# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# 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_3-clpy-pbbr3_auto
_database_code_depnum_ccdc_archive 'CCDC 2499860'
loop_
_audit_author_name
_audit_author_address
'N.I. Selivanov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2025-11-03 deposited with the CCDC.	2026-01-05 downloaded from the CCDC.
;
_audit_creation_date             2024-10-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C5 H5 Cl N'
_chemical_formula_sum            'C5 H5 Br3 Cl N Pb'
_chemical_formula_weight         561.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20  H20  Br12  Cl4  N4  Pb4  '
_chemical_oxdiff_usercomment     296K
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.2210(4)
_cell_length_b                   8.0654(3)
_cell_length_c                   15.8229(6)
_cell_angle_alpha                90
_cell_angle_beta                 104.415(4)
_cell_angle_gamma                90
_cell_volume                     1139.71(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5890
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      35.5740
_cell_measurement_theta_min      3.4420
_shelx_estimated_absorpt_T_max   0.292
_shelx_estimated_absorpt_T_min   0.108
_exptl_absorpt_coefficient_mu    25.501
_exptl_absorpt_correction_T_max  0.296
_exptl_absorpt_correction_T_min  0.100
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.272
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             984
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
13 1 -3 0.0306
-1 9 -12 0.0442
-13 0 2 0.0300
3 -9 11 0.0421
-3 0 -20 0.0513
5 -9 -10 0.0749
-7 8 -6 0.0500
1 2 21 0.0629
-6 10 7 0.0658
-8 0 20 0.0590
6 2 -21 0.0427
11 -5 -11 0.0490
9 3 11 0.0548
-3 -11 -4 0.0787
-12 -1 -1 0.0285
-7 -9 8 0.0536

_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.064
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
12.8513 1.3027 -3.3711 -0.0707 0.8698 -0.4882
-1.4851 9.2895 -11.5788 -0.0311 0.4206 0.9067
-12.8488 -0.4856 2.3348 0.0673 -0.8246 0.5617
3.0372 -8.9748 10.9721 0.0219 -0.3068 -0.9515
-2.7923 -0.0121 -19.9109 -0.7692 -0.0596 0.6362
5.4169 -9.4863 -10.1114 -0.8145 -0.0666 -0.5763
-6.9181 8.4874 -5.6792 0.1602 0.0155 0.9870
1.1690 2.3859 20.5375 0.8996 0.0706 -0.4310
-5.9811 9.7562 7.4837 0.7251 0.0598 0.6860
-8.3614 0.4014 20.0959 0.7929 -0.6068 -0.0553
5.8580 1.8509 -21.4661 -0.7451 0.5693 0.3474
11.0441 -5.0996 -10.7124 -0.6409 0.4927 -0.5886
8.6486 2.9708 11.4199 0.5745 0.6088 -0.5471
-3.2104 -10.5849 -4.4436 -0.6457 -0.6805 -0.3464
-12.3092 -1.0754 -1.3866 -0.1027 -0.7989 0.5927
-6.7872 -9.3539 7.7606 -0.1198 -0.9095 -0.3980

