# Electronic Supplementary Material (ESI) for Materials Chemistry Frontiers.
# This journal is © the Partner Organisations 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1rt
_database_code_depnum_ccdc_archive 'CCDC 2132780'
loop_
_audit_author_name
_audit_author_address
'Dongying Fu Fu'
;Institute of Crystalline Materials, Shanxi University, Taiyuan
China
;
_audit_update_record             
;
2022-01-06 deposited with the CCDC.	2022-03-29 downloaded from the CCDC.
;
_audit_creation_date             2021-12-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C9 H16 N O'
_chemical_formula_sum            'C9 H16 Br3 N O Pb'
_chemical_formula_weight         601.15
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C N H Pb O Br'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.6914(3)
_cell_length_b                   10.0950(4)
_cell_length_c                   16.6347(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1459.52(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5633
_cell_measurement_temperature    301.77(10)
_cell_measurement_theta_max      31.1130
_cell_measurement_theta_min      2.3650
_shelx_estimated_absorpt_T_max   0.220
_shelx_estimated_absorpt_T_min   0.183
_exptl_absorpt_coefficient_mu    19.751
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
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    2.736
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.786
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8254
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.752
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.826
_diffrn_reflns_theta_min         2.360
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      301.77(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.786
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -8.00  79.00   0.50    2.00    --    5.05  24.00 -19.00  174
  2  ω    -27.00  10.00   0.50    2.00    --    5.05 -24.00 175.00   74
  3  ω    -18.00  21.00   0.50    2.00    --   -5.21 -99.00  90.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0054921000
_diffrn_orient_matrix_UB_12      -0.0507556000
_diffrn_orient_matrix_UB_13      0.0293588000
_diffrn_orient_matrix_UB_21      0.0275867000
_diffrn_orient_matrix_UB_22      -0.0444855000
_diffrn_orient_matrix_UB_23      -0.0297732000
_diffrn_orient_matrix_UB_31      0.0765720000
_diffrn_orient_matrix_UB_32      0.0194251000
_diffrn_orient_matrix_UB_33      0.0085433000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.682
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.706
_reflns_number_gt                3079
_reflns_number_total             3449
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.963
_refine_diff_density_min         -1.673
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details 
;
 Flack x determined using 1130 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(7)
_refine_ls_extinction_coef       0.0023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         3449
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0335
_refine_ls_restrained_S_all      1.062
_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)+(0.0471P)²+1.5833P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0812
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Ternary CH refined with riding coordinates:
 C6(H6), C7(H7)
1.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C8(H8A,H8B), C12(H12A,H12B), C5(H5A,H5B), C13(H13A,H13B)
1.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
1.d Idealised tetrahedral OH refined as rotating group:
 O15(H15)
;
_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
Pb1 Pb 0.46349(4) 0.25482(4) 0.49280(2) 0.03223(13) Uani 1 1 d . . . . .
Br2 Br 0.22969(12) 0.42103(13) 0.57296(7) 0.0435(3) Uani 1 1 d . . . . .
Br3 Br 0.38347(14) 0.04227(13) 0.59249(7) 0.0468(3) Uani 1 1 d . . . . .
Br4 Br 0.23590(15) 0.16437(15) 0.37824(8) 0.0526(3) Uani 1 1 d . . . . .
C10 C 0.3321(12) 0.8178(12) 0.2765(7) 0.040(3) Uani 1 1 d . . . . .
N1 N 0.2390(9) 0.7167(8) 0.3214(4) 0.0272(17) Uani 1 1 d . . . . .
C11 C 0.2373(13) 0.7500(15) 0.4097(6) 0.045(2) Uani 1 1 d . . . . .
H11A H 0.167279 0.691055 0.437695 0.054 Uiso 1 1 calc R U . . .
H11B H 0.201485 0.840129 0.417209 0.054 Uiso 1 1 calc R U . . .
O15 O 0.5135(9) 0.4753(9) 0.3812(5) 0.051(2) Uani 1 1 d . . . . .
H15 H 0.605472 0.471769 0.391914 0.076 Uiso 1 1 calc R U . . .
C6 C 0.5143(12) 0.7175(11) 0.3755(7) 0.038(2) Uani 1 1 d . . . . .
H6 H 0.619519 0.718578 0.396584 0.046 Uiso 1 1 calc R U . . .
C7 C 0.4838(12) 0.5899(11) 0.3331(6) 0.035(2) Uani 1 1 d . . . . .
H7 H 0.545853 0.585770 0.284025 0.042 Uiso 1 1 calc R U . . .
C8 C 0.3124(12) 0.5821(12) 0.3111(7) 0.041(2) Uani 1 1 d . . . . .
H8A H 0.301432 0.553107 0.255763 0.049 Uiso 1 1 calc R U . . .
H8B H 0.261237 0.518204 0.345407 0.049 Uiso 1 1 calc R U . . .
C12 C 0.3980(13) 0.7355(15) 0.4443(6) 0.048(3) Uani 1 1 d . . . . .
H12A H 0.401795 0.659476 0.479863 0.058 Uiso 1 1 calc R U . . .
H12B H 0.424139 0.813794 0.475243 0.058 Uiso 1 1 calc R U . . .
C14 C -0.0223(15) 0.8294(17) 0.3039(8) 0.058(4) Uani 1 1 d . . . . .
H14A H -0.111670 0.827388 0.269990 0.088 Uiso 1 1 calc R U . . .
H14B H 0.034413 0.909393 0.294053 0.088 Uiso 1 1 calc R U . . .
H14C H -0.053457 0.826487 0.359186 0.088 Uiso 1 1 calc R U . . .
C5 C 0.4929(14) 0.8287(14) 0.3136(8) 0.048(3) Uani 1 1 d . . . . .
H5A H 0.504719 0.914117 0.339539 0.058 Uiso 1 1 calc R U . . .
H5B H 0.570392 0.821243 0.271871 0.058 Uiso 1 1 calc R U . . .
C13 C 0.0778(11) 0.7117(12) 0.2856(7) 0.040(3) Uani 1 1 d . . . . .
H13A H 0.086896 0.703385 0.227682 0.048 Uiso 1 1 calc R U . . .
H13B H 0.026739 0.632718 0.305249 0.048 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
Pb1 0.03169(19) 0.0326(2) 0.0324(2) 0.00121(18) 0.00179(12) 0.00136(17)
Br2 0.0386(5) 0.0453(7) 0.0467(6) -0.0150(5) -0.0007(4) 0.0038(5)
Br3 0.0496(6) 0.0424(7) 0.0484(6) 0.0131(5) 0.0101(5) 0.0012(5)
Br4 0.0520(7) 0.0608(9) 0.0450(6) -0.0157(6) -0.0113(5) 0.0060(6)
C10 0.039(6) 0.038(7) 0.044(6) 0.016(5) -0.005(4) -0.011(5)
N1 0.033(4) 0.025(5) 0.023(4) -0.005(3) -0.002(3) -0.001(3)
C11 0.054(6) 0.056(8) 0.025(4) -0.005(6) 0.005(4) 0.000(6)
O15 0.039(4) 0.043(5) 0.069(5) 0.016(4) -0.001(4) 0.005(4)
C6 0.037(5) 0.036(6) 0.042(5) 0.001(5) -0.011(4) -0.004(4)
C7 0.036(5) 0.029(6) 0.040(5) 0.010(5) 0.003(4) -0.003(4)
C8 0.043(6) 0.029(6) 0.049(6) -0.006(5) -0.003(5) 0.006(5)
C12 0.060(7) 0.054(8) 0.030(5) -0.005(6) -0.012(4) -0.003(6)
C14 0.038(6) 0.081(11) 0.057(8) 0.004(7) -0.004(5) 0.020(7)
C5 0.046(7) 0.038(7) 0.061(8) 0.010(6) -0.007(5) -0.015(5)
C13 0.031(5) 0.041(7) 0.048(6) 0.000(5) -0.007(4) -0.005(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 2.9534(11) . ?
Pb1 Br2 3.1146(12) 3_556 ?
Pb1 Br3 2.7997(12) . ?
Pb1 Br4 2.8945(12) . ?
C10 N1 1.501(13) . ?
C10 C5 1.532(15) . ?
N1 C11 1.508(12) . ?
N1 C8 1.511(14) . ?
N1 C13 1.523(12) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.517(16) . ?
O15 H15 0.8200 . ?
O15 C7 1.429(13) . ?
C6 H6 0.9800 . ?
C6 C7 1.491(16) . ?
C6 C12 1.538(16) . ?
C6 C5 1.534(17) . ?
C7 H7 0.9800 . ?
C7 C8 1.536(15) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14 C13 1.503(19) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br2 173.45(2) . 3_556 ?
Br3 Pb1 Br2 87.46(4) . 3_556 ?
Br3 Pb1 Br2 89.83(4) . . ?
Br3 Pb1 Br4 88.76(4) . . ?
Br4 Pb1 Br2 90.36(3) . . ?
Br4 Pb1 Br2 95.54(3) . 3_556 ?
Pb1 Br2 Pb1 91.65(3) . 3_456 ?
N1 C10 C5 109.9(9) . . ?
C10 N1 C11 109.8(9) . . ?
C10 N1 C8 109.1(8) . . ?
C10 N1 C13 108.9(8) . . ?
C11 N1 C8 108.4(9) . . ?
C11 N1 C13 112.3(8) . . ?
C8 N1 C13 108.3(8) . . ?
N1 C11 H11A 109.7 . . ?
N1 C11 H11B 109.7 . . ?
N1 C11 C12 109.8(9) . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11A 109.7 . . ?
C12 C11 H11B 109.7 . . ?
C7 O15 H15 109.5 . . ?
C7 C6 H6 110.2 . . ?
C7 C6 C12 109.7(9) . . ?
C7 C6 C5 107.1(9) . . ?
C12 C6 H6 110.2 . . ?
C5 C6 H6 110.2 . . ?
C5 C6 C12 109.5(10) . . ?
O15 C7 C6 113.7(9) . . ?
O15 C7 H7 109.4 . . ?
O15 C7 C8 105.5(9) . . ?
C6 C7 H7 109.4 . . ?
C6 C7 C8 109.2(9) . . ?
C8 C7 H7 109.4 . . ?
N1 C8 C7 109.7(9) . . ?
N1 C8 H8A 109.7 . . ?
N1 C8 H8B 109.7 . . ?
C7 C8 H8A 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
C11 C12 C6 109.5(8) . . ?
C11 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
C6 C12 H12A 109.8 . . ?
C6 C12 H12B 109.8 . . ?
H12A C12 H12B 108.2 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
C10 C5 C6 109.2(9) . . ?
C10 C5 H5A 109.8 . . ?
C10 C5 H5B 109.8 . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.3 . . ?
N1 C13 H13A 108.4 . . ?
N1 C13 H13B 108.4 . . ?
C14 C13 N1 115.3(10) . . ?
C14 C13 H13A 108.4 . . ?
C14 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N1 C11 C12 -66.2(13) . . . . ?
C10 N1 C8 C7 52.0(11) . . . . ?
C10 N1 C13 C14 -72.1(12) . . . . ?
N1 C10 C5 C6 9.0(15) . . . . ?
N1 C11 C12 C6 10.5(16) . . . . ?
C11 N1 C8 C7 -67.6(11) . . . . ?
C11 N1 C13 C14 49.7(14) . . . . ?
O15 C7 C8 N1 135.8(9) . . . . ?
C6 C7 C8 N1 13.1(12) . . . . ?
C7 C6 C12 C11 -65.2(14) . . . . ?
C7 C6 C5 C10 55.6(13) . . . . ?
C8 N1 C11 C12 52.9(13) . . . . ?
C8 N1 C13 C14 169.4(10) . . . . ?
C12 C6 C7 O15 -67.0(11) . . . . ?
C12 C6 C7 C8 50.6(12) . . . . ?
C12 C6 C5 C10 -63.3(13) . . . . ?
C5 C10 N1 C11 54.4(12) . . . . ?
C5 C10 N1 C8 -64.2(12) . . . . ?
C5 C10 N1 C13 177.7(10) . . . . ?
C5 C6 C7 O15 174.3(9) . . . . ?
C5 C6 C7 C8 -68.1(11) . . . . ?
C5 C6 C12 C11 52.0(14) . . . . ?
C13 N1 C11 C12 172.5(11) . . . . ?
C13 N1 C8 C7 170.4(9) . . . . ?

