# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_(DCAn)Br
_database_code_depnum_ccdc_archive 'CCDC 2240927'
loop_
_audit_author_name
_audit_author_address
'Binbin Luo'
;Shantou University
China
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
_audit_creation_date             2023-01-11
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br, C17 H17 Cl N'
_chemical_formula_sum            'C17 H17 Br Cl N'
_chemical_formula_weight         350.67
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Br Pb Cl'
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'
Cl Cl 0.3639 0.7018 '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'

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

_cell_length_a                   10.55490(10)
_cell_length_b                   13.17590(10)
_cell_length_c                   11.98320(10)
_cell_angle_alpha                90
_cell_angle_beta                 113.4820(10)
_cell_angle_gamma                90
_cell_volume                     1528.50(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5437
_cell_measurement_temperature    300.10(10)
_cell_measurement_theta_max      73.9750
_cell_measurement_theta_min      4.7210
_shelx_estimated_absorpt_T_max   0.782
_shelx_estimated_absorpt_T_min   0.232
_exptl_absorpt_coefficient_mu    5.169
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (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    1.524
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7703
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.269
_diffrn_reflns_theta_min         4.734
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.10(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00  47.00   0.50    0.50    --    0.00  37.00 -60.00  132
  2  ω    -13.00  26.00   0.50    0.50    --    0.00  37.00  30.00   78
  3  ω     34.00  87.00   0.50    0.50    --    0.00  37.00  30.00  106
  4  ω     77.00 145.00   0.50    0.50    --   95.80  30.00  30.00  136
  5  ω     13.00 104.00   0.50    0.50    --   95.80 -30.00 120.00  182
  6  ω     22.00 105.00   0.50    0.50    --   95.80 -77.00-150.00  166
  7  ω     11.00 112.00   0.50    0.50    --   95.80 -82.00  60.00  202
  8  ω     39.00 125.00   0.50    0.50    --   95.80 -77.00 -90.00  172
  9  ω     78.00 167.00   0.50    0.50    --   95.80  30.00 -60.00  178
;
_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      -0.0913168000
_diffrn_orient_matrix_UB_12      -0.0788960000
_diffrn_orient_matrix_UB_13      0.0276021000
_diffrn_orient_matrix_UB_21      -0.0518391000
_diffrn_orient_matrix_UB_22      0.0827249000
_diffrn_orient_matrix_UB_23      0.0623466000
_diffrn_orient_matrix_UB_31      -0.1195764000
_diffrn_orient_matrix_UB_32      0.0243953000
_diffrn_orient_matrix_UB_33      -0.1225384000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2766
_reflns_number_total             3002
_reflns_odcompleteness_completeness 99.72
_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 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0101(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   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3002
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0250
_refine_ls_restrained_S_all      1.052
_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)+(0.0302P)²+0.5173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0674
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Ternary CH refined with riding coordinates:
 N1(H1)
1.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
1.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C16(H16), C6(H6), C13(H13), C8(H8), C7(H7), C14(H14), C15(H15)
1.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.65263(2) 0.36251(2) 1.09971(2) 0.05749(11) Uani 1 1 d . . . . .
Cl1 Cl 0.87992(5) 0.42548(5) 0.52670(5) 0.06689(17) Uani 1 1 d . . . . .
N1 N 0.44664(15) 0.35485(10) 0.82022(13) 0.0374(3) Uani 1 1 d . . . . .
H1 H 0.522398 0.383275 0.891149 0.045 Uiso 1 1 calc R U . . .
C17 C 0.66426(17) 0.47217(12) 0.73399(14) 0.0347(3) Uani 1 1 d . . . . .
C10 C 0.62722(17) 0.37214(11) 0.51295(15) 0.0354(3) Uani 1 1 d . . . . .
C12 C 0.77420(17) 0.47094(12) 0.69171(15) 0.0375(3) Uani 1 1 d . . . . .
C4 C 0.54025(16) 0.42000(12) 0.66872(14) 0.0339(3) Uani 1 1 d . . . . .
C5 C 0.52093(17) 0.36801(11) 0.56000(15) 0.0336(3) Uani 1 1 d . . . . .
C11 C 0.74979(18) 0.42258(13) 0.58165(16) 0.0388(4) Uani 1 1 d . . . . .
C2 C 0.4849(2) 0.24874(13) 0.80403(17) 0.0463(4) Uani 1 1 d . . . . .
H2A H 0.410599 0.217772 0.737303 0.069 Uiso 1 1 calc R U . . .
H2B H 0.502282 0.210785 0.877043 0.069 Uiso 1 1 calc R U . . .
H2C H 0.566641 0.249283 0.787295 0.069 Uiso 1 1 calc R U . . .
C9 C 0.6029(2) 0.32513(13) 0.39895(16) 0.0430(4) Uani 1 1 d . . . . .
H9 H 0.669005 0.330836 0.366193 0.052 Uiso 1 1 calc R U . . .
C16 C 0.6878(2) 0.52715(14) 0.84325(16) 0.0450(4) Uani 1 1 d . . . . .
H16 H 0.617552 0.531376 0.871369 0.054 Uiso 1 1 calc R U . . .
C6 C 0.40063(18) 0.30959(14) 0.49201(16) 0.0429(4) Uani 1 1 d . . . . .
H6 H 0.331273 0.303473 0.520942 0.052 Uiso 1 1 calc R U . . .
C3 C 0.42534(17) 0.42335(13) 0.71333(15) 0.0375(3) Uani 1 1 d . . . . .
H3A H 0.339609 0.404540 0.646799 0.045 Uiso 1 1 calc R U . . .
H3B H 0.415442 0.492595 0.736162 0.045 Uiso 1 1 calc R U . . .
C13 C 0.90211(19) 0.51884(14) 0.76372(18) 0.0482(4) Uani 1 1 d . . . . .
H13 H 0.974826 0.516223 0.738602 0.058 Uiso 1 1 calc R U . . .
C1 C 0.3201(2) 0.35569(16) 0.8470(2) 0.0549(5) Uani 1 1 d . . . . .
H1A H 0.243731 0.328459 0.778699 0.082 Uiso 1 1 calc R U . . .
H1B H 0.299513 0.424127 0.861671 0.082 Uiso 1 1 calc R U . . .
H1C H 0.335518 0.315036 0.917676 0.082 Uiso 1 1 calc R U . . .
C8 C 0.4859(2) 0.27259(15) 0.33772(17) 0.0498(4) Uani 1 1 d . . . . .
H8 H 0.471914 0.242774 0.263372 0.060 Uiso 1 1 calc R U . . .
C7 C 0.3849(2) 0.26283(15) 0.38639(18) 0.0501(4) Uani 1 1 d . . . . .
H7 H 0.306548 0.223846 0.345586 0.060 Uiso 1 1 calc R U . . .
C14 C 0.9193(2) 0.56776(15) 0.86744(19) 0.0550(5) Uani 1 1 d . . . . .
H14 H 1.003625 0.598080 0.913353 0.066 Uiso 1 1 calc R U . . .
C15 C 0.8105(2) 0.57331(16) 0.90680(17) 0.0550(5) Uani 1 1 d . . . . .
H15 H 0.822788 0.609085 0.977283 0.066 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C11 1.7442(16) . ?
N1 H1 0.9800 . ?
N1 C2 1.489(2) . ?
N1 C3 1.509(2) . ?
N1 C1 1.493(2) . ?
C17 C12 1.439(2) . ?
C17 C4 1.408(2) . ?
C17 C16 1.429(2) . ?
C10 C5 1.444(2) . ?
C10 C11 1.394(2) . ?
C10 C9 1.427(2) . ?
C12 C11 1.393(2) . ?
C12 C13 1.427(2) . ?
C4 C5 1.413(2) . ?
C4 C3 1.508(2) . ?
C5 C6 1.430(2) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C9 H9 0.9300 . ?
C9 C8 1.349(3) . ?
C16 H16 0.9300 . ?
C16 C15 1.357(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.357(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C13 H13 0.9300 . ?
C13 C14 1.347(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C8 H8 0.9300 . ?
C8 C7 1.410(3) . ?
C7 H7 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.406(3) . ?
C15 H15 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 H1 107.6 . . ?
C2 N1 C3 114.03(13) . . ?
C2 N1 C1 110.34(14) . . ?
C3 N1 H1 107.6 . . ?
C1 N1 H1 107.6 . . ?
C1 N1 C3 109.53(14) . . ?
C4 C17 C12 120.03(14) . . ?
C4 C17 C16 122.70(15) . . ?
C16 C17 C12 117.27(15) . . ?
C11 C10 C5 118.03(14) . . ?
C11 C10 C9 122.88(15) . . ?
C9 C10 C5 119.09(15) . . ?
C11 C12 C17 117.86(15) . . ?
C11 C12 C13 123.24(16) . . ?
C13 C12 C17 118.90(16) . . ?
C17 C4 C5 120.64(14) . . ?
C17 C4 C3 119.32(14) . . ?
C5 C4 C3 120.00(14) . . ?
C4 C5 C10 119.52(14) . . ?
C4 C5 C6 123.75(14) . . ?
C6 C5 C10 116.72(15) . . ?
C10 C11 Cl1 118.19(13) . . ?
C12 C11 Cl1 118.09(13) . . ?
C12 C11 C10 123.71(15) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C10 C9 H9 119.3 . . ?
C8 C9 C10 121.34(16) . . ?
C8 C9 H9 119.3 . . ?
C17 C16 H16 119.3 . . ?
C15 C16 C17 121.33(18) . . ?
C15 C16 H16 119.3 . . ?
C5 C6 H6 119.1 . . ?
C7 C6 C5 121.78(17) . . ?
C7 C6 H6 119.1 . . ?
N1 C3 H3A 108.6 . . ?
N1 C3 H3B 108.6 . . ?
C4 C3 N1 114.48(13) . . ?
C4 C3 H3A 108.6 . . ?
C4 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 121.09(18) . . ?
C14 C13 H13 119.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C9 C8 H8 120.0 . . ?
C9 C8 C7 120.04(17) . . ?
C7 C8 H8 120.0 . . ?
C6 C7 C8 120.84(18) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C13 C14 H14 119.8 . . ?
C13 C14 C15 120.47(18) . . ?
C15 C14 H14 119.8 . . ?
C16 C15 C14 120.84(18) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C17 C12 C11 Cl1 177.32(12) . . . . ?
C17 C12 C11 C10 -2.6(2) . . . . ?
C17 C12 C13 C14 -2.4(3) . . . . ?
C17 C4 C5 C10 -2.6(2) . . . . ?
C17 C4 C5 C6 176.98(15) . . . . ?
C17 C4 C3 N1 -77.36(19) . . . . ?
C17 C16 C15 C14 -0.5(3) . . . . ?
C10 C5 C6 C7 -2.0(3) . . . . ?
C10 C9 C8 C7 -0.3(3) . . . . ?
C12 C17 C4 C5 -1.5(2) . . . . ?
C12 C17 C4 C3 -179.11(14) . . . . ?
C12 C17 C16 C15 -2.2(3) . . . . ?
C12 C13 C14 C15 -0.4(3) . . . . ?
C4 C17 C12 C11 4.0(2) . . . . ?
C4 C17 C12 C13 -175.96(15) . . . . ?
C4 C17 C16 C15 177.33(17) . . . . ?
C4 C5 C6 C7 178.40(17) . . . . ?
C5 C10 C11 Cl1 178.68(11) . . . . ?
C5 C10 C11 C12 -1.4(2) . . . . ?
C5 C10 C9 C8 -3.5(3) . . . . ?
C5 C4 C3 N1 104.96(17) . . . . ?
C5 C6 C7 C8 -1.8(3) . . . . ?
C11 C10 C5 C4 4.0(2) . . . . ?
C11 C10 C5 C6 -175.60(15) . . . . ?
C11 C10 C9 C8 176.63(17) . . . . ?
C11 C12 C13 C14 177.64(18) . . . . ?
C2 N1 C3 C4 -49.41(19) . . . . ?
C9 C10 C5 C4 -175.83(15) . . . . ?
C9 C10 C5 C6 4.5(2) . . . . ?
C9 C10 C11 Cl1 -1.5(2) . . . . ?
C9 C10 C11 C12 178.45(16) . . . . ?
C9 C8 C7 C6 3.0(3) . . . . ?
C16 C17 C12 C11 -176.38(15) . . . . ?
C16 C17 C12 C13 3.6(2) . . . . ?
C16 C17 C4 C5 178.97(15) . . . . ?
C16 C17 C4 C3 1.3(2) . . . . ?
C3 C4 C5 C10 175.02(14) . . . . ?
C3 C4 C5 C6 -5.4(2) . . . . ?
C13 C12 C11 Cl1 -2.7(2) . . . . ?
C13 C12 C11 C10 177.39(16) . . . . ?
C13 C14 C15 C16 1.9(3) . . . . ?
C1 N1 C3 C4 -173.60(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 1.310
_oxdiff_exptl_absorpt_empirical_full_min 0.803
####################################################################### 
# 
# 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_1-C3
_database_code_depnum_ccdc_archive 'CCDC 2240928'
loop_
_audit_author_name
_audit_author_address
'Binbin Luo'
;Shantou University
China
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
_audit_creation_date             2023-01-08
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'Br10 Pb3, 4(C17 H17 Cl N), 2(C3 H8 O)'
_chemical_formula_sum            'C74 H84 Br10 Cl4 N4 O2 Pb3'
_chemical_formula_weight         2623.92
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Pb Br'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.4204(5)
_cell_length_b                   9.8038(2)
_cell_length_c                   40.7386(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.275(2)
_cell_angle_gamma                90
_cell_volume                     8548.4(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    297.98(10)
_cell_measurement_theta_max      70.9170
_cell_measurement_theta_min      4.0930
_shelx_estimated_absorpt_T_max   0.838
_shelx_estimated_absorpt_T_min   0.121
_exptl_absorpt_coefficient_mu    18.266
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (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    2.039
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             4944
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            19499
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.967
_diffrn_reflns_theta_min         4.131
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00  16.00   0.50    4.29    --    0.00 -37.00  60.00   76
  2  ω     20.00  86.00   0.50    4.29    --    0.00  37.00 -60.00  132
  3  ω    -81.00 -53.00   0.50    4.29    --    0.00 -37.00  60.00   56
  4  ω    131.00 177.00   0.50   17.17    --   89.30  30.00-180.00   92
  5  ω     91.00 174.00   0.50   17.17    --   89.30  30.00-150.00  166
  6  ω      1.00  95.00   0.50   17.17    --   89.30 -82.00   0.00  188
  7  ω     13.00 110.00   0.50   17.17    --   89.30 -45.00  30.00  194
  8  ω     77.00 114.00   0.50   17.17    --   89.30 -61.00   0.00   74
  9  ω     74.00 123.00   0.50   17.17    --   89.30  30.00-180.00   98
 10  ω     71.00 168.00   0.50   17.17    --   89.30  45.00 -90.00  194
;
_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      -0.0143664000
_diffrn_orient_matrix_UB_12      0.0867143000
_diffrn_orient_matrix_UB_13      0.0303238000
_diffrn_orient_matrix_UB_21      -0.0251795000
_diffrn_orient_matrix_UB_22      0.1149870000
_diffrn_orient_matrix_UB_23      -0.0226434000
_diffrn_orient_matrix_UB_31      -0.0658944000
_diffrn_orient_matrix_UB_32      -0.0627911000
_diffrn_orient_matrix_UB_33      0.0004192000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6827
_reflns_number_total             7933
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.982
_refine_diff_density_min         -1.798
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7933
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0479
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0754P)²+121.6773P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1450
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C35A-C36A
 1.5 with sigma of 0.02
 C37B-C35B
 2.56 with sigma of 0.02
 C35B-C36B
 1.54 with sigma of 0.02
 C37B-C36B
 1.54 with sigma of 0.02
 C35A-C37A
 2.56 with sigma of 0.02
 O1A-C37A
 1.44 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C35B \\sim C36B \\sim C37B: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C35A \\sim C36A \\sim C37A: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C5 \\sim C6 \\sim C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002 within 2A
Uanis(C35B) \\sim Ueq, Uanis(C36B) \\sim Ueq, Uanis(C37B) \\sim Ueq, Uanis(O1B)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 O1B, C36B, C37B, C35B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C36A, O1A, C37A, C35A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: O1A(0.5) H1AA(0.5) C37A(0.5) H37A(0.5) H37B(0.5) C35A(0.5)
 H35A(0.5) H35B(0.5) H35C(0.5) C36A(0.5) H36A(0.5) H36B(0.5) O1B(0.5) H1B(0.5)
 C35B(0.5) H35D(0.5) H35E(0.5) H35F(0.5) C36B(0.5) H36C(0.5) H36D(0.5)
 C37B(0.5) H37C(0.5) H37D(0.5)
5.a Everything fixed:
 H1B
5.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
5.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C15(H15A,H15B), C37A(H37A,H37B), C36A(H36A,H36B), C36B(H36C,
 H36D), C37B(H37C,H37D)
5.d Aromatic/amide H refined with riding coordinates:
 C23(H23), C22(H22), C31(H31), C32(H32), C11(H11), C21(H21), C26(H26), C3(H3),
 C33(H33), C14(H14), C12(H12), C6(H6), C13(H13), C34(H34), C2(H2A), C1(H1A)
5.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C17(H17A,H17B,
 H17C), C35A(H35A,H35B,H35C), C35B(H35D,H35E,H35F)
5.f Idealised tetrahedral OH refined as rotating group:
 O1A(H1AA)
;
_atom_sites_solution_hydrogens   mixed
_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
Pb2 Pb 0.67539(2) 0.79418(3) 0.72763(2) 0.04144(12) Uani 1 1 d . . . . .
Pb1 Pb 0.500000 0.79993(5) 0.750000 0.04386(14) Uani 1 2 d S T P . .
Br1 Br 0.61517(5) 0.78227(10) 0.79413(2) 0.0535(2) Uani 1 1 d . . . . .
Br4 Br 0.74707(4) 0.55113(10) 0.75215(2) 0.0575(3) Uani 1 1 d . . . . .
Br3 Br 0.57103(5) 1.01447(10) 0.71509(2) 0.0595(3) Uani 1 1 d . . . . .
Br5 Br 0.74635(5) 0.80786(11) 0.66561(3) 0.0633(3) Uani 1 1 d . . . . .
Br2 Br 0.56955(5) 0.61162(12) 0.70265(3) 0.0709(3) Uani 1 1 d . . . . .
Cl2 Cl 0.9067(2) 0.7683(4) 0.52705(7) 0.0981(11) Uani 1 1 d . . . . .
Cl1 Cl 0.5829(2) 0.2311(4) 0.49554(7) 0.1083(13) Uani 1 1 d . . . . .
N1 N 0.6864(4) 0.2870(7) 0.65379(18) 0.0506(17) Uani 1 1 d . . . . .
H1 H 0.692711 0.370272 0.641050 0.061 Uiso 1 1 calc R U . . .
N2 N 0.8961(3) 0.7902(7) 0.69318(17) 0.0478(17) Uani 1 1 d . . . . .
H2 H 0.860939 0.832780 0.680916 0.057 Uiso 1 1 calc R U . . .
C20 C 0.9541(4) 0.8101(9) 0.6736(2) 0.0482(19) Uani 1 1 d . . . . .
H20A H 0.971169 0.900014 0.678180 0.058 Uiso 1 1 calc R U . . .
H20B H 0.985239 0.743282 0.680627 0.058 Uiso 1 1 calc R U . . .
C24 C 0.9533(4) 0.6734(9) 0.6209(2) 0.0472(19) Uani 1 1 d . . . . .
C7 C 0.6146(4) 0.2264(9) 0.6062(2) 0.049(2) Uani 1 1 d . . . . .
C18 C 0.8808(5) 0.6417(11) 0.6975(3) 0.063(3) Uani 1 1 d . . . . .
H18A H 0.877288 0.598257 0.676403 0.095 Uiso 1 1 calc R U . . .
H18B H 0.841943 0.633254 0.708300 0.095 Uiso 1 1 calc R U . . .
H18C H 0.913437 0.598681 0.710625 0.095 Uiso 1 1 calc R U . . .
C23 C 0.9768(5) 0.5543(10) 0.6374(2) 0.056(2) Uani 1 1 d . . . . .
H23 H 0.984136 0.557034 0.660022 0.067 Uiso 1 1 calc R U . . .
C27 C 0.9408(4) 0.7959(8) 0.6375(2) 0.0449(18) Uani 1 1 d . . . . .
O1A O 0.734(2) 0.520(4) 0.6263(12) 0.104(9) Uani 0.5 1 d D . P A 1
H1AA H 0.722076 0.597106 0.631346 0.157 Uiso 0.5 1 calc R U P A 1
C16 C 0.7396(6) 0.1952(12) 0.6483(3) 0.080(3) Uani 1 1 d . . . . .
H16A H 0.734406 0.112183 0.660394 0.119 Uiso 1 1 calc R U . . .
H16B H 0.777750 0.238900 0.655615 0.119 Uiso 1 1 calc R U . . .
H16C H 0.741192 0.174719 0.625299 0.119 Uiso 1 1 calc R U . . .
C28 C 0.9174(4) 0.9103(9) 0.6198(2) 0.051(2) Uani 1 1 d . . . . .
C25 C 0.9430(5) 0.6636(10) 0.5862(2) 0.054(2) Uani 1 1 d . . . . .
C30 C 0.9192(5) 0.7786(11) 0.5693(2) 0.062(3) Uani 1 1 d . . . . .
C15 C 0.6251(5) 0.2276(10) 0.6428(2) 0.056(2) Uani 1 1 d . . . . .
H15A H 0.591993 0.279608 0.652487 0.067 Uiso 1 1 calc R U . . .
H15B H 0.622668 0.134795 0.650943 0.067 Uiso 1 1 calc R U . . .
C22 C 0.9888(6) 0.4372(12) 0.6210(3) 0.077(3) Uani 1 1 d . . . . .
H22 H 1.004158 0.361364 0.632392 0.092 Uiso 1 1 calc R U . . .
C19 C 0.9030(6) 0.8595(15) 0.7257(2) 0.079(3) Uani 1 1 d . . . . .
H19A H 0.934170 0.813187 0.739162 0.119 Uiso 1 1 calc R U . . .
H19B H 0.863830 0.857428 0.736374 0.119 Uiso 1 1 calc R U . . .
H19C H 0.915516 0.952495 0.722621 0.119 Uiso 1 1 calc R U . . .
C8 C 0.5927(4) 0.3470(10) 0.5905(2) 0.052(2) Uani 1 1 d . . . . .
C5 C 0.6159(7) 0.1101(12) 0.5532(3) 0.0869(16) Uani 1 1 d . U . . .
C17 C 0.6870(7) 0.3252(14) 0.6889(3) 0.087(4) Uani 1 1 d . . . . .
H17A H 0.677847 0.246448 0.701855 0.130 Uiso 1 1 calc R U . . .
H17B H 0.656099 0.394246 0.692171 0.130 Uiso 1 1 calc R U . . .
H17C H 0.727540 0.359829 0.695498 0.130 Uiso 1 1 calc R U . . .
C31 C 0.9071(5) 1.0380(10) 0.6352(3) 0.064(3) Uani 1 1 d . . . . .
H31 H 0.914937 1.046639 0.657749 0.076 Uiso 1 1 calc R U . . .
C4 C 0.6258(7) 0.1083(12) 0.5881(3) 0.0866(16) Uani 1 1 d . U . . .
C9 C 0.5818(5) 0.3482(10) 0.5556(2) 0.058(2) Uani 1 1 d . . . . .
C32 C 0.8859(6) 1.1477(12) 0.6177(3) 0.079(3) Uani 1 1 d . . . . .
H32 H 0.880537 1.230965 0.628192 0.095 Uiso 1 1 calc R U . . .
C10 C 0.5939(6) 0.2298(11) 0.5384(2) 0.066(3) Uani 1 1 d . . . . .
C11 C 0.5798(5) 0.4710(11) 0.6076(3) 0.061(2) Uani 1 1 d . . . . .
H11 H 0.586058 0.474383 0.630320 0.073 Uiso 1 1 calc R U . . .
C21 C 0.9783(6) 0.4304(12) 0.5872(3) 0.082(3) Uani 1 1 d . . . . .
H21 H 0.986080 0.349264 0.576228 0.098 Uiso 1 1 calc R U . . .
C29 C 0.9057(5) 0.9001(10) 0.5851(2) 0.058(2) Uani 1 1 d . . . . .
C26 C 0.9573(6) 0.5381(11) 0.5701(3) 0.072(3) Uani 1 1 d . . . . .
H26 H 0.951826 0.531694 0.547359 0.086 Uiso 1 1 calc R U . . .
C3 C 0.6465(7) -0.0170(12) 0.6026(3) 0.0871(16) Uani 1 1 d . U . . .
H3 H 0.652316 -0.021106 0.625346 0.105 Uiso 1 1 calc R U . . .
C33 C 0.8721(7) 1.1354(13) 0.5837(3) 0.094(4) Uani 1 1 d . . . . .
H33 H 0.856192 1.210055 0.571981 0.113 Uiso 1 1 calc R U . . .
C14 C 0.5598(6) 0.4701(11) 0.5399(3) 0.074(3) Uani 1 1 d . . . . .
H14 H 0.553014 0.472291 0.517236 0.089 Uiso 1 1 calc R U . . .
C12 C 0.5589(6) 0.5822(12) 0.5915(3) 0.080(3) Uani 1 1 d . . . . .
H12 H 0.551021 0.661292 0.603238 0.097 Uiso 1 1 calc R U . . .
C6 C 0.6299(7) -0.0096(12) 0.5350(3) 0.0877(16) Uani 1 1 d . U . . .
H6 H 0.625027 -0.007973 0.512209 0.105 Uiso 1 1 calc R U . . .
C13 C 0.5488(7) 0.5813(13) 0.5578(3) 0.084(4) Uani 1 1 d . . . . .
H13 H 0.534007 0.659857 0.547276 0.101 Uiso 1 1 calc R U . . .
C34 C 0.8816(7) 1.0185(13) 0.5680(3) 0.084(4) Uani 1 1 d . . . . .
H34 H 0.872459 1.013153 0.545578 0.101 Uiso 1 1 calc R U . . .
C37A C 0.783(2) 0.531(7) 0.6037(8) 0.139(7) Uani 0.5 1 d D U P A 1
H37A H 0.821437 0.497524 0.614049 0.167 Uiso 0.5 1 calc R U P A 1
H37B H 0.788828 0.625779 0.597943 0.167 Uiso 0.5 1 calc R U P A 1
C35A C 0.739(2) 0.532(4) 0.5448(8) 0.140(7) Uani 0.5 1 d D U P A 1
H35A H 0.736908 0.480898 0.524681 0.210 Uiso 0.5 1 calc R U P A 1
H35B H 0.764002 0.611879 0.542117 0.210 Uiso 0.5 1 calc R U P A 1
H35C H 0.697564 0.558105 0.550473 0.210 Uiso 0.5 1 calc R U P A 1
C36A C 0.767(2) 0.446(4) 0.5715(9) 0.139(7) Uani 0.5 1 d D U P A 1
H36A H 0.805508 0.405018 0.563940 0.167 Uiso 0.5 1 calc R U P A 1
H36B H 0.738803 0.372635 0.576460 0.167 Uiso 0.5 1 calc R U P A 1
C2 C 0.6578(7) -0.1285(12) 0.5851(3) 0.0878(16) Uani 1 1 d . U . . .
H2A H 0.670654 -0.208249 0.595708 0.105 Uiso 1 1 calc R U . . .
C1 C 0.6504(7) -0.1264(12) 0.5502(3) 0.0881(16) Uani 1 1 d . U . . .
H1A H 0.659292 -0.203444 0.537887 0.106 Uiso 1 1 calc R U . . .
O1B O 0.741(2) 0.516(5) 0.6248(14) 0.133(11) Uani 0.5 1 d . U P B 2
H1B H 0.709250 0.490940 0.625540 0.200 Uiso 0.5 1 d . U P C 2
C35B C 0.7761(19) 0.486(7) 0.5410(9) 0.187(9) Uani 0.5 1 d D U P B 2
H35D H 0.755447 0.412735 0.529279 0.281 Uiso 0.5 1 calc R U P B 2
H35E H 0.818262 0.459732 0.546831 0.281 Uiso 0.5 1 calc R U P B 2
H35F H 0.776509 0.565532 0.527215 0.281 Uiso 0.5 1 calc R U P B 2
C36B C 0.7412(17) 0.518(8) 0.5721(10) 0.187(9) Uani 0.5 1 d D U P B 2
H36C H 0.721823 0.607070 0.569843 0.225 Uiso 0.5 1 calc R U P B 2
H36D H 0.708204 0.451337 0.574481 0.225 Uiso 0.5 1 calc R U P B 2
C37B C 0.784(3) 0.517(11) 0.6033(10) 0.187(9) Uani 0.5 1 d D U P B 2
H37C H 0.809671 0.435703 0.604653 0.225 Uiso 0.5 1 calc R U P B 2
H37D H 0.809825 0.597495 0.604977 0.225 Uiso 0.5 1 calc R U P B 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
Pb2 Br1 3.0490(10) . ?
Pb2 Br4 2.9852(10) . ?
Pb2 Br4 3.1105(10) 4_656 ?
Pb2 Br3 3.1356(11) . ?
Pb2 Br5 3.0028(11) . ?
Pb2 Br2 3.0323(11) . ?
Pb1 Br1 2.9994(9) 2_656 ?
Pb1 Br1 2.9993(9) . ?
Pb1 Br3 2.9889(10) . ?
Pb1 Br3 2.9889(10) 2_656 ?
Pb1 Br2 3.0946(11) 2_656 ?
Pb1 Br2 3.0947(11) . ?
Cl2 C30 1.735(10) . ?
Cl1 C10 1.753(10) . ?
N1 H1 0.9800 . ?
N1 C16 1.475(13) . ?
N1 C15 1.489(12) . ?
N1 C17 1.478(12) . ?
N2 H2 0.9800 . ?
N2 C20 1.514(11) . ?
N2 C18 1.504(12) . ?
N2 C19 1.493(13) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C27 1.493(12) . ?
C24 C23 1.429(13) . ?
C24 C27 1.410(12) . ?
C24 C25 1.425(12) . ?
C7 C15 1.499(12) . ?
C7 C8 1.416(12) . ?
C7 C4 1.399(14) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C23 H23 0.9300 . ?
C23 C22 1.358(14) . ?
C27 C28 1.414(12) . ?
O1A H1AA 0.8200 . ?
O1A C37A 1.43(2) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C28 C31 1.422(13) . ?
C28 C29 1.431(13) . ?
C25 C30 1.406(14) . ?
C25 C26 1.433(13) . ?
C30 C29 1.389(14) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C22 H22 0.9300 . ?
C22 C21 1.388(17) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C8 C9 1.433(13) . ?
C8 C11 1.434(14) . ?
C5 C4 1.430(16) . ?
C5 C10 1.393(15) . ?
C5 C6 1.426(16) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C31 H31 0.9300 . ?
C31 C32 1.358(15) . ?
C4 C3 1.427(16) . ?
C9 C10 1.385(15) . ?
C9 C14 1.426(14) . ?
C32 H32 0.9300 . ?
C32 C33 1.413(18) . ?
C11 H11 0.9300 . ?
C11 C12 1.340(15) . ?
C21 H21 0.9300 . ?
C21 C26 1.333(16) . ?
C29 C34 1.438(14) . ?
C26 H26 0.9300 . ?
C3 H3 0.9300 . ?
C3 C2 1.334(16) . ?
C33 H33 0.9300 . ?
C33 C34 1.331(18) . ?
C14 H14 0.9300 . ?
C14 C13 1.336(17) . ?
C12 H12 0.9300 . ?
C12 C13 1.383(17) . ?
C6 H6 0.9300 . ?
C6 C1 1.365(16) . ?
C13 H13 0.9300 . ?
C34 H34 0.9300 . ?
C37A H37A 0.9700 . ?
C37A H37B 0.9700 . ?
C37A C36A 1.58(6) . ?
C35A H35A 0.9600 . ?
C35A H35B 0.9600 . ?
C35A H35C 0.9600 . ?
C35A C36A 1.485(19) . ?
C36A H36A 0.9700 . ?
C36A H36B 0.9700 . ?
C2 H2A 0.9300 . ?
C2 C1 1.425(17) . ?
C1 H1A 0.9300 . ?
O1B H1B 0.7274 . ?
O1B C37B 1.29(5) . ?
C35B H35D 0.9600 . ?
C35B H35E 0.9600 . ?
C35B H35F 0.9600 . ?
C35B C36B 1.532(19) . ?
C36B H36C 0.9700 . ?
C36B H36D 0.9700 . ?
C36B C37B 1.53(2) . ?
C37B H37C 0.9700 . ?
C37B H37D 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb2 Br4 92.06(3) . 4_656 ?
Br1 Pb2 Br3 81.20(3) . . ?
Br4 Pb2 Br1 84.39(3) . . ?
Br4 Pb2 Br4 107.198(9) . 4_656 ?
Br4 Pb2 Br3 81.67(3) 4_656 . ?
Br4 Pb2 Br3 163.37(3) . . ?
Br4 Pb2 Br5 92.66(3) . . ?
Br4 Pb2 Br2 90.51(3) . . ?
Br5 Pb2 Br1 174.60(3) . . ?
Br5 Pb2 Br4 84.48(3) . 4_656 ?
Br5 Pb2 Br3 102.33(3) . . ?
Br5 Pb2 Br2 98.09(3) . . ?
Br2 Pb2 Br1 86.48(3) . . ?
Br2 Pb2 Br4 162.02(3) . 4_656 ?
Br2 Pb2 Br3 80.40(3) . . ?
Br1 Pb1 Br1 173.38(4) . 2_656 ?
Br1 Pb1 Br2 86.24(3) . . ?
Br1 Pb1 Br2 89.82(3) . 2_656 ?
Br1 Pb1 Br2 86.23(3) 2_656 2_656 ?
Br1 Pb1 Br2 89.82(3) 2_656 . ?
Br3 Pb1 Br1 84.48(3) . . ?
Br3 Pb1 Br1 84.48(3) 2_656 2_656 ?
Br3 Pb1 Br1 100.22(3) 2_656 . ?
Br3 Pb1 Br1 100.22(3) . 2_656 ?
Br3 Pb1 Br3 90.55(5) . 2_656 ?
Br3 Pb1 Br2 81.75(3) . . ?
Br3 Pb1 Br2 169.47(3) . 2_656 ?
Br3 Pb1 Br2 81.75(3) 2_656 2_656 ?
Br3 Pb1 Br2 169.47(3) 2_656 . ?
Br2 Pb1 Br2 106.75(5) 2_656 . ?
Pb1 Br1 Pb2 80.33(2) . . ?
Pb2 Br4 Pb2 175.75(4) . 4_646 ?
Pb1 Br3 Pb2 79.10(2) . . ?
Pb2 Br2 Pb1 79.09(3) . . ?
C16 N1 H1 107.8 . . ?
C16 N1 C15 113.1(8) . . ?
C16 N1 C17 108.9(9) . . ?
C15 N1 H1 107.8 . . ?
C17 N1 H1 107.8 . . ?
C17 N1 C15 111.3(9) . . ?
C20 N2 H2 107.8 . . ?
C18 N2 H2 107.8 . . ?
C18 N2 C20 111.9(7) . . ?
C19 N2 H2 107.8 . . ?
C19 N2 C20 110.7(8) . . ?
C19 N2 C18 110.5(8) . . ?
N2 C20 H20A 109.2 . . ?
N2 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C27 C20 N2 112.2(7) . . ?
C27 C20 H20A 109.2 . . ?
C27 C20 H20B 109.2 . . ?
C27 C24 C23 122.7(8) . . ?
C27 C24 C25 120.7(8) . . ?
C25 C24 C23 116.7(8) . . ?
C8 C7 C15 118.6(8) . . ?
C4 C7 C15 120.6(9) . . ?
C4 C7 C8 120.8(9) . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C24 C23 H23 119.0 . . ?
C22 C23 C24 122.0(9) . . ?
C22 C23 H23 119.0 . . ?
C24 C27 C20 121.4(8) . . ?
C24 C27 C28 120.0(8) . . ?
C28 C27 C20 118.6(8) . . ?
C37A O1A H1AA 109.5 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C27 C28 C31 122.1(8) . . ?
C27 C28 C29 119.6(8) . . ?
C31 C28 C29 118.3(8) . . ?
C24 C25 C26 119.0(9) . . ?
C30 C25 C24 118.0(8) . . ?
C30 C25 C26 123.0(9) . . ?
C25 C30 Cl2 118.5(8) . . ?
C29 C30 Cl2 118.8(8) . . ?
C29 C30 C25 122.6(9) . . ?
N1 C15 C7 113.4(8) . . ?
N1 C15 H15A 108.9 . . ?
N1 C15 H15B 108.9 . . ?
C7 C15 H15A 108.9 . . ?
C7 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C23 C22 H22 119.9 . . ?
C23 C22 C21 120.1(10) . . ?
C21 C22 H22 119.9 . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C7 C8 C9 119.7(9) . . ?
C7 C8 C11 123.7(9) . . ?
C9 C8 C11 116.6(8) . . ?
C10 C5 C4 118.3(10) . . ?
C10 C5 C6 122.9(11) . . ?
C6 C5 C4 118.8(10) . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C28 C31 H31 119.3 . . ?
C32 C31 C28 121.4(10) . . ?
C32 C31 H31 119.3 . . ?
C7 C4 C5 119.6(10) . . ?
C7 C4 C3 123.4(10) . . ?
C3 C4 C5 117.0(11) . . ?
C10 C9 C8 117.9(9) . . ?
C10 C9 C14 122.8(10) . . ?
C14 C9 C8 119.3(10) . . ?
C31 C32 H32 120.0 . . ?
C31 C32 C33 120.0(11) . . ?
C33 C32 H32 120.0 . . ?
C5 C10 Cl1 117.8(9) . . ?
C9 C10 Cl1 118.5(8) . . ?
C9 C10 C5 123.7(10) . . ?
C8 C11 H11 119.4 . . ?
C12 C11 C8 121.3(10) . . ?
C12 C11 H11 119.4 . . ?
C22 C21 H21 119.4 . . ?
C26 C21 C22 121.2(10) . . ?
C26 C21 H21 119.4 . . ?
C28 C29 C34 117.8(9) . . ?
C30 C29 C28 119.1(8) . . ?
C30 C29 C34 123.1(10) . . ?
C25 C26 H26 119.5 . . ?
C21 C26 C25 121.0(10) . . ?
C21 C26 H26 119.5 . . ?
C4 C3 H3 118.5 . . ?
C2 C3 C4 123.0(11) . . ?
C2 C3 H3 118.5 . . ?
C32 C33 H33 119.6 . . ?
C34 C33 C32 120.8(11) . . ?
C34 C33 H33 119.6 . . ?
C9 C14 H14 119.9 . . ?
C13 C14 C9 120.2(10) . . ?
C13 C14 H14 119.9 . . ?
C11 C12 H12 119.4 . . ?
C11 C12 C13 121.2(11) . . ?
C13 C12 H12 119.4 . . ?
C5 C6 H6 119.2 . . ?
C1 C6 C5 121.7(11) . . ?
C1 C6 H6 119.2 . . ?
C14 C13 C12 121.4(10) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C29 C34 H34 119.2 . . ?
C33 C34 C29 121.6(11) . . ?
C33 C34 H34 119.2 . . ?
O1A C37A H37A 109.4 . . ?
O1A C37A H37B 109.4 . . ?
O1A C37A C36A 111(4) . . ?
H37A C37A H37B 108.0 . . ?
C36A C37A H37A 109.4 . . ?
C36A C37A H37B 109.4 . . ?
H35A C35A H35B 109.5 . . ?
H35A C35A H35C 109.5 . . ?
H35B C35A H35C 109.5 . . ?
C36A C35A H35A 109.5 . . ?
C36A C35A H35B 109.5 . . ?
C36A C35A H35C 109.5 . . ?
C37A C36A H36A 109.2 . . ?
C37A C36A H36B 109.2 . . ?
C35A C36A C37A 112(3) . . ?
C35A C36A H36A 109.2 . . ?
C35A C36A H36B 109.2 . . ?
H36A C36A H36B 107.9 . . ?
C3 C2 H2A 119.8 . . ?
C3 C2 C1 120.5(11) . . ?
C1 C2 H2A 119.8 . . ?
C6 C1 C2 119.0(11) . . ?
C6 C1 H1A 120.5 . . ?
C2 C1 H1A 120.5 . . ?
C37B O1B H1B 135.8 . . ?
H35D C35B H35E 109.5 . . ?
H35D C35B H35F 109.5 . . ?
H35E C35B H35F 109.5 . . ?
C36B C35B H35D 109.5 . . ?
C36B C35B H35E 109.5 . . ?
C36B C35B H35F 109.5 . . ?
C35B C36B H36C 109.0 . . ?
C35B C36B H36D 109.0 . . ?
H36C C36B H36D 107.8 . . ?
C37B C36B C35B 113.0(19) . . ?
C37B C36B H36C 109.0 . . ?
C37B C36B H36D 109.0 . . ?
O1B C37B C36B 99(4) . . ?
O1B C37B H37C 112.0 . . ?
O1B C37B H37D 112.0 . . ?
C36B C37B H37C 112.0 . . ?
C36B C37B H37D 112.0 . . ?
H37C C37B H37D 109.7 . . ?

