?
Br3 Pb1 Br3 174.94(9) . 4_566 ?
Pb1 Br1 Pb1 79.25(6) . 4_566 ?
Pb1 Br2 Pb1 77.99(6) . 4_566 ?
Pb1 Br3 Pb1 78.67(6) . 4_466 ?
C6 S1 C7 89.3(17) . . ?
C1 N1 C8 124(3) . . ?
C7 N1 C1 117(4) . . ?
C7 N1 C8 119(3) . . ?
N1 C1 C2 128(3) . . ?
N1 C1 C6 111(3) . . ?
C6 C1 C2 121(3) . . ?
C1 C2 H2 121.4 . . ?
C3 C2 C1 117(3) . . ?
C3 C2 H2 121.4 . . ?
C2 C3 H3 117.7 . . ?
C4 C3 C2 125(3) . . ?
C4 C3 H3 117.7 . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 119(3) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 120.6 . . ?
C6 C5 C4 119(3) . . ?
C6 C5 H5 120.6 . . ?
C1 C6 S1 112(2) . . ?
C1 C6 C5 119(3) . . ?
C5 C6 S1 129(2) . . ?
S1 C7 H7 124.5 . . ?
N1 C7 S1 111(3) . . ?
N1 C7 H7 124.5 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_cmp2
_database_code_depnum_ccdc_archive 'CCDC 2296330'
loop_
_audit_author_name
_audit_author_address
'Guang-Ning Liu'
;University of Jinan
China
;
_audit_update_record             
;
2023-09-21 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_audit_creation_date             2023-09-20
_chemical_oxdiff_formula         'C H N S Br Pb'
_diffrn_orient_matrix_UB_11      -0.0172086000
_diffrn_orient_matrix_UB_12      0.0594442000
_diffrn_orient_matrix_UB_13      -0.0218828000
_diffrn_orient_matrix_UB_21      0.0358088000
_diffrn_orient_matrix_UB_22      0.0368702000
_diffrn_orient_matrix_UB_23      -0.0066077000
_diffrn_orient_matrix_UB_31      0.0051855000
_diffrn_orient_matrix_UB_32      -0.0576396000
_diffrn_orient_matrix_UB_33      -0.0268689000
_audit_creation_method           
;
FinalCif V106 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C9 H10 Br3 N Pb S'
_chemical_formula_moiety         'Br3 Pb, C9 H10 N S'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_chemical_formula_weight         611.16
_chemical_melting_point          ?
_exptl_crystal_colour_primary    yellow
_space_group_crystal_system      orthorhombic
_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. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   17.7030(10)
_cell_length_b                   7.8270(3)
_cell_length_c                   20.1031(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2785.5(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2021
_cell_measurement_theta_min      4.1490
_cell_measurement_theta_max      28.6940
_exptl_crystal_description       prism
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.915
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_vrf_PLAT342_61                  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02286 Ang.  
RESPONSE: The presence of the heavy atom of Pb in the asymmetric unit distorts
the positions of lighter atoms, hereby lowering the precision of C-C bonds.
;
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    20.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.07230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   0.044
_shelx_estimated_absorpt_T_max   0.422
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_ambient_temperature_device_make ?
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0355
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   35.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  178.0000  -90.0000 53

#__ type_ start__ end____ width___ exp.time_
  2 omega  -53.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -37.0000  -30.0000 86

#__ type_ start__ end____ width___ exp.time_
  3 omega  -83.00  -48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9507  -57.0000  120.0000 35
;
_diffrn_reflns_number            7972
_diffrn_reflns_av_unetI/netI     0.1333
_diffrn_reflns_av_R_equivalents  0.1061
_diffrn_reflns_theta_min         3.067
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2546
_reflns_number_gt                1292
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_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.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0504P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         2546
_refine_ls_number_parameters     138
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0667
_refine_ls_wR_factor_ref         0.1604
_refine_ls_wR_factor_gt          0.1294
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_restrained_S_all      0.910
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.555
_refine_diff_density_min         -3.082
_refine_diff_density_rms         0.435
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00061(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_
_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 0.74687(4) 0.13602(7) 0.41722(3) 0.0333(3) Uani 1 1 d . . . . .
Br1 Br 0.88200(12) 0.3617(2) 0.41007(9) 0.0425(5) Uani 1 1 d . . . . .
Br2 Br 0.68352(13) 0.3756(2) 0.31827(8) 0.0443(6) Uani 1 1 d . . . . .
Br3 Br 0.67680(12) 0.3833(2) 0.51501(8) 0.0416(5) Uani 1 1 d . . . . .
S1 S 0.5070(3) 0.2626(5) 0.4474(2) 0.0441(13) Uani 1 1 d . . . . .
N1 N 0.4575(10) 0.4694(14) 0.3619(6) 0.040(4) Uani 1 1 d . . . . .
C1 C 0.4274(12) 0.204(2) 0.4029(8) 0.042(5) Uani 1 1 d . . . . .
C2 C 0.3857(13) 0.051(2) 0.4060(8) 0.044(5) Uani 1 1 d . . . . .
H2 H 0.3978 -0.0327 0.4369 0.053 Uiso 1 1 calc R . . . .
C3 C 0.3291(15) 0.029(2) 0.3644(8) 0.058(7) Uani 1 1 d . . . . .
H3 H 0.3032 -0.0739 0.3650 0.069 Uiso 1 1 calc R . . . .
C4 C 0.3058(14) 0.1595(19) 0.3181(8) 0.049(6) Uani 1 1 d . . . . .
H4 H 0.2639 0.1452 0.2908 0.059 Uiso 1 1 calc R . . . .
C5 C 0.3493(11) 0.308(2) 0.3163(8) 0.036(4) Uani 1 1 d . . . . .
H5 H 0.3373 0.3931 0.2859 0.043 Uiso 1 1 calc R . . . .
C6 C 0.4087(11) 0.3297(19) 0.3581(8) 0.031(4) Uani 1 1 d . U . . .
C7 C 0.5087(12) 0.446(2) 0.4075(7) 0.038(4) Uani 1 1 d . U . . .
H7 H 0.5447 0.5292 0.4170 0.046 Uiso 1 1 calc R . . . .
C8 C 0.4507(14) 0.6242(17) 0.3192(8) 0.050(6) Uani 1 1 d . . . . .
H8A H 0.4794 0.7169 0.3389 0.060 Uiso 1 1 calc R . . . .
H8B H 0.3982 0.6590 0.3171 0.060 Uiso 1 1 calc R . . . .
C9 C 0.4790(14) 0.592(2) 0.2506(8) 0.058(6) Uani 1 1 d . . . . .
H9A H 0.4683 0.6892 0.2231 0.088 Uiso 1 1 calc GR . . . .
H9B H 0.4544 0.4929 0.2327 0.088 Uiso 1 1 calc GR . . . .
H9C H 0.5325 0.5730 0.2519 0.088 Uiso 1 1 calc GR . . . .