_shelx_res_file                  
;
TITL
    hyy_n_et_knc_pbbr3_300k_auto.res
    created by SHELXL-2018/3 at 08:52:35 on 15-Nov-2021
CELL 0.71073 8.691409 10.094963 16.634683 90 90 90
ZERR 4 0.000304 0.000417 0.000582 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br N O Pb
UNIT 36 64 12 4 4 4

L.S. 34
PLAN  9
SIZE 0.13 0.12 0.11
TEMP 29
CONF
fmap 2
acta
MORE -1
BOND $H
REM <olex2.extras>
REM <HklSrc "%.\\HYY_N_Et_KNC_PbBr3_300K_auto.hkl">
REM </olex2.extras>

WGHT    0.047100    1.583300
EXTI    0.002274
FVAR       1.16777
PB1   6    0.463493    0.254823    0.492798    11.00000    0.03169    0.03264 =
         0.03236    0.00121    0.00179    0.00136
BR2   3    0.229687    0.421031    0.572957    11.00000    0.03858    0.04531 =
         0.04673   -0.01496   -0.00070    0.00378
BR3   3    0.383472    0.042265    0.592492    11.00000    0.04957    0.04239 =
         0.04844    0.01309    0.01005    0.00121
BR4   3    0.235902    0.164371    0.378237    11.00000    0.05205    0.06079 =
         0.04503   -0.01569   -0.01127    0.00598
C10   1    0.332059    0.817811    0.276467    11.00000    0.03904    0.03772 =
         0.04388    0.01551   -0.00458   -0.01107
N1    4    0.238999    0.716718    0.321365    11.00000    0.03349    0.02525 =
         0.02292   -0.00546   -0.00187   -0.00136
C11   1    0.237329    0.749972    0.409725    11.00000    0.05387    0.05596 =
         0.02532   -0.00465    0.00535   -0.00006
AFIX  23
H11A  2    0.167279    0.691055    0.437695    11.00000   -1.20000
H11B  2    0.201485    0.840129    0.417209    11.00000   -1.20000
AFIX   0
O15   5    0.513483    0.475323    0.381180    11.00000    0.03899    0.04331 =
         0.06925    0.01573   -0.00125    0.00498
AFIX 147
H15   2    0.605472    0.471769    0.391914    11.00000   -1.50000
AFIX   0
C6    1    0.514266    0.717464    0.375463    11.00000    0.03711    0.03643 =
         0.04186    0.00079   -0.01072   -0.00369
AFIX  13
H6    2    0.619519    0.718578    0.396584    11.00000   -1.20000
AFIX   0
C7    1    0.483769    0.589888    0.333140    11.00000    0.03585    0.02933 =
         0.03955    0.00983    0.00343   -0.00299
AFIX  13
H7    2    0.545853    0.585770    0.284025    11.00000   -1.20000
AFIX   0
C8    1    0.312421    0.582130    0.311054    11.00000    0.04343    0.02892 =
         0.04925   -0.00582   -0.00299    0.00593
AFIX  23
H8A   2    0.301432    0.553107    0.255763    11.00000   -1.20000
H8B   2    0.261237    0.518204    0.345407    11.00000   -1.20000
AFIX   0
C12   1    0.398032    0.735533    0.444282    11.00000    0.06003    0.05407 =
         0.02978   -0.00476   -0.01201   -0.00281
AFIX  23
H12A  2    0.401795    0.659476    0.479863    11.00000   -1.20000
H12B  2    0.424139    0.813794    0.475243    11.00000   -1.20000
AFIX   0
C14   1   -0.022260    0.829381    0.303853    11.00000    0.03790    0.08063 =
         0.05650    0.00402   -0.00393    0.02030
AFIX 137
H14A  2   -0.111670    0.827388    0.269990    11.00000   -1.50000
H14B  2    0.034413    0.909393    0.294053    11.00000   -1.50000
H14C  2   -0.053457    0.826487    0.359186    11.00000   -1.50000
AFIX   0
C5    1    0.492908    0.828666    0.313596    11.00000    0.04636    0.03827 =
         0.06067    0.01036   -0.00703   -0.01496
AFIX  23
H5A   2    0.504719    0.914117    0.339539    11.00000   -1.20000
H5B   2    0.570392    0.821243    0.271871    11.00000   -1.20000
AFIX   0
C13   1    0.077849    0.711749    0.285580    11.00000    0.03095    0.04084 =
         0.04830    0.00024   -0.00729   -0.00451
AFIX  23
H13A  2    0.086896    0.703385    0.227682    11.00000   -1.20000
H13B  2    0.026739    0.632718    0.305249    11.00000   -1.20000
AFIX   0
HKLF 4