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
Cl2 C30 C29 C28 -178.4(8) . . . . ?
Cl2 C30 C29 C34 0.1(17) . . . . ?
N2 C20 C27 C24 -98.8(10) . . . . ?
N2 C20 C27 C28 83.5(10) . . . . ?
C20 C27 C28 C31 0.9(14) . . . . ?
C20 C27 C28 C29 178.6(9) . . . . ?
C24 C23 C22 C21 0.0(19) . . . . ?
C24 C27 C28 C31 -176.8(9) . . . . ?
C24 C27 C28 C29 0.9(14) . . . . ?
C24 C25 C30 Cl2 179.8(8) . . . . ?
C24 C25 C30 C29 0.3(16) . . . . ?
C24 C25 C26 C21 1.7(18) . . . . ?
C7 C8 C9 C10 -0.7(15) . . . . ?
C7 C8 C9 C14 180.0(10) . . . . ?
C7 C8 C11 C12 -179.7(11) . . . . ?
C7 C4 C3 C2 -179.1(14) . . . . ?
C18 N2 C20 C27 80.0(9) . . . . ?
C23 C24 C27 C20 2.5(14) . . . . ?
C23 C24 C27 C28 -179.9(9) . . . . ?
C23 C24 C25 C30 179.2(9) . . . . ?
C23 C24 C25 C26 -0.7(14) . . . . ?
C23 C22 C21 C26 1(2) . . . . ?
C27 C24 C23 C22 -179.7(10) . . . . ?
C27 C24 C25 C30 -1.1(14) . . . . ?
C27 C24 C25 C26 178.9(10) . . . . ?
C27 C28 C31 C32 178.5(11) . . . . ?
C27 C28 C29 C30 -1.7(15) . . . . ?
C27 C28 C29 C34 179.6(10) . . . . ?
O1A C37A C36A C35A 96(5) . . . . ?
C16 N1 C15 C7 -74.5(11) . . . . ?
C28 C31 C32 C33 1.7(19) . . . . ?
C28 C29 C34 C33 2(2) . . . . ?
C25 C24 C23 C22 -0.1(15) . . . . ?
C25 C24 C27 C20 -177.1(8) . . . . ?
C25 C24 C27 C28 0.5(14) . . . . ?
C25 C30 C29 C28 1.1(17) . . . . ?
C25 C30 C29 C34 179.7(12) . . . . ?
C30 C25 C26 C21 -178.2(12) . . . . ?
C30 C29 C34 C33 -176.6(14) . . . . ?
C15 C7 C8 C9 -179.5(9) . . . . ?
C15 C7 C8 C11 -0.2(15) . . . . ?
C15 C7 C4 C5 -179.4(12) . . . . ?
C15 C7 C4 C3 1(2) . . . . ?
C22 C21 C26 C25 -2(2) . . . . ?
C19 N2 C20 C27 -156.2(8) . . . . ?
C8 C7 C15 N1 -82.3(11) . . . . ?
C8 C7 C4 C5 1(2) . . . . ?
C8 C7 C4 C3 -178.6(13) . . . . ?
C8 C9 C10 Cl1 -178.3(8) . . . . ?
C8 C9 C10 C5 0.2(19) . . . . ?
C8 C9 C14 C13 -0.8(19) . . . . ?
C8 C11 C12 C13 0(2) . . . . ?
C5 C4 C3 C2 1(2) . . . . ?
C5 C6 C1 C2 0(2) . . . . ?
C17 N1 C15 C7 162.4(9) . . . . ?
C31 C28 C29 C30 176.1(10) . . . . ?
C31 C28 C29 C34 -2.5(15) . . . . ?
C31 C32 C33 C34 -2(2) . . . . ?
C4 C7 C15 N1 98.2(12) . . . . ?
C4 C7 C8 C9 0.1(16) . . . . ?
C4 C7 C8 C11 179.4(11) . . . . ?
C4 C5 C10 Cl1 179.3(12) . . . . ?
C4 C5 C10 C9 1(2) . . . . ?
C4 C5 C6 C1 2(2) . . . . ?
C4 C3 C2 C1 1(3) . . . . ?
C9 C8 C11 C12 -0.3(16) . . . . ?
C9 C14 C13 C12 1(2) . . . . ?
C32 C33 C34 C29 0(2) . . . . ?
C10 C5 C4 C7 -1(2) . . . . ?
C10 C5 C4 C3 178.2(14) . . . . ?
C10 C5 C6 C1 -178.8(15) . . . . ?
C10 C9 C14 C13 179.9(13) . . . . ?
C11 C8 C9 C10 179.9(10) . . . . ?
C11 C8 C9 C14 0.6(15) . . . . ?
C11 C12 C13 C14 0(2) . . . . ?
C29 C28 C31 C32 0.7(16) . . . . ?
C26 C25 C30 Cl2 -0.2(16) . . . . ?
C26 C25 C30 C29 -179.7(11) . . . . ?
C3 C2 C1 C6 -2(2) . . . . ?
C14 C9 C10 Cl1 1.0(17) . . . . ?
C14 C9 C10 C5 179.5(13) . . . . ?
C6 C5 C4 C7 177.5(14) . . . . ?
C6 C5 C4 C3 -3(2) . . . . ?
C6 C5 C10 Cl1 0(2) . . . . ?
C6 C5 C10 C9 -178.1(13) . . . . ?
C35B C36B C37B O1B -167(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.664
_oxdiff_exptl_absorpt_empirical_full_min 0.664
####################################################################### 
# 
# 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_1-C4
_database_code_depnum_ccdc_archive 'CCDC 2240930'
loop_
_audit_author_name
_audit_author_address
'Binbin Luo'
;Shantou University
China
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
_audit_creation_date             2023-01-08
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br10 Pb3, 4(C17 H17 Cl N), 2(C4 H10 O)'
_chemical_formula_sum            'C76 H88 Br10 Cl4 N4 O2 Pb3'
_chemical_formula_weight         2651.97
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O Pb Cl Br'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.4718(2)
_cell_length_b                   9.80050(10)
_cell_length_c                   40.8581(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.2310(10)
_cell_angle_gamma                90
_cell_volume                     8591.43(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14668
_cell_measurement_temperature    296.42(12)
_cell_measurement_theta_max      70.7120
_cell_measurement_theta_min      4.3100
_shelx_estimated_absorpt_T_max   0.839
_shelx_estimated_absorpt_T_min   0.122
_exptl_absorpt_coefficient_mu    18.183
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (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    2.050
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5008
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.2
_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  0.0233
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            21132
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.000
_diffrn_reflns_theta_min         4.332
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.42(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  23.00   0.50    1.29    --    0.00  77.00 -90.00  106
  2  ω     56.00  82.00   0.50    1.29    --    0.00  77.00 -90.00   52
  3  ω     47.00  73.00   0.50    1.29    --    0.00  77.00-180.00   52
  4  ω    -30.00  16.00   0.50    1.29    --    0.00  77.00-180.00   92
  5  ω     15.00 117.00   0.50    5.15    --   89.30 -15.00 -30.00  204
  6  ω     61.00 103.00   0.50    5.15    --   89.30  77.00 120.00   84
  7  ω      3.00 107.00   0.50    5.15    --   89.30 -30.00 -90.00  208
  8  ω     32.00 113.00   0.50    5.15    --   89.30 -82.00  60.00  162
  9  ω     15.00 107.00   0.50    5.15    --   89.30 -61.00 150.00  184
 10  ω     62.00 113.00   0.50    5.15    --   89.30 -82.00 150.00  102
 11  ω      5.00  45.00   0.50    5.15    --   89.30 -82.00 150.00   80
;
_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      0.0565988000
_diffrn_orient_matrix_UB_12      0.0130906000
_diffrn_orient_matrix_UB_13      0.0241458000
_diffrn_orient_matrix_UB_21      -0.0439881000
_diffrn_orient_matrix_UB_22      0.0011684000
_diffrn_orient_matrix_UB_23      0.0288952000
_diffrn_orient_matrix_UB_31      0.0044117000
_diffrn_orient_matrix_UB_32      -0.1566580000
_diffrn_orient_matrix_UB_33      0.0022364000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7445
_reflns_number_total             8025
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.697
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8025
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0247
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0234P)²+24.6644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0601
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O1B-C38B
 1.44 with sigma of 0.02
 C38A-O1A
 1.44 with sigma of 0.02
 C37A-C36A = C37A-C38A
 1.54 with sigma of 0.02
 C35A-C37A
 2.56 with sigma of 0.02
 C36B-C38B
 2.56 with sigma of 0.02
 C35B-C37B
 2.56 with sigma of 0.02
 C36A-C38A
 2.56 with sigma of 0.02
 C35A-C36A \\sim C37A-C38A
 with sigma of 0.02
 C35B-C36B \\sim C37B-C38B
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C38B \\sim C35B \\sim C36B \\sim C37B: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
C38A \\sim C37A \\sim C36A \\sim C35A: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Uanis(C35A) \\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(C37A) \\sim Ueq,
Uanis(C38A) \\sim Ueq, Uanis(O1A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O1B) \\sim Ueq, Uanis(C38B) \\sim Ueq, Uanis(C37B) \\sim Ueq, Uanis(C36B)
\\sim Ueq, Uanis(C35B) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
3. Others
 Fixed Sof: O1A(0.5) H1AA(0.5) C38A(0.5) H38A(0.5) H38B(0.5) C36A(0.5)
 H36A(0.5) H36B(0.5) C37A(0.5) H37A(0.5) H37B(0.5) C35B(0.5) H35D(0.5)
 H35E(0.5) H35F(0.5) C37B(0.5) H37C(0.5) H37D(0.5) C36B(0.5) H36C(0.5)
 H36D(0.5) O1B(0.5) H1BA(0.5) C38B(0.5) H38C(0.5) H38D(0.5) C35A(0.5) H35A(0.5)
 H35B(0.5) H35C(0.5)
4.a Ternary CH refined with riding coordinates:
 N2(H2), N1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C20(H20A,H20B), C38A(H38A,H38B), C36A(H36A,H36B), C37A(H37A,
 H37B), C37B(H37C,H37D), C36B(H36C,H36D), C38B(H38C,H38D)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C24(H24), C7(H7), C6(H6), C21(H21), C5(H5), C31(H31), C15(H15),
 C23(H23), C22(H22), C4(H4), C34(H34), C17(H17), C32(H32), C16(H16), C33(H33)
4.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C19(H19A,H19B,H19C), C1(H1A,H1B,H1C), C18(H18A,H18B,H18C),
 C35B(H35D,H35E,H35F), C35A(H35A,H35B,H35C)
4.e Idealised tetrahedral OH refined as rotating group:
 O1A(H1AA), O1B(H1BA)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.82461(2) -0.30051(2) 0.77204(2) 0.03358(5) Uani 1 1 d . . . . .
Pb2 Pb 1.000000 -0.30549(2) 0.750000 0.03616(6) Uani 1 2 d S T P . .
Br4 Br 0.88500(2) -0.28734(4) 0.70579(2) 0.04539(10) Uani 1 1 d . . . . .
Br2 Br 0.75324(2) -0.05684(4) 0.74832(2) 0.04734(10) Uani 1 1 d . . . . .
Br5 Br 1.07081(2) -0.52097(4) 0.71563(2) 0.04896(11) Uani 1 1 d . . . . .
Br1 Br 0.75262(2) -0.31806(5) 0.83353(2) 0.04954(11) Uani 1 1 d . . . . .
Br3 Br 0.92988(2) -0.11868(5) 0.79779(2) 0.06064(13) Uani 1 1 d . . . . .
Cl1 Cl 0.90671(7) 0.23026(13) 0.52774(3) 0.0684(3) Uani 1 1 d . . . . .
Cl2 Cl 1.07738(7) 0.27468(14) 0.49617(3) 0.0704(4) Uani 1 1 d . . . . .
N2 N 1.18596(15) 0.2082(3) 0.65361(7) 0.0378(7) Uani 1 1 d . . . . .
H2 H 1.191237 0.124082 0.641061 0.045 Uiso 1 1 calc R U . . .
N1 N 0.89633(15) 0.2028(3) 0.69387(7) 0.0385(7) Uani 1 1 d . . . . .
H1 H 0.861377 0.160019 0.681613 0.046 Uiso 1 1 calc R U . . .
O1A O 0.7286(5) 0.4653(10) 0.6246(2) 0.058(2) Uani 0.5 1 d D U P A 1
H1AA H 0.735390 0.437729 0.643306 0.087 Uiso 0.5 1 calc R U P A 1
C10 C 0.94106(17) 0.1996(3) 0.63770(8) 0.0330(7) Uani 1 1 d . . . . .
C3 C 0.95419(17) 0.1841(4) 0.67411(9) 0.0363(8) Uani 1 1 d . . . . .
H3A H 0.985227 0.250788 0.681217 0.044 Uiso 1 1 calc R U . . .
H3B H 0.971400 0.094068 0.678443 0.044 Uiso 1 1 calc R U . . .
C27 C 1.11324(17) 0.2723(4) 0.60653(9) 0.0346(8) Uani 1 1 d . . . . .
C13 C 0.9189(2) 0.2197(4) 0.56996(9) 0.0422(9) Uani 1 1 d . . . . .
C8 C 0.91770(17) 0.0861(4) 0.62011(9) 0.0357(8) Uani 1 1 d . . . . .
C25 C 1.09125(16) 0.1537(4) 0.59042(9) 0.0342(7) Uani 1 1 d . . . . .
C11 C 0.95333(16) 0.3232(4) 0.62170(9) 0.0331(7) Uani 1 1 d . . . . .
C12 C 0.94235(18) 0.3334(4) 0.58678(9) 0.0372(8) Uani 1 1 d . . . . .
C14 C 0.97703(18) 0.4417(4) 0.63820(10) 0.0421(9) Uani 1 1 d . . . . .
H14 H 0.984938 0.438105 0.660721 0.050 Uiso 1 1 calc R U . . .
C2 C 0.8811(2) 0.3509(5) 0.69782(12) 0.0533(11) Uani 1 1 d . . . . .
H2A H 0.915716 0.396641 0.708566 0.080 Uiso 1 1 calc R U . . .
H2B H 0.844946 0.359883 0.710771 0.080 Uiso 1 1 calc R U . . .
H2C H 0.872804 0.390980 0.676664 0.080 Uiso 1 1 calc R U . . .
C19 C 1.2394(2) 0.2996(5) 0.64696(14) 0.0609(13) Uani 1 1 d . . . . .
H19A H 1.240178 0.317778 0.623886 0.091 Uiso 1 1 calc R U . . .
H19B H 1.277652 0.256074 0.654078 0.091 Uiso 1 1 calc R U . . .
H19C H 1.234926 0.383862 0.658611 0.091 Uiso 1 1 calc R U . . .
C26 C 1.07958(18) 0.1542(4) 0.55574(9) 0.0384(8) Uani 1 1 d . . . . .
C24 C 1.07938(18) 0.0288(4) 0.60749(10) 0.0438(9) Uani 1 1 d . . . . .
H24 H 1.086389 0.025150 0.630080 0.053 Uiso 1 1 calc R U . . .
C7 C 0.9067(2) -0.0428(4) 0.63499(10) 0.0475(10) Uani 1 1 d . . . . .
H7 H 0.914212 -0.052621 0.657436 0.057 Uiso 1 1 calc R U . . .
C9 C 0.90585(19) 0.0959(4) 0.58529(9) 0.0409(8) Uani 1 1 d . . . . .
C20 C 1.12415(18) 0.2692(4) 0.64316(9) 0.0383(8) Uani 1 1 d . . . . .
H20A H 1.121967 0.361589 0.651558 0.046 Uiso 1 1 calc R U . . .
H20B H 1.091171 0.216793 0.652763 0.046 Uiso 1 1 calc R U . . .
C28 C 1.12360(18) 0.3922(4) 0.58861(9) 0.0382(8) Uani 1 1 d . . . . .
C29 C 1.11265(19) 0.3925(4) 0.55361(9) 0.0422(9) Uani 1 1 d . . . . .
C1 C 0.9032(3) 0.1326(6) 0.72621(11) 0.0688(14) Uani 1 1 d . . . . .
H1A H 0.908300 0.036340 0.722833 0.103 Uiso 1 1 calc R U . . .
H1B H 0.866614 0.148298 0.738467 0.103 Uiso 1 1 calc R U . . .
H1C H 0.939050 0.167881 0.738155 0.103 Uiso 1 1 calc R U . . .
C30 C 1.09074(19) 0.2733(4) 0.53864(9) 0.0415(9) Uani 1 1 d . . . . .
C18 C 1.1867(3) 0.1709(5) 0.68913(11) 0.0666(14) Uani 1 1 d . . . . .
H18A H 1.226041 0.129842 0.695292 0.100 Uiso 1 1 calc R U . . .
H18B H 1.153718 0.107407 0.692883 0.100 Uiso 1 1 calc R U . . .
H18C H 1.180900 0.251536 0.701996 0.100 Uiso 1 1 calc R U . . .
C6 C 0.8857(2) -0.1515(4) 0.61727(12) 0.0580(12) Uani 1 1 d . . . . .
H6 H 0.879909 -0.234796 0.627609 0.070 Uiso 1 1 calc R U . . .
C21 C 1.0576(2) 0.0321(4) 0.54005(11) 0.0504(10) Uani 1 1 d . . . . .
H21 H 1.050202 0.031445 0.517466 0.060 Uiso 1 1 calc R U . . .
C5 C 0.8726(3) -0.1395(5) 0.58370(12) 0.0650(14) Uani 1 1 d . . . . .
H5 H 0.857154 -0.214346 0.571976 0.078 Uiso 1 1 calc R U . . .
C31 C 1.1454(2) 0.5163(4) 0.60332(11) 0.0516(11) Uani 1 1 d . . . . .
H31 H 1.152042 0.519583 0.625928 0.062 Uiso 1 1 calc R U . . .
C15 C 0.9884(2) 0.5593(4) 0.62210(12) 0.0543(11) Uani 1 1 d . . . . .
H15 H 1.003479 0.634959 0.633632 0.065 Uiso 1 1 calc R U . . .
C23 C 1.0583(2) -0.0833(5) 0.59149(13) 0.0585(12) Uani 1 1 d . . . . .
H23 H 1.050953 -0.162808 0.603132 0.070 Uiso 1 1 calc R U . . .
C22 C 1.0474(2) -0.0811(5) 0.55727(12) 0.0588(12) Uani 1 1 d . . . . .
H22 H 1.032963 -0.159300 0.546553 0.071 Uiso 1 1 calc R U . . .
C4 C 0.8821(2) -0.0201(5) 0.56799(11) 0.0569(11) Uani 1 1 d . . . . .
H4 H 0.872952 -0.013779 0.545603 0.068 Uiso 1 1 calc R U . . .
C34 C 1.1244(2) 0.5148(5) 0.53597(11) 0.0590(12) Uani 1 1 d . . . . .
H34 H 1.117592 0.515958 0.513360 0.071 Uiso 1 1 calc R U . . .
C17 C 0.9556(2) 0.4592(4) 0.57098(11) 0.0499(10) Uani 1 1 d . . . . .
H17 H 0.948972 0.466382 0.548417 0.060 Uiso 1 1 calc R U . . .
C32 C 1.1565(3) 0.6288(5) 0.58554(13) 0.0676(14) Uani 1 1 d . . . . .
H32 H 1.171726 0.707246 0.595863 0.081 Uiso 1 1 calc R U . . .
C16 C 0.9774(2) 0.5674(5) 0.58789(12) 0.0580(12) Uani 1 1 d . . . . .
H16 H 0.985282 0.648530 0.576984 0.070 Uiso 1 1 calc R U . . .
C33 C 1.1452(3) 0.6279(5) 0.55121(14) 0.0736(16) Uani 1 1 d . . . . .
H33 H 1.152134 0.706524 0.539124 0.088 Uiso 1 1 calc R U . . .
C38A C 0.7857(8) 0.466(4) 0.6075(4) 0.113(3) Uani 0.5 1 d D U P A 1
H38A H 0.805128 0.377345 0.605395 0.135 Uiso 0.5 1 calc R U P A 1
H38B H 0.815503 0.534814 0.614972 0.135 Uiso 0.5 1 calc R U P A 1
C36A C 0.7381(9) 0.4546(16) 0.5488(3) 0.114(3) Uani 0.5 1 d D U P A 1
H36A H 0.701444 0.396690 0.547131 0.136 Uiso 0.5 1 calc R U P A 1
H36B H 0.774581 0.397393 0.546637 0.136 Uiso 0.5 1 calc R U P A 1
C37A C 0.7406(8) 0.5124(17) 0.5756(3) 0.113(3) Uani 0.5 1 d D U P A 1
H37A H 0.698345 0.512768 0.583139 0.136 Uiso 0.5 1 calc R U P A 1
H37B H 0.750997 0.606769 0.571162 0.136 Uiso 0.5 1 calc R U P A 1
C35B C 0.7305(8) 0.5012(18) 0.5158(4) 0.112(3) Uani 0.5 1 d D U P B 2
H35D H 0.746808 0.546201 0.497067 0.167 Uiso 0.5 1 calc R U P B 2
H35E H 0.693349 0.547192 0.522128 0.167 Uiso 0.5 1 calc R U P B 2
H35F H 0.720696 0.408201 0.510260 0.167 Uiso 0.5 1 calc R U P B 2
C37B C 0.7780(8) 0.5262(17) 0.5744(4) 0.111(3) Uani 0.5 1 d D U P B 2
H37C H 0.815002 0.582814 0.576465 0.133 Uiso 0.5 1 calc R U P B 2
H37D H 0.743647 0.588450 0.577545 0.133 Uiso 0.5 1 calc R U P B 2
C36B C 0.7733(8) 0.5041(18) 0.5408(4) 0.111(3) Uani 0.5 1 d D U P B 2
H36C H 0.803550 0.568471 0.532849 0.133 Uiso 0.5 1 calc R U P B 2
H36D H 0.793043 0.415587 0.538826 0.133 Uiso 0.5 1 calc R U P B 2
O1B O 0.7454(4) 0.4839(10) 0.6316(3) 0.065(3) Uani 0.5 1 d D U P B 2
H1BA H 0.727940 0.413396 0.636912 0.098 Uiso 0.5 1 calc R U P B 2
C38B C 0.7806(10) 0.459(3) 0.6028(4) 0.110(3) Uani 0.5 1 d D U P B 2
H38C H 0.823951 0.462791 0.610287 0.132 Uiso 0.5 1 calc R U P B 2
H38D H 0.772409 0.364421 0.597091 0.132 Uiso 0.5 1 calc R U P B 2
C35A C 0.7347(9) 0.5773(17) 0.5169(4) 0.115(3) Uani 0.5 1 d D U P A 1
H35A H 0.756905 0.543909 0.498602 0.172 Uiso 0.5 1 calc R U P A 1
H35B H 0.753369 0.660892 0.524632 0.172 Uiso 0.5 1 calc R U P A 1
H35C H 0.691987 0.593625 0.510229 0.172 Uiso 0.5 1 calc R U P A 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 Br4 3.0492(4) . ?
Pb1 Br2 3.1127(4) 4_646 ?
Pb1 Br2 2.9791(4) . ?
Pb1 Br5 3.1428(5) 2_756 ?
Pb1 Br1 3.0056(5) . ?
Pb1 Br3 3.0342(5) . ?
Pb2 Br4 3.0073(4) . ?
Pb2 Br4 3.0074(4) 2_756 ?
Pb2 Br5 2.9848(4) 2_756 ?
Pb2 Br5 2.9848(4) . ?
Pb2 Br3 3.1083(5) . ?
Pb2 Br3 3.1082(5) 2_756 ?
Cl1 C13 1.738(4) . ?
Cl2 C30 1.748(4) . ?
N2 H2 0.9800 . ?
N2 C19 1.489(5) . ?
N2 C20 1.502(5) . ?
N2 C18 1.496(5) . ?
N1 H1 0.9800 . ?
N1 C3 1.519(5) . ?
N1 C2 1.498(5) . ?
N1 C1 1.492(5) . ?
O1A H1AA 0.8200 . ?
O1A C38A 1.433(16) . ?
C10 C3 1.511(5) . ?
C10 C8 1.406(5) . ?
C10 C11 1.406(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C27 C25 1.408(5) . ?
C27 C20 1.506(5) . ?
C27 C28 1.407(5) . ?
C13 C12 1.393(5) . ?
C13 C9 1.399(5) . ?
C8 C7 1.425(5) . ?
C8 C9 1.439(5) . ?
C25 C26 1.430(5) . ?
C25 C24 1.437(5) . ?
C11 C12 1.441(5) . ?
C11 C14 1.427(5) . ?
C12 C17 1.426(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.353(6) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C26 C30 1.386(6) . ?
C26 C21 1.429(5) . ?
C24 H24 0.9300 . ?
C24 C23 1.347(6) . ?
C7 H7 0.9300 . ?
C7 C6 1.355(6) . ?
C9 C4 1.422(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C28 C29 1.440(5) . ?
C28 C31 1.427(5) . ?
C29 C30 1.392(5) . ?
C29 C34 1.426(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C6 H6 0.9300 . ?
C6 C5 1.394(7) . ?
C21 H21 0.9300 . ?
C21 C22 1.336(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.354(7) . ?
C31 H31 0.9300 . ?
C31 C32 1.347(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.411(6) . ?
C23 H23 0.9300 . ?
C23 C22 1.409(7) . ?
C22 H22 0.9300 . ?
C4 H4 0.9300 . ?
C34 H34 0.9300 . ?
C34 C33 1.339(7) . ?
C17 H17 0.9300 . ?
C17 C16 1.340(6) . ?
C32 H32 0.9300 . ?
C32 C33 1.414(7) . ?
C16 H16 0.9300 . ?
C33 H33 0.9300 . ?
C38A H38A 0.9700 . ?
C38A H38B 0.9700 . ?
C38A C37A 1.657(15) . ?
C36A H36A 0.9700 . ?
C36A H36B 0.9700 . ?
C36A C37A 1.233(14) . ?
C36A C35A 1.771(17) . ?
C37A H37A 0.9700 . ?
C37A H37B 0.9700 . ?
C35B H35D 0.9600 . ?
C35B H35E 0.9600 . ?
C35B H35F 0.9600 . ?
C35B C36B 1.350(17) . ?
C37B H37C 0.9700 . ?
C37B H37D 0.9700 . ?
C37B C36B 1.391(18) . ?
C37B C38B 1.332(19) . ?
C36B H36C 0.9700 . ?
C36B H36D 0.9700 . ?
O1B H1BA 0.8200 . ?
O1B C38B 1.443(15) . ?
C38B H38C 0.9700 . ?
C38B H38D 0.9700 . ?
C35A H35A 0.9600 . ?
C35A H35B 0.9600 . ?
C35A H35C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br4 Pb1 Br2 92.261(12) . 4_646 ?
Br4 Pb1 Br5 81.111(12) . 2_756 ?
Br2 Pb1 Br4 84.746(12) . . ?
Br2 Pb1 Br2 107.212(5) . 4_646 ?
Br2 Pb1 Br5 82.004(12) 4_646 2_756 ?
Br2 Pb1 Br5 163.448(13) . 2_756 ?
Br2 Pb1 Br1 92.466(12) . . ?
Br2 Pb1 Br3 90.509(14) . . ?
Br1 Pb1 Br4 174.133(13) . . ?
Br1 Pb1 Br2 83.619(13) . 4_646 ?
Br1 Pb1 Br5 102.370(12) . 2_756 ?
Br1 Pb1 Br3 98.286(14) . . ?
Br3 Pb1 Br4 86.918(14) . . ?
Br3 Pb1 Br2 162.123(13) . 4_646 ?
Br3 Pb1 Br5 80.225(13) . 2_756 ?
Br4 Pb2 Br4 173.217(18) . 2_756 ?
Br4 Pb2 Br3 86.331(13) 2_756 2_756 ?
Br4 Pb2 Br3 89.672(12) 2_756 . ?
Br4 Pb2 Br3 86.331(12) . . ?
Br4 Pb2 Br3 89.675(12) . 2_756 ?
Br5 Pb2 Br4 100.406(12) 2_756 2_756 ?
Br5 Pb2 Br4 100.408(12) . . ?
Br5 Pb2 Br4 84.438(11) . 2_756 ?
Br5 Pb2 Br4 84.438(12) 2_756 . ?
Br5 Pb2 Br5 89.93(2) . 2_756 ?
Br5 Pb2 Br3 168.627(15) . . ?
Br5 Pb2 Br3 81.555(14) 2_756 . ?
Br5 Pb2 Br3 168.628(15) 2_756 2_756 ?
Br5 Pb2 Br3 81.555(14) . 2_756 ?
Br3 Pb2 Br3 107.82(2) 2_756 . ?
Pb2 Br4 Pb1 80.325(10) . . ?
Pb1 Br2 Pb1 176.367(17) . 4_656 ?
Pb2 Br5 Pb1 79.166(10) . 2_756 ?
Pb1 Br3 Pb2 78.971(11) . . ?
C19 N2 H2 107.7 . . ?
C19 N2 C20 112.8(3) . . ?
C19 N2 C18 110.2(4) . . ?
C20 N2 H2 107.7 . . ?
C18 N2 H2 107.7 . . ?
C18 N2 C20 110.4(3) . . ?
C3 N1 H1 107.6 . . ?
C2 N1 H1 107.6 . . ?
C2 N1 C3 111.2(3) . . ?
C1 N1 H1 107.6 . . ?
C1 N1 C3 111.1(3) . . ?
C1 N1 C2 111.5(4) . . ?
C38A O1A H1AA 109.5 . . ?
C8 C10 C3 118.2(3) . . ?
C11 C10 C3 120.9(3) . . ?
C11 C10 C8 120.9(3) . . ?
N1 C3 H3A 109.0 . . ?
N1 C3 H3B 109.0 . . ?
C10 C3 N1 112.7(3) . . ?
C10 C3 H3A 109.0 . . ?
C10 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C25 C27 C20 119.0(3) . . ?
C28 C27 C25 120.2(3) . . ?
C28 C27 C20 120.8(3) . . ?
C12 C13 Cl1 118.7(3) . . ?
C12 C13 C9 123.2(3) . . ?
C9 C13 Cl1 118.1(3) . . ?
C10 C8 C7 123.0(3) . . ?
C10 C8 C9 119.9(3) . . ?
C7 C8 C9 117.1(3) . . ?
C27 C25 C26 120.2(3) . . ?
C27 C25 C24 122.6(3) . . ?
C26 C25 C24 117.2(3) . . ?
C10 C11 C12 119.6(3) . . ?
C10 C11 C14 123.5(3) . . ?
C14 C11 C12 116.9(3) . . ?
C13 C12 C11 118.4(3) . . ?
C13 C12 C17 122.9(4) . . ?
C17 C12 C11 118.7(4) . . ?
C11 C14 H14 119.0 . . ?
C15 C14 C11 122.1(4) . . ?
C15 C14 H14 119.0 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C30 C26 C25 118.4(3) . . ?
C30 C26 C21 122.7(4) . . ?
C21 C26 C25 119.0(4) . . ?
C25 C24 H24 119.3 . . ?
C23 C24 C25 121.4(4) . . ?
C23 C24 H24 119.3 . . ?
C8 C7 H7 119.1 . . ?
C6 C7 C8 121.7(4) . . ?
C6 C7 H7 119.1 . . ?
C13 C9 C8 118.0(3) . . ?
C13 C9 C4 123.0(4) . . ?
C4 C9 C8 119.0(4) . . ?
N2 C20 C27 113.1(3) . . ?
N2 C20 H20A 109.0 . . ?
N2 C20 H20B 109.0 . . ?
C27 C20 H20A 109.0 . . ?
C27 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C27 C28 C29 119.7(3) . . ?
C27 C28 C31 123.3(3) . . ?
C31 C28 C29 117.0(4) . . ?
C30 C29 C28 118.3(4) . . ?
C30 C29 C34 123.2(4) . . ?
C34 C29 C28 118.5(4) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C26 C30 Cl2 118.8(3) . . ?
C26 C30 C29 123.2(3) . . ?
C29 C30 Cl2 118.0(3) . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C7 C6 H6 119.7 . . ?
C7 C6 C5 120.6(4) . . ?
C5 C6 H6 119.7 . . ?
C26 C21 H21 119.4 . . ?
C22 C21 C26 121.1(4) . . ?
C22 C21 H21 119.4 . . ?
C6 C5 H5 119.6 . . ?
C4 C5 C6 120.7(4) . . ?
C4 C5 H5 119.6 . . ?
C28 C31 H31 118.9 . . ?
C32 C31 C28 122.2(4) . . ?
C32 C31 H31 118.9 . . ?
C14 C15 H15 119.9 . . ?
C14 C15 C16 120.2(4) . . ?
C16 C15 H15 119.9 . . ?
C24 C23 H23 119.7 . . ?
C24 C23 C22 120.6(4) . . ?
C22 C23 H23 119.7 . . ?
C21 C22 C23 120.7(4) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C9 C4 H4 119.6 . . ?
C5 C4 C9 120.9(4) . . ?
C5 C4 H4 119.6 . . ?
C29 C34 H34 119.2 . . ?
C33 C34 C29 121.6(4) . . ?
C33 C34 H34 119.2 . . ?
C12 C17 H17 119.2 . . ?
C16 C17 C12 121.5(4) . . ?
C16 C17 H17 119.2 . . ?
C31 C32 H32 119.9 . . ?
C31 C32 C33 120.2(4) . . ?
C33 C32 H32 119.9 . . ?
C15 C16 H16 119.7 . . ?
C17 C16 C15 120.5(4) . . ?
C17 C16 H16 119.7 . . ?
C34 C33 C32 120.5(4) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
O1A C38A H38A 114.6 . . ?
O1A C38A H38B 114.6 . . ?
O1A C38A C37A 84.3(10) . . ?
H38A C38A H38B 111.7 . . ?
C37A C38A H38A 114.6 . . ?
C37A C38A H38B 114.6 . . ?
H36A C36A H36B 108.2 . . ?
C37A C36A H36A 109.7 . . ?
C37A C36A H36B 109.7 . . ?
C37A C36A C35A 109.9(13) . . ?
C35A C36A H36A 109.7 . . ?
C35A C36A H36B 109.7 . . ?
C38A C37A H37A 106.0 . . ?
C38A C37A H37B 106.0 . . ?
C36A C37A C38A 125.3(16) . . ?
C36A C37A H37A 106.0 . . ?
C36A C37A H37B 106.0 . . ?
H37A C37A H37B 106.3 . . ?
H35D C35B H35E 109.5 . . ?
H35D C35B H35F 109.5 . . ?
H35E C35B H35F 109.5 . . ?
C36B C35B H35D 109.5 . . ?
C36B C35B H35E 109.5 . . ?
C36B C35B H35F 109.5 . . ?
H37C C37B H37D 104.6 . . ?
C36B C37B H37C 101.6 . . ?
C36B C37B H37D 101.6 . . ?
C38B C37B H37C 101.6 . . ?
C38B C37B H37D 101.6 . . ?
C38B C37B C36B 141.4(19) . . ?
C35B C36B C37B 140.6(17) . . ?
C35B C36B H36C 101.9 . . ?
C35B C36B H36D 101.9 . . ?
C37B C36B H36C 101.9 . . ?
C37B C36B H36D 101.9 . . ?
H36C C36B H36D 104.7 . . ?
C38B O1B H1BA 109.5 . . ?
C37B C38B O1B 128(2) . . ?
C37B C38B H38C 105.2 . . ?
C37B C38B H38D 105.2 . . ?
O1B C38B H38C 105.2 . . ?
O1B C38B H38D 105.2 . . ?
H38C C38B H38D 105.9 . . ?
C36A C35A H35A 109.5 . . ?
C36A C35A H35B 109.5 . . ?
C36A C35A H35C 109.5 . . ?
H35A C35A H35B 109.5 . . ?
H35A C35A H35C 109.5 . . ?
H35B C35A H35C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl1 C13 C12 C11 -179.0(3) . . . . ?
Cl1 C13 C12 C17 1.4(6) . . . . ?
Cl1 C13 C9 C8 178.2(3) . . . . ?
Cl1 C13 C9 C4 -1.3(6) . . . . ?
O1A C38A C37A C36A -126(2) . . . . ?
C10 C8 C7 C6 -178.3(4) . . . . ?
C10 C8 C9 C13 0.7(6) . . . . ?
C10 C8 C9 C4 -179.8(4) . . . . ?
C10 C11 C12 C13 0.9(5) . . . . ?
C10 C11 C12 C17 -179.5(4) . . . . ?
C10 C11 C14 C15 180.0(4) . . . . ?
C3 C10 C8 C7 -0.9(5) . . . . ?
C3 C10 C8 C9 -178.7(3) . . . . ?
C3 C10 C11 C12 177.8(3) . . . . ?
C3 C10 C11 C14 -1.6(5) . . . . ?
C27 C25 C26 C30 0.3(5) . . . . ?
C27 C25 C26 C21 179.7(4) . . . . ?
C27 C25 C24 C23 180.0(4) . . . . ?
C27 C28 C29 C30 1.3(6) . . . . ?
C27 C28 C29 C34 -179.0(4) . . . . ?
C27 C28 C31 C32 178.2(5) . . . . ?
C13 C12 C17 C16 179.1(4) . . . . ?
C13 C9 C4 C5 177.3(5) . . . . ?
C8 C10 C3 N1 -83.1(4) . . . . ?
C8 C10 C11 C12 -0.6(5) . . . . ?
C8 C10 C11 C14 -180.0(4) . . . . ?
C8 C7 C6 C5 -1.5(7) . . . . ?
C8 C9 C4 C5 -2.2(7) . . . . ?
C25 C27 C20 N2 82.2(4) . . . . ?
C25 C27 C28 C29 -1.1(5) . . . . ?
C25 C27 C28 C31 179.5(4) . . . . ?
C25 C26 C30 Cl2 179.4(3) . . . . ?
C25 C26 C30 C29 -0.1(6) . . . . ?
C25 C26 C21 C22 0.5(6) . . . . ?
C25 C24 C23 C22 0.1(7) . . . . ?
C11 C10 C3 N1 98.5(4) . . . . ?
C11 C10 C8 C7 177.6(4) . . . . ?
C11 C10 C8 C9 -0.2(5) . . . . ?
C11 C12 C17 C16 -0.5(6) . . . . ?
C11 C14 C15 C16 -0.6(7) . . . . ?
C12 C13 C9 C8 -0.3(6) . . . . ?
C12 C13 C9 C4 -179.8(4) . . . . ?
C12 C11 C14 C15 0.6(6) . . . . ?
C12 C17 C16 C15 0.5(7) . . . . ?
C14 C11 C12 C13 -179.6(4) . . . . ?
C14 C11 C12 C17 0.0(5) . . . . ?
C14 C15 C16 C17 0.0(7) . . . . ?
C2 N1 C3 C10 -79.0(4) . . . . ?
C19 N2 C20 C27 72.5(4) . . . . ?
C26 C25 C24 C23 0.2(6) . . . . ?
C26 C21 C22 C23 -0.2(7) . . . . ?
C24 C25 C26 C30 -179.9(4) . . . . ?
C24 C25 C26 C21 -0.5(5) . . . . ?
C24 C23 C22 C21 -0.1(8) . . . . ?
C7 C8 C9 C13 -177.3(4) . . . . ?
C7 C8 C9 C4 2.2(6) . . . . ?
C7 C6 C5 C4 1.6(8) . . . . ?
C9 C13 C12 C11 -0.5(6) . . . . ?
C9 C13 C12 C17 179.9(4) . . . . ?
C9 C8 C7 C6 -0.4(6) . . . . ?
C20 C27 C25 C26 179.1(3) . . . . ?
C20 C27 C25 C24 -0.7(5) . . . . ?
C20 C27 C28 C29 -179.8(4) . . . . ?
C20 C27 C28 C31 0.7(6) . . . . ?
C28 C27 C25 C26 0.3(5) . . . . ?
C28 C27 C25 C24 -179.5(3) . . . . ?
C28 C27 C20 N2 -99.0(4) . . . . ?
C28 C29 C30 Cl2 179.8(3) . . . . ?
C28 C29 C30 C26 -0.7(6) . . . . ?
C28 C29 C34 C33 -0.1(8) . . . . ?
C28 C31 C32 C33 1.7(8) . . . . ?
C29 C28 C31 C32 -1.2(7) . . . . ?
C29 C34 C33 C32 0.5(9) . . . . ?
C1 N1 C3 C10 156.2(3) . . . . ?
C30 C26 C21 C22 179.9(4) . . . . ?
C30 C29 C34 C33 179.6(5) . . . . ?
C18 N2 C20 C27 -163.7(3) . . . . ?
C6 C5 C4 C9 0.2(8) . . . . ?
C21 C26 C30 Cl2 0.0(6) . . . . ?
C21 C26 C30 C29 -179.5(4) . . . . ?
C31 C28 C29 C30 -179.3(4) . . . . ?
C31 C28 C29 C34 0.4(6) . . . . ?
C31 C32 C33 C34 -1.3(9) . . . . ?
C34 C29 C30 Cl2 0.1(6) . . . . ?
C34 C29 C30 C26 179.6(4) . . . . ?
C36B C37B C38B O1B -132(3) . . . . ?
C38B C37B C36B C35B 97(4) . . . . ?
C35A C36A C37A C38A -138.3(18) . . . . ?

