# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_03-2
_database_code_depnum_ccdc_archive 'CCDC 2011534'
loop_
_audit_author_name
_audit_author_address
Duan
;Nanjingxiaozhuang university
China
;
_audit_update_record             
;
2020-06-23 deposited with the CCDC.	2020-10-29 downloaded from the CCDC.
;
_audit_creation_date             2019-03-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Pb, C6 H16 N2'
_chemical_formula_sum            'C6 H16 Cl4 N2 Pb'
_chemical_formula_weight         465.20
_chemical_absolute_configuration ad
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   7.7465(6)
_cell_length_b                   13.5915(9)
_cell_length_c                   16.9107(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1780.5(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3210
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.9010
_cell_measurement_theta_min      2.8380
_shelx_estimated_absorpt_T_max   0.500
_shelx_estimated_absorpt_T_min   0.404
_exptl_absorpt_coefficient_mu    10.049
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5525
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.922
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00  68.00   1.00    2.67    --  -11.59  19.00 120.00  106
  2  ω     26.00  59.00   1.00    2.67    --   11.74  37.00-180.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0225631000
_diffrn_orient_matrix_UB_12      -0.0349095000
_diffrn_orient_matrix_UB_13      -0.0294116000
_diffrn_orient_matrix_UB_21      -0.0341916000
_diffrn_orient_matrix_UB_22      -0.0314779000
_diffrn_orient_matrix_UB_23      0.0295863000
_diffrn_orient_matrix_UB_31      -0.0818747000
_diffrn_orient_matrix_UB_32      0.0227482000
_diffrn_orient_matrix_UB_33      -0.0041695000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.642
_reflns_Friedel_fraction_full    0.884
_reflns_Friedel_fraction_max     0.884
_reflns_number_gt                2850
_reflns_number_total             2978
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.415
_refine_diff_density_min         -4.556
_refine_diff_density_rms         0.339
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.107(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2978
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0641
_refine_ls_restrained_S_all      1.100
_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)+(0.0279P)²+94.4011P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1477
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.893(16)
 0.107(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3. Rigid bond restraints
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.002 and sigma
for terminal atoms of 0.004
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
5.a Ternary CH refined with riding coordinates:
 C6(H6), C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B), C2(H2D,H2E)
5.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N1(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
Pb01 Pb 0.30688(7) 0.70277(3) 0.37667(3) 0.01153(10) Uani 1 1 d . . . . .
Cl1 Cl -0.0079(5) 0.6598(3) 0.3055(2) 0.0222(10) Uani 1 1 d . . . . .
Cl2 Cl 0.4723(5) 0.6530(3) 0.24474(19) 0.0164(9) Uani 1 1 d . . . . .
Cl3 Cl 0.3241(5) 0.5071(2) 0.4332(2) 0.0207(9) Uani 1 1 d . . . . .
Cl4 Cl 0.6429(5) 0.7361(3) 0.4569(2) 0.0268(11) Uani 1 1 d . . . . .
C6 C 0.8061(17) 0.4365(8) 0.3861(7) 0.0068(12) Uani 1 1 d . U . . .
H6 H 0.922522 0.434356 0.363485 0.008 Uiso 1 1 calc R . . . .
N2 N 0.7034(16) 0.5085(8) 0.3411(6) 0.0136(19) Uani 1 1 d . U . . .
H2A H 0.681586 0.484864 0.293061 0.016 Uiso 1 1 calc GR . . . .
H2B H 0.762301 0.564531 0.336872 0.016 Uiso 1 1 calc GR . . . .
H2C H 0.604372 0.519788 0.366186 0.016 Uiso 1 1 calc GR . . . .
C5 C 0.7214(17) 0.3366(9) 0.3732(9) 0.0163(12) Uani 1 1 d . U . . .
H5A H 0.600949 0.339819 0.388743 0.020 Uiso 1 1 calc R . . . .
H5B H 0.726254 0.319490 0.317564 0.020 Uiso 1 1 calc R . . . .
C3 C 0.821(2) 0.2833(11) 0.5096(8) 0.0220(13) Uani 1 1 d . U . . .
H3A H 0.706052 0.285297 0.531966 0.026 Uiso 1 1 calc R . . . .
H3B H 0.886908 0.233025 0.537069 0.026 Uiso 1 1 calc R . . . .
C1 C 0.8209(19) 0.4632(9) 0.4730(7) 0.0079(7) Uani 1 1 d . U . . .
H1 H 0.704310 0.472651 0.494193 0.009 Uiso 1 1 calc R . . . .
