# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2022240'
_audit_update_record             
;
2020-11-04 deposited with the CCDC.	2020-11-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H36 Br10 N4 O2 Pb3'
_chemical_formula_weight         1713.14

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.3186(13)
_cell_length_b                   15.9262(17)
_cell_length_c                   11.5922(13)
_cell_angle_alpha                90
_cell_angle_beta                 118.5478(12)
_cell_angle_gamma                90
_cell_volume                     1835.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6453
_cell_measurement_theta_min      2.048
_cell_measurement_theta_max      27.559

_exptl_crystal_description       prism
_exptl_crystal_colour            yellowish
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.100
_exptl_crystal_F_000             1520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    24.627
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.312
_exptl_absorpt_correction_T_max  0.601
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21579
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.048
_diffrn_reflns_theta_max         27.559
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4227
_reflns_number_gt                3222
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.985
_reflns_Friedel_fraction_max     0.987
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4227
_refine_ls_number_parameters     141
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1674
_refine_ls_wR_factor_gt          0.1565
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.008

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 0.000000 0.500000 0.500000 0.03197(19) Uani 1 2 d S . P . .
Pb2 Pb 0.30172(4) 0.48878(3) 0.86722(4) 0.03411(17) Uani 1 1 d . . . . .
Br4 Br 0.11333(12) 0.35116(7) 0.68851(11) 0.0380(3) Uani 1 1 d . . . . .
Br3 Br 0.04122(12) 0.58858(9) 0.74928(12) 0.0435(3) Uani 1 1 d . . . . .
Br2 Br 0.29392(13) 0.53772(9) 0.59670(13) 0.0447(3) Uani 1 1 d . . . . .
Br1 Br 0.46057(12) 0.63577(8) 1.03866(12) 0.0420(3) Uani 1 1 d . . . . .
O1 O 0.0550(8) 0.8068(6) 0.5866(9) 0.045(2) Uani 1 1 d . . . . .
C7 C 0.0907(11) 0.8906(8) 0.6262(12) 0.039(3) Uani 1 1 d . . . . .
H7A H 0.017373 0.918127 0.632029 0.046 Uiso 1 1 calc R U . . .
H7B H 0.105176 0.919857 0.560573 0.046 Uiso 1 1 calc R U . . .
N1 N 0.3304(9) 0.8508(6) 0.7536(8) 0.029(2) Uani 1 1 d . . . . .
H1C H 0.353399 0.879500 0.692233 0.034 Uiso 1 1 calc R U . . .
C6 C 0.4529(11) 0.8530(8) 0.8895(12) 0.042(3) Uani 1 1 d . . . . .
H6A H 0.475293 0.911014 0.916386 0.051 Uiso 1 1 calc R U . . .
H6B H 0.430112 0.826089 0.951403 0.051 Uiso 1 1 calc R U . . .
C5 C 0.2896(11) 0.7645(8) 0.7069(12) 0.039(3) Uani 1 1 d . . . . .
H5A H 0.273887 0.733062 0.769967 0.046 Uiso 1 1 calc R U . . .
H5B H 0.360063 0.736538 0.696413 0.046 Uiso 1 1 calc R U . . .
C4 C 0.6916(11) 0.8143(10) 1.0337(14) 0.063(5) Uani 1 1 d . . . . .
H4A H 0.717166 0.872274 1.058877 0.076 Uiso 1 1 calc R U . . .
H4B H 0.666783 0.789705 1.095631 0.076 Uiso 1 1 calc R U . . .
C3 C 0.2124(12) 0.8960(8) 0.7530(12) 0.041(3) Uani 1 1 d . . . . .
H3A H 0.194763 0.871861 0.820092 0.049 Uiso 1 1 calc R U . . .
H3B H 0.235712 0.954591 0.774835 0.049 Uiso 1 1 calc R U . . .
C2 C 0.1599(12) 0.7686(10) 0.5743(13) 0.050(4) Uani 1 1 d . . . . .
H2A H 0.176983 0.799978 0.512112 0.060 Uiso 1 1 calc R U . . .
H2B H 0.133241 0.712148 0.540214 0.060 Uiso 1 1 calc R U . . .
N2 N 0.8068(10) 0.7677(8) 1.0377(11) 0.050(3) Uani 1 1 d . . . . .
H2C H 0.876111 0.769938 1.118532 0.075 Uiso 1 1 calc R U . . .