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 2.977(2) . ?
Pb1 Br1 3.136(2) 8_755 ?
Pb1 Br2 3.1032(18) 8_755 ?
Pb1 Br2 2.9550(17) . ?
Pb1 Br3 3.0989(18) 8_755 ?
Pb1 Br3 3.0248(18) . ?
Br1 Pb1 3.136(2) 8_765 ?
Br2 Pb1 3.1032(18) 8_765 ?
Br3 Pb1 3.0989(18) 8_765 ?
S1 C1 1.73(2) . ?
S1 C7 1.645(17) . ?
N1 C6 1.40(2) . ?
N1 C7 1.30(2) . ?
N1 C8 1.490(17) . ?
C1 C2 1.40(2) . ?
C1 C6 1.37(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.31(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.44(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.39(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.36(2) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.49(2) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 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 171.30(6) . 8_755 ?
Br1 Pb1 Br2 92.27(5) . 8_755 ?
Br1 Pb1 Br3 88.93(5) . . ?
Br1 Pb1 Br3 93.38(5) . 8_755 ?
Br2 Pb1 Br1 97.33(6) . 8_755 ?
Br2 Pb1 Br1 84.02(5) . . ?
Br2 Pb1 Br1 79.04(5) 8_755 8_755 ?
Br2 Pb1 Br2 97.82(6) . 8_755 ?
Br2 Pb1 Br3 82.87(5) . . ?
Br2 Pb1 Br3 176.07(6) . 8_755 ?
Br3 Pb1 Br1 84.79(5) 8_755 8_755 ?
Br3 Pb1 Br1 99.76(5) . 8_755 ?
Br3 Pb1 Br2 79.30(5) 8_755 8_755 ?
Br3 Pb1 Br2 178.68(5) . 8_755 ?
Br3 Pb1 Br3 100.07(6) . 8_755 ?
Pb1 Br1 Pb1 79.60(5) . 8_765 ?
Pb1 Br2 Pb1 80.48(4) . 8_765 ?
Pb1 Br3 Pb1 79.47(4) . 8_765 ?
C7 S1 C1 89.7(9) . . ?
C6 N1 C8 123.8(16) . . ?
C7 N1 C6 111.0(14) . . ?
C7 N1 C8 125.2(17) . . ?
C2 C1 S1 129.1(14) . . ?
C6 C1 S1 110.1(13) . . ?
C6 C1 C2 120.7(18) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 C1 118.9(17) . . ?
C3 C2 H2 120.5 . . ?
C2 C3 H3 118.8 . . ?
C2 C3 C4 122.4(17) . . ?
C4 C3 H3 118.8 . . ?
C3 C4 H4 121.7 . . ?
C5 C4 C3 116.6(19) . . ?
C5 C4 H4 121.7 . . ?
C4 C5 H5 119.4 . . ?
C6 C5 C4 121.2(16) . . ?
C6 C5 H5 119.4 . . ?
C1 C6 N1 112.2(16) . . ?
C5 C6 N1 127.8(15) . . ?
C5 C6 C1 120.0(16) . . ?
S1 C7 H7 121.5 . . ?
N1 C7 S1 117.0(15) . . ?
N1 C7 H7 121.5 . . ?
N1 C8 H8A 109.3 . . ?
N1 C8 H8B 109.3 . . ?
N1 C8 C9 111.6(14) . . ?
H8A C8 H8B 108.0 . . ?
C9 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_cmp4
_database_code_depnum_ccdc_archive 'CCDC 2296332'
loop_
_audit_author_name
_audit_author_address
'Guang-Ning Liu'
;University of Jinan
China
;
_audit_update_record             
;
2023-09-21 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_audit_creation_date             2023-09-20
_chemical_oxdiff_formula         'C H P Br Pb'
_diffrn_orient_matrix_UB_11      -0.0187265000
_diffrn_orient_matrix_UB_12      0.0249888000
_diffrn_orient_matrix_UB_13      0.0220311000
_diffrn_orient_matrix_UB_21      0.0116363000
_diffrn_orient_matrix_UB_22      -0.0670550000
_diffrn_orient_matrix_UB_23      0.0164743000
_diffrn_orient_matrix_UB_31      0.0223022000
_diffrn_orient_matrix_UB_32      0.0560487000
_diffrn_orient_matrix_UB_33      0.0098812000
_audit_creation_method           
;
FinalCif V106 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C19 H18 Br3 P Pb'
_chemical_formula_moiety         'Br3 Pb, C19 H18 P'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_chemical_formula_weight         724.22
_chemical_melting_point          ?
_exptl_crystal_colour_primary    red
_space_group_crystal_system      orthorhombic
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
3.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.601(2)
_cell_length_b                   7.8074(7)
_cell_length_c                   24.284(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4285.1(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3661
_cell_measurement_theta_min      3.8520
_cell_measurement_theta_max      28.5050
_exptl_crystal_description       prism
_exptl_crystal_colour            'clear light red'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.245
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_vrf_PLAT342_61                  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02439 Ang.  
RESPONSE: The presence of the heavy atom of Pb in the asymmetric unit distorts
the positions of lighter atoms, hereby lowering the precision of C-C bonds.
;
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    13.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.11823
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_ambient_temperature_device_make ?
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0355
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -51.00   33.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -57.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
  2 omega  -25.00   55.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -99.0000  -90.0000 80

#__ type_ start__ end____ width___ exp.time_
  3 omega   35.00   88.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  178.0000  120.0000 53

#__ type_ start__ end____ width___ exp.time_
  4 omega  -11.00   14.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569   77.0000 -150.0000 25
;
_diffrn_reflns_number            16987
_diffrn_reflns_av_unetI/netI     0.1011
_diffrn_reflns_av_R_equivalents  0.1042
_diffrn_reflns_theta_min         3.168
_diffrn_reflns_theta_max         25.318
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3915
_reflns_number_gt                2336
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_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.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0726P)²+13.1542P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         3915
_refine_ls_number_parameters     218
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0708
_refine_ls_wR_factor_ref         0.1775
_refine_ls_wR_factor_gt          0.1525
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.020
_refine_diff_density_min         -2.040
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

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'
P P 0.1023 0.0942 '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'

_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_
_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 0.24928(2) 0.16653(7) 0.58954(2) 0.0378(2) Uani 1 1 d . . . . .
Br1 Br 0.31030(6) -0.08018(19) 0.66870(7) 0.0494(4) Uani 1 1 d . . . . .
Br2 Br 0.35351(6) 0.4123(2) 0.59489(7) 0.0538(5) Uani 1 1 d . . . . .
Br3 Br 0.29073(7) -0.08081(18) 0.50109(6) 0.0482(4) Uani 1 1 d . . . . .
P1 P 0.40090(15) 0.4339(5) 0.38278(17) 0.0395(9) Uani 1 1 d . . . . .
C1 C 0.4350(6) 0.5921(16) 0.3399(6) 0.039(3) Uani 1 1 d . . . . .
C2 C 0.4942(6) 0.6347(19) 0.3471(7) 0.053(4) Uani 1 1 d . . . . .
H2 H 0.5173 0.5744 0.3721 0.064 Uiso 1 1 calc R . . . .
C3 C 0.5181(8) 0.765(2) 0.3173(8) 0.062(5) Uani 1 1 d . . . . .
H3 H 0.5574 0.7956 0.3231 0.075 Uiso 1 1 calc R . . . .
C4 C 0.4860(8) 0.852(2) 0.2795(9) 0.066(5) Uani 1 1 d . . . . .
H4 H 0.5034 0.9396 0.2593 0.079 Uiso 1 1 calc R . . . .
C5 C 0.4271(8) 0.810(2) 0.2706(9) 0.073(6) Uani 1 1 d . U . . .
H5 H 0.4050 0.8684 0.2442 0.087 Uiso 1 1 calc R . . . .
C6 C 0.4017(7) 0.6807(17) 0.3017(8) 0.062(5) Uani 1 1 d . U . . .
H6 H 0.3620 0.6533 0.2968 0.075 Uiso 1 1 calc R . . . .
C7 C 0.3581(5) 0.2803(17) 0.3426(6) 0.039(4) Uani 1 1 d . . . . .
C8 C 0.3557(6) 0.2810(19) 0.2866(7) 0.050(4) Uani 1 1 d . . . . .
H8 H 0.3767 0.3624 0.2667 0.061 Uiso 1 1 calc R . . . .
C9 C 0.3224(7) 0.162(2) 0.2601(7) 0.059(4) Uani 1 1 d . . . . .
H9 H 0.3208 0.1607 0.2218 0.071 Uiso 1 1 calc R . . . .
C10 C 0.2911(6) 0.0428(18) 0.2899(8) 0.058(5) Uani 1 1 d . . . . .
H10 H 0.2673 -0.0361 0.2716 0.069 Uiso 1 1 calc R . . . .
C11 C 0.2945(7) 0.039(2) 0.3468(8) 0.058(5) Uani 1 1 d . . . . .
H11 H 0.2744 -0.0453 0.3663 0.070 Uiso 1 1 calc R . . . .
C12 C 0.3274(7) 0.1592(18) 0.3746(7) 0.054(4) Uani 1 1 d . . . . .
H12 H 0.3293 0.1603 0.4128 0.064 Uiso 1 1 calc R . . . .
C13 C 0.4577(5) 0.3188(17) 0.4190(7) 0.039(4) Uani 1 1 d . . . . .
C14 C 0.4613(8) 0.3224(19) 0.4755(8) 0.058(5) Uani 1 1 d . . . . .
H14 H 0.4338 0.3838 0.4960 0.069 Uiso 1 1 calc R . . . .
C15 C 0.5065(8) 0.2333(19) 0.5016(8) 0.069(5) Uani 1 1 d . . . . .
H15 H 0.5083 0.2300 0.5398 0.083 Uiso 1 1 calc R . . . .
C16 C 0.5477(9) 0.152(2) 0.4713(11) 0.079(7) Uani 1 1 d . . . . .
H16 H 0.5788 0.0971 0.4892 0.094 Uiso 1 1 calc R . . . .
C17 C 0.5453(8) 0.147(2) 0.4151(11) 0.084(7) Uani 1 1 d . . . . .
H17 H 0.5738 0.0868 0.3952 0.101 Uiso 1 1 calc R . . . .
C18 C 0.4992(6) 0.2330(19) 0.3875(8) 0.060(4) Uani 1 1 d . . . . .
H18 H 0.4968 0.2324 0.3493 0.072 Uiso 1 1 calc R . . . .
C19 C 0.3528(6) 0.5386(19) 0.4307(8) 0.059(5) Uani 1 1 d . . . . .
H19A H 0.3260 0.6120 0.4111 0.088 Uiso 1 1 calc GR . . . .
H19B H 0.3758 0.6057 0.4559 0.088 Uiso 1 1 calc GR . . . .
H19C H 0.3307 0.4542 0.4508 0.088 Uiso 1 1 calc GR . . . .