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17390
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.623
_diffrn_reflns_theta_min         3.404
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -10.00  15.00   0.50    5.00    --   17.79 -65.00 160.00   50
  2  ω      5.00  90.00   0.50    5.00    --   17.79  65.00 -64.00  170
  3  ω      8.00  45.00   0.50    5.00    --  -19.04  65.00 -64.00   74
  4  ω    -92.00  -1.00   0.50    5.00    --  -19.04 -65.00 160.00  182
  5  ω     47.00  89.00   0.50    5.00    --   17.79-178.00 120.00   84
  6  ω      7.00  91.00   0.50    5.00    --   17.79  38.00-180.00  168
  7  ω      7.00  44.50   0.50    5.00    --   17.79  19.00 -60.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0000814000
_diffrn_orient_matrix_UB_12      0.0447716000
_diffrn_orient_matrix_UB_13      0.0385952000
_diffrn_orient_matrix_UB_21      0.0613356000
_diffrn_orient_matrix_UB_22      0.0480533000
_diffrn_orient_matrix_UB_23      -0.0056371000
_diffrn_orient_matrix_UB_31      -0.0504546000
_diffrn_orient_matrix_UB_32      0.0584909000
_diffrn_orient_matrix_UB_33      -0.0249111000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3307
_reflns_number_total             4619
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.264
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       0.00303(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         4619
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0344
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0181P)²+0.0093P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0609
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), N1(H1A), C3(H3), C4(H4), C5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.88340(5) 0.25841(5) 0.86082(3) 0.04345(11) Uani 1 1 d . . . . .
Pb1 Pb 1.01752(2) 0.04267(2) 0.75029(2) 0.03682(6) Uani 1 1 d . . . . .
Br2 Br 0.88768(5) 0.28476(5) 0.60538(3) 0.04753(11) Uani 1 1 d . . . . .
Br3 Br 0.74859(5) -0.13764(5) 0.70690(3) 0.04823(12) Uani 1 1 d . . . . .
C1 C 0.2871(6) 0.3849(5) 0.5506(3) 0.0542(11) Uani 1 1 d . . . . .
H1 H 0.2479 0.4907 0.5377 0.065 Uiso 1 1 calc R U . . .
Cl1 Cl 0.52821(19) 0.53653(14) 0.64503(12) 0.0830(5) Uani 1 1 d . . . . .
N1 N 0.2084(4) 0.2514(5) 0.5170(2) 0.0542(9) Uani 1 1 d . . . . .
H1A H 0.1209 0.2656 0.4827 0.065 Uiso 1 1 calc R U . . .
C2 C 0.4249(5) 0.3633(4) 0.6038(3) 0.0448(10) Uani 1 1 d . . . . .
C3 C 0.4817(6) 0.2074(5) 0.6241(4) 0.0620(13) Uani 1 1 d . . . . .
H3 H 0.5764 0.1925 0.6610 0.074 Uiso 1 1 calc R U . . .
C4 C 0.3957(7) 0.0733(6) 0.5886(4) 0.0676(15) Uani 1 1 d . . . . .
H4 H 0.4317 -0.0337 0.6022 0.081 Uiso 1 1 calc R U . . .
C5 C 0.2590(6) 0.0964(6) 0.5341(3) 0.0588(12) Uani 1 1 d . . . . .
H5 H 0.2012 0.0063 0.5089 0.071 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0503(3) 0.0426(2) 0.0401(2) -0.00115(16) 0.01625(19) -0.00077(17)
Pb1 0.04181(11) 0.02907(9) 0.03837(9) -0.00106(5) 0.00771(6) -0.00165(6)
Br2 0.0608(3) 0.0444(2) 0.0337(2) -0.00001(15) 0.00483(19) -0.00197(18)
Br3 0.0375(3) 0.0360(2) 0.0676(3) -0.00191(17) 0.0064(2) -0.00170(16)
C1 0.058(3) 0.042(2) 0.061(3) 0.006(2) 0.013(2) 0.004(2)
Cl1 0.0675(10) 0.0558(8) 0.1212(14) -0.0258(7) 0.0149(9) -0.0199(6)
N1 0.043(2) 0.064(2) 0.048(2) 0.0045(17) -0.0017(17) -0.0036(18)
C2 0.042(3) 0.038(2) 0.056(3) -0.0052(18) 0.014(2) -0.0083(17)
C3 0.038(3) 0.056(3) 0.087(4) 0.010(2) 0.005(2) 0.002(2)
C4 0.064(4) 0.037(2) 0.100(4) 0.008(2) 0.017(3) 0.006(2)
C5 0.061(4) 0.052(3) 0.062(3) -0.008(2) 0.014(3) -0.019(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Pb1 2.9483(4) . ?
Br1 Pb1 3.1594(4) 2_756 ?
Pb1 Br1 3.1594(4) 2_746 ?
Pb1 Br2 3.0516(4) 2_746 ?
Pb1 Br2 3.0227(4) . ?
Pb1 Br3 2.8085(4) . ?
Br2 Pb1 3.0516(4) 2_756 ?
C1 H1 0.9300 . ?
C1 N1 1.333(6) . ?
C1 C2 1.349(6) . ?
Cl1 C2 1.725(4) . ?
N1 H1A 0.8600 . ?
N1 C5 1.338(6) . ?
C2 C3 1.369(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.376(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.352(7) . ?
C5 H5 0.9300 . ?

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
Pb1 Br1 Pb1 82.881(10) . 2_756 ?
Br1 Pb1 Br1 168.659(11) . 2_746 ?
Br1 Pb1 Br2 85.603(12) . . ?
Br1 Pb1 Br2 92.447(12) . 2_746 ?
Br2 Pb1 Br1 99.289(12) . 2_746 ?
Br2 Pb1 Br1 81.557(11) 2_746 2_746 ?
Br2 Pb1 Br2 173.506(7) . 2_746 ?
Br3 Pb1 Br1 81.271(12) . 2_746 ?
Br3 Pb1 Br1 88.592(13) . . ?
Br3 Pb1 Br2 84.319(13) . 2_746 ?
Br3 Pb1 Br2 89.437(13) . . ?
Pb1 Br2 Pb1 83.515(11) . 2_756 ?
N1 C1 H1 120.7 . . ?
N1 C1 C2 118.6(4) . . ?
C2 C1 H1 120.7 . . ?
C1 N1 H1A 118.4 . . ?
C1 N1 C5 123.1(4) . . ?
C5 N1 H1A 118.4 . . ?
C1 C2 Cl1 118.5(3) . . ?
C1 C2 C3 120.7(4) . . ?
C3 C2 Cl1 120.8(4) . . ?
C2 C3 H3 120.7 . . ?
C2 C3 C4 118.6(5) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.2(4) . . ?
C5 C4 H4 119.9 . . ?
N1 C5 C4 118.7(4) . . ?
N1 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 C5 C4 0.7(7) . . . . ?
C1 C2 C3 C4 0.4(8) . . . . ?
Cl1 C2 C3 C4 -179.1(4) . . . . ?
N1 C1 C2 Cl1 178.4(3) . . . . ?
N1 C1 C2 C3 -1.1(7) . . . . ?
C2 C1 N1 C5 0.6(7) . . . . ?
C2 C3 C4 C5 0.9(9) . . . . ?
C3 C4 C5 N1 -1.4(8) . . . . ?