H2D H 0.783387 0.714380 1.015534 0.075 Uiso 1 1 calc R U . . .
H2E H 0.829996 0.790764 0.981534 0.075 Uiso 1 1 calc R U . . .
Br5 Br 0.29079(18) 0.42756(12) 1.09428(17) 0.0709(5) Uiso 1 1 d . . . . .
C1 C 0.5720(11) 0.8110(8) 0.8958(11) 0.036(3) Uiso 1 1 d . . . . .
H1A H 0.596037 0.838052 0.834924 0.043 Uiso 1 1 calc R U . . .
H1B H 0.550281 0.752861 0.869075 0.043 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 Br2 3.0200(13) 3_566 ?
Pb1 Br2 3.0200(13) . ?
Pb1 Br3 3.0446(13) . ?
Pb1 Br3 3.0446(13) 3_566 ?
Pb1 Br4 3.0594(12) . ?
Pb1 Br4 3.0595(12) 3_566 ?
Pb2 Br5 2.864(2) . ?
Pb2 Br3 3.0391(13) . ?
Pb2 Br1 3.0409(13) . ?
Pb2 Br4 3.0692(12) . ?
Pb2 Br1 3.0916(13) 3_667 ?
Pb2 Br2 3.1914(15) . ?
O1 C2 1.400(15) . ?
O1 C7 1.406(14) . ?
C7 C3 1.460(16) . ?
N1 C5 1.469(14) . ?
N1 C3 1.514(14) . ?
N1 C6 1.522(13) . ?
C6 C1 1.475(17) . ?
C5 C2 1.538(15) . ?
C4 N2 1.481(18) . ?
C4 C1 1.524(16) . ?

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 180.0 3_566 . ?
Br2 Pb1 Br3 94.96(4) 3_566 . ?
Br2 Pb1 Br3 85.04(4) . . ?
Br2 Pb1 Br3 85.04(4) 3_566 3_566 ?
Br2 Pb1 Br3 94.96(4) . 3_566 ?
Br3 Pb1 Br3 180.00(2) . 3_566 ?
Br2 Pb1 Br4 97.04(4) 3_566 . ?
Br2 Pb1 Br4 82.97(4) . . ?
Br3 Pb1 Br4 81.91(3) . . ?
Br3 Pb1 Br4 98.09(3) 3_566 . ?
Br2 Pb1 Br4 82.97(4) 3_566 3_566 ?
Br2 Pb1 Br4 97.03(4) . 3_566 ?
Br3 Pb1 Br4 98.09(3) . 3_566 ?
Br3 Pb1 Br4 81.91(3) 3_566 3_566 ?
Br4 Pb1 Br4 180.0 . 3_566 ?
Br5 Pb2 Br3 97.63(5) . . ?
Br5 Pb2 Br1 86.17(5) . . ?
Br3 Pb2 Br1 92.00(4) . . ?
Br5 Pb2 Br4 93.21(5) . . ?
Br3 Pb2 Br4 81.84(4) . . ?
Br1 Pb2 Br4 173.68(4) . . ?
Br5 Pb2 Br1 82.52(5) . 3_667 ?
Br3 Pb2 Br1 171.08(4) . 3_667 ?
Br1 Pb2 Br1 96.91(3) . 3_667 ?
Br4 Pb2 Br1 89.24(4) . 3_667 ?
Br5 Pb2 Br2 173.21(5) . . ?
Br3 Pb2 Br2 82.23(4) . . ?
Br1 Pb2 Br2 100.62(4) . . ?
Br4 Pb2 Br2 80.04(4) . . ?
Br1 Pb2 Br2 96.56(4) 3_667 . ?
Pb1 Br4 Pb2 81.24(3) . . ?
Pb2 Br3 Pb1 81.97(3) . . ?
Pb1 Br2 Pb2 79.89(3) . . ?
Pb2 Br1 Pb2 83.09(3) . 3_667 ?
C2 O1 C7 108.7(10) . . ?
O1 C7 C3 111.8(10) . . ?
C5 N1 C3 108.8(9) . . ?
C5 N1 C6 111.9(9) . . ?
C3 N1 C6 111.0(9) . . ?
C1 C6 N1 113.6(11) . . ?
N1 C5 C2 108.1(10) . . ?
N2 C4 C1 110.1(13) . . ?