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 3.0690(15) 7_665 ?
Pb1 Br1 3.0507(16) . ?
Pb1 Br2 3.0410(16) . ?
Pb1 Br2 3.0583(16) 7_655 ?
Pb1 Br3 3.0366(15) . ?
Pb1 Br3 3.0534(16) 7_665 ?
Br1 Pb1 3.0691(15) 7_655 ?
Br2 Pb1 3.0584(15) 7_665 ?
Br3 Pb1 3.0534(16) 7_655 ?
P1 C1 1.790(13) . ?
P1 C7 1.824(14) . ?
P1 C13 1.797(14) . ?
P1 C19 1.791(15) . ?
C1 C2 1.390(19) . ?
C1 C6 1.38(2) . ?
C2 C3 1.36(2) . ?
C3 C4 1.35(2) . ?
C4 C5 1.39(2) . ?
C5 C6 1.39(2) . ?
C7 C8 1.36(2) . ?
C7 C12 1.406(19) . ?
C8 C9 1.36(2) . ?
C9 C10 1.37(2) . ?
C10 C11 1.38(2) . ?
C11 C12 1.37(2) . ?
C13 C14 1.37(2) . ?
C13 C18 1.383(19) . ?
C14 C15 1.39(2) . ?
C15 C16 1.35(2) . ?
C16 C17 1.37(3) . ?
C17 C18 1.41(2) . ?

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 102.15(5) . 7_665 ?
Br1 Pb1 Br2 84.65(4) . 7_655 ?
Br1 Pb1 Br3 170.09(4) . 7_665 ?
Br2 Pb1 Br1 84.63(4) . 7_665 ?
Br2 Pb1 Br1 91.22(4) . . ?
Br2 Pb1 Br1 93.34(4) 7_655 7_665 ?
Br2 Pb1 Br2 174.93(7) . 7_655 ?
Br2 Pb1 Br3 81.48(4) . 7_665 ?
Br3 Pb1 Br1 84.53(4) . . ?
Br3 Pb1 Br1 83.94(4) 7_665 7_665 ?
Br3 Pb1 Br1 171.19(4) . 7_665 ?
Br3 Pb1 Br2 81.47(4) . 7_655 ?
Br3 Pb1 Br2 102.95(4) 7_665 7_655 ?
Br3 Pb1 Br2 101.10(4) . . ?
Br3 Pb1 Br3 90.26(5) . 7_665 ?
Pb1 Br1 Pb1 79.27(4) . 7_655 ?
Pb1 Br2 Pb1 79.59(3) . 7_665 ?
Pb1 Br3 Pb1 79.74(4) . 7_655 ?
C1 P1 C7 111.8(7) . . ?
C1 P1 C13 108.8(6) . . ?
C1 P1 C19 108.9(7) . . ?
C13 P1 C7 108.2(6) . . ?
C19 P1 C7 109.0(7) . . ?
C19 P1 C13 110.2(8) . . ?
C2 C1 P1 120.4(12) . . ?
C6 C1 P1 120.2(11) . . ?
C6 C1 C2 119.2(13) . . ?
C3 C2 C1 119.6(16) . . ?
C4 C3 C2 121.5(16) . . ?
C3 C4 C5 120.3(16) . . ?
C6 C5 C4 118.8(17) . . ?
C1 C6 C5 120.5(15) . . ?
C8 C7 P1 123.5(11) . . ?
C8 C7 C12 122.3(14) . . ?
C12 C7 P1 114.1(12) . . ?
C9 C8 C7 119.5(15) . . ?
C8 C9 C10 119.9(16) . . ?
C9 C10 C11 120.8(14) . . ?
C12 C11 C10 120.4(14) . . ?
C11 C12 C7 117.0(15) . . ?
C14 C13 P1 121.3(12) . . ?
C14 C13 C18 121.4(15) . . ?
C18 C13 P1 117.2(13) . . ?
C13 C14 C15 119.3(17) . . ?
C16 C15 C14 120(2) . . ?
C15 C16 C17 122(2) . . ?
C16 C17 C18 119(2) . . ?
C13 C18 C17 118.1(19) . . ?

_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_cmp5
_database_code_depnum_ccdc_archive 'CCDC 2296333'
loop_
_audit_author_name
_audit_author_address
'Guang-Ning Liu'
;University of Jinan
China
;
_audit_update_record             
;
2023-09-21 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_audit_creation_date             2023-09-20
_chemical_oxdiff_formula         'C H P Br Pb'
_diffrn_orient_matrix_UB_11      0.0127732000
_diffrn_orient_matrix_UB_12      0.0529725000
_diffrn_orient_matrix_UB_13      -0.0195801000
_diffrn_orient_matrix_UB_21      0.0233334000
_diffrn_orient_matrix_UB_22      0.0221109000
_diffrn_orient_matrix_UB_23      0.0177594000
_diffrn_orient_matrix_UB_31      0.0174438000
_diffrn_orient_matrix_UB_32      -0.0683628000
_diffrn_orient_matrix_UB_33      -0.0094187000
_audit_creation_method           
;
FinalCif V106 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C20 H20 Br3 P Pb'
_chemical_formula_moiety         'Br3 Pb, C20 H20 P'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_chemical_formula_weight         738.25
_chemical_melting_point          ?
_exptl_crystal_colour_primary    colourless
_space_group_crystal_system      orthorhombic
_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:
 C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.2970(12)
_cell_length_b                   7.9480(4)
_cell_length_c                   25.2706(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4478.4(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1791
_cell_measurement_theta_min      3.2290
_cell_measurement_theta_max      27.2770
_exptl_crystal_description       prism
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.190
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_vrf_PLAT342_61                  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02011 Ang.  
RESPONSE: The presence of the heavy atom of Pb in the asymmetric unit distorts
the positions of lighter atoms, hereby lowering the precision of C-C bonds.
;
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    12.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.20324
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_ambient_temperature_device_make ?
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0355
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   35.00   88.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7007  178.0000   90.0000 53

#__ type_ start__ end____ width___ exp.time_
  2 omega  -25.00   52.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7007  -99.0000  -90.0000 77

