# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

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

data_x1
_database_code_depnum_ccdc_archive 'CCDC 2157694'
loop_
_audit_author_name
_audit_author_address
'Yi Liu'
;Fujian Institute of Research on the Structure of Matter
China
;
_audit_update_record             
;
2022-03-10 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2021-10-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(Br14 Pb4), 2(C4 H12 N), C H5 N2'
_chemical_formula_sum            'C9 H29 Br7 N4 Pb2'
_chemical_formula_weight         1167.11
_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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   8.3299(4)
_cell_length_b                   37.549(3)
_cell_length_c                   8.4639(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2647.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5443
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.423
_cell_measurement_theta_min      2.905
_shelx_estimated_absorpt_T_max   0.389
_shelx_estimated_absorpt_T_min   0.204
_exptl_absorpt_coefficient_mu    23.269
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1415 before and 0.0761 after correction. The Ratio of minimum to maximum transmission is 0.3914. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.928
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21033
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.467
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'Bruker APEX3 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX3 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2289
_reflns_number_total             3070
_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 V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XS (Sheldrick, 2008)'
_refine_diff_density_max         2.056
_refine_diff_density_min         -1.763
_refine_diff_density_rms         0.311
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         3070
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0554
_refine_ls_restrained_S_all      1.084
_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)+(0.0697P)²+39.4185P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1605
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 3(10)
 -2(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-C1 = N2-C1
 1.35 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim N2: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
N3 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
5.a Riding coordinates:
 N3(H3A,H3B,H3C), N1(H1A,H1B), N2(H2C,H2D)
5.b Ternary CH refined with riding coordinates:
 C3(H3)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
5.d Aromatic/amide H refined with riding coordinates:
 C1(H1)
5.e Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   mixed
_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 -0.25462(4) 0.16827(2) -0.50419(4) 0.02544(18) Uani 1 1 d . . . . .
Br1 Br -0.2463(2) 0.250000 -0.5083(2) 0.0403(5) Uani 1 2 d S T P . .
Br2 Br -0.46195(16) 0.16788(4) -0.79589(15) 0.0430(4) Uani 1 1 d . . . . .
Br3 Br -0.54783(14) 0.17312(4) -0.28904(14) 0.0362(3) Uani 1 1 d . . . . .
Br4 Br -0.22664(15) 0.09150(4) -0.45981(16) 0.0380(3) Uani 1 1 d . . . . .
N3 N -0.8208(12) 0.1096(3) -0.4233(11) 0.036(2) Uani 1 1 d . U . . .
H3A H -0.785068 0.103517 -0.324870 0.043 Uiso 1 1 d R . . . .
H3B H -0.920238 0.100357 -0.438590 0.043 Uiso 1 1 d R . . . .
H3C H -0.824688 0.133727 -0.431390 0.043 Uiso 1 1 d R . . . .
C2 C -0.7181(18) 0.0904(4) -0.5427(17) 0.045(3) Uani 1 1 d . U . . .
H2A H -0.770840 0.092148 -0.647268 0.055 Uiso 1 1 calc R . . . .
H2B H -0.613674 0.102887 -0.550435 0.055 Uiso 1 1 calc R . . . .
C3 C -0.688(2) 0.0533(5) -0.5095(18) 0.060(3) Uani 1 1 d . U . . .
H3 H -0.616223 0.053038 -0.414543 0.072 Uiso 1 1 calc R . . . .
C4 C -0.823(3) 0.0309(5) -0.469(3) 0.082(5) Uani 1 1 d . U . . .
H4A H -0.916829 0.038296 -0.530670 0.123 Uiso 1 1 calc GR . . . .
H4B H -0.846204 0.033221 -0.356279 0.123 Uiso 1 1 calc GR . . . .
H4C H -0.797006 0.006044 -0.493643 0.123 Uiso 1 1 calc GR . . . .
C5 C -0.590(2) 0.0366(5) -0.6412(18) 0.074(5) Uani 1 1 d . U . . .
H5A H -0.661887 0.029942 -0.728221 0.111 Uiso 1 1 calc GR . . . .
H5B H -0.535606 0.015310 -0.601370 0.111 Uiso 1 1 calc GR . . . .
H5C H -0.510529 0.053752 -0.679198 0.111 Uiso 1 1 calc GR . . . .