_shelx_res_file                  
;
TITL 3-clpy-pbbr3_auto_a.res in P2(1)/c
REM Old TITL 3-ClPy-PbBr3_auto in P21/c #14
REM SHELXT solution in P2(1)/c
REM R1 0.099, Rweak 0.004, Alpha 0.022, Orientation as input
REM Formula found by SHELXT: C2 Br3 Cl N Pb
CELL 0.71073 9.220984 8.065371 15.822862 90 104.4153 90
ZERR 4 0.000421 0.000265 0.000624 0 0.0043 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br Cl N Pb
UNIT 20 20 12 4 4 4

L.S. 20
PLAN  7
SIZE 0.064 0.102 0.157
TEMP 23(2)
CONF
HTAB
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\3-ClPy-PbBr3_auto.hkl">
REM </olex2.extras>

WGHT    0.018100    0.009300
EXTI    0.003028
FVAR       0.82530
BR1   3    0.883404    0.258410    0.860822    11.00000    0.05029    0.04263 =
         0.04009   -0.00115    0.01625   -0.00077
PB1   6    1.017516    0.042667    0.750295    11.00000    0.04181    0.02907 =
         0.03837   -0.00106    0.00771   -0.00165
BR2   3    0.887682    0.284764    0.605377    11.00000    0.06080    0.04437 =
         0.03374   -0.00001    0.00483   -0.00197
BR3   3    0.748594   -0.137640    0.706900    11.00000    0.03751    0.03604 =
         0.06760   -0.00191    0.00641   -0.00170
C1    1    0.287105    0.384860    0.550635    11.00000    0.05833    0.04179 =
         0.06143    0.00572    0.01279    0.00432
AFIX  43
H1    2    0.247871    0.490720    0.537693    11.00000   -1.20000
AFIX   0
CL1   4    0.528208    0.536528    0.645033    11.00000    0.06750    0.05579 =
         0.12119   -0.02585    0.01485   -0.01988
N1    5    0.208383    0.251406    0.517015    11.00000    0.04346    0.06398 =
         0.04829    0.00448   -0.00173   -0.00358
AFIX  43
H1A   2    0.120944    0.265580    0.482736    11.00000   -1.20000
AFIX   0
C2    1    0.424884    0.363253    0.603829    11.00000    0.04165    0.03771 =
         0.05589   -0.00516    0.01370   -0.00832
C3    1    0.481707    0.207410    0.624074    11.00000    0.03771    0.05555 =
         0.08695    0.00966    0.00452    0.00188
AFIX  43
H3    2    0.576435    0.192511    0.661018    11.00000   -1.20000
AFIX   0
C4    1    0.395678    0.073255    0.588597    11.00000    0.06447    0.03676 =
         0.09965    0.00811    0.01692    0.00569
AFIX  43
H4    2    0.431725   -0.033676    0.602180    11.00000   -1.20000
AFIX   0
C5    1    0.258966    0.096374    0.534077    11.00000    0.06127    0.05245 =
         0.06184   -0.00798    0.01363   -0.01860
AFIX  43
H5    2    0.201160    0.006295    0.508904    11.00000   -1.20000
AFIX   0
HKLF 4

REM  3-clpy-pbbr3_auto_a.res in P2(1)/c
REM R1 =  0.0344 for    3307 Fo > 4sig(Fo)  and  0.0621 for all    4619 data
REM    101 parameters refined using      0 restraints

END

WGHT      0.0181      0.0093

REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, y+1/2, -z+3/2
HTAB C1 Br1_$1
EQIV $2 -x+1, -y+1, -z+1
HTAB C1 Br2_$2
EQIV $3 x-1, -y+1/2, z-1/2
HTAB N1 Br1_$3
HTAB C3 Br3
HTAB C4 Br3
EQIV $4 -x+1, y-1/2, -z+3/2
HTAB C5 Br1_$4
EQIV $5 -x+1, -y, -z+1
HTAB C5 Br2_$5

REM Highest difference peak  1.264,  deepest hole -0.889,  1-sigma level  0.166
Q1    1   1.1018  0.0424  0.7388  11.00000  0.05    1.26
Q2    1   0.9115  0.0457  0.7710  11.00000  0.05    1.08
Q3    1   1.0137  0.0703  0.7026  11.00000  0.05    1.07
Q4    1   1.0233  0.0078  0.7021  11.00000  0.05    1.03
Q5    1   1.0121  0.0627  0.8000  11.00000  0.05    0.93
Q6    1   0.5381  0.4785  0.6812  11.00000  0.05    0.83
Q7    1   1.0839  0.1481  0.7605  11.00000  0.05    0.70
;
_shelx_res_checksum              97776
_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 5.924
_oxdiff_exptl_absorpt_empirical_full_min 0.587
####################################################################### 
# 
# 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_3-ipy-pbbr3
_database_code_depnum_ccdc_archive 'CCDC 2499861'
loop_
_audit_author_name
_audit_author_address
'N.I. Selivanov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2025-11-03 deposited with the CCDC.	2026-01-05 downloaded from the CCDC.
;
_audit_creation_date             2024-10-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C5 H5 I N'
_chemical_formula_sum            'C5 H5 Br3 I N Pb'
_chemical_formula_weight         652.92
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb1 Br3 I1 C5 N1 H5'
_chemical_oxdiff_usercomment     296K
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.6254(4)
_cell_length_b                   8.0836(3)
_cell_length_c                   15.7786(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.349(5)
_cell_angle_gamma                90
_cell_volume                     1183.91(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6454
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      37.5820
_cell_measurement_theta_min      3.3530
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    26.931
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.038
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.663
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1128
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 0 22 0.0403
0 -11 6 0.1440
5 0 -22 0.0382
4 2 -22 0.0397
1 10 -10 0.1437
-4 10 12 0.1513
-12 0 -4 0.0134
12 0 4 0.0134

_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.027
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.4791 -0.3928 22.1851 0.3294 0.9321 0.1504
0.1745 -10.9696 5.7234 0.0478 0.1274 0.9907
4.5387 -0.0855 -22.1903 -0.3311 -0.9373 -0.1086
4.2046 2.0756 -21.8492 -0.3186 -0.9005 -0.2961
0.7923 10.1609 -9.9765 -0.1140 -0.3153 -0.9421
-3.5851 9.5297 11.8535 0.2093 0.5993 -0.7727
-12.1622 0.1998 -4.2336 -0.9641 0.2300 -0.1325
12.1622 -0.1998 4.2336 0.9641 -0.2300 0.1325