#__ type_ start__ end____ width___ exp.time_
  3 omega  -15.00   28.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7007  -37.0000    0.0000 43
;
_diffrn_reflns_number            13237
_diffrn_reflns_av_unetI/netI     0.0977
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_theta_min         3.180
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4151
_reflns_number_gt                2156
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_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.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0141P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4151
_refine_ls_number_parameters     227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1022
_refine_ls_wR_factor_gt          0.0769
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.241
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

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'
P P 0.1023 0.0942 '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'

_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_
_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 0.74974(2) 0.74398(6) 0.41272(2) 0.03738(16) Uani 1 1 d . . . . .
Br1 Br 0.68996(6) 0.98168(17) 0.33623(4) 0.0465(3) Uani 1 1 d . . . . .
Br2 Br 0.64379(5) 0.52209(17) 0.40969(5) 0.0477(3) Uani 1 1 d . . . . .
Br3 Br 0.70386(6) 0.97218(17) 0.49569(4) 0.0485(4) Uani 1 1 d . . . . .
P1 P 0.60385(15) 0.6378(4) 0.62802(12) 0.0387(8) Uani 1 1 d . . . . .
C1 C 0.5488(6) 0.7309(15) 0.5868(5) 0.044(3) Uani 1 1 d . . . . .
C2 C 0.5461(6) 0.7040(16) 0.5324(5) 0.049(4) Uani 1 1 d . . . . .
H2 H 0.5763 0.6436 0.5156 0.059 Uiso 1 1 calc R . . . .
C3 C 0.4986(8) 0.7670(19) 0.5033(7) 0.070(5) Uani 1 1 d . . . . .
H3 H 0.4969 0.7511 0.4669 0.084 Uiso 1 1 calc R . . . .
C4 C 0.4545(7) 0.8528(18) 0.5289(8) 0.069(5) Uani 1 1 d . . . . .
H4 H 0.4219 0.8922 0.5095 0.083 Uiso 1 1 calc R . . . .
C5 C 0.4565(7) 0.883(2) 0.5823(7) 0.072(5) Uani 1 1 d . . . . .
H5 H 0.4265 0.9450 0.5988 0.087 Uiso 1 1 calc R . . . .
C6 C 0.5024(6) 0.8211(16) 0.6103(5) 0.051(4) Uani 1 1 d . . . . .
H6 H 0.5034 0.8391 0.6467 0.061 Uiso 1 1 calc R . . . .
C7 C 0.5675(5) 0.4787(16) 0.6672(4) 0.040(3) Uani 1 1 d . . . . .
C8 C 0.5111(6) 0.4192(17) 0.6546(5) 0.054(4) Uani 1 1 d . . . . .
H8 H 0.4901 0.4668 0.6265 0.065 Uiso 1 1 calc R . . . .
C9 C 0.4860(7) 0.292(2) 0.6828(6) 0.073(5) Uani 1 1 d . . . . .
H9 H 0.4476 0.2540 0.6745 0.088 Uiso 1 1 calc R . . . .
C10 C 0.5175(9) 0.218(2) 0.7235(7) 0.077(5) Uani 1 1 d . . . . .
H10 H 0.5003 0.1300 0.7423 0.093 Uiso 1 1 calc R . . . .
C11 C 0.5720(8) 0.2710(18) 0.7366(6) 0.065(5) Uani 1 1 d . . . . .
H11 H 0.5921 0.2221 0.7650 0.078 Uiso 1 1 calc R . . . .
C12 C 0.5987(6) 0.3975(17) 0.7083(5) 0.052(4) Uani 1 1 d . . . . .
H12 H 0.6378 0.4300 0.7163 0.063 Uiso 1 1 calc R . . . .
C13 C 0.6400(6) 0.7990(15) 0.6678(5) 0.044(3) Uani 1 1 d . . . . .
C14 C 0.6430(6) 0.7955(16) 0.7226(5) 0.044(3) Uani 1 1 d . . . . .
H14 H 0.6239 0.7105 0.7415 0.052 Uiso 1 1 calc R . . . .
C15 C 0.6747(6) 0.9203(18) 0.7491(5) 0.055(4) Uani 1 1 d . . . . .
H15 H 0.6775 0.9179 0.7858 0.066 Uiso 1 1 calc R . . . .
C16 C 0.7017(6) 1.0452(17) 0.7215(6) 0.054(4) Uani 1 1 d . . . . .
H16 H 0.7238 1.1265 0.7394 0.065 Uiso 1 1 calc R . . . .
C17 C 0.6968(6) 1.0533(18) 0.6675(6) 0.058(4) Uani 1 1 d . . . . .
H17 H 0.7146 1.1414 0.6490 0.069 Uiso 1 1 calc R . . . .
C18 C 0.6658(6) 0.9315(17) 0.6407(5) 0.054(4) Uani 1 1 d . . . . .
H18 H 0.6620 0.9380 0.6041 0.065 Uiso 1 1 calc R . . . .
C19 C 0.6622(5) 0.5367(15) 0.5899(5) 0.046(3) Uani 1 1 d . . . . .
H19A H 0.6762 0.6149 0.5631 0.055 Uiso 1 1 calc R . . . .
H19B H 0.6957 0.5125 0.6131 0.055 Uiso 1 1 calc R . . . .
C20 C 0.6434(6) 0.3746(15) 0.5628(5) 0.056(4) Uani 1 1 d . . . . .
H20A H 0.6733 0.3427 0.5374 0.085 Uiso 1 1 calc GR . . . .
H20B H 0.6058 0.3915 0.5451 0.085 Uiso 1 1 calc GR . . . .
H20C H 0.6392 0.2872 0.5887 0.085 Uiso 1 1 calc GR . . . .


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 3.1449(13) 7_755 ?
Pb1 Br1 3.0137(13) . ?
Pb1 Br2 2.9491(13) . ?
Pb1 Br3 2.9551(13) . ?
Pb1 Br3 3.1832(13) 7_755 ?
Br1 Pb1 3.1448(13) 7_765 ?
Br3 Pb1 3.1832(13) 7_765 ?
P1 C1 1.772(13) . ?
P1 C7 1.798(12) . ?
P1 C13 1.817(13) . ?
P1 C19 1.808(11) . ?
C1 C2 1.394(16) . ?
C1 C6 1.391(15) . ?
C2 C3 1.383(17) . ?
C3 C4 1.360(19) . ?
C4 C5 1.37(2) . ?
C5 C6 1.338(18) . ?
C7 C8 1.382(16) . ?
C7 C12 1.406(15) . ?
C8 C9 1.360(18) . ?
C9 C10 1.377(19) . ?
C10 C11 1.327(19) . ?
C11 C12 1.371(17) . ?
C13 C14 1.386(15) . ?
C13 C18 1.382(16) . ?
C14 C15 1.390(16) . ?
C15 C16 1.355(17) . ?
C16 C17 1.371(17) . ?
C17 C18 1.368(17) . ?
C19 C20 1.518(15) . ?