C4 C 0.812(2) 0.2593(11) 0.4209(9) 0.0250(13) Uani 1 1 d . U . . .
H4A H 0.928187 0.251261 0.400687 0.030 Uiso 1 1 calc R . . . .
H4B H 0.752055 0.197131 0.414113 0.030 Uiso 1 1 calc R . . . .
N1 N 0.9194(15) 0.5556(8) 0.4848(7) 0.0103(19) Uani 1 1 d . U . . .
H1A H 0.852727 0.606821 0.472934 0.012 Uiso 1 1 calc GR . . . .
H1B H 1.011792 0.555533 0.453497 0.012 Uiso 1 1 calc GR . . . .
H1C H 0.952911 0.559853 0.535024 0.012 Uiso 1 1 calc GR . . . .
C2 C 0.9074(17) 0.3815(9) 0.5192(8) 0.0083(7) Uani 1 1 d . U . . .
H2D H 1.026549 0.376086 0.502135 0.010 Uiso 1 1 calc R . . . .
H2E H 0.907820 0.398890 0.574849 0.010 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb01 Cl1 2.781(4) . ?
Pb01 Cl2 2.660(3) . ?
Pb01 Cl3 2.829(3) . ?
Pb01 Cl4 2.970(4) . ?
C6 H6 0.9800 . ?
C6 N2 1.473(16) . ?
C6 C5 1.523(17) . ?
C6 C1 1.519(17) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 1.50(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.54(2) . ?
C3 C2 1.50(2) . ?
C1 H1 0.9800 . ?
C1 N1 1.482(17) . ?
C1 C2 1.514(18) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C2 H2D 0.9700 . ?
C2 H2E 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
Cl1 Pb01 Cl3 89.44(11) . . ?
Cl1 Pb01 Cl4 176.44(11) . . ?
Cl2 Pb01 Cl1 90.36(12) . . ?
Cl2 Pb01 Cl3 91.25(11) . . ?
Cl2 Pb01 Cl4 89.98(11) . . ?
Cl3 Pb01 Cl4 87.01(11) . . ?
N2 C6 H6 108.4 . . ?
N2 C6 C5 106.6(10) . . ?
N2 C6 C1 112.4(10) . . ?
C5 C6 H6 108.4 . . ?
C1 C6 H6 108.4 . . ?
C1 C6 C5 112.6(11) . . ?
C6 N2 H2A 109.5 . . ?
C6 N2 H2B 109.5 . . ?
C6 N2 H2C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
C4 C5 C6 110.3(12) . . ?
C4 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.0 . . ?
C4 C3 H3B 110.0 . . ?
C2 C3 H3A 110.0 . . ?
C2 C3 H3B 110.0 . . ?
C2 C3 C4 108.4(12) . . ?
C6 C1 H1 108.4 . . ?
N1 C1 C6 111.8(10) . . ?
N1 C1 H1 108.4 . . ?
N1 C1 C2 108.9(11) . . ?
C2 C1 C6 110.9(10) . . ?
C2 C1 H1 108.4 . . ?
C5 C4 C3 113.5(13) . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C3 C2 C1 113.6(11) . . ?
C3 C2 H2D 108.8 . . ?
C3 C2 H2E 108.8 . . ?
C1 C2 H2D 108.8 . . ?
C1 C2 H2E 108.8 . . ?
H2D C2 H2E 107.7 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.577 0.186 0.250 291.5 91.7 ?
2 -0.608 0.069 0.750 291.5 102.3 ?


_olex2_date_sample_data_collection 2019-03-21
_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 2.107
_oxdiff_exptl_absorpt_empirical_full_min 0.701
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.893(16)
2 0.107(16)

####################################################################### 
# 
# 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_2-0613
_database_code_depnum_ccdc_archive 'CCDC 2011535'
loop_
_audit_author_name
_audit_author_address
Duan
;Nanjingxiaozhuang university
China
;
_audit_update_record             
;
2020-06-23 deposited with the CCDC.	2020-10-29 downloaded from the CCDC.