REM
REM wR2 = 0.0812, GooF = S = 1.062, Restrained GooF = 1.062 for all data
REM R1 = 0.0335 for 3079 Fo > 4sig(Fo) and 0.0412 for all 3449 data
REM 139 parameters refined using 0 restraints

END

WGHT      0.0471      1.5681

REM Highest difference peak  1.963,  deepest hole -1.673,  1-sigma level  0.185
Q1    1   0.4664  0.2009  0.4427  11.00000  0.05    1.96
Q2    1   0.4662  0.3135  0.4420  11.00000  0.05    1.77
Q3    1   0.4614  0.3155  0.5450  11.00000  0.05    1.74
Q4    1   0.4652  0.2032  0.5395  11.00000  0.05    1.72
Q5    1   0.4571  0.2514  0.5967  11.00000  0.05    1.15
Q6    1   0.4780  0.2573  0.3893  11.00000  0.05    1.04
Q7    1   0.4749  0.3857  0.4925  11.00000  0.05    1.00
Q8    1   0.4478  0.1336  0.4932  11.00000  0.05    0.88
Q9    1   0.5520  0.2603  0.4778  11.00000  0.05    0.88
;
_shelx_res_checksum              43618
_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 3.208
_oxdiff_exptl_absorpt_empirical_full_min 0.610
####################################################################### 
# 
# 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_2ht
_database_code_depnum_ccdc_archive 'CCDC 2132788'
loop_
_audit_author_name
_audit_author_address
'Dongying Fu'
;Institute of Crystalline Materials, Shanxi University, Taiyuan
China
;
_audit_update_record             
;
2022-01-06 deposited with the CCDC.	2022-03-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 N, Br3 Pb, O'
_chemical_formula_sum            'C8 Br3 N O Pb'
_chemical_formula_weight         573.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_H-M_alt        'P 63 2 2'
_space_group_name_Hall           'P 6c 2c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   10.761(2)
_cell_length_b                   10.761(2)
_cell_length_c                   7.887(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     790.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    493(2)
_cell_measurement_reflns_used    391
_cell_measurement_theta_min      3.3650
_cell_measurement_theta_max      29.2400

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.406
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   0.108
_exptl_transmission_factor_max   0.135
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    18.218
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      493(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4354
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.185
_diffrn_reflns_theta_max         31.237
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             746
_reflns_number_gt                124
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.495
_reflns_Friedel_fraction_max     0.782
_reflns_Friedel_fraction_full    1.000

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0500P)²+1.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 21 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.7(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         746
_refine_ls_number_parameters     40
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.2673
_refine_ls_R_factor_gt           0.0894
_refine_ls_wR_factor_ref         0.2561
_refine_ls_wR_factor_gt          0.1907
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002

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
O1 O 0.414(14) 0.889(16) 0.48(2) 0.647(5) Uani 0.1667 1 d . U P . .
Pb1 Pb 1.0000 1.0000 0.0000 0.2967(9) Uani 1 6 d S T P . .
Br1 Br 0.7536(3) 0.87682(17) 0.2500 0.401(2) Uani 1 2 d S T P . .
N1 N 0.3333 0.6667 0.7500 0.651(3) Uani 1 6 d DS TU P . .
C2 C 0.4426(17) 0.8108(9) 0.6797(7) 0.651(3) Uani 0.5 1 d D U P . .
C3 C 0.4687(11) 0.7902(13) 0.4977(7) 0.649(3) Uani 0.5 1 d D U P . .
C1 C 0.3333 0.6667 0.4288(7) 0.649(3) Uani 1 3 d DS TU P . .

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
O1 0.648(8) 0.650(5) 0.644(8) -0.002(6) 0.002(8) 0.324(4)
Pb1 0.2849(10) 0.2849(10) 0.3203(19) 0.000 0.000 0.1424(5)
Br1 0.276(3) 0.402(3) 0.482(4) -0.036(7) 0.000 0.1378(13)
N1 0.651(4) 0.651(4) 0.651(5) 0.000 0.000 0.3255(18)
C2 0.651(4) 0.650(4) 0.650(4) 0.000(3) 0.000(4) 0.324(3)
C3 0.650(4) 0.650(4) 0.648(4) 0.000(4) 0.000(4) 0.324(3)
C1 0.649(3) 0.649(3) 0.648(5) 0.000 0.000 0.3247(17)

_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
O1 C3 1.46(18) . ?
Pb1 Br1 3.026(3) 5_564 ?
Pb1 Br1 3.026(3) 2_765 ?
Pb1 Br1 3.026(3) 6_654 ?
Pb1 Br1 3.026(3) 3_675 ?
Pb1 Br1 3.026(3) 4_774 ?
Pb1 Br1 3.026(3) . ?
Br1 Pb1 3.026(3) 4_775 ?
N1 C2 1.507(7) 11_556 ?
N1 C2 1.507(7) 2_665 ?
N1 C2 1.507(7) 10_666 ?
N1 C2 1.507(7) 12_566 ?
N1 C2 1.507(7) 3_565 ?
N1 C2 1.507(7) . ?
C2 C2 1.37(2) 11_556 ?
C2 C3 1.500(9) . ?
C3 C1 1.500(8) . ?
C1 C3 1.500(8) 2_665 ?
C1 C3 1.500(8) 3_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 180.0 5_564 2_765 ?
Br1 Pb1 Br1 82.14(6) 5_564 6_654 ?
Br1 Pb1 Br1 97.86(6) 2_765 6_654 ?
Br1 Pb1 Br1 97.86(6) 5_564 3_675 ?
Br1 Pb1 Br1 82.14(6) 2_765 3_675 ?
Br1 Pb1 Br1 180.0 6_654 3_675 ?
Br1 Pb1 Br1 82.14(6) 5_564 4_774 ?
Br1 Pb1 Br1 97.86(6) 2_765 4_774 ?
Br1 Pb1 Br1 82.14(6) 6_654 4_774 ?
Br1 Pb1 Br1 97.86(6) 3_675 4_774 ?
Br1 Pb1 Br1 97.86(6) 5_564 . ?
Br1 Pb1 Br1 82.14(6) 2_765 . ?
Br1 Pb1 Br1 97.86(6) 6_654 . ?
Br1 Pb1 Br1 82.14(6) 3_675 . ?
Br1 Pb1 Br1 180.0 4_774 . ?
Pb1 Br1 Pb1 81.31(8) 4_775 . ?
C2 N1 C2 95.0(15) 11_556 2_665 ?
C2 N1 C2 107.3(3) 11_556 10_666 ?
C2 N1 C2 54.0(10) 2_665 10_666 ?
C2 N1 C2 107.3(3) 11_556 12_566 ?
C2 N1 C2 155.1(16) 2_665 12_566 ?
C2 N1 C2 107.3(3) 10_666 12_566 ?
C2 N1 C2 155.1(16) 11_556 3_565 ?
C2 N1 C2 107.3(3) 2_665 3_565 ?
C2 N1 C2 95.0(15) 10_666 3_565 ?
C2 N1 C2 54.0(10) 12_566 3_565 ?
C2 N1 C2 54.0(10) 11_556 . ?
C2 N1 C2 107.3(3) 2_665 . ?
C2 N1 C2 155.1(15) 10_666 . ?
C2 N1 C2 95.0(15) 12_566 . ?
C2 N1 C2 107.3(3) 3_565 . ?
C2 C2 C3 158(2) 11_556 . ?
C2 C2 N1 63.0(5) 11_556 . ?
C3 C2 N1 107.9(6) . . ?
O1 C3 C2 78(8) . . ?
O1 C3 C1 93(5) . . ?
C2 C3 C1 107.9(7) . . ?
C3 C1 C3 107.6(3) 2_665 3_565 ?
C3 C1 C3 107.6(3) 2_665 . ?
C3 C1 C3 107.6(3) 3_565 . ?