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 102.15(4) . 7_755 ?
Br1 Pb1 Br3 79.40(3) 7_755 7_755 ?
Br1 Pb1 Br3 172.58(4) . 7_755 ?
Br2 Pb1 Br1 90.22(4) . . ?
Br2 Pb1 Br1 85.99(4) . 7_755 ?
Br2 Pb1 Br3 96.21(4) . . ?
Br2 Pb1 Br3 82.62(4) . 7_755 ?
Br3 Pb1 Br1 85.25(4) . . ?
Br3 Pb1 Br1 172.30(4) . 7_755 ?
Br3 Pb1 Br3 93.54(4) . 7_755 ?
Pb1 Br1 Pb1 80.34(3) . 7_765 ?
Pb1 Br3 Pb1 80.60(3) . 7_765 ?
C1 P1 C7 107.8(6) . . ?
C1 P1 C13 109.7(6) . . ?
C1 P1 C19 111.8(6) . . ?
C7 P1 C13 113.0(6) . . ?
C7 P1 C19 107.8(6) . . ?
C19 P1 C13 106.8(6) . . ?
C2 C1 P1 123.1(11) . . ?
C6 C1 P1 118.6(10) . . ?
C6 C1 C2 118.0(13) . . ?
C3 C2 C1 120.1(14) . . ?
C4 C3 C2 118.9(15) . . ?
C3 C4 C5 122.1(16) . . ?
C6 C5 C4 118.8(15) . . ?
C5 C6 C1 122.1(13) . . ?
C8 C7 P1 121.6(10) . . ?
C8 C7 C12 117.6(12) . . ?
C12 C7 P1 120.4(10) . . ?
C9 C8 C7 120.7(14) . . ?
C8 C9 C10 119.8(15) . . ?
C11 C10 C9 121.4(16) . . ?
C10 C11 C12 119.9(15) . . ?
C11 C12 C7 120.5(13) . . ?
C14 C13 P1 124.0(10) . . ?
C18 C13 P1 116.6(10) . . ?
C18 C13 C14 119.4(12) . . ?
C13 C14 C15 119.4(12) . . ?
C16 C15 C14 120.0(12) . . ?
C15 C16 C17 120.8(13) . . ?
C18 C17 C16 120.0(13) . . ?
C17 C18 C13 120.3(12) . . ?
C20 C19 P1 114.7(8) . . ?

####################################################################### 
# 
# 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_cmp3
_database_code_depnum_ccdc_archive 'CCDC 2296331'
loop_
_audit_author_name
_audit_author_address
'Guang-Ning Liu'
;University of Jinan
China
;
_audit_update_record             
;
2023-09-21 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_audit_creation_date             2023-09-20
_chemical_oxdiff_formula         'C H N S Br Pb'
_diffrn_orient_matrix_UB_11      0.0750795000
_diffrn_orient_matrix_UB_12      0.0062571000
_diffrn_orient_matrix_UB_13      -0.0099777000
_diffrn_orient_matrix_UB_21      0.0081234000
_diffrn_orient_matrix_UB_22      -0.0307687000
_diffrn_orient_matrix_UB_23      -0.0118533000
_diffrn_orient_matrix_UB_31      -0.0262791000
_diffrn_orient_matrix_UB_32      0.0083367000
_diffrn_orient_matrix_UB_33      -0.0362487000
_audit_creation_method           
;
FinalCif V106 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C20 H24 Br8 N2 Pb3 S2'
_chemical_formula_moiety         'Br8 Pb3, 2(C10 H12 N S)'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_chemical_formula_weight         1617.38
_chemical_melting_point          ?
_exptl_crystal_colour_primary    colourless
_space_group_crystal_system      monoclinic
_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
 C9, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C9 \\sim C10: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C18(H18A,H18B), C19(H19A,H19B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
_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.
;

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                   8.8791(4)
_cell_length_b                   21.8322(14)
_cell_length_c                   17.9977(10)
_cell_angle_alpha                90
_cell_angle_beta                 91.913(5)
_cell_angle_gamma                90
_cell_volume                     3486.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2929
_cell_measurement_theta_min      3.0050
_cell_measurement_theta_max      27.8660
_exptl_crystal_description       prism
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.081
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_vrf_PLAT342_14                  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03125 Ang.  
RESPONSE: The presence of the heavy atom of Pb in the asymmetric unit distorts
the positions of lighter atoms, hereby lowering the precision of C-C bonds.
;
_reflns_odcompleteness_theta     26.32
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    23.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.20429
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_ambient_temperature_device_make ?
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0355
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -53.00   35.00   1.0000   28.6000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -37.0000  -30.0000 88

#__ type_ start__ end____ width___ exp.time_
  2 omega   -3.00   85.00   1.0000   28.6000
omega____ theta____ kappa____ phi______ frames
    -       15.8569   37.0000  150.0000 88

#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   22.00   1.0000   28.6000
omega____ theta____ kappa____ phi______ frames
    -      -16.9507  -99.0000  120.0000 47

#__ type_ start__ end____ width___ exp.time_
  4 omega   35.00   88.00   1.0000   28.6000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  178.0000 -120.0000 53

#__ type_ start__ end____ width___ exp.time_
  5 omega  -85.00  -49.00   1.0000   28.6000
omega____ theta____ kappa____ phi______ frames
    -      -16.9507  -77.0000  -30.0000 36
;
_diffrn_reflns_number            19454
_diffrn_reflns_av_unetI/netI     0.1725
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_theta_min         2.958
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             6330
_reflns_number_gt                3025
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_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.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS (G. Sheldrick)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0274P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         6330
_refine_ls_number_parameters     318
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0707
_refine_ls_wR_factor_ref         0.1591
_refine_ls_wR_factor_gt          0.1343
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_restrained_S_all      0.878
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         4.591
_refine_diff_density_min         -1.908
_refine_diff_density_rms         0.319
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'