_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 3.049
_oxdiff_exptl_absorpt_empirical_full_min 0.570
####################################################################### 
# 
# 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_1-C2
_database_code_depnum_ccdc_archive 'CCDC 2240931'
loop_
_audit_author_name
_audit_author_address
'Binbin Luo'
;Shantou University
China
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
_audit_creation_date             2023-01-08
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'Br10 Pb3, 4(C17 H17 Cl N), 2(C2 H6 O)'
_chemical_formula_sum            'C72 H80 Br10 Cl4 N4 O2 Pb3'
_chemical_formula_weight         2595.87
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c h o n Pb Br Cl'
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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.4608(3)
_cell_length_b                   9.8836(2)
_cell_length_c                   39.2773(6)
_cell_angle_alpha                90
_cell_angle_beta                 98.840(2)
_cell_angle_gamma                90
_cell_volume                     8232.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11805
_cell_measurement_temperature    297.99(10)
_cell_measurement_theta_max      70.7320
_cell_measurement_theta_min      4.4010
_shelx_estimated_absorpt_T_max   0.833
_shelx_estimated_absorpt_T_min   0.116
_exptl_absorpt_coefficient_mu    18.959
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (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    2.094
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             4880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            19272
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.140
_diffrn_reflns_theta_min         4.434
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     43.00  69.00   0.50    2.84    --    0.00  38.00  60.00   52
  2  ω    -17.00  13.00   0.50    2.84    --    0.00  19.00-120.00   60
  3  ω    -13.00  19.00   0.50    2.84    --    0.00  38.00  60.00   64
  4  ω     42.00  83.00   0.50    2.84    --    0.00  19.00-120.00   82
  5  ω     43.00  98.00   0.50   11.36    --   89.30 -30.00   0.00  110
  6  ω      0.00  26.00   0.50   11.36    --   89.30 -30.00 120.00   52
  7  ω     58.00 177.00   0.50   11.36    --   89.30  82.00 150.00  238
  8  ω     58.00 113.00   0.50   11.36    --   89.30 -77.00   0.00  110
  9  ω      2.00  27.00   0.50   11.36    --   89.30 -77.00   0.00   50
 10  ω     66.00  92.00   0.50   11.36    --   89.30 -30.00 120.00   52
 11  ω     61.00 112.00   0.50   11.36    --   89.30 -61.00  30.00  102
 12  ω     76.00 169.00   0.50   11.36    --   89.30  30.00 -90.00  186
 13  ω      2.00  56.00   0.50   11.36    --   89.30 -61.00  30.00  108
;
_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      0.0049492000
_diffrn_orient_matrix_UB_12      0.0469952000
_diffrn_orient_matrix_UB_13      -0.0369075000
_diffrn_orient_matrix_UB_21      0.0272508000
_diffrn_orient_matrix_UB_22      0.1363202000
_diffrn_orient_matrix_UB_23      0.0141577000
_diffrn_orient_matrix_UB_31      0.0670892000
_diffrn_orient_matrix_UB_32      -0.0589200000
_diffrn_orient_matrix_UB_33      0.0033560000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6986
_reflns_number_total             7677
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.149
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         7677
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0291
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0353P)²+30.7455P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0771
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O1A-C36A
 1.42 with sigma of 0.02
 C36A-C35A
 1.51 with sigma of 0.02
 O1B-C36B
 1.42 with sigma of 0.02
 C36B-C35B
 1.51 with sigma of 0.02
 O1B-C35B
 2.37 with sigma of 0.04
 O1A-C35A
 2.37 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
O1B \\sim C36B \\sim C35B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O1A \\sim C36A \\sim C35A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 O1B, C36B, C35B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1A, C36A, C35A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1B, C35B, C36B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1A, C35A, C36A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: O1A(0.6) H1AA(0.6) C36A(0.6) H36A(0.6) H36B(0.6) C35A(0.6)
 H35A(0.6) H35B(0.6) H35C(0.6) O1B(0.4) H1BA(0.4) C36B(0.4) H36C(0.4) H36D(0.4)
 C35B(0.4) H35D(0.4) H35E(0.4) H35F(0.4)
5.a Everything fixed:
 H1BA
5.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
5.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C3(H3A,H3B), C36A(H36A,H36B), C36B(H36C,H36D)
5.d Aromatic/amide H refined with riding coordinates:
 C26(H26), C31(H31), C32(H32), C33(H33), C21(H21), C4(H4), C5(H5), C6(H6),
 C34(H34), C7(H7), C16(H16), C17(H17), C22(H22), C15(H15), C23(H23), C14(H14)
5.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C19(H19A,H19B,H19C),
 C35A(H35A,H35B,H35C), C35B(H35D,H35E,H35F)
5.f Idealised tetrahedral OH refined as rotating group:
 O1A(H1AA)
;
_atom_sites_solution_hydrogens   mixed
_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
Pb2 Pb 0.18354(2) 0.20738(2) 0.27295(2) 0.04285(6) Uani 1 1 d . . . . .
Pb1 Pb 0.000000 0.20353(3) 0.250000 0.04406(8) Uani 1 2 d S T P . .
Br3 Br 0.09834(2) 0.22057(6) 0.20333(2) 0.05565(13) Uani 1 1 d . . . . .
Br4 Br 0.24679(2) 0.45045(6) 0.24928(2) 0.05874(14) Uani 1 1 d . . . . .
Br1 Br 0.08288(3) -0.00984(6) 0.28647(2) 0.06065(14) Uani 1 1 d . . . . .
Br5 Br 0.27796(3) 0.18339(6) 0.33790(2) 0.06338(15) Uani 1 1 d . . . . .
Br2 Br 0.08862(3) 0.39031(7) 0.29942(2) 0.07313(18) Uani 1 1 d . . . . .
Cl2 Cl 0.48444(11) 0.2384(2) 0.48434(4) 0.0993(6) Uani 1 1 d . . . . .
Cl1 Cl 0.16736(12) 0.7669(3) 0.51556(5) 0.1171(7) Uani 1 1 d . . . . .
N1 N 0.2199(2) 0.7164(4) 0.34956(11) 0.0524(9) Uani 1 1 d . . . . .
H1 H 0.229882 0.630333 0.361560 0.063 Uiso 1 1 calc R U . . .
N2 N 0.41773(19) 0.2115(4) 0.31007(10) 0.0507(10) Uani 1 1 d . . . . .
H2 H 0.387353 0.169235 0.323016 0.061 Uiso 1 1 calc R U . . .
C20 C 0.4826(2) 0.1937(5) 0.33085(11) 0.0450(10) Uani 1 1 d . . . . .
H20A H 0.498554 0.104890 0.326165 0.054 Uiso 1 1 calc R U . . .
H20B H 0.510832 0.260604 0.323538 0.054 Uiso 1 1 calc R U . . .
C27 C 0.4828(2) 0.2078(4) 0.36899(11) 0.0428(10) Uani 1 1 d . . . . .
C26 C 0.5176(2) 0.4488(5) 0.36896(14) 0.0568(12) Uani 1 1 d . . . . .
H26 H 0.518067 0.445578 0.345341 0.068 Uiso 1 1 calc R U . . .
C10 C 0.1645(2) 0.7720(5) 0.39980(13) 0.0509(11) Uani 1 1 d . . . . .
C3 C 0.1613(3) 0.7728(6) 0.36135(14) 0.0588(13) Uani 1 1 d . . . . .
H3A H 0.155010 0.865071 0.353092 0.071 Uiso 1 1 calc R U . . .
H3B H 0.125151 0.720068 0.351085 0.071 Uiso 1 1 calc R U . . .
C25 C 0.5003(2) 0.3306(5) 0.38627(12) 0.0473(10) Uani 1 1 d . . . . .
C28 C 0.4661(2) 0.0948(5) 0.38735(12) 0.0479(10) Uani 1 1 d . . . . .
C18 C 0.4003(3) 0.3582(6) 0.30549(16) 0.0670(15) Uani 1 1 d . . . . .
H18A H 0.401585 0.399853 0.327668 0.100 Uiso 1 1 calc R U . . .
H18B H 0.358527 0.365795 0.292760 0.100 Uiso 1 1 calc R U . . .
H18C H 0.429653 0.402815 0.293107 0.100 Uiso 1 1 calc R U . . .
C2 C 0.2754(3) 0.8057(6) 0.3578(2) 0.0810(19) Uani 1 1 d . . . . .
H2A H 0.267694 0.889528 0.345560 0.122 Uiso 1 1 calc R U . . .
H2B H 0.311718 0.762333 0.351163 0.122 Uiso 1 1 calc R U . . .
H2C H 0.282953 0.823306 0.382161 0.122 Uiso 1 1 calc R U . . .
C31 C 0.4499(2) -0.0320(5) 0.37135(13) 0.0576(12) Uani 1 1 d . . . . .
H31 H 0.449302 -0.040331 0.347717 0.069 Uiso 1 1 calc R U . . .
C1 C 0.2080(4) 0.6876(7) 0.31192(15) 0.0822(19) Uani 1 1 d . . . . .
H1A H 0.174310 0.623169 0.307075 0.123 Uiso 1 1 calc R U . . .
H1B H 0.245471 0.651348 0.304884 0.123 Uiso 1 1 calc R U . . .
H1C H 0.196395 0.769869 0.299539 0.123 Uiso 1 1 calc R U . . .
C30 C 0.4838(3) 0.2265(6) 0.44002(13) 0.0615(14) Uani 1 1 d . . . . .
C24 C 0.5009(2) 0.3404(6) 0.42280(13) 0.0563(12) Uani 1 1 d . . . . .
C32 C 0.4355(3) -0.1404(6) 0.38937(16) 0.0697(15) Uani 1 1 d . . . . .
H32 H 0.425675 -0.222216 0.378108 0.084 Uiso 1 1 calc R U . . .
C33 C 0.4352(3) -0.1312(7) 0.42498(17) 0.0793(18) Uani 1 1 d . . . . .
H33 H 0.425110 -0.206742 0.437177 0.095 Uiso 1 1 calc R U . . .
C19 C 0.4127(3) 0.1409(8) 0.27611(13) 0.0822(19) Uani 1 1 d . . . . .
H19A H 0.441974 0.180224 0.262791 0.123 Uiso 1 1 calc R U . . .
H19B H 0.370574 0.150404 0.263917 0.123 Uiso 1 1 calc R U . . .
H19C H 0.422217 0.046644 0.279824 0.123 Uiso 1 1 calc R U . . .
C11 C 0.1493(2) 0.6518(6) 0.41608(14) 0.0548(12) Uani 1 1 d . . . . .
C21 C 0.5332(3) 0.5649(6) 0.38620(18) 0.0760(16) Uani 1 1 d . . . . .
H21 H 0.544384 0.640046 0.374236 0.091 Uiso 1 1 calc R U . . .
C29 C 0.4662(3) 0.1039(6) 0.42396(12) 0.0560(12) Uani 1 1 d . . . . .
C9 C 0.1807(3) 0.8891(6) 0.41936(14) 0.0608(13) Uani 1 1 d . . . . .
C4 C 0.1967(4) 1.0143(6) 0.40401(19) 0.0824(19) Uani 1 1 d . . . . .
H4 H 0.195168 1.018784 0.380247 0.099 Uiso 1 1 calc R U . . .
C5 C 0.2135(5) 1.1236(8) 0.4230(2) 0.108(3) Uani 1 1 d . . . . .
H5 H 0.224075 1.202489 0.412329 0.130 Uiso 1 1 calc R U . . .
C6 C 0.2154(5) 1.1214(9) 0.4586(3) 0.122(3) Uani 1 1 d . . . . .
H6 H 0.227392 1.198939 0.471321 0.146 Uiso 1 1 calc R U . . .
C34 C 0.4493(3) -0.0132(7) 0.44157(15) 0.0746(17) Uani 1 1 d . . . . .
H34 H 0.448040 -0.008221 0.465097 0.090 Uiso 1 1 calc R U . . .
C12 C 0.1507(3) 0.6493(7) 0.45267(15) 0.0657(14) Uani 1 1 d . . . . .
C7 C 0.2002(4) 1.0095(9) 0.4748(2) 0.103(2) Uani 1 1 d . . . . .
H7 H 0.201493 1.010733 0.498584 0.123 Uiso 1 1 calc R U . . .
C16 C 0.1178(4) 0.4166(7) 0.4145(2) 0.096(2) Uani 1 1 d . . . . .
H16 H 0.106434 0.337865 0.402079 0.115 Uiso 1 1 calc R U . . .
C17 C 0.1325(3) 0.5301(6) 0.39751(18) 0.0711(16) Uani 1 1 d . . . . .
H17 H 0.131452 0.527870 0.373760 0.085 Uiso 1 1 calc R U . . .
C22 C 0.5330(3) 0.5744(7) 0.42144(18) 0.0837(19) Uani 1 1 d . . . . .
H22 H 0.542831 0.656345 0.432639 0.100 Uiso 1 1 calc R U . . .
C15 C 0.1196(4) 0.4173(9) 0.4504(3) 0.105(3) Uani 1 1 d . . . . .
H15 H 0.109437 0.338845 0.461425 0.126 Uiso 1 1 calc R U . . .
C8 C 0.1819(3) 0.8870(7) 0.45574(16) 0.0707(15) Uani 1 1 d . . . . .
C23 C 0.5187(3) 0.4668(7) 0.43946(16) 0.0769(17) Uani 1 1 d . . . . .
H23 H 0.520368 0.474062 0.463189 0.092 Uiso 1 1 calc R U . . .
C14 C 0.1354(4) 0.5267(8) 0.4687(2) 0.093(2) Uani 1 1 d . . . . .
H14 H 0.136497 0.524249 0.492486 0.111 Uiso 1 1 calc R U . . .
C13 C 0.1658(3) 0.7684(8) 0.47102(16) 0.0754(17) Uani 1 1 d . . . . .
O1A O 0.2747(11) 0.488(3) 0.3762(4) 0.088(4) Uani 0.6 1 d D U P A 1
H1AA H 0.273504 0.410376 0.368608 0.132 Uiso 0.6 1 calc R U P A 1
C36A C 0.3301(12) 0.503(2) 0.4027(5) 0.148(9) Uani 0.6 1 d D U P A 1
H36A H 0.367399 0.503934 0.391539 0.178 Uiso 0.6 1 calc R U P A 1
H36B H 0.327646 0.590609 0.413685 0.178 Uiso 0.6 1 calc R U P A 1
C35A C 0.3379(9) 0.4015(19) 0.4288(4) 0.130(6) Uani 0.6 1 d D U P A 1
H35A H 0.347641 0.316659 0.418959 0.196 Uiso 0.6 1 calc R U P A 1
H35B H 0.299620 0.392744 0.438470 0.196 Uiso 0.6 1 calc R U P A 1
H35C H 0.371736 0.426593 0.446645 0.196 Uiso 0.6 1 calc R U P A 1
O1B O 0.284(2) 0.470(5) 0.3689(7) 0.104(7) Uani 0.4 1 d D U P B 2
H1BA H 0.255710 0.506180 0.377070 0.157 Uiso 0.4 1 d . U P C 2
C36B C 0.3389(13) 0.456(3) 0.3952(6) 0.101(7) Uani 0.4 1 d D U P B 2
H36C H 0.369539 0.527191 0.393788 0.121 Uiso 0.4 1 calc R U P B 2
H36D H 0.359063 0.368445 0.394321 0.121 Uiso 0.4 1 calc R U P B 2
C35B C 0.3079(15) 0.470(4) 0.4261(6) 0.149(10) Uani 0.4 1 d D U P B 2
H35D H 0.263809 0.449619 0.420184 0.224 Uiso 0.4 1 calc R U P B 2
H35E H 0.312770 0.561251 0.434552 0.224 Uiso 0.4 1 calc R U P B 2
H35F H 0.326837 0.408721 0.443619 0.224 Uiso 0.4 1 calc R U P B 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
Pb2 Br3 3.0497(5) . ?
Pb2 Br4 3.1382(5) 4_545 ?
Pb2 Br4 2.9776(5) . ?
Pb2 Br1 3.1481(6) . ?
Pb2 Br5 3.0135(6) . ?
Pb2 Br2 3.0250(6) . ?
Pb1 Br3 3.0053(5) . ?
Pb1 Br3 3.0053(5) 2 ?
Pb1 Br1 2.9799(5) . ?
Pb1 Br1 2.9798(6) 2 ?
Pb1 Br2 3.1077(6) . ?
Pb1 Br2 3.1079(6) 2 ?
Cl2 C30 1.742(5) . ?
Cl1 C13 1.745(6) . ?
N1 H1 0.9800 . ?
N1 C3 1.512(6) . ?
N1 C2 1.479(7) . ?
N1 C1 1.488(7) . ?
N2 H2 0.9800 . ?
N2 C20 1.512(6) . ?
N2 C18 1.501(7) . ?
N2 C19 1.495(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C27 1.504(6) . ?
C27 C25 1.413(7) . ?
C27 C28 1.404(6) . ?
C26 H26 0.9300 . ?
C26 C25 1.430(7) . ?
C26 C21 1.348(8) . ?
C10 C3 1.501(7) . ?
C10 C11 1.410(7) . ?
C10 C9 1.404(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C25 C24 1.436(7) . ?
C28 C31 1.421(7) . ?
C28 C29 1.440(6) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C31 H31 0.9300 . ?
C31 C32 1.347(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C30 C24 1.391(8) . ?
C30 C29 1.392(8) . ?
C24 C23 1.435(8) . ?
C32 H32 0.9300 . ?
C32 C33 1.403(9) . ?
C33 H33 0.9300 . ?
C33 C34 1.347(9) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C11 C12 1.433(8) . ?
C11 C17 1.425(8) . ?
C21 H21 0.9300 . ?
C21 C22 1.388(9) . ?
C29 C34 1.423(8) . ?
C9 C4 1.440(8) . ?
C9 C8 1.425(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.330(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.392(12) . ?
C6 H6 0.9300 . ?
C6 C7 1.341(12) . ?
C34 H34 0.9300 . ?
C12 C14 1.428(9) . ?
C12 C13 1.393(10) . ?
C7 H7 0.9300 . ?
C7 C8 1.446(10) . ?
C16 H16 0.9300 . ?
C16 C17 1.366(9) . ?
C16 C15 1.407(12) . ?
C17 H17 0.9300 . ?
C22 H22 0.9300 . ?
C22 C23 1.339(9) . ?
C15 H15 0.9300 . ?
C15 C14 1.314(11) . ?
C8 C13 1.385(9) . ?
C23 H23 0.9300 . ?
C14 H14 0.9300 . ?
O1A H1AA 0.8200 . ?
O1A C36A 1.463(15) . ?
C36A H36A 0.9700 . ?
C36A H36B 0.9700 . ?
C36A C35A 1.429(17) . ?
C35A H35A 0.9600 . ?
C35A H35B 0.9600 . ?
C35A H35C 0.9600 . ?
O1B H1BA 0.8177 . ?
O1B C36B 1.446(17) . ?
C36B H36C 0.9700 . ?
C36B H36D 0.9700 . ?
C36B C35B 1.478(18) . ?
C35B H35D 0.9600 . ?
C35B H35E 0.9600 . ?
C35B H35F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br3 Pb2 Br4 91.764(15) . 4_545 ?
Br3 Pb2 Br1 81.257(15) . . ?
Br4 Pb2 Br3 85.688(15) . . ?
Br4 Pb2 Br4 107.847(5) . 4_545 ?
Br4 Pb2 Br1 82.168(15) 4_545 . ?
Br4 Pb2 Br1 163.832(15) . . ?
Br4 Pb2 Br5 92.771(16) . . ?
Br4 Pb2 Br2 89.337(17) . . ?
Br5 Pb2 Br3 174.206(17) . . ?
Br5 Pb2 Br4 83.383(16) . 4_545 ?
Br5 Pb2 Br1 101.133(16) . . ?
Br5 Pb2 Br2 99.018(18) . . ?
Br2 Pb2 Br3 86.560(17) . . ?
Br2 Pb2 Br4 162.576(17) . 4_545 ?
Br2 Pb2 Br1 80.435(17) . . ?
Br3 Pb1 Br3 173.57(2) . 2 ?
Br3 Pb1 Br2 90.312(15) . 2 ?
Br3 Pb1 Br2 90.314(15) 2 . ?
Br3 Pb1 Br2 85.868(16) . . ?
Br3 Pb1 Br2 85.867(16) 2 2 ?
Br1 Pb1 Br3 84.813(15) 2 2 ?
Br1 Pb1 Br3 99.774(15) . 2 ?
Br1 Pb1 Br3 84.813(15) . . ?
Br1 Pb1 Br3 99.773(15) 2 . ?
Br1 Pb1 Br1 89.90(3) 2 . ?
Br1 Pb1 Br2 81.801(18) 2 2 ?
Br1 Pb1 Br2 169.545(19) . 2 ?
Br1 Pb1 Br2 81.800(18) . . ?
Br1 Pb1 Br2 169.545(19) 2 . ?
Br2 Pb1 Br2 107.12(3) . 2 ?
Pb1 Br3 Pb2 80.281(13) . . ?
Pb2 Br4 Pb2 177.88(2) . 4 ?
Pb1 Br1 Pb2 79.086(13) . . ?
Pb2 Br2 Pb1 79.052(14) . . ?
C3 N1 H1 107.7 . . ?
C2 N1 H1 107.7 . . ?
C2 N1 C3 113.1(4) . . ?
C2 N1 C1 110.0(5) . . ?
C1 N1 H1 107.7 . . ?
C1 N1 C3 110.5(5) . . ?
C20 N2 H2 107.5 . . ?
C18 N2 H2 107.5 . . ?
C18 N2 C20 111.7(4) . . ?
C19 N2 H2 107.5 . . ?
C19 N2 C20 111.2(4) . . ?
C19 N2 C18 111.2(4) . . ?
N2 C20 H20A 109.0 . . ?
N2 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C27 C20 N2 112.8(4) . . ?
C27 C20 H20A 109.0 . . ?
C27 C20 H20B 109.0 . . ?
C25 C27 C20 121.2(4) . . ?
C28 C27 C20 118.4(4) . . ?
C28 C27 C25 120.4(4) . . ?
C25 C26 H26 119.3 . . ?
C21 C26 H26 119.3 . . ?
C21 C26 C25 121.3(5) . . ?
C11 C10 C3 118.9(5) . . ?
C9 C10 C3 121.0(5) . . ?
C9 C10 C11 120.1(5) . . ?
N1 C3 H3A 108.9 . . ?
N1 C3 H3B 108.9 . . ?
C10 C3 N1 113.3(4) . . ?
C10 C3 H3A 108.9 . . ?
C10 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
C27 C25 C26 122.9(4) . . ?
C27 C25 C24 119.9(4) . . ?
C26 C25 C24 117.2(5) . . ?
C27 C28 C31 122.5(4) . . ?
C27 C28 C29 120.1(4) . . ?
C31 C28 C29 117.3(4) . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C28 C31 H31 119.0 . . ?
C32 C31 C28 122.0(5) . . ?
C32 C31 H31 119.0 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C24 C30 Cl2 118.0(4) . . ?
C24 C30 C29 123.9(5) . . ?
C29 C30 Cl2 118.1(4) . . ?
C30 C24 C25 117.9(5) . . ?
C30 C24 C23 123.7(5) . . ?
C23 C24 C25 118.4(5) . . ?
C31 C32 H32 119.7 . . ?
C31 C32 C33 120.6(6) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 H33 119.9 . . ?
C34 C33 C32 120.2(6) . . ?
C34 C33 H33 119.9 . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C10 C11 C12 119.9(5) . . ?
C10 C11 C17 122.5(5) . . ?
C17 C11 C12 117.6(5) . . ?
C26 C21 H21 119.3 . . ?
C26 C21 C22 121.3(6) . . ?
C22 C21 H21 119.3 . . ?
C30 C29 C28 117.7(5) . . ?
C30 C29 C34 124.0(5) . . ?
C34 C29 C28 118.3(5) . . ?
C10 C9 C4 122.3(5) . . ?
C10 C9 C8 120.1(5) . . ?
C8 C9 C4 117.6(6) . . ?
C9 C4 H4 119.2 . . ?
C5 C4 C9 121.6(7) . . ?
C5 C4 H4 119.2 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 120.9(8) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.2(8) . . ?
C7 C6 H6 119.4 . . ?
C33 C34 C29 121.6(5) . . ?
C33 C34 H34 119.2 . . ?
C29 C34 H34 119.2 . . ?
C14 C12 C11 119.2(6) . . ?
C13 C12 C11 118.1(5) . . ?
C13 C12 C14 122.7(6) . . ?
C6 C7 H7 119.7 . . ?
C6 C7 C8 120.7(7) . . ?
C8 C7 H7 119.7 . . ?
C17 C16 H16 119.6 . . ?
C17 C16 C15 120.8(7) . . ?
C15 C16 H16 119.6 . . ?
C11 C17 H17 119.9 . . ?
C16 C17 C11 120.2(7) . . ?
C16 C17 H17 119.9 . . ?
C21 C22 H22 119.7 . . ?
C23 C22 C21 120.6(6) . . ?
C23 C22 H22 119.7 . . ?
C16 C15 H15 119.4 . . ?
C14 C15 C16 121.3(7) . . ?
C14 C15 H15 119.4 . . ?
C9 C8 C7 118.0(6) . . ?
C13 C8 C9 118.6(6) . . ?
C13 C8 C7 123.4(6) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 C24 121.2(6) . . ?
C22 C23 H23 119.4 . . ?
C12 C14 H14 119.5 . . ?
C15 C14 C12 120.9(7) . . ?
C15 C14 H14 119.5 . . ?
C12 C13 Cl1 118.6(5) . . ?
C8 C13 Cl1 118.3(6) . . ?
C8 C13 C12 123.1(6) . . ?
C36A O1A H1AA 109.5 . . ?
O1A C36A H36A 108.4 . . ?
O1A C36A H36B 108.4 . . ?
H36A C36A H36B 107.5 . . ?
C35A C36A O1A 115.5(19) . . ?
C35A C36A H36A 108.4 . . ?
C35A C36A H36B 108.4 . . ?
C36A C35A H35A 109.5 . . ?
C36A C35A H35B 109.5 . . ?
C36A C35A H35C 109.5 . . ?
H35A C35A H35B 109.5 . . ?
H35A C35A H35C 109.5 . . ?
H35B C35A H35C 109.5 . . ?
C36B O1B H1BA 109.6 . . ?
O1B C36B H36C 111.9 . . ?
O1B C36B H36D 111.9 . . ?
O1B C36B C35B 99.1(19) . . ?
H36C C36B H36D 109.6 . . ?
C35B C36B H36C 111.9 . . ?
C35B C36B H36D 111.9 . . ?
C36B C35B H35D 109.5 . . ?
C36B C35B H35E 109.5 . . ?
C36B C35B H35F 109.5 . . ?
H35D C35B H35E 109.5 . . ?
H35D C35B H35F 109.5 . . ?
H35E C35B H35F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl2 C30 C24 C25 -179.9(4) . . . . ?
Cl2 C30 C24 C23 -0.2(8) . . . . ?
Cl2 C30 C29 C28 -179.7(4) . . . . ?
Cl2 C30 C29 C34 -0.8(8) . . . . ?
N2 C20 C27 C25 -98.2(5) . . . . ?
N2 C20 C27 C28 82.9(5) . . . . ?
C20 C27 C25 C26 1.2(7) . . . . ?
C20 C27 C25 C24 -179.1(4) . . . . ?
C20 C27 C28 C31 0.7(7) . . . . ?
C20 C27 C28 C29 179.5(4) . . . . ?
C27 C25 C24 C30 -0.1(7) . . . . ?
C27 C25 C24 C23 -179.8(5) . . . . ?
C27 C28 C31 C32 178.4(5) . . . . ?
C27 C28 C29 C30 -0.7(7) . . . . ?
C27 C28 C29 C34 -179.7(5) . . . . ?
C26 C25 C24 C30 179.6(5) . . . . ?
C26 C25 C24 C23 -0.1(7) . . . . ?
C26 C21 C22 C23 1.8(11) . . . . ?
C10 C11 C12 C14 -179.9(5) . . . . ?
C10 C11 C12 C13 1.5(8) . . . . ?
C10 C11 C17 C16 -179.5(6) . . . . ?
C10 C9 C4 C5 -178.3(7) . . . . ?
C10 C9 C8 C7 178.8(6) . . . . ?
C10 C9 C8 C13 -1.1(9) . . . . ?
C3 C10 C11 C12 -178.7(5) . . . . ?
C3 C10 C11 C17 1.4(7) . . . . ?
C3 C10 C9 C4 -1.6(8) . . . . ?
C3 C10 C9 C8 178.5(5) . . . . ?
C25 C27 C28 C31 -178.1(5) . . . . ?
C25 C27 C28 C29 0.7(7) . . . . ?
C25 C26 C21 C22 -0.2(10) . . . . ?
C25 C24 C23 C22 1.6(9) . . . . ?
C28 C27 C25 C26 -179.9(4) . . . . ?
C28 C27 C25 C24 -0.3(7) . . . . ?
C28 C31 C32 C33 0.9(9) . . . . ?
C28 C29 C34 C33 1.7(9) . . . . ?
C18 N2 C20 C27 79.9(5) . . . . ?
C2 N1 C3 C10 -70.5(6) . . . . ?
C31 C28 C29 C30 178.1(5) . . . . ?
C31 C28 C29 C34 -0.8(7) . . . . ?
C31 C32 C33 C34 0.0(10) . . . . ?
C1 N1 C3 C10 165.7(5) . . . . ?
C30 C24 C23 C22 -178.1(6) . . . . ?
C30 C29 C34 C33 -177.2(6) . . . . ?
C24 C30 C29 C28 0.4(9) . . . . ?
C24 C30 C29 C34 179.3(6) . . . . ?
C32 C33 C34 C29 -1.3(11) . . . . ?
C19 N2 C20 C27 -155.3(4) . . . . ?
C11 C10 C3 N1 -82.7(6) . . . . ?
C11 C10 C9 C4 179.9(5) . . . . ?
C11 C10 C9 C8 0.0(8) . . . . ?
C11 C12 C14 C15 -0.5(11) . . . . ?
C11 C12 C13 Cl1 179.7(4) . . . . ?
C11 C12 C13 C8 -2.8(10) . . . . ?
C21 C26 C25 C27 179.1(5) . . . . ?
C21 C26 C25 C24 -0.6(8) . . . . ?
C21 C22 C23 C24 -2.5(11) . . . . ?
C29 C28 C31 C32 -0.4(8) . . . . ?
C29 C30 C24 C25 0.0(8) . . . . ?
C29 C30 C24 C23 179.7(6) . . . . ?
C9 C10 C3 N1 98.8(6) . . . . ?
C9 C10 C11 C12 -0.2(7) . . . . ?
C9 C10 C11 C17 179.9(5) . . . . ?
C9 C4 C5 C6 -0.9(14) . . . . ?
C9 C8 C13 Cl1 -179.9(5) . . . . ?
C9 C8 C13 C12 2.6(10) . . . . ?
C4 C9 C8 C7 -1.1(9) . . . . ?
C4 C9 C8 C13 179.0(6) . . . . ?
C4 C5 C6 C7 -0.2(16) . . . . ?
C5 C6 C7 C8 0.6(16) . . . . ?
C6 C7 C8 C9 0.1(12) . . . . ?
C6 C7 C8 C13 180.0(8) . . . . ?
C12 C11 C17 C16 0.6(8) . . . . ?
C7 C8 C13 Cl1 0.2(10) . . . . ?
C7 C8 C13 C12 -177.3(7) . . . . ?
C16 C15 C14 C12 0.5(13) . . . . ?
C17 C11 C12 C14 -0.1(8) . . . . ?
C17 C11 C12 C13 -178.6(5) . . . . ?
C17 C16 C15 C14 0.1(13) . . . . ?
C15 C16 C17 C11 -0.6(11) . . . . ?
C8 C9 C4 C5 1.6(11) . . . . ?
C14 C12 C13 Cl1 1.2(9) . . . . ?
C14 C12 C13 C8 178.8(6) . . . . ?
C13 C12 C14 C15 178.0(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 1.589
_oxdiff_exptl_absorpt_empirical_full_min 0.751
####################################################################### 
# 
# 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_1-C1
_database_code_depnum_ccdc_archive 'CCDC 2240933'
loop_
_audit_author_name
_audit_author_address
'Binbin Luo'
;Shantou University
China
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
_audit_creation_date             2023-01-08
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'Br10 Pb3, 4(C17 H17 Cl N), 2(C H4 O)'
_chemical_formula_sum            'C70 H76 Br10 Cl4 N4 O2 Pb3'
_chemical_formula_weight         2567.81
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Pb Br'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.3980(3)
_cell_length_b                   9.82910(10)
_cell_length_c                   38.8397(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.8460(10)
_cell_angle_gamma                90
_cell_volume                     8022.96(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11015
_cell_measurement_temperature    297.98(10)
_cell_measurement_theta_max      70.7020
_cell_measurement_theta_min      4.2230
_shelx_estimated_absorpt_T_max   0.697
_shelx_estimated_absorpt_T_min   0.112
_exptl_absorpt_coefficient_mu    19.444
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (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    2.126
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             4816
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            18521
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.129
_diffrn_reflns_theta_min         4.207
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -28.00   7.00   0.50    2.29    --    0.00 -38.00  60.00   70
  2  ω     46.00  87.00   0.50    2.29    --    0.00  38.00 -60.00   82
  3  ω    -76.00 -48.00   0.50    2.29    --    0.00 -38.00  60.00   56
  4  ω     -9.00  18.00   0.50    2.29    --    0.00  38.00 -60.00   54
  5  ω     82.00 171.00   0.50    9.14    --   89.30  61.00 -30.00  178
  6  ω     61.00 179.00   0.50    9.14    --   89.30  82.00  30.00  236
  7  ω     56.00 113.00   0.50    9.14    --   89.30 -61.00 -90.00  114
  8  ω     86.00 119.00   0.50    9.14    --   89.30 -77.00-180.00   66
  9  ω      0.00  39.00   0.50    9.14    --   89.30 -77.00-180.00   78
 10  ω     16.00  90.00   0.50    9.14    --   89.30 -30.00 -90.00  148
 11  ω      0.00  25.00   0.50    9.14    --   89.30 -61.00 -90.00   50
 12  ω      0.00  55.00   0.50    9.14    --   89.30   0.00-120.00  110
;
_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      0.0097402000
_diffrn_orient_matrix_UB_12      -0.1063121000
_diffrn_orient_matrix_UB_13      -0.0276529000
_diffrn_orient_matrix_UB_21      -0.0349166000
_diffrn_orient_matrix_UB_22      0.0934192000
_diffrn_orient_matrix_UB_23      -0.0292691000
_diffrn_orient_matrix_UB_31      0.0636981000
_diffrn_orient_matrix_UB_32      0.0673565000
_diffrn_orient_matrix_UB_33      -0.0030668000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6700
_reflns_number_total             7475
_reflns_odcompleteness_completeness 99.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         7475
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0236
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0279P)²+13.0651P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0609
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
1.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C20(H20A,H20B)
1.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C4(H4), C32(H32), C33(H33), C31(H31), C6(H6), C17(H17),
 C7(H7), C34(H34), C16(H16), C5(H5), C24(H24), C21(H21), C23(H23), C22(H22)
1.d Tetrahedral OH refined with riding coordinates:
 O1(H1D)
1.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C2(H2A,H2B,H2C), C19(H19A,H19B,H19C),
 C35(H35A,H35B,H35C)
;
_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 0.68530(2) -0.28795(2) 0.27325(2) 0.03692(5) Uani 1 1 d . . . . .
Pb2 Pb 0.500000 -0.28954(2) 0.250000 0.03970(6) Uani 1 2 d S T P . .
Br4 Br 0.59563(2) -0.27319(5) 0.20239(2) 0.04950(10) Uani 1 1 d . . . . .
Br5 Br 0.41456(2) -0.50489(4) 0.21295(2) 0.05163(11) Uani 1 1 d . . . . .
Br1 Br 0.78510(2) -0.31469(5) 0.33850(2) 0.05368(11) Uani 1 1 d . . . . .
Br2 Br 0.74593(2) -0.04174(4) 0.24907(2) 0.05248(11) Uani 1 1 d . . . . .
Br3 Br 0.59199(2) -0.10398(5) 0.30147(2) 0.06534(14) Uani 1 1 d . . . . .
Cl1 Cl 0.98178(9) 0.76122(15) 0.48582(3) 0.0906(5) Uani 1 1 d . . . . .
Cl2 Cl 0.66959(9) 0.31408(18) 0.51992(4) 0.0927(5) Uani 1 1 d . . . . .
N1 N 0.92212(15) 0.7158(3) 0.30964(8) 0.0416(7) Uani 1 1 d . . . . .
H1 H 0.891972 0.672705 0.322369 0.050 Uiso 1 1 calc R U . . .
N2 N 0.72649(16) 0.2166(3) 0.35442(9) 0.0454(8) Uani 1 1 d . . . . .
H2 H 0.734361 0.128982 0.366504 0.054 Uiso 1 1 calc R U . . .
O1 O 0.7825(2) -0.0247(4) 0.37894(12) 0.0926(12) Uani 1 1 d . . . . .
H1D H 0.768604 -0.099704 0.372069 0.139 Uiso 1 1 calc R U . . .
C11 C 0.96989(17) 0.6064(4) 0.38876(9) 0.0389(8) Uani 1 1 d . . . . .
C12 C 0.9681(2) 0.6190(4) 0.42557(10) 0.0466(9) Uani 1 1 d . . . . .
C9 C 1.00399(17) 0.8432(4) 0.38727(9) 0.0375(7) Uani 1 1 d . . . . .
C14 C 0.95517(19) 0.4761(4) 0.37330(11) 0.0485(9) Uani 1 1 d . . . . .
H14 H 0.956210 0.464514 0.349652 0.058 Uiso 1 1 calc R U . . .
C10 C 0.98725(17) 0.7186(3) 0.37019(9) 0.0368(8) Uani 1 1 d . . . . .
C8 C 1.00274(19) 0.8569(4) 0.42392(10) 0.0443(8) Uani 1 1 d . . . . .
C13 C 0.9845(2) 0.7445(5) 0.44143(10) 0.0506(10) Uani 1 1 d . . . . .
C27 C 0.67109(19) 0.2864(4) 0.40337(11) 0.0437(9) Uani 1 1 d . . . . .
C28 C 0.65504(18) 0.1713(4) 0.42143(10) 0.0437(8) Uani 1 1 d . . . . .
C15 C 0.9398(2) 0.3692(5) 0.39170(12) 0.0588(11) Uani 1 1 d . . . . .
H15 H 0.930599 0.285655 0.380683 0.071 Uiso 1 1 calc R U . . .
C4 C 1.02282(19) 0.9602(4) 0.36997(11) 0.0480(9) Uani 1 1 d . . . . .
H4 H 1.024395 0.954177 0.346257 0.058 Uiso 1 1 calc R U . . .
C3 C 0.98781(17) 0.7004(4) 0.33175(9) 0.0400(8) Uani 1 1 d . . . . .
H3A H 1.004258 0.610830 0.327942 0.048 Uiso 1 1 calc R U . . .
H3B H 1.016007 0.767357 0.324478 0.048 Uiso 1 1 calc R U . . .
C32 C 0.6219(3) -0.0643(5) 0.42235(16) 0.0745(15) Uani 1 1 d . . . . .
H32 H 0.610365 -0.145572 0.410612 0.089 Uiso 1 1 calc R U . . .
C33 C 0.6225(3) -0.0550(6) 0.45860(18) 0.0855(17) Uani 1 1 d . . . . .
H33 H 0.611692 -0.130742 0.470569 0.103 Uiso 1 1 calc R U . . .
C20 C 0.6683(2) 0.2770(4) 0.36429(11) 0.0478(9) Uani 1 1 d . . . . .
H20A H 0.631706 0.222342 0.354069 0.057 Uiso 1 1 calc R U . . .
H20B H 0.661938 0.367530 0.354300 0.057 Uiso 1 1 calc R U . . .
C31 C 0.6378(2) 0.0438(4) 0.40462(13) 0.0581(11) Uani 1 1 d . . . . .
H31 H 0.637590 0.035430 0.380747 0.070 Uiso 1 1 calc R U . . .
C6 C 1.0367(3) 1.0910(5) 0.42281(13) 0.0670(13) Uani 1 1 d . . . . .
H6 H 1.046995 1.173281 0.434320 0.080 Uiso 1 1 calc R U . . .
C17 C 0.9507(2) 0.5032(5) 0.44378(12) 0.0621(12) Uani 1 1 d . . . . .
H17 H 0.948444 0.510907 0.467380 0.074 Uiso 1 1 calc R U . . .
C25 C 0.6870(2) 0.4179(5) 0.45827(12) 0.0596(11) Uani 1 1 d . . . . .
C7 C 1.0204(2) 0.9840(5) 0.44062(12) 0.0613(12) Uani 1 1 d . . . . .
H7 H 1.020583 0.992996 0.464480 0.074 Uiso 1 1 calc R U . . .
C34 C 0.6384(3) 0.0608(6) 0.47609(14) 0.0733(14) Uani 1 1 d . . . . .
H34 H 0.638882 0.064160 0.500067 0.088 Uiso 1 1 calc R U . . .
C16 C 0.9376(2) 0.3831(5) 0.42749(13) 0.0669(13) Uani 1 1 d . . . . .
H16 H 0.926990 0.308564 0.439981 0.080 Uiso 1 1 calc R U . . .
C26 C 0.6871(2) 0.4093(4) 0.42129(11) 0.0508(10) Uani 1 1 d . . . . .
C5 C 1.0386(2) 1.0802(5) 0.38691(13) 0.0618(12) Uani 1 1 d . . . . .
H5 H 1.050420 1.154590 0.374808 0.074 Uiso 1 1 calc R U . . .
C29 C 0.6547(2) 0.1794(5) 0.45841(12) 0.0531(10) Uani 1 1 d . . . . .
C1 C 0.9036(2) 0.8625(5) 0.30455(12) 0.0597(11) Uani 1 1 d . . . . .
H1A H 0.904132 0.904200 0.326949 0.089 Uiso 1 1 calc R U . . .
H1B H 0.861665 0.868942 0.290585 0.089 Uiso 1 1 calc R U . . .
H1C H 0.933302 0.908441 0.292839 0.089 Uiso 1 1 calc R U . . .
C24 C 0.7042(3) 0.5442(6) 0.47583(15) 0.0830(17) Uani 1 1 d . . . . .
H24 H 0.704722 0.551374 0.499759 0.100 Uiso 1 1 calc R U . . .
C21 C 0.7031(3) 0.5292(4) 0.40424(14) 0.0673(13) Uani 1 1 d . . . . .
H21 H 0.702376 0.526669 0.380234 0.081 Uiso 1 1 calc R U . . .
C23 C 0.7198(3) 0.6528(6) 0.45804(19) 0.097(2) Uani 1 1 d . . . . .
H23 H 0.731034 0.733959 0.469915 0.116 Uiso 1 1 calc R U . . .
C30 C 0.6703(2) 0.3028(5) 0.47512(12) 0.0583(11) Uani 1 1 d . . . . .
C18 C 0.7845(2) 0.3011(5) 0.36473(18) 0.0813(17) Uani 1 1 d . . . . .
H18A H 0.779387 0.385062 0.351885 0.122 Uiso 1 1 calc R U . . .
H18B H 0.820647 0.252873 0.359571 0.122 Uiso 1 1 calc R U . . .
H18C H 0.790949 0.319963 0.389396 0.122 Uiso 1 1 calc R U . . .
C22 C 0.7192(3) 0.6457(6) 0.42175(18) 0.093(2) Uani 1 1 d . . . . .
H22 H 0.730089 0.721719 0.409896 0.111 Uiso 1 1 calc R U . . .
C2 C 0.9169(2) 0.6443(6) 0.27543(11) 0.0716(14) Uani 1 1 d . . . . .
H2A H 0.946156 0.684005 0.262348 0.107 Uiso 1 1 calc R U . . .
H2B H 0.874309 0.652916 0.262380 0.107 Uiso 1 1 calc R U . . .
H2C H 0.926948 0.549731 0.279500 0.107 Uiso 1 1 calc R U . . .
C19 C 0.7151(3) 0.1892(6) 0.31571(13) 0.0795(16) Uani 1 1 d . . . . .
H19A H 0.677984 0.133042 0.309314 0.119 Uiso 1 1 calc R U . . .
H19B H 0.751287 0.143292 0.309895 0.119 Uiso 1 1 calc R U . . .
H19C H 0.708592 0.273763 0.303178 0.119 Uiso 1 1 calc R U . . .
C35 C 0.8368(4) -0.0405(9) 0.4035(2) 0.135(3) Uani 1 1 d . . . . .
H35A H 0.859762 -0.118681 0.397805 0.202 Uiso 1 1 calc R U . . .
H35B H 0.825927 -0.052998 0.426198 0.202 Uiso 1 1 calc R U . . .
H35C H 0.862956 0.039050 0.403863 0.202 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br4 3.0477(4) . ?
Pb1 Br5 3.1356(4) 2_655 ?
Pb1 Br1 3.0026(5) . ?
Pb1 Br2 2.9799(4) . ?
Pb1 Br2 3.1015(4) 4_645 ?
Pb1 Br3 3.0467(5) . ?
Pb2 Br4 3.0091(4) 2_655 ?
Pb2 Br4 3.0092(4) . ?
Pb2 Br5 2.9840(4) . ?
Pb2 Br5 2.9840(4) 2_655 ?
Pb2 Br3 3.1171(5) . ?
Pb2 Br3 3.1171(5) 2_655 ?
Cl1 C13 1.743(4) . ?
Cl2 C30 1.747(5) . ?
N1 H1 0.9800 . ?
N1 C3 1.511(5) . ?
N1 C1 1.499(6) . ?
N1 C2 1.489(5) . ?
N2 H2 0.9800 . ?
N2 C20 1.494(5) . ?
N2 C18 1.484(6) . ?
N2 C19 1.501(6) . ?
O1 H1D 0.8200 . ?
O1 C35 1.368(8) . ?
C11 C12 1.443(5) . ?
C11 C14 1.424(5) . ?
C11 C10 1.406(5) . ?
C12 C13 1.394(6) . ?
C12 C17 1.426(6) . ?
C9 C10 1.407(5) . ?
C9 C8 1.435(5) . ?
C9 C4 1.427(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.346(6) . ?
C10 C3 1.506(5) . ?
C8 C13 1.392(6) . ?
C8 C7 1.426(6) . ?
C27 C28 1.408(5) . ?
C27 C20 1.511(6) . ?
C27 C26 1.404(6) . ?
C28 C31 1.429(6) . ?
C28 C29 1.440(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.406(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.362(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C32 H32 0.9300 . ?
C32 C33 1.409(8) . ?
C32 C31 1.344(7) . ?
C33 H33 0.9300 . ?
C33 C34 1.336(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C31 H31 0.9300 . ?
C6 H6 0.9300 . ?
C6 C7 1.341(6) . ?
C6 C5 1.406(7) . ?
C17 H17 0.9300 . ?
C17 C16 1.344(7) . ?
C25 C26 1.439(6) . ?
C25 C24 1.431(7) . ?
C25 C30 1.387(6) . ?
C7 H7 0.9300 . ?
C34 H34 0.9300 . ?
C34 C29 1.430(6) . ?
C16 H16 0.9300 . ?
C26 C21 1.425(6) . ?
C5 H5 0.9300 . ?
C29 C30 1.386(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C24 H24 0.9300 . ?
C24 C23 1.347(8) . ?
C21 H21 0.9300 . ?
C21 C22 1.343(7) . ?
C23 H23 0.9300 . ?
C23 C22 1.409(9) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C22 H22 0.9300 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br4 Pb1 Br5 81.562(12) . 2_655 ?
Br4 Pb1 Br2 92.132(12) . 4_645 ?
Br1 Pb1 Br4 173.332(13) . . ?
Br1 Pb1 Br5 101.271(12) . 2_655 ?
Br1 Pb1 Br2 82.298(13) . 4_645 ?
Br1 Pb1 Br3 99.116(14) . . ?
Br2 Pb1 Br4 85.083(12) . . ?
Br2 Pb1 Br5 163.194(12) . 2_655 ?
Br2 Pb1 Br5 82.834(12) 4_645 2_655 ?
Br2 Pb1 Br1 93.118(13) . . ?
Br2 Pb1 Br2 107.911(4) . 4_645 ?
Br2 Pb1 Br3 89.145(13) . . ?
Br3 Pb1 Br4 87.290(14) . . ?
Br3 Pb1 Br5 80.108(13) . 2_655 ?
Br3 Pb1 Br2 162.832(13) . 4_645 ?
Br4 Pb2 Br4 173.876(19) 2_655 . ?
Br4 Pb2 Br3 86.702(12) 2_655 2_655 ?
Br4 Pb2 Br3 86.703(12) . . ?
Br4 Pb2 Br3 89.714(12) . 2_655 ?
Br4 Pb2 Br3 89.714(12) 2_655 . ?
Br5 Pb2 Br4 84.749(11) . 2_655 ?
Br5 Pb2 Br4 99.630(12) . . ?
Br5 Pb2 Br4 84.749(11) 2_655 . ?
Br5 Pb2 Br4 99.632(12) 2_655 2_655 ?
Br5 Pb2 Br5 89.633(19) . 2_655 ?
Br5 Pb2 Br3 81.380(14) 2_655 . ?
Br5 Pb2 Br3 81.380(14) . 2_655 ?
Br5 Pb2 Br3 168.527(15) . . ?
Br5 Pb2 Br3 168.527(15) 2_655 2_655 ?
Br3 Pb2 Br3 108.38(2) 2_655 . ?
Pb2 Br4 Pb1 80.099(10) . . ?
Pb2 Br5 Pb1 79.076(10) . 2_655 ?
Pb1 Br2 Pb1 177.231(17) . 4_655 ?
Pb1 Br3 Pb2 78.432(11) . . ?
C3 N1 H1 107.5 . . ?
C1 N1 H1 107.5 . . ?
C1 N1 C3 111.4(3) . . ?
C2 N1 H1 107.5 . . ?
C2 N1 C3 111.4(3) . . ?
C2 N1 C1 111.3(3) . . ?
C20 N2 H2 107.6 . . ?
C20 N2 C19 110.0(4) . . ?
C18 N2 H2 107.6 . . ?
C18 N2 C20 113.8(3) . . ?
C18 N2 C19 109.9(4) . . ?
C19 N2 H2 107.6 . . ?
C35 O1 H1D 109.5 . . ?
C14 C11 C12 116.7(3) . . ?
C10 C11 C12 120.0(3) . . ?
C10 C11 C14 123.2(3) . . ?
C13 C12 C11 117.6(3) . . ?
C13 C12 C17 123.7(4) . . ?
C17 C12 C11 118.8(4) . . ?
C10 C9 C8 120.0(3) . . ?
C10 C9 C4 123.3(3) . . ?
C4 C9 C8 116.8(3) . . ?
C11 C14 H14 118.8 . . ?
C15 C14 C11 122.3(4) . . ?
C15 C14 H14 118.8 . . ?
C11 C10 C9 120.6(3) . . ?
C11 C10 C3 117.9(3) . . ?
C9 C10 C3 121.5(3) . . ?
C13 C8 C9 118.0(4) . . ?
C13 C8 C7 123.3(4) . . ?
C7 C8 C9 118.8(4) . . ?
C12 C13 Cl1 117.9(3) . . ?
C8 C13 Cl1 118.2(3) . . ?
C8 C13 C12 123.9(4) . . ?
C28 C27 C20 119.0(4) . . ?
C26 C27 C28 120.3(4) . . ?
C26 C27 C20 120.7(4) . . ?
C27 C28 C31 122.9(4) . . ?
C27 C28 C29 120.0(4) . . ?
C31 C28 C29 117.1(4) . . ?
C14 C15 H15 119.8 . . ?
C14 C15 C16 120.4(4) . . ?
C16 C15 H15 119.8 . . ?
C9 C4 H4 118.8 . . ?
C5 C4 C9 122.4(4) . . ?
C5 C4 H4 118.8 . . ?
N1 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
C10 C3 N1 111.8(3) . . ?
C10 C3 H3A 109.3 . . ?
C10 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C31 C32 C33 120.3(5) . . ?
C32 C33 H33 119.4 . . ?
C34 C33 C32 121.2(5) . . ?
C34 C33 H33 119.4 . . ?
N2 C20 C27 113.9(3) . . ?
N2 C20 H20A 108.8 . . ?
N2 C20 H20B 108.8 . . ?
C27 C20 H20A 108.8 . . ?
C27 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C28 C31 H31 119.1 . . ?
C32 C31 C28 121.8(5) . . ?
C32 C31 H31 119.1 . . ?
C7 C6 H6 119.6 . . ?
C7 C6 C5 120.7(4) . . ?
C5 C6 H6 119.6 . . ?
C12 C17 H17 119.4 . . ?
C16 C17 C12 121.2(4) . . ?
C16 C17 H17 119.4 . . ?
C24 C25 C26 118.6(4) . . ?
C30 C25 C26 118.1(4) . . ?
C30 C25 C24 123.3(5) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 C8 121.7(4) . . ?
C6 C7 H7 119.2 . . ?
C33 C34 H34 119.6 . . ?
C33 C34 C29 120.8(5) . . ?
C29 C34 H34 119.6 . . ?
C15 C16 H16 119.7 . . ?
C17 C16 C15 120.5(4) . . ?
C17 C16 H16 119.7 . . ?
C27 C26 C25 120.0(4) . . ?
C27 C26 C21 122.6(4) . . ?
C21 C26 C25 117.4(4) . . ?
C4 C5 C6 119.6(4) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C34 C29 C28 118.8(4) . . ?
C30 C29 C28 118.0(4) . . ?
C30 C29 C34 123.2(4) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C25 C24 H24 119.7 . . ?
C23 C24 C25 120.6(5) . . ?
C23 C24 H24 119.7 . . ?
C26 C21 H21 119.0 . . ?
C22 C21 C26 122.1(5) . . ?
C22 C21 H21 119.0 . . ?
C24 C23 H23 119.4 . . ?
C24 C23 C22 121.2(5) . . ?
C22 C23 H23 119.4 . . ?
C25 C30 Cl2 118.0(4) . . ?
C29 C30 Cl2 118.4(3) . . ?
C29 C30 C25 123.6(4) . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C22 C23 120.1(5) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O1 C35 H35A 109.5 . . ?
O1 C35 H35B 109.5 . . ?
O1 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 C12 C13 Cl1 179.5(3) . . . . ?
C11 C12 C13 C8 -0.5(7) . . . . ?
C11 C12 C17 C16 1.5(7) . . . . ?
C11 C14 C15 C16 0.2(7) . . . . ?
C11 C10 C3 N1 82.2(4) . . . . ?
C12 C11 C14 C15 0.4(6) . . . . ?
C12 C11 C10 C9 1.1(5) . . . . ?
C12 C11 C10 C3 -179.5(3) . . . . ?
C12 C17 C16 C15 -0.9(8) . . . . ?
C9 C10 C3 N1 -98.3(4) . . . . ?
C9 C8 C13 Cl1 -179.1(3) . . . . ?
C9 C8 C13 C12 0.8(7) . . . . ?
C9 C8 C7 C6 1.4(7) . . . . ?
C9 C4 C5 C6 0.3(7) . . . . ?
C14 C11 C12 C13 177.9(4) . . . . ?
C14 C11 C12 C17 -1.2(6) . . . . ?
C14 C11 C10 C9 -177.2(4) . . . . ?
C14 C11 C10 C3 2.3(5) . . . . ?
C14 C15 C16 C17 0.1(8) . . . . ?
C10 C11 C12 C13 -0.5(6) . . . . ?
C10 C11 C12 C17 -179.6(4) . . . . ?
C10 C11 C14 C15 178.7(4) . . . . ?
C10 C9 C8 C13 -0.2(6) . . . . ?
C10 C9 C8 C7 179.5(4) . . . . ?
C10 C9 C4 C5 179.6(4) . . . . ?
C8 C9 C10 C11 -0.7(5) . . . . ?
C8 C9 C10 C3 179.8(3) . . . . ?
C8 C9 C4 C5 -0.5(6) . . . . ?
C13 C12 C17 C16 -177.5(5) . . . . ?
C13 C8 C7 C6 -178.9(5) . . . . ?
C27 C28 C31 C32 -179.1(4) . . . . ?
C27 C28 C29 C34 -179.8(4) . . . . ?
C27 C28 C29 C30 0.1(6) . . . . ?
C27 C26 C21 C22 -179.0(5) . . . . ?
C28 C27 C20 N2 -83.3(4) . . . . ?
C28 C27 C26 C25 -0.1(6) . . . . ?
C28 C27 C26 C21 -179.4(4) . . . . ?
C28 C29 C30 Cl2 179.6(3) . . . . ?
C28 C29 C30 C25 -0.8(7) . . . . ?
C4 C9 C10 C11 179.2(3) . . . . ?
C4 C9 C10 C3 -0.3(6) . . . . ?
C4 C9 C8 C13 179.9(4) . . . . ?
C4 C9 C8 C7 -0.4(6) . . . . ?
C32 C33 C34 C29 0.6(9) . . . . ?
C33 C32 C31 C28 -0.8(8) . . . . ?
C33 C34 C29 C28 -1.4(8) . . . . ?
C33 C34 C29 C30 178.7(6) . . . . ?
C20 C27 C28 C31 1.8(6) . . . . ?
C20 C27 C28 C29 -177.3(4) . . . . ?
C20 C27 C26 C25 177.4(4) . . . . ?
C20 C27 C26 C21 -1.9(6) . . . . ?
C31 C28 C29 C34 1.1(6) . . . . ?
C31 C28 C29 C30 -179.1(4) . . . . ?
C31 C32 C33 C34 0.5(9) . . . . ?
C17 C12 C13 Cl1 -1.5(6) . . . . ?
C17 C12 C13 C8 178.6(4) . . . . ?
C25 C26 C21 C22 1.7(8) . . . . ?
C25 C24 C23 C22 0.3(11) . . . . ?
C7 C8 C13 Cl1 1.2(6) . . . . ?
C7 C8 C13 C12 -178.9(4) . . . . ?
C7 C6 C5 C4 0.8(8) . . . . ?
C34 C29 C30 Cl2 -0.5(7) . . . . ?
C34 C29 C30 C25 179.1(5) . . . . ?
C26 C27 C28 C31 179.4(4) . . . . ?
C26 C27 C28 C29 0.3(6) . . . . ?
C26 C27 C20 N2 99.2(4) . . . . ?
C26 C25 C24 C23 0.5(9) . . . . ?
C26 C25 C30 Cl2 -179.4(4) . . . . ?
C26 C25 C30 C29 1.0(7) . . . . ?
C26 C21 C22 C23 -1.0(10) . . . . ?
C5 C6 C7 C8 -1.6(8) . . . . ?
C29 C28 C31 C32 0.0(6) . . . . ?
C1 N1 C3 C10 78.6(4) . . . . ?
C24 C25 C26 C27 179.3(5) . . . . ?
C24 C25 C26 C21 -1.4(7) . . . . ?
C24 C25 C30 Cl2 0.8(7) . . . . ?
C24 C25 C30 C29 -178.8(5) . . . . ?
C24 C23 C22 C21 0.0(11) . . . . ?
C30 C25 C26 C27 -0.5(7) . . . . ?
C30 C25 C26 C21 178.8(5) . . . . ?
C30 C25 C24 C23 -179.8(6) . . . . ?
C18 N2 C20 C27 -65.9(5) . . . . ?
C2 N1 C3 C10 -156.4(3) . . . . ?
C19 N2 C20 C27 170.3(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.716
_oxdiff_exptl_absorpt_empirical_full_min 0.615
####################################################################### 
# 
# 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_1-C5
_database_code_depnum_ccdc_archive 'CCDC 2240929'
loop_
_audit_author_name
_audit_author_address
'Binbin Luo'
;Shantou University
China
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
_audit_creation_date             2023-01-08
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'Br10 Pb3, 4(C17 H17 Cl N), 2(C5 H12 O)'
_chemical_formula_sum            'C78 H92 Br10 Cl4 N4 O2 Pb3'
_chemical_formula_weight         2680.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Cl Pb Br '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.5945(4)
_cell_length_b                   9.8290(2)
_cell_length_c                   41.2029(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.467(2)
_cell_angle_gamma                90
_cell_volume                     8737.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15236
_cell_measurement_temperature    297.99(10)
_cell_measurement_theta_max      70.7500
_cell_measurement_theta_min      4.3130
_shelx_estimated_absorpt_T_max   0.841
_shelx_estimated_absorpt_T_min   0.124
_exptl_absorpt_coefficient_mu    17.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (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    2.037
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5072
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            21234
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.909
_diffrn_reflns_theta_min         4.098
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00  22.00   0.50   11.59    --    0.00 -57.00  60.00   82
  2  ω     35.00  83.00   0.50   11.59    --    0.00  77.00 -90.00   96
  3  ω    -88.00 -50.00   0.50   11.59    --    0.00 -57.00  60.00   76
  4  ω    -18.00  22.00   0.50   11.59    --    0.00  77.00 -90.00   80
  5  ω     22.00  93.00   0.50   46.37    --   89.30 -30.00 150.00  142
  6  ω      0.00 107.00   0.50   46.37    --   89.30 -30.00 -30.00  214
  7  ω     20.00 122.00   0.50   46.37    --   89.30 -82.00-180.00  204
  8  ω     25.00  92.00   0.50   46.37    --   89.30 -82.00 150.00  134
  9  ω     49.00 114.00   0.50   46.37    --   89.30 -61.00-180.00  130
 10  ω     25.00 117.00   0.50   46.37    --   89.30 -15.00  30.00  184
;
_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      0.0306700000
_diffrn_orient_matrix_UB_12      -0.0102630000
_diffrn_orient_matrix_UB_13      0.0343065000
_diffrn_orient_matrix_UB_21      0.0641644000
_diffrn_orient_matrix_UB_22      -0.0117922000
_diffrn_orient_matrix_UB_23      -0.0149710000
_diffrn_orient_matrix_UB_31      0.0068499000
_diffrn_orient_matrix_UB_32      0.1558077000
_diffrn_orient_matrix_UB_33      0.0011215000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7354
_reflns_number_total             8139
_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 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.745
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8139
_refine_ls_number_restraints     150
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0301
_refine_ls_restrained_S_all      1.136
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0380P)²+45.6175P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0825
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O1B-C39B
 1.44 with sigma of 0.02
 O1A-C37A
 3.1 with sigma of 0.02
 C38B-C36B
 2.56 with sigma of 0.02
 C38A-C35A
 3.1 with sigma of 0.02
 C39B-C37B = C37B-C35B
 2.56 with sigma of 0.02
 C38A-C39A = C38A-C37A = C36A-C37A = C36A-C35A
 1.54 with sigma of 0.02
 C38B-C39B = C37B-C38B = C37B-C36B = C36B-C35B
 1.54 with sigma of 0.02
 C39A-C36A
 3.1 with sigma of 0.02
 C39A-C37A = C37A-C35A
 2.56 with sigma of 0.02
 C38B-C35B
 3.1 with sigma of 0.02
 O1A-C38A = C38A-C36A
 2.56 with sigma of 0.02
 C39B-C36B
 3.1 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
O1A \\sim C39A \\sim C38A \\sim C37A \\sim C36A \\sim C35A: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Uanis(O1B) \\sim Ueq, Uanis(C39B) \\sim Ueq, Uanis(C38B) \\sim Ueq, Uanis(C37B)
\\sim Ueq, Uanis(C36B) \\sim Ueq, Uanis(C35B) \\sim Ueq: with sigma of 0.001
and sigma for terminal atoms of 0.002
Uanis(C39A) \\sim Ueq, Uanis(C38A) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(C37A)
\\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(C35A) \\sim Ueq: with sigma of 0.001
and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 O1B, C39B, C37B, C38B, C36B, C35B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: C37A(0.4) H37A(0.4) H37B(0.4) O1A(0.4) H1A(0.4) C36A(0.4)
 H36A(0.4) H36B(0.4) C35A(0.4) H35A(0.4) H35B(0.4) H35C(0.4) C39A(0.4)
 H39A(0.4) H39B(0.4) C38A(0.4) H38A(0.4) H38B(0.4) O1B(0.6) H1B(0.6) C39B(0.6)
 H39C(0.6) H39D(0.6) C38B(0.6) H38C(0.6) H38D(0.6) C35B(0.6) H35D(0.6)
 H35E(0.6) H35F(0.6) C36B(0.6) H36C(0.6) H36D(0.6) C37B(0.6) H37C(0.6) H37D(0.6)
5.a Everything fixed:
 H1B
5.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
5.c Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C32(H32A,H32B), C37A(H37A,H37B), C36A(H36A,H36B), C39A(H39A,
 H39B), C38A(H38A,H38B), C39B(H39C,H39D), C38B(H38C,H38D), C36B(H36C,H36D),
 C37B(H37C,H37D)
5.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C27(H27), C23(H23), C6(H6), C11(H11), C5(H5), C4(H4), C28(H28),
 C20(H20), C22(H22), C21(H21), C12(H12), C13(H13), C3(H3), C29(H29), C30(H30)
5.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C35A(H35A,H35B,H35C), C35B(H35D,H35E,H35F)
5.f Idealised tetrahedral OH refined as rotating group:
 O1A(H1A)
;
_atom_sites_solution_hydrogens   mixed
_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
Pb2 Pb 0.67502(2) 0.19704(2) 0.72885(2) 0.03861(7) Uani 1 1 d . . . . .
Pb1 Pb 0.500000 0.19276(3) 0.750000 0.04116(8) Uani 1 2 d S T P . .
Br3 Br 0.61418(3) 0.21087(6) 0.79461(2) 0.05160(14) Uani 1 1 d . . . . .
Br4 Br 0.75321(2) -0.05937(6) 0.74950(2) 0.05327(14) Uani 1 1 d . . . . .
Br5 Br 0.74608(3) 0.17328(6) 0.66835(2) 0.05525(15) Uani 1 1 d . . . . .
Br2 Br 0.57020(3) -0.02243(6) 0.71647(2) 0.05569(15) Uani 1 1 d . . . . .
Br1 Br 0.57127(3) 0.37838(7) 0.70260(2) 0.06766(18) Uani 1 1 d . . . . .
Cl1 Cl 0.90917(9) 0.23456(18) 0.52930(4) 0.0759(5) Uani 1 1 d . . . . .
Cl2 Cl 0.57352(10) 0.7741(2) 0.49775(4) 0.0804(5) Uani 1 1 d . . . . .
N1 N 0.8960(2) 0.1986(4) 0.69402(10) 0.0449(10) Uani 1 1 d . . . . .
H1 H 0.861391 0.156634 0.681501 0.054 Uiso 1 1 calc R U . . .
C25 C 0.6127(2) 0.7727(5) 0.60703(12) 0.0411(10) Uani 1 1 d . . . . .
C15 C 0.9541(2) 0.1826(5) 0.67468(12) 0.0422(11) Uani 1 1 d . . . . .
H15A H 0.984427 0.249860 0.682012 0.051 Uiso 1 1 calc R U . . .
H15B H 0.971759 0.093237 0.678878 0.051 Uiso 1 1 calc R U . . .
C8 C 0.9412(2) 0.1990(5) 0.63860(12) 0.0388(10) Uani 1 1 d . . . . .
C10 C 0.9767(2) 0.4406(5) 0.63980(14) 0.0500(12) Uani 1 1 d . . . . .
H10 H 0.983951 0.436113 0.662191 0.060 Uiso 1 1 calc R U . . .
C9 C 0.9538(2) 0.3234(5) 0.62289(12) 0.0398(10) Uani 1 1 d . . . . .
C17 C 0.8808(3) 0.3457(6) 0.69857(16) 0.0614(15) Uani 1 1 d . . . . .
H17A H 0.914623 0.389835 0.710181 0.092 Uiso 1 1 calc R U . . .
H17B H 0.843990 0.353471 0.710714 0.092 Uiso 1 1 calc R U . . .
H17C H 0.873977 0.388045 0.677729 0.092 Uiso 1 1 calc R U . . .
C32 C 0.6230(2) 0.7698(5) 0.64349(12) 0.0453(11) Uani 1 1 d . . . . .
H32A H 0.620498 0.862027 0.651710 0.054 Uiso 1 1 calc R U . . .
H32B H 0.590038 0.717570 0.652760 0.054 Uiso 1 1 calc R U . . .
C24 C 0.5908(2) 0.6535(5) 0.59125(12) 0.0410(10) Uani 1 1 d . . . . .
C7 C 0.9184(2) 0.0869(5) 0.62071(12) 0.0425(10) Uani 1 1 d . . . . .
C26 C 0.6222(2) 0.8912(5) 0.58927(13) 0.0456(11) Uani 1 1 d . . . . .
C1 C 0.9206(3) 0.2214(6) 0.57128(12) 0.0488(12) Uani 1 1 d . . . . .
C27 C 0.6443(3) 1.0152(6) 0.60354(15) 0.0601(15) Uani 1 1 d . . . . .
H27 H 0.652295 1.018279 0.625887 0.072 Uiso 1 1 calc R U . . .
C14 C 0.9432(2) 0.3348(5) 0.58839(12) 0.0437(11) Uani 1 1 d . . . . .
C16 C 0.9026(3) 0.1273(8) 0.72574(15) 0.0753(19) Uani 1 1 d . . . . .
H16A H 0.910253 0.032387 0.722137 0.113 Uiso 1 1 calc R U . . .
H16B H 0.865132 0.137562 0.737242 0.113 Uiso 1 1 calc R U . . .
H16C H 0.936644 0.165761 0.738365 0.113 Uiso 1 1 calc R U . . .
C23 C 0.5799(2) 0.5296(6) 0.60834(14) 0.0523(13) Uani 1 1 d . . . . .
H23 H 0.587549 0.526666 0.630712 0.063 Uiso 1 1 calc R U . . .
C6 C 0.9063(3) -0.0422(5) 0.63525(14) 0.0530(13) Uani 1 1 d . . . . .
H6 H 0.912896 -0.053074 0.657557 0.064 Uiso 1 1 calc R U . . .
C11 C 0.9882(3) 0.5586(6) 0.62416(16) 0.0621(15) Uani 1 1 d . . . . .
H11 H 1.003348 0.633120 0.635925 0.075 Uiso 1 1 calc R U . . .
C31 C 0.6097(3) 0.8924(5) 0.55465(13) 0.0506(12) Uani 1 1 d . . . . .
C19 C 0.5786(2) 0.6535(5) 0.55696(13) 0.0476(12) Uani 1 1 d . . . . .
C5 C 0.8855(3) -0.1484(6) 0.61710(17) 0.0660(16) Uani 1 1 d . . . . .
H5 H 0.878762 -0.231559 0.627130 0.079 Uiso 1 1 calc R U . . .
C2 C 0.9072(2) 0.0986(5) 0.58624(12) 0.0468(11) Uani 1 1 d . . . . .
C18 C 0.5887(3) 0.7725(6) 0.53982(13) 0.0519(13) Uani 1 1 d . . . . .
C4 C 0.8739(3) -0.1363(7) 0.58349(17) 0.0726(19) Uani 1 1 d . . . . .
H4 H 0.858880 -0.210364 0.571499 0.087 Uiso 1 1 calc R U . . .
C28 C 0.6539(4) 1.1280(6) 0.58585(18) 0.077(2) Uani 1 1 d . . . . .
H28 H 0.669020 1.206434 0.596056 0.093 Uiso 1 1 calc R U . . .
C20 C 0.5564(3) 0.5316(6) 0.54148(15) 0.0627(16) Uani 1 1 d . . . . .
H20 H 0.548710 0.530724 0.519098 0.075 Uiso 1 1 calc R U . . .
C22 C 0.5585(3) 0.4160(6) 0.59262(18) 0.0662(16) Uani 1 1 d . . . . .
H22 H 0.551851 0.336632 0.604242 0.079 Uiso 1 1 calc R U . . .
C21 C 0.5465(3) 0.4187(7) 0.55873(17) 0.0709(18) Uani 1 1 d . . . . .
H21 H 0.531457 0.340984 0.548194 0.085 Uiso 1 1 calc R U . . .
C12 C 0.9777(3) 0.5696(6) 0.59049(17) 0.0670(16) Uani 1 1 d . . . . .
H12 H 0.985090 0.651787 0.580143 0.080 Uiso 1 1 calc R U . . .
C13 C 0.9567(3) 0.4610(6) 0.57287(15) 0.0576(14) Uani 1 1 d . . . . .
H13 H 0.951034 0.468704 0.550443 0.069 Uiso 1 1 calc R U . . .
C3 C 0.8845(3) -0.0173(6) 0.56867(15) 0.0661(16) Uani 1 1 d . . . . .
H3 H 0.876906 -0.010379 0.546344 0.079 Uiso 1 1 calc R U . . .
C29 C 0.6413(4) 1.1280(7) 0.5521(2) 0.085(2) Uani 1 1 d . . . . .
H29 H 0.647670 1.206727 0.540145 0.102 Uiso 1 1 calc R U . . .
C30 C 0.6201(3) 1.0149(7) 0.53695(16) 0.0720(18) Uani 1 1 d . . . . .
H30 H 0.612140 1.016308 0.514589 0.086 Uiso 1 1 calc R U . . .
C37A C 0.7456(15) 0.569(2) 0.5589(5) 0.171(5) Uani 0.4 1 d D U P A 1
H37A H 0.766827 0.638834 0.547096 0.205 Uiso 0.4 1 calc R U P A 1
H37B H 0.719534 0.611049 0.574579 0.205 Uiso 0.4 1 calc R U P A 1
O1A O 0.7409(16) 0.472(4) 0.6316(6) 0.169(5) Uani 0.4 1 d D U P A 1
H1A H 0.710604 0.424441 0.634561 0.254 Uiso 0.4 1 calc R U P A 1
C36A C 0.7067(12) 0.474(4) 0.5351(6) 0.171(5) Uani 0.4 1 d D U P A 1
H36A H 0.705131 0.382729 0.544099 0.205 Uiso 0.4 1 calc R U P A 1
H36B H 0.664559 0.507739 0.532608 0.205 Uiso 0.4 1 calc R U P A 1
N2 N 0.6841(2) 0.7098(4) 0.65468(11) 0.0461(10) Uani 1 1 d . . . . .
H2 H 0.689338 0.624451 0.642815 0.055 Uiso 1 1 calc R U . . .
C33 C 0.7379(3) 0.7991(6) 0.6478(2) 0.0708(19) Uani 1 1 d . . . . .
H33A H 0.736382 0.822738 0.625144 0.106 Uiso 1 1 calc R U . . .
H33B H 0.775823 0.751613 0.653112 0.106 Uiso 1 1 calc R U . . .
H33C H 0.736061 0.880385 0.660612 0.106 Uiso 1 1 calc R U . . .
C34 C 0.6850(4) 0.6765(7) 0.68993(15) 0.076(2) Uani 1 1 d . . . . .
H34A H 0.680623 0.758581 0.702238 0.114 Uiso 1 1 calc R U . . .
H34B H 0.723650 0.633488 0.696172 0.114 Uiso 1 1 calc R U . . .
H34C H 0.651434 0.615920 0.694106 0.114 Uiso 1 1 calc R U . . .
C35A C 0.7345(15) 0.469(4) 0.5029(6) 0.169(5) Uani 0.4 1 d D U P A 1
H35A H 0.776189 0.502389 0.504756 0.254 Uiso 0.4 1 calc R U P A 1
H35B H 0.710518 0.523599 0.487795 0.254 Uiso 0.4 1 calc R U P A 1
H35C H 0.734825 0.376178 0.495335 0.254 Uiso 0.4 1 calc R U P A 1
C39A C 0.7693(16) 0.427(4) 0.6072(6) 0.170(5) Uani 0.4 1 d D U P A 1
H39A H 0.744725 0.347667 0.601309 0.204 Uiso 0.4 1 calc R U P A 1
H39B H 0.806889 0.390897 0.617617 0.204 Uiso 0.4 1 calc R U P A 1
C38A C 0.7915(11) 0.469(4) 0.5753(6) 0.170(5) Uani 0.4 1 d D U P A 1
H38A H 0.796147 0.390121 0.561603 0.205 Uiso 0.4 1 calc R U P A 1
H38B H 0.831761 0.512793 0.578210 0.205 Uiso 0.4 1 calc R U P A 1
O1B O 0.7300(4) 0.4653(10) 0.6329(2) 0.0611(16) Uani 0.6 1 d D U P B 2
H1B H 0.711900 0.547740 0.620390 0.092 Uiso 0.6 1 d . U P C 2
C39B C 0.7897(5) 0.4641(14) 0.6163(3) 0.0794(19) Uani 0.6 1 d D U P B 2
H39C H 0.822349 0.499682 0.630823 0.095 Uiso 0.6 1 calc R U P B 2
H39D H 0.800343 0.371433 0.610696 0.095 Uiso 0.6 1 calc R U P B 2
C38B C 0.7848(7) 0.5445(14) 0.5878(3) 0.091(2) Uani 0.6 1 d D U P B 2
H38C H 0.825240 0.561455 0.579264 0.109 Uiso 0.6 1 calc R U P B 2
H38D H 0.764815 0.630791 0.591928 0.109 Uiso 0.6 1 calc R U P B 2
C35B C 0.7359(9) 0.5853(19) 0.5127(3) 0.124(3) Uani 0.6 1 d D U P B 2
H35D H 0.726547 0.663847 0.525460 0.186 Uiso 0.6 1 calc R U P B 2
H35E H 0.698346 0.550236 0.502574 0.186 Uiso 0.6 1 calc R U P B 2
H35F H 0.763971 0.610466 0.496280 0.186 Uiso 0.6 1 calc R U P B 2
C36B C 0.7644(8) 0.4816(17) 0.5336(3) 0.115(2) Uani 0.6 1 d D U P B 2
H36C H 0.761523 0.396592 0.521661 0.138 Uiso 0.6 1 calc R U P B 2
H36D H 0.808123 0.503803 0.535990 0.138 Uiso 0.6 1 calc R U P B 2
C37B C 0.7445(7) 0.4555(15) 0.5643(3) 0.103(2) Uani 0.6 1 d D U P B 2
H37C H 0.749705 0.359906 0.569624 0.124 Uiso 0.6 1 calc R U P B 2
H37D H 0.701028 0.478870 0.565678 0.124 Uiso 0.6 1 calc R U P B 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
Pb2 Br3 3.0645(6) . ?
Pb2 Br4 3.1309(6) . ?
Pb2 Br4 2.9684(6) 4_656 ?
Pb2 Br5 2.9923(6) . ?
Pb2 Br2 3.1524(6) . ?
Pb2 Br1 3.0263(6) . ?
Pb1 Br3 3.0166(6) . ?
Pb1 Br3 3.0166(5) 2_656 ?
Pb1 Br2 2.9766(6) . ?
Pb1 Br2 2.9766(6) 2_656 ?
Pb1 Br1 3.1258(7) . ?
Pb1 Br1 3.1259(7) 2_656 ?
Cl1 C1 1.741(5) . ?
Cl2 C18 1.750(5) . ?
N1 H1 0.9800 . ?
N1 C15 1.524(6) . ?
N1 C17 1.495(7) . ?
N1 C16 1.485(7) . ?
C25 C32 1.509(7) . ?
C25 C24 1.411(7) . ?
C25 C26 1.396(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C8 1.510(7) . ?
C8 C9 1.415(7) . ?
C8 C7 1.403(7) . ?
C10 H10 0.9300 . ?
C10 C9 1.424(7) . ?
C10 C11 1.355(8) . ?
C9 C14 1.434(7) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 N2 1.500(6) . ?
C24 C23 1.431(7) . ?
C24 C19 1.426(7) . ?
C7 C6 1.432(7) . ?
C7 C2 1.435(7) . ?
C26 C27 1.425(7) . ?
C26 C31 1.441(7) . ?
C1 C14 1.395(7) . ?
C1 C2 1.392(7) . ?
C27 H27 0.9300 . ?
C27 C28 1.349(9) . ?
C14 C13 1.432(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C23 H23 0.9300 . ?
C23 C22 1.362(8) . ?
C6 H6 0.9300 . ?
C6 C5 1.349(8) . ?
C11 H11 0.9300 . ?
C11 C12 1.400(9) . ?
C31 C18 1.395(8) . ?
C31 C30 1.430(8) . ?
C19 C18 1.388(8) . ?
C19 C20 1.430(7) . ?
C5 H5 0.9300 . ?
C5 C4 1.402(9) . ?
C2 C3 1.425(8) . ?
C4 H4 0.9300 . ?
C4 C3 1.344(9) . ?
C28 H28 0.9300 . ?
C28 C29 1.406(10) . ?
C20 H20 0.9300 . ?
C20 C21 1.340(9) . ?
C22 H22 0.9300 . ?
C22 C21 1.409(9) . ?
C21 H21 0.9300 . ?
C12 H12 0.9300 . ?
C12 C13 1.358(9) . ?
C13 H13 0.9300 . ?
C3 H3 0.9300 . ?
C29 H29 0.9300 . ?
C29 C30 1.346(10) . ?
C30 H30 0.9300 . ?
C37A H37A 0.9700 . ?
C37A H37B 0.9700 . ?
C37A C36A 1.571(18) . ?
C37A C38A 1.528(18) . ?
O1A H1A 0.8200 . ?
O1A C39A 1.28(3) . ?
C36A H36A 0.9700 . ?
C36A H36B 0.9700 . ?
C36A C35A 1.478(18) . ?
N2 H2 0.9800 . ?
N2 C33 1.492(7) . ?
N2 C34 1.488(7) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35A H35A 0.9600 . ?
C35A H35B 0.9600 . ?
C35A H35C 0.9600 . ?
C39A H39A 0.9700 . ?
C39A H39B 0.9700 . ?
C39A C38A 1.478(17) . ?
C38A H38A 0.9700 . ?
C38A H38B 0.9700 . ?
O1B H1B 1.0271 . ?
O1B C39B 1.485(13) . ?
C39B H39C 0.9700 . ?
C39B H39D 0.9700 . ?
C39B C38B 1.415(13) . ?
C38B H38C 0.9700 . ?
C38B H38D 0.9700 . ?
C38B C37B 1.546(14) . ?
C35B H35D 0.9600 . ?
C35B H35E 0.9600 . ?
C35B H35F 0.9600 . ?
C35B C36B 1.453(15) . ?
C36B H36C 0.9700 . ?
C36B H36D 0.9700 . ?
C36B C37B 1.379(13) . ?
C37B H37C 0.9700 . ?
C37B H37D 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 Pb2 Br4 92.420(16) . . ?
Br3 Pb2 Br2 80.866(16) . . ?
Br4 Pb2 Br3 86.366(16) 4_656 . ?
Br4 Pb2 Br4 107.405(6) 4_656 . ?
Br4 Pb2 Br5 91.922(17) 4_656 . ?
Br4 Pb2 Br2 82.427(15) . . ?
Br4 Pb2 Br2 164.266(17) 4_656 . ?
Br4 Pb2 Br1 90.077(18) 4_656 . ?
Br5 Pb2 Br3 174.142(17) . . ?
Br5 Pb2 Br4 82.738(17) . . ?
Br5 Pb2 Br2 101.666(16) . . ?
Br5 Pb2 Br1 98.42(2) . . ?
Br1 Pb2 Br3 87.190(19) . . ?
Br1 Pb2 Br4 162.462(18) . . ?
Br1 Pb2 Br2 80.200(17) . . ?
Br3 Pb1 Br3 173.23(2) . 2_656 ?
Br3 Pb1 Br1 89.791(16) . 2_656 ?
Br3 Pb1 Br1 86.259(17) 2_656 2_656 ?
Br3 Pb1 Br1 89.791(16) 2_656 . ?
Br3 Pb1 Br1 86.260(17) . . ?
Br2 Pb1 Br3 100.278(16) . 2_656 ?
Br2 Pb1 Br3 100.276(16) 2_656 . ?
Br2 Pb1 Br3 84.575(16) 2_656 2_656 ?
Br2 Pb1 Br3 84.575(16) . . ?
Br2 Pb1 Br2 89.44(3) . 2_656 ?
Br2 Pb1 Br1 168.24(2) 2_656 . ?
Br2 Pb1 Br1 81.400(19) 2_656 2_656 ?
Br2 Pb1 Br1 81.401(19) . . ?
Br2 Pb1 Br1 168.24(2) . 2_656 ?
Br1 Pb1 Br1 108.58(3) . 2_656 ?
Pb1 Br3 Pb2 80.152(14) . . ?
Pb2 Br4 Pb2 178.04(2) 4_646 . ?
Pb1 Br2 Pb2 79.347(14) . . ?
Pb2 Br1 Pb1 79.030(15) . . ?
C15 N1 H1 107.9 . . ?
C17 N1 H1 107.9 . . ?
C17 N1 C15 110.8(4) . . ?
C16 N1 H1 107.9 . . ?
C16 N1 C15 111.2(5) . . ?
C16 N1 C17 111.1(5) . . ?
C24 C25 C32 118.4(5) . . ?
C26 C25 C32 121.2(4) . . ?
C26 C25 C24 120.4(4) . . ?
N1 C15 H15A 109.1 . . ?
N1 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
C8 C15 N1 112.5(4) . . ?
C8 C15 H15A 109.1 . . ?
C8 C15 H15B 109.1 . . ?
C9 C8 C15 120.8(4) . . ?
C7 C8 C15 118.6(4) . . ?
C7 C8 C9 120.6(4) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C11 C10 C9 121.8(5) . . ?
C8 C9 C10 123.0(5) . . ?
C8 C9 C14 119.7(4) . . ?
C10 C9 C14 117.3(5) . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C25 C32 H32A 108.8 . . ?
C25 C32 H32B 108.8 . . ?
H32A C32 H32B 107.7 . . ?
N2 C32 C25 113.8(4) . . ?
N2 C32 H32A 108.8 . . ?
N2 C32 H32B 108.8 . . ?
C25 C24 C23 122.6(5) . . ?
C25 C24 C19 120.0(5) . . ?
C19 C24 C23 117.4(5) . . ?
C8 C7 C6 122.8(5) . . ?
C8 C7 C2 119.8(4) . . ?
C6 C7 C2 117.3(5) . . ?
C25 C26 C27 123.5(5) . . ?
C25 C26 C31 120.0(4) . . ?
C27 C26 C31 116.5(5) . . ?
C14 C1 Cl1 118.3(4) . . ?
C2 C1 Cl1 118.7(4) . . ?
C2 C1 C14 122.9(5) . . ?
C26 C27 H27 118.8 . . ?
C28 C27 C26 122.5(6) . . ?
C28 C27 H27 118.8 . . ?
C1 C14 C9 118.4(5) . . ?
C1 C14 C13 122.7(5) . . ?
C13 C14 C9 118.9(5) . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C24 C23 H23 119.2 . . ?
C22 C23 C24 121.6(6) . . ?
C22 C23 H23 119.2 . . ?
C7 C6 H6 119.5 . . ?
C5 C6 C7 121.0(5) . . ?
C5 C6 H6 119.5 . . ?
C10 C11 H11 119.6 . . ?
C10 C11 C12 120.8(6) . . ?
C12 C11 H11 119.6 . . ?
C18 C31 C26 118.1(5) . . ?
C18 C31 C30 122.9(5) . . ?
C30 C31 C26 119.0(5) . . ?
C24 C19 C20 119.1(5) . . ?
C18 C19 C24 118.5(5) . . ?
C18 C19 C20 122.4(5) . . ?
C6 C5 H5 119.2 . . ?
C6 C5 C4 121.5(6) . . ?
C4 C5 H5 119.2 . . ?
C1 C2 C7 118.6(5) . . ?
C1 C2 C3 122.8(5) . . ?
C3 C2 C7 118.6(5) . . ?
C31 C18 Cl2 118.0(4) . . ?
C19 C18 Cl2 119.0(4) . . ?
C19 C18 C31 123.0(5) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 C5 119.7(6) . . ?
C3 C4 H4 120.1 . . ?
C27 C28 H28 119.8 . . ?
C27 C28 C29 120.5(6) . . ?
C29 C28 H28 119.8 . . ?
C19 C20 H20 119.5 . . ?
C21 C20 C19 121.0(6) . . ?
C21 C20 H20 119.5 . . ?
C23 C22 H22 120.0 . . ?
C23 C22 C21 120.0(6) . . ?
C21 C22 H22 120.0 . . ?
C20 C21 C22 120.9(6) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.3(6) . . ?
C13 C12 H12 119.8 . . ?
C14 C13 H13 119.6 . . ?
C12 C13 C14 120.8(6) . . ?
C12 C13 H13 119.6 . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.8(6) . . ?
C4 C3 H3 119.1 . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.4(6) . . ?
C30 C29 H29 119.8 . . ?
C31 C30 H30 119.4 . . ?
C29 C30 C31 121.1(6) . . ?
C29 C30 H30 119.4 . . ?
H37A C37A H37B 109.2 . . ?
C36A C37A H37A 111.3 . . ?
C36A C37A H37B 111.3 . . ?
C38A C37A H37A 111.3 . . ?
C38A C37A H37B 111.3 . . ?
C38A C37A C36A 102.6(15) . . ?
C39A O1A H1A 109.5 . . ?
C37A C36A H36A 109.5 . . ?
C37A C36A H36B 109.5 . . ?
H36A C36A H36B 108.1 . . ?
C35A C36A C37A 110.7(17) . . ?
C35A C36A H36A 109.5 . . ?
C35A C36A H36B 109.5 . . ?
C32 N2 H2 107.5 . . ?
C33 N2 C32 113.0(4) . . ?
C33 N2 H2 107.5 . . ?
C34 N2 C32 111.2(5) . . ?
C34 N2 H2 107.5 . . ?
C34 N2 C33 109.8(5) . . ?
N2 C33 H33A 109.5 . . ?
N2 C33 H33B 109.5 . . ?
N2 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N2 C34 H34A 109.5 . . ?
N2 C34 H34B 109.5 . . ?
N2 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36A C35A H35A 109.5 . . ?
C36A C35A H35B 109.5 . . ?
C36A C35A H35C 109.5 . . ?
H35A C35A H35B 109.5 . . ?
H35A C35A H35C 109.5 . . ?
H35B C35A H35C 109.5 . . ?
O1A C39A H39A 101.5 . . ?
O1A C39A H39B 101.5 . . ?
O1A C39A C38A 142(3) . . ?
H39A C39A H39B 104.6 . . ?
C38A C39A H39A 101.5 . . ?
C38A C39A H39B 101.5 . . ?
C37A C38A H38A 109.6 . . ?
C37A C38A H38B 109.6 . . ?
C39A C38A C37A 110.1(15) . . ?
C39A C38A H38A 109.6 . . ?
C39A C38A H38B 109.6 . . ?
H38A C38A H38B 108.2 . . ?
C39B O1B H1B 95.5 . . ?
O1B C39B H39C 109.7 . . ?
O1B C39B H39D 109.7 . . ?
H39C C39B H39D 108.2 . . ?
C38B C39B O1B 110.0(10) . . ?
C38B C39B H39C 109.7 . . ?
C38B C39B H39D 109.7 . . ?
C39B C38B H38C 111.2 . . ?
C39B C38B H38D 111.2 . . ?
C39B C38B C37B 102.9(10) . . ?
H38C C38B H38D 109.1 . . ?
C37B C38B H38C 111.2 . . ?
C37B C38B H38D 111.2 . . ?
H35D C35B H35E 109.5 . . ?
H35D C35B H35F 109.5 . . ?
H35E C35B H35F 109.5 . . ?
C36B C35B H35D 109.5 . . ?
C36B C35B H35E 109.5 . . ?
C36B C35B H35F 109.5 . . ?
C35B C36B H36C 106.8 . . ?
C35B C36B H36D 106.8 . . ?
H36C C36B H36D 106.6 . . ?
C37B C36B C35B 122.2(14) . . ?
C37B C36B H36C 106.8 . . ?
C37B C36B H36D 106.8 . . ?
C38B C37B H37C 110.5 . . ?
C38B C37B H37D 110.5 . . ?
C36B C37B C38B 106.3(11) . . ?
C36B C37B H37C 110.5 . . ?
C36B C37B H37D 110.5 . . ?
H37C C37B H37D 108.7 . . ?