_refine_diff_density_max         0.210
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.096



_shelx_res_file                  
;

    P6322.res created by SHELXL-2014/7

TITL P6322 in P6(3)22
CELL 0.71073  10.7607  10.7607   7.8869  90.000  90.000 120.000
ZERR    2.00   0.0024   0.0024   0.0035   0.000   0.000   0.000
LATT -1
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SYMM -X, -Y, 0.5+Z
SYMM Y, -X+Y, 0.5+Z
SYMM X-Y, X, 0.5+Z
SYMM Y, X, -Z
SYMM X-Y, -Y, -Z
SYMM -X, -X+Y, -Z
SYMM -Y, -X, 0.5-Z
SYMM -X+Y, Y, 0.5-Z
SYMM X, X-Y, 0.5-Z
SFAC Br C  N  Pb O
UNIT 6 16 2 2 2
L.S. 152
ACTA
BOND
FMAP 2
PLAN 20
DFIX 2.43 0.01 C1 C2
DFIX 2.43 0.01 N1 C3
DFIX 2.53 0.01 C1 N1
DFIX 1.5 0.01 C2 N1 C3 C2 C3 C1
ISOR 0.01 C1 C2 C3 N1  O1
DELU 0.01 C1 C2 C3 N1  O1
SIMU 0.01 C1 C2 C3 N1  O1
DAMP 2000
WGHT    0.050000    1.000000
FVAR       0.58646
MOLE 1
O1    5    0.413806    0.889299    0.483574    10.16667    0.64756    0.64969 =
         0.64379   -0.00207    0.00162    0.32351
PB1   4    1.000000    1.000000    0.000000    10.16667    0.28489    0.28489 =
         0.32025    0.00000    0.00000    0.14244
BR1   1    0.753637    0.876819    0.250000    10.50000    0.27565    0.40237 =
         0.48194   -0.03558    0.00000    0.13782
N1    3    0.333333    0.666667    0.750000    10.16667    0.65093    0.65093 =
         0.65077    0.00000    0.00000    0.32546
C2    2    0.442585    0.810824    0.679660    10.50000    0.65051    0.65006 =
         0.64975   -0.00022    0.00004    0.32388
C3    2    0.468744    0.790195    0.497721    10.50000    0.64959    0.64971 =
         0.64767   -0.00031    0.00020    0.32369
C1    2    0.333333    0.666667    0.428779    10.33333    0.64941    0.64941 =
         0.64752    0.00000    0.00000    0.32470
HKLF 4

REM  P6322 in P6(3)22
REM R1 =  0.0894 for     124 Fo > 4sig(Fo)  and  0.2673 for all     746 data
REM     40 parameters refined using     68 restraints