_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_
_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 -0.24491(8) 0.49846(4) 0.99968(4) 0.0364(3) Uani 1 1 d . . . . .
Pb2 Pb -0.02110(9) 0.58204(4) 0.79004(5) 0.0348(2) Uani 1 1 d . . . . .
Pb3 Pb 0.48068(9) 0.57314(4) 0.79267(5) 0.0354(3) Uani 1 1 d . . . . .
Br1 Br -0.4896(3) 0.59073(10) 0.97634(13) 0.0462(6) Uani 1 1 d . . . . .
Br2 Br -0.2218(2) 0.51844(10) 1.16668(12) 0.0395(6) Uani 1 1 d . . . . .
Br3 Br -0.0119(2) 0.59696(10) 0.97469(12) 0.0438(6) Uani 1 1 d . . . . .
Br4 Br -0.2563(2) 0.48088(10) 0.82892(12) 0.0407(6) Uani 1 1 d . . . . .
Br5 Br -0.0235(2) 0.55456(10) 0.63834(13) 0.0425(6) Uani 1 1 d . . . . .
Br6 Br 0.2354(2) 0.66913(10) 0.77497(13) 0.0451(6) Uani 1 1 d . . . . .
Br7 Br 0.4723(2) 0.52969(10) 0.64564(12) 0.0427(6) Uani 1 1 d . . . . .
Br8 Br 0.7125(2) 0.66971(10) 0.76740(14) 0.0470(6) Uani 1 1 d . . . . .
S1 S 0.6591(6) 0.5813(3) 0.4945(3) 0.0453(15) Uani 1 1 d . . . . .
N1 N 0.7508(15) 0.6887(8) 0.5258(9) 0.031(4) Uani 1 1 d . . . A 1
C1 C 0.815(2) 0.6789(9) 0.4567(12) 0.033(5) Uani 1 1 d . . . . .
C2 C 0.899(2) 0.7168(11) 0.4120(16) 0.057(8) Uani 1 1 d . . . . .
H2 H 0.9214 0.7570 0.4252 0.068 Uiso 1 1 calc R . . . .
C3 C 0.944(2) 0.6921(10) 0.3492(12) 0.036(5) Uani 1 1 d . . . . .
H3 H 1.0072 0.7156 0.3205 0.044 Uiso 1 1 calc R . . . .
C4 C 0.907(2) 0.6349(9) 0.3229(12) 0.034(5) Uani 1 1 d . U . . .
H4 H 0.9428 0.6216 0.2777 0.040 Uiso 1 1 calc R . . . .
C5 C 0.820(2) 0.5986(11) 0.3615(13) 0.045(6) Uani 1 1 d . . . . .
H5 H 0.7890 0.5608 0.3425 0.054 Uiso 1 1 calc R . . . .
C6 C 0.774(2) 0.6178(11) 0.4308(12) 0.044(6) Uani 1 1 d . . . . .
C7 C 0.678(2) 0.6414(10) 0.5466(12) 0.038(5) Uani 1 1 d . U . . .
H7 H 0.6347 0.6416 0.5930 0.046 Uiso 1 1 calc R . . A .
C8 C 0.782(2) 0.7439(10) 0.5665(12) 0.045(6) Uani 1 1 d . . . . .
H8A H 0.7136 0.7474 0.6071 0.054 Uiso 1 1 calc R . . A .
H8B H 0.7665 0.7790 0.5341 0.054 Uiso 1 1 calc R . . A .
C9 C 0.946(3) 0.7439(13) 0.5976(15) 0.070(7) Uani 1 1 d . U . . .
H9A H 0.9648 0.7064 0.6254 0.084 Uiso 1 1 calc R . . . .
H9B H 1.0145 0.7450 0.5568 0.084 Uiso 1 1 calc R . . . .
C10 C 0.973(3) 0.7960(13) 0.6454(16) 0.085(8) Uani 1 1 d . U . . .
H10A H 0.9509 0.8330 0.6183 0.128 Uiso 1 1 calc GR . . . .
H10B H 1.0769 0.7963 0.6622 0.128 Uiso 1 1 calc GR . . . .
H10C H 0.9098 0.7935 0.6875 0.128 Uiso 1 1 calc GR . . . .
S2 S 1.1932(6) 0.5647(3) 0.4678(4) 0.0481(16) Uani 1 1 d . . . . .
N2 N 1.2913(17) 0.6331(8) 0.3666(10) 0.038(5) Uani 1 1 d . . . . .
C11 C 1.313(2) 0.6682(9) 0.4373(11) 0.026(4) Uani 1 1 d . U . . .
C12 C 1.373(2) 0.7281(11) 0.4436(14) 0.053(6) Uani 1 1 d . U . . .
H12 H 1.4035 0.7510 0.4033 0.063 Uiso 1 1 calc R . . . .
C13 C 1.381(3) 0.7481(11) 0.5141(15) 0.071(9) Uani 1 1 d . . . . .
H13 H 1.4256 0.7862 0.5229 0.085 Uiso 1 1 calc R . . . .
C14 C 1.330(3) 0.7168(10) 0.5737(11) 0.045(6) Uani 1 1 d . . . . .
H14 H 1.3370 0.7350 0.6204 0.053 Uiso 1 1 calc R . . . .
C15 C 1.267(2) 0.6585(10) 0.5670(15) 0.058(8) Uani 1 1 d . . . . .
H15 H 1.2292 0.6377 0.6074 0.070 Uiso 1 1 calc R . . B .
C16 C 1.264(2) 0.6338(9) 0.4962(13) 0.039(6) Uani 1 1 d . . . C 1
C17 C 1.240(3) 0.5797(10) 0.3820(13) 0.050(7) Uani 1 1 d . . . . .
H17 H 1.2291 0.5500 0.3451 0.061 Uiso 1 1 calc R . . . .
C18 C 1.335(2) 0.6559(9) 0.2985(13) 0.047(6) Uani 1 1 d . . . . .
H18A H 1.3129 0.6994 0.2970 0.056 Uiso 1 1 calc R . . . .
H18B H 1.2732 0.6366 0.2596 0.056 Uiso 1 1 calc R . . . .
C19 C 1.502(2) 0.6467(12) 0.2806(12) 0.053(7) Uani 1 1 d . . . . .
H19A H 1.5642 0.6684 0.3172 0.064 Uiso 1 1 calc R . . . .
H19B H 1.5261 0.6035 0.2843 0.064 Uiso 1 1 calc R . . . .
C20 C 1.537(2) 0.6696(10) 0.2032(12) 0.050(6) Uani 1 1 d . U . . .
H20A H 1.4919 0.6428 0.1665 0.075 Uiso 1 1 calc GR . . . .
H20B H 1.6444 0.6702 0.1978 0.075 Uiso 1 1 calc GR . . . .
H20C H 1.4978 0.7103 0.1964 0.075 Uiso 1 1 calc GR . . . .


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 2.982(2) . ?
Pb1 Br1 3.099(3) 3_467 ?
Pb1 Br2 3.037(2) . ?
Pb1 Br3 3.028(2) . ?
Pb1 Br3 3.112(2) 3_567 ?
Pb1 Br4 3.095(2) . ?
Pb2 Br2 3.155(2) 3_567 ?
Pb2 Br4 3.134(2) . ?
Pb2 Br5 2.795(2) . ?
Pb2 Br6 2.986(2) . ?
Pb2 Br8 3.060(2) 1_455 ?
Pb3 Br2 3.151(2) 3_567 ?
Pb3 Br4 3.136(2) 1_655 ?
Pb3 Br6 3.031(2) . ?
Pb3 Br7 2.810(2) . ?
Pb3 Br8 2.992(2) . ?
Br1 Pb1 3.099(2) 3_467 ?
Br2 Pb2 3.155(2) 3_567 ?
Br2 Pb3 3.151(2) 3_567 ?
Br3 Pb1 3.112(2) 3_567 ?
Br4 Pb3 3.136(2) 1_455 ?
Br8 Pb2 3.060(2) 1_655 ?
S1 C6 1.75(2) . ?
S1 C7 1.62(2) . ?
N1 C1 1.40(2) . ?
N1 C7 1.28(2) . ?
N1 C8 1.43(2) . ?
C1 C2 1.39(3) . ?
C1 C6 1.45(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.33(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.37(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.32(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.39(3) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.54(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.44(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
S2 C16 1.71(2) . ?
S2 C17 1.64(2) . ?
N2 C11 1.49(2) . ?
N2 C17 1.29(2) . ?
N2 C18 1.39(3) . ?
C11 C12 1.41(3) . ?
C11 C16 1.38(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.34(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.36(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.39(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.38(3) . ?
C17 H17 0.9300 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.54(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.52(3) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 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 83.69(7) . 3_467 ?
Br1 Pb1 Br2 93.86(7) . . ?
Br1 Pb1 Br3 179.41(7) . 3_567 ?
Br1 Pb1 Br3 89.86(7) . . ?
Br1 Pb1 Br3 96.65(6) 3_467 3_567 ?
Br1 Pb1 Br4 86.82(6) . . ?
Br2 Pb1 Br1 88.80(6) . 3_467 ?
Br2 Pb1 Br3 85.67(6) . 3_567 ?
Br2 Pb1 Br4 177.68(7) . . ?
Br3 Pb1 Br1 173.53(6) . 3_467 ?
Br3 Pb1 Br2 91.20(6) . . ?
Br3 Pb1 Br3 89.81(6) . 3_567 ?
Br3 Pb1 Br4 86.58(6) . . ?
Br4 Pb1 Br1 93.48(6) . 3_467 ?
Br4 Pb1 Br3 93.64(6) . 3_567 ?
Br4 Pb2 Br2 84.83(6) . 3_567 ?
Br5 Pb2 Br2 94.29(7) . 3_567 ?
Br5 Pb2 Br4 94.79(7) . . ?
Br5 Pb2 Br6 91.65(7) . . ?
Br5 Pb2 Br8 91.35(7) . 1_455 ?
Br6 Pb2 Br2 87.02(6) . 3_567 ?
Br6 Pb2 Br4 169.96(6) . . ?
Br6 Pb2 Br8 100.27(6) . 1_455 ?
Br8 Pb2 Br2 170.66(7) 1_455 3_567 ?
Br8 Pb2 Br4 87.29(6) 1_455 . ?
Br4 Pb3 Br2 95.07(6) 1_655 3_567 ?
Br6 Pb3 Br2 86.33(6) . 3_567 ?
Br6 Pb3 Br4 173.34(7) . 1_655 ?
Br7 Pb3 Br2 90.45(6) . 3_567 ?
Br7 Pb3 Br4 88.58(7) . 1_655 ?
Br7 Pb3 Br6 97.93(7) . . ?
Br7 Pb3 Br8 95.25(7) . . ?
Br8 Pb3 Br2 173.38(7) . 3_567 ?
Br8 Pb3 Br4 88.45(6) . 1_655 ?
Br8 Pb3 Br6 89.55(6) . . ?
Pb1 Br1 Pb1 96.31(7) . 3_467 ?
Pb1 Br2 Pb2 99.65(7) . 3_567 ?
Pb1 Br2 Pb3 96.48(6) . 3_567 ?
Pb3 Br2 Pb2 89.97(6) 3_567 3_567 ?
Pb1 Br3 Pb1 90.20(6) . 3_567 ?
Pb1 Br4 Pb2 97.73(6) . . ?
Pb1 Br4 Pb3 97.25(7) . 1_455 ?
Pb2 Br4 Pb3 89.89(6) . 1_455 ?
Pb2 Br6 Pb3 95.61(7) . . ?
Pb3 Br8 Pb2 94.11(7) . 1_655 ?
C7 S1 C6 87.7(11) . . ?
C1 N1 C8 120.4(17) . . ?
C7 N1 C1 111.0(19) . . ?
C7 N1 C8 128.3(19) . . ?
N1 C1 C6 108.8(17) . . ?
C2 C1 N1 132(2) . . ?
C2 C1 C6 120(2) . . ?
C1 C2 H2 122.1 . . ?
C3 C2 C1 116(2) . . ?
C3 C2 H2 122.1 . . ?
C2 C3 H3 117.0 . . ?
C2 C3 C4 126(2) . . ?
C4 C3 H3 117.0 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120(2) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 120.6 . . ?
C4 C5 C6 119(2) . . ?
C6 C5 H5 120.6 . . ?
C1 C6 S1 110.5(16) . . ?
C5 C6 S1 130.0(19) . . ?
C5 C6 C1 119(2) . . ?
S1 C7 H7 119.1 . . ?
N1 C7 S1 121.8(18) . . ?
N1 C7 H7 119.1 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
N1 C8 C9 110.5(17) . . ?
H8A C8 H8B 108.1 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C10 C9 C8 111(2) . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C17 S2 C16 90.3(11) . . ?
C17 N2 C11 108.7(18) . . ?
C17 N2 C18 129(2) . . ?
C18 N2 C11 122.3(18) . . ?
C12 C11 N2 125.6(19) . . ?
C16 C11 N2 109.8(17) . . ?
C16 C11 C12 125(2) . . ?
C11 C12 H12 123.6 . . ?
C13 C12 C11 113(2) . . ?
C13 C12 H12 123.6 . . ?
C12 C13 H13 117.6 . . ?
C12 C13 C14 125(2) . . ?
C14 C13 H13 117.6 . . ?
C13 C14 H14 118.9 . . ?
C13 C14 C15 122(2) . . ?
C15 C14 H14 118.9 . . ?
C14 C15 H15 122.2 . . ?
C16 C15 C14 116(2) . . ?
C16 C15 H15 122.2 . . ?
C11 C16 S2 111.9(16) . . ?
C15 C16 S2 128.2(19) . . ?
C15 C16 C11 120(2) . . ?
S2 C17 H17 120.5 . . ?
N2 C17 S2 119.0(18) . . ?
N2 C17 H17 120.5 . . ?
N2 C18 H18A 108.3 . . ?
N2 C18 H18B 108.3 . . ?
N2 C18 C19 115.8(17) . . ?
H18A C18 H18B 107.4 . . ?
C19 C18 H18A 108.3 . . ?
C19 C18 H18B 108.3 . . ?
C18 C19 H19A 109.1 . . ?
C18 C19 H19B 109.1 . . ?
H19A C19 H19B 107.9 . . ?
C20 C19 C18 112.3(18) . . ?
C20 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