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
Cl1 C1 C14 C9 -178.8(4) . . . . ?
Cl1 C1 C14 C13 0.6(8) . . . . ?
Cl1 C1 C2 C7 178.2(4) . . . . ?
Cl1 C1 C2 C3 0.2(8) . . . . ?
N1 C15 C8 C9 99.7(5) . . . . ?
N1 C15 C8 C7 -82.6(5) . . . . ?
C25 C32 N2 C33 70.9(6) . . . . ?
C25 C32 N2 C34 -165.2(5) . . . . ?
C25 C24 C23 C22 179.7(5) . . . . ?
C25 C24 C19 C18 0.0(8) . . . . ?
C25 C24 C19 C20 -179.9(5) . . . . ?
C25 C26 C27 C28 179.1(6) . . . . ?
C25 C26 C31 C18 -0.6(8) . . . . ?
C25 C26 C31 C30 -179.7(6) . . . . ?
C15 C8 C9 C10 -2.5(7) . . . . ?
C15 C8 C9 C14 177.7(4) . . . . ?
C15 C8 C7 C6 0.6(7) . . . . ?
C15 C8 C7 C2 -178.5(4) . . . . ?
C8 C9 C14 C1 -0.1(7) . . . . ?
C8 C9 C14 C13 -179.5(5) . . . . ?
C8 C7 C6 C5 -178.7(6) . . . . ?
C8 C7 C2 C1 1.4(8) . . . . ?
C8 C7 C2 C3 179.5(5) . . . . ?
C10 C9 C14 C1 -179.8(5) . . . . ?
C10 C9 C14 C13 0.7(7) . . . . ?
C10 C11 C12 C13 -1.2(10) . . . . ?
C9 C8 C7 C6 178.4(5) . . . . ?
C9 C8 C7 C2 -0.7(7) . . . . ?
C9 C10 C11 C12 0.3(9) . . . . ?
C9 C14 C13 C12 -1.7(9) . . . . ?
C17 N1 C15 C8 -80.1(5) . . . . ?
C32 C25 C24 C23 -1.9(7) . . . . ?
C32 C25 C24 C19 178.0(5) . . . . ?
C32 C25 C26 C27 2.4(8) . . . . ?
C32 C25 C26 C31 -177.6(5) . . . . ?
C24 C25 C32 N2 82.6(6) . . . . ?
C24 C25 C26 C27 -179.9(5) . . . . ?
C24 C25 C26 C31 0.0(8) . . . . ?
C24 C23 C22 C21 -0.2(10) . . . . ?
C24 C19 C18 Cl2 -179.7(4) . . . . ?
C24 C19 C18 C31 -0.6(9) . . . . ?
C24 C19 C20 C21 0.6(9) . . . . ?
C7 C8 C9 C10 179.8(5) . . . . ?
C7 C8 C9 C14 0.0(7) . . . . ?
C7 C6 C5 C4 -1.1(10) . . . . ?
C7 C2 C3 C4 -0.3(10) . . . . ?
C26 C25 C32 N2 -99.7(6) . . . . ?
C26 C25 C24 C23 -179.6(5) . . . . ?
C26 C25 C24 C19 0.3(7) . . . . ?
C26 C27 C28 C29 1.1(12) . . . . ?
C26 C31 C18 Cl2 -180.0(4) . . . . ?
C26 C31 C18 C19 0.9(9) . . . . ?
C26 C31 C30 C29 0.0(11) . . . . ?
C1 C14 C13 C12 178.9(6) . . . . ?
C1 C2 C3 C4 177.6(7) . . . . ?
C27 C26 C31 C18 179.3(5) . . . . ?
C27 C26 C31 C30 0.3(8) . . . . ?
C27 C28 C29 C30 -0.8(13) . . . . ?
C14 C1 C2 C7 -1.5(8) . . . . ?
C14 C1 C2 C3 -179.5(6) . . . . ?
C16 N1 C15 C8 155.9(5) . . . . ?
C23 C24 C19 C18 179.9(5) . . . . ?
C23 C24 C19 C20 -0.1(8) . . . . ?
C23 C22 C21 C20 0.7(11) . . . . ?
C6 C7 C2 C1 -177.7(5) . . . . ?
C6 C7 C2 C3 0.3(8) . . . . ?
C6 C5 C4 C3 1.1(11) . . . . ?
C11 C10 C9 C8 -179.8(5) . . . . ?
C11 C10 C9 C14 -0.1(8) . . . . ?
C11 C12 C13 C14 1.9(10) . . . . ?
C31 C26 C27 C28 -0.8(9) . . . . ?
C19 C24 C23 C22 -0.1(8) . . . . ?
C19 C20 C21 C22 -0.9(11) . . . . ?
C5 C4 C3 C2 -0.4(11) . . . . ?
C2 C7 C6 C5 0.4(8) . . . . ?
C2 C1 C14 C9 0.9(8) . . . . ?
C2 C1 C14 C13 -179.7(5) . . . . ?
C18 C31 C30 C29 -179.0(7) . . . . ?
C18 C19 C20 C21 -179.3(6) . . . . ?
C28 C29 C30 C31 0.2(13) . . . . ?
C20 C19 C18 Cl2 0.2(8) . . . . ?
C20 C19 C18 C31 179.3(6) . . . . ?
C30 C31 C18 Cl2 -0.9(9) . . . . ?
C30 C31 C18 C19 179.9(6) . . . . ?
O1A C39A C38A C37A -36(6) . . . . ?
C36A C37A C38A C39A -98(2) . . . . ?
C38A C37A C36A C35A -91(2) . . . . ?
O1B C39B C38B C37B -73.4(13) . . . . ?
C39B C38B C37B C36B -147.4(13) . . . . ?
C35B C36B C37B C38B -92.6(18) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.449
_oxdiff_exptl_absorpt_empirical_full_min 0.574
####################################################################### 
# 
# 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. 
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#######################################################################

