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

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

data_hy
_database_code_depnum_ccdc_archive 'CCDC 2249681'
loop_
_audit_author_name
_audit_author_address
C
;Zhengzhou University
China
;
_audit_update_record             
;
2023-03-18 deposited with the CCDC.	2023-05-30 downloaded from the CCDC.
;
_audit_creation_date             2023-03-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        (C3H10N)3PbBr5
_chemical_formula_moiety         'Br5 Pb, 3(C3 H10 N)'
_chemical_formula_sum            'C9 H30 Br5 N3 Pb'
_chemical_formula_weight         787.10
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_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'
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      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, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   8.6172(3)
_cell_length_b                   11.8062(5)
_cell_length_c                   21.5472(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2192.13(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4980
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      28.7000
_cell_measurement_theta_min      2.7730
_shelx_estimated_absorpt_T_max   0.730
_shelx_estimated_absorpt_T_min   0.633
_exptl_absorpt_coefficient_mu    16.802
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.385
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1448
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12421
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.874
_diffrn_reflns_theta_min         1.890
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     17.00  97.00   0.50    0.80    --    7.30  82.00-120.00  160
  2  ω    -12.00  84.00   0.50    0.80    --    7.30  57.00-150.00  192
  3  ω    -27.00  -2.00   0.50    0.80    --    7.30  82.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0020363000
_diffrn_orient_matrix_UB_12      0.0471881000
_diffrn_orient_matrix_UB_13      0.0203705000
_diffrn_orient_matrix_UB_21      -0.0236409000
_diffrn_orient_matrix_UB_22      -0.0352364000
_diffrn_orient_matrix_UB_23      0.0249087000
_diffrn_orient_matrix_UB_31      0.0788415000
_diffrn_orient_matrix_UB_32      -0.0117814000
_diffrn_orient_matrix_UB_33      0.0069543000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.664
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.772
_reflns_number_gt                4294
_reflns_number_total             4853
_reflns_odcompleteness_completeness 99.88
_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 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.349
_refine_diff_density_min         -2.151
_refine_diff_density_rms         0.553
_refine_ls_abs_structure_details 
;
 Flack x determined using 1567 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4853
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0353
_refine_ls_restrained_S_all      1.163
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0640P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.1142
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups, All N(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 N3-C9A = N3-C9B = N2-C5 = N1-C2
 1.48 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C9B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: H8BD(0.5) H8BE(0.5) H8BF(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5)
 H3BD(0.5) H3BE(0.5) H3BF(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) H7AA(0.5)
 H7AB(0.5) H7AC(0.5) H7BE(0.5) H7BF(0.5) H7BD(0.5) C9B(0.5) H9B(0.5) C9A(0.5)
 H9A(0.5)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C9B(H9B), C9A(H9A)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C8(H8BD,H8BE,H8BF), C8(H8AA,H8AB,H8AC), N1(H1A,H1B,H1C),
 C4(H4A,H4B,H4C), C1(H1D,H1E,H1F), N3(H3BD,H3BE,H3BF), N3(H3AA,H3AB,H3AC),
 C7(H7AA,H7AB,H7AC), C7(H7BE,H7BF,H7BD), C6(H6A,H6B,H6C), N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.48834(5) 0.66329(4) 0.41423(2) 0.02207(15) Uani 1 1 d . . . . .
Br5 Br 0.77749(16) 0.57590(13) 0.34827(7) 0.0303(3) Uani 1 1 d . . . . .
Br3 Br 0.22957(16) 0.77710(12) 0.48391(6) 0.0299(3) Uani 1 1 d . . . . .
Br2 Br 0.41872(17) 0.46498(12) 0.49152(8) 0.0357(4) Uani 1 1 d . . . . .
Br4 Br 0.5440(2) 0.90644(14) 0.36497(8) 0.0401(4) Uani 1 1 d . . . . .
Br1 Br 0.2559(2) 0.58236(18) 0.32669(8) 0.0484(5) Uani 1 1 d . . . . .
C3 C 0.0278(15) 0.5190(10) 0.4737(6) 0.022(3) Uani 1 1 d . . . . .
H3A H 0.136083 0.532349 0.461879 0.033 Uiso 1 1 calc GR . . . .
H3B H 0.004838 0.559695 0.512246 0.033 Uiso 1 1 calc GR . . . .
H3C H -0.040877 0.546115 0.440645 0.033 Uiso 1 1 calc GR . . . .
C8 C 0.9351(16) 0.8513(12) 0.3793(6) 0.025(3) Uani 1 1 d . . . . .