;
_audit_creation_date             2020-01-13
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H8 N)'
_chemical_formula_sum            'C6 H16 Br4 N2 Pb'
_chemical_formula_weight         643.04
_chemical_absolute_configuration ad
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.8000(5)
_cell_length_b                   11.7153(5)
_cell_length_c                   9.9520(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1375.77(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3634
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.2340
_cell_measurement_theta_min      2.6650
_shelx_estimated_absorpt_T_max   0.223
_shelx_estimated_absorpt_T_min   0.162
_exptl_absorpt_coefficient_mu    23.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.105
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7134
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.990
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_min         2.046
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  79.00   1.00    5.00    --   11.74  77.00 -30.00   93
  2  ω    -33.00  53.00   1.00    5.00    --  -11.59  57.00-150.00   86
  3  ω    -84.00 -34.00   1.00    5.00    --  -11.59 -57.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0021513000
_diffrn_orient_matrix_UB_12      -0.0030854000
_diffrn_orient_matrix_UB_13      0.0710631000
_diffrn_orient_matrix_UB_21      -0.0600546000
_diffrn_orient_matrix_UB_22      -0.0008846000
_diffrn_orient_matrix_UB_23      -0.0026206000
_diffrn_orient_matrix_UB_31      0.0010688000
_diffrn_orient_matrix_UB_32      -0.0605257000
_diffrn_orient_matrix_UB_33      -0.0036167000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.718
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2301
_reflns_number_total             2426
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.405
_refine_diff_density_min         -1.873
_refine_diff_density_rms         0.383
_refine_ls_abs_structure_details 
;
 Flack x determined using 836 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(14)
_refine_ls_extinction_coef       0.00203(7)
_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   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2426
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0420
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0436P)²+18.5097P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1079
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma
of 0.002 and sigma for terminal atoms of 0.004
3.a Ternary CH refined with riding coordinates:
 C3(H3), C4(H4)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5A,H5B), C1(H1D,H1E), C6(H6A,H6B)
3.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.74745(3) 0.27301(3) 0.50589(4) 0.00701(8) Uani 1 1 d . . . . .
Br3 Br 0.82058(8) 0.51838(7) 0.52313(10) 0.0092(2) Uani 1 1 d . . . . .
Br4 Br 0.74729(9) 0.29249(9) 0.80399(10) 0.0090(2) Uani 1 1 d . . . . .
Br1 Br 0.50448(8) 0.31955(7) 0.50464(10) 0.0131(2) Uani 1 1 d . . . . .
Br2 Br 0.74394(9) 0.28706(9) 0.20825(10) 0.0092(2) Uani 1 1 d . . . . .
C3 C 0.5374(8) 0.0523(8) 0.1108(11) 0.0055(12) Uani 1 1 d . U . . .
H3 H 0.616594 0.027174 0.114019 0.007 Uiso 1 1 calc R U . . .
N1 N 0.5155(9) 0.1270(7) 0.2307(9) 0.013(2) Uani 1 1 d . . . . .
H1A H 0.453912 0.169045 0.216089 0.015 Uiso 1 1 calc R U . . .
H1B H 0.574740 0.172596 0.244101 0.015 Uiso 1 1 calc R U . . .
H1C H 0.504835 0.083541 0.302980 0.015 Uiso 1 1 calc R U . . .
C2 C 0.5205(7) 0.1236(7) -0.0175(10) 0.0069(12) Uani 1 1 d . U . . .
H2A H 0.444498 0.155087 -0.017902 0.008 Uiso 1 1 calc R U . . .
H2B H 0.573638 0.186828 -0.017359 0.008 Uiso 1 1 calc R U . . .
C5 C 0.8834(8) 0.0456(8) -0.0132(11) 0.0091(12) Uani 1 1 d . U . . .
H5A H 0.832726 0.110862 -0.012761 0.011 Uiso 1 1 calc R U . . .
H5B H 0.837515 -0.023098 -0.012270 0.011 Uiso 1 1 calc R U . . .
C1 C 0.5382(9) 0.0524(9) -0.1452(11) 0.0101(12) Uani 1 1 d . U . . .
H1D H 0.521646 0.098786 -0.223498 0.012 Uiso 1 1 calc R U . . .
H1E H 0.616746 0.028446 -0.150615 0.012 Uiso 1 1 calc R U . . .
N2 N 0.8818(7) 0.0440(7) 0.2342(9) 0.0075(17) Uani 1 1 d . U . . .
H2C H 0.832440 0.101439 0.231041 0.009 Uiso 1 1 calc R U . . .
H2D H 0.923597 0.049873 0.308242 0.009 Uiso 1 1 calc R U . . .
H2E H 0.844418 -0.021983 0.235043 0.009 Uiso 1 1 calc R U . . .
C6 C 0.9565(9) 0.0479(9) -0.1415(11) 0.0110(12) Uani 1 1 d . U . . .