END

WGHT      0.1633      0.0000

REM Highest difference peak  0.210,  deepest hole -0.400,  1-sigma level  0.096
Q1    1   0.3333  0.6667  0.2500  10.16667  0.05    0.21
Q2    1   0.4080  0.8077  0.3573  11.00000  0.05    0.17
Q3    1   0.5029  0.7454  0.5420  11.00000  0.05    0.16
Q4    1   0.8175  0.9962  0.2500  11.00000  0.05    0.14
Q5    1   0.4887  0.9723  0.4253  11.00000  0.05    0.12
Q6    1   0.4150  0.8199  0.6308  11.00000  0.05    0.11
Q7    1   0.4390  0.8781  0.7500  10.50000  0.05    0.09
Q8    1   0.9437  1.0000  0.0000  10.50000  0.05    0.07
Q9    1   1.0000  1.0973  0.0000  10.50000  0.05    0.07
;
_shelx_res_checksum              45431
####################################################################### 
# 
# 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_2rt
_database_code_depnum_ccdc_archive 'CCDC 2132786'
loop_
_audit_author_name
_audit_author_address
'Dongying Fu'
;Institute of Crystalline Materials, Shanxi University, Taiyuan
China
;
_audit_update_record             
;
2022-01-06 deposited with the CCDC.	2022-03-29 downloaded from the CCDC.
;
_audit_creation_date             2021-11-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C9 H17 F N O'
_chemical_formula_sum            'C9 H17 Br3 F N O Pb'
_chemical_formula_weight         621.16
_chemical_absolute_configuration syn
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C N H F Pb Br'
_chemical_oxdiff_usercomment     \
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'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   7.6940(3)
_cell_length_b                   10.0253(4)
_cell_length_c                   19.4354(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1499.14(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4504
_cell_measurement_temperature    280(1)
_cell_measurement_theta_max      29.9350
_cell_measurement_theta_min      2.8230
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.242
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
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    2.752
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.818
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_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            8772
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.766
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.881
_diffrn_reflns_theta_min         2.286
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      280(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.818
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  35.00   0.50    2.79    --    5.05 -99.00 120.00  102
  2  ω    -18.00  28.00   0.50    2.79    --   -5.21 -99.00  60.00   92
  3  ω    -42.00 -11.00   0.50    2.79    --   -5.21 -57.00 -39.00   62
  4  ω     -7.00  33.00   0.50    2.79    --    5.05 -99.00-134.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0134575000
_diffrn_orient_matrix_UB_12      0.0419853000
_diffrn_orient_matrix_UB_13      0.0289085000
_diffrn_orient_matrix_UB_21      -0.0860604000
_diffrn_orient_matrix_UB_22      0.0247178000
_diffrn_orient_matrix_UB_23      -0.0031945000
_diffrn_orient_matrix_UB_31      -0.0303307000
_diffrn_orient_matrix_UB_32      -0.0512888000
_diffrn_orient_matrix_UB_33      0.0220238000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.643
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.698
_reflns_number_gt                2949
_reflns_number_total             3627
_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 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.911
_refine_diff_density_min         -1.492
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details 
;
 Flack x determined using 1050 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3627
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0282
_refine_ls_restrained_S_all      0.993
_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)+(0.0322P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0636
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C17(H17A,H17B), C11(H11A,
 H11B), C12(H12A,H12B)
2.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_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
Pb1 Pb 0.66498(3) 0.75204(3) 0.00029(2) 0.03459(9) Uani 1 1 d . . . . .
Br3 Br 0.41401(13) 0.72451(9) 0.11998(4) 0.0520(2) Uani 1 1 d . . . . .
Br4 Br 0.92598(12) 0.93218(8) 0.07583(4) 0.0499(2) Uani 1 1 d . . . . .
Br5 Br 0.89093(12) 0.53545(8) 0.04747(5) 0.0505(2) Uani 1 1 d . . . . .
F1 F 0.9477(10) 0.5376(7) 0.2358(4) 0.097(2) Uani 1 1 d . . . . .
C2 C 0.4511(14) 0.7620(10) 0.3827(5) 0.067(3) Uani 1 1 d . . . . .
H2 H 0.334753 0.770790 0.402741 0.080 Uiso 1 1 calc R U . . .
C3 C 0.6456(15) 0.8473(11) 0.2954(5) 0.070(3) Uani 1 1 d . . . . .
H3A H 0.701479 0.932764 0.303170 0.084 Uiso 1 1 calc R U . . .
H3B H 0.643142 0.831504 0.246170 0.084 Uiso 1 1 calc R U . . .
C4 C 0.4675(13) 0.8529(10) 0.3214(6) 0.066(3) Uani 1 1 d . . . . .
H4A H 0.387260 0.825034 0.285647 0.080 Uiso 1 1 calc R U . . .
H4B H 0.438927 0.943577 0.334495 0.080 Uiso 1 1 calc R U . . .
C5 C 0.9597(17) 0.6738(13) 0.2343(6) 0.088(4) Uani 1 1 d . . . . .
H5A H 0.872545 0.709596 0.203313 0.106 Uiso 1 1 calc R U . . .
H5B H 1.073281 0.699809 0.217285 0.106 Uiso 1 1 calc R U . . .
C6 C 0.7612(16) 0.7733(12) 0.4067(7) 0.097(5) Uani 1 1 d . . . . .
H6A H 0.814113 0.699352 0.431172 0.117 Uiso 1 1 calc R U . . .
H6B H 0.832691 0.851802 0.413625 0.117 Uiso 1 1 calc R U . . .
C17 C 0.582(2) 0.7979(12) 0.4339(5) 0.091(4) Uani 1 1 d . . . . .
H17A H 0.563594 0.745586 0.475256 0.109 Uiso 1 1 calc R U . . .
H17B H 0.569131 0.891372 0.445804 0.109 Uiso 1 1 calc R U . . .
N9 N 0.7497(9) 0.7405(7) 0.3292(4) 0.0478(16) Uani 1 1 d . . . . .
C10 C 0.4832(11) 0.6182(9) 0.3627(4) 0.047(2) Uani 1 1 d . . . . .
H10 H 0.486757 0.560697 0.403502 0.056 Uiso 1 1 calc R U . . .
C11 C 0.6540(11) 0.6116(8) 0.3233(5) 0.051(2) Uani 1 1 d . . . . .
H11A H 0.725164 0.539963 0.341524 0.061 Uiso 1 1 calc R U . . .
H11B H 0.630847 0.592596 0.275198 0.061 Uiso 1 1 calc R U . . .
O3 O 0.3534(9) 0.5747(8) 0.3160(4) 0.072(2) Uani 1 1 d . . . . .
H3 H 0.272924 0.540904 0.337439 0.108 Uiso 1 1 calc R U . . .
C12 C 0.9326(13) 0.7299(12) 0.3058(7) 0.080(3) Uani 1 1 d . . . . .
H12A H 0.995096 0.674075 0.338233 0.096 Uiso 1 1 calc R U . . .
H12B H 0.984376 0.818008 0.307563 0.096 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
Pb1 0.02540(13) 0.03772(15) 0.04066(15) -0.00102(14) -0.00122(10) -0.00052(10)
Br3 0.0560(5) 0.0635(6) 0.0366(4) 0.0051(3) 0.0014(4) 0.0055(5)
Br4 0.0446(4) 0.0475(5) 0.0576(5) -0.0191(4) 0.0032(4) 0.0001(4)
Br5 0.0506(5) 0.0397(4) 0.0611(5) 0.0119(4) 0.0018(4) 0.0037(4)
F1 0.117(6) 0.082(5) 0.093(5) -0.008(4) 0.035(4) 0.029(4)
C2 0.072(6) 0.059(6) 0.070(6) -0.016(5) 0.026(5) 0.006(5)
C3 0.099(9) 0.054(7) 0.055(6) 0.018(5) 0.010(6) 0.012(5)
C4 0.066(7) 0.039(6) 0.095(8) 0.004(5) -0.017(6) 0.016(4)
C5 0.083(10) 0.102(10) 0.080(8) 0.040(7) 0.039(7) 0.023(7)
C6 0.098(9) 0.079(8) 0.115(10) -0.045(7) -0.077(9) 0.013(7)
C17 0.153(13) 0.071(7) 0.047(6) -0.006(5) 0.002(8) 0.003(9)
N9 0.036(3) 0.035(4) 0.073(5) 0.000(3) 0.000(3) -0.004(3)
C10 0.051(5) 0.042(5) 0.047(5) -0.001(4) 0.010(4) -0.011(4)
C11 0.044(5) 0.030(4) 0.078(7) -0.007(4) 0.004(4) -0.010(3)
O3 0.056(4) 0.080(6) 0.081(5) -0.003(4) 0.004(4) -0.024(4)
C12 0.054(6) 0.083(8) 0.103(9) 0.026(7) 0.005(6) -0.012(6)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br3 3.0357(9) . ?
Pb1 Br3 3.0316(9) 3_565 ?
Pb1 Br4 2.9968(9) 3_465 ?
Pb1 Br4 3.0739(9) . ?
Pb1 Br5 3.1379(9) 3_465 ?
Pb1 Br5 2.9288(9) . ?
F1 C5 1.369(13) . ?
C2 H2 0.9800 . ?
C2 C4 1.506(15) . ?
C2 C17 1.457(16) . ?
C2 C10 1.514(12) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.461(15) . ?
C3 N9 1.489(12) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C12 1.515(17) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C17 1.500(19) . ?
C6 N9 1.544(14) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
N9 C11 1.492(10) . ?
N9 C12 1.483(12) . ?
C10 H10 0.9800 . ?
C10 C11 1.524(11) . ?
C10 O3 1.418(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
O3 H3 0.8200 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br3 Pb1 Br3 179.153(16) 3_565 . ?
Br3 Pb1 Br4 95.91(2) . . ?
Br3 Pb1 Br4 84.83(2) 3_565 . ?
Br3 Pb1 Br5 98.28(3) 3_565 3_465 ?
Br3 Pb1 Br5 82.01(2) . 3_465 ?
Br4 Pb1 Br3 86.10(3) 3_465 . ?
Br4 Pb1 Br3 93.15(3) 3_465 3_565 ?
Br4 Pb1 Br4 177.04(3) 3_465 . ?
Br4 Pb1 Br5 81.95(2) 3_465 3_465 ?
Br4 Pb1 Br5 100.45(3) . 3_465 ?
Br5 Pb1 Br3 85.62(3) . 3_565 ?
Br5 Pb1 Br3 94.03(3) . . ?
Br5 Pb1 Br4 93.55(3) . 3_465 ?
Br5 Pb1 Br4 84.16(3) . . ?
Br5 Pb1 Br5 174.17(3) . 3_465 ?
Pb1 Br3 Pb1 78.706(19) 3_465 . ?
Pb1 Br4 Pb1 78.641(18) 3_565 . ?
Pb1 Br5 Pb1 78.632(19) . 3_565 ?
C4 C2 H2 109.7 . . ?
C4 C2 C10 111.0(8) . . ?
C17 C2 H2 109.7 . . ?
C17 C2 C4 109.5(9) . . ?
C17 C2 C10 107.4(9) . . ?
C10 C2 H2 109.7 . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C4 C3 N9 112.3(8) . . ?
N9 C3 H3A 109.2 . . ?
N9 C3 H3B 109.2 . . ?
C2 C4 H4A 109.8 . . ?
C2 C4 H4B 109.8 . . ?
C3 C4 C2 109.2(8) . . ?
C3 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
F1 C5 H5A 109.7 . . ?
F1 C5 H5B 109.7 . . ?
F1 C5 C12 109.9(9) . . ?
H5A C5 H5B 108.2 . . ?
C12 C5 H5A 109.7 . . ?
C12 C5 H5B 109.7 . . ?
H6A C6 H6B 108.3 . . ?
C17 C6 H6A 109.9 . . ?
C17 C6 H6B 109.9 . . ?
C17 C6 N9 109.0(8) . . ?
N9 C6 H6A 109.9 . . ?
N9 C6 H6B 109.9 . . ?
C2 C17 C6 110.7(8) . . ?
C2 C17 H17A 109.5 . . ?
C2 C17 H17B 109.5 . . ?
C6 C17 H17A 109.5 . . ?
C6 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
C3 N9 C6 108.0(8) . . ?
C3 N9 C11 108.9(8) . . ?
C11 N9 C6 106.7(8) . . ?
C12 N9 C3 115.3(8) . . ?
C12 N9 C6 105.0(8) . . ?
C12 N9 C11 112.5(7) . . ?
C2 C10 H10 110.9 . . ?
C2 C10 C11 108.1(7) . . ?
C11 C10 H10 110.9 . . ?
O3 C10 C2 110.0(9) . . ?
O3 C10 H10 110.9 . . ?
O3 C10 C11 105.7(6) . . ?
N9 C11 C10 110.4(7) . . ?
N9 C11 H11A 109.6 . . ?
N9 C11 H11B 109.6 . . ?
C10 C11 H11A 109.6 . . ?
C10 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C10 O3 H3 109.5 . . ?
C5 C12 H12A 108.3 . . ?
C5 C12 H12B 108.3 . . ?
N9 C12 C5 116.0(10) . . ?
N9 C12 H12A 108.3 . . ?
N9 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F1 C5 C12 N9 -79.9(12) . . . . ?
C2 C10 C11 N9 11.2(11) . . . . ?
C3 N9 C11 C10 -64.2(10) . . . . ?
C3 N9 C12 C5 -72.0(12) . . . . ?
C4 C2 C17 C6 -64.9(12) . . . . ?
C4 C2 C10 C11 51.1(11) . . . . ?
C4 C2 C10 O3 -63.9(10) . . . . ?
C4 C3 N9 C6 -62.4(12) . . . . ?
C4 C3 N9 C11 53.1(11) . . . . ?
C4 C3 N9 C12 -179.5(9) . . . . ?
C6 N9 C11 C10 52.1(10) . . . . ?
C6 N9 C12 C5 169.3(10) . . . . ?
C17 C2 C4 C3 55.0(12) . . . . ?
C17 C2 C10 C11 -68.5(10) . . . . ?
C17 C2 C10 O3 176.5(8) . . . . ?
C17 C6 N9 C3 51.6(12) . . . . ?
C17 C6 N9 C11 -65.3(11) . . . . ?
C17 C6 N9 C12 175.1(10) . . . . ?
N9 C3 C4 C2 8.8(13) . . . . ?
N9 C6 C17 C2 9.5(14) . . . . ?
C10 C2 C4 C3 -63.3(12) . . . . ?
C10 C2 C17 C6 55.7(12) . . . . ?
C11 N9 C12 C5 53.6(12) . . . . ?
O3 C10 C11 N9 129.0(8) . . . . ?
C12 N9 C11 C10 166.8(8) . . . . ?