H8BD H 0.827170 0.861825 0.366203 0.037 Uiso 0.5 1 calc GR . P A 2
H8BE H 0.951816 0.889299 0.419162 0.037 Uiso 0.5 1 calc GR . P A 2
H8BF H 0.956753 0.770176 0.383777 0.037 Uiso 0.5 1 calc GR . P A 2
H8AA H 0.894247 0.777039 0.367136 0.037 Uiso 0.5 1 calc GR . P B 1
H8AB H 0.860593 0.889122 0.406677 0.037 Uiso 0.5 1 calc GR . P B 1
H8AC H 1.033819 0.841284 0.401216 0.037 Uiso 0.5 1 calc GR . P B 1
N1 N 0.039(2) 0.3315(13) 0.4246(7) 0.069(5) Uani 1 1 d D . . . .
H1A H -0.039606 0.341598 0.396987 0.083 Uiso 1 1 calc GR . . . .
H1B H 0.050620 0.256277 0.432608 0.083 Uiso 1 1 calc GR . . . .
H1C H 0.128709 0.359426 0.408384 0.083 Uiso 1 1 calc GR . . . .
C4 C 0.4696(18) 0.8920(13) 0.2135(7) 0.034(4) Uani 1 1 d . . . . .
H4A H 0.497786 0.878671 0.256949 0.051 Uiso 1 1 calc GR . . . .
H4B H 0.362265 0.919147 0.211266 0.051 Uiso 1 1 calc GR . . . .
H4C H 0.539170 0.948936 0.195630 0.051 Uiso 1 1 calc GR . . . .
C1 C -0.161(2) 0.3762(15) 0.5080(10) 0.051(5) Uani 1 1 d . . . . .
H1D H -0.167727 0.406817 0.550150 0.077 Uiso 1 1 calc GR . . . .
H1E H -0.185654 0.295193 0.508628 0.077 Uiso 1 1 calc GR . . . .
H1F H -0.234378 0.415889 0.481005 0.077 Uiso 1 1 calc GR . . . .
C2 C 0.002(2) 0.3925(10) 0.4835(6) 0.035(3) Uani 1 1 d D . . . .
H2 H 0.076241 0.366131 0.516129 0.042 Uiso 1 1 calc R . . . .
N3 N 1.008(3) 0.8469(16) 0.2713(8) 0.087(6) Uani 1 1 d D U . . .
H3BD H 1.091382 0.853895 0.245883 0.105 Uiso 0.5 1 calc GR . P C 2
H3BE H 0.924140 0.881152 0.253618 0.105 Uiso 0.5 1 calc GR . P C 2
H3BF H 0.986582 0.772154 0.277407 0.105 Uiso 0.5 1 calc GR . P C 2
H3AA H 1.018034 0.887901 0.235837 0.105 Uiso 0.5 1 calc GR . P D 1
H3AB H 0.934153 0.792477 0.265792 0.105 Uiso 0.5 1 calc GR . P D 1
H3AC H 1.099936 0.813597 0.280847 0.105 Uiso 0.5 1 calc GR . P D 1
C7 C 1.044(3) 1.0221(18) 0.3334(10) 0.083(8) Uani 1 1 d . . . . .
H7AA H 0.994240 1.064429 0.367207 0.124 Uiso 0.5 1 calc GR . P E 1
H7AB H 1.044496 1.068551 0.295743 0.124 Uiso 0.5 1 calc GR . P E 1
H7AC H 1.150576 1.003345 0.345139 0.124 Uiso 0.5 1 calc GR . P E 1
H7BE H 1.046471 1.052093 0.291046 0.124 Uiso 0.5 1 calc GR . P F 2
H7BF H 1.135911 1.047727 0.356092 0.124 Uiso 0.5 1 calc GR . P F 2
H7BD H 0.950253 1.049539 0.354556 0.124 Uiso 0.5 1 calc GR . P F 2
C6 C 0.624(2) 0.7133(19) 0.1931(10) 0.069(6) Uani 1 1 d . U . . .
H6A H 0.718707 0.751979 0.180082 0.104 Uiso 1 1 calc GR . . . .
H6B H 0.613150 0.641888 0.170310 0.104 Uiso 1 1 calc GR . . . .
H6C H 0.628549 0.697532 0.237755 0.104 Uiso 1 1 calc GR . . . .
C5 C 0.483(3) 0.789(2) 0.1795(14) 0.099(8) Uani 1 1 d D U . . .
H5 H 0.519538 0.821415 0.139191 0.119 Uiso 1 1 calc R . . . .
N2 N 0.337(3) 0.741(2) 0.1582(14) 0.136(10) Uani 1 1 d D U . . .