data_1-C7
_database_code_depnum_ccdc_archive 'CCDC 2240932'
loop_
_audit_author_name
_audit_author_address
'Binbin Luo'
;Shantou University
China
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
_audit_creation_date             2023-01-08
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Br10 Pb3, 4(C17 H17 Cl N), 2(H2 O), 2(C7 H16 O)'
_chemical_formula_sum            'C82 H104 Br10 Cl4 N4 O4 Pb3'
_chemical_formula_weight         2772.16
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Cl Pb Br'
_chemical_oxdiff_usercomment     c7oh
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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.5955(4)
_cell_length_b                   9.98480(10)
_cell_length_c                   22.1409(4)
_cell_angle_alpha                90
_cell_angle_beta                 115.695(2)
_cell_angle_gamma                90
_cell_volume                     4501.29(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12002
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      70.6430
_cell_measurement_theta_min      4.3540
_shelx_estimated_absorpt_T_max   0.477
_shelx_estimated_absorpt_T_min   0.024
_exptl_absorpt_coefficient_mu    17.404
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'translucent light colourless'
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.83
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21474
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.280
_diffrn_reflns_theta_min         4.001
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     22.00  84.00   0.50    0.50    --    0.00  19.00 120.00  124
  2  ω    -11.00  16.00   0.50    0.50    --    0.00  19.00 120.00   54
  3  ω    -12.00  36.00   0.50    0.50    --    0.00  38.00  30.00   96
  4  ω     51.00  86.00   0.50    0.50    --    0.00  38.00  30.00   70
  5  ω      0.00 115.00   0.50    0.71    --   89.30 -77.00 -90.00  230
  6  ω     66.00 124.00   0.50    0.71    --   89.30  77.00  60.00  116
  7  ω     98.00 179.00   0.50    0.71    --   89.30  30.00 120.00  162
  8  ω      7.00  34.00   0.50    0.71    --   89.30 -30.00  30.00   54
  9  ω     59.00 103.00   0.50    0.71    --   89.30 -30.00  30.00   88
 10  ω     67.00  98.00   0.50    0.71    --   89.30  61.00  30.00   62
 11  ω    105.00 131.00   0.50    0.71    --   89.30  61.00  30.00   52
 12  ω    150.00 176.00   0.50    0.71    --   89.30  77.00  60.00   52
 13  ω     31.00 106.00   0.50    0.71    --   89.30 -30.00 -90.00  150
 14  ω      0.00  26.00   0.50    0.71    --   89.30 -30.00 -90.00   52
;
_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      0.0502318000
_diffrn_orient_matrix_UB_12      0.1146806000
_diffrn_orient_matrix_UB_13      0.0168652000
_diffrn_orient_matrix_UB_21      0.0485803000
_diffrn_orient_matrix_UB_22      -0.0795053000
_diffrn_orient_matrix_UB_23      0.0610198000
_diffrn_orient_matrix_UB_31      0.0289169000
_diffrn_orient_matrix_UB_32      -0.0658510000
_diffrn_orient_matrix_UB_33      -0.0442520000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7706
_reflns_number_total             8369
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.712
_refine_diff_density_min         -2.907
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8369
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0324
_refine_ls_restrained_S_all      1.112
_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)+(0.0597P)²+7.8996P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0981
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 H1WB-H1
 2.2 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C39A \\sim C38A \\sim C37A \\sim C36A \\sim C35A: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002 within 2A
C39B \\sim C38B \\sim C37B \\sim C36B \\sim C35B: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002 within 2A
Br5A \\sim Br5B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(Br5B) \\sim Ueq, Uanis(Br5A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Others
 Fixed Sof: Br5B(0.75) H40A(0.5) H40B(0.5) H40C(0.5) H40D(0.5) C36A(0.5)
 H36A(0.5) H36B(0.5) C39A(0.5) H39A(0.5) H39B(0.5) C35A(0.5) H35A(0.5)
 H35B(0.5) H35C(0.5) C38A(0.5) H38A(0.5) H38B(0.5) C37A(0.5) H37A(0.5)
 H37B(0.5) C36B(0.5) H36C(0.5) H36D(0.5) C38B(0.5) H38C(0.5) H38D(0.5)
 C35B(0.5) H35D(0.5) H35E(0.5) H35F(0.5) C39B(0.5) H39C(0.5) H39D(0.5)
 C37B(0.5) H37C(0.5) H37D(0.5) Br5A(0.25)
4.a Free rotating group:
 O1W(H1WA,H1WB)
4.b Ternary CH refined with riding coordinates:
 N2(H2A), N1(H1)
4.c Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C15(H15A,H15B), C41(H41A,H41B), C40(H40A,H40B), C40(H40C,
 H40D), C36A(H36A,H36B), C39A(H39A,H39B), C38A(H38A,H38B), C37A(H37A,H37B),
 C36B(H36C,H36D), C38B(H38C,H38D), C39B(H39C,H39D), C37B(H37C,H37D)
4.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C12(H12), C11(H11), C23(H23), C20(H20), C27(H27),
 C21(H21), C28(H28), C22(H22), C5(H5), C6(H6), C29(H29), C4(H4), C30(H30),
 C3(H3)
4.e Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C16(H16A,H16B,H16C), C33(H33A,H33B,H33C), C17(H17A,H17B,
 H17C), C35A(H35A,H35B,H35C), C35B(H35D,H35E,H35F)
4.f Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb2 Pb 0.45479(2) -0.01016(2) 0.30774(2) 0.01869(7) Uani 1 1 d . . . . .
Pb1 Pb 0.500000 0.000000 0.500000 0.02253(9) Uani 1 2 d S . P . .
Br1 Br 0.50320(2) 0.21990(5) 0.24306(2) 0.02442(11) Uani 1 1 d . . . . .
Br2 Br 0.59506(2) -0.00061(4) 0.43923(3) 0.02930(13) Uani 1 1 d . . . . .
Br4 Br 0.42683(2) 0.19966(5) 0.38974(2) 0.02759(12) Uani 1 1 d . . . . .
Br3 Br 0.42106(2) -0.20279(5) 0.39242(2) 0.02742(12) Uani 1 1 d . . . . .
Br5B Br 0.32669(5) 0.00178(11) 0.21196(4) 0.0237(2) Uani 0.75 1 d . U P A 1
Cl2 Cl -0.00097(6) 0.50668(10) 0.18233(6) 0.0292(3) Uani 1 1 d . . . . .
Cl1 Cl 0.05544(6) -0.00057(10) -0.13688(7) 0.0310(3) Uani 1 1 d . . . . .
O1W O 0.36979(17) 0.2118(3) 0.09917(17) 0.0355(8) Uani 1 1 d G . . . .
H1WA H 0.380585 0.277840 0.081867 0.053 Uiso 1 1 d G U . . .
H1WB H 0.399506 0.198331 0.138622 0.053 Uiso 1 1 d DG U . . .
O2 O 0.26275(15) 0.3215(4) 0.11110(17) 0.0366(8) Uani 1 1 d . . . . .
H2 H 0.297115 0.281531 0.115565 0.055 Uiso 1 1 calc R U . . .
N2 N 0.30946(18) 0.4850(3) 0.22039(19) 0.0193(8) Uani 1 1 d . . . . .
H2A H 0.280730 0.416445 0.188049 0.023 Uiso 1 1 calc R U . . .
N1 N 0.39030(19) -0.0185(4) 0.0449(2) 0.0271(9) Uani 1 1 d . . . . .
H1 H 0.369971 0.065347 0.052056 0.033 Uiso 1 1 calc DR U . . .
C10 C 0.2863(2) 0.1920(4) -0.0737(2) 0.0256(9) Uani 1 1 d . . . . .
H10 H 0.332691 0.184610 -0.055694 0.031 Uiso 1 1 calc R U . . .
C9 C 0.24831(19) 0.0761(4) -0.07467(19) 0.0206(8) Uani 1 1 d . . . . .
C32 C 0.2943(2) 0.4850(4) 0.2805(2) 0.0185(9) Uani 1 1 d . . . . .
H32A H 0.312298 0.402562 0.307064 0.022 Uiso 1 1 calc R U . . .
H32B H 0.315916 0.562768 0.309398 0.022 Uiso 1 1 calc R U . . .
C8 C 0.2772(2) -0.0491(5) -0.0500(2) 0.0232(9) Uani 1 1 d . . . . .
C14 C 0.17833(18) 0.0926(4) -0.10182(19) 0.0187(8) Uani 1 1 d . . . . .
C25 C 0.2213(2) 0.4915(4) 0.2599(2) 0.0189(9) Uani 1 1 d . . . . .
C24 C 0.1840(2) 0.3741(4) 0.2354(2) 0.0200(8) Uani 1 1 d . . . . .
C15 C 0.3504(2) -0.0641(5) -0.0262(2) 0.0266(9) Uani 1 1 d . . . . .
H15A H 0.360467 -0.159418 -0.029912 0.032 Uiso 1 1 calc R U . . .
H15B H 0.363838 -0.011796 -0.056198 0.032 Uiso 1 1 calc R U . . .
C34 C 0.3790(2) 0.4459(5) 0.2401(2) 0.0301(10) Uani 1 1 d . . . . .
H34A H 0.408284 0.507580 0.274537 0.045 Uiso 1 1 calc R U . . .
H34B H 0.388284 0.449981 0.200793 0.045 Uiso 1 1 calc R U . . .
H34C H 0.386288 0.354465 0.257923 0.045 Uiso 1 1 calc R U . . .
C16 C 0.3920(3) -0.1186(6) 0.0947(2) 0.0428(13) Uani 1 1 d . . . . .
H16A H 0.412528 -0.201089 0.089096 0.064 Uiso 1 1 calc R U . . .
H16B H 0.347076 -0.137877 0.088219 0.064 Uiso 1 1 calc R U . . .
H16C H 0.417454 -0.083137 0.140003 0.064 Uiso 1 1 calc R U . . .
C26 C 0.1911(2) 0.6121(4) 0.2641(2) 0.0213(9) Uani 1 1 d . . . . .
C13 C 0.1503(2) 0.2207(4) -0.1272(2) 0.0237(9) Uani 1 1 d . . . . .
H13 H 0.104000 0.231717 -0.146049 0.028 Uiso 1 1 calc R U . . .
C33 C 0.2951(2) 0.6163(5) 0.1856(2) 0.0327(10) Uani 1 1 d . . . . .
H33A H 0.248854 0.639166 0.171509 0.049 Uiso 1 1 calc R U . . .
H33B H 0.304069 0.611041 0.146089 0.049 Uiso 1 1 calc R U . . .
H33C H 0.323017 0.685383 0.216091 0.049 Uiso 1 1 calc R U . . .
C19 C 0.1136(2) 0.3779(4) 0.2117(2) 0.0218(9) Uani 1 1 d . . . . .
C18 C 0.0845(2) 0.4995(4) 0.2145(2) 0.0212(10) Uani 1 1 d . . . . .
C12 C 0.1887(2) 0.3265(5) -0.1247(2) 0.0339(11) Uani 1 1 d . . . . .
H12 H 0.169270 0.411247 -0.141044 0.041 Uiso 1 1 calc R U . . .
C11 C 0.2577(2) 0.3111(5) -0.0977(3) 0.0349(11) Uani 1 1 d . . . . .
H11 H 0.284256 0.385758 -0.096537 0.042 Uiso 1 1 calc R U . . .
C23 C 0.2124(2) 0.2486(4) 0.2316(2) 0.0242(9) Uani 1 1 d . . . . .
H23 H 0.258770 0.242314 0.247825 0.029 Uiso 1 1 calc R U . . .
C20 C 0.0763(2) 0.2583(5) 0.1854(2) 0.0274(9) Uani 1 1 d . . . . .
H20 H 0.029959 0.259800 0.170195 0.033 Uiso 1 1 calc R U . . .
C1 C 0.1404(2) -0.0196(5) -0.1028(2) 0.0252(10) Uani 1 1 d . . . . .
C27 C 0.2269(2) 0.7332(4) 0.2908(2) 0.0242(9) Uani 1 1 d . . . . .
H27 H 0.273165 0.733356 0.306077 0.029 Uiso 1 1 calc R U . . .
C31 C 0.1209(2) 0.6169(4) 0.2413(2) 0.0206(8) Uani 1 1 d . . . . .
C21 C 0.1062(2) 0.1434(5) 0.1819(2) 0.0313(10) Uani 1 1 d . . . . .
H21 H 0.080725 0.065347 0.163525 0.038 Uiso 1 1 calc R U . . .
C28 C 0.1965(2) 0.8475(5) 0.2948(2) 0.0309(10) Uani 1 1 d . . . . .
H28 H 0.221690 0.925953 0.313083 0.037 Uiso 1 1 calc R U . . .
C22 C 0.1753(2) 0.1383(5) 0.2055(2) 0.0305(10) Uani 1 1 d . . . . .
H22 H 0.195759 0.056654 0.203080 0.037 Uiso 1 1 calc R U . . .
C17 C 0.4590(3) 0.0137(6) 0.0553(4) 0.0458(15) Uani 1 1 d . . . . .
H17A H 0.457560 0.081454 0.022693 0.069 Uiso 1 1 calc R U . . .
H17B H 0.480073 -0.067611 0.049290 0.069 Uiso 1 1 calc R U . . .
H17C H 0.484066 0.048364 0.100811 0.069 Uiso 1 1 calc R U . . .
C7 C 0.2378(2) -0.1590(5) -0.0503(2) 0.0290(10) Uani 1 1 d . . . . .
C5 C 0.2259(3) -0.3931(6) -0.0243(3) 0.0565(17) Uani 1 1 d . . . . .
H5 H 0.245132 -0.476921 -0.005900 0.068 Uiso 1 1 calc R U . . .
C6 C 0.2643(3) -0.2885(5) -0.0245(3) 0.0441(14) Uani 1 1 d . . . . .
H6 H 0.310456 -0.301632 -0.006894 0.053 Uiso 1 1 calc R U . . .
C2 C 0.1673(2) -0.1433(5) -0.0776(2) 0.0286(10) Uani 1 1 d . . . . .
C29 C 0.1272(2) 0.8512(5) 0.2719(3) 0.0334(11) Uani 1 1 d . . . . .
H29 H 0.106402 0.932072 0.274850 0.040 Uiso 1 1 calc R U . . .
C41 C 0.2070(2) 0.2482(6) 0.0665(2) 0.0369(11) Uani 1 1 d . . . . .
H41A H 0.205453 0.160341 0.086529 0.044 Uiso 1 1 calc R U . . .
H41B H 0.210028 0.232098 0.023869 0.044 Uiso 1 1 calc R U . . .
C4 C 0.1570(3) -0.3758(6) -0.0518(3) 0.0528(16) Uani 1 1 d . . . . .
H4 H 0.130037 -0.449066 -0.052042 0.063 Uiso 1 1 calc R U . . .
C30 C 0.0906(2) 0.7399(5) 0.2459(2) 0.0273(9) Uani 1 1 d . . . . .
H30 H 0.044314 0.743585 0.230537 0.033 Uiso 1 1 calc R U . . .
C3 C 0.1285(2) -0.2561(5) -0.0780(2) 0.0382(12) Uani 1 1 d . . . . .
H3 H 0.082101 -0.247675 -0.096796 0.046 Uiso 1 1 calc R U . . .
C40 C 0.1461(2) 0.3253(6) 0.0534(3) 0.0453(14) Uani 1 1 d . . . . .
H40A H 0.143916 0.333638 0.096908 0.054 Uiso 0.5 1 calc R U P B 1
H40B H 0.153106 0.416838 0.040498 0.054 Uiso 0.5 1 calc R U P B 1
H40C H 0.142261 0.405039 0.025320 0.054 Uiso 0.5 1 calc R U P C 2
H40D H 0.145260 0.354244 0.095755 0.054 Uiso 0.5 1 calc R U P C 2
C36A C -0.0633(5) 0.1643(12) -0.0451(5) 0.0372(13) Uani 0.5 1 d . U P D 1
H36A H -0.036603 0.100755 -0.057216 0.045 Uiso 0.5 1 calc R U P D 1
H36B H -0.054714 0.147279 0.002084 0.045 Uiso 0.5 1 calc R U P D 1
C39A C 0.0808(5) 0.2835(12) 0.0043(5) 0.0379(13) Uani 0.5 1 d . U P D 1
H39A H 0.075299 0.188005 0.012912 0.046 Uiso 0.5 1 calc R U P D 1
H39B H 0.080059 0.288542 -0.040618 0.046 Uiso 0.5 1 calc R U P D 1
C35A C -0.1357(5) 0.1429(13) -0.0905(6) 0.0375(16) Uani 0.5 1 d . U P D 1
H35A H -0.144909 0.169222 -0.136396 0.056 Uiso 0.5 1 calc R U P D 1
H35B H -0.162165 0.197419 -0.074672 0.056 Uiso 0.5 1 calc R U P D 1
H35C H -0.146687 0.048087 -0.089881 0.056 Uiso 0.5 1 calc R U P D 1
C38A C 0.0218(5) 0.3578(12) 0.0013(5) 0.0379(12) Uani 0.5 1 d . U P D 1
H38A H 0.027206 0.453915 -0.006001 0.046 Uiso 0.5 1 calc R U P D 1
H38B H 0.020585 0.349391 0.045288 0.046 Uiso 0.5 1 calc R U P D 1
C37A C -0.0437(5) 0.3115(11) -0.0526(5) 0.0379(12) Uani 0.5 1 d . U P D 1
H37A H -0.042564 0.320147 -0.096623 0.045 Uiso 0.5 1 calc R U P D 1
H37B H -0.078314 0.372349 -0.052739 0.045 Uiso 0.5 1 calc R U P D 1
C36B C -0.1032(5) 0.2549(12) -0.0638(5) 0.0439(14) Uani 0.5 1 d . U P D 2
H36C H -0.102815 0.312749 -0.027294 0.053 Uiso 0.5 1 calc R U P D 2
H36D H -0.111274 0.312992 -0.102832 0.053 Uiso 0.5 1 calc R U P D 2
C38B C 0.0227(5) 0.2793(12) -0.0100(5) 0.0428(13) Uani 0.5 1 d . U P D 2
H38C H 0.019181 0.348760 -0.043339 0.051 Uiso 0.5 1 calc R U P D 2
H38D H 0.020771 0.325922 0.028565 0.051 Uiso 0.5 1 calc R U P D 2
C35B C -0.1582(6) 0.1571(13) -0.0827(6) 0.0456(18) Uani 0.5 1 d . U P D 2
H35D H -0.166134 0.115127 -0.125554 0.068 Uiso 0.5 1 calc R U P D 2
H35E H -0.197962 0.203782 -0.087014 0.068 Uiso 0.5 1 calc R U P D 2
H35F H -0.146538 0.088088 -0.047956 0.068 Uiso 0.5 1 calc R U P D 2
C39B C 0.0876(6) 0.2167(13) 0.0134(6) 0.0425(14) Uani 0.5 1 d . U P D 2
H39C H 0.093194 0.180514 -0.025459 0.051 Uiso 0.5 1 calc R U P D 2
H39D H 0.090830 0.141091 0.043613 0.051 Uiso 0.5 1 calc R U P D 2
C37B C -0.0371(6) 0.1902(13) -0.0412(6) 0.0434(13) Uani 0.5 1 d . U P D 2
H37C H -0.035821 0.144973 -0.080375 0.052 Uiso 0.5 1 calc R U P D 2
H37D H -0.033346 0.119709 -0.008241 0.052 Uiso 0.5 1 calc R U P D 2
Br5A Br 0.32802(19) -0.0135(4) 0.1901(2) 0.0453(8) Uani 0.25 1 d . U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb2 Br1 3.1436(4) . ?
Pb2 Br1 3.2182(5) 2_645 ?
Pb2 Br4 3.0132(5) . ?
Pb2 Br3 3.0058(5) . ?
Pb2 Br5B 2.7509(10) . ?
Pb2 Br5A 2.919(4) . ?
Pb1 Br2 2.9883(5) . ?
Pb1 Br2 2.9884(5) 3_656 ?
Pb1 Br4 3.0278(5) 3_656 ?
Pb1 Br4 3.0278(5) . ?
Pb1 Br3 3.0448(5) . ?
Pb1 Br3 3.0448(5) 3_656 ?
Cl2 C18 1.746(5) . ?
Cl1 C1 1.743(5) . ?
O1W H1WA 0.8498 . ?
O1W H1WB 0.8504 . ?
O2 H2 0.8400 . ?
O2 C41 1.421(5) . ?
N2 H2A 1.0000 . ?
N2 C32 1.513(6) . ?
N2 C34 1.490(5) . ?
N2 C33 1.483(5) . ?
N1 H1 1.0000 . ?
N1 C15 1.506(6) . ?
N1 C16 1.478(6) . ?
N1 C17 1.501(7) . ?
C10 H10 0.9500 . ?
C10 C9 1.435(6) . ?
C10 C11 1.347(6) . ?
C9 C8 1.407(6) . ?
C9 C14 1.437(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C25 1.510(6) . ?
C8 C15 1.511(6) . ?
C8 C7 1.411(6) . ?
C14 C13 1.430(6) . ?
C14 C1 1.405(6) . ?
C25 C24 1.408(6) . ?
C25 C26 1.407(6) . ?
C24 C19 1.444(5) . ?
C24 C23 1.428(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C26 C27 1.431(6) . ?
C26 C31 1.443(5) . ?
C13 H13 0.9500 . ?
C13 C12 1.352(6) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C19 C18 1.395(6) . ?
C19 C20 1.432(6) . ?
C18 C31 1.406(6) . ?
C12 H12 0.9500 . ?
C12 C11 1.417(6) . ?
C11 H11 0.9500 . ?
C23 H23 0.9500 . ?
C23 C22 1.353(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.351(7) . ?
C1 C2 1.382(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.355(6) . ?
C31 C30 1.431(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.416(6) . ?
C28 H28 0.9500 . ?
C28 C29 1.422(6) . ?
C22 H22 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C7 C6 1.436(6) . ?
C7 C2 1.447(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.359(8) . ?
C5 C4 1.416(8) . ?
C6 H6 0.9500 . ?
C2 C3 1.424(6) . ?
C29 H29 0.9500 . ?
C29 C30 1.355(6) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C40 1.489(7) . ?
C4 H4 0.9500 . ?
C4 C3 1.362(7) . ?
C30 H30 0.9500 . ?
C3 H3 0.9500 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 H40C 0.9900 . ?
C40 H40D 0.9900 . ?
C40 C39A 1.465(12) . ?
C40 C39B 1.642(13) . ?
C36A H36A 0.9900 . ?
C36A H36B 0.9900 . ?
C36A C35A 1.518(14) . ?
C36A C37A 1.565(16) . ?
C39A H39A 0.9900 . ?
C39A H39B 0.9900 . ?
C39A C38A 1.501(15) . ?
C35A H35A 0.9800 . ?
C35A H35B 0.9800 . ?
C35A H35C 0.9800 . ?
C38A H38A 0.9900 . ?
C38A H38B 0.9900 . ?
C38A C37A 1.514(13) . ?
C37A H37A 0.9900 . ?
C37A H37B 0.9900 . ?
C36B H36C 0.9900 . ?
C36B H36D 0.9900 . ?
C36B C35B 1.490(17) . ?
C36B C37B 1.500(15) . ?
C38B H38C 0.9900 . ?
C38B H38D 0.9900 . ?
C38B C39B 1.468(15) . ?
C38B C37B 1.512(16) . ?
C35B H35D 0.9800 . ?
C35B H35E 0.9800 . ?
C35B H35F 0.9800 . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
C37B H37C 0.9900 . ?
C37B H37D 0.9900 . ?

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 Pb2 Br1 103.836(5) . 2_645 ?
Br4 Pb2 Br1 88.382(13) . . ?
Br4 Pb2 Br1 164.491(13) . 2_645 ?
Br3 Pb2 Br1 82.822(13) . 2_645 ?
Br3 Pb2 Br1 169.791(14) . . ?
Br3 Pb2 Br4 83.854(15) . . ?
Br5B Pb2 Br1 97.94(2) . 2_645 ?
Br5B Pb2 Br1 94.29(2) . . ?
Br5B Pb2 Br4 90.51(2) . . ?
Br5B Pb2 Br3 92.40(2) . . ?
Br5A Pb2 Br1 90.15(8) . . ?
Br5A Pb2 Br4 99.47(8) . . ?
Br5A Pb2 Br3 97.65(8) . . ?
Br2 Pb1 Br2 180.0 . 3_656 ?
Br2 Pb1 Br4 83.463(13) 3_656 3_656 ?
Br2 Pb1 Br4 96.538(13) . 3_656 ?
Br2 Pb1 Br4 96.535(13) 3_656 . ?
Br2 Pb1 Br4 83.464(13) . . ?
Br2 Pb1 Br3 86.449(13) . . ?
Br2 Pb1 Br3 93.550(13) 3_656 . ?
Br2 Pb1 Br3 86.450(13) 3_656 3_656 ?
Br2 Pb1 Br3 93.551(13) . 3_656 ?
Br4 Pb1 Br4 179.998(13) 3_656 . ?
Br4 Pb1 Br3 97.052(14) 3_656 . ?
Br4 Pb1 Br3 82.948(14) 3_656 3_656 ?
Br4 Pb1 Br3 82.948(14) . . ?
Br4 Pb1 Br3 97.053(14) . 3_656 ?
Br3 Pb1 Br3 179.999(16) . 3_656 ?
Pb2 Br1 Pb2 170.006(17) . 2_655 ?
Pb2 Br4 Pb1 81.034(12) . . ?
Pb2 Br3 Pb1 80.875(12) . . ?
H1WA O1W H1WB 109.4 . . ?
C41 O2 H2 109.5 . . ?
C32 N2 H2A 107.8 . . ?
C34 N2 H2A 107.8 . . ?
C34 N2 C32 110.8(3) . . ?
C33 N2 H2A 107.8 . . ?
C33 N2 C32 112.1(3) . . ?
C33 N2 C34 110.4(3) . . ?
C15 N1 H1 108.2 . . ?
C16 N1 H1 108.2 . . ?
C16 N1 C15 112.7(4) . . ?
C16 N1 C17 109.9(4) . . ?
C17 N1 H1 108.2 . . ?
C17 N1 C15 109.7(4) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C11 C10 C9 121.7(4) . . ?
C10 C9 C14 117.1(4) . . ?
C8 C9 C10 122.5(4) . . ?
C8 C9 C14 120.3(4) . . ?
N2 C32 H32A 109.3 . . ?
N2 C32 H32B 109.3 . . ?
H32A C32 H32B 108.0 . . ?
C25 C32 N2 111.6(4) . . ?
C25 C32 H32A 109.3 . . ?
C25 C32 H32B 109.3 . . ?
C9 C8 C15 118.4(4) . . ?
C9 C8 C7 120.3(4) . . ?
C7 C8 C15 121.2(4) . . ?
C13 C14 C9 119.1(4) . . ?
C1 C14 C9 117.9(4) . . ?
C1 C14 C13 123.0(4) . . ?
C24 C25 C32 118.2(4) . . ?
C26 C25 C32 121.0(4) . . ?
C26 C25 C24 120.8(4) . . ?
C25 C24 C19 119.9(4) . . ?
C25 C24 C23 123.0(4) . . ?
C23 C24 C19 117.1(4) . . ?
N1 C15 C8 113.7(4) . . ?
N1 C15 H15A 108.8 . . ?
N1 C15 H15B 108.8 . . ?
C8 C15 H15A 108.8 . . ?
C8 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
N2 C34 H34A 109.5 . . ?
N2 C34 H34B 109.5 . . ?
N2 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C25 C26 C27 123.2(4) . . ?
C25 C26 C31 119.8(4) . . ?
C27 C26 C31 117.1(4) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 C14 121.1(4) . . ?
C12 C13 H13 119.5 . . ?
N2 C33 H33A 109.5 . . ?
N2 C33 H33B 109.5 . . ?
N2 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C18 C19 C24 118.3(4) . . ?
C18 C19 C20 122.5(4) . . ?
C20 C19 C24 119.2(4) . . ?
C19 C18 Cl2 118.5(3) . . ?
C19 C18 C31 122.9(4) . . ?
C31 C18 Cl2 118.6(3) . . ?
C13 C12 H12 119.9 . . ?
C13 C12 C11 120.1(4) . . ?
C11 C12 H12 119.9 . . ?
C10 C11 C12 120.9(4) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C24 C23 H23 119.1 . . ?
C22 C23 C24 121.9(4) . . ?
C22 C23 H23 119.1 . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.6(4) . . ?
C21 C20 H20 119.7 . . ?
C14 C1 Cl1 118.0(3) . . ?
C2 C1 Cl1 118.7(3) . . ?
C2 C1 C14 123.3(4) . . ?
C26 C27 H27 119.1 . . ?
C28 C27 C26 121.8(4) . . ?
C28 C27 H27 119.1 . . ?
C18 C31 C26 118.3(4) . . ?
C18 C31 C30 122.4(4) . . ?
C30 C31 C26 119.4(4) . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.6(4) . . ?
C22 C21 H21 119.7 . . ?
C27 C28 H28 119.7 . . ?
C27 C28 C29 120.7(4) . . ?
C29 C28 H28 119.7 . . ?
C23 C22 C21 120.6(4) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C8 C7 C6 123.0(4) . . ?
C8 C7 C2 119.7(4) . . ?
C6 C7 C2 117.3(4) . . ?
C6 C5 H5 120.3 . . ?
C6 C5 C4 119.4(5) . . ?
C4 C5 H5 120.3 . . ?
C7 C6 H6 118.8 . . ?
C5 C6 C7 122.4(5) . . ?
C5 C6 H6 118.8 . . ?
C1 C2 C7 118.4(4) . . ?
C1 C2 C3 122.9(4) . . ?
C3 C2 C7 118.6(4) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 C28 120.3(4) . . ?
C30 C29 H29 119.9 . . ?
O2 C41 H41A 109.8 . . ?
O2 C41 H41B 109.8 . . ?
O2 C41 C40 109.6(4) . . ?
H41A C41 H41B 108.2 . . ?
C40 C41 H41A 109.8 . . ?
C40 C41 H41B 109.8 . . ?
C5 C4 H4 119.4 . . ?
C3 C4 C5 121.2(5) . . ?
C3 C4 H4 119.4 . . ?
C31 C30 H30 119.6 . . ?
C29 C30 C31 120.8(4) . . ?
C29 C30 H30 119.6 . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.1(5) . . ?
C4 C3 H3 119.5 . . ?
C41 C40 H40A 106.6 . . ?
C41 C40 H40B 106.6 . . ?
C41 C40 H40C 111.2 . . ?
C41 C40 H40D 111.2 . . ?
C41 C40 C39B 102.9(6) . . ?
H40A C40 H40B 106.5 . . ?
H40C C40 H40D 109.1 . . ?
C39A C40 C41 123.1(7) . . ?
C39A C40 H40A 106.6 . . ?
C39A C40 H40B 106.6 . . ?
C39B C40 H40C 111.2 . . ?
C39B C40 H40D 111.2 . . ?
H36A C36A H36B 108.2 . . ?
C35A C36A H36A 109.7 . . ?
C35A C36A H36B 109.7 . . ?
C35A C36A C37A 109.6(9) . . ?
C37A C36A H36A 109.7 . . ?
C37A C36A H36B 109.7 . . ?
C40 C39A H39A 107.6 . . ?
C40 C39A H39B 107.6 . . ?
C40 C39A C38A 118.9(9) . . ?
H39A C39A H39B 107.0 . . ?
C38A C39A H39A 107.6 . . ?
C38A C39A H39B 107.6 . . ?
C36A C35A H35A 109.5 . . ?
C36A C35A H35B 109.5 . . ?
C36A C35A H35C 109.5 . . ?
H35A C35A H35B 109.5 . . ?
H35A C35A H35C 109.5 . . ?
H35B C35A H35C 109.5 . . ?
C39A C38A H38A 108.4 . . ?
C39A C38A H38B 108.4 . . ?
C39A C38A C37A 115.5(9) . . ?
H38A C38A H38B 107.5 . . ?
C37A C38A H38A 108.4 . . ?
C37A C38A H38B 108.4 . . ?
C36A C37A H37A 108.4 . . ?
C36A C37A H37B 108.4 . . ?
C38A C37A C36A 115.4(9) . . ?
C38A C37A H37A 108.4 . . ?
C38A C37A H37B 108.4 . . ?
H37A C37A H37B 107.5 . . ?
H36C C36B H36D 107.7 . . ?
C35B C36B H36C 108.9 . . ?
C35B C36B H36D 108.9 . . ?
C35B C36B C37B 113.5(11) . . ?
C37B C36B H36C 108.9 . . ?
C37B C36B H36D 108.9 . . ?
H38C C38B H38D 107.2 . . ?
C39B C38B H38C 107.8 . . ?
C39B C38B H38D 107.8 . . ?
C39B C38B C37B 118.0(10) . . ?
C37B C38B H38C 107.8 . . ?
C37B C38B H38D 107.8 . . ?
C36B C35B H35D 109.5 . . ?
C36B C35B H35E 109.5 . . ?
C36B C35B H35F 109.5 . . ?
H35D C35B H35E 109.5 . . ?
H35D C35B H35F 109.5 . . ?
H35E C35B H35F 109.5 . . ?
C40 C39B H39C 109.5 . . ?
C40 C39B H39D 109.5 . . ?
C38B C39B C40 110.9(9) . . ?
C38B C39B H39C 109.5 . . ?
C38B C39B H39D 109.5 . . ?
H39C C39B H39D 108.0 . . ?
C36B C37B C38B 117.5(10) . . ?
C36B C37B H37C 107.9 . . ?
C36B C37B H37D 107.9 . . ?
C38B C37B H37C 107.9 . . ?
C38B C37B H37D 107.9 . . ?
H37C C37B H37D 107.2 . . ?

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
Cl2 C18 C31 C26 -176.4(3) . . . . ?
Cl2 C18 C31 C30 3.0(6) . . . . ?
Cl1 C1 C2 C7 179.0(4) . . . . ?
Cl1 C1 C2 C3 -0.3(7) . . . . ?
O2 C41 C40 C39A 173.7(7) . . . . ?
O2 C41 C40 C39B -170.1(6) . . . . ?
N2 C32 C25 C24 76.8(5) . . . . ?
N2 C32 C25 C26 -102.4(5) . . . . ?
C10 C9 C8 C15 -4.6(6) . . . . ?
C10 C9 C8 C7 178.2(4) . . . . ?
C10 C9 C14 C13 1.1(6) . . . . ?
C10 C9 C14 C1 -179.6(4) . . . . ?
C9 C10 C11 C12 0.3(8) . . . . ?
C9 C8 C15 N1 83.7(5) . . . . ?
C9 C8 C7 C6 -178.6(5) . . . . ?
C9 C8 C7 C2 1.3(7) . . . . ?
C9 C14 C13 C12 -1.3(6) . . . . ?
C9 C14 C1 Cl1 -179.0(3) . . . . ?
C9 C14 C1 C2 1.6(7) . . . . ?
C32 C25 C24 C19 -176.6(4) . . . . ?
C32 C25 C24 C23 2.4(6) . . . . ?
C32 C25 C26 C27 -3.1(7) . . . . ?
C32 C25 C26 C31 177.3(4) . . . . ?
C8 C9 C14 C13 -179.4(4) . . . . ?
C8 C9 C14 C1 -0.1(6) . . . . ?
C8 C7 C6 C5 179.0(6) . . . . ?
C8 C7 C2 C1 0.1(7) . . . . ?
C8 C7 C2 C3 179.4(4) . . . . ?
C14 C9 C8 C15 175.9(4) . . . . ?
C14 C9 C8 C7 -1.3(6) . . . . ?
C14 C13 C12 C11 1.1(7) . . . . ?
C14 C1 C2 C7 -1.6(7) . . . . ?
C14 C1 C2 C3 179.2(5) . . . . ?
C25 C24 C19 C18 -0.6(6) . . . . ?
C25 C24 C19 C20 178.5(4) . . . . ?
C25 C24 C23 C22 -177.5(4) . . . . ?
C25 C26 C27 C28 -179.4(4) . . . . ?
C25 C26 C31 C18 -0.7(6) . . . . ?
C25 C26 C31 C30 179.9(4) . . . . ?
C24 C25 C26 C27 177.8(4) . . . . ?
C24 C25 C26 C31 -1.9(6) . . . . ?
C24 C19 C18 Cl2 177.0(3) . . . . ?
C24 C19 C18 C31 -2.0(6) . . . . ?
C24 C19 C20 C21 -0.8(6) . . . . ?
C24 C23 C22 C21 -1.1(7) . . . . ?
C15 C8 C7 C6 4.3(7) . . . . ?
C15 C8 C7 C2 -175.8(4) . . . . ?
C34 N2 C32 C25 -166.4(3) . . . . ?
C16 N1 C15 C8 79.1(5) . . . . ?
C26 C25 C24 C19 2.5(6) . . . . ?
C26 C25 C24 C23 -178.4(4) . . . . ?
C26 C27 C28 C29 -0.5(7) . . . . ?
C26 C31 C30 C29 -0.5(7) . . . . ?
C13 C14 C1 Cl1 0.3(6) . . . . ?
C13 C14 C1 C2 -179.1(4) . . . . ?
C13 C12 C11 C10 -0.6(8) . . . . ?
C33 N2 C32 C25 69.7(4) . . . . ?
C19 C24 C23 C22 1.6(6) . . . . ?
C19 C18 C31 C26 2.7(6) . . . . ?
C19 C18 C31 C30 -177.9(4) . . . . ?
C19 C20 C21 C22 1.3(7) . . . . ?
C18 C19 C20 C21 178.3(4) . . . . ?
C18 C31 C30 C29 -179.9(4) . . . . ?
C11 C10 C9 C8 179.9(4) . . . . ?
C11 C10 C9 C14 -0.6(6) . . . . ?
C23 C24 C19 C18 -179.7(4) . . . . ?
C23 C24 C19 C20 -0.6(6) . . . . ?
C20 C19 C18 Cl2 -2.0(6) . . . . ?
C20 C19 C18 C31 178.9(4) . . . . ?
C20 C21 C22 C23 -0.4(7) . . . . ?
C1 C14 C13 C12 179.4(4) . . . . ?
C1 C2 C3 C4 -179.1(5) . . . . ?
C27 C26 C31 C18 179.7(4) . . . . ?
C27 C26 C31 C30 0.2(6) . . . . ?
C27 C28 C29 C30 0.2(8) . . . . ?
C31 C26 C27 C28 0.3(6) . . . . ?
C28 C29 C30 C31 0.3(7) . . . . ?
C17 N1 C15 C8 -158.1(4) . . . . ?
C7 C8 C15 N1 -99.1(5) . . . . ?
C7 C2 C3 C4 1.6(8) . . . . ?
C5 C4 C3 C2 -1.0(9) . . . . ?
C6 C7 C2 C1 180.0(5) . . . . ?
C6 C7 C2 C3 -0.7(7) . . . . ?
C6 C5 C4 C3 -0.5(10) . . . . ?
C2 C7 C6 C5 -0.8(8) . . . . ?
C41 C40 C39A C38A 172.0(8) . . . . ?
C41 C40 C39B C38B -174.3(8) . . . . ?
C4 C5 C6 C7 1.5(10) . . . . ?
C40 C39A C38A C37A 177.7(9) . . . . ?
C39A C38A C37A C36A 63.4(13) . . . . ?
C35A C36A C37A C38A 165.6(9) . . . . ?
C35B C36B C37B C38B -170.0(11) . . . . ?
C39B C38B C37B C36B 178.9(11) . . . . ?
C37B C38B C39B C40 -173.3(9) . . . . ?