_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 2.071
_oxdiff_exptl_absorpt_empirical_full_min 0.665
####################################################################### 
# 
# 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_1ht
_database_code_depnum_ccdc_archive 'CCDC 2132781'
loop_
_audit_author_name
_audit_author_address
'Dongying Fu'
;Institute of Crystalline Materials, Shanxi University, Taiyuan
China
;
_audit_update_record             
;
2022-01-06 deposited with the CCDC.	2022-03-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br3 Pb, C6, 2(C0.50), 2(C)'
_chemical_formula_sum            '	C9 Br3 Pb'
_chemical_formula_weight         555.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_H-M_alt        'P 63 2 2'
_space_group_name_Hall           'P 6c 2c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   10.719(3)
_cell_length_b                   10.719(3)
_cell_length_c                   7.963(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     792.3(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    463
_cell_measurement_reflns_used    466
_cell_measurement_theta_min      3.3360
_cell_measurement_theta_max      28.3290

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.326
_exptl_crystal_F_000             482
_exptl_transmission_factor_min   0.108
_exptl_transmission_factor_max   0.135
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    18.175
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      463(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3501
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.371
_diffrn_reflns_theta_max         31.129
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             719
_reflns_number_gt                143
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.514
_reflns_Friedel_fraction_max     0.780
_reflns_Friedel_fraction_full    1.000

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0300P)²+0.0100P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 30 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(5)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         719
_refine_ls_number_parameters     48
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.1993
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1431
_refine_ls_wR_factor_gt          0.1141
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.009

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 0.24770(17) 0.12385(8) 0.7500 0.3242(8) Uani 1 2 d S T P . .
C1 C 0.2673(12) 0.7423(11) 0.553(2) 0.371(6) Uani 0.1667 1 d D U P . .
C2 C 0.3333 0.6667 0.4544(14) 0.377(4) Uani 0.5 3 d DS TU P . .
C3 C 0.3554(16) 0.5675(12) 0.5734(16) 0.380(5) Uani 0.1667 1 d D U P . .
C4 C 0.3706(8) 0.6294(8) 0.7500 0.389(6) Uani 0.6667 2 d DS TU P . .
C5 C 0.452(5) 0.629(5) 0.596(3) 0.378(5) Uani 0.3333 1 d . U P . .
C6 C 0.2445(18) 0.489(4) 0.7500 0.391(5) Uani 0.6667 2 d S TU P . .
Pb1 Pb 0.0000 0.0000 1.0000 0.2391(4) Uani 1 6 d S T P . .