N1 N -0.338(3) 0.250000 -0.105(2) 0.067(5) Uani 1 2 d DS TU P . .
H1A H -0.238610 0.250000 -0.140172 0.080 Uiso 1 2 d RS T P . .
H1B H -0.418650 0.250000 -0.172312 0.080 Uiso 1 2 d RS T P . .
N2 N -0.150(2) 0.250000 0.093(2) 0.077(6) Uani 1 2 d DS TU P . .
H2C H -0.069396 0.250000 0.025226 0.092 Uiso 1 2 d RS T P . .
H2D H -0.131026 0.250000 0.194796 0.092 Uiso 1 2 d RS T P . .
C1 C -0.296(3) 0.250000 0.044(3) 0.084(6) Uani 1 2 d DS TU P . .
H1 H -0.378834 0.250000 0.121407 0.101 Uiso 1 2 calc RS T P . .


_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 Br1 3.0698(5) . ?
Pb1 Br2 2.9676(12) 6_654 ?
Pb1 Br2 3.0131(12) . ?
Pb1 Br3 3.0265(12) 6_655 ?
Pb1 Br3 3.0520(12) . ?
Pb1 Br4 2.9162(16) . ?
N3 H3A 0.9136 . ?
N3 H3B 0.9081 . ?
N3 H3C 0.9081 . ?
N3 C2 1.508(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.44(2) . ?
C3 H3 1.0000 . ?
C3 C4 1.44(3) . ?
C3 C5 1.51(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
N1 H1A 0.8787 . ?
N1 H1B 0.8844 . ?
N1 C1 1.308(17) . ?
N2 H2C 0.8802 . ?
N2 H2D 0.8780 . ?
N2 C1 1.285(17) . ?
C1 H1 0.9500 . ?

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 Br1 88.85(4) 6_654 . ?
Br2 Pb1 Br1 90.48(4) . . ?
Br2 Pb1 Br2 90.207(13) 6_654 . ?
Br2 Pb1 Br3 176.31(4) 6_654 . ?
Br2 Pb1 Br3 90.02(3) 6_654 6_655 ?
Br2 Pb1 Br3 91.75(3) . . ?
Br2 Pb1 Br3 176.82(4) . 6_655 ?
Br3 Pb1 Br1 88.00(4) . . ?
Br3 Pb1 Br1 86.35(4) 6_655 . ?
Br3 Pb1 Br3 87.857(13) 6_655 . ?
Br4 Pb1 Br1 171.04(4) . . ?
Br4 Pb1 Br2 90.16(4) . 6_654 ?
Br4 Pb1 Br2 98.43(4) . . ?
Br4 Pb1 Br3 92.64(4) . . ?
Br4 Pb1 Br3 84.74(4) . 6_655 ?
Pb1 Br1 Pb1 177.11(6) 8_565 . ?
Pb1 Br2 Pb1 159.73(5) 6_554 . ?
Pb1 Br3 Pb1 160.25(5) 6 . ?
H3A N3 H3B 109.3 . . ?
H3A N3 H3C 109.3 . . ?
H3B N3 H3C 109.8 . . ?
C2 N3 H3A 107.8 . . ?
C2 N3 H3B 103.8 . . ?
C2 N3 H3C 116.5 . . ?
N3 C2 H2A 108.4 . . ?
N3 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
C3 C2 N3 115.5(12) . . ?
C3 C2 H2A 108.4 . . ?
C3 C2 H2B 108.4 . . ?
C2 C3 H3 105.6 . . ?
C2 C3 C5 110.5(15) . . ?
C4 C3 C2 118.0(18) . . ?
C4 C3 H3 105.6 . . ?
C4 C3 C5 110.5(16) . . ?
C5 C3 H3 105.6 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
H1A N1 H1B 119.6 . . ?
C1 N1 H1A 94.6 . . ?
C1 N1 H1B 145.8 . . ?
H2C N2 H2D 120.2 . . ?
C1 N2 H2C 120.9 . . ?
C1 N2 H2D 118.9 . . ?
N1 C1 H1 118.0 . . ?
N2 C1 N1 124(3) . . ?
N2 C1 H1 118.0 . . ?

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
N3 C2 C3 C4 49(2) . . . . ?