C7 C3 N1 112.5(10) . . ?
O1 C2 C5 111.6(10) . . ?
C6 C1 C4 111.7(11) . . ?

_refine_diff_density_max         2.360
_refine_diff_density_min         -3.344
_refine_diff_density_rms         0.259

####################################################################### 
# 
# 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_Com-3
_database_code_depnum_ccdc_archive 'CCDC 2022242'
_audit_update_record             
;
2020-08-08 deposited with the CCDC.	2020-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-12-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br10 Pb3, 2(C6 H18 N2)'
_chemical_formula_sum            'C12 H36 Br10 N4 Pb3'
_chemical_formula_weight         1657.13
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
Pb -3.20855 10.15388 31.06170 13.06370 18.44200 5.96960 0.69020 2.35760 8.61800
47.25790 13.4118003845
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Br -0.28346 2.55990 17.17890 5.23580 5.63770 3.98510 2.17230 16.57960 0.26090
41.43280 2.95569992065
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_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 2ybc (x-z,y,z)'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x-1/2,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   11.3799(8)
_cell_length_b                   14.9895(11)
_cell_length_c                   11.4899(8)
_cell_angle_alpha                90
_cell_angle_beta                 116.7445(8)
_cell_angle_gamma                90
_cell_volume                     1750.3(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5573
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.41
_cell_measurement_temperature    296(2)
_exptl_absorpt_coefficient_mu    25.820
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light colourless'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.1441
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20582
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.87
_diffrn_reflns_theta_min         2.09
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9423
_diffrn_measured_fraction_theta_max 0.9382
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -15
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              -7
_reflns_number_gt                3224
_reflns_number_total             4330
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_refine_diff_density_max         3.8100
_refine_diff_density_min         -2.5603
_refine_diff_density_rms         0.5293
_refine_ls_d_res_high            0.7359
_refine_ls_d_res_low             9.7360
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.9785
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     137
_refine_ls_number_reflns         4330
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0511
_refine_ls_restrained_S_all      0.9785
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1089P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1679
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C6(H6a,H6b)
2.c Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C4(H4a,H4b,H4c), C3(H3a,H3b,H3c), C8(H8a,H8b,H8c)
;
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pb1 Pb 0.0 0.0 0.0 0.03308(19) Uani 1.000000 2 S T P
Pb2 Pb 0.07451(4) -0.00781(2) 0.36129(4) 0.03296(17) Uani 1.000000 1 . . .
Br5 Br 0.09440(11) 0.14068(6) 0.55817(11) 0.0378(3) Uani 1.000000 1 . . .
Br4 Br 0.19545(11) 0.10381(8) 0.23225(11) 0.0431(3) Uani 1.000000 1 . . .
Br3 Br -0.19163(11) 0.05542(8) 0.10496(12) 0.0446(3) Uani 1.000000 1 . . .
Br2 Br -0.07252(11) 0.15463(7) -0.19227(11) 0.0390(3) Uani 1.000000 1 . . .
Br1 Br 0.32537(12) -0.05529(7) 0.56652(12) 0.0485(4) Uani 1.000000 1 . . .
N1 N 0.4540(8) 0.1455(5) 0.6720(8) 0.0306(18) Uani 1.000000 1 . . .
C1 C 0.4327(11) 0.1964(6) 0.7716(9) 0.032(2) Uani 1.000000 1 . . .
N2 N 0.4148(8) 0.1821(5) 0.9788(8) 0.0327(19) Uani 1.000000 1 . . .
C6 C 0.4387(10) 0.1334(7) 0.8796(10) 0.033(2) Uani 1.000000 1 . . .
C5 C 0.4258(13) 0.2035(8) 0.5560(11) 0.047(3) Uani 1.000000 1 . . .
C4 C 0.2719(12) 0.2069(9) 0.9306(13) 0.052(3) Uani 1.000000 1 . . .
C3 C 0.5890(15) 0.1096(11) 0.7186(15) 0.076(5) Uani 1.000000 1 . . .
C8 C 0.4599(12) 0.1293(9) 1.1024(11) 0.048(3) Uani 1.000000 1 . . .
H1 H 0.3967(8) 0.0988(5) 0.6455(8) 0.037(2) Uiso 1.000000 1 R . .
H1a H 0.4997(11) 0.2421(6) 0.8089(9) 0.038(3) Uiso 1.000000 1 R . .