_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 2.614
_oxdiff_exptl_absorpt_empirical_full_min 0.605
####################################################################### 
# 
# 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_1-C6
_database_code_depnum_ccdc_archive 'CCDC 2240936'
loop_
_audit_author_name
_audit_author_address
'Binbin Luo'
;Shantou University
China
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
_audit_creation_date             2023-01-08
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Br10 Pb3, 4(C17 H17 Cl N), 2(H2 O), 2(C6 H14 O)'
_chemical_formula_sum            'C80 H100 Br10 Cl4 N4 O4 Pb3'
_chemical_formula_weight         2744.10
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O Cl Br Pb'
_chemical_oxdiff_usercomment     c7oh
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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.6272(3)
_cell_length_b                   9.91720(10)
_cell_length_c                   22.1336(3)
_cell_angle_alpha                90
_cell_angle_beta                 117.360(2)
_cell_angle_gamma                90
_cell_volume                     4411.15(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11402
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.8790
_cell_measurement_theta_min      3.9700
_shelx_estimated_absorpt_T_max   0.537
_shelx_estimated_absorpt_T_min   0.046
_exptl_absorpt_coefficient_mu    17.752
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (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    2.066
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2608
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23043
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.168
_diffrn_reflns_theta_min         3.997
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  22.00   0.50    0.50    --    0.00 -57.00 -60.00   52
  2  ω    -21.00  15.00   0.50    0.50    --    0.00 -38.00 120.00   72
  3  ω    -78.00 -52.00   0.50    0.50    --    0.00 -38.00 120.00   52
  4  ω     -7.00  18.00   0.50    0.50    --    0.00  38.00-180.00   50
  5  ω     52.00  89.00   0.50    0.50    --    0.00  38.00-180.00   74
  6  ω    -88.00 -43.00   0.50    0.50    --    0.00 -57.00 -60.00   90
  7  ω     21.00 109.00   0.50    0.50    --   89.30 -45.00  60.00  176
  8  ω     37.00 106.00   0.50    0.50    --   89.30 -30.00-150.00  138
  9  ω     23.00  99.00   0.50    0.50    --   89.30 -30.00  60.00  152
 10  ω      3.00 113.00   0.50    0.50    --   89.30 -15.00-180.00  220
 11  ω    116.00 178.00   0.50    0.50    --   89.30  30.00 150.00  124
 12  ω     67.00 142.00   0.50    0.50    --   89.30  15.00  90.00  150
 13  ω    141.00 167.00   0.50    0.50    --   89.30  30.00 -60.00   52
 14  ω      5.00  42.00   0.50    0.50    --   89.30 -45.00 -30.00   74
;
_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      -0.0708261000
_diffrn_orient_matrix_UB_12      0.0275438000
_diffrn_orient_matrix_UB_13      -0.0569127000
_diffrn_orient_matrix_UB_21      0.0127956000
_diffrn_orient_matrix_UB_22      -0.0947490000
_diffrn_orient_matrix_UB_23      -0.0478771000
_diffrn_orient_matrix_UB_31      -0.0264461000
_diffrn_orient_matrix_UB_32      -0.1199747000
_diffrn_orient_matrix_UB_33      0.0247220000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7578
_reflns_number_total             8284
_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 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.280
_refine_diff_density_min         -2.380
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8284
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0344
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0576P)²+9.7512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0957
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 H1-H2A
 2.2 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C40B \\sim C39B \\sim C38B \\sim C37B: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
C37A \\sim C38A \\sim C39A \\sim C40A: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Br5B: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Br5B \\sim Br5A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(Br5B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: Br5B(0.75) H36A(0.75) H36B(0.75) H36C(0.25) H36D(0.25) C37A(0.75)
 H37A(0.75) H37B(0.75) C38A(0.75) H38A(0.75) H38B(0.75) C40A(0.75) H40A(0.75)
 H40B(0.75) H40C(0.75) C39A(0.75) H39A(0.75) H39B(0.75) C39B(0.25) H39C(0.25)
 H39D(0.25) C40B(0.25) H40D(0.25) H40E(0.25) H40F(0.25) C37B(0.25) H37C(0.25)
 H37D(0.25) C38B(0.25) H38C(0.25) H38D(0.25) Br5A(0.25)
4.a Free rotating group:
 O1W(H1WA,H1WB)
4.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
4.c Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C15(H15A,H15B), C35(H35A,H35B), C36(H36A,H36B), C36(H36C,
 H36D), C37A(H37A,H37B), C38A(H38A,H38B), C39A(H39A,H39B), C39B(H39C,H39D),
 C37B(H37C,H37D), C38B(H38C,H38D)
4.d Aromatic/amide H refined with riding coordinates:
 C27(H27), C30(H30), C28(H28), C29(H29), C23(H23), C11(H11), C4(H4), C5(H5),
 C3(H3), C12(H12), C13(H13), C20(H20), C6(H6), C10(H10), C22(H22), C21(H21)
4.e Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C34(H34A,H34B,
 H34C), C40A(H40A,H40B,H40C), C40B(H40D,H40E,H40F)
4.f Idealised tetrahedral OH refined as rotating group:
 O2(H2A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 1.000000 0.500000 1.000000 0.02167(8) Uani 1 2 d S . P . .
Pb2 Pb 0.95460(2) 0.48868(2) 0.80622(2) 0.01983(7) Uani 1 1 d . . . . .
Br4 Br 0.99668(2) 0.22220(5) 0.76052(3) 0.02707(12) Uani 1 1 d . . . . .
Br2 Br 0.90828(2) 0.31502(5) 0.88557(2) 0.02711(12) Uani 1 1 d . . . . .
Br3 Br 0.93504(3) 0.71185(5) 0.89072(3) 0.02908(12) Uani 1 1 d . . . . .
Br5B Br 0.81983(9) 0.5032(2) 0.70307(8) 0.0255(2) Uani 0.75 1 d . U P A 1
Br1 Br 0.91032(2) 0.53334(6) 1.06433(3) 0.03337(13) Uani 1 1 d . . . . .
Cl2 Cl 0.56215(6) 0.48788(11) 0.36097(7) 0.0290(3) Uani 1 1 d . . . . .
Cl1 Cl 0.49070(6) 1.00745(12) 0.67462(7) 0.0323(3) Uani 1 1 d . . . . .
O1W O 0.84524(19) 0.6984(4) 0.5978(2) 0.0396(9) Uani 1 1 d G . . . .
H1WA H 0.880313 0.746136 0.612334 0.059 Uiso 1 1 d G U . . .
H1WB H 0.852210 0.644926 0.630448 0.059 Uiso 1 1 d G U . . .
N1 N 0.8027(2) 0.9894(4) 0.7116(2) 0.0242(9) Uani 1 1 d . . . . .
H1 H 0.770527 0.928765 0.675349 0.029 Uiso 1 1 calc DR U . . .
N2 N 0.8975(2) 0.5043(4) 0.5454(2) 0.0253(9) Uani 1 1 d . . . . .
H2 H 0.870707 0.580286 0.549821 0.030 Uiso 1 1 calc R U . . .
O2 O 0.7390(2) 0.8560(4) 0.5883(2) 0.0424(9) Uani 1 1 d . . . . .
H2A H 0.774579 0.819725 0.593454 0.064 Uiso 1 1 calc DR U . . .
C27 C 0.7893(2) 0.7017(5) 0.4194(2) 0.0250(10) Uani 1 1 d . . . . .
H27 H 0.836407 0.698593 0.437753 0.030 Uiso 1 1 calc R U . . .
C32 C 0.8614(2) 0.4513(5) 0.4736(2) 0.0239(9) Uani 1 1 d . . . . .
H32A H 0.874499 0.505009 0.443917 0.029 Uiso 1 1 calc R U . . .
H32B H 0.874978 0.356664 0.472660 0.029 Uiso 1 1 calc R U . . .
C25 C 0.7871(2) 0.4574(5) 0.4461(2) 0.0216(9) Uani 1 1 d . . . . .
C8 C 0.7143(2) 0.9905(4) 0.7501(2) 0.0217(10) Uani 1 1 d . . . . .
C33 C 0.9050(3) 0.4016(6) 0.5964(3) 0.0328(11) Uani 1 1 d . . . . .
H33A H 0.861131 0.366418 0.586925 0.049 Uiso 1 1 calc R U . . .
H33B H 0.926065 0.442265 0.641867 0.049 Uiso 1 1 calc R U . . .
H33C H 0.932889 0.327760 0.594504 0.049 Uiso 1 1 calc R U . . .
C30 C 0.6515(2) 0.7169(5) 0.3655(2) 0.0257(10) Uani 1 1 d . . . . .
H30 H 0.604449 0.723595 0.346671 0.031 Uiso 1 1 calc R U . . .
C28 C 0.7574(2) 0.8188(5) 0.3932(3) 0.0322(11) Uani 1 1 d . . . . .
H28 H 0.782006 0.896120 0.392838 0.039 Uiso 1 1 calc R U . . .
C24 C 0.7506(2) 0.3437(5) 0.4473(2) 0.0229(9) Uani 1 1 d . . . . .
C26 C 0.7542(2) 0.5814(5) 0.4203(2) 0.0203(9) Uani 1 1 d . . . . .
C15 C 0.7882(2) 0.9823(5) 0.7719(3) 0.0233(10) Uani 1 1 d . . . . .
H15A H 0.805935 0.896696 0.796685 0.028 Uiso 1 1 calc R U . . .
H15B H 0.811187 1.057506 0.803490 0.028 Uiso 1 1 calc R U . . .
C17 C 0.8715(2) 0.9388(6) 0.7311(3) 0.0341(12) Uani 1 1 d . . . . .
H17A H 0.903981 0.993823 0.768343 0.051 Uiso 1 1 calc R U . . .
H17B H 0.880341 0.944726 0.691790 0.051 Uiso 1 1 calc R U . . .
H17C H 0.875225 0.844662 0.745920 0.051 Uiso 1 1 calc R U . . .
C29 C 0.6873(2) 0.8268(5) 0.3661(3) 0.0301(11) Uani 1 1 d . . . . .
H29 H 0.665258 0.909885 0.348284 0.036 Uiso 1 1 calc R U . . .
C23 C 0.7803(2) 0.2154(5) 0.4732(3) 0.0292(11) Uani 1 1 d . . . . .
H23 H 0.826843 0.204922 0.489532 0.035 Uiso 1 1 calc R U . . .
C9 C 0.6761(2) 0.8727(5) 0.7242(2) 0.0237(10) Uani 1 1 d . . . . .
C31 C 0.6831(2) 0.5919(5) 0.3925(2) 0.0207(9) Uani 1 1 d . . . . .
C11 C 0.6648(3) 0.6365(5) 0.6908(3) 0.0322(11) Uani 1 1 d . . . . .
H11 H 0.684403 0.554842 0.686329 0.039 Uiso 1 1 calc R U . . .
C19 C 0.6791(2) 0.3536(5) 0.4212(2) 0.0233(9) Uani 1 1 d . . . . .
C18 C 0.6484(2) 0.4770(5) 0.3940(3) 0.0226(10) Uani 1 1 d . . . . .
C16 C 0.7939(3) 1.1274(5) 0.6831(3) 0.0346(12) Uani 1 1 d . . . . .
H16A H 0.749827 1.161475 0.673744 0.052 Uiso 1 1 calc R U . . .
H16B H 0.797639 1.125216 0.640717 0.052 Uiso 1 1 calc R U . . .
H16C H 0.828257 1.186823 0.715872 0.052 Uiso 1 1 calc R U . . .
C7 C 0.6852(2) 1.1112(5) 0.7562(2) 0.0210(9) Uani 1 1 d . . . . .
C14 C 0.6049(2) 0.8772(5) 0.7014(2) 0.0254(10) Uani 1 1 d . . . . .
C4 C 0.6220(2) 1.3522(5) 0.7639(3) 0.0299(11) Uani 1 1 d . . . . .
H4 H 0.601450 1.433735 0.766937 0.036 Uiso 1 1 calc R U . . .
C5 C 0.6918(2) 1.3486(5) 0.7862(3) 0.0294(11) Uani 1 1 d . . . . .
H5 H 0.717586 1.428118 0.803446 0.035 Uiso 1 1 calc R U . . .
C34 C 0.9652(2) 0.5592(5) 0.5601(3) 0.0311(11) Uani 1 1 d . . . . .
H34A H 0.993824 0.485012 0.560064 0.047 Uiso 1 1 calc R U . . .
H34B H 0.985376 0.603304 0.604672 0.047 Uiso 1 1 calc R U . . .
H34C H 0.960269 0.624834 0.524941 0.047 Uiso 1 1 calc R U . . .
C2 C 0.6144(2) 1.1159(5) 0.7334(2) 0.0230(10) Uani 1 1 d . . . . .
C3 C 0.5848(2) 1.2404(5) 0.7386(3) 0.0286(10) Uani 1 1 d . . . . .
H3 H 0.538234 1.244130 0.723963 0.034 Uiso 1 1 calc R U . . .
C12 C 0.5959(3) 0.6423(5) 0.6694(3) 0.0328(11) Uani 1 1 d . . . . .
H12 H 0.569459 0.564249 0.650587 0.039 Uiso 1 1 calc R U . . .
C13 C 0.5668(2) 0.7576(5) 0.6751(3) 0.0292(11) Uani 1 1 d . . . . .
H13 H 0.520413 0.758665 0.661471 0.035 Uiso 1 1 calc R U . . .
C20 C 0.6426(2) 0.2366(5) 0.4231(3) 0.0299(11) Uani 1 1 d . . . . .
H20 H 0.595700 0.241877 0.405721 0.036 Uiso 1 1 calc R U . . .
C6 C 0.7217(2) 1.2328(5) 0.7829(2) 0.0236(9) Uani 1 1 d . . . . .
H6 H 0.768526 1.232257 0.798956 0.028 Uiso 1 1 calc R U . . .
C10 C 0.7037(2) 0.7477(5) 0.7179(2) 0.0265(10) Uani 1 1 d . . . . .
H10 H 0.750270 0.741444 0.732961 0.032 Uiso 1 1 calc R U . . .
C35 C 0.6845(3) 0.7701(6) 0.5488(3) 0.0496(16) Uani 1 1 d . . . . .
H35A H 0.689977 0.683089 0.572759 0.060 Uiso 1 1 calc R U . . .
H35B H 0.683760 0.751657 0.504528 0.060 Uiso 1 1 calc R U . . .
C22 C 0.7440(3) 0.1087(5) 0.4753(3) 0.0346(12) Uani 1 1 d . . . . .
H22 H 0.765737 0.025895 0.494340 0.041 Uiso 1 1 calc R U . . .
C21 C 0.6744(3) 0.1187(5) 0.4494(3) 0.0344(12) Uani 1 1 d . . . . .
H21 H 0.649630 0.042266 0.450511 0.041 Uiso 1 1 calc R U . . .
C36 C 0.6200(3) 0.8335(6) 0.5370(3) 0.0435(14) Uani 1 1 d . . . . .
H36A H 0.612481 0.917774 0.510417 0.052 Uiso 0.75 1 calc R U P B 1
H36B H 0.620665 0.855479 0.580902 0.052 Uiso 0.75 1 calc R U P B 1
H36C H 0.620236 0.925116 0.519256 0.052 Uiso 0.25 1 calc R U P C 2
H36D H 0.622823 0.846035 0.582589 0.052 Uiso 0.25 1 calc R U P C 2
C1 C 0.5774(2) 0.9999(5) 0.7062(3) 0.0238(11) Uani 1 1 d . . . . .
C37A C 0.5660(5) 0.7330(11) 0.4982(5) 0.0521(16) Uani 0.75 1 d . U P D 1
H37A H 0.574152 0.650355 0.525978 0.063 Uiso 0.75 1 calc R U P D 1
H37B H 0.568169 0.708192 0.455931 0.063 Uiso 0.75 1 calc R U P D 1
C38A C 0.4972(6) 0.7854(11) 0.4799(5) 0.0523(14) Uani 0.75 1 d . U P D 1
H38A H 0.495620 0.814336 0.521993 0.063 Uiso 0.75 1 calc R U P D 1
H38B H 0.488142 0.865411 0.450261 0.063 Uiso 0.75 1 calc R U P D 1
C40A C 0.3735(4) 0.7344(10) 0.4180(4) 0.0532(16) Uani 0.75 1 d . U P D 1
H40A H 0.365161 0.804141 0.383629 0.080 Uiso 0.75 1 calc R U P D 1
H40B H 0.367840 0.772854 0.455777 0.080 Uiso 0.75 1 calc R U P D 1
H40C H 0.342005 0.660028 0.397575 0.080 Uiso 0.75 1 calc R U P D 1
C39A C 0.4437(4) 0.6823(10) 0.4441(5) 0.0537(14) Uani 0.75 1 d . U P D 1
H39A H 0.450193 0.606885 0.475924 0.064 Uiso 0.75 1 calc R U P D 1
H39B H 0.448958 0.645597 0.405306 0.064 Uiso 0.75 1 calc R U P D 1
C39B C 0.4180(13) 0.774(3) 0.4354(12) 0.042(3) Uani 0.25 1 d . U P D 2
H39C H 0.412049 0.773060 0.388168 0.051 Uiso 0.25 1 calc R U P D 2
H39D H 0.381825 0.828941 0.436212 0.051 Uiso 0.25 1 calc R U P D 2
C40B C 0.4147(13) 0.631(3) 0.4583(12) 0.043(3) Uani 0.25 1 d . U P D 2
H40D H 0.368108 0.601888 0.438874 0.064 Uiso 0.25 1 calc R U P D 2
H40E H 0.434680 0.627887 0.508082 0.064 Uiso 0.25 1 calc R U P D 2
H40F H 0.439121 0.570072 0.442786 0.064 Uiso 0.25 1 calc R U P D 2
C37B C 0.5451(15) 0.772(3) 0.4885(14) 0.042(3) Uani 0.25 1 d . U P D 2
H37C H 0.540456 0.765031 0.441920 0.051 Uiso 0.25 1 calc R U P D 2
H37D H 0.545030 0.678205 0.504187 0.051 Uiso 0.25 1 calc R U P D 2
C38B C 0.4850(14) 0.836(3) 0.4826(14) 0.042(3) Uani 0.25 1 d . U P D 2
H38C H 0.484884 0.929797 0.467783 0.051 Uiso 0.25 1 calc R U P D 2
H38D H 0.488177 0.839367 0.528674 0.051 Uiso 0.25 1 calc R U P D 2
Br5A Br 0.8220(3) 0.4946(7) 0.6899(3) 0.0530(13) Uani 0.25 1 d . U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 3.0424(5) 3_767 ?
Pb1 Br2 3.0423(5) . ?
Pb1 Br3 3.0261(5) . ?
Pb1 Br3 3.0261(5) 3_767 ?
Pb1 Br1 2.9850(5) . ?
Pb1 Br1 2.9849(5) 3_767 ?
Pb2 Br4 3.1302(5) . ?
Pb2 Br4 3.2027(5) 2_756 ?
Pb2 Br2 2.9734(5) . ?
Pb2 Br3 3.0582(5) . ?
Pb2 Br5B 2.8519(19) . ?
Pb2 Br1 3.0901(6) 3_767 ?
Pb2 Br5A 2.921(7) . ?
Cl2 C18 1.744(5) . ?
Cl1 C1 1.756(5) . ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8500 . ?
N1 H1 1.0000 . ?
N1 C15 1.516(7) . ?
N1 C17 1.498(6) . ?
N1 C16 1.482(6) . ?
N2 H2 1.0000 . ?
N2 C32 1.509(6) . ?
N2 C33 1.472(6) . ?
N2 C34 1.514(6) . ?
O2 H2A 0.8400 . ?
O2 C35 1.422(7) . ?
C27 H27 0.9500 . ?
C27 C28 1.350(7) . ?
C27 C26 1.439(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C25 1.505(6) . ?
C25 C24 1.405(6) . ?
C25 C26 1.415(7) . ?
C8 C15 1.515(7) . ?
C8 C9 1.409(6) . ?
C8 C7 1.402(6) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C30 H30 0.9500 . ?
C30 C29 1.355(7) . ?
C30 C31 1.418(6) . ?
C28 H28 0.9500 . ?
C28 C29 1.417(7) . ?
C24 C23 1.430(6) . ?
C24 C19 1.448(6) . ?
C26 C31 1.438(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C29 H29 0.9500 . ?
C23 H23 0.9500 . ?
C23 C22 1.353(7) . ?
C9 C14 1.449(6) . ?
C9 C10 1.424(7) . ?
C31 C18 1.394(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.406(7) . ?
C11 C10 1.365(7) . ?
C19 C18 1.399(7) . ?
C19 C20 1.436(7) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C7 C2 1.443(6) . ?
C7 C6 1.427(6) . ?
C14 C13 1.424(7) . ?
C14 C1 1.393(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.424(7) . ?
C4 C3 1.348(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.352(7) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C2 C3 1.435(7) . ?
C2 C1 1.387(6) . ?
C3 H3 0.9500 . ?
C12 H12 0.9500 . ?
C12 C13 1.354(7) . ?
C13 H13 0.9500 . ?
C20 H20 0.9500 . ?
C20 C21 1.356(7) . ?
C6 H6 0.9500 . ?
C10 H10 0.9500 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.496(9) . ?
C22 H22 0.9500 . ?
C22 C21 1.411(7) . ?
C21 H21 0.9500 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 H36C 0.9900 . ?
C36 H36D 0.9900 . ?
C36 C37A 1.503(12) . ?
C36 C37B 1.65(3) . ?
C37A H37A 0.9900 . ?
C37A H37B 0.9900 . ?
C37A C38A 1.511(13) . ?
C38A H38A 0.9900 . ?
C38A H38B 0.9900 . ?
C38A C39A 1.502(14) . ?
C40A H40A 0.9800 . ?
C40A H40B 0.9800 . ?
C40A H40C 0.9800 . ?
C40A C39A 1.509(12) . ?
C39A H39A 0.9900 . ?
C39A H39B 0.9900 . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
C39B C40B 1.52(3) . ?
C39B C38B 1.52(4) . ?
C40B H40D 0.9800 . ?
C40B H40E 0.9800 . ?
C40B H40F 0.9800 . ?
C37B H37C 0.9900 . ?
C37B H37D 0.9900 . ?
C37B C38B 1.45(4) . ?
C38B H38C 0.9900 . ?
C38B H38D 0.9900 . ?

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 180.00(2) . 3_767 ?
Br3 Pb1 Br2 81.853(14) . . ?
Br3 Pb1 Br2 98.147(14) . 3_767 ?
Br3 Pb1 Br2 81.853(14) 3_767 3_767 ?
Br3 Pb1 Br2 98.147(14) 3_767 . ?
Br3 Pb1 Br3 180.0 . 3_767 ?
Br1 Pb1 Br2 96.357(14) . . ?
Br1 Pb1 Br2 83.642(14) . 3_767 ?
Br1 Pb1 Br2 83.642(14) 3_767 . ?
Br1 Pb1 Br2 96.359(14) 3_767 3_767 ?
Br1 Pb1 Br3 83.255(15) 3_767 . ?
Br1 Pb1 Br3 96.745(15) . . ?
Br1 Pb1 Br3 96.748(15) 3_767 3_767 ?
Br1 Pb1 Br3 83.253(15) . 3_767 ?
Br1 Pb1 Br1 180.0 3_767 . ?
Br4 Pb2 Br4 103.955(6) . 2_756 ?
Br2 Pb2 Br4 168.736(15) . 2_756 ?
Br2 Pb2 Br4 86.791(15) . . ?
Br2 Pb2 Br3 82.448(15) . . ?
Br2 Pb2 Br1 83.013(15) . 3_767 ?
Br3 Pb2 Br4 163.654(15) . . ?
Br3 Pb2 Br4 86.329(14) . 2_756 ?
Br3 Pb2 Br1 81.002(15) . 3_767 ?
Br5B Pb2 Br4 93.57(4) . 2_756 ?
Br5B Pb2 Br4 98.97(4) . . ?
Br5B Pb2 Br2 87.97(4) . . ?
Br5B Pb2 Br3 92.93(3) . . ?
Br5B Pb2 Br1 169.70(3) . 3_767 ?
Br1 Pb2 Br4 85.520(14) 3_767 . ?
Br1 Pb2 Br4 94.320(15) 3_767 2_756 ?
Br5A Pb2 Br4 94.22(14) . . ?
Br5A Pb2 Br2 91.97(15) . . ?
Br5A Pb2 Br3 98.40(13) . . ?
Br5A Pb2 Br1 174.99(15) . 3_767 ?
Pb2 Br4 Pb2 168.460(19) . 2_746 ?
Pb2 Br2 Pb1 81.472(12) . . ?
Pb1 Br3 Pb2 80.371(12) . . ?
Pb1 Br1 Pb2 80.497(13) . 3_767 ?
H1WA O1W H1WB 104.5 . . ?
C15 N1 H1 107.9 . . ?
C17 N1 H1 107.9 . . ?
C17 N1 C15 110.4(4) . . ?
C16 N1 H1 107.9 . . ?
C16 N1 C15 112.1(4) . . ?
C16 N1 C17 110.6(4) . . ?
C32 N2 H2 107.9 . . ?
C32 N2 C34 110.8(4) . . ?
C33 N2 H2 107.9 . . ?
C33 N2 C32 112.5(4) . . ?
C33 N2 C34 109.6(4) . . ?
C34 N2 H2 107.9 . . ?
C35 O2 H2A 109.5 . . ?
C28 C27 H27 119.0 . . ?
C28 C27 C26 121.9(4) . . ?
C26 C27 H27 119.0 . . ?
N2 C32 H32A 109.2 . . ?
N2 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
C25 C32 N2 112.0(4) . . ?
C25 C32 H32A 109.2 . . ?
C25 C32 H32B 109.2 . . ?
C24 C25 C32 121.2(4) . . ?
C24 C25 C26 120.0(4) . . ?
C26 C25 C32 118.8(4) . . ?
C9 C8 C15 117.8(4) . . ?
C7 C8 C15 120.9(4) . . ?
C7 C8 C9 121.3(4) . . ?
N2 C33 H33A 109.5 . . ?
N2 C33 H33B 109.5 . . ?
N2 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C29 C30 H30 119.5 . . ?
C29 C30 C31 121.0(4) . . ?
C31 C30 H30 119.5 . . ?
C27 C28 H28 119.9 . . ?
C27 C28 C29 120.3(5) . . ?
C29 C28 H28 119.9 . . ?
C25 C24 C23 123.3(4) . . ?
C25 C24 C19 119.8(4) . . ?
C23 C24 C19 116.9(4) . . ?
C25 C26 C27 122.3(4) . . ?
C25 C26 C31 120.9(4) . . ?
C31 C26 C27 116.8(4) . . ?
N1 C15 H15A 109.3 . . ?
N1 C15 H15B 109.3 . . ?
C8 C15 N1 111.8(4) . . ?
C8 C15 H15A 109.3 . . ?
C8 C15 H15B 109.3 . . ?
H15A C15 H15B 107.9 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C30 C29 C28 120.5(5) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C24 C23 H23 119.0 . . ?
C22 C23 C24 122.0(5) . . ?
C22 C23 H23 119.0 . . ?
C8 C9 C14 119.5(4) . . ?
C8 C9 C10 123.1(4) . . ?
C10 C9 C14 117.4(4) . . ?
C30 C31 C26 119.5(4) . . ?
C18 C31 C30 123.0(4) . . ?
C18 C31 C26 117.5(4) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.4(5) . . ?
C18 C19 C24 118.3(4) . . ?
C18 C19 C20 122.7(4) . . ?
C20 C19 C24 119.0(4) . . ?
C31 C18 Cl2 118.3(4) . . ?
C31 C18 C19 123.4(4) . . ?
C19 C18 Cl2 118.3(4) . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C8 C7 C2 119.3(4) . . ?
C8 C7 C6 123.6(4) . . ?
C6 C7 C2 117.1(4) . . ?
C13 C14 C9 118.9(5) . . ?
C1 C14 C9 117.7(4) . . ?
C1 C14 C13 123.4(4) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.3(5) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.4(5) . . ?
C6 C5 H5 119.8 . . ?
N2 C34 H34A 109.5 . . ?
N2 C34 H34B 109.5 . . ?
N2 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C3 C2 C7 118.9(4) . . ?
C1 C2 C7 118.5(4) . . ?
C1 C2 C3 122.6(4) . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C11 C12 H12 119.5 . . ?
C13 C12 C11 121.0(5) . . ?
C13 C12 H12 119.5 . . ?
C14 C13 H13 119.6 . . ?
C12 C13 C14 120.8(5) . . ?
C12 C13 H13 119.6 . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.7(5) . . ?
C21 C20 H20 119.7 . . ?
C7 C6 H6 118.9 . . ?
C5 C6 C7 122.1(4) . . ?
C5 C6 H6 118.9 . . ?
C9 C10 H10 119.2 . . ?
C11 C10 C9 121.5(5) . . ?
C11 C10 H10 119.2 . . ?
O2 C35 H35A 109.5 . . ?
O2 C35 H35B 109.5 . . ?
O2 C35 C36 110.9(5) . . ?
H35A C35 H35B 108.1 . . ?
C36 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
C23 C22 H22 119.6 . . ?
C23 C22 C21 120.8(5) . . ?
C21 C22 H22 119.6 . . ?
C20 C21 C22 120.5(5) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
C35 C36 H36A 110.3 . . ?
C35 C36 H36B 110.3 . . ?
C35 C36 H36C 105.9 . . ?
C35 C36 H36D 105.9 . . ?
C35 C36 C37A 107.0(6) . . ?
C35 C36 C37B 125.7(12) . . ?
H36A C36 H36B 108.6 . . ?
H36C C36 H36D 106.2 . . ?
C37A C36 H36A 110.3 . . ?
C37A C36 H36B 110.3 . . ?
C37B C36 H36C 105.9 . . ?
C37B C36 H36D 105.9 . . ?
C14 C1 Cl1 117.7(4) . . ?
C2 C1 Cl1 118.6(4) . . ?
C2 C1 C14 123.7(5) . . ?
C36 C37A H37A 109.0 . . ?
C36 C37A H37B 109.0 . . ?
C36 C37A C38A 113.1(8) . . ?
H37A C37A H37B 107.8 . . ?
C38A C37A H37A 109.0 . . ?
C38A C37A H37B 109.0 . . ?
C37A C38A H38A 109.0 . . ?
C37A C38A H38B 109.0 . . ?
H38A C38A H38B 107.8 . . ?
C39A C38A C37A 112.9(8) . . ?
C39A C38A H38A 109.0 . . ?
C39A C38A H38B 109.0 . . ?
H40A C40A H40B 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
C38A C39A C40A 114.8(9) . . ?
C38A C39A H39A 108.6 . . ?
C38A C39A H39B 108.6 . . ?
C40A C39A H39A 108.6 . . ?
C40A C39A H39B 108.6 . . ?
H39A C39A H39B 107.5 . . ?
H39C C39B H39D 108.2 . . ?
C40B C39B H39C 109.8 . . ?
C40B C39B H39D 109.8 . . ?
C38B C39B H39C 109.8 . . ?
C38B C39B H39D 109.8 . . ?
C38B C39B C40B 109(2) . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40E 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C36 C37B H37C 106.7 . . ?
C36 C37B H37D 106.7 . . ?
H37C C37B H37D 106.6 . . ?
C38B C37B C36 122(2) . . ?
C38B C37B H37C 106.7 . . ?
C38B C37B H37D 106.7 . . ?
C39B C38B H38C 107.6 . . ?
C39B C38B H38D 107.6 . . ?
C37B C38B C39B 119(2) . . ?
C37B C38B H38C 107.6 . . ?
C37B C38B H38D 107.6 . . ?
H38C C38B H38D 107.0 . . ?

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
N2 C32 C25 C24 -97.5(5) . . . . ?
N2 C32 C25 C26 80.9(5) . . . . ?
O2 C35 C36 C37A -177.2(6) . . . . ?
O2 C35 C36 C37B 174.8(13) . . . . ?
C27 C28 C29 C30 -0.8(8) . . . . ?
C27 C26 C31 C30 0.6(6) . . . . ?
C27 C26 C31 C18 -179.0(4) . . . . ?
C32 C25 C24 C23 -0.8(7) . . . . ?
C32 C25 C24 C19 179.2(4) . . . . ?
C32 C25 C26 C27 0.1(6) . . . . ?
C32 C25 C26 C31 179.0(4) . . . . ?
C25 C24 C23 C22 178.3(5) . . . . ?
C25 C24 C19 C18 1.3(7) . . . . ?
C25 C24 C19 C20 -179.7(4) . . . . ?
C25 C26 C31 C30 -178.4(4) . . . . ?
C25 C26 C31 C18 2.0(6) . . . . ?
C8 C9 C14 C13 179.9(4) . . . . ?
C8 C9 C14 C1 0.0(7) . . . . ?
C8 C9 C10 C11 -178.2(5) . . . . ?
C8 C7 C2 C3 -178.9(4) . . . . ?
C8 C7 C2 C1 0.2(7) . . . . ?
C8 C7 C6 C5 178.0(5) . . . . ?
C33 N2 C32 C25 83.8(5) . . . . ?
C30 C31 C18 Cl2 0.1(6) . . . . ?
C30 C31 C18 C19 -179.3(5) . . . . ?
C28 C27 C26 C25 178.3(5) . . . . ?
C28 C27 C26 C31 -0.6(7) . . . . ?
C24 C25 C26 C27 178.5(4) . . . . ?
C24 C25 C26 C31 -2.6(6) . . . . ?
C24 C23 C22 C21 2.2(9) . . . . ?
C24 C19 C18 Cl2 178.7(3) . . . . ?
C24 C19 C18 C31 -1.9(7) . . . . ?
C24 C19 C20 C21 0.5(7) . . . . ?
C26 C27 C28 C29 0.7(8) . . . . ?
C26 C25 C24 C23 -179.2(4) . . . . ?
C26 C25 C24 C19 0.9(7) . . . . ?
C26 C31 C18 Cl2 179.7(3) . . . . ?
C26 C31 C18 C19 0.2(7) . . . . ?
C15 C8 C9 C14 -178.6(4) . . . . ?
C15 C8 C9 C10 0.2(7) . . . . ?
C15 C8 C7 C2 178.5(4) . . . . ?
C15 C8 C7 C6 -0.3(7) . . . . ?
C17 N1 C15 C8 -162.3(4) . . . . ?
C29 C30 C31 C26 -0.7(7) . . . . ?
C29 C30 C31 C18 178.9(5) . . . . ?
C23 C24 C19 C18 -178.6(4) . . . . ?
C23 C24 C19 C20 0.4(7) . . . . ?
C23 C22 C21 C20 -1.2(9) . . . . ?
C9 C8 C15 N1 79.3(5) . . . . ?
C9 C8 C7 C2 -2.0(7) . . . . ?
C9 C8 C7 C6 179.1(5) . . . . ?
C9 C14 C13 C12 -2.2(7) . . . . ?
C9 C14 C1 Cl1 176.9(3) . . . . ?
C9 C14 C1 C2 -1.9(7) . . . . ?
C31 C30 C29 C28 0.8(8) . . . . ?
C11 C12 C13 C14 1.7(8) . . . . ?
C19 C24 C23 C22 -1.8(7) . . . . ?
C19 C20 C21 C22 -0.2(8) . . . . ?
C18 C19 C20 C21 179.5(5) . . . . ?
C16 N1 C15 C8 73.9(5) . . . . ?
C7 C8 C15 N1 -101.3(5) . . . . ?
C7 C8 C9 C14 1.9(7) . . . . ?
C7 C8 C9 C10 -179.2(5) . . . . ?
C7 C2 C3 C4 0.4(7) . . . . ?
C7 C2 C1 Cl1 -177.0(3) . . . . ?
C7 C2 C1 C14 1.8(7) . . . . ?
C14 C9 C10 C11 0.7(7) . . . . ?
C4 C5 C6 C7 1.3(8) . . . . ?
C5 C4 C3 C2 -0.1(8) . . . . ?
C34 N2 C32 C25 -153.0(4) . . . . ?
C2 C7 C6 C5 -0.9(7) . . . . ?
C3 C4 C5 C6 -0.8(8) . . . . ?
C3 C2 C1 Cl1 2.1(7) . . . . ?
C3 C2 C1 C14 -179.1(5) . . . . ?
C12 C11 C10 C9 -1.3(8) . . . . ?
C13 C14 C1 Cl1 -3.0(7) . . . . ?
C13 C14 C1 C2 178.2(5) . . . . ?
C20 C19 C18 Cl2 -0.3(7) . . . . ?
C20 C19 C18 C31 179.2(5) . . . . ?
C6 C7 C2 C3 0.0(6) . . . . ?
C6 C7 C2 C1 179.1(4) . . . . ?
C10 C9 C14 C13 0.9(7) . . . . ?
C10 C9 C14 C1 -178.9(4) . . . . ?
C10 C11 C12 C13 0.0(8) . . . . ?
C35 C36 C37A C38A -177.7(8) . . . . ?
C35 C36 C37B C38B 176.5(17) . . . . ?
C36 C37A C38A C39A -177.3(9) . . . . ?
C36 C37B C38B C39B 178(2) . . . . ?
C1 C14 C13 C12 177.7(5) . . . . ?
C1 C2 C3 C4 -178.6(5) . . . . ?
C37A C38A C39A C40A -173.5(9) . . . . ?
C40B C39B C38B C37B 60(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.941
_oxdiff_exptl_absorpt_empirical_full_min 0.595
####################################################################### 
# 
# 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_1-C8
_database_code_depnum_ccdc_archive 'CCDC 2240934'
loop_
_audit_author_name
_audit_author_address
'Binbin Luo'
;Shantou University
China
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_1-C8                
;
PROBLEM: Check Calcd Resid. Dens.  1.16Ang From Br5             3.79 eA-3
RESPONSE: resulting from the heavy atom effect
;
# Added during the CSD deposition process: Thursday 09 February 2023 11:29 AM
# end Validation Reply Form

_audit_creation_date             2023-01-08
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Br10 Pb3, 4(C17 H17 Cl N), 2(H2 O), 2(C8 H18 O)'
_chemical_formula_sum            'C84 H108 Br10 Cl4 N4 O4 Pb3'
_chemical_formula_weight         2800.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N Pb Br'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.4859(2)
_cell_length_b                   10.01480(10)
_cell_length_c                   22.3690(2)
_cell_angle_alpha                90
_cell_angle_beta                 114.2300(10)
_cell_angle_gamma                90
_cell_volume                     4593.55(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16064
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.7700
_cell_measurement_theta_min      3.9640
_shelx_estimated_absorpt_T_max   0.514
_shelx_estimated_absorpt_T_min   0.100
_exptl_absorpt_coefficient_mu    17.063
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (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    2.025
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2672
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.045
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25811
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.128
_diffrn_reflns_theta_min         3.970
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_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  78.00   0.50    0.50    --    0.00  38.00  30.00  122
  2  ω    -66.00 -14.00   0.50    0.50    --    0.00 -19.00 120.00  104
  3  ω     50.00  88.00   0.50    0.50    --    0.00  57.00 -90.00   76
  4  ω    -17.00  23.00   0.50    0.50    --    0.00  57.00 -90.00   80
  5  ω     87.00 131.00   0.50    0.50    --   89.30  30.00-180.00   88
  6  ω     70.00 158.00   0.50    0.50    --   89.30  45.00-150.00  176
  7  ω     79.00 158.00   0.50    0.50    --   89.30  45.00-180.00  158
  8  ω    121.00 166.00   0.50    0.50    --   89.30  30.00 -60.00   90
  9  ω      1.00  80.00   0.50    0.50    --   89.30 -61.00 -60.00  158
 10  ω     76.00 108.00   0.50    0.50    --   89.30  30.00 -60.00   64
 11  ω     12.00 107.00   0.50    0.50    --   89.30 -61.00  60.00  190
 12  ω     26.00  83.00   0.50    0.50    --   89.30 -45.00  60.00  114
 13  ω     18.00  81.00   0.50    0.50    --   89.30 -61.00 -30.00  126
;
_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      0.0126667000
_diffrn_orient_matrix_UB_12      -0.0780721000
_diffrn_orient_matrix_UB_13      0.0634448000
_diffrn_orient_matrix_UB_21      -0.0424737000
_diffrn_orient_matrix_UB_22      0.1003519000
_diffrn_orient_matrix_UB_23      0.0172097000
_diffrn_orient_matrix_UB_31      -0.0606636000
_diffrn_orient_matrix_UB_32      -0.0865665000
_diffrn_orient_matrix_UB_33      -0.0371998000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7954
_reflns_number_total             8650
_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 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         3.943
_refine_diff_density_min         -1.484
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         8650
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0359
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0421P)²+22.5327P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0957
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C42A-O1
 1.4 with sigma of 0.02
 C42A-C41A \\sim C40A-C41A \\sim C39A-C40A \\sim C39A-C38A \\sim C37A-C38A
\\sim C36A-C37A \\sim C35A-
 C36A
 with sigma of 0.02
 C41B-C42B \\sim C41B-C40B \\sim C39B-C40B \\sim C37B-C38B \\sim C39B-C38B
\\sim C37B-C36B \\sim C35B-
 C36B
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C42B \\sim C41B \\sim C38B \\sim C36B \\sim C39B \\sim C37B \\sim C40B \\sim
C35B: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
C35A \\sim C40A \\sim C41A \\sim C39A \\sim C42A \\sim C38A \\sim C37A \\sim
C36A: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
3. Others
 Fixed Sof: H1A(0.6) H1B(0.4) C42B(0.6) H42A(0.6) H42B(0.6) C36B(0.6)
 H36A(0.6) H36B(0.6) C37B(0.6) H37A(0.6) H37B(0.6) C35B(0.6) H35A(0.6)
 H35B(0.6) H35C(0.6) C41B(0.6) H41A(0.6) H41B(0.6) C39B(0.6) H39A(0.6)
 H39B(0.6) C38B(0.6) H38A(0.6) H38B(0.6) C40B(0.6) H40A(0.6) H40B(0.6)
 C40A(0.4) H40C(0.4) H40D(0.4) C41A(0.4) H41C(0.4) H41D(0.4) C38A(0.4)
 H38C(0.4) H38D(0.4) C39A(0.4) H39C(0.4) H39D(0.4) C42A(0.4) H42C(0.4)
 H42D(0.4) C36A(0.4) H36C(0.4) H36D(0.4) C37A(0.4) H37C(0.4) H37D(0.4)
 C35A(0.4) H35D(0.4) H35E(0.4) H35F(0.4)
4.a Free rotating group:
 O2W(H2WA,H2WB)
4.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
4.c Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C15(H15A,H15B), C42B(H42A,H42B), C36B(H36A,H36B), C37B(H37A,
 H37B), C41B(H41A,H41B), C39B(H39A,H39B), C38B(H38A,H38B), C40B(H40A,H40B),
 C40A(H40C,H40D), C41A(H41C,H41D), C38A(H38C,H38D), C39A(H39C,H39D), C42A(H42C,
 H42D), C36A(H36C,H36D), C37A(H37C,H37D)
4.d Aromatic/amide H refined with riding coordinates:
 C27(H27), C29(H29), C30(H30), C6(H6), C4(H4), C3(H3), C5(H5), C10(H10),
 C28(H28), C12(H12), C23(H23), C13(H13), C11(H11), C22(H22), C20(H20), C21(H21)
4.e Tetrahedral OH refined with riding coordinates:
 O1(H1A), O1(H1B)
4.f Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C34(H34A,H34B,H34C), C33(H33A,H33B,
 H33C), C35B(H35A,H35B,H35C), C35A(H35D,H35E,H35F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb2 Pb 0.45962(2) 0.99830(2) 0.31157(2) 0.02054(7) Uani 1 1 d . . . . .
Pb1 Pb 0.500000 1.000000 0.500000 0.02492(9) Uani 1 2 d S . P . .
Br2 Br 0.41936(3) 0.80690(5) 0.39209(2) 0.03004(13) Uani 1 1 d . . . . .
Br6 Br 0.49487(2) 0.72722(5) 0.25637(2) 0.02649(12) Uani 1 1 d . . . . .
Br4 Br 0.43491(3) 1.20788(5) 0.39558(3) 0.03363(14) Uani 1 1 d . . . . .
Br3 Br 0.59663(3) 0.99609(6) 0.43940(3) 0.03789(16) Uani 1 1 d . . . . .
Br5 Br 0.33281(3) 1.02334(7) 0.21976(3) 0.03810(15) Uani 1 1 d . . . A 1
Cl2 Cl 0.93895(7) 0.49770(13) 0.63734(7) 0.0380(3) Uani 1 1 d . . . . .
Cl1 Cl 1.00173(6) 0.01907(15) 0.31453(7) 0.0379(3) Uani 1 1 d . . . . .
N1 N 0.6876(2) -0.0092(4) 0.2756(2) 0.0230(9) Uani 1 1 d . . . . .
H1 H 0.716162 -0.073091 0.309635 0.028 Uiso 1 1 calc R U . . .
N2 N 0.6103(2) 0.4885(4) 0.4553(2) 0.0285(10) Uani 1 1 d . . . . .
H2 H 0.632662 0.570731 0.449521 0.034 Uiso 1 1 calc R U . . .
C8 C 0.7814(2) -0.0033(4) 0.2418(2) 0.0208(10) Uani 1 1 d . . . . .
C31 C 0.8175(2) 0.5941(5) 0.6035(2) 0.0230(10) Uani 1 1 d . . . . .
C26 C 0.7475(2) 0.5807(5) 0.5762(2) 0.0243(10) Uani 1 1 d . . . . .
C16 C 0.6190(2) -0.0547(6) 0.2550(3) 0.0315(11) Uani 1 1 d . . . . .
H16A H 0.589803 0.004618 0.220709 0.047 Uiso 1 1 calc R U . . .
H16B H 0.607532 -0.052641 0.292807 0.047 Uiso 1 1 calc R U . . .
H16C H 0.614616 -0.146055 0.238049 0.047 Uiso 1 1 calc R U . . .
C27 C 0.7107(3) 0.6964(6) 0.5750(3) 0.0339(12) Uani 1 1 d . . . . .
H27 H 0.664459 0.690782 0.556208 0.041 Uiso 1 1 calc R U . . .
C32 C 0.6449(3) 0.4444(6) 0.5261(2) 0.0316(12) Uani 1 1 d . . . . .
H32A H 0.629323 0.499480 0.553524 0.038 Uiso 1 1 calc R U . . .
H32B H 0.633211 0.350339 0.529780 0.038 Uiso 1 1 calc R U . . .
C2 C 0.8891(2) -0.1120(5) 0.2892(2) 0.0248(10) Uani 1 1 d . . . . .
C15 C 0.7077(2) -0.0135(5) 0.2190(2) 0.0212(10) Uani 1 1 d . . . . .
H15A H 0.686527 0.061042 0.188675 0.025 Uiso 1 1 calc R U . . .
H15B H 0.692271 -0.098157 0.194681 0.025 Uiso 1 1 calc R U . . .
C7 C 0.8193(2) -0.1185(5) 0.2667(2) 0.0227(10) Uani 1 1 d . . . . .
C17 C 0.6965(3) 0.1252(6) 0.3069(3) 0.0357(12) Uani 1 1 d . . . . .
H17A H 0.668989 0.190344 0.274763 0.054 Uiso 1 1 calc R U . . .
H17B H 0.742334 0.152056 0.322461 0.054 Uiso 1 1 calc R U . . .
H17C H 0.684097 0.121514 0.344058 0.054 Uiso 1 1 calc R U . . .
C34 C 0.6131(3) 0.3867(6) 0.4085(3) 0.0444(15) Uani 1 1 d . . . . .
H34A H 0.658694 0.366182 0.418046 0.067 Uiso 1 1 calc R U . . .
H34B H 0.591438 0.421255 0.363665 0.067 Uiso 1 1 calc R U . . .
H34C H 0.590871 0.305378 0.412692 0.067 Uiso 1 1 calc R U . . .
C9 C 0.8105(2) 0.1187(5) 0.2377(2) 0.0226(10) Uani 1 1 d . . . . .
C25 C 0.7181(2) 0.4559(5) 0.5521(2) 0.0268(10) Uani 1 1 d . . . . .
C18 C 0.8543(3) 0.4809(5) 0.6054(3) 0.0285(11) Uani 1 1 d . . . . .
C1 C 0.9164(3) 0.0098(5) 0.2853(3) 0.0258(11) Uani 1 1 d . . . . .
C33 C 0.5408(3) 0.5249(7) 0.4412(3) 0.0463(15) Uani 1 1 d . . . . .
H33A H 0.517357 0.445065 0.444917 0.069 Uiso 1 1 calc R U . . .
H33B H 0.519596 0.561258 0.396770 0.069 Uiso 1 1 calc R U . . .
H33C H 0.540348 0.592073 0.472904 0.069 Uiso 1 1 calc R U . . .
C29 C 0.8081(3) 0.8263(6) 0.6265(3) 0.0448(15) Uani 1 1 d . . . . .
H29 H 0.827743 0.909957 0.643509 0.054 Uiso 1 1 calc R U . . .
C30 C 0.8459(3) 0.7206(5) 0.6283(3) 0.0325(12) Uani 1 1 d . . . . .
H30 H 0.891963 0.730480 0.646335 0.039 Uiso 1 1 calc R U . . .
C6 C 0.7914(2) -0.2440(5) 0.2717(3) 0.0288(11) Uani 1 1 d . . . . .
H6 H 0.745354 -0.251585 0.256410 0.035 Uiso 1 1 calc R U . . .
C14 C 0.8804(2) 0.1263(5) 0.2606(2) 0.0275(11) Uani 1 1 d . . . . .
C4 C 0.8976(3) -0.3453(6) 0.3197(3) 0.0408(14) Uani 1 1 d . . . . .
H4 H 0.923735 -0.421862 0.337967 0.049 Uiso 1 1 calc R U . . .
C3 C 0.9261(3) -0.2300(6) 0.3147(3) 0.0334(12) Uani 1 1 d . . . . .
H3 H 0.972058 -0.227442 0.328626 0.040 Uiso 1 1 calc R U . . .
C5 C 0.8295(3) -0.3529(6) 0.2981(3) 0.0376(13) Uani 1 1 d . . . . .
H5 H 0.809889 -0.434638 0.301872 0.045 Uiso 1 1 calc R U . . .
C10 C 0.7744(3) 0.2390(5) 0.2126(3) 0.0313(11) Uani 1 1 d . . . . .
H10 H 0.728203 0.237021 0.197204 0.038 Uiso 1 1 calc R U . . .
C28 C 0.7392(3) 0.8135(6) 0.5994(3) 0.0472(15) Uani 1 1 d . . . . .
H28 H 0.713083 0.888530 0.598587 0.057 Uiso 1 1 calc R U . . .
C12 C 0.8039(3) 0.3553(6) 0.2101(3) 0.0415(14) Uani 1 1 d . . . . .
H12 H 0.778530 0.433356 0.193273 0.050 Uiso 1 1 calc R U . . .
C24 C 0.7565(3) 0.3435(5) 0.5552(3) 0.0345(12) Uani 1 1 d . . . . .
C23 C 0.7298(3) 0.2149(6) 0.5313(3) 0.0541(18) Uani 1 1 d . . . . .
H23 H 0.683944 0.202661 0.514359 0.065 Uiso 1 1 calc R U . . .
C13 C 0.9095(3) 0.2500(6) 0.2567(3) 0.0382(13) Uani 1 1 d . . . . .
H13 H 0.955520 0.255112 0.271336 0.046 Uiso 1 1 calc R U . . .
C19 C 0.8267(3) 0.3564(6) 0.5824(3) 0.0354(13) Uani 1 1 d . . . . .
C11 C 0.8730(3) 0.3611(6) 0.2327(3) 0.0451(15) Uani 1 1 d . . . . .
H11 H 0.893511 0.442931 0.230944 0.054 Uiso 1 1 calc R U . . .
C22 C 0.7685(4) 0.1092(7) 0.5323(4) 0.076(3) Uani 1 1 d . . . . .
H22 H 0.749223 0.025757 0.514509 0.091 Uiso 1 1 calc R U . . .
C20 C 0.8650(3) 0.2418(6) 0.5841(3) 0.0532(18) Uani 1 1 d . . . . .
H20 H 0.911170 0.248999 0.602994 0.064 Uiso 1 1 calc R U . . .
C21 C 0.8371(4) 0.1233(7) 0.5596(4) 0.069(3) Uani 1 1 d . . . . .
H21 H 0.863707 0.048913 0.560749 0.083 Uiso 1 1 calc R U . . .
O2W O 0.6313(3) 0.7127(5) 0.3975(2) 0.0578(13) Uani 1 1 d G . . . .
H2WA H 0.620830 0.784084 0.411379 0.087 Uiso 1 1 d G U . . .
H2WB H 0.601579 0.702319 0.359174 0.087 Uiso 1 1 d G U . . .
O1 O 0.7347(2) 0.8391(5) 0.3859(2) 0.0527(12) Uani 1 1 d D . . . .
H1A H 0.704199 0.799034 0.390821 0.079 Uiso 0.6 1 calc R U P B 1
H1B H 0.697476 0.815874 0.382237 0.079 Uiso 0.4 1 calc R U P C 2
C42B C 0.7976(6) 0.7952(17) 0.4369(6) 0.0718(19) Uani 0.6 1 d D U P D 1
H42A H 0.810854 0.709188 0.424273 0.086 Uiso 0.6 1 calc R U P D 1
H42B H 0.793800 0.782811 0.479089 0.086 Uiso 0.6 1 calc R U P D 1
C36B C 1.1344(5) 0.6919(17) 0.5914(5) 0.0744(18) Uani 0.6 1 d D U P D 1
H36A H 1.150274 0.778629 0.613385 0.089 Uiso 0.6 1 calc R U P D 1
H36B H 1.127552 0.632925 0.623577 0.089 Uiso 0.6 1 calc R U P D 1
C37B C 1.0695(6) 0.7150(18) 0.5360(5) 0.0749(17) Uani 0.6 1 d D U P D 1
H37A H 1.076961 0.755322 0.499210 0.090 Uiso 0.6 1 calc R U P D 1
H37B H 1.048455 0.627271 0.520870 0.090 Uiso 0.6 1 calc R U P D 1
C35B C 1.1861(7) 0.634(2) 0.5764(7) 0.079(2) Uani 0.6 1 d D U P D 1
H35A H 1.167470 0.566841 0.541713 0.119 Uiso 0.6 1 calc R U P D 1
H35B H 1.218381 0.591118 0.615841 0.119 Uiso 0.6 1 calc R U P D 1
H35C H 1.207254 0.704086 0.561690 0.119 Uiso 0.6 1 calc R U P D 1
C41B C 0.8465(5) 0.8990(18) 0.4436(5) 0.0726(18) Uani 0.6 1 d D U P D 1
H41A H 0.829938 0.987071 0.449952 0.087 Uiso 0.6 1 calc R U P D 1
H41B H 0.853940 0.902959 0.403014 0.087 Uiso 0.6 1 calc R U P D 1
C39B C 0.9639(5) 0.8253(19) 0.4913(5) 0.0748(17) Uani 0.6 1 d D U P D 1
H39A H 0.973686 0.892949 0.464376 0.090 Uiso 0.6 1 calc R U P D 1
H39B H 0.951253 0.742405 0.464900 0.090 Uiso 0.6 1 calc R U P D 1
C38B C 1.0256(5) 0.7973(17) 0.5496(5) 0.0748(17) Uani 0.6 1 d D U P D 1
H38A H 1.047423 0.883130 0.567681 0.090 Uiso 0.6 1 calc R U P D 1
H38B H 1.014883 0.753798 0.583649 0.090 Uiso 0.6 1 calc R U P D 1
C40B C 0.9092(5) 0.8697(18) 0.5005(5) 0.0740(17) Uani 0.6 1 d D U P D 1
H40A H 0.922260 0.952096 0.527142 0.089 Uiso 0.6 1 calc R U P D 1
H40B H 0.899805 0.801776 0.527562 0.089 Uiso 0.6 1 calc R U P D 1
C40A C 0.8968(7) 0.7042(18) 0.4817(9) 0.0571(18) Uani 0.4 1 d D U P D 2
H40C H 0.888259 0.667200 0.518515 0.069 Uiso 0.4 1 calc R U P D 2
H40D H 0.890737 0.631353 0.449820 0.069 Uiso 0.4 1 calc R U P D 2
C41A C 0.8475(7) 0.8163(19) 0.4484(9) 0.0567(19) Uani 0.4 1 d D U P D 2
H41C H 0.854769 0.892416 0.478801 0.068 Uiso 0.4 1 calc R U P D 2
H41D H 0.852518 0.848249 0.408824 0.068 Uiso 0.4 1 calc R U P D 2
C38A C 1.0184(7) 0.6441(18) 0.5285(9) 0.0580(18) Uani 0.4 1 d D U P D 2
H38C H 1.010174 0.586450 0.489955 0.070 Uiso 0.4 1 calc R U P D 2
H38D H 1.011678 0.588204 0.561725 0.070 Uiso 0.4 1 calc R U P D 2
C39A C 0.9661(7) 0.7534(19) 0.5073(10) 0.0576(18) Uani 0.4 1 d D U P D 2
H39C H 0.974012 0.812576 0.545283 0.069 Uiso 0.4 1 calc R U P D 2
H39D H 0.971105 0.808008 0.472786 0.069 Uiso 0.4 1 calc R U P D 2
C42A C 0.7803(7) 0.7587(19) 0.4299(10) 0.056(2) Uani 0.4 1 d D U P D 2
H42C H 0.777902 0.668811 0.410635 0.068 Uiso 0.4 1 calc R U P D 2
H42D H 0.771455 0.749657 0.469549 0.068 Uiso 0.4 1 calc R U P D 2
C36A C 1.1387(7) 0.5685(18) 0.5648(9) 0.0576(19) Uani 0.4 1 d D U P D 2
H36C H 1.136076 0.503569 0.597074 0.069 Uiso 0.4 1 calc R U P D 2
H36D H 1.125993 0.521790 0.522366 0.069 Uiso 0.4 1 calc R U P D 2
C37A C 1.0907(7) 0.6851(19) 0.5568(10) 0.0580(18) Uani 0.4 1 d D U P D 2
H37C H 1.101999 0.726965 0.600241 0.070 Uiso 0.4 1 calc R U P D 2
H37D H 1.096714 0.753322 0.527786 0.070 Uiso 0.4 1 calc R U P D 2
C35A C 1.2092(8) 0.619(2) 0.5881(11) 0.059(2) Uani 0.4 1 d D U P D 2
H35D H 1.210602 0.692796 0.559748 0.089 Uiso 0.4 1 calc R U P D 2
H35E H 1.237318 0.546540 0.585967 0.089 Uiso 0.4 1 calc R U P D 2
H35F H 1.224438 0.651303 0.633370 0.089 Uiso 0.4 1 calc R U P D 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
Pb2 Br2 3.0127(5) . ?
Pb2 Br6 3.2133(5) . ?
Pb2 Br6 3.1447(5) 2_655 ?
Pb2 Br4 3.0171(6) . ?
Pb2 Br3 3.2308(6) . ?
Pb2 Br5 2.7576(6) . ?
Pb1 Br2 3.0434(5) . ?
Pb1 Br2 3.0434(5) 3_676 ?
Pb1 Br4 3.0210(5) . ?
Pb1 Br4 3.0210(5) 3_676 ?
Pb1 Br3 2.9964(6) 3_676 ?
Pb1 Br3 2.9963(6) . ?
Cl2 C18 1.745(6) . ?
Cl1 C1 1.758(5) . ?
N1 H1 1.0000 . ?
N1 C16 1.488(6) . ?
N1 C15 1.509(6) . ?
N1 C17 1.492(6) . ?
N2 H2 1.0000 . ?
N2 C32 1.515(6) . ?
N2 C34 1.481(7) . ?
N2 C33 1.507(7) . ?
C8 C15 1.525(7) . ?
C8 C7 1.406(6) . ?
C8 C9 1.406(6) . ?
C31 C26 1.441(7) . ?
C31 C18 1.395(7) . ?
C31 C30 1.424(7) . ?
C26 C27 1.417(7) . ?
C26 C25 1.413(7) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C27 H27 0.9500 . ?
C27 C28 1.341(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C25 1.509(7) . ?
C2 C7 1.441(6) . ?
C2 C1 1.383(7) . ?
C2 C3 1.423(7) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C7 C6 1.429(7) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C9 C14 1.441(7) . ?
C9 C10 1.433(7) . ?
C25 C24 1.403(8) . ?
C18 C19 1.394(7) . ?
C1 C14 1.397(7) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C29 H29 0.9500 . ?
C29 C30 1.348(8) . ?
C29 C28 1.419(8) . ?
C30 H30 0.9500 . ?
C6 H6 0.9500 . ?
C6 C5 1.363(7) . ?
C14 C13 1.420(8) . ?
C4 H4 0.9500 . ?
C4 C3 1.346(8) . ?
C4 C5 1.407(8) . ?
C3 H3 0.9500 . ?
C5 H5 0.9500 . ?
C10 H10 0.9500 . ?
C10 C12 1.354(8) . ?
C28 H28 0.9500 . ?
C12 H12 0.9500 . ?
C12 C11 1.423(8) . ?
C24 C23 1.429(8) . ?
C24 C19 1.445(8) . ?
C23 H23 0.9500 . ?
C23 C22 1.364(10) . ?
C13 H13 0.9500 . ?
C13 C11 1.356(8) . ?
C19 C20 1.425(8) . ?
C11 H11 0.9500 . ?
C22 H22 0.9500 . ?
C22 C21 1.414(11) . ?
C20 H20 0.9500 . ?
C20 C21 1.348(9) . ?
C21 H21 0.9500 . ?
O2W H2WA 0.8502 . ?
O2W H2WB 0.8501 . ?
O1 H1A 0.8400 . ?
O1 H1B 0.8400 . ?
O1 C42B 1.473(13) . ?
O1 C42A 1.355(15) . ?
C42B H42A 0.9900 . ?
C42B H42B 0.9900 . ?
C42B C41B 1.475(13) . ?
C36B H36A 0.9900 . ?
C36B H36B 0.9900 . ?
C36B C37B 1.495(11) . ?
C36B C35B 1.457(13) . ?
C37B H37A 0.9900 . ?
C37B H37B 0.9900 . ?
C37B C38B 1.412(13) . ?
C35B H35A 0.9800 . ?
C35B H35B 0.9800 . ?
C35B H35C 0.9800 . ?
C41B H41A 0.9900 . ?
C41B H41B 0.9900 . ?
C41B C40B 1.489(11) . ?
C39B H39A 0.9900 . ?
C39B H39B 0.9900 . ?
C39B C38B 1.490(11) . ?
C39B C40B 1.399(12) . ?
C38B H38A 0.9900 . ?
C38B H38B 0.9900 . ?
C40B H40A 0.9900 . ?
C40B H40B 0.9900 . ?
C40A H40C 0.9900 . ?
C40A H40D 0.9900 . ?
C40A C41A 1.538(15) . ?
C40A C39A 1.505(15) . ?
C41A H41C 0.9900 . ?
C41A H41D 0.9900 . ?
C41A C42A 1.509(15) . ?
C38A H38C 0.9900 . ?
C38A H38D 0.9900 . ?
C38A C39A 1.533(15) . ?
C38A C37A 1.539(15) . ?
C39A H39C 0.9900 . ?
C39A H39D 0.9900 . ?
C42A H42C 0.9900 . ?
C42A H42D 0.9900 . ?
C36A H36C 0.9900 . ?
C36A H36D 0.9900 . ?
C36A C37A 1.550(15) . ?
C36A C35A 1.538(15) . ?
C37A H37C 0.9900 . ?
C37A H37D 0.9900 . ?
C35A H35D 0.9800 . ?
C35A H35E 0.9800 . ?
C35A H35F 0.9800 . ?