H2A H 0.354165 0.695170 0.125011 0.163 Uiso 1 1 calc GR . . . .
H2B H 0.271381 0.798126 0.146873 0.163 Uiso 1 1 calc GR . . . .
H2C H 0.292586 0.700211 0.189371 0.163 Uiso 1 1 calc GR . . . .
C9B C 1.042(4) 0.901(3) 0.3315(11) 0.035(8) Uani 0.5 1 d D U P G 2
H9B H 1.148576 0.875912 0.343135 0.042 Uiso 0.5 1 calc R . P G 2
C9A C 0.961(4) 0.922(2) 0.3224(10) 0.030(7) Uani 0.5 1 d D . P G 1
H9A H 0.854501 0.948620 0.310487 0.036 Uiso 0.5 1 calc R . P G 1


_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 Br5 3.0485(15) . ?
Pb1 Br3 3.1037(14) 4_566 ?
Pb1 Br3 3.0054(14) . ?
Pb1 Br2 2.9352(16) . ?
Pb1 Br4 3.0979(17) . ?
Pb1 Br1 2.9124(17) . ?
C9Bb H9B 1.0000 . ?
C9Aa H9A 1.0000 . ?
Br3 Pb1 3.1037(14) 4_466 ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C3 C2 1.524(17) . ?
C8 H8BD 0.9800 . ?
C8 H8BE 0.9800 . ?
C8 H8BF 0.9800 . ?
C8 H8AA 0.9800 . ?
C8 H8AB 0.9800 . ?
C8 H8AC 0.9800 . ?
C8 C9B 1.50(4) . ?
C8 C9A 1.50(3) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C2 1.494(11) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4 C5 1.42(3) . ?
C1 H1D 0.9800 . ?
C1 H1E 0.9800 . ?
C1 H1F 0.9800 . ?
C1 C2 1.51(2) . ?
C2 H2 1.0000 . ?
N3 H3BD 0.9100 . ?
N3 H3BE 0.9100 . ?
N3 H3BF 0.9100 . ?
N3 H3AA 0.9100 . ?
N3 H3AB 0.9100 . ?
N3 H3AC 0.9100 . ?
N3 C9B 1.473(13) . ?
N3 C9A 1.471(13) . ?
C7 H7AA 0.9800 . ?
C7 H7AB 0.9800 . ?
C7 H7AC 0.9800 . ?
C7 H7BE 0.9800 . ?
C7 H7BF 0.9800 . ?
C7 H7BD 0.9800 . ?
C7 C9B 1.43(4) . ?
C7 C9A 1.40(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 C5 1.53(3) . ?
C5 H5 1.0000 . ?
C5 N2 1.460(12) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?

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
Br5 Pb1 Br3 81.89(4) . 4_566 ?
Br5 Pb1 Br4 91.56(5) . . ?
Br3 Pb1 Br5 172.18(4) . . ?
Br3 Pb1 Br3 92.422(15) . 4_566 ?
Br3 Pb1 Br4 82.63(4) . . ?
Br2 Pb1 Br5 99.30(4) . . ?
Br2 Pb1 Br3 85.50(4) . . ?
Br2 Pb1 Br3 85.21(4) . 4_566 ?
Br2 Pb1 Br4 164.84(5) . . ?
C9Bb C8 H8BD 109.5 . . ?
C9Bb C8 H8BE 109.5 . . ?
H8BDb C8 H8BE 109.5 . . ?
C9Bb C8 H8BF 109.5 . . ?
H8BDb C8 H8BF 109.5 . . ?
H8BEb C8 H8BF 109.5 . . ?
C9Aa C8 H8AA 109.5 . . ?
H8AAa C8 H8AB 109.5 . . ?
C9Aa C8 H8AB 109.5 . . ?
H8ABa C8 H8AC 109.5 . . ?
H8AAa C8 H8AC 109.5 . . ?
C9Aa C8 H8AC 109.5 . . ?
C9Bb N3 H3BD 109.5 . . ?
C9Bb N3 H3BE 109.5 . . ?
Br4 Pb1 Br3 85.90(4) . 4_566 ?
Br1 Pb1 Br5 98.58(5) . . ?
Br1 Pb1 Br3 173.19(5) . 4_566 ?
Br1 Pb1 Br3 87.71(5) . . ?
Br1 Pb1 Br2 88.01(5) . . ?
Br1 Pb1 Br4 100.87(5) . . ?
Pb1 Br3 Pb1 162.10(5) . 4_466 ?
H3BDb N3 H3BE 109.5 . . ?
C9Bb N3 H3BF 109.5 . . ?