H1b H 0.3475(11) 0.2256(6) 0.7310(9) 0.038(3) Uiso 1.000000 1 R . .
H2 H 0.4624(8) 0.2335(5) 0.9977(8) 0.039(2) Uiso 1.000000 1 R . .
H6a H 0.3731(10) 0.0869(7) 0.8415(10) 0.040(3) Uiso 1.000000 1 R . .
H6b H 0.5245(10) 0.1052(7) 0.9210(10) 0.040(3) Uiso 1.000000 1 R . .
H5a H 0.337(3) 0.226(5) 0.521(5) 0.070(4) Uiso 1.000000 1 GR . .
H5b H 0.486(5) 0.253(3) 0.582(2) 0.070(4) Uiso 1.000000 1 GR . .
H5c H 0.436(8) 0.1692(17) 0.490(3) 0.070(4) Uiso 1.000000 1 GR . .
H4a H 0.245(3) 0.245(5) 0.856(6) 0.077(5) Uiso 1.000000 1 GR . .
H4b H 0.2191(14) 0.1538(10) 0.906(8) 0.077(5) Uiso 1.000000 1 GR . .
H4c H 0.2607(19) 0.237(5) 0.999(3) 0.077(5) Uiso 1.000000 1 GR . .
H3a H 0.6512(17) 0.1578(14) 0.749(10) 0.115(7) Uiso 1.000000 1 GR . .
H3b H 0.607(4) 0.069(6) 0.789(7) 0.115(7) Uiso 1.000000 1 GR . .
H3c H 0.596(3) 0.079(6) 0.648(3) 0.115(7) Uiso 1.000000 1 GR . .
H8a H 0.407(6) 0.077(3) 1.086(2) 0.072(4) Uiso 1.000000 1 GR . .
H8b H 0.550(3) 0.112(5) 1.132(5) 0.072(4) Uiso 1.000000 1 GR . .
H8c H 0.451(8) 0.165(2) 1.168(3) 0.072(4) Uiso 1.000000 1 GR . .


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 3.0245(11) . ?
Pb1 Br4 3.0245(11) 3 ?
Pb1 Br3 3.0443(13) . ?
Pb1 Br3 3.0443(13) 3 ?
Pb1 Br2 3.0484(12) . ?
Pb1 Br2 3.0484(12) 3 ?
Pb2 Br5 3.1084(11) . ?
Pb2 Br4 2.9544(12) . ?
Pb2 Br2 2.9284(11) 3 ?
Pb2 Br1 2.8562(12) . ?
N1 C1 1.483(13) . ?
N1 C5 1.501(14) . ?
N1 C3 1.482(16) . ?
C1 C6 1.537(14) . ?
N2 C6 1.477(13) . ?
N2 C4 1.509(14) . ?
N2 C8 1.501(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
Br4 Pb1 Br4 180.0 3 . ?
Br3 Pb1 Br4 96.69(3) . 3 ?
Br3 Pb1 Br4 96.69(3) 3 . ?
Br3 Pb1 Br4 83.31(3) . . ?
Br3 Pb1 Br4 83.31(3) 3 3 ?
Br3 Pb1 Br3 180.0 3 . ?
Br2 Pb1 Br4 84.26(3) 3 . ?
Br2 Pb1 Br4 95.74(3) 3 3 ?
Br2 Pb1 Br4 95.74(3) . . ?
Br2 Pb1 Br4 84.26(3) . 3 ?
Br2 Pb1 Br3 94.07(3) . . ?
Br2 Pb1 Br3 94.07(3) 3 3 ?
Br2 Pb1 Br3 85.93(3) . 3 ?
Br2 Pb1 Br3 85.93(3) 3 . ?
Br2 Pb1 Br2 180.0 3 . ?
Br4 Pb2 Br5 93.55(3) . . ?
Br2 Pb2 Br5 175.61(3) 3 . ?
Br2 Pb2 Br4 87.66(3) 3 . ?
Br1 Pb2 Br5 81.91(3) . . ?
Br1 Pb2 Br4 92.13(4) . . ?
Br1 Pb2 Br2 93.83(3) . 3 ?
Pb2 Br4 Pb1 80.08(3) . . ?
Pb2 Br2 Pb1 80.09(3) 3 . ?
C5 N1 C1 110.0(8) . . ?