H6A H 0.907899 0.040375 -0.219611 0.013 Uiso 1 1 calc R U . . .
H6B H 0.995241 0.120780 -0.147620 0.013 Uiso 1 1 calc R U . . .
C4 C 0.9581(8) 0.0487(8) 0.1117(11) 0.0063(12) Uani 1 1 d . U . . .
H4 H 0.999993 0.120885 0.112893 0.008 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 Br3 3.1027(9) 3_646 ?
Pb1 Br3 3.0062(9) . ?
Pb1 Br4 2.9754(10) . ?
Pb1 Br1 3.2227(10) 4_556 ?
Pb1 Br1 2.9184(10) . ?
Pb1 Br2 2.9670(11) . ?
C3 C3 1.511(19) 2_655 ?
C3 H3 0.9800 . ?
C3 N1 1.502(13) . ?
C3 C2 1.539(14) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.534(14) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.542(15) . ?
C5 C4 1.525(14) . ?
C1 C1 1.52(2) 2_655 ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N2 C4 1.516(13) . ?
C6 C6 1.52(2) 2_755 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C4 C4 1.51(2) 2_755 ?
C4 H4 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
Br3 Pb1 Br3 177.356(14) . 3_646 ?
Br3 Pb1 Br1 93.06(3) . 4_556 ?
Br3 Pb1 Br1 85.24(2) 3_646 4_556 ?
Br4 Pb1 Br3 82.53(3) . . ?
Br4 Pb1 Br3 99.58(3) . 3_646 ?
Br4 Pb1 Br1 93.37(3) . 4_556 ?
Br1 Pb1 Br3 95.95(3) . . ?
Br1 Pb1 Br3 85.70(3) . 3_646 ?
Br1 Pb1 Br4 89.39(3) . . ?
Br1 Pb1 Br1 170.848(15) . 4_556 ?
Br1 Pb1 Br2 88.38(3) . . ?
Br2 Pb1 Br3 90.45(3) . . ?
Br2 Pb1 Br3 87.52(3) . 3_646 ?
Br2 Pb1 Br4 172.38(3) . . ?
Br2 Pb1 Br1 89.96(3) . 4_556 ?
Pb1 Br3 Pb1 147.12(3) . 3_656 ?
Pb1 Br1 Pb1 149.52(3) . 4_456 ?
C3 C3 H3 108.3 2_655 . ?
C3 C3 C2 111.4(6) 2_655 . ?
N1 C3 C3 111.8(7) . 2_655 ?
N1 C3 H3 108.3 . . ?
N1 C3 C2 108.7(7) . . ?
C2 C3 H3 108.3 . . ?
C3 N1 H1A 109.5 . . ?
C3 N1 H1B 109.5 . . ?
C3 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C3 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C1 C2 C3 112.0(7) . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H5A C5 H5B 108.1 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 C6 110.6(8) . . ?
C2 C1 H1D 109.4 . . ?
C2 C1 H1E 109.4 . . ?
C1 C1 C2 111.0(7) 2_655 . ?
C1 C1 H1D 109.4 2_655 . ?
C1 C1 H1E 109.4 2_655 . ?
H1D C1 H1E 108.0 . . ?
H2C N2 H2D 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
C4 N2 H2C 109.5 . . ?
C4 N2 H2D 109.5 . . ?
C4 N2 H2E 109.5 . . ?
C5 C6 H6A 109.4 . . ?
C5 C6 H6B 109.3 . . ?
C6 C6 C5 111.4(7) 2_755 . ?
C6 C6 H6A 109.4 2_755 . ?
C6 C6 H6B 109.3 2_755 . ?
H6A C6 H6B 108.0 . . ?
C5 C4 H4 108.8 . . ?
N2 C4 C5 108.1(8) . . ?
N2 C4 C4 111.2(7) . 2_755 ?
N2 C4 H4 108.8 . . ?
C4 C4 C5 111.2(7) 2_755 . ?
C4 C4 H4 108.8 2_755 . ?

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
C3 C3 C2 C1 -54.7(12) 2_655 . . . ?
C3 C2 C1 C1 55.1(12) . . . 2_655 ?
N1 C3 C2 C1 -178.4(8) . . . . ?
C6 C5 C4 N2 -179.0(8) . . . . ?
C6 C5 C4 C4 -56.6(11) . . . 2_755 ?
C4 C5 C6 C6 54.9(12) . . . 2_755 ?

_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 2.776
_oxdiff_exptl_absorpt_empirical_full_min 0.511