H3BEb N3 H3BF 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3BDb N3 H3BF 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C9Aa N3 H3AA 109.5 . . ?
C9Aa N3 H3AB 109.5 . . ?
H3AAa N3 H3AB 109.5 . . ?
C9Aa N3 H3AC 109.5 . . ?
H3ABa N3 H3AC 109.5 . . ?
H3AAa N3 H3AC 109.5 . . ?
C9Aa C7 H7AA 109.5 . . ?
H7AAa C7 H7AB 109.5 . . ?
C9Aa C7 H7AB 109.5 . . ?
C9Aa C7 H7AC 109.5 . . ?
H7AAa C7 H7AC 109.5 . . ?
H7ABa C7 H7AC 109.5 . . ?
C9Bb C7 H7BE 109.5 . . ?
H7BEb C7 H7BF 109.5 . . ?
C9Bb C7 H7BF 109.5 . . ?
H7BEb C7 H7BD 109.5 . . ?
C9Bb C7 H7BD 109.5 . . ?
H7BFb C7 H7BD 109.5 . . ?
C8 C9Bb H9B 106.0 . . ?
C8 C9Aa H9A 104.4 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H1D C1 H1E 109.5 . . ?
H1D C1 H1F 109.5 . . ?
H1E C1 H1F 109.5 . . ?
C2 C1 H1D 109.5 . . ?
C2 C1 H1E 109.5 . . ?
C2 C1 H1F 109.5 . . ?
C3 C2 H2 108.0 . . ?
N1 C2 C3 108.8(11) . . ?
N1 C2 C1 115.7(15) . . ?
N1 C2 H2 108.0 . . ?
C1 C2 C3 108.0(12) . . ?
C1 C2 H2 108.0 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
C4 C5 C6 117.8(18) . . ?
C4 C5 H5 98.3 . . ?
C4 C5 N2 115(2) . . ?
N3 C9Bb C8 108(2) . . ?
N3 C9Aa C8 108.3(19) . . ?
N3 C9Bb H9B 106.0 . . ?
N3 C9Aa H9A 104.4 . . ?
C7 C9Aa C8 114.0(19) . . ?
C7 C9Bb C8 112(2) . . ?
C7 C9Aa N3 120(2) . . ?
C7 C9Bb N3 117(3) . . ?
C7 C9Bb H9B 106.0 . . ?
C7 C9Aa H9A 104.4 . . ?
C6 C5 H5 98.3 . . ?
N2 C5 C6 121(2) . . ?
N2 C5 H5 98.3 . . ?
C5 N2 H2A 109.5 . . ?
C5 N2 H2B 109.5 . . ?
C5 N2 H2C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?

_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 3.663
_oxdiff_exptl_absorpt_empirical_full_min 0.684
####################################################################### 
# 
# 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_hy_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2249682'
loop_
_audit_author_name
_audit_author_address
RF
;Zhengzhou University
China
;
_audit_update_record             
;
2023-03-18 deposited with the CCDC.	2023-05-30 downloaded from the CCDC.
;
_audit_creation_date             2023-03-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H7 F3 N)'
_chemical_formula_sum            'C6 H14 Br4 F6 N2 Pb'
_chemical_formula_weight         755.02
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 '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           18
_space_group_name_H-M_alt        'P 2 21 21'
_space_group_name_Hall           'P 2bc 2'
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                   7.9087(2)
_cell_length_b                   8.9042(3)
_cell_length_c                   24.2405(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1707.03(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3869
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      73.3180
_cell_measurement_theta_min      3.6220
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    30.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.938
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            7425
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.784
_diffrn_reflns_theta_min         3.647
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -89.00  29.00   0.50    0.50    --    0.00 -38.00  60.00  236
  2  ω     84.00 181.00   0.50    0.50    --   98.80  45.00-180.00  194
  3  ω     10.00  43.00   0.50    0.50    --   98.80 -82.00-120.00   66
  4  ω     79.00 116.00   0.50    0.50    --   98.80  45.00  60.00   74
  5  ω    156.00 181.00   0.50    0.50    --   98.80  45.00  60.00   50
  6  ω     76.00 188.00   0.50    0.50    --   98.80  45.00 150.00  224
  7  ω     48.00 100.00   0.50    0.50    --   98.80 -61.00-120.00  104
  8  ω     46.00 129.00   0.50    0.50    --   98.80 -82.00-120.00  166
  9  ω     69.00 136.00   0.50    0.50    --   98.80 -82.00 -60.00  134
 10  ω      9.00  42.00   0.50    0.50    --   98.80 -61.00-120.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0517166000
_diffrn_orient_matrix_UB_12      0.0258416000
_diffrn_orient_matrix_UB_13      -0.1093793000
_diffrn_orient_matrix_UB_21      0.0365941000
_diffrn_orient_matrix_UB_22      0.0576008000
_diffrn_orient_matrix_UB_23      -0.1452909000
_diffrn_orient_matrix_UB_31      0.0048666000
_diffrn_orient_matrix_UB_32      -0.1611744000
_diffrn_orient_matrix_UB_33      -0.0696384000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.679
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                2961
_reflns_number_total             3291
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.925
_refine_diff_density_min         -2.624
_refine_diff_density_rms         0.406
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3291
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0592
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1044P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1587
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C9(H9)
2.b Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c), N3(H3a,H3b,H3c), C13(H13a,H13b,H13c), C15(H15a,H15b,H15c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.25610(6) 0.84172(6) 0.25099(3) 0.0226(3) Uani 1 1 d . . . . .