C3 N1 C1 114.3(10) . . ?
C3 N1 C5 107.7(10) . . ?
C6 C1 N1 110.1(8) . . ?
C4 N2 C6 112.3(8) . . ?
C8 N2 C6 111.4(8) . . ?
C8 N2 C4 109.3(9) . . ?
N2 C6 C1 111.3(8) . . ?

_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_Com-2-[DMPrDA]2Pb3Br10
_database_code_depnum_ccdc_archive 'CCDC 2022241'
_audit_update_record             
;
2020-08-08 deposited with the CCDC.	2020-11-05 downloaded from the CCDC.
;
_audit_creation_date             2020-08-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_formula_moiety         '0.5(Br20 Pb6), 2(C5 H16 N2)'
_chemical_formula_sum            'C10 H32 Br10 N4 Pb3'
_chemical_formula_weight         1629.08
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
Pb -3.20855 10.15388 31.06170 13.06370 18.44200 5.96960 0.69020 2.35760 8.61800
47.25790 13.4118003845
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Br -0.28346 2.55990 17.17890 5.23580 5.63770 3.98510 2.17230 16.57960 0.26090
41.43280 2.95569992065
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_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_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z+1/2
3 -x,-y,-z
4 x,-y,z-1/2
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z+1/2
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z-1/2

_symmetry_Int_Tables_number      15
_cell_length_a                   20.368(3)
_cell_length_b                   8.0895(12)
_cell_length_c                   22.524(3)
_cell_angle_alpha                90
_cell_angle_beta                 114.5690(17)
_cell_angle_gamma                90
_cell_volume                     3375.2(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3992
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.01
_cell_measurement_theta_min      2.27
_exptl_absorpt_coefficient_mu    26.776
_exptl_absorpt_correction_T_max  0.0485
_exptl_absorpt_correction_T_min  0.0348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_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    3.2057
_exptl_crystal_description       prism
_exptl_crystal_F_000             2822.3232
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19091
_diffrn_reflns_theta_full        27.2977
_diffrn_reflns_theta_max         27.30
_diffrn_reflns_theta_min         1.99
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9847
_diffrn_measured_fraction_theta_max 0.9847
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              23
_reflns_limit_h_min              -26
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                2876
_reflns_number_total             3740
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         4.7670
_refine_diff_density_min         -2.9860
_refine_diff_density_rms         0.4515
_refine_ls_d_res_high            0.7749
_refine_ls_d_res_low             10.2422
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0423
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    23
_refine_ls_number_parameters     125
_refine_ls_number_reflns         3740
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0474
_refine_ls_restrained_S_all      1.0423
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0675P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1207
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N2(H2a,H2b), N1(H1a,H1b), C5(H5a,H5b), C3(H3a,H3b), C2(H2c,H2d)
2.b Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C1(H1c,H1d,H1e)
;
_atom_sites_solution_primary     direct
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pb1 Pb 0.54769(2) 0.57930(5) 0.600059(18) 0.02999(16) Uani 1.000000 1 . . .
Pb2 Pb 0.5 0.64111(7) 0.75 0.03200(18) Uani 1.000000 2 S T P
Br5 Br 0.58264(6) 0.38253(13) 0.72122(5) 0.0397(3) Uani 1.000000 1 . . .
Br4 Br 0.50177(6) 0.25084(13) 0.53302(5) 0.0390(3) Uani 1.000000 1 . . .
Br3 Br 0.69048(6) 0.53307(16) 0.60656(7) 0.0484(3) Uani 1.000000 1 . . .
Br2 Br 0.39396(6) 0.62566(15) 0.60812(6) 0.0429(3) Uani 1.000000 1 . . .
Br1 Br 0.57588(7) 0.88351(14) 0.68575(7) 0.0487(3) Uani 1.000000 1 . . .
N2 N 0.6850(5) 0.1283(11) 0.6430(4) 0.039(2) Uani 1.000000 1 . . .
H2a H 0.6759(5) 0.2324(11) 0.6276(4) 0.047(3) Uiso 1.000000 1 R . .
H2b H 0.6444(5) 0.0872(11) 0.6440(4) 0.047(3) Uiso 1.000000 1 R . .
N1 N 0.6084(6) -0.0361(12) 0.4190(5) 0.047(2) Uani 1.000000 1 . . .