####################################################################### 
# 
# 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_cmp6
_database_code_depnum_ccdc_archive 'CCDC 2296334'
loop_
_audit_author_name
_audit_author_address
'Guang-Ning Liu'
;University of Jinan
China
;
_audit_update_record             
;
2023-09-21 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_audit_creation_date             2023-09-20
_chemical_oxdiff_formula         'C H N P Br Pb'
_diffrn_orient_matrix_UB_11      0.0071618000
_diffrn_orient_matrix_UB_12      -0.0803502000
_diffrn_orient_matrix_UB_13      0.0121553000
_diffrn_orient_matrix_UB_21      0.0076357000
_diffrn_orient_matrix_UB_22      -0.0290629000
_diffrn_orient_matrix_UB_23      -0.0302831000
_diffrn_orient_matrix_UB_31      0.0524103000
_diffrn_orient_matrix_UB_32      0.0152277000
_diffrn_orient_matrix_UB_33      0.0062869000
_audit_creation_method           
;
FinalCif V106 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C21 H22 Br3 P Pb'
_chemical_formula_moiety         'Br3 Pb, C21 H22 P'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_chemical_formula_weight         752.27
_chemical_melting_point          ?
_exptl_crystal_colour_primary    yellow
_space_group_crystal_system      monoclinic
_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. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
3.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
3.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_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.
;

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                   13.3422(12)
_cell_length_b                   8.1688(8)
_cell_length_c                   21.4738(18)
_cell_angle_alpha                90
_cell_angle_beta                 95.977(8)
_cell_angle_gamma                90
_cell_volume                     2327.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2575
_cell_measurement_theta_min      3.5630
_cell_measurement_theta_max      25.1050
_exptl_crystal_description       prism
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.147
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    12.470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.21804
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   0.088
_shelx_estimated_absorpt_T_max   0.435
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_ambient_temperature_device_make ?
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0355
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -3.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569   37.0000   90.0000 88

#__ type_ start__ end____ width___ exp.time_
  2 omega  -51.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -57.0000  -90.0000 84

#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9507  -99.0000   60.0000 47

#__ type_ start__ end____ width___ exp.time_
  4 omega   35.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  178.0000  150.0000 53

#__ type_ start__ end____ width___ exp.time_
  5 omega  -85.00  -34.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9507  -77.0000 -120.0000 51
;
_diffrn_reflns_number            13335
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_theta_min         3.070
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4248
_reflns_number_gt                2906
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_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.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0175P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4248
_refine_ls_number_parameters     236
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0673
_refine_ls_wR_factor_gt          0.0581
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.979
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

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'
P P 0.1023 0.0942 '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'