Br2 Br 0.42316(18) 1.16627(19) 0.24991(8) 0.0310(4) Uani 1 1 d . . . . .
Br3 Br 0.2155(2) 0.8762(2) 0.37398(9) 0.0297(5) Uani 1 1 d . . . . .
Br4 Br 0.2333(2) 0.84798(18) 0.12973(8) 0.0289(4) Uani 1 1 d . . . . .
Br5 Br 0.05308(18) 0.5590(2) 0.25198(9) 0.0332(4) Uani 1 1 d . . . . .
N1 N 0.1701(18) 1.2137(16) 0.1382(6) 0.032(3) Uani 1 1 d . . . . .
H1A H 0.068077 1.235228 0.124916 0.039 Uiso 1 1 calc GR . . . .
H1B H 0.176931 1.244423 0.173103 0.039 Uiso 1 1 calc GR . . . .
H1C H 0.186802 1.114892 0.136765 0.039 Uiso 1 1 calc GR . . . .
F2 F 0.3510(13) 1.5038(12) 0.3548(4) 0.037(2) Uani 1 1 d . . . . .
N3 N 0.1692(16) 1.2397(17) 0.3585(6) 0.027(3) Uani 1 1 d . . . . .
H3A H 0.194896 1.292661 0.328485 0.032 Uiso 1 1 calc GR . . . .
H3B H 0.061627 1.255790 0.367481 0.032 Uiso 1 1 calc GR . . . .
H3C H 0.184648 1.142424 0.351681 0.032 Uiso 1 1 calc GR . . . .
F4 F 0.4039(13) 1.5058(14) 0.4419(5) 0.046(3) Uani 1 1 d . . . . .
C5 C 0.2811(19) 1.287(2) 0.4052(7) 0.026(3) Uani 1 1 d . . . . .
H5 H 0.393661 1.243223 0.400295 0.031 Uiso 1 1 calc R . . . .
F6 F 0.239(2) 1.1310(14) 0.0305(6) 0.069(4) Uani 1 1 d . . . . .
F7 F 0.1305(14) 1.3535(16) 0.0288(5) 0.056(4) Uani 1 1 d . . . . .
C8 C 0.267(2) 1.273(2) 0.0434(8) 0.032(4) Uani 1 1 d . . . . .
C9 C 0.304(2) 1.2929(19) 0.1040(7) 0.026(4) Uani 1 1 d . . . . .
H9 H 0.412671 1.244339 0.111693 0.031 Uiso 1 1 calc R . . . .
F10 F 0.3967(15) 1.3195(18) 0.0136(5) 0.060(4) Uani 1 1 d . . . . .
F12 F 0.1455(13) 1.5221(12) 0.4143(6) 0.048(3) Uani 1 1 d . . . . .
C13 C 0.206(3) 1.233(2) 0.4593(9) 0.048(5) Uani 1 1 d . . . . .
H13A H 0.096859 1.277208 0.464477 0.072 Uiso 1 1 calc GR . . . .
H13B H 0.279231 1.261834 0.489179 0.072 Uiso 1 1 calc GR . . . .
H13C H 0.195941 1.125582 0.458535 0.072 Uiso 1 1 calc GR . . . .
C15 C 0.319(2) 1.456(2) 0.1209(10) 0.046(5) Uani 1 1 d . . . . .
H15A H 0.237311 1.514463 0.101068 0.068 Uiso 1 1 calc GR . . . .
H15B H 0.430687 1.491549 0.112518 0.068 Uiso 1 1 calc GR . . . .
H15C H 0.298791 1.464876 0.159790 0.068 Uiso 1 1 calc GR . . . .
C17 C 0.295(2) 1.457(2) 0.4046(8) 0.036(4) Uani 1 1 d . . . . .