H1a H 0.5685(6) -0.0652(12) 0.4242(5) 0.056(3) Uiso 1.000000 1 R . .
H1b H 0.6043(6) 0.0718(12) 0.4083(5) 0.056(3) Uiso 1.000000 1 R . .
C5 C 0.6712(8) -0.0568(16) 0.4820(7) 0.056(3) Uani 1.000000 1 . . .
H5a H 0.6766(8) -0.1720(16) 0.4951(7) 0.067(4) Uiso 1.000000 1 R . .
H5b H 0.7149(8) -0.0214(16) 0.4784(7) 0.067(4) Uiso 1.000000 1 R . .
C4 C 0.6106(8) -0.1337(18) 0.3630(7) 0.065(4) Uani 1.000000 1 . . .
H4a H 0.570(3) -0.106(9) 0.3236(11) 0.097(6) Uiso 1.000000 1 GR . .
H4b H 0.654(3) -0.108(9) 0.358(3) 0.097(6) Uiso 1.000000 1 GR . .
H4c H 0.610(5) -0.2497(18) 0.372(2) 0.097(6) Uiso 1.000000 1 GR . .
C3 C 0.7059(8) 0.027(2) 0.5992(7) 0.066(4) Uani 1.000000 1 . . .
H3a H 0.7544(8) 0.056(2) 0.6053(7) 0.079(5) Uiso 1.000000 1 R . .
H3b H 0.7060(8) -0.089(2) 0.6106(7) 0.079(5) Uiso 1.000000 1 R . .
C2 C 0.6579(11) 0.0501(18) 0.5327(7) 0.084(6) Uani 1.000000 1 . . .
H2c H 0.6600(11) 0.1654(18) 0.5218(7) 0.101(7) Uiso 1.000000 1 R . .
H2d H 0.6092(11) 0.0287(18) 0.5283(7) 0.101(7) Uiso 1.000000 1 R . .
C1 C 0.7432(8) 0.1300(19) 0.7097(8) 0.089(6) Uani 1.000000 1 . . .
H1c H 0.772(4) 0.228(8) 0.716(2) 0.134(9) Uiso 1.000000 1 GR . .
H1d H 0.7224(8) 0.128(16) 0.7409(8) 0.134(9) Uiso 1.000000 1 GR . .
H1e H 0.773(4) 0.035(9) 0.716(2) 0.134(9) Uiso 1.000000 1 GR . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br5 2.9786(12) . ?
Pb1 Br4 3.0620(12) 3_666 ?
Pb1 Br4 3.0067(12) . ?
Pb1 Br3 2.8752(13) . ?
Pb1 Br1 3.0314(13) . ?
Pb2 Br5 2.9217(12) . ?
Pb2 Br5 2.9217(12) 2_656 ?
Pb2 Br2 3.0254(12) . ?
Pb2 Br2 3.0254(12) 2_656 ?
N2 C3 1.473(16) . ?
N2 C1 1.478(17) . ?
N1 C5 1.471(16) . ?
N1 C4 1.505(16) . ?
C5 C2 1.544(18) . ?
C3 C2 1.42(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br4 Pb1 Br5 173.06(3) 3_666 . ?
Br4 Pb1 Br5 83.91(3) . . ?
Br3 Pb1 Br5 91.86(4) . . ?
Br3 Pb1 Br4 90.43(4) . . ?
Br3 Pb1 Br4 91.28(4) . 3_666 ?
Br1 Pb1 Br5 86.60(3) . . ?
Br1 Pb1 Br4 166.95(3) . . ?
Br1 Pb1 Br4 99.04(3) . 3_666 ?
Br1 Pb1 Br3 98.82(4) . . ?
Br5 Pb2 Br5 88.56(5) 2_656 . ?
Br2 Pb2 Br5 88.89(3) . 2_656 ?
Br2 Pb2 Br5 87.72(3) . . ?
Br2 Pb2 Br5 87.72(3) 2_656 2_656 ?
Br2 Pb2 Br5 88.89(3) 2_656 . ?
Br2 Pb2 Br2 175.26(5) . 2_656 ?
Pb2 Br5 Pb1 83.13(3) 2_656 . ?
C1 N2 C3 110.7(11) . . ?
C4 N1 C5 115.6(10) . . ?
C2 C5 N1 107.5(11) . . ?
C2 C3 N2 111.7(12) . . ?
C3 C2 C5 116.8(13) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