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21790
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.096
_diffrn_reflns_theta_min         3.342
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     53.00  95.00   0.50    5.00    --   23.84  12.00 116.00   84
  2  ω    -37.00 -12.00   0.50    5.00    --   23.84 -12.00 -55.00   50
  3  ω    -99.00 -16.00   0.50    5.00    --  -25.09 -12.00 -55.00  166
  4  ω    -24.00  44.00   0.50    5.00    --  -25.09  12.00 116.00  136
  5  ω     39.00  76.00   0.50    5.00    --   23.84-178.00 -90.00   74
  6  ω     67.00  92.00   0.50    5.00    --   23.84 178.00 -60.00   50
  7  ω     39.00  95.00   0.50    5.00    --   23.84-178.00  60.00  112
  8  ω    -71.00  -5.00   0.50    5.00    --  -25.09 -77.00-180.00  132
  9  ω    -64.00 -18.50   0.50    5.00    --  -25.09 -57.00-120.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0693531000
_diffrn_orient_matrix_UB_12      0.0119058000
_diffrn_orient_matrix_UB_13      0.0290596000
_diffrn_orient_matrix_UB_21      -0.0312701000
_diffrn_orient_matrix_UB_22      0.0065733000
_diffrn_orient_matrix_UB_23      0.0358195000
_diffrn_orient_matrix_UB_31      0.0071405000
_diffrn_orient_matrix_UB_32      -0.0867103000
_diffrn_orient_matrix_UB_33      0.0066871000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3624
_reflns_number_total             5950
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.315
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.202
_refine_ls_extinction_coef       0.00112(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         5950
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0436
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0323P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0839
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), N1(H1A), C3(H3), C4(H4), C5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.75809(6) 0.10215(5) 0.71051(4) 0.04625(13) Uani 1 1 d . . . . .
Pb1 Pb 1.02085(2) -0.07485(2) 0.75207(2) 0.03627(7) Uani 1 1 d . . . . .
Br2 Br 0.89228(6) -0.30175(5) 0.60366(3) 0.04435(13) Uani 1 1 d . . . . .
Br3 Br 0.89334(6) -0.28905(5) 0.86167(3) 0.04267(12) Uani 1 1 d . . . . .
C1 C 0.2750(6) 0.6187(6) 0.5591(4) 0.0492(13) Uani 1 1 d . . . . .
H1 H 0.2305 0.5157 0.5541 0.059 Uiso 1 1 calc R U . . .
I1 I 0.53824(5) 0.42494(4) 0.64982(3) 0.05544(11) Uani 1 1 d . . . . .
N1 N 0.2000(5) 0.7532(6) 0.5242(3) 0.0564(12) Uani 1 1 d . . . . .
H1A H 0.1105 0.7412 0.4971 0.068 Uiso 1 1 calc R U . . .
C2 C 0.4167(5) 0.6347(6) 0.6018(3) 0.0393(10) Uani 1 1 d . . . . .
C3 C 0.4808(7) 0.7901(6) 0.6104(4) 0.0580(14) Uani 1 1 d . . . . .
H3 H 0.5772 0.8039 0.6404 0.070 Uiso 1 1 calc R U . . .
C4 C 0.3970(8) 0.9228(6) 0.5731(5) 0.0668(18) Uani 1 1 d . . . . .
H4 H 0.4381 1.0277 0.5781 0.080 Uiso 1 1 calc R U . . .
C5 C 0.2566(8) 0.9048(6) 0.5294(4) 0.0556(15) Uani 1 1 d . . . . .
H5 H 0.2014 0.9951 0.5038 0.067 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0331(3) 0.0357(2) 0.0660(3) 0.00249(19) 0.0061(2) 0.00265(18)
Pb1 0.03747(11) 0.03100(9) 0.03914(10) 0.00117(6) 0.00805(7) 0.00188(7)
Br2 0.0531(3) 0.0418(2) 0.0350(2) 0.00015(17) 0.0060(2) -0.0012(2)
Br3 0.0464(3) 0.0442(2) 0.0400(3) 0.00110(17) 0.0160(2) 0.0003(2)
C1 0.044(3) 0.043(3) 0.057(3) -0.005(2) 0.008(3) -0.008(2)
I1 0.0491(2) 0.04406(19) 0.0702(3) 0.00888(14) 0.01066(19) 0.00794(15)
N1 0.040(3) 0.067(3) 0.054(3) -0.002(2) -0.003(2) 0.010(2)
C2 0.038(3) 0.038(2) 0.041(3) -0.0019(18) 0.009(2) 0.002(2)
C3 0.047(4) 0.044(3) 0.078(4) -0.008(3) 0.008(3) -0.005(2)
C4 0.067(5) 0.039(3) 0.087(5) -0.004(3) 0.007(4) -0.003(3)
C5 0.074(5) 0.045(3) 0.048(3) 0.005(2) 0.016(3) 0.013(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Pb1 2.8278(5) . ?
Pb1 Br2 2.9741(5) . ?
Pb1 Br2 3.1220(5) 2_756 ?
Pb1 Br3 2.9358(5) . ?
Pb1 Br3 3.1662(5) 2_756 ?
Br2 Pb1 3.1221(5) 2_746 ?
Br3 Pb1 3.1662(5) 2_746 ?
C1 H1 0.9300 . ?
C1 N1 1.340(7) . ?
C1 C2 1.359(7) . ?
I1 C2 2.085(5) . ?
N1 H1A 0.8600 . ?
N1 C5 1.335(7) . ?
C2 C3 1.390(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.378(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.353(10) . ?
C5 H5 0.9300 . ?