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 0.2482(12) 0.3619(16) 0.3245(13) -0.015(3) 0.000 0.1241(6)
C1 0.375(8) 0.375(8) 0.359(11) 0.003(9) -0.003(9) 0.185(5)
C2 0.379(5) 0.379(5) 0.374(6) 0.000 0.000 0.189(2)
C3 0.382(6) 0.375(6) 0.378(6) -0.001(6) -0.001(6) 0.186(5)
C4 0.381(5) 0.381(5) 0.380(6) 0.001(5) 0.001(5) 0.172(6)
C5 0.380(6) 0.376(7) 0.375(7) -0.003(7) 0.001(6) 0.187(5)
C6 0.401(8) 0.369(7) 0.392(7) 0.000 0.005(7) 0.184(4)
Pb1 0.2543(5) 0.2543(5) 0.2088(6) 0.000 0.000 0.1271(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 3.0414(14) 4_554 ?
Br1 Pb1 3.0414(14) . ?
C1 C3 0.923(18) 3_565 ?
C1 C5 1.06(5) 2_665 ?
C1 C2 1.534(15) . ?
C1 C3 1.592(16) 2_665 ?
C1 C6 1.602(19) 3_565 ?
C1 C5 1.84(4) 3_565 ?
C1 C4 1.922(16) 2_665 ?
C1 C4 1.953(15) 3_565 ?
C2 C3 1.528(14) 3_565 ?
C2 C3 1.528(14) 2_665 ?
C2 C3 1.528(14) . ?
C2 C1 1.534(15) 3_565 ?
C2 C1 1.534(15) 2_665 ?
C2 C5 1.89(5) 3_565 ?
C2 C5 1.89(5) . ?
C2 C5 1.89(5) 2_665 ?
C3 C5 0.93(4) . ?
C3 C1 0.923(17) 2_665 ?
C3 C4 1.528(13) . ?
C3 C1 1.592(16) 3_565 ?
C3 C6 1.76(2) . ?
C3 C5 1.82(6) 3_565 ?
C4 C4 1.20(3) 3_565 ?
C4 C4 1.20(3) 2_665 ?
C4 C6 1.44(3) . ?
C4 C6 1.44(3) 2_665 ?
C4 C5 1.51(3) 10_666 ?
C4 C5 1.51(3) . ?
C4 C3 1.529(13) 10_666 ?
C4 C1 1.922(16) 3_565 ?
C4 C1 1.922(16) 12_566 ?
C4 C1 1.953(15) 2_665 ?
C4 C1 1.953(15) 11_556 ?
C5 C1 1.06(5) 3_565 ?
C5 C6 1.70(4) 2_665 ?
C5 C3 1.82(6) 2_665 ?
C5 C1 1.84(4) 2_665 ?
C6 C4 1.44(3) 3_565 ?
C6 C1 1.602(19) 12_566 ?
C6 C1 1.602(19) 2_665 ?
C6 C5 1.70(4) 10_666 ?
C6 C5 1.70(4) 3_565 ?
C6 C3 1.76(2) 11_556 ?
Pb1 Br1 3.0414(14) 5 ?
Pb1 Br1 3.0414(14) 2 ?
Pb1 Br1 3.0414(14) 6 ?
Pb1 Br1 3.0414(14) 3 ?
Pb1 Br1 3.0414(14) 4 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Pb1 Br1 Pb1 81.77(5) 4_554 . ?
C3 C1 C5 133(3) 3_565 2_665 ?
C3 C1 C2 72.1(12) 3_565 . ?
C5 C1 C2 91(2) 2_665 . ?
C3 C1 C3 108.3(19) 3_565 2_665 ?
C5 C1 C3 34(2) 2_665 2_665 ?
C2 C1 C3 58.5(8) . 2_665 ?
C3 C1 C6 83.8(15) 3_565 3_565 ?
C5 C1 C6 76.2(17) 2_665 3_565 ?
C2 C1 C6 132.8(16) . 3_565 ?
C3 C1 C6 94.0(13) 2_665 3_565 ?
C3 C1 C5 6.6(19) 3_565 3_565 ?
C5 C1 C5 127(4) 2_665 3_565 ?
C2 C1 C5 67.4(14) . 3_565 ?
C3 C1 C5 101.7(19) 2_665 3_565 ?
C6 C1 C5 84.5(12) 3_565 3_565 ?
C3 C1 C4 84.0(16) 3_565 2_665 ?
C5 C1 C4 51(2) 2_665 2_665 ?
C2 C1 C4 89.7(8) . 2_665 ?
C3 C1 C4 50.5(7) 2_665 2_665 ?
C6 C1 C4 47.0(12) 3_565 2_665 ?
C5 C1 C4 79.7(15) 3_565 2_665 ?
C3 C1 C4 49.7(12) 3_565 3_565 ?
C5 C1 C4 87(2) 2_665 3_565 ?
C2 C1 C4 88.6(7) . 3_565 ?
C3 C1 C4 79.0(11) 2_665 3_565 ?
C6 C1 C4 46.3(12) 3_565 3_565 ?
C5 C1 C4 46.8(10) 3_565 3_565 ?
C4 C1 C4 36.0(9) 2_665 3_565 ?
C3 C2 C3 85.6(9) 3_565 2_665 ?
C3 C2 C3 85.6(9) 3_565 . ?
C3 C2 C3 85.6(9) 2_665 . ?
C3 C2 C1 35.1(7) 3_565 . ?
C3 C2 C1 62.7(7) 2_665 . ?
C3 C2 C1 108.8(10) . . ?
C3 C2 C1 108.8(10) 3_565 3_565 ?
C3 C2 C1 35.1(7) 2_665 3_565 ?
C3 C2 C1 62.7(7) . 3_565 ?
C1 C2 C1 96.0(9) . 3_565 ?
C3 C2 C1 62.7(7) 3_565 2_665 ?
C3 C2 C1 108.8(10) 2_665 2_665 ?
C3 C2 C1 35.1(7) . 2_665 ?
C1 C2 C1 96.0(9) . 2_665 ?
C1 C2 C1 96.0(9) 3_565 2_665 ?
C3 C2 C5 29.1(13) 3_565 3_565 ?
C3 C2 C5 102.1(13) 2_665 3_565 ?
C3 C2 C5 63.6(15) . 3_565 ?
C1 C2 C5 64.0(13) . 3_565 ?
C1 C2 C5 110.2(14) 3_565 3_565 ?
C1 C2 C5 34.3(13) 2_665 3_565 ?
C3 C2 C5 102.1(13) 3_565 . ?
C3 C2 C5 63.6(15) 2_665 . ?
C3 C2 C5 29.1(13) . . ?
C1 C2 C5 110.2(14) . . ?
C1 C2 C5 34.3(13) 3_565 . ?
C1 C2 C5 64.0(13) 2_665 . ?
C5 C2 C5 88.1(17) 3_565 . ?
C3 C2 C5 63.6(15) 3_565 2_665 ?
C3 C2 C5 29.1(13) 2_665 2_665 ?
C3 C2 C5 102.1(13) . 2_665 ?
C1 C2 C5 34.3(13) . 2_665 ?
C1 C2 C5 64.0(13) 3_565 2_665 ?
C1 C2 C5 110.2(14) 2_665 2_665 ?
C5 C2 C5 88.1(17) 3_565 2_665 ?
C5 C2 C5 88.1(17) . 2_665 ?
C5 C3 C1 167(4) . 2_665 ?
C5 C3 C2 97(3) . . ?
C1 C3 C2 72.8(14) 2_665 . ?
C5 C3 C4 71(2) . . ?
C1 C3 C4 102.8(16) 2_665 . ?
C2 C3 C4 106.8(10) . . ?
C5 C3 C1 40(3) . 3_565 ?
C1 C3 C1 128.0(18) 2_665 3_565 ?
C2 C3 C1 58.8(7) . 3_565 ?
C4 C3 C1 76.0(8) . 3_565 ?
C5 C3 C6 115.9(18) . . ?
C1 C3 C6 64.8(14) 2_665 . ?
C2 C3 C6 121.7(12) . . ?
C4 C3 C6 51.1(10) . . ?
C1 C3 C6 126.0(14) 3_565 . ?
C5 C3 C5 143(4) . 3_565 ?
C1 C3 C5 25.2(16) 2_665 3_565 ?
C2 C3 C5 67.8(12) . 3_565 ?
C4 C3 C5 80.7(12) . 3_565 ?
C1 C3 C5 110.7(16) 3_565 3_565 ?
C6 C3 C5 56.6(10) . 3_565 ?
C4 C4 C4 59.999(7) 3_565 2_665 ?
C4 C4 C6 65.3(8) 3_565 . ?
C4 C4 C6 125.3(8) 2_665 . ?
C4 C4 C6 125.3(8) 3_565 2_665 ?
C4 C4 C6 65.3(8) 2_665 2_665 ?
C6 C4 C6 169.3(16) . 2_665 ?
C4 C4 C5 106.9(19) 3_565 10_666 ?
C4 C4 C5 125.5(17) 2_665 10_666 ?
C6 C4 C5 70.4(15) . 10_666 ?
C6 C4 C5 104.0(16) 2_665 10_666 ?
C4 C4 C5 125.5(17) 3_565 . ?
C4 C4 C5 106.9(19) 2_665 . ?
C6 C4 C5 104.0(16) . . ?
C6 C4 C5 70.4(15) 2_665 . ?
C5 C4 C5 120(4) 10_666 . ?
C4 C4 C3 96.4(8) 3_565 . ?
C4 C4 C3 112.4(6) 2_665 . ?
C6 C4 C3 72.8(5) . . ?
C6 C4 C3 104.1(6) 2_665 . ?
C5 C4 C3 121.9(18) 10_666 . ?
C5 C4 C3 35.5(15) . . ?
C4 C4 C3 112.4(6) 3_565 10_666 ?
C4 C4 C3 96.4(8) 2_665 10_666 ?
C6 C4 C3 104.0(6) . 10_666 ?
C6 C4 C3 72.8(5) 2_665 10_666 ?
C5 C4 C3 35.5(15) 10_666 10_666 ?
C5 C4 C3 121.9(18) . 10_666 ?
C3 C4 C3 147.0(15) . 10_666 ?
C4 C4 C1 107.1(5) 3_565 3_565 ?
C4 C4 C1 73.4(5) 2_665 3_565 ?
C6 C4 C1 125.2(4) . 3_565 ?
C6 C4 C1 54.7(4) 2_665 3_565 ?
C5 C4 C1 146(2) 10_666 3_565 ?
C5 C4 C1 33.5(19) . 3_565 ?
C3 C4 C1 53.5(6) . 3_565 ?
C3 C4 C1 126.3(7) 10_666 3_565 ?
C4 C4 C1 73.4(5) 3_565 12_566 ?
C4 C4 C1 107.1(5) 2_665 12_566 ?
C6 C4 C1 54.7(4) . 12_566 ?
C6 C4 C1 125.2(4) 2_665 12_566 ?
C5 C4 C1 33.5(19) 10_666 12_566 ?
C5 C4 C1 146(2) . 12_566 ?
C3 C4 C1 126.3(7) . 12_566 ?
C3 C4 C1 53.5(6) 10_666 12_566 ?
C1 C4 C1 179.4(11) 3_565 12_566 ?
C4 C4 C1 70.6(5) 3_565 2_665 ?
C4 C4 C1 105.3(6) 2_665 2_665 ?
C6 C4 C1 53.8(4) . 2_665 ?
C6 C4 C1 126.7(4) 2_665 2_665 ?
C5 C4 C1 120.0(15) 10_666 2_665 ?
C5 C4 C1 62.6(15) . 2_665 ?
C3 C4 C1 27.4(7) . 2_665 ?
C3 C4 C1 155.5(9) 10_666 2_665 ?
C1 C4 C1 72.1(8) 3_565 2_665 ?
C1 C4 C1 107.9(8) 12_566 2_665 ?
C4 C4 C1 105.3(6) 3_565 11_556 ?
C4 C4 C1 70.6(5) 2_665 11_556 ?
C6 C4 C1 126.7(4) . 11_556 ?
C6 C4 C1 53.8(4) 2_665 11_556 ?
C5 C4 C1 62.6(15) 10_666 11_556 ?
C5 C4 C1 120.0(15) . 11_556 ?
C3 C4 C1 155.5(9) . 11_556 ?
C3 C4 C1 27.4(7) 10_666 11_556 ?
C1 C4 C1 107.9(8) 3_565 11_556 ?
C1 C4 C1 72.1(8) 12_566 11_556 ?
C1 C4 C1 175.4(11) 2_665 11_556 ?
C3 C5 C1 106(5) . 3_565 ?
C3 C5 C4 73(3) . . ?
C1 C5 C4 95(4) 3_565 . ?
C3 C5 C6 123(4) . 2_665 ?
C1 C5 C6 66(2) 3_565 2_665 ?
C4 C5 C6 52.7(15) . 2_665 ?
C3 C5 C3 92(4) . 2_665 ?
C1 C5 C3 21.7(17) 3_565 2_665 ?
C4 C5 C3 75(2) . 2_665 ?
C6 C5 C3 59.8(17) 2_665 2_665 ?
C3 C5 C1 7(2) . 2_665 ?
C1 C5 C1 100(3) 3_565 2_665 ?
C4 C5 C1 70.6(18) . 2_665 ?
C6 C5 C1 118(3) 2_665 2_665 ?
C3 C5 C1 86(2) 2_665 2_665 ?
C3 C5 C2 53(2) . . ?
C1 C5 C2 54(2) 3_565 . ?
C4 C5 C2 92(3) . . ?
C6 C5 C2 106(3) 2_665 . ?
C3 C5 C2 48.6(14) 2_665 . ?
C1 C5 C2 48.6(12) 2_665 . ?
C4 C6 C4 49.3(16) . 3_565 ?
C4 C6 C1 78.3(12) . 12_566 ?
C4 C6 C1 79.8(12) 3_565 12_566 ?
C4 C6 C1 79.8(12) . 2_665 ?
C4 C6 C1 78.3(12) 3_565 2_665 ?
C1 C6 C1 156(3) 12_566 2_665 ?
C4 C6 C5 56.8(15) . 10_666 ?
C4 C6 C5 88(2) 3_565 10_666 ?
C1 C6 C5 37.5(14) 12_566 10_666 ?
C1 C6 C5 131.3(18) 2_665 10_666 ?
C4 C6 C5 88(2) . 3_565 ?
C4 C6 C5 56.8(15) 3_565 3_565 ?
C1 C6 C5 131.2(18) 12_566 3_565 ?
C1 C6 C5 37.5(14) 2_665 3_565 ?
C5 C6 C5 142(4) 10_666 3_565 ?
C4 C6 C3 56.0(9) . . ?
C4 C6 C3 78.8(14) 3_565 . ?
C1 C6 C3 132.9(18) 12_566 . ?
C1 C6 C3 31.4(6) 2_665 . ?
C5 C6 C3 100.3(16) 10_666 . ?
C5 C6 C3 63.6(18) 3_565 . ?
C4 C6 C3 78.8(14) . 11_556 ?
C4 C6 C3 56.0(9) 3_565 11_556 ?
C1 C6 C3 31.4(6) 12_566 11_556 ?
C1 C6 C3 132.9(18) 2_665 11_556 ?
C5 C6 C3 63.6(18) 10_666 11_556 ?
C5 C6 C3 100.2(16) 3_565 11_556 ?
C3 C6 C3 131(2) . 11_556 ?
Br1 Pb1 Br1 180.0 5 2 ?
Br1 Pb1 Br1 98.20(4) 5 . ?
Br1 Pb1 Br1 81.80(4) 2 . ?
Br1 Pb1 Br1 81.80(4) 5 6 ?
Br1 Pb1 Br1 98.20(4) 2 6 ?
Br1 Pb1 Br1 98.20(4) . 6 ?
Br1 Pb1 Br1 98.20(4) 5 3 ?
Br1 Pb1 Br1 81.80(4) 2 3 ?
Br1 Pb1 Br1 81.80(4) . 3 ?
Br1 Pb1 Br1 180.0 6 3 ?
Br1 Pb1 Br1 81.80(4) 5 4 ?
Br1 Pb1 Br1 98.20(4) 2 4 ?
Br1 Pb1 Br1 180.0 . 4 ?
Br1 Pb1 Br1 81.80(4) 6 4 ?
Br1 Pb1 Br1 98.20(4) 3 4 ?