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 Pb2 Br6 171.885(15) . 2_655 ?
Br2 Pb2 Br6 82.775(15) . . ?
Br2 Pb2 Br4 83.850(16) . . ?
Br2 Pb2 Br3 82.985(16) . . ?
Br6 Pb2 Br6 104.464(6) 2_655 . ?
Br6 Pb2 Br3 92.952(15) 2_655 . ?
Br6 Pb2 Br3 92.197(15) . . ?
Br4 Pb2 Br6 88.479(15) . 2_655 ?
Br4 Pb2 Br6 164.702(15) . . ?
Br4 Pb2 Br3 78.810(17) . . ?
Br5 Pb2 Br2 91.747(18) . . ?
Br5 Pb2 Br6 97.667(17) . . ?
Br5 Pb2 Br6 90.911(17) . 2_655 ?
Br5 Pb2 Br4 90.120(18) . . ?
Br5 Pb2 Br3 168.163(19) . . ?
Br2 Pb1 Br2 180.0 . 3_676 ?
Br4 Pb1 Br2 96.736(16) . 3_676 ?
Br4 Pb1 Br2 96.737(16) 3_676 . ?
Br4 Pb1 Br2 83.263(16) 3_676 3_676 ?
Br4 Pb1 Br2 83.264(16) . . ?
Br4 Pb1 Br4 180.0 . 3_676 ?
Br3 Pb1 Br2 86.532(15) . . ?
Br3 Pb1 Br2 93.467(15) . 3_676 ?
Br3 Pb1 Br2 93.467(15) 3_676 . ?
Br3 Pb1 Br2 86.534(15) 3_676 3_676 ?
Br3 Pb1 Br4 97.449(16) 3_676 . ?
Br3 Pb1 Br4 82.552(16) 3_676 3_676 ?
Br3 Pb1 Br4 97.448(16) . 3_676 ?
Br3 Pb1 Br4 82.552(16) . . ?
Br3 Pb1 Br3 179.999(10) . 3_676 ?
Pb2 Br2 Pb1 80.938(13) . . ?
Pb2 Br6 Pb2 169.140(19) 2_645 . ?
Pb2 Br4 Pb1 81.232(14) . . ?
Pb1 Br3 Pb2 78.182(15) . . ?
C16 N1 H1 107.4 . . ?
C16 N1 C15 111.1(4) . . ?
C16 N1 C17 110.1(4) . . ?
C15 N1 H1 107.4 . . ?
C17 N1 H1 107.4 . . ?
C17 N1 C15 113.0(4) . . ?
C32 N2 H2 107.8 . . ?
C34 N2 H2 107.8 . . ?
C34 N2 C32 112.7(4) . . ?
C34 N2 C33 111.1(5) . . ?
C33 N2 H2 107.8 . . ?
C33 N2 C32 109.4(5) . . ?
C7 C8 C15 118.4(4) . . ?
C9 C8 C15 120.5(4) . . ?
C9 C8 C7 121.1(5) . . ?
C18 C31 C26 117.9(4) . . ?
C18 C31 C30 123.1(5) . . ?
C30 C31 C26 119.0(5) . . ?
C27 C26 C31 117.3(5) . . ?
C25 C26 C31 120.2(5) . . ?
C25 C26 C27 122.5(5) . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C26 C27 H27 119.0 . . ?
C28 C27 C26 121.9(5) . . ?
C28 C27 H27 119.0 . . ?
N2 C32 H32A 109.0 . . ?
N2 C32 H32B 109.0 . . ?
H32A C32 H32B 107.8 . . ?
C25 C32 N2 113.0(4) . . ?
C25 C32 H32A 109.0 . . ?
C25 C32 H32B 109.0 . . ?
C1 C2 C7 117.7(5) . . ?
C1 C2 C3 123.9(5) . . ?
C3 C2 C7 118.4(5) . . ?
N1 C15 C8 112.1(4) . . ?
N1 C15 H15A 109.2 . . ?
N1 C15 H15B 109.2 . . ?
C8 C15 H15A 109.2 . . ?
C8 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C8 C7 C2 119.8(5) . . ?
C8 C7 C6 122.6(4) . . ?
C6 C7 C2 117.6(4) . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C34 H34A 109.5 . . ?
N2 C34 H34B 109.5 . . ?
N2 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C8 C9 C14 119.4(4) . . ?
C8 C9 C10 123.4(4) . . ?
C10 C9 C14 117.1(4) . . ?
C26 C25 C32 118.7(5) . . ?
C24 C25 C26 120.6(5) . . ?
C24 C25 C32 120.6(5) . . ?
C31 C18 Cl2 117.9(4) . . ?
C19 C18 Cl2 118.9(4) . . ?
C19 C18 C31 123.2(5) . . ?
C2 C1 Cl1 117.8(4) . . ?
C2 C1 C14 124.2(5) . . ?
C14 C1 Cl1 118.0(4) . . ?
N2 C33 H33A 109.5 . . ?
N2 C33 H33B 109.5 . . ?
N2 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C29 H29 119.8 . . ?
C30 C29 C28 120.4(5) . . ?
C28 C29 H29 119.8 . . ?
C31 C30 H30 119.6 . . ?
C29 C30 C31 120.7(5) . . ?
C29 C30 H30 119.6 . . ?
C7 C6 H6 119.4 . . ?
C5 C6 C7 121.3(5) . . ?
C5 C6 H6 119.4 . . ?
C1 C14 C9 117.8(5) . . ?
C1 C14 C13 123.1(5) . . ?
C13 C14 C9 119.1(5) . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.3(5) . . ?
C5 C4 H4 119.8 . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.8(5) . . ?
C4 C3 H3 119.1 . . ?
C6 C5 C4 120.6(5) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C9 C10 H10 119.0 . . ?
C12 C10 C9 122.0(5) . . ?
C12 C10 H10 119.0 . . ?
C27 C28 C29 120.6(5) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C10 C12 H12 119.9 . . ?
C10 C12 C11 120.2(5) . . ?
C11 C12 H12 119.9 . . ?
C25 C24 C23 123.3(5) . . ?
C25 C24 C19 119.5(5) . . ?
C23 C24 C19 117.1(5) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 C24 121.8(6) . . ?
C22 C23 H23 119.1 . . ?
C14 C13 H13 119.3 . . ?
C11 C13 C14 121.4(5) . . ?
C11 C13 H13 119.3 . . ?
C18 C19 C24 118.6(5) . . ?
C18 C19 C20 122.5(5) . . ?
C20 C19 C24 118.9(5) . . ?
C12 C11 H11 119.9 . . ?
C13 C11 C12 120.2(5) . . ?
C13 C11 H11 119.9 . . ?
C23 C22 H22 119.9 . . ?
C23 C22 C21 120.2(6) . . ?
C21 C22 H22 119.9 . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.5(6) . . ?
C21 C20 H20 119.3 . . ?
C22 C21 H21 119.8 . . ?
C20 C21 C22 120.5(7) . . ?
C20 C21 H21 119.8 . . ?
H2WA O2W H2WB 104.5 . . ?
C42B O1 H1A 109.5 . . ?
C42A O1 H1B 109.5 . . ?
O1 C42B H42A 110.1 . . ?
O1 C42B H42B 110.1 . . ?
O1 C42B C41B 107.9(11) . . ?
H42A C42B H42B 108.4 . . ?
C41B C42B H42A 110.1 . . ?
C41B C42B H42B 110.1 . . ?
H36A C36B H36B 107.1 . . ?
C37B C36B H36A 107.8 . . ?
C37B C36B H36B 107.8 . . ?
C35B C36B H36A 107.8 . . ?
C35B C36B H36B 107.8 . . ?
C35B C36B C37B 118.1(11) . . ?
C36B C37B H37A 108.2 . . ?
C36B C37B H37B 108.2 . . ?
H37A C37B H37B 107.4 . . ?
C38B C37B C36B 116.3(11) . . ?
C38B C37B H37A 108.2 . . ?
C38B C37B H37B 108.2 . . ?
C36B C35B H35A 109.5 . . ?
C36B C35B H35B 109.5 . . ?
C36B C35B H35C 109.5 . . ?
H35A C35B H35B 109.5 . . ?
H35A C35B H35C 109.5 . . ?
H35B C35B H35C 109.5 . . ?
C42B C41B H41A 109.5 . . ?
C42B C41B H41B 109.5 . . ?
C42B C41B C40B 110.7(12) . . ?
H41A C41B H41B 108.1 . . ?
C40B C41B H41A 109.5 . . ?
C40B C41B H41B 109.5 . . ?
H39A C39B H39B 107.0 . . ?
C38B C39B H39A 107.5 . . ?
C38B C39B H39B 107.5 . . ?
C40B C39B H39A 107.5 . . ?
C40B C39B H39B 107.5 . . ?
C40B C39B C38B 119.4(11) . . ?
C37B C38B C39B 113.8(11) . . ?
C37B C38B H38A 108.8 . . ?
C37B C38B H38B 108.8 . . ?
C39B C38B H38A 108.8 . . ?
C39B C38B H38B 108.8 . . ?
H38A C38B H38B 107.7 . . ?
C41B C40B H40A 107.0 . . ?
C41B C40B H40B 107.0 . . ?
C39B C40B C41B 121.2(11) . . ?
C39B C40B H40A 107.0 . . ?
C39B C40B H40B 107.0 . . ?
H40A C40B H40B 106.8 . . ?
H40C C40A H40D 107.9 . . ?
C41A C40A H40C 109.2 . . ?
C41A C40A H40D 109.2 . . ?
C39A C40A H40C 109.2 . . ?
C39A C40A H40D 109.2 . . ?
C39A C40A C41A 111.8(16) . . ?
C40A C41A H41C 110.3 . . ?
C40A C41A H41D 110.3 . . ?
H41C C41A H41D 108.5 . . ?
C42A C41A C40A 107.2(14) . . ?
C42A C41A H41C 110.3 . . ?
C42A C41A H41D 110.3 . . ?
H38C C38A H38D 107.0 . . ?
C39A C38A H38C 107.6 . . ?
C39A C38A H38D 107.6 . . ?
C39A C38A C37A 118.9(16) . . ?
C37A C38A H38C 107.6 . . ?
C37A C38A H38D 107.6 . . ?
C40A C39A C38A 115.3(16) . . ?
C40A C39A H39C 108.5 . . ?
C40A C39A H39D 108.5 . . ?
C38A C39A H39C 108.5 . . ?
C38A C39A H39D 108.5 . . ?
H39C C39A H39D 107.5 . . ?
O1 C42A C41A 110.3(14) . . ?
O1 C42A H42C 109.6 . . ?
O1 C42A H42D 109.6 . . ?
C41A C42A H42C 109.6 . . ?
C41A C42A H42D 109.6 . . ?
H42C C42A H42D 108.1 . . ?
H36C C36A H36D 108.0 . . ?
C37A C36A H36C 109.4 . . ?
C37A C36A H36D 109.4 . . ?
C35A C36A H36C 109.4 . . ?
C35A C36A H36D 109.4 . . ?
C35A C36A C37A 111.2(16) . . ?
C38A C37A C36A 114.5(16) . . ?
C38A C37A H37C 108.6 . . ?
C38A C37A H37D 108.6 . . ?
C36A C37A H37C 108.6 . . ?
C36A C37A H37D 108.6 . . ?
H37C C37A H37D 107.6 . . ?
C36A C35A H35D 109.5 . . ?
C36A C35A H35E 109.5 . . ?
C36A C35A H35F 109.5 . . ?
H35D C35A H35E 109.5 . . ?
H35D C35A H35F 109.5 . . ?
H35E C35A H35F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl2 C18 C19 C24 -179.2(4) . . . . ?
Cl2 C18 C19 C20 0.2(8) . . . . ?
Cl1 C1 C14 C9 -179.0(4) . . . . ?
Cl1 C1 C14 C13 1.4(7) . . . . ?
N2 C32 C25 C26 83.8(6) . . . . ?
N2 C32 C25 C24 -99.3(6) . . . . ?
C8 C7 C6 C5 -177.8(5) . . . . ?
C8 C9 C14 C1 0.9(7) . . . . ?
C8 C9 C14 C13 -179.5(5) . . . . ?
C8 C9 C10 C12 179.0(5) . . . . ?
C31 C26 C27 C28 -1.6(8) . . . . ?
C31 C26 C25 C32 177.8(4) . . . . ?
C31 C26 C25 C24 0.9(7) . . . . ?
C31 C18 C19 C24 0.1(9) . . . . ?
C31 C18 C19 C20 179.5(6) . . . . ?
C26 C31 C18 Cl2 179.1(4) . . . . ?
C26 C31 C18 C19 -0.2(8) . . . . ?
C26 C31 C30 C29 0.1(8) . . . . ?
C26 C27 C28 C29 1.3(10) . . . . ?
C26 C25 C24 C23 -179.6(5) . . . . ?
C26 C25 C24 C19 -1.1(8) . . . . ?
C16 N1 C15 C8 -165.0(4) . . . . ?
C27 C26 C25 C32 -2.2(7) . . . . ?
C27 C26 C25 C24 -179.1(5) . . . . ?
C32 C25 C24 C23 3.5(8) . . . . ?
C32 C25 C24 C19 -177.9(5) . . . . ?
C2 C7 C6 C5 1.4(7) . . . . ?
C2 C1 C14 C9 0.0(8) . . . . ?
C2 C1 C14 C13 -179.7(5) . . . . ?
C15 C8 C7 C2 -179.5(4) . . . . ?
C15 C8 C7 C6 -0.3(7) . . . . ?
C15 C8 C9 C14 179.0(4) . . . . ?
C15 C8 C9 C10 0.0(7) . . . . ?
C7 C8 C15 N1 79.6(5) . . . . ?
C7 C8 C9 C14 -1.2(7) . . . . ?
C7 C8 C9 C10 179.8(5) . . . . ?
C7 C2 C1 Cl1 178.5(4) . . . . ?
C7 C2 C1 C14 -0.5(7) . . . . ?
C7 C2 C3 C4 -1.6(8) . . . . ?
C7 C6 C5 C4 -1.5(9) . . . . ?
C17 N1 C15 C8 70.6(5) . . . . ?
C34 N2 C32 C25 77.7(6) . . . . ?
C9 C8 C15 N1 -100.6(5) . . . . ?
C9 C8 C7 C2 0.7(7) . . . . ?
C9 C8 C7 C6 179.9(5) . . . . ?
C9 C14 C13 C11 0.7(9) . . . . ?
C9 C10 C12 C11 0.1(9) . . . . ?
C25 C26 C27 C28 178.4(5) . . . . ?
C25 C24 C23 C22 176.8(7) . . . . ?
C25 C24 C19 C18 0.6(8) . . . . ?
C25 C24 C19 C20 -178.9(6) . . . . ?
C18 C31 C26 C27 179.7(5) . . . . ?
C18 C31 C26 C25 -0.3(7) . . . . ?
C18 C31 C30 C29 -178.7(6) . . . . ?
C18 C19 C20 C21 -177.8(7) . . . . ?
C1 C2 C7 C8 0.2(7) . . . . ?
C1 C2 C7 C6 -179.1(4) . . . . ?
C1 C2 C3 C4 177.6(5) . . . . ?
C1 C14 C13 C11 -179.7(6) . . . . ?
C33 N2 C32 C25 -158.2(5) . . . . ?
C30 C31 C26 C27 0.8(7) . . . . ?
C30 C31 C26 C25 -179.2(4) . . . . ?
C30 C31 C18 Cl2 -2.1(7) . . . . ?
C30 C31 C18 C19 178.6(5) . . . . ?
C30 C29 C28 C27 -0.3(11) . . . . ?
C14 C9 C10 C12 0.1(8) . . . . ?
C14 C13 C11 C12 -0.5(10) . . . . ?
C3 C2 C7 C8 179.4(5) . . . . ?
C3 C2 C7 C6 0.2(7) . . . . ?
C3 C2 C1 Cl1 -0.7(7) . . . . ?
C3 C2 C1 C14 -179.7(5) . . . . ?
C3 C4 C5 C6 0.1(9) . . . . ?
C5 C4 C3 C2 1.5(9) . . . . ?
C10 C9 C14 C1 179.9(5) . . . . ?
C10 C9 C14 C13 -0.5(7) . . . . ?
C10 C12 C11 C13 0.1(10) . . . . ?
C28 C29 C30 C31 -0.4(10) . . . . ?
C24 C23 C22 C21 2.5(13) . . . . ?
C24 C19 C20 C21 1.6(11) . . . . ?
C23 C24 C19 C18 179.2(6) . . . . ?
C23 C24 C19 C20 -0.2(9) . . . . ?
C23 C22 C21 C20 -1.0(14) . . . . ?
C19 C24 C23 C22 -1.8(10) . . . . ?
C19 C20 C21 C22 -1.1(13) . . . . ?
O1 C42B C41B C40B 172.5(11) . . . . ?
C42B C41B C40B C39B 107.5(19) . . . . ?
C36B C37B C38B C39B 175.6(15) . . . . ?
C35B C36B C37B C38B -166.5(17) . . . . ?
C38B C39B C40B C41B 179.9(16) . . . . ?
C40B C39B C38B C37B 160.9(17) . . . . ?
C40A C41A C42A O1 -164.2(15) . . . . ?
C41A C40A C39A C38A -168.0(16) . . . . ?
C39A C40A C41A C42A -175.4(16) . . . . ?
C39A C38A C37A C36A -169.5(16) . . . . ?
C37A C38A C39A C40A -178.6(17) . . . . ?
C35A C36A C37A C38A 175.4(16) . . . . ?

_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 4.710
_oxdiff_exptl_absorpt_empirical_full_min 0.680
####################################################################### 
# 
# 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_DCAn
_database_code_depnum_ccdc_archive 'CCDC 2240942'
loop_
_audit_author_name
_audit_author_address
'Binbin Luo'
;Shantou University
China
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
_audit_creation_date             2023-01-08
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H16 Cl N'
_chemical_formula_sum            'C17 H16 Cl N'
_chemical_formula_weight         269.76
_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'
Cl Cl 0.3639 0.7018 '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'

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

_cell_length_a                   9.3418(6)
_cell_length_b                   10.7903(6)
_cell_length_c                   14.0401(8)
_cell_angle_alpha                90
_cell_angle_beta                 100.427(2)
_cell_angle_gamma                90
_cell_volume                     1391.88(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    262.00
_cell_measurement_theta_max      66.750
_cell_measurement_theta_min      5.202
_shelx_estimated_absorpt_T_max   0.567
_shelx_estimated_absorpt_T_min   0.502
_exptl_absorpt_coefficient_mu    2.285
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5348
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1323 before and 0.0651 after correction.
The Ratio of minimum to maximum transmission is 0.7104.
The λ/2 correction factor is Not present.
;
_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    1.287
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17707
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.745
_diffrn_reflns_theta_max         66.745
_diffrn_reflns_theta_min         5.202
_diffrn_ambient_temperature      262.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2013
_reflns_number_total             2442
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.200
_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     174
_refine_ls_number_reflns         2442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.1032
_refine_ls_restrained_S_all      1.160
_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)+(0.1864P)²+0.3037P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2547
_refine_ls_wR_factor_ref         0.2797
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
1.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C11(H11), C10(H10), C8(H8), C9(H9), C1(H1), C3(H3), C2(H2)
1.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.70207(12) 0.84734(9) 0.51165(7) 0.0862(5) Uani 1 1 d . . . . .
N1 N 0.3042(2) 0.4498(3) 0.73933(16) 0.0550(7) Uani 1 1 d . . . . .
C6 C 0.4703(3) 0.5290(3) 0.63281(18) 0.0456(7) Uani 1 1 d . . . . .
C5 C 0.3901(3) 0.6159(3) 0.57064(18) 0.0501(7) Uani 1 1 d . . . . .
C15 C 0.3934(3) 0.4194(3) 0.6668(2) 0.0513(7) Uani 1 1 d . . . . .
H15A H 0.331672 0.381889 0.611337 0.062 Uiso 1 1 calc R U . . .
H15B H 0.465581 0.358319 0.694032 0.062 Uiso 1 1 calc R U . . .
C12 C 0.6956(3) 0.6431(3) 0.6208(2) 0.0527(8) Uani 1 1 d . . . . .
C4 C 0.2345(3) 0.6070(4) 0.5421(2) 0.0652(9) Uani 1 1 d . . . . .
H4 H 0.184941 0.542684 0.565985 0.078 Uiso 1 1 calc R U . . .
C14 C 0.4608(4) 0.7174(3) 0.53219(19) 0.0576(8) Uani 1 1 d . . . . .
C7 C 0.6227(3) 0.5427(3) 0.65948(18) 0.0473(7) Uani 1 1 d . . . . .
C13 C 0.6127(4) 0.7254(3) 0.5591(2) 0.0580(8) Uani 1 1 d . . . . .
C11 C 0.8521(4) 0.6508(4) 0.6480(3) 0.0671(10) Uani 1 1 d . . . . .
H11 H 0.901035 0.713812 0.622050 0.080 Uiso 1 1 calc R U . . .
C10 C 0.9291(3) 0.5698(4) 0.7095(3) 0.0733(10) Uani 1 1 d . . . . .
H10 H 1.029689 0.577418 0.725720 0.088 Uiso 1 1 calc R U . . .
C8 C 0.7120(3) 0.4606(3) 0.7249(2) 0.0609(8) Uani 1 1 d . . . . .
H8 H 0.667921 0.395329 0.751749 0.073 Uiso 1 1 calc R U . . .
C16 C 0.3924(4) 0.4975(4) 0.8276(2) 0.0781(11) Uani 1 1 d . . . . .
H16A H 0.330783 0.518333 0.872964 0.117 Uiso 1 1 calc R U . . .
H16B H 0.443594 0.570111 0.812831 0.117 Uiso 1 1 calc R U . . .
H16C H 0.461256 0.435438 0.855222 0.117 Uiso 1 1 calc R U . . .
C9 C 0.8581(3) 0.4743(4) 0.7492(3) 0.0721(10) Uani 1 1 d . . . . .
H9 H 0.911681 0.419409 0.792730 0.086 Uiso 1 1 calc R U . . .
C1 C 0.3771(5) 0.8027(4) 0.4682(3) 0.0793(11) Uani 1 1 d . . . . .
H1 H 0.422854 0.868245 0.442883 0.095 Uiso 1 1 calc R U . . .
C3 C 0.1598(4) 0.6904(5) 0.4811(3) 0.0858(13) Uani 1 1 d . . . . .
H3 H 0.059304 0.682807 0.463328 0.103 Uiso 1 1 calc R U . . .
C17 C 0.2242(4) 0.3387(4) 0.7586(3) 0.0831(13) Uani 1 1 d . . . . .
H17A H 0.291608 0.272477 0.778455 0.125 Uiso 1 1 calc R U . . .
H17B H 0.158201 0.315006 0.700926 0.125 Uiso 1 1 calc R U . . .
H17C H 0.170310 0.355855 0.809243 0.125 Uiso 1 1 calc R U . . .
C2 C 0.2320(6) 0.7892(5) 0.4440(3) 0.0967(14) Uani 1 1 d . . . . .
H2 H 0.178387 0.845955 0.402153 0.116 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C13 1.754(3) . ?
N1 C15 1.465(3) . ?
N1 C16 1.452(4) . ?
N1 C17 1.463(5) . ?
C6 C5 1.402(4) . ?
C6 C15 1.506(4) . ?
C6 C7 1.413(4) . ?
C5 C4 1.439(4) . ?
C5 C14 1.435(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C12 C7 1.437(4) . ?
C12 C13 1.376(5) . ?
C12 C11 1.445(5) . ?
C4 H4 0.9300 . ?
C4 C3 1.347(6) . ?
C14 C13 1.403(5) . ?
C14 C1 1.418(5) . ?
C7 C8 1.430(4) . ?
C11 H11 0.9300 . ?
C11 C10 1.342(6) . ?
C10 H10 0.9300 . ?
C10 C9 1.395(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.353(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C9 H9 0.9300 . ?
C1 H1 0.9300 . ?
C1 C2 1.344(7) . ?
C3 H3 0.9300 . ?
C3 C2 1.411(7) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C2 H2 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C16 N1 C15 111.4(2) . . ?
C16 N1 C17 111.2(3) . . ?
C17 N1 C15 108.6(3) . . ?
C5 C6 C15 119.4(2) . . ?
C5 C6 C7 119.6(3) . . ?
C7 C6 C15 120.9(3) . . ?
C6 C5 C4 121.9(3) . . ?
C6 C5 C14 120.9(3) . . ?
C14 C5 C4 117.2(3) . . ?
N1 C15 C6 114.1(2) . . ?
N1 C15 H15A 108.7 . . ?
N1 C15 H15B 108.7 . . ?
C6 C15 H15A 108.7 . . ?
C6 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
C7 C12 C11 118.0(3) . . ?
C13 C12 C7 118.2(3) . . ?
C13 C12 C11 123.8(3) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 C5 120.9(4) . . ?
C3 C4 H4 119.5 . . ?
C13 C14 C5 117.2(3) . . ?
C13 C14 C1 123.1(3) . . ?
C1 C14 C5 119.7(3) . . ?
C6 C7 C12 120.2(3) . . ?
C6 C7 C8 123.2(3) . . ?
C8 C7 C12 116.6(3) . . ?
C12 C13 Cl1 118.1(2) . . ?
C12 C13 C14 123.8(3) . . ?
C14 C13 Cl1 118.1(3) . . ?
C12 C11 H11 118.9 . . ?
C10 C11 C12 122.1(3) . . ?
C10 C11 H11 118.9 . . ?
C11 C10 H10 120.0 . . ?
C11 C10 C9 120.0(3) . . ?
C9 C10 H10 120.0 . . ?
C7 C8 H8 118.7 . . ?
C9 C8 C7 122.6(3) . . ?
C9 C8 H8 118.7 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C10 C9 H9 119.7 . . ?
C8 C9 C10 120.7(3) . . ?
C8 C9 H9 119.7 . . ?
C14 C1 H1 119.8 . . ?
C2 C1 C14 120.4(4) . . ?
C2 C1 H1 119.8 . . ?
C4 C3 H3 119.6 . . ?
C4 C3 C2 120.8(4) . . ?
C2 C3 H3 119.6 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C1 C2 C3 121.1(4) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?

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
C6 C5 C4 C3 -179.0(3) . . . . ?
C6 C5 C14 C13 0.2(4) . . . . ?
C6 C5 C14 C1 179.0(3) . . . . ?
C6 C7 C8 C9 179.4(3) . . . . ?
C5 C6 C15 N1 -73.5(3) . . . . ?
C5 C6 C7 C12 -1.8(4) . . . . ?
C5 C6 C7 C8 178.0(2) . . . . ?
C5 C4 C3 C2 -0.3(6) . . . . ?
C5 C14 C13 Cl1 179.1(2) . . . . ?
C5 C14 C13 C12 -1.0(4) . . . . ?
C5 C14 C1 C2 0.4(5) . . . . ?
C15 C6 C5 C4 3.2(4) . . . . ?
C15 C6 C5 C14 -176.3(2) . . . . ?
C15 C6 C7 C12 175.6(2) . . . . ?
C15 C6 C7 C8 -4.6(4) . . . . ?
C12 C7 C8 C9 -0.8(5) . . . . ?
C12 C11 C10 C9 0.2(5) . . . . ?
C4 C5 C14 C13 -179.3(2) . . . . ?
C4 C5 C14 C1 -0.6(4) . . . . ?
C4 C3 C2 C1 0.1(7) . . . . ?
C14 C5 C4 C3 0.5(5) . . . . ?
C14 C1 C2 C3 -0.2(7) . . . . ?
C7 C6 C5 C4 -179.3(2) . . . . ?
C7 C6 C5 C14 1.2(4) . . . . ?
C7 C6 C15 N1 109.0(3) . . . . ?
C7 C12 C13 Cl1 -179.72(19) . . . . ?
C7 C12 C13 C14 0.4(4) . . . . ?
C7 C12 C11 C10 -1.9(5) . . . . ?
C7 C8 C9 C10 -0.9(6) . . . . ?
C13 C12 C7 C6 1.1(4) . . . . ?
C13 C12 C7 C8 -178.7(2) . . . . ?
C13 C12 C11 C10 179.0(3) . . . . ?
C13 C14 C1 C2 179.1(4) . . . . ?
C11 C12 C7 C6 -178.1(2) . . . . ?
C11 C12 C7 C8 2.1(4) . . . . ?
C11 C12 C13 Cl1 -0.6(4) . . . . ?
C11 C12 C13 C14 179.5(3) . . . . ?
C11 C10 C9 C8 1.3(6) . . . . ?
C16 N1 C15 C6 -62.9(4) . . . . ?
C1 C14 C13 Cl1 0.4(4) . . . . ?
C1 C14 C13 C12 -179.7(3) . . . . ?
C17 N1 C15 C6 174.2(3) . . . . ?