_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 3.1776(17) . ?
Pb1 Br2 2.9793(15) 4_645 ?
Pb1 Br3 3.014(2) . ?
Pb1 Br4 2.945(2) . ?
Pb1 Br5 3.1186(15) 4 ?
Pb1 Br5 2.9862(17) . ?
Br2 Pb1 2.9792(15) 4_655 ?
Br5 Pb1 3.1187(15) 4_545 ?
N1 C9 1.52(2) . ?
F2 C17 1.35(2) . ?
N3 C5 1.50(2) . ?
F4 C17 1.32(2) . ?
C5 C13 1.52(3) . ?
C5 C17 1.52(3) . ?
F6 C8 1.32(2) . ?
F7 C8 1.35(2) . ?
C8 C9 1.51(2) . ?
C8 F10 1.32(2) . ?
C9 C15 1.51(3) . ?
F12 C17 1.34(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br2 97.05(2) 4_645 . ?
Br2 Pb1 Br3 98.70(5) 4_645 . ?
Br2 Pb1 Br5 90.90(5) 4_645 . ?
Br2 Pb1 Br5 173.06(5) 4_645 4 ?
Br3 Pb1 Br2 87.70(5) . . ?
Br3 Pb1 Br5 82.89(6) . 4 ?
Br4 Pb1 Br2 93.14(5) . 4_645 ?
Br4 Pb1 Br2 90.00(5) . . ?
Br4 Pb1 Br3 168.13(6) . . ?
Br4 Pb1 Br5 89.48(5) . . ?
Br4 Pb1 Br5 85.25(6) . 4 ?
Br5 Pb1 Br2 172.05(5) . . ?
Br5 Pb1 Br2 76.22(4) 4 . ?
Br5 Pb1 Br3 91.18(6) . . ?
Br5 Pb1 Br5 95.830(16) . 4 ?
Pb1 Br2 Pb1 146.20(6) 4_655 . ?
Pb1 Br5 Pb1 160.79(7) . 4_545 ?
N3 C5 C13 109.5(14) . . ?
N3 C5 C17 108.5(14) . . ?
C17 C5 C13 110.7(15) . . ?
F6 C8 F7 108.2(17) . . ?
F6 C8 C9 112.1(14) . . ?
F7 C8 C9 110.4(15) . . ?
F10 C8 F6 107.6(17) . . ?
F10 C8 F7 108.1(14) . . ?
F10 C8 C9 110.2(15) . . ?
C8 C9 N1 110.0(14) . . ?
C8 C9 C15 113.1(16) . . ?
C15 C9 N1 110.7(14) . . ?
F2 C17 C5 109.8(15) . . ?
F4 C17 F2 107.2(14) . . ?
F4 C17 C5 111.5(17) . . ?
F4 C17 F12 108.3(15) . . ?
F12 C17 F2 108.3(18) . . ?
F12 C17 C5 111.6(15) . . ?

_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 3.040
_oxdiff_exptl_absorpt_empirical_full_min 0.332
####################################################################### 
# 
# 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_hy_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2249985'
loop_
_audit_author_name
_audit_author_address
SF
;Zhengzhou University
China
;
_audit_update_record             
;
2023-03-18 deposited with the CCDC.	2023-05-30 downloaded from the CCDC.