_refine_diff_density_max         0.303
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.096

# start Validation Reply Form
_vrf_PLAT260_P6322               
;
PROBLEM: Large Average Ueq of Residue Including        C4      0.390 Check 
RESPONSE: This is caused by the severely disordered organic cations.
;
# end Validation Reply Form

_shelx_res_file                  
;

    P6322.res created by SHELXL-2014/7


TITL P6322 in P6(3)22
CELL 0.71073  10.7188  10.7188   7.9632  90.000  90.000 120.000
ZERR   2.00   0.0032   0.0032   0.0035   0.000   0.000   0.000
LATT -1
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SYMM -X, -Y, 0.5+Z
SYMM Y, -X+Y, 0.5+Z
SYMM X-Y, X, 0.5+Z
SYMM Y, X, -Z
SYMM X-Y, -Y, -Z
SYMM -X, -X+Y, -Z
SYMM -Y, -X, 0.5-Z
SYMM -X+Y, Y, 0.5-Z
SYMM X, X-Y, 0.5-Z
SFAC Br C  N  Pb O
UNIT 6 18 0 2 0
L.S. 52
ACTA
BOND
FMAP 2
PLAN 4
MORE -1
ISOR 0.02 C1 C2 C3 C4 C5 C6
DELU 0.02 C1 C2 C3 C4 C5 C6
SIMU 0.02 C1 C2 C3 C4 C5 C6
DFIX 2.56 0.02 C1 C4
DFIX 2.49 0.02  C4 C2 C1 C3
DFIX 1.53 0.02 C1 C2 C2 C3 C3 C4
TEMP 190
WGHT    0.030000    0.010000
FVAR       0.60643
BR1   1    0.247698    0.123849    0.750000    10.50000    0.24823    0.36189 =
         0.32452   -0.01455    0.00000    0.12412
C1    2    0.267252    0.742289    0.553334    10.16667    0.37483    0.37471 =
         0.35924    0.00321   -0.00309    0.18495
C2    2    0.333333    0.666667    0.454404    10.16667    0.37855    0.37855 =
         0.37434    0.00000    0.00000    0.18928
C3    2    0.355414    0.567501    0.573411    10.16667    0.38240    0.37520 =
         0.37816   -0.00053   -0.00051    0.18609
C4    2    0.370593    0.629407    0.750000    10.33333    0.38111    0.38111 =
         0.38016    0.00093    0.00093    0.17200
C5    2    0.452204    0.629232    0.595644    10.33333    0.37965    0.37573 =
         0.37516   -0.00267    0.00141    0.18711
C6    2    0.244466    0.488931    0.750000    10.33333    0.40136    0.36855 =
         0.39214    0.00000    0.00479    0.18428
PB1   4    0.000000    0.000000    1.000000    10.16667    0.25426    0.25426 =
         0.20876    0.00000    0.00000    0.12713
HKLF 4

REM  P6322 in P6(3)22
REM R1 =  0.0532 for     143 Fo > 4sig(Fo)  and  0.1993 for all     719 data
REM     48 parameters refined using    103 restraints

END

WGHT      0.1177      0.0000

REM Highest difference peak  0.303,  deepest hole -0.244,  1-sigma level  0.096
Q1    1   0.4376  0.5624  0.7500  10.50000  0.05    0.30
Q2    1   0.0000  0.0000  1.2500  10.16667  0.05    0.30
Q3    1   0.2916  0.7084  0.4953  11.00000  0.05    0.21
Q4    1   0.3681  0.6279  0.5164  11.00000  0.05    0.19
;
_shelx_res_checksum              14463