N3 C2 C3 C5 177.4(13) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 3(10)
2 -2(10)

####################################################################### 
# 
# 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_mo_lyy370831310k_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2157696'
loop_
_audit_author_name
_audit_author_address
'Yi Liu'
;Fujian Institute of Research on the Structure of Matter
China
;
_audit_update_record             
;
2022-03-10 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2021-09-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(Br3.5 Pb), C8 H24 N2, C H5 N2'
_chemical_formula_sum            'C9 H29 Br7 N4 Pb2'
_chemical_formula_weight         1167.11
_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      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'y, -x, z'
'x, -y, -z'
'-x, y, -z'
'-x, -y, z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'y, -x, -z'
'-y, x, -z'
'-x, y, z'
'x, -y, z'
'x, y, -z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   5.9841(2)
_cell_length_b                   5.9841(2)
_cell_length_c                   38.4072(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1375.34(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1702
_cell_measurement_temperature    310(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   0.326
_shelx_estimated_absorpt_T_min   0.123
_exptl_absorpt_coefficient_mu    22.394
_exptl_absorpt_correction_T_max  0.0206
_exptl_absorpt_correction_T_min  0.0026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1762 before and 0.0751 after correction. The Ratio of minimum to maximum transmission is 0.1262. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.818
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            5626
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.468
_diffrn_reflns_theta_min         3.182
_diffrn_ambient_temperature      309.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                448
_reflns_number_total             538
_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 V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.023
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         538
_refine_ls_number_restraints     98
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0386
_refine_ls_restrained_S_all      0.989
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0638P)²+5.0867P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1119
_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) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C0AA = C0AA-C1AA
 1.5 with sigma of 0.02
 C1AA-C4
 1.5 with sigma of 0.02
 C3-C1AA
 1.5 with sigma of 0.02
 N3-C5
 1.3 with sigma of 0.02
 N2-C5
 1.3 with sigma of 0.02
 C1AA-N1
 2.5 with sigma of 0.04
 C4-C0AA
 2.5 with sigma of 0.04
 C4-C3
 2.5 with sigma of 0.04
 C3-C0AA
 2.5 with sigma of 0.04
 N2-N3
 2.3 with sigma of 0.04
3. Rigid bond restraints
 C4, C3, C1AA, C0AA, N1, C5, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C4 \\sim C1AA \\sim C3 \\sim C0AA \\sim N1 \\sim N3 \\sim C5: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
N2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C5) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.2
Uanis(N1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.2
Uanis(N2) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: N1(0.125) H1A(0.125) H1B(0.125) H1C(0.125) C1AA(0.125) H1AA(0.125)
 C0AA(0.125) H0AA(0.125) H0AB(0.125) C4(0.125) H4A(0.125) H4B(0.125) H4C(0.125)
 C3(0.125) H3A(0.125) H3B(0.125) H3C(0.125) C5(0.0625) H5(0.0625) N3(0.0625)
 H3D(0.0625) H3E(0.0625) N2(0.0625) H2A(0.0625) H2B(0.0625)
6.a Ternary CH refined with riding coordinates:
 C1AA(H1AA)
6.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5)
6.d X=CH2 refined with riding coordinates:
 N3(H3D,H3E), N2(H2A,H2B)
6.e Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb -0.500000 -0.500000 0.41896(2) 0.06948(9) Uani 1 8 d S T P . .
Br3 Br -0.500000 -0.500000 0.500000 0.1114(5) Uani 1 16 d S T P . .
Br1 Br 0.000000 -0.500000 0.41911(3) 0.1370(4) Uani 1 4 d S T P . .
Br2 Br -0.500000 -0.500000 0.34553(4) 0.2067(10) Uani 1 8 d S T P . .