_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_
_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 0.75197(2) 0.79440(3) 0.75196(2) 0.04451(10) Uani 1 1 d . . . . .
Br1 Br 0.87901(6) 1.02194(10) 0.68916(4) 0.0612(2) Uani 1 1 d . . . . .
Br2 Br 0.72276(6) 0.60556(11) 0.64092(4) 0.0636(2) Uani 1 1 d . . . . .
Br3 Br 0.57697(6) 1.00119(11) 0.71980(4) 0.0673(3) Uani 1 1 d . . . . .
P1 P 0.22004(14) 0.1303(2) 0.56402(9) 0.0434(5) Uani 1 1 d . . . . .
C1 C 0.3149(5) 0.2801(8) 0.5831(3) 0.0408(18) Uani 1 1 d . . . . .
C2 C 0.3683(6) 0.2971(11) 0.6408(4) 0.067(2) Uani 1 1 d . . . . .
H2 H 0.3566 0.2242 0.6725 0.080 Uiso 1 1 calc R . . . .
C3 C 0.4383(7) 0.4181(13) 0.6529(5) 0.080(3) Uani 1 1 d . . . . .
H3 H 0.4739 0.4274 0.6923 0.096 Uiso 1 1 calc R . . . .
C4 C 0.4553(7) 0.5263(11) 0.6058(7) 0.087(4) Uani 1 1 d . . . . .
H4 H 0.5026 0.6096 0.6133 0.104 Uiso 1 1 calc R . . . .
C5 C 0.4029(7) 0.5110(11) 0.5483(5) 0.077(3) Uani 1 1 d . . . . .
H5 H 0.4143 0.5844 0.5166 0.093 Uiso 1 1 calc R . . . .
C6 C 0.3336(6) 0.3882(10) 0.5366(4) 0.059(2) Uani 1 1 d . . . . .
H6 H 0.2989 0.3779 0.4970 0.071 Uiso 1 1 calc R . . . .
C7 C 0.2230(6) -0.0250(9) 0.6236(3) 0.0475(19) Uani 1 1 d . . . . .
C8 C 0.1332(6) -0.0843(9) 0.6416(4) 0.058(2) Uani 1 1 d . . . . .
H8 H 0.0722 -0.0372 0.6261 0.069 Uiso 1 1 calc R . . . .
C9 C 0.1354(8) -0.2162(12) 0.6835(4) 0.078(3) Uani 1 1 d . . . . .
H9 H 0.0755 -0.2582 0.6954 0.094 Uiso 1 1 calc R . . . .
C10 C 0.2260(10) -0.2837(11) 0.7071(5) 0.089(3) Uani 1 1 d . . . . .
H10 H 0.2270 -0.3725 0.7342 0.106 Uiso 1 1 calc R . . . .
C11 C 0.3153(8) -0.2209(11) 0.6906(4) 0.085(3) Uani 1 1 d . . . . .
H11 H 0.3764 -0.2649 0.7078 0.102 Uiso 1 1 calc R . . . .
C12 C 0.3142(7) -0.0924(10) 0.6486(4) 0.062(2) Uani 1 1 d . . . . .
H12 H 0.3746 -0.0509 0.6371 0.075 Uiso 1 1 calc R . . . .
C13 C 0.1004(5) 0.2303(8) 0.5583(3) 0.0425(18) Uani 1 1 d . . . . .
C14 C 0.0355(6) 0.2288(9) 0.5042(4) 0.054(2) Uani 1 1 d . . . . .
H14 H 0.0539 0.1757 0.4688 0.065 Uiso 1 1 calc R . . . .
C15 C -0.0577(6) 0.3063(9) 0.5021(4) 0.059(2) Uani 1 1 d . . . . .
H15 H -0.1016 0.3062 0.4655 0.071 Uiso 1 1 calc R . . . .
C16 C -0.0838(6) 0.3827(10) 0.5547(5) 0.063(2) Uani 1 1 d . . . . .
H16 H -0.1463 0.4336 0.5538 0.076 Uiso 1 1 calc R . . . .
C17 C -0.0203(7) 0.3854(10) 0.6077(4) 0.064(2) Uani 1 1 d . . . . .
H17 H -0.0391 0.4392 0.6429 0.076 Uiso 1 1 calc R . . . .
C18 C 0.0721(6) 0.3093(9) 0.6104(4) 0.059(2) Uani 1 1 d . . . . .
H18 H 0.1154 0.3112 0.6473 0.071 Uiso 1 1 calc R . . . .
C19 C 0.2393(6) 0.0382(9) 0.4900(3) 0.056(2) Uani 1 1 d . . . . .
H19A H 0.1854 -0.0392 0.4785 0.067 Uiso 1 1 calc R . . . .
H19B H 0.2363 0.1225 0.4581 0.067 Uiso 1 1 calc R . . . .
C20 C 0.3431(8) -0.0528(11) 0.4921(4) 0.100(3) Uani 1 1 d . U . . .
H20A H 0.3969 0.0253 0.5028 0.120 Uiso 1 1 calc R . . . .
H20B H 0.3466 -0.1351 0.5248 0.120 Uiso 1 1 calc R . . . .
C21 C 0.3590(8) -0.1295(14) 0.4347(4) 0.131(5) Uani 1 1 d . . . . .
H21A H 0.3637 -0.0476 0.4030 0.197 Uiso 1 1 calc GR . . . .
H21B H 0.3037 -0.2015 0.4221 0.197 Uiso 1 1 calc GR . . . .
H21C H 0.4205 -0.1914 0.4399 0.197 Uiso 1 1 calc GR . . . .


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 3.1728(8) 2_646 ?
Pb1 Br1 2.9364(8) . ?
Pb1 Br2 2.8326(9) . ?
Pb1 Br3 2.9062(9) . ?
Br1 Pb1 3.1728(8) 2_656 ?
P1 C1 1.777(7) . ?
P1 C7 1.799(7) . ?
P1 C13 1.786(7) . ?
P1 C19 1.801(7) . ?
C1 C2 1.370(10) . ?
C1 C6 1.374(9) . ?
C2 H2 0.9300 . ?
C2 C3 1.366(11) . ?
C3 H3 0.9300 . ?
C3 C4 1.380(12) . ?
C4 H4 0.9300 . ?
C4 C5 1.360(13) . ?
C5 H5 0.9300 . ?
C5 C6 1.370(11) . ?
C6 H6 0.9300 . ?
C7 C8 1.385(9) . ?
C7 C12 1.392(10) . ?
C8 H8 0.9300 . ?
C8 C9 1.402(11) . ?
C9 H9 0.9300 . ?
C9 C10 1.376(12) . ?
C10 H10 0.9300 . ?
C10 C11 1.376(12) . ?
C11 H11 0.9300 . ?
C11 C12 1.384(10) . ?
C12 H12 0.9300 . ?
C13 C14 1.376(9) . ?
C13 C18 1.377(9) . ?
C14 H14 0.9300 . ?
C14 C15 1.392(10) . ?
C15 H15 0.9300 . ?
C15 C16 1.366(10) . ?
C16 H16 0.9300 . ?
C16 C17 1.347(10) . ?
C17 H17 0.9300 . ?
C17 C18 1.378(10) . ?
C18 H18 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.568(10) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.418(11) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 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 174.44(2) . 2_646 ?
Br2 Pb1 Br1 89.63(3) . . ?
Br2 Pb1 Br1 85.42(2) . 2_646 ?
Br2 Pb1 Br3 94.58(3) . . ?
Br3 Pb1 Br1 90.62(3) . . ?
Br3 Pb1 Br1 92.30(2) . 2_646 ?
Pb1 Br1 Pb1 83.846(18) . 2_656 ?
C1 P1 C7 111.1(4) . . ?
C1 P1 C13 108.1(3) . . ?
C1 P1 C19 109.1(3) . . ?
C7 P1 C19 109.7(3) . . ?
C13 P1 C7 108.9(3) . . ?
C13 P1 C19 109.9(4) . . ?
C2 C1 P1 124.6(6) . . ?
C2 C1 C6 118.3(7) . . ?
C6 C1 P1 117.0(6) . . ?
C1 C2 H2 119.1 . . ?
C3 C2 C1 121.7(8) . . ?
C3 C2 H2 119.1 . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 119.1(9) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 120.1 . . ?
C5 C4 C3 119.9(9) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.4(9) . . ?
C6 C5 H5 119.8 . . ?
C1 C6 H6 119.7 . . ?
C5 C6 C1 120.6(8) . . ?
C5 C6 H6 119.7 . . ?
C8 C7 P1 119.3(6) . . ?
C8 C7 C12 120.1(7) . . ?
C12 C7 P1 120.5(6) . . ?
C7 C8 H8 120.4 . . ?
C7 C8 C9 119.2(8) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.2(9) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.5(9) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.0(9) . . ?
C12 C11 H11 120.0 . . ?
C7 C12 H12 120.0 . . ?
C11 C12 C7 120.1(8) . . ?
C11 C12 H12 120.0 . . ?
C14 C13 P1 122.2(6) . . ?
C14 C13 C18 119.3(7) . . ?
C18 C13 P1 118.5(6) . . ?
C13 C14 H14 119.9 . . ?
C13 C14 C15 120.3(7) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 H15 120.5 . . ?
C16 C15 C14 119.0(8) . . ?
C16 C15 H15 120.5 . . ?
C15 C16 H16 119.5 . . ?
C17 C16 C15 121.0(8) . . ?
C17 C16 H16 119.5 . . ?
C16 C17 H17 119.7 . . ?
C16 C17 C18 120.6(8) . . ?
C18 C17 H17 119.7 . . ?
C13 C18 C17 119.9(8) . . ?
C13 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
P1 C19 H19A 109.1 . . ?
P1 C19 H19B 109.1 . . ?
H19A C19 H19B 107.9 . . ?
C20 C19 P1 112.4(6) . . ?
C20 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 C19 113.4(8) . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?