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 Br2 82.054(16) . 2_756 ?
Br1 Pb1 Br2 88.237(16) . . ?
Br1 Pb1 Br3 86.978(16) . . ?
Br1 Pb1 Br3 81.422(14) . 2_756 ?
Br2 Pb1 Br2 170.234(11) . 2_756 ?
Br2 Pb1 Br3 80.655(13) 2_756 2_756 ?
Br2 Pb1 Br3 96.913(13) . 2_756 ?
Br3 Pb1 Br2 93.472(14) . 2_756 ?
Br3 Pb1 Br2 87.038(14) . . ?
Br3 Pb1 Br3 167.602(13) . 2_756 ?
Pb1 Br2 Pb1 83.494(12) . 2_746 ?
Pb1 Br3 Pb1 83.341(12) . 2_746 ?
N1 C1 H1 120.4 . . ?
N1 C1 C2 119.2(5) . . ?
C2 C1 H1 120.4 . . ?
C1 N1 H1A 118.2 . . ?
C5 N1 C1 123.6(5) . . ?
C5 N1 H1A 118.2 . . ?
C1 C2 I1 119.7(4) . . ?
C1 C2 C3 119.7(5) . . ?
C3 C2 I1 120.5(4) . . ?
C2 C3 H3 121.1 . . ?
C4 C3 C2 117.9(6) . . ?
C4 C3 H3 121.1 . . ?
C3 C4 H4 119.1 . . ?
C5 C4 C3 121.8(5) . . ?
C5 C4 H4 119.1 . . ?
N1 C5 C4 117.8(5) . . ?
N1 C5 H5 121.1 . . ?
C4 C5 H5 121.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 C5 C4 -0.7(9) . . . . ?
C1 C2 C3 C4 -1.3(9) . . . . ?
I1 C2 C3 C4 176.4(5) . . . . ?
N1 C1 C2 I1 -176.3(4) . . . . ?
N1 C1 C2 C3 1.5(8) . . . . ?
C2 C1 N1 C5 -0.5(8) . . . . ?
C2 C3 C4 C5 0.1(10) . . . . ?
C3 C4 C5 N1 0.9(10) . . . . ?

_shelx_res_file                  
;
TITL 3-IPy-PbBr3.res in P2(1)/c
REM Old TITL 3-IPy-PbBr3 in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.164, Rweak 0.008, Alpha 0.034, Orientation as input
REM Formula found by SHELXT: I4 Pb
CELL 0.71073 9.6254 8.083634 15.778616 90 105.349 90
ZERR 4 0.000434 0.000274 0.000695 0 0.0046 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br I N Pb
UNIT 20 20 12 4 4 4

L.S. 20
PLAN  7
TEMP 23(2)
CONF
HTAB
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\3-IPy-PbBr3.hkl">
REM </olex2.extras>

WGHT    0.032300
EXTI    0.001122
FVAR       0.80382
BR1   3    0.758088    0.102153    0.710506    11.00000    0.03309    0.03568 =
         0.06600    0.00249    0.00611    0.00265
PB1   6    1.020855   -0.074848    0.752067    11.00000    0.03747    0.03100 =
         0.03914    0.00117    0.00805    0.00188
BR2   3    0.892285   -0.301753    0.603661    11.00000    0.05311    0.04178 =
         0.03495    0.00015    0.00598   -0.00122
BR3   3    0.893336   -0.289047    0.861667    11.00000    0.04645    0.04423 =
         0.03996    0.00110    0.01604    0.00030
C1    1    0.274980    0.618734    0.559099    11.00000    0.04435    0.04337 =
         0.05655   -0.00472    0.00776   -0.00781
AFIX  43
H1    2    0.230544    0.515711    0.554141    11.00000   -1.20000
AFIX   0
I1    4    0.538236    0.424940    0.649818    11.00000    0.04914    0.04406 =
         0.07020    0.00888    0.01066    0.00794
N1    5    0.199980    0.753182    0.524237    11.00000    0.03964    0.06697 =
         0.05417   -0.00192   -0.00253    0.01030
AFIX  43
H1A   2    0.110498    0.741172    0.497064    11.00000   -1.20000
AFIX   0
C2    1    0.416741    0.634722    0.601782    11.00000    0.03815    0.03770 =
         0.04126   -0.00194    0.00902    0.00239
C3    1    0.480840    0.790067    0.610422    11.00000    0.04731    0.04409 =
         0.07796   -0.00769    0.00830   -0.00546
AFIX  43
H3    2    0.577219    0.803946    0.640438    11.00000   -1.20000
AFIX   0
C4    1    0.397035    0.922816    0.573102    11.00000    0.06702    0.03881 =
         0.08671   -0.00414    0.00674   -0.00275
AFIX  43
H4    2    0.438121    1.027697    0.578093    11.00000   -1.20000
AFIX   0
C5    1    0.256620    0.904832    0.529391    11.00000    0.07417    0.04503 =
         0.04757    0.00513    0.01631    0.01305
AFIX  43
H5    2    0.201363    0.995100    0.503776    11.00000   -1.20000
AFIX   0
HKLF 4

REM  3-IPy-PbBr3.res in P2(1)/c
REM R1 =  0.0436 for    3624 Fo > 4sig(Fo)  and  0.0911 for all    5950 data
REM    101 parameters refined using      0 restraints