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

data_1-C9
_database_code_depnum_ccdc_archive 'CCDC 2240935'
loop_
_audit_author_name
_audit_author_address
'Binbin Luo'
;Shantou University
China
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
_audit_creation_date             2023-01-08
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Br16 Pb5, 6(C17 H17 Cl N), 4(C9 H20 O), 2(H2 O)'
_chemical_formula_sum            'C138 H186 Br16 Cl6 N6 O6 Pb5'
_chemical_formula_weight         4552.13
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O Pb Br Cl'
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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5838(2)
_cell_length_b                   19.9092(4)
_cell_length_c                   20.8586(2)
_cell_angle_alpha                100.8410(10)
_cell_angle_beta                 101.844(2)
_cell_angle_gamma                91.795(2)
_cell_volume                     3815.55(12)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    25629
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.9810
_cell_measurement_theta_min      3.4690
_shelx_estimated_absorpt_T_max   0.487
_shelx_estimated_absorpt_T_min   0.057
_exptl_absorpt_coefficient_mu    16.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (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    1.981
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2176
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38507
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.282
_diffrn_reflns_theta_min         2.832
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  19.00   0.50    0.50    --    0.00  38.00  30.00   66
  2  ω    -21.00  15.00   0.50    0.50    --    0.00 -38.00 150.00   72
  3  ω     30.00  87.00   0.50    0.50    --    0.00  38.00  30.00  114
  4  ω     33.00  87.00   0.50    0.50    --    0.00  19.00 -60.00  108
  5  ω    -27.00  36.00   0.50    0.50    --    0.00  77.00 -60.00  126
  6  ω    -85.00 -47.00   0.50    0.50    --    0.00 -38.00 150.00   76
  7  ω     87.00 113.00   0.50    1.07    --   89.30 -82.00-150.00   52
  8  ω     40.00  66.00   0.50    1.07    --   89.30 -82.00-150.00   52
  9  ω      0.00 113.00   0.50    1.07    --   89.30 -61.00 150.00  226
 10  ω     70.00 163.00   0.50    1.07    --   89.30  45.00 -90.00  186
 11  ω     33.00  76.00   0.50    1.07    --   89.30 -82.00 -60.00   86
 12  ω     83.00 115.00   0.50    1.07    --   89.30 -82.00 -60.00   64
 13  ω    112.00 177.00   0.50    1.07    --   89.30  30.00   0.00  130
 14  ω     13.00  98.00   0.50    1.07    --   89.30 -82.00  60.00  170
 15  ω     44.00 103.00   0.50    1.07    --   89.30 -30.00 -90.00  118
 16  ω     81.00 106.00   0.50    1.07    --   89.30 -15.00 -90.00   50
 17  ω      0.00  40.00   0.50    1.07    --   89.30 -15.00 -90.00   80
 18  ω     21.00 121.00   0.50    1.07    --   89.30 -82.00 150.00  200
 19  ω      3.00  79.00   0.50    1.07    --   89.30 -61.00  60.00  152
 20  ω     92.00 118.00   0.50    1.07    --   89.30 -82.00   0.00   52
 21  ω     81.00 110.00   0.50    1.07    --   89.30 -82.00-120.00   58
 22  ω     82.00 107.00   0.50    1.07    --   89.30 -82.00  90.00   50
 23  ω     16.00 109.00   0.50    1.07    --   89.30 -61.00 -60.00  186
 24  ω     89.00 174.00   0.50    1.07    --   89.30  45.00-120.00  170
;
_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      0.0760079000
_diffrn_orient_matrix_UB_12      -0.0623304000
_diffrn_orient_matrix_UB_13      -0.0281429000
_diffrn_orient_matrix_UB_21      -0.0233415000
_diffrn_orient_matrix_UB_22      -0.0348489000
_diffrn_orient_matrix_UB_23      0.0573254000
_diffrn_orient_matrix_UB_31      -0.1442130000
_diffrn_orient_matrix_UB_32      -0.0337732000
_diffrn_orient_matrix_UB_33      -0.0430229000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13069
_reflns_number_total             14237
_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 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.725
_refine_diff_density_min         -1.682
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         14237
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0331
_refine_ls_restrained_S_all      1.052
_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)+(0.0589P)²+3.4484P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0922
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Free rotating group:
 O3(H3B,H3C)
1.b Ternary CH refined with riding coordinates:
 N3(H3), N2(H2), N1(H1)
1.c Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C15(H15A,H15B), C48(H48A,H48B), C68(H68A,H68B), C67(H67A,
 H67B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C66(H66A,H66B),
 C65(H65A,H65B), C64(H64A,H64B), C59(H59A,H59B), C52(H52A,H52B), C53(H53A,H53B),
  C54(H54A,H54B), C58(H58A,H58B), C57(H57A,H57B), C55(H55A,H55B), C56(H56A,H56B)
1.d Aromatic/amide H refined with riding coordinates:
 C27(H27), C39(H39), C28(H28), C10(H10), C23(H23), C6(H6), C38(H38), C11(H11),
 C5(H5), C20(H20), C44(H44), C21(H21), C3(H3A), C22(H22), C29(H29), C43(H43),
 C4(H4), C12(H12), C30(H30), C37(H37), C13(H13), C36(H36), C45(H45), C46(H46)
1.e Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C50(H50A,H50B,H50C), C16(H16A,H16B,H16C), C49(H49A,H49B,
 H49C), C17(H17A,H17B,H17C), C32(H32A,H32B,H32C), C60(H60A,H60B,H60C), C51(H51A,
 H51B,H51C)
1.f Idealised tetrahedral OH refined as rotating group:
 O2(H2A), O1(H1A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb3 Pb 0.500000 0.000000 0.500000 0.01909(7) Uani 1 2 d S . P . .
Pb2 Pb 0.49884(2) 0.18784(2) 0.47979(2) 0.01867(6) Uani 1 1 d . . . . .
Pb1 Pb 0.44003(2) 0.38374(2) 0.46823(2) 0.01912(6) Uani 1 1 d . . . . .
Br8 Br 0.71531(5) 0.07878(2) 0.44982(2) 0.02195(11) Uani 1 1 d . . . . .
Br6 Br 0.28122(5) 0.06236(2) 0.40716(2) 0.02409(11) Uani 1 1 d . . . . .
Br2 Br 0.56822(5) 0.49649(2) 0.41364(2) 0.02597(11) Uani 1 1 d . . . . .
Br3 Br 0.16379(5) 0.39586(3) 0.40096(3) 0.02729(11) Uani 1 1 d . . . . .
Br4 Br 0.43603(5) 0.26064(3) 0.36287(2) 0.02667(11) Uani 1 1 d . . . . .
Br1 Br 0.73608(5) 0.29076(3) 0.52401(3) 0.02782(12) Uani 1 1 d . . . . .
Br5 Br 0.32070(6) 0.28708(3) 0.54402(3) 0.02830(12) Uani 1 1 d . . . . .
Br7 Br 0.52311(6) 0.12951(3) 0.60301(3) 0.03103(12) Uani 1 1 d . . . . .
Cl2 Cl 0.20215(13) 0.10204(6) 0.95017(5) 0.0287(2) Uani 1 1 d . . . . .
Cl3 Cl -0.26874(13) 0.09422(7) 0.00505(6) 0.0324(3) Uani 1 1 d . . . . .
Cl1 Cl 1.23858(14) 0.49224(7) 0.97626(6) 0.0330(3) Uani 1 1 d . . . . .
O2 O 0.1079(4) 0.24027(18) 0.27407(18) 0.0290(8) Uani 1 1 d . . . . .
H2A H 0.178685 0.266453 0.296409 0.043 Uiso 1 1 calc R U . . .
O3 O 0.7376(4) 0.42772(18) 0.63960(18) 0.0293(8) Uani 1 1 d G . . . .
H3B H 0.708717 0.389736 0.612997 0.044 Uiso 1 1 d G U . . .
H3C H 0.681132 0.456139 0.625081 0.044 Uiso 1 1 d G U . . .
N3 N -0.0755(4) 0.19664(19) 0.34167(18) 0.0193(8) Uani 1 1 d . . . . .
H3 H -0.000837 0.205411 0.316439 0.023 Uiso 1 1 calc R U . . .
N2 N 0.0853(4) 0.11972(19) 0.61959(19) 0.0213(8) Uani 1 1 d . . . . .
H2 H 0.178998 0.140214 0.648623 0.026 Uiso 1 1 calc R U . . .
N1 N 1.0254(4) 0.43825(19) 0.63440(18) 0.0204(8) Uani 1 1 d . . . . .
H1 H 0.926946 0.441723 0.643209 0.025 Uiso 1 1 calc R U . . .
O1 O 0.3027(5) 0.2099(3) 0.6890(2) 0.0610(15) Uani 1 1 d . . . . .
H1A H 0.381760 0.218851 0.679915 0.092 Uiso 1 1 calc R U . . .
C33 C 0.1071(6) 0.0970(3) 0.5505(2) 0.0263(10) Uani 1 1 d . . . . .
H33A H 0.176462 0.061880 0.550199 0.039 Uiso 1 1 calc R U . . .
H33B H 0.143249 0.136289 0.535008 0.039 Uiso 1 1 calc R U . . .
H33C H 0.015950 0.077893 0.520803 0.039 Uiso 1 1 calc R U . . .
C50 C -0.0008(5) 0.1963(3) 0.4117(2) 0.0259(10) Uani 1 1 d . . . . .
H50A H 0.052431 0.240762 0.431452 0.039 Uiso 1 1 calc R U . . .
H50B H 0.065687 0.159919 0.411737 0.039 Uiso 1 1 calc R U . . .
H50C H -0.071279 0.188150 0.437879 0.039 Uiso 1 1 calc R U . . .
C16 C 1.0176(6) 0.4436(3) 0.5630(2) 0.0265(10) Uani 1 1 d . . . . .
H16A H 0.979732 0.487324 0.555518 0.040 Uiso 1 1 calc R U . . .
H16B H 0.954416 0.405679 0.533433 0.040 Uiso 1 1 calc R U . . .
H16C H 1.113412 0.441389 0.553414 0.040 Uiso 1 1 calc R U . . .
C31 C 0.0374(5) 0.0598(2) 0.6473(2) 0.0206(9) Uani 1 1 d . . . . .
H31A H -0.067622 0.050813 0.632411 0.025 Uiso 1 1 calc R U . . .
H31B H 0.082045 0.018243 0.629253 0.025 Uiso 1 1 calc R U . . .
C27 C 0.3219(5) 0.0366(2) 0.7175(2) 0.0223(10) Uani 1 1 d . . . . .
H27 H 0.299912 0.032823 0.670356 0.027 Uiso 1 1 calc R U . . .
C26 C 0.2164(5) 0.0595(2) 0.7542(2) 0.0184(9) Uani 1 1 d . . . . .
C15 C 1.1200(5) 0.4977(2) 0.6804(2) 0.0207(9) Uani 1 1 d . . . . .
H15A H 1.074709 0.540904 0.674879 0.025 Uiso 1 1 calc R U . . .
H15B H 1.212845 0.499872 0.666790 0.025 Uiso 1 1 calc R U . . .
C49 C -0.1700(5) 0.2548(2) 0.3415(3) 0.0250(10) Uani 1 1 d . . . . .
H49A H -0.239146 0.249936 0.369367 0.038 Uiso 1 1 calc R U . . .
H49B H -0.221180 0.254545 0.295682 0.038 Uiso 1 1 calc R U . . .
H49C H -0.111829 0.298250 0.359479 0.038 Uiso 1 1 calc R U . . .
C17 C 1.0735(5) 0.3703(2) 0.6453(2) 0.0238(10) Uani 1 1 d . . . . .
H17A H 1.005784 0.333999 0.615979 0.036 Uiso 1 1 calc R U . . .
H17B H 1.078109 0.367209 0.692060 0.036 Uiso 1 1 calc R U . . .
H17C H 1.168479 0.364908 0.635226 0.036 Uiso 1 1 calc R U . . .
C24 C -0.0229(5) 0.0953(2) 0.7622(2) 0.0189(9) Uani 1 1 d . . . . .
C39 C 0.0576(5) 0.0799(2) 0.2307(2) 0.0218(10) Uani 1 1 d . . . . .
H39 H 0.078416 0.085291 0.277976 0.026 Uiso 1 1 calc R U . . .
C25 C 0.0773(5) 0.0735(2) 0.7231(2) 0.0205(9) Uani 1 1 d . . . . .
C48 C -0.1551(5) 0.1284(2) 0.3069(2) 0.0203(9) Uani 1 1 d . . . . .
H48A H -0.097641 0.091004 0.320491 0.024 Uiso 1 1 calc R U . . .
H48B H -0.246474 0.124929 0.321650 0.024 Uiso 1 1 calc R U . . .
C32 C -0.0186(6) 0.1746(3) 0.6202(3) 0.0316(12) Uani 1 1 d . . . . .
H32A H 0.016072 0.212092 0.601806 0.047 Uiso 1 1 calc R U . . .
H32B H -0.027478 0.192063 0.666241 0.047 Uiso 1 1 calc R U . . .
H32C H -0.112096 0.155347 0.592981 0.047 Uiso 1 1 calc R U . . .
C28 C 0.4518(5) 0.0202(2) 0.7470(3) 0.0265(10) Uani 1 1 d . . . . .
H28 H 0.518223 0.003653 0.720715 0.032 Uiso 1 1 calc R U . . .
C10 C 1.3878(5) 0.4491(2) 0.7494(2) 0.0238(10) Uani 1 1 d . . . . .
H10 H 1.371782 0.448302 0.702801 0.029 Uiso 1 1 calc R U . . .
C7 C 1.0428(5) 0.5123(2) 0.7908(2) 0.0202(9) Uani 1 1 d . . . . .
C23 C -0.1662(5) 0.1082(2) 0.7336(2) 0.0239(10) Uani 1 1 d . . . . .
H23 H -0.196714 0.100687 0.686331 0.029 Uiso 1 1 calc R U . . .
C6 C 0.9080(5) 0.5344(2) 0.7618(2) 0.0214(9) Uani 1 1 d . . . . .
H6 H 0.888802 0.538146 0.716138 0.026 Uiso 1 1 calc R U . . .
C41 C -0.1862(5) 0.1191(2) 0.2316(2) 0.0194(9) Uani 1 1 d . . . . .
C38 C 0.1588(5) 0.0571(2) 0.1963(3) 0.0259(10) Uani 1 1 d . . . . .
H38 H 0.248467 0.046498 0.219903 0.031 Uiso 1 1 calc R U . . .
C9 C 1.2777(5) 0.4710(2) 0.7839(2) 0.0208(9) Uani 1 1 d . . . . .
C11 C 1.5136(5) 0.4294(3) 0.7800(3) 0.0305(11) Uani 1 1 d . . . . .
H11 H 1.582629 0.414144 0.754794 0.037 Uiso 1 1 calc R U . . .
C5 C 0.8060(5) 0.5504(2) 0.7982(2) 0.0247(10) Uani 1 1 d . . . . .
H5 H 0.717390 0.564773 0.777379 0.030 Uiso 1 1 calc R U . . .
C20 C -0.0855(5) 0.1287(2) 0.8728(3) 0.0247(10) Uani 1 1 d . . . . .
H20 H -0.059104 0.135782 0.920153 0.030 Uiso 1 1 calc R U . . .
C01A C 0.2548(5) 0.0681(2) 0.8262(2) 0.0197(9) Uani 1 1 d . . . . .
C68 C 0.0302(6) 0.2724(3) 0.2231(3) 0.0282(11) Uani 1 1 d . . . . .
H68A H 0.029950 0.322018 0.241396 0.034 Uiso 1 1 calc R U . . .
H68B H -0.070223 0.252921 0.210589 0.034 Uiso 1 1 calc R U . . .
C40 C -0.0790(5) 0.0961(2) 0.1973(2) 0.0185(9) Uani 1 1 d . . . . .
C44 C -0.5643(5) 0.1679(2) 0.1917(3) 0.0266(10) Uani 1 1 d . . . . .
H44 H -0.638102 0.182128 0.214245 0.032 Uiso 1 1 calc R U . . .
C67 C 0.0916(5) 0.2633(3) 0.1617(3) 0.0274(11) Uani 1 1 d . . . . .
H67A H 0.110015 0.214507 0.148331 0.033 Uiso 1 1 calc R U . . .
H67B H 0.183948 0.290925 0.171790 0.033 Uiso 1 1 calc R U . . .
C21 C -0.2196(5) 0.1415(3) 0.8433(3) 0.0272(11) Uani 1 1 d . . . . .
H21 H -0.285929 0.157244 0.869905 0.033 Uiso 1 1 calc R U . . .
C3 C 0.9578(5) 0.5262(2) 0.8964(2) 0.0260(10) Uani 1 1 d . . . . .
H3A H 0.973571 0.523797 0.942404 0.031 Uiso 1 1 calc R U . . .
C22 C -0.2598(5) 0.1310(3) 0.7727(3) 0.0273(11) Uani 1 1 d . . . . .
H22 H -0.353441 0.140120 0.752188 0.033 Uiso 1 1 calc R U . . .
C19 C 0.0164(5) 0.1050(2) 0.8341(2) 0.0204(9) Uani 1 1 d . . . . .
C29 C 0.4889(5) 0.0278(3) 0.8184(3) 0.0275(11) Uani 1 1 d . . . . .
H29 H 0.580282 0.016300 0.839317 0.033 Uiso 1 1 calc R U . . .
C43 C -0.4348(5) 0.1543(2) 0.2273(2) 0.0235(10) Uani 1 1 d . . . . .
H43 H -0.420834 0.159276 0.274441 0.028 Uiso 1 1 calc R U . . .
C2 C 1.0682(5) 0.5092(2) 0.8609(2) 0.0206(9) Uani 1 1 d . . . . .
C4 C 0.8302(5) 0.5458(2) 0.8659(3) 0.0269(10) Uani 1 1 d . . . . .
H4 H 0.757651 0.556311 0.890373 0.032 Uiso 1 1 calc R U . . .
C8 C 1.1470(5) 0.4929(2) 0.7536(2) 0.0196(9) Uani 1 1 d . . . . .
C14 C 1.3082(5) 0.4709(2) 0.8552(2) 0.0210(9) Uani 1 1 d . . . . .
C12 C 1.5428(5) 0.4313(3) 0.8502(3) 0.0314(12) Uani 1 1 d . . . . .
H12 H 1.632321 0.418693 0.871942 0.038 Uiso 1 1 calc R U . . .
C30 C 0.3950(5) 0.0511(3) 0.8561(2) 0.0252(10) Uani 1 1 d . . . . .
H30 H 0.421990 0.056458 0.903291 0.030 Uiso 1 1 calc R U . . .
C37 C 0.1324(5) 0.0488(3) 0.1261(3) 0.0271(11) Uani 1 1 d . . . . .
H37 H 0.204225 0.032781 0.102880 0.033 Uiso 1 1 calc R U . . .
C13 C 1.4440(5) 0.4510(3) 0.8854(3) 0.0268(11) Uani 1 1 d . . . . .
H13 H 1.464939 0.451833 0.932050 0.032 Uiso 1 1 calc R U . . .
C61 C -0.0592(6) 0.3055(3) -0.2019(3) 0.0335(12) Uani 1 1 d . . . . .
H61A H 0.027420 0.334879 -0.199890 0.040 Uiso 1 1 calc R U . . .
H61B H -0.035209 0.257083 -0.210762 0.040 Uiso 1 1 calc R U . . .
C36 C 0.0048(5) 0.0636(2) 0.0917(2) 0.0253(10) Uani 1 1 d . . . . .
H36 H -0.011833 0.057974 0.044429 0.030 Uiso 1 1 calc R U . . .
C45 C -0.5881(5) 0.1607(3) 0.1220(3) 0.0307(11) Uani 1 1 d . . . . .
H45 H -0.677539 0.170748 0.097672 0.037 Uiso 1 1 calc R U . . .
C47 C -0.3472(5) 0.1246(2) 0.1236(2) 0.0218(10) Uani 1 1 d . . . . .
C35 C -0.1047(5) 0.0875(2) 0.1255(2) 0.0212(9) Uani 1 1 d . . . . .
C60 C -0.1767(7) 0.3172(3) -0.2584(3) 0.0458(15) Uani 1 1 d . . . . .
H60A H -0.148765 0.301670 -0.301137 0.069 Uiso 1 1 calc R U . . .
H60B H -0.192243 0.366190 -0.252743 0.069 Uiso 1 1 calc R U . . .
H60C H -0.265080 0.291354 -0.258005 0.069 Uiso 1 1 calc R U . . .
C46 C -0.4836(5) 0.1396(3) 0.0891(2) 0.0255(10) Uani 1 1 d . . . . .
H46 H -0.502012 0.134574 0.041867 0.031 Uiso 1 1 calc R U . . .
C62 C -0.1035(6) 0.3216(3) -0.1351(3) 0.0339(12) Uani 1 1 d . . . . .
H62A H -0.194328 0.294571 -0.138709 0.041 Uiso 1 1 calc R U . . .
H62B H -0.121902 0.370703 -0.125473 0.041 Uiso 1 1 calc R U . . .
C18 C 0.1543(5) 0.0911(2) 0.8634(2) 0.0227(10) Uani 1 1 d . . . . .
C51 C 0.5972(7) 0.3659(3) 1.2539(3) 0.0434(15) Uani 1 1 d . . . . .
H51A H 0.567766 0.412727 1.255099 0.065 Uiso 1 1 calc R U . . .
H51B H 0.676803 0.365562 1.291727 0.065 Uiso 1 1 calc R U . . .
H51C H 0.516622 0.335864 1.256640 0.065 Uiso 1 1 calc R U . . .
C42 C -0.3216(5) 0.1332(2) 0.1958(2) 0.0189(9) Uani 1 1 d . . . . .
C63 C 0.0063(6) 0.3064(3) -0.0768(3) 0.0301(11) Uani 1 1 d . . . . .
H63A H 0.086974 0.341826 -0.065037 0.036 Uiso 1 1 calc R U . . .
H63B H 0.044189 0.261537 -0.090842 0.036 Uiso 1 1 calc R U . . .
C1 C 1.2017(5) 0.4908(2) 0.8902(2) 0.0232(10) Uani 1 1 d . . . . .
C66 C -0.0103(5) 0.2853(3) 0.1039(3) 0.0284(11) Uani 1 1 d . . . . .
H66A H -0.098805 0.254493 0.091534 0.034 Uiso 1 1 calc R U . . .
H66B H -0.036724 0.332282 0.119553 0.034 Uiso 1 1 calc R U . . .
C34 C -0.2381(5) 0.1030(2) 0.0920(2) 0.0226(10) Uani 1 1 d . . . . .
C65 C 0.0508(6) 0.2843(3) 0.0418(3) 0.0317(11) Uani 1 1 d . . . . .
H65A H 0.137615 0.316162 0.053579 0.038 Uiso 1 1 calc R U . . .
H65B H 0.079326 0.237632 0.026507 0.038 Uiso 1 1 calc R U . . .
C64 C -0.0542(6) 0.3045(3) -0.0149(3) 0.0317(11) Uani 1 1 d . . . . .
H64A H -0.085453 0.350465 0.001039 0.038 Uiso 1 1 calc R U . . .
H64B H -0.139559 0.271685 -0.027597 0.038 Uiso 1 1 calc R U . . .
C59 C 0.3005(7) 0.2466(4) 0.7557(4) 0.0539(18) Uani 1 1 d . . . . .
H59A H 0.208860 0.232534 0.766005 0.065 Uiso 1 1 calc R U . . .
H59B H 0.298441 0.295988 0.754159 0.065 Uiso 1 1 calc R U . . .
C52 C 0.6421(7) 0.3417(3) 1.1924(4) 0.0481(16) Uani 1 1 d . . . . .
H52A H 0.669920 0.294171 1.191744 0.058 Uiso 1 1 calc R U . . .
H52B H 0.728474 0.370222 1.192240 0.058 Uiso 1 1 calc R U . . .
C53 C 0.5348(8) 0.3423(3) 1.1298(3) 0.0514(18) Uani 1 1 d . . . . .
H53A H 0.447662 0.314709 1.130657 0.062 Uiso 1 1 calc R U . . .
H53B H 0.508453 0.390059 1.130263 0.062 Uiso 1 1 calc R U . . .
C54 C 0.5773(8) 0.3164(4) 1.0659(4) 0.0547(18) Uani 1 1 d . . . . .
H54A H 0.619664 0.272035 1.068601 0.066 Uiso 1 1 calc R U . . .
H54B H 0.653264 0.348864 1.061308 0.066 Uiso 1 1 calc R U . . .
C58 C 0.4144(8) 0.2398(3) 0.8120(4) 0.0545(18) Uani 1 1 d . . . . .
H58A H 0.503571 0.263792 0.808272 0.065 Uiso 1 1 calc R U . . .
H58B H 0.431204 0.190703 0.809513 0.065 Uiso 1 1 calc R U . . .
C57 C 0.3818(8) 0.2683(4) 0.8782(4) 0.0540(18) Uani 1 1 d . . . . .
H57A H 0.304045 0.238025 0.884714 0.065 Uiso 1 1 calc R U . . .
H57B H 0.343504 0.313597 0.875984 0.065 Uiso 1 1 calc R U . . .
C55 C 0.4617(8) 0.3061(4) 1.0037(4) 0.0548(18) Uani 1 1 d . . . . .
H55A H 0.383703 0.275452 1.009457 0.066 Uiso 1 1 calc R U . . .
H55B H 0.422400 0.350962 1.000178 0.066 Uiso 1 1 calc R U . . .
C56 C 0.5001(8) 0.2774(4) 0.9395(4) 0.0569(18) Uani 1 1 d . . . . .
H56A H 0.538177 0.232143 0.942507 0.068 Uiso 1 1 calc R U . . .
H56B H 0.578252 0.307711 0.933535 0.068 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb3 Br8 3.0190(5) 2_656 ?
Pb3 Br8 3.0190(5) . ?
Pb3 Br6 3.0148(5) . ?
Pb3 Br6 3.0148(5) 2_656 ?
Pb3 Br7 2.9998(5) 2_656 ?
Pb3 Br7 2.9999(5) . ?
Pb2 Br8 3.1166(5) . ?
Pb2 Br6 3.1367(5) . ?
Pb2 Br4 3.0320(5) . ?
Pb2 Br1 2.8905(5) . ?
Pb2 Br5 2.9610(5) . ?
Pb2 Br7 2.9836(5) . ?
Pb1 Br2 3.1056(5) 2_666 ?
Pb1 Br2 3.0344(5) . ?
Pb1 Br3 2.7711(5) . ?
Pb1 Br4 2.9617(5) . ?
Pb1 Br5 3.0429(5) . ?
Cl2 C18 1.744(5) . ?
Cl3 C34 1.751(5) . ?
Cl1 C1 1.752(5) . ?
O2 H2A 0.8400 . ?
O2 C68 1.433(6) . ?
O3 H3B 0.8500 . ?
O3 H3C 0.8495 . ?
N3 H3 1.0000 . ?
N3 C50 1.490(6) . ?
N3 C49 1.493(6) . ?
N3 C48 1.513(5) . ?
N2 H2 1.0000 . ?
N2 C33 1.486(6) . ?
N2 C31 1.518(6) . ?
N2 C32 1.500(6) . ?
N1 H1 1.0000 . ?
N1 C16 1.500(6) . ?
N1 C15 1.514(6) . ?
N1 C17 1.485(6) . ?
O1 H1A 0.8400 . ?
O1 C59 1.449(8) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C25 1.517(6) . ?
C27 H27 0.9500 . ?
C27 C26 1.424(6) . ?
C27 C28 1.351(7) . ?
C26 C25 1.418(6) . ?
C26 C01A 1.447(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C8 1.517(6) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C24 C25 1.411(6) . ?
C24 C23 1.432(6) . ?
C24 C19 1.443(6) . ?
C39 H39 0.9500 . ?
C39 C38 1.361(7) . ?
C39 C40 1.429(6) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C41 1.512(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C28 H28 0.9500 . ?
C28 C29 1.436(7) . ?
C10 H10 0.9500 . ?
C10 C9 1.430(7) . ?
C10 C11 1.350(7) . ?
C7 C6 1.430(6) . ?
C7 C2 1.446(6) . ?
C7 C8 1.406(6) . ?
C23 H23 0.9500 . ?
C23 C22 1.365(7) . ?
C6 H6 0.9500 . ?
C6 C5 1.365(7) . ?
C41 C40 1.408(6) . ?
C41 C42 1.423(6) . ?
C38 H38 0.9500 . ?
C38 C37 1.410(7) . ?
C9 C8 1.404(6) . ?
C9 C14 1.456(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.425(8) . ?
C5 H5 0.9500 . ?
C5 C4 1.404(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.359(7) . ?
C20 C19 1.428(6) . ?
C01A C30 1.440(6) . ?
C01A C18 1.393(7) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C68 C67 1.500(7) . ?
C40 C35 1.444(6) . ?
C44 H44 0.9500 . ?
C44 C43 1.372(7) . ?
C44 C45 1.403(7) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C67 C66 1.530(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.418(7) . ?
C3 H3A 0.9500 . ?
C3 C2 1.426(7) . ?
C3 C4 1.363(7) . ?
C22 H22 0.9500 . ?
C19 C18 1.397(6) . ?
C29 H29 0.9500 . ?
C29 C30 1.350(7) . ?
C43 H43 0.9500 . ?
C43 C42 1.416(6) . ?
C2 C1 1.391(7) . ?
C4 H4 0.9500 . ?
C14 C13 1.427(6) . ?
C14 C1 1.398(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.337(7) . ?
C30 H30 0.9500 . ?
C37 H37 0.9500 . ?
C37 C36 1.356(7) . ?
C13 H13 0.9500 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C60 1.512(8) . ?
C61 C62 1.519(7) . ?
C36 H36 0.9500 . ?
C36 C35 1.426(6) . ?
C45 H45 0.9500 . ?
C45 C46 1.360(7) . ?
C47 C46 1.426(7) . ?
C47 C42 1.451(6) . ?
C47 C34 1.385(7) . ?
C35 C34 1.399(7) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C46 H46 0.9500 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 C63 1.521(7) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C51 C52 1.438(9) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.524(7) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C66 C65 1.525(7) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C65 C64 1.513(7) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C58 1.460(10) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C53 1.489(9) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.478(10) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C54 C55 1.500(10) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C57 1.490(10) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C56 1.502(10) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C56 1.478(11) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?

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
Br8 Pb3 Br8 180.0 . 2_656 ?
Br6 Pb3 Br8 95.394(13) . 2_656 ?
Br6 Pb3 Br8 84.606(13) 2_656 2_656 ?
Br6 Pb3 Br8 84.607(13) . . ?
Br6 Pb3 Br8 95.394(13) 2_656 . ?
Br6 Pb3 Br6 180.0 . 2_656 ?
Br7 Pb3 Br8 96.890(14) . 2_656 ?
Br7 Pb3 Br8 83.111(14) . . ?
Br7 Pb3 Br8 96.887(14) 2_656 . ?
Br7 Pb3 Br8 83.111(14) 2_656 2_656 ?
Br7 Pb3 Br6 91.185(13) . 2_656 ?
Br7 Pb3 Br6 88.816(13) . . ?
Br7 Pb3 Br6 88.816(13) 2_656 2_656 ?
Br7 Pb3 Br6 91.183(13) 2_656 . ?
Br7 Pb3 Br7 180.0 2_656 . ?
Br8 Pb2 Br6 80.995(13) . . ?
Br4 Pb2 Br8 107.688(14) . . ?
Br4 Pb2 Br6 93.538(14) . . ?
Br1 Pb2 Br8 88.543(14) . . ?
Br1 Pb2 Br6 166.806(16) . . ?
Br1 Pb2 Br4 81.946(15) . . ?
Br1 Pb2 Br5 88.593(15) . . ?
Br1 Pb2 Br7 99.645(16) . . ?
Br5 Pb2 Br8 165.244(15) . . ?
Br5 Pb2 Br6 103.536(15) . . ?
Br5 Pb2 Br4 86.223(14) . . ?
Br5 Pb2 Br7 84.484(15) . . ?
Br7 Pb2 Br8 81.733(14) . . ?
Br7 Pb2 Br6 86.855(15) . . ?
Br7 Pb2 Br4 170.525(15) . . ?
Br2 Pb1 Br2 82.722(14) . 2_666 ?
Br2 Pb1 Br5 170.859(15) . . ?
Br3 Pb1 Br2 94.272(15) . 2_666 ?
Br3 Pb1 Br2 93.796(15) . . ?
Br3 Pb1 Br4 85.533(15) . . ?
Br3 Pb1 Br5 89.021(16) . . ?
Br4 Pb1 Br2 102.863(15) . . ?
Br4 Pb1 Br2 174.413(15) . 2_666 ?
Br4 Pb1 Br5 86.013(15) . . ?
Br5 Pb1 Br2 88.401(14) . 2_666 ?
Pb3 Br8 Pb2 77.506(11) . . ?
Pb3 Br6 Pb2 77.259(11) . . ?
Pb1 Br2 Pb1 97.277(14) . 2_666 ?
Pb1 Br4 Pb2 83.798(13) . . ?
Pb2 Br5 Pb1 83.619(14) . . ?
Pb2 Br7 Pb3 79.884(13) . . ?
C68 O2 H2A 109.5 . . ?
H3B O3 H3C 104.5 . . ?
C50 N3 H3 107.5 . . ?
C50 N3 C49 109.2(4) . . ?
C50 N3 C48 112.4(3) . . ?
C49 N3 H3 107.5 . . ?
C49 N3 C48 112.6(3) . . ?
C48 N3 H3 107.5 . . ?
C33 N2 H2 108.0 . . ?
C33 N2 C31 111.4(4) . . ?
C33 N2 C32 109.4(4) . . ?
C31 N2 H2 108.0 . . ?
C32 N2 H2 108.0 . . ?
C32 N2 C31 112.1(4) . . ?
C16 N1 H1 107.9 . . ?
C16 N1 C15 109.7(3) . . ?
C15 N1 H1 107.9 . . ?
C17 N1 H1 107.9 . . ?
C17 N1 C16 110.0(4) . . ?
C17 N1 C15 113.2(3) . . ?
C59 O1 H1A 109.5 . . ?
N2 C33 H33A 109.5 . . ?
N2 C33 H33B 109.5 . . ?
N2 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N3 C50 H50A 109.5 . . ?
N3 C50 H50B 109.5 . . ?
N3 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C31 H31A 109.2 . . ?
N2 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C25 C31 N2 111.9(4) . . ?
C25 C31 H31A 109.2 . . ?
C25 C31 H31B 109.2 . . ?
C26 C27 H27 118.7 . . ?
C28 C27 H27 118.7 . . ?
C28 C27 C26 122.7(5) . . ?
C27 C26 C01A 117.7(4) . . ?
C25 C26 C27 122.9(4) . . ?
C25 C26 C01A 119.5(4) . . ?
N1 C15 H15A 108.8 . . ?
N1 C15 H15B 108.8 . . ?
N1 C15 C8 113.6(4) . . ?
H15A C15 H15B 107.7 . . ?
C8 C15 H15A 108.8 . . ?
C8 C15 H15B 108.8 . . ?
N3 C49 H49A 109.5 . . ?
N3 C49 H49B 109.5 . . ?
N3 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C25 C24 C23 122.7(4) . . ?
C25 C24 C19 120.3(4) . . ?
C23 C24 C19 117.0(4) . . ?
C38 C39 H39 119.3 . . ?
C38 C39 C40 121.5(5) . . ?
C40 C39 H39 119.3 . . ?
C26 C25 C31 118.2(4) . . ?
C24 C25 C31 121.5(4) . . ?
C24 C25 C26 120.2(4) . . ?
N3 C48 H48A 109.0 . . ?
N3 C48 H48B 109.0 . . ?
H48A C48 H48B 107.8 . . ?
C41 C48 N3 112.7(4) . . ?
C41 C48 H48A 109.0 . . ?
C41 C48 H48B 109.0 . . ?
N2 C32 H32A 109.5 . . ?
N2 C32 H32B 109.5 . . ?
N2 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C27 C28 H28 120.2 . . ?
C27 C28 C29 119.5(5) . . ?
C29 C28 H28 120.2 . . ?
C9 C10 H10 118.5 . . ?
C11 C10 H10 118.5 . . ?
C11 C10 C9 123.1(5) . . ?
C6 C7 C2 117.0(4) . . ?
C8 C7 C6 122.6(4) . . ?
C8 C7 C2 120.3(4) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 C24 121.5(5) . . ?
C22 C23 H23 119.3 . . ?
C7 C6 H6 119.2 . . ?
C5 C6 C7 121.7(4) . . ?
C5 C6 H6 119.2 . . ?
C40 C41 C48 119.0(4) . . ?
C40 C41 C42 120.4(4) . . ?
C42 C41 C48 120.6(4) . . ?
C39 C38 H38 119.5 . . ?
C39 C38 C37 121.0(5) . . ?
C37 C38 H38 119.5 . . ?
C10 C9 C14 116.0(4) . . ?
C8 C9 C10 124.3(4) . . ?
C8 C9 C14 119.8(4) . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.0(5) . . ?
C12 C11 H11 120.0 . . ?
C6 C5 H5 119.5 . . ?
C6 C5 C4 121.0(5) . . ?
C4 C5 H5 119.5 . . ?
C21 C20 H20 119.3 . . ?
C21 C20 C19 121.4(5) . . ?
C19 C20 H20 119.3 . . ?
C30 C01A C26 118.2(4) . . ?
C18 C01A C26 118.9(4) . . ?
C18 C01A C30 122.9(4) . . ?
O2 C68 H68A 109.0 . . ?
O2 C68 H68B 109.0 . . ?
O2 C68 C67 113.0(4) . . ?
H68A C68 H68B 107.8 . . ?
C67 C68 H68A 109.0 . . ?
C67 C68 H68B 109.0 . . ?
C39 C40 C35 117.0(4) . . ?
C41 C40 C39 122.6(4) . . ?
C41 C40 C35 120.4(4) . . ?
C43 C44 H44 119.9 . . ?
C43 C44 C45 120.3(5) . . ?
C45 C44 H44 119.9 . . ?
C68 C67 H67A 109.4 . . ?
C68 C67 H67B 109.4 . . ?
C68 C67 C66 111.2(4) . . ?
H67A C67 H67B 108.0 . . ?
C66 C67 H67A 109.4 . . ?
C66 C67 H67B 109.4 . . ?
C20 C21 H21 120.2 . . ?
C20 C21 C22 119.6(5) . . ?
C22 C21 H21 120.2 . . ?
C2 C3 H3A 119.3 . . ?
C4 C3 H3A 119.3 . . ?
C4 C3 C2 121.4(5) . . ?
C23 C22 C21 121.1(5) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C20 C19 C24 119.4(4) . . ?
C18 C19 C24 118.4(4) . . ?
C18 C19 C20 122.2(4) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 C28 120.5(5) . . ?
C30 C29 H29 119.7 . . ?
C44 C43 H43 119.1 . . ?
C44 C43 C42 121.8(5) . . ?
C42 C43 H43 119.1 . . ?
C3 C2 C7 118.9(4) . . ?
C1 C2 C7 117.4(4) . . ?
C1 C2 C3 123.6(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 C5 119.9(5) . . ?
C3 C4 H4 120.0 . . ?
C7 C8 C15 119.7(4) . . ?
C9 C8 C15 119.5(4) . . ?
C9 C8 C7 120.7(4) . . ?
C13 C14 C9 118.7(4) . . ?
C1 C14 C9 117.5(4) . . ?
C1 C14 C13 123.8(4) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 C11 119.9(5) . . ?
C13 C12 H12 120.0 . . ?
C01A C30 H30 119.3 . . ?
C29 C30 C01A 121.4(5) . . ?
C29 C30 H30 119.3 . . ?
C38 C37 H37 119.9 . . ?
C36 C37 C38 120.2(5) . . ?
C36 C37 H37 119.9 . . ?
C14 C13 H13 118.9 . . ?
C12 C13 C14 122.2(5) . . ?
C12 C13 H13 118.9 . . ?
H61A C61 H61B 108.0 . . ?
C60 C61 H61A 109.3 . . ?
C60 C61 H61B 109.3 . . ?
C60 C61 C62 111.6(5) . . ?
C62 C61 H61A 109.3 . . ?
C62 C61 H61B 109.3 . . ?
C37 C36 H36 119.6 . . ?
C37 C36 C35 120.9(5) . . ?
C35 C36 H36 119.6 . . ?
C44 C45 H45 119.9 . . ?
C46 C45 C44 120.3(5) . . ?
C46 C45 H45 119.9 . . ?
C46 C47 C42 118.0(4) . . ?
C34 C47 C46 123.5(4) . . ?
C34 C47 C42 118.5(4) . . ?
C36 C35 C40 119.4(4) . . ?
C34 C35 C40 117.7(4) . . ?
C34 C35 C36 122.9(4) . . ?
C61 C60 H60A 109.5 . . ?
C61 C60 H60B 109.5 . . ?
C61 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C45 C46 C47 121.8(5) . . ?
C45 C46 H46 119.1 . . ?
C47 C46 H46 119.1 . . ?
C61 C62 H62A 108.7 . . ?
C61 C62 H62B 108.7 . . ?
C61 C62 C63 114.2(5) . . ?
H62A C62 H62B 107.6 . . ?
C63 C62 H62A 108.7 . . ?
C63 C62 H62B 108.7 . . ?
C01A C18 Cl2 118.5(4) . . ?
C01A C18 C19 122.8(4) . . ?
C19 C18 Cl2 118.7(4) . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C52 C51 H51A 109.5 . . ?
C52 C51 H51B 109.5 . . ?
C52 C51 H51C 109.5 . . ?
C41 C42 C47 119.2(4) . . ?
C43 C42 C41 123.0(4) . . ?
C43 C42 C47 117.8(4) . . ?
C62 C63 H63A 108.9 . . ?
C62 C63 H63B 108.9 . . ?
C62 C63 C64 113.2(4) . . ?
H63A C63 H63B 107.7 . . ?
C64 C63 H63A 108.9 . . ?
C64 C63 H63B 108.9 . . ?
C2 C1 Cl1 118.1(4) . . ?
C2 C1 C14 124.1(4) . . ?
C14 C1 Cl1 117.8(4) . . ?
C67 C66 H66A 108.7 . . ?
C67 C66 H66B 108.7 . . ?
H66A C66 H66B 107.6 . . ?
C65 C66 C67 114.3(4) . . ?
C65 C66 H66A 108.7 . . ?
C65 C66 H66B 108.7 . . ?
C47 C34 Cl3 118.2(4) . . ?
C47 C34 C35 123.8(4) . . ?
C35 C34 Cl3 117.9(4) . . ?
C66 C65 H65A 109.0 . . ?
C66 C65 H65B 109.0 . . ?
H65A C65 H65B 107.8 . . ?
C64 C65 C66 112.9(4) . . ?
C64 C65 H65A 109.0 . . ?
C64 C65 H65B 109.0 . . ?
C63 C64 H64A 108.8 . . ?
C63 C64 H64B 108.8 . . ?
C65 C64 C63 113.8(4) . . ?
C65 C64 H64A 108.8 . . ?
C65 C64 H64B 108.8 . . ?
H64A C64 H64B 107.7 . . ?
O1 C59 H59A 107.4 . . ?
O1 C59 H59B 107.4 . . ?
O1 C59 C58 119.9(6) . . ?
H59A C59 H59B 106.9 . . ?
C58 C59 H59A 107.4 . . ?
C58 C59 H59B 107.4 . . ?
C51 C52 H52A 108.3 . . ?
C51 C52 H52B 108.3 . . ?
C51 C52 C53 116.0(6) . . ?
H52A C52 H52B 107.4 . . ?
C53 C52 H52A 108.3 . . ?
C53 C52 H52B 108.3 . . ?
C52 C53 H53A 108.0 . . ?
C52 C53 H53B 108.0 . . ?
H53A C53 H53B 107.3 . . ?
C54 C53 C52 117.1(7) . . ?
C54 C53 H53A 108.0 . . ?
C54 C53 H53B 108.0 . . ?
C53 C54 H54A 108.1 . . ?
C53 C54 H54B 108.1 . . ?
C53 C54 C55 116.7(6) . . ?
H54A C54 H54B 107.3 . . ?
C55 C54 H54A 108.1 . . ?
C55 C54 H54B 108.1 . . ?
C59 C58 H58A 108.9 . . ?
C59 C58 H58B 108.9 . . ?
C59 C58 C57 113.3(6) . . ?
H58A C58 H58B 107.7 . . ?
C57 C58 H58A 108.9 . . ?
C57 C58 H58B 108.9 . . ?
C58 C57 H57A 107.7 . . ?
C58 C57 H57B 107.7 . . ?
C58 C57 C56 118.6(7) . . ?
H57A C57 H57B 107.1 . . ?
C56 C57 H57A 107.7 . . ?
C56 C57 H57B 107.7 . . ?
C54 C55 H55A 107.9 . . ?
C54 C55 H55B 107.9 . . ?
H55A C55 H55B 107.2 . . ?
C56 C55 C54 117.8(7) . . ?
C56 C55 H55A 107.9 . . ?
C56 C55 H55B 107.9 . . ?
C57 C56 H56A 108.2 . . ?
C57 C56 H56B 108.2 . . ?
C55 C56 C57 116.2(7) . . ?
C55 C56 H56A 108.2 . . ?
C55 C56 H56B 108.2 . . ?
H56A C56 H56B 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
O2 C68 C67 C66 168.5(4) . . . . ?
N3 C48 C41 C40 82.8(5) . . . . ?
N3 C48 C41 C42 -97.2(5) . . . . ?
N2 C31 C25 C26 -84.8(5) . . . . ?
N2 C31 C25 C24 99.3(5) . . . . ?
N1 C15 C8 C7 -80.2(5) . . . . ?
N1 C15 C8 C9 101.8(5) . . . . ?
O1 C59 C58 C57 -167.9(6) . . . . ?
C33 N2 C31 C25 154.4(4) . . . . ?
C50 N3 C48 C41 -159.6(4) . . . . ?
C16 N1 C15 C8 -174.0(4) . . . . ?
C27 C26 C25 C31 3.3(6) . . . . ?
C27 C26 C25 C24 179.3(4) . . . . ?
C27 C26 C01A C30 -1.9(6) . . . . ?
C27 C26 C01A C18 179.3(4) . . . . ?
C27 C28 C29 C30 0.1(7) . . . . ?
C26 C27 C28 C29 -2.1(7) . . . . ?
C26 C01A C30 C29 0.1(7) . . . . ?
C26 C01A C18 Cl2 -179.5(3) . . . . ?
C26 C01A C18 C19 1.3(7) . . . . ?
C49 N3 C48 C41 76.5(5) . . . . ?
C17 N1 C15 C8 -50.7(5) . . . . ?
C24 C23 C22 C21 -1.4(7) . . . . ?
C24 C19 C18 Cl2 -179.4(3) . . . . ?
C24 C19 C18 C01A -0.2(7) . . . . ?
C39 C38 C37 C36 -0.1(7) . . . . ?
C39 C40 C35 C36 0.2(6) . . . . ?
C39 C40 C35 C34 179.9(4) . . . . ?
C25 C26 C01A C30 177.8(4) . . . . ?
C25 C26 C01A C18 -1.0(6) . . . . ?
C25 C24 C23 C22 -178.2(5) . . . . ?
C25 C24 C19 C20 178.5(4) . . . . ?
C25 C24 C19 C18 -1.2(6) . . . . ?
C48 C41 C40 C39 1.2(6) . . . . ?
C48 C41 C40 C35 -179.2(4) . . . . ?
C48 C41 C42 C43 -2.0(7) . . . . ?
C48 C41 C42 C47 179.1(4) . . . . ?
C32 N2 C31 C25 -82.7(5) . . . . ?
C28 C27 C26 C25 -176.7(4) . . . . ?
C28 C27 C26 C01A 3.0(7) . . . . ?
C28 C29 C30 C01A 0.9(7) . . . . ?
C10 C9 C8 C15 -3.3(7) . . . . ?
C10 C9 C8 C7 178.6(4) . . . . ?
C10 C9 C14 C13 1.5(6) . . . . ?
C10 C9 C14 C1 -178.8(4) . . . . ?
C10 C11 C12 C13 1.8(8) . . . . ?
C7 C6 C5 C4 0.2(7) . . . . ?
C7 C2 C1 Cl1 175.9(3) . . . . ?
C7 C2 C1 C14 -4.5(7) . . . . ?
C23 C24 C25 C31 -2.2(7) . . . . ?
C23 C24 C25 C26 -178.1(4) . . . . ?
C23 C24 C19 C20 -2.0(6) . . . . ?
C23 C24 C19 C18 178.4(4) . . . . ?
C6 C7 C2 C3 1.7(6) . . . . ?
C6 C7 C2 C1 -177.1(4) . . . . ?
C6 C7 C8 C15 2.4(7) . . . . ?
C6 C7 C8 C9 -179.6(4) . . . . ?
C6 C5 C4 C3 1.0(7) . . . . ?
C41 C40 C35 C36 -179.4(4) . . . . ?
C41 C40 C35 C34 0.3(6) . . . . ?
C38 C39 C40 C41 179.2(4) . . . . ?
C38 C39 C40 C35 -0.4(6) . . . . ?
C38 C37 C36 C35 -0.2(7) . . . . ?
C9 C10 C11 C12 -1.5(8) . . . . ?
C9 C14 C13 C12 -1.3(7) . . . . ?
C9 C14 C1 Cl1 -178.9(3) . . . . ?
C9 C14 C1 C2 1.4(7) . . . . ?
C11 C10 C9 C8 178.9(5) . . . . ?
C11 C10 C9 C14 -0.2(7) . . . . ?
C11 C12 C13 C14 -0.4(8) . . . . ?
C20 C21 C22 C23 0.2(7) . . . . ?
C20 C19 C18 Cl2 0.9(6) . . . . ?
C20 C19 C18 C01A -179.9(4) . . . . ?
C01A C26 C25 C31 -176.3(4) . . . . ?
C01A C26 C25 C24 -0.3(6) . . . . ?
C68 C67 C66 C65 174.2(4) . . . . ?
C40 C39 C38 C37 0.3(7) . . . . ?
C40 C41 C42 C43 178.0(4) . . . . ?
C40 C41 C42 C47 -0.9(6) . . . . ?
C40 C35 C34 Cl3 178.8(3) . . . . ?
C40 C35 C34 C47 -1.4(7) . . . . ?
C44 C43 C42 C41 179.8(4) . . . . ?
C44 C43 C42 C47 -1.3(7) . . . . ?
C44 C45 C46 C47 -0.6(8) . . . . ?
C67 C66 C65 C64 178.5(4) . . . . ?
C21 C20 C19 C24 0.9(7) . . . . ?
C21 C20 C19 C18 -179.5(5) . . . . ?
C3 C2 C1 Cl1 -2.8(6) . . . . ?
C3 C2 C1 C14 176.8(5) . . . . ?
C19 C24 C25 C31 177.3(4) . . . . ?
C19 C24 C25 C26 1.4(6) . . . . ?
C19 C24 C23 C22 2.3(7) . . . . ?
C19 C20 C21 C22 0.0(7) . . . . ?
C43 C44 C45 C46 0.8(8) . . . . ?
C2 C7 C6 C5 -1.5(6) . . . . ?
C2 C7 C8 C15 -178.9(4) . . . . ?
C2 C7 C8 C9 -0.8(7) . . . . ?
C2 C3 C4 C5 -0.8(7) . . . . ?
C4 C3 C2 C7 -0.6(7) . . . . ?
C4 C3 C2 C1 178.1(5) . . . . ?
C8 C7 C6 C5 177.2(4) . . . . ?
C8 C7 C2 C3 -177.1(4) . . . . ?
C8 C7 C2 C1 4.1(6) . . . . ?
C8 C9 C14 C13 -177.6(4) . . . . ?
C8 C9 C14 C1 2.1(6) . . . . ?
C14 C9 C8 C15 175.7(4) . . . . ?
C14 C9 C8 C7 -2.4(7) . . . . ?
C30 C01A C18 Cl2 1.8(6) . . . . ?
C30 C01A C18 C19 -177.4(4) . . . . ?
C37 C36 C35 C40 0.1(7) . . . . ?
C37 C36 C35 C34 -179.6(5) . . . . ?
C13 C14 C1 Cl1 0.7(6) . . . . ?
C13 C14 C1 C2 -178.9(4) . . . . ?
C61 C62 C63 C64 -164.7(5) . . . . ?
C36 C35 C34 Cl3 -1.5(6) . . . . ?
C36 C35 C34 C47 178.3(5) . . . . ?
C45 C44 C43 C42 0.2(7) . . . . ?
C60 C61 C62 C63 176.2(5) . . . . ?
C46 C47 C42 C41 -179.6(4) . . . . ?
C46 C47 C42 C43 1.4(6) . . . . ?
C46 C47 C34 Cl3 0.6(6) . . . . ?
C46 C47 C34 C35 -179.2(5) . . . . ?
C62 C63 C64 C65 175.7(4) . . . . ?
C18 C01A C30 C29 178.8(5) . . . . ?
C51 C52 C53 C54 -178.8(6) . . . . ?
C42 C41 C40 C39 -178.8(4) . . . . ?
C42 C41 C40 C35 0.8(6) . . . . ?
C42 C47 C46 C45 -0.5(7) . . . . ?
C42 C47 C34 Cl3 -178.9(3) . . . . ?
C42 C47 C34 C35 1.3(7) . . . . ?
C1 C14 C13 C12 179.0(5) . . . . ?
C66 C65 C64 C63 178.0(4) . . . . ?
C34 C47 C46 C45 -180.0(5) . . . . ?
C34 C47 C42 C41 -0.1(6) . . . . ?
C34 C47 C42 C43 -179.1(4) . . . . ?
C59 C58 C57 C56 -168.1(6) . . . . ?
C52 C53 C54 C55 170.1(6) . . . . ?
C53 C54 C55 C56 -177.4(6) . . . . ?
C54 C55 C56 C57 -179.5(6) . . . . ?
C58 C57 C56 C55 179.7(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.946
_oxdiff_exptl_absorpt_empirical_full_min 0.770