N1 N -0.0827(14) 0.000(3) 0.3650(2) 0.128(3) Uani 0.125 1 d DS TU P A -1
H1A H -0.208479 0.042927 0.354645 0.153 Uiso 0.125 1 calc GR . . A -1
H1B H -0.051319 0.093465 0.382400 0.153 Uiso 0.125 1 calc GR . . A -1
H1C H -0.099594 -0.137525 0.373450 0.153 Uiso 0.125 1 calc GR . . A -1
C1AA C 0.034(2) -0.0076(15) 0.30173(17) 0.156(2) Uani 0.125 1 d D U . A -1
H1AA H -0.105708 0.077691 0.300497 0.187 Uiso 0.125 1 calc R . . A -1
C0AA C 0.1049(16) 0.002(5) 0.33917(17) 0.148(2) Uani 0.125 1 d D U . A -1
H0AA H 0.201767 -0.124251 0.343877 0.177 Uiso 0.125 1 calc R . . A -1
H0AB H 0.192041 0.136928 0.342679 0.177 Uiso 0.125 1 calc R . . A -1
C4 C 0.193(2) 0.110(2) 0.2777(3) 0.152(4) Uani 0.125 1 d D U . A -1
H4A H 0.317332 0.013861 0.272747 0.228 Uiso 0.125 1 calc GR . . A -1
H4B H 0.245979 0.244231 0.288688 0.228 Uiso 0.125 1 calc GR . . A -1
H4C H 0.117608 0.147362 0.256467 0.228 Uiso 0.125 1 calc GR . . A -1
C3 C -0.025(4) -0.2395(14) 0.2901(4) 0.186(5) Uani 0.125 1 d D U . A -1
H3A H -0.053808 -0.239208 0.265500 0.280 Uiso 0.125 1 calc GR . . A -1
H3B H -0.155968 -0.289258 0.302268 0.280 Uiso 0.125 1 calc GR . . A -1
H3C H 0.097116 -0.338588 0.295052 0.280 Uiso 0.125 1 calc GR . . A -1
C5 C -0.0022(17) -0.0695(17) 0.4843(3) 0.107(3) Uani 0.0625 1 d D U . B -1
H5 H -0.012258 -0.032438 0.460815 0.129 Uiso 0.0625 1 calc R . . B -1
N3 N 0.1416(18) 0.036(2) 0.5035(4) 0.084(5) Uani 0.0625 1 d D U . B -1
H3D H 0.153598 0.004556 0.525232 0.100 Uiso 0.0625 1 calc R . . B -1
H3E H 0.224861 0.137998 0.494433 0.100 Uiso 0.0625 1 calc R . . B -1
N2 N -0.132(2) -0.2245(19) 0.4963(7) 0.32(3) Uani 0.0625 1 d D U . B -1
H2A H -0.125763 -0.261247 0.517965 0.381 Uiso 0.0625 1 calc R . . B -1
H2B H -0.225452 -0.290466 0.482720 0.381 Uiso 0.0625 1 calc R . . B -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 Br3 3.1127(3) . ?
Pb1 Br1 2.99206(10) 1_455 ?
Pb1 Br1 2.99206(10) 2_455 ?
Pb1 Br1 2.99206(10) 2_445 ?
Pb1 Br1 2.99206(10) . ?
Pb1 Br2 2.8200(16) . ?
N1 C0AA 1.499(11) . ?
C1AA C0AA 1.501(9) . ?
C1AA C4 1.500(13) . ?
C1AA C3 1.500(12) . ?
C5 N3 1.297(13) . ?
C5 N2 1.297(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br3 89.88(2) 2_445 . ?
Br1 Pb1 Br3 89.89(2) . . ?
Br1 Pb1 Br3 89.88(2) 2_455 . ?
Br1 Pb1 Br3 89.88(2) 1_455 . ?
Br1 Pb1 Br1 90.0 . 2_445 ?
Br1 Pb1 Br1 179.77(4) 2_455 2_445 ?
Br1 Pb1 Br1 90.0 2_445 1_455 ?
Br1 Pb1 Br1 179.77(4) . 1_455 ?
Br1 Pb1 Br1 90.0 2_455 1_455 ?
Br1 Pb1 Br1 90.0 . 2_455 ?
Br2 Pb1 Br3 180.0 . . ?
Br2 Pb1 Br1 90.12(2) . 1_455 ?
Br2 Pb1 Br1 90.12(2) . 2_455 ?
Br2 Pb1 Br1 90.11(2) . . ?
Br2 Pb1 Br1 90.12(2) . 2_445 ?
Pb1 Br3 Pb1 180.0 17_446 . ?
Pb1 Br1 Pb1 179.77(4) 1_655 . ?
C4 C1AA C0AA 113.0(10) . . ?
C3 C1AA C0AA 112.8(13) . . ?
C3 C1AA C4 113.6(10) . . ?
N1 C0AA C1AA 115.0(8) . . ?
N2 C5 N3 123.0(15) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