END

WGHT      0.0323      0.0000

REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, -y, -z+1
HTAB C1 Br2_$1
EQIV $2 x-1, y+1, z
HTAB N1 Br2_$2
EQIV $3 x-1, -y+1/2, z-1/2
HTAB N1 Br3_$3
EQIV $4 x, y+1, z
HTAB C3 Br1_$4
EQIV $5 -x+1, -y+1, -z+1
HTAB C5 Br2_$5
EQIV $6 -x+1, y+3/2, -z+3/2
HTAB C5 Br3_$6

REM Highest difference peak  1.315,  deepest hole -1.132,  1-sigma level  0.202
Q1    1   0.4692  0.4009  0.6282  11.00000  0.05    1.32
Q2    1   0.5448  0.4969  0.6797  11.00000  0.05    1.25
Q3    1   0.9467 -0.0756  0.7163  11.00000  0.05    1.17
Q4    1   0.6848  0.0750  0.6961  11.00000  0.05    1.11
Q5    1   1.0934 -0.1196  0.7764  11.00000  0.05    1.10
Q6    1   1.0223  0.0228  0.7530  11.00000  0.05    1.10
Q7    1   1.0517 -0.1259  0.7993  11.00000  0.05    1.03
;
_shelx_res_checksum              66133
_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 3.407
_oxdiff_exptl_absorpt_empirical_full_min 0.523
####################################################################### 
# 
# 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_3-brpy-pbbr3
_database_code_depnum_ccdc_archive 'CCDC 2499862'
loop_
_audit_author_name
_audit_author_address
'N.I. Selivanov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2025-11-03 deposited with the CCDC.	2026-01-05 downloaded from the CCDC.
;
_audit_creation_date             2024-10-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C5 H5 Br N'
_chemical_formula_sum            'C5 H5 Br4 N Pb'
_chemical_formula_weight         605.93
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb1 Br4 C5 N1 H5'
_chemical_oxdiff_usercomment     296K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.3638(3)
_cell_length_b                   8.0748(2)
_cell_length_c                   15.7895(7)
_cell_angle_alpha                90
_cell_angle_beta                 104.490(4)
_cell_angle_gamma                90
_cell_volume                     1155.88(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6661
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.3280
_cell_measurement_theta_min      3.3850
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    28.370
_exptl_absorpt_correction_T_max  0.348
_exptl_absorpt_correction_T_min  0.037
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.482
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-13 0 3 0.0614
-8 0 20 0.0231
11 0 6 0.0722
2 0 -22 0.0512
10 0 -19 0.0240
1 -11 1 0.0874
-4 -8 16 0.0767
-6 0 22 0.0304
-7 2 21 0.0388
-1 11 0 0.0893
4 7 -17 0.0620
10 -6 5 0.0893
-11 3 15 0.0422
-8 6 -10 0.0608
4 2 -22 0.0415
10 7 -2 0.0793
4 -2 -22 0.0499
-11 -6 11 0.0672
-2 -1 2 0.0672
0 -1 0 0.0837
-12 2 -4 0.0571

_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.054
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-13.1065 -0.1191 3.0118 -0.8720 0.3088 0.3798
-8.1147 -0.1989 20.4234 -0.1457 0.0543 0.9878
11.4292 0.0458 5.9645 0.9429 -0.3327 0.0173
1.5357 0.1605 -22.0643 -0.3590 0.1240 -0.9251
9.6384 0.1994 -18.7890 0.2892 -0.1048 -0.9515
1.1832 -11.3129 0.8438 -0.2324 -0.9721 0.0308
-3.9030 -7.6614 16.2587 -0.1560 -0.6436 0.7493
-6.4422 -0.1258 21.5356 -0.0007 0.0095 1.0000
-6.5767 2.0953 21.0437 0.0449 0.2000 0.9788
-1.3236 11.3129 -0.3758 0.2324 0.9726 -0.0091
4.0815 7.3727 -16.7316 0.1500 0.6183 -0.7715
10.0245 -5.6488 4.8368 0.6502 -0.7597 0.0091
-11.1428 3.1442 14.5992 -0.3873 0.4489 0.8053
-8.0810 5.5199 -10.0562 -0.6276 0.7343 -0.2587
3.5008 1.7454 -22.0033 -0.1709 0.2038 -0.9640
9.9002 7.4167 -1.7541 0.8866 0.3692 -0.2786
3.5858 -2.0279 -21.9078 -0.2744 -0.1112 -0.9552
-10.5494 -5.8354 11.1993 -0.6836 -0.2860 0.6715
-1.9995 -0.9992 2.0018 -0.1290 -0.0445 0.1222
0.0011 -1.0007 -0.0001 -0.0295 -0.0828 0.0017
-11.7764 2.2963 -3.7425 -0.8507 0.5203 0.0755