;
_audit_creation_date             2022-07-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H7 F3 N)'
_chemical_formula_sum            'C6 H14 Br4 F6 N2 Pb'
_chemical_formula_weight         755.02
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 '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           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   24.2480(2)
_cell_length_b                   8.90729(7)
_cell_length_c                   7.91028(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1708.49(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10803
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      73.6090
_cell_measurement_theta_min      5.2620
_shelx_estimated_absorpt_T_max   0.749
_shelx_estimated_absorpt_T_min   0.460
_exptl_absorpt_coefficient_mu    30.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.935
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15698
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.741
_diffrn_reflns_theta_min         5.290
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     41.00  88.00   0.50    0.50    --    0.00  57.00   0.00   94
  2  ω    -21.00  30.00   0.50    0.50    --    0.00 -77.00   0.00  102
  3  ω    -37.00   7.00   0.50    0.50    --    0.00  82.00  60.00   88
  4  ω    -28.00   1.00   0.50    0.50    --    0.00  57.00   0.00   58
  5  ω     18.00  89.00   0.50    0.50    --    0.00  82.00  60.00  142
  6  ω    -89.00 -45.00   0.50    0.50    --    0.00 -77.00   0.00   88
  7  ω     13.00 159.00   0.50    0.50    --   98.80 -15.00 -60.00  292
  8  ω     16.00 126.00   0.50    0.50    --   98.80 -82.00 120.00  220
  9  ω     45.00  72.00   0.50    0.50    --   98.80 -15.00  90.00   54
 10  ω     61.00 134.00   0.50    0.50    --   98.80 -82.00-120.00  146
 11  ω     38.00 176.00   0.50    0.50    --   98.80  15.00   0.00  276
 12  ω     52.00 101.00   0.50    0.50    --   98.80 -82.00  30.00   98
 13  ω     16.00 135.00   0.50    0.50    --   98.80 -82.00 -90.00  238
 14  ω     19.00 136.00   0.50    0.50    --   98.80 -82.00 -60.00  234
 15  ω     66.00 100.00   0.50    0.50    --   98.80 -82.00  90.00   68
 16  ω    148.00 188.00   0.50    0.50    --   98.80  45.00  90.00   80
 17  ω     80.00 117.00   0.50    0.50    --   98.80  45.00  90.00   74
 18  ω     94.00 120.00   0.50    0.50    --   98.80 -82.00-180.00   52
 19  ω     18.00 127.00   0.50    0.50    --   98.80 -61.00 120.00  218
 20  ω     22.00  47.00   0.50    0.50    --   98.80 -82.00   0.00   50
 21  ω     96.00 126.00   0.50    0.50    --   98.80 -82.00   0.00   60
 22  ω     98.00 145.00   0.50    0.50    --   98.80 -15.00  90.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0111210000
_diffrn_orient_matrix_UB_12      0.0008773000
_diffrn_orient_matrix_UB_13      -0.1916901000
_diffrn_orient_matrix_UB_21      0.0625243000
_diffrn_orient_matrix_UB_22      -0.0053244000
_diffrn_orient_matrix_UB_23      -0.0340609000
_diffrn_orient_matrix_UB_31      -0.0019807000
_diffrn_orient_matrix_UB_32      -0.1729181000
_diffrn_orient_matrix_UB_33      0.0000107000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.707
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                3223
_reflns_number_total             3382
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         6.425
_refine_diff_density_min         -4.435
_refine_diff_density_rms         0.437
_refine_ls_abs_structure_details 
;
 Flack x determined using 1281 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3382
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0627
_refine_ls_restrained_S_all      1.123
_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)+(0.1558P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.1944
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C14(H14), C1AA(H1AA)
2.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C8(H8A,H8B,H8C), N9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.25101(2) 0.34178(6) 0.25598(6) 0.0233(3) Uani 1 1 d . . . . .
Br2 Br 0.24994(7) 0.66650(19) 0.4230(2) 0.0312(5) Uani 1 1 d . . . . .
Br3 Br 0.12966(8) 0.34801(18) 0.2334(2) 0.0296(5) Uani 1 1 d . . . . .
Br4 Br 0.37405(8) 0.3764(2) 0.2154(2) 0.0307(5) Uani 1 1 d . . . . .
Br5 Br 0.25202(7) 0.0584(2) 0.0529(2) 0.0341(5) Uani 1 1 d . . . . .
N1 N 0.3626(6) 0.2156(15) -0.1688(18) 0.030(3) Uani 1 1 d . . . . .
H1A H 0.326911 0.234451 -0.185371 0.037 Uiso 1 1 calc GR . . . .
H1B H 0.372716 0.251198 -0.068381 0.037 Uiso 1 1 calc GR . . . .
H1C H 0.368278 0.116978 -0.171964 0.037 Uiso 1 1 calc GR . . . .
C5 C 0.4560(8) 0.274(2) -0.266(3) 0.039(4) Uani 1 1 d . . . . .
F8 F 0.4870(5) 0.3208(18) -0.3967(17) 0.063(4) Uani 1 1 d . . . . .
F10 F 0.4710(5) 0.3523(14) -0.1313(15) 0.051(3) Uani 1 1 d . . . . .
F12 F 0.4694(5) 0.1310(14) -0.238(2) 0.067(4) Uani 1 1 d . . . . .
C14 C 0.3960(6) 0.2906(18) -0.306(2) 0.030(4) Uani 1 1 d . . . . .
H14 H 0.388329 0.240277 -0.413119 0.036 Uiso 1 1 calc R . . . .
F3 F 0.0579(5) 0.5070(13) -0.4031(16) 0.050(3) Uani 1 1 d . . . . .
F4 F 0.1453(4) 0.5052(12) -0.3498(14) 0.039(2) Uani 1 1 d . . . . .
F0AA F 0.0866(6) 0.5207(11) -0.1478(13) 0.046(3) Uani 1 1 d . . . . .
C6 C 0.0958(7) 0.4602(19) -0.294(2) 0.029(3) Uani 1 1 d . . . . .