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12978
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         3.379
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     32.00  72.00   0.50    5.00    --   23.84-138.00-140.00   80
  2  ω    -70.00 -45.00   0.50    5.00    --  -25.09 132.00 104.00   50
  3  ω    -80.00 -52.00   0.50    5.00    --  -25.09 138.00 -78.00   56
  4  ω      1.00  97.00   0.50    5.00    --   23.84  77.00 120.00  192
  5  ω    -97.00 -71.00   0.50    5.00    --  -25.09 -77.00 -30.00   52
  6  ω    -90.00 -61.00   0.50    5.00    --  -25.09-178.00-150.00   58
  7  ω    -91.00 -41.00   0.50    5.00    --  -25.09-178.00 120.00  100
  8  ω    -88.00 -11.00   0.50    5.00    --  -25.09 -57.00 -90.00  154
  9  ω    -58.00  -4.00   0.50    5.00    --  -25.09 -77.00 -30.00  108
 10  ω    -97.00 -72.00   0.50    5.00    --  -25.09 -77.00  90.00   50
 11  ω    -30.00  -5.00   0.50    5.00    --  -25.09 -77.00  90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0711906000
_diffrn_orient_matrix_UB_12      0.0295843000
_diffrn_orient_matrix_UB_13      0.0214387000
_diffrn_orient_matrix_UB_21      -0.0258818000
_diffrn_orient_matrix_UB_22      0.0827164000
_diffrn_orient_matrix_UB_23      -0.0068187000
_diffrn_orient_matrix_UB_31      -0.0196409000
_diffrn_orient_matrix_UB_32      -0.0017529000
_diffrn_orient_matrix_UB_33      0.0405470000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2308
_reflns_number_total             2647
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.171
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.00051(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2647
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0275
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0253P)²+2.9968P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0649
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), N1(H1A), C3(H3), C4(H4), C5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.88761(7) 1.26883(8) 0.86171(4) 0.04385(16) Uani 1 1 d . . . . .
Pb1 Pb 1.01929(2) 1.05368(3) 0.75089(2) 0.03745(10) Uani 1 1 d . . . . .
Br2 Br 0.89011(8) 1.28985(8) 0.60510(4) 0.04700(17) Uani 1 1 d . . . . .
Br3 Br 0.75219(6) 0.87562(8) 0.70888(5) 0.04808(18) Uani 1 1 d . . . . .
C1 C 0.2830(7) 0.3834(8) 0.5525(5) 0.0478(16) Uani 1 1 d . . . . .
H1 H 0.2409 0.4881 0.5422 0.057 Uiso 1 1 calc R U . . .
Br4 Br 0.53358(9) 0.55352(9) 0.64612(7) 0.0675(2) Uani 1 1 d . . . . .
N1 N 0.2061(6) 0.2483(8) 0.5189(4) 0.0561(15) Uani 1 1 d . . . . .
H1A H 0.1178 0.2615 0.4871 0.067 Uiso 1 1 calc R U . . .
C2 C 0.4231(7) 0.3647(8) 0.6017(4) 0.0425(14) Uani 1 1 d . . . . .
C3 C 0.4826(8) 0.2075(9) 0.6192(7) 0.064(2) Uani 1 1 d . . . . .
H3 H 0.5774 0.1927 0.6544 0.077 Uiso 1 1 calc R U . . .
C4 C 0.3976(9) 0.0736(9) 0.5832(6) 0.068(2) Uani 1 1 d . . . . .
H4 H 0.4357 -0.0328 0.5940 0.081 Uiso 1 1 calc R U . . .
C5 C 0.2588(9) 0.0955(9) 0.5321(6) 0.0601(19) Uani 1 1 d . . . . .
H5 H 0.2021 0.0052 0.5070 0.072 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0462(3) 0.0428(3) 0.0443(4) -0.0010(3) 0.0146(3) -0.0007(3)
Pb1 0.03775(14) 0.02955(13) 0.04292(16) -0.00113(9) 0.00606(10) -0.00198(8)
Br2 0.0552(4) 0.0426(3) 0.0388(4) -0.0003(3) 0.0035(3) -0.0008(3)
Br3 0.0335(3) 0.0354(3) 0.0706(5) -0.0021(3) 0.0043(3) -0.0022(2)
C1 0.045(3) 0.042(3) 0.054(4) 0.003(3) 0.007(3) 0.004(3)
Br4 0.0560(4) 0.0488(4) 0.0944(7) -0.0160(4) 0.0126(4) -0.0130(3)
N1 0.042(3) 0.062(4) 0.056(4) 0.007(3) -0.005(3) -0.006(3)
C2 0.039(3) 0.037(3) 0.053(4) -0.002(3) 0.014(3) -0.007(3)
C3 0.040(4) 0.046(4) 0.096(7) 0.009(4) -0.001(4) 0.001(3)
C4 0.064(5) 0.037(4) 0.096(7) 0.000(4) 0.007(5) 0.004(3)
C5 0.062(5) 0.054(4) 0.063(5) -0.004(4) 0.014(4) -0.015(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Pb1 2.9462(7) . ?
Br1 Pb1 3.1603(7) 2_756 ?
Pb1 Br1 3.1602(7) 2_746 ?
Pb1 Br2 3.0762(7) 2_746 ?
Pb1 Br2 3.0009(7) . ?
Pb1 Br3 2.8164(6) . ?
Br2 Pb1 3.0762(7) 2_756 ?
C1 H1 0.9300 . ?
C1 N1 1.341(9) . ?
C1 C2 1.356(9) . ?
Br4 C2 1.877(6) . ?
N1 H1A 0.8600 . ?
N1 C5 1.326(9) . ?
C2 C3 1.386(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.377(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.359(11) . ?
C5 H5 0.9300 . ?

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
Pb1 Br1 Pb1 83.089(16) . 2_756 ?
Br1 Pb1 Br1 168.146(18) . 2_746 ?
Br1 Pb1 Br2 86.134(19) . . ?
Br1 Pb1 Br2 92.77(2) . 2_746 ?
Br2 Pb1 Br1 98.393(19) . 2_746 ?
Br2 Pb1 Br1 81.251(18) 2_746 2_746 ?
Br2 Pb1 Br2 172.210(13) . 2_746 ?
Br3 Pb1 Br1 81.353(19) . 2_746 ?
Br3 Pb1 Br1 87.82(2) . . ?
Br3 Pb1 Br2 83.40(2) . 2_746 ?
Br3 Pb1 Br2 88.85(2) . . ?
Pb1 Br2 Pb1 83.652(17) . 2_756 ?
N1 C1 H1 120.6 . . ?
N1 C1 C2 118.9(6) . . ?
C2 C1 H1 120.6 . . ?
C1 N1 H1A 118.2 . . ?
C5 N1 C1 123.6(6) . . ?
C5 N1 H1A 118.2 . . ?
C1 C2 Br4 119.2(5) . . ?
C1 C2 C3 119.9(6) . . ?
C3 C2 Br4 120.9(5) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 C2 118.4(7) . . ?
C4 C3 H3 120.8 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.7(7) . . ?
C5 C4 H4 119.6 . . ?
N1 C5 C4 118.5(7) . . ?
N1 C5 H5 120.8 . . ?
C4 C5 H5 120.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 C5 C4 0.8(12) . . . . ?
C1 C2 C3 C4 2.0(12) . . . . ?
Br4 C2 C3 C4 -178.5(7) . . . . ?
N1 C1 C2 Br4 178.1(5) . . . . ?
N1 C1 C2 C3 -2.4(11) . . . . ?
C2 C1 N1 C5 1.0(11) . . . . ?
C2 C3 C4 C5 -0.2(14) . . . . ?
C3 C4 C5 N1 -1.1(14) . . . . ?

_shelx_res_file                  
;
TITL 3-brpy-pbbr3_a.res in P2(1)/c
REM Old TITL 3-BrPy-PbBr3 in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.126, Rweak 0.007, Alpha 0.039, Orientation as input
REM Formula found by SHELXT: Br4 Pb
CELL 0.71073 9.363804 8.074795 15.789534 90 104.49 90
ZERR 4 0.000345 0.000245 0.000706 0 0.0042 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br N Pb
UNIT 20 20 16 4 4

L.S. 20
PLAN  7
TEMP 23(2)
CONF
BOND $H
list 4
MORE -1
fmap 2 53
acta
OMIT -4 55
REM <olex2.extras>
REM <HklSrc "%.\\3-BrPy-PbBr3.hkl">
REM </olex2.extras>

WGHT    0.025300    2.996800
EXTI    0.000507
FVAR       1.14851
BR1   3    0.887608    1.268829    0.861711    11.00000    0.04625    0.04276 =
         0.04430   -0.00096    0.01463   -0.00070
PB1   5    1.019290    1.053678    0.750892    11.00000    0.03775    0.02955 =
         0.04292   -0.00113    0.00606   -0.00198
BR2   3    0.890107    1.289849    0.605104    11.00000    0.05518    0.04257 =
         0.03884   -0.00026    0.00347   -0.00085
BR3   3    0.752189    0.875622    0.708878    11.00000    0.03355    0.03542 =
         0.07063   -0.00205    0.00433   -0.00221
C1    1    0.283016    0.383395    0.552478    11.00000    0.04463    0.04208 =
         0.05378    0.00279    0.00702    0.00446
AFIX  43
H1    2    0.240938    0.488130    0.542157    11.00000   -1.20000
AFIX   0
BR4   3    0.533578    0.553519    0.646119    11.00000    0.05603    0.04881 =
         0.09443   -0.01604    0.01265   -0.01296
N1    4    0.206114    0.248273    0.518897    11.00000    0.04159    0.06178 =
         0.05599    0.00651   -0.00468   -0.00582
AFIX  43
H1A   2    0.117815    0.261463    0.487068    11.00000   -1.20000
AFIX   0
C2    1    0.423144    0.364708    0.601727    11.00000    0.03892    0.03708 =
         0.05307   -0.00152    0.01434   -0.00678
C3    1    0.482561    0.207453    0.619213    11.00000    0.03974    0.04631 =
         0.09598    0.00890   -0.00056    0.00065
AFIX  43
H3    2    0.577434    0.192664    0.654376    11.00000   -1.20000
AFIX   0
C4    1    0.397612    0.073647    0.583219    11.00000    0.06385    0.03691 =
         0.09582    0.00047    0.00681    0.00410
AFIX  43
H4    2    0.435666   -0.032832    0.594021    11.00000   -1.20000
AFIX   0
C5    1    0.258835    0.095458    0.532107    11.00000    0.06213    0.05415 =
         0.06318   -0.00419    0.01436   -0.01533
AFIX  43
H5    2    0.202106    0.005250    0.506957    11.00000   -1.20000
AFIX   0
HKLF 4

REM  3-brpy-pbbr3_a.res in P2(1)/c
REM R1 =  0.0275 for    2308 Fo > 4sig(Fo)  and  0.0347 for all    2647 data
REM    101 parameters refined using      0 restraints

END

WGHT      0.0253      2.9967

REM Highest difference peak  1.171,  deepest hole -0.891,  1-sigma level  0.157
Q1    1   0.9484  1.0412  0.7760  11.00000  0.05    1.17
Q2    1   1.0850  1.0657  0.7233  11.00000  0.05    1.00
Q3    1   0.5447  0.4816  0.6860  11.00000  0.05    0.77
Q4    1   1.0611  1.0660  0.8147  11.00000  0.05    0.75
Q5    1   0.9970  1.1152  0.7021  11.00000  0.05    0.74
Q6    1   1.0729  1.1443  0.7822  11.00000  0.05    0.72
Q7    1   0.8510  0.9030  0.7015  11.00000  0.05    0.68
;
_shelx_res_checksum              7275
_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 1.723
_oxdiff_exptl_absorpt_empirical_full_min 0.726