C8 C 0.0402(7) 0.229(2) -0.208(3) 0.043(5) Uani 1 1 d . . . . .
H8A H 0.034765 0.272083 -0.097495 0.065 Uiso 1 1 calc GR . . . .
H8B H 0.041654 0.121733 -0.198331 0.065 Uiso 1 1 calc GR . . . .
H8C H 0.010157 0.257248 -0.279997 0.065 Uiso 1 1 calc GR . . . .
N9 N 0.1419(6) 0.2395(15) -0.1689(18) 0.028(3) Uani 1 1 d . . . . .
H9A H 0.148803 0.142310 -0.184318 0.034 Uiso 1 1 calc GR . . . .
H9B H 0.132893 0.255568 -0.061380 0.034 Uiso 1 1 calc GR . . . .
H9C H 0.171785 0.292718 -0.194773 0.034 Uiso 1 1 calc GR . . . .
C10 C 0.3787(9) 0.455(2) -0.321(2) 0.048(5) Uani 1 1 d . . . . .
H10A H 0.339214 0.461515 -0.318969 0.071 Uiso 1 1 calc GR . . . .
H10B H 0.392371 0.495230 -0.425189 0.071 Uiso 1 1 calc GR . . . .
H10C H 0.393699 0.510749 -0.227821 0.071 Uiso 1 1 calc GR . . . .
C1AA C 0.0944(7) 0.2870(18) -0.282(2) 0.030(3) Uani 1 1 d . . . . .
H1AA H 0.099633 0.244082 -0.395151 0.036 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 2.9808(17) 4_546 ?
Pb1 Br2 3.1801(17) . ?
Pb1 Br3 2.949(2) . ?
Pb1 Br4 3.016(2) . ?
Pb1 Br5 3.1141(17) 4 ?
Pb1 Br5 2.9922(18) . ?
Br2 Pb1 2.9808(17) 4_556 ?
Br5 Pb1 3.1141(17) 4_545 ?
N1 C14 1.51(2) . ?
C5 F8 1.34(2) . ?
C5 F10 1.33(2) . ?
C5 F12 1.33(2) . ?
C5 C14 1.50(2) . ?
C14 C10 1.53(2) . ?
F3 C6 1.328(19) . ?
F4 C6 1.338(19) . ?
F0AA C6 1.30(2) . ?
C6 C1AA 1.55(2) . ?
C8 C1AA 1.53(2) . ?
N9 C1AA 1.52(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br2 97.03(2) 4_546 . ?
Br2 Pb1 Br4 98.73(5) 4_546 . ?
Br2 Pb1 Br5 90.88(5) 4_546 . ?
Br2 Pb1 Br5 173.06(5) 4_546 4 ?
Br3 Pb1 Br2 93.08(5) . 4_546 ?
Br3 Pb1 Br2 89.99(5) . . ?
Br3 Pb1 Br4 168.16(6) . . ?
Br3 Pb1 Br5 89.51(5) . . ?
Br3 Pb1 Br5 85.25(5) . 4 ?
Br4 Pb1 Br2 87.67(5) . . ?
Br4 Pb1 Br5 82.91(5) . 4 ?
Br5 Pb1 Br2 76.26(5) 4 . ?
Br5 Pb1 Br2 172.09(5) . . ?
Br5 Pb1 Br4 91.20(5) . . ?
Br5 Pb1 Br5 95.834(18) . 4 ?
Pb1 Br2 Pb1 146.14(6) 4_556 . ?
Pb1 Br5 Pb1 160.67(7) . 4_545 ?
F8 C5 C14 110.7(16) . . ?
F10 C5 F8 107.3(15) . . ?
F10 C5 C14 112.3(15) . . ?
F12 C5 F8 107.1(17) . . ?
F12 C5 F10 107.4(18) . . ?
F12 C5 C14 111.7(15) . . ?
N1 C14 C10 109.5(14) . . ?
C5 C14 N1 109.3(15) . . ?
C5 C14 C10 112.4(15) . . ?
F3 C6 F4 108.3(13) . . ?
F3 C6 C1AA 109.7(15) . . ?
F4 C6 C1AA 109.8(14) . . ?
F0AA C6 F3 109.2(14) . . ?
F0AA C6 F4 108.9(16) . . ?
F0AA C6 C1AA 110.9(13) . . ?
C8 C1AA C6 112.3(14) . . ?
N9 C1AA C6 107.3(13) . . ?
N9 C1AA C8 109.2(15) . . ?

_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 2.146
_oxdiff_exptl_absorpt_empirical_full_min 0.476
