# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2021

####################################################################### 
# 
# 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_C3H8N6_PbBr4
_database_code_depnum_ccdc_archive 'CCDC 2053225'
_audit_update_record             
;
2021-10-03 deposited with the CCDC.	2021-10-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br4 Pb, C3 H8 N6'
_chemical_formula_sum            'C3 H8 Br4 N6 Pb'
_chemical_formula_weight         654.95

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   6.0130(4)
_cell_length_b                   21.3814(14)
_cell_length_c                   10.2099(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.132(3)
_cell_angle_gamma                90.00
_cell_volume                     1272.92(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4010
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      25.8

_exptl_crystal_description       prism
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      3.417
_exptl_crystal_density_diffrn    3.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160.0
_exptl_absorpt_coefficient_mu    25.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_T_max  0.045
_exptl_absorpt_process_details   '(Coppens et al., 1965)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14718
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0884
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         30.91
_reflns_number_total             4023
_reflns_number_gt                2639
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0811P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4010
_refine_ls_number_parameters     128
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1569
_refine_ls_wR_factor_gt          0.1333
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.64269(7) 0.665567(19) 0.28318(4) 0.02604(16) Uani 1 1 d . . .
Br2 Br 0.5685(2) 0.58041(5) 0.05538(10) 0.0319(3) Uani 1 1 d . . .
Br1 Br 0.7283(2) 0.55414(5) 0.44511(11) 0.0344(3) Uani 1 1 d . . .
Br3 Br 0.15073(19) 0.64579(6) 0.26913(13) 0.0382(3) Uani 1 1 d . . .
Br4 Br 0.6534(2) 0.77073(6) 0.06716(12) 0.0400(3) Uani 1 1 d . . .
N3 N 0.8789(15) 0.4461(4) 0.2589(9) 0.031(2) Uani 1 1 d . . .
H3 H 0.8541 0.4811 0.2943 0.037 Uiso 1 1 calc R . .
N1 N 0.7806(18) 0.3393(4) 0.2192(9) 0.032(2) Uani 1 1 d . . .
N5 N 1.0481(16) 0.3883(5) 0.1186(9) 0.033(2) Uani 1 1 d . . .
H5 H 1.1431 0.3852 0.0681 0.040 Uiso 1 1 calc R . .
N6 N 0.9256(17) 0.2883(4) 0.0640(10) 0.039(2) Uani 1 1 d . . .
H6A H 0.8449 0.2559 0.0719 0.047 Uiso 1 1 calc R . .
H6B H 1.0136 0.2877 0.0091 0.047 Uiso 1 1 calc R . .
N4 N 1.1571(18) 0.4906(5) 0.1669(10) 0.042(3) Uani 1 1 d . . .
H4A H 1.1450 0.5255 0.2067 0.050 Uiso 1 1 calc R . .
H4B H 1.2528 0.4872 0.1169 0.050 Uiso 1 1 calc R . .
C2 C 1.0296(19) 0.4428(5) 0.1822(10) 0.027(2) Uani 1 1 d . . .
C1 C 0.7668(18) 0.3944(5) 0.2802(10) 0.026(2) Uani 1 1 d . . .
C3 C 0.915(2) 0.3376(6) 0.1345(12) 0.037(3) Uani 1 1 d . . .
N2 N 0.6274(19) 0.3987(5) 0.3605(10) 0.046(3) Uani 1 1 d . . .
H2A H 0.6103 0.4338 0.3976 0.055 Uiso 1 1 calc R . .
H2B H 0.5531 0.3662 0.3761 0.055 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb 0.0279(2) 0.0257(2) 0.0262(2) -0.00029(15) 0.00985(16) -0.00058(16)
Br2 0.0346(6) 0.0346(6) 0.0290(5) -0.0080(4) 0.0127(5) -0.0048(5)
Br1 0.0456(7) 0.0299(6) 0.0311(6) 0.0041(5) 0.0161(5) 0.0096(5)
Br3 0.0245(6) 0.0417(7) 0.0506(7) -0.0055(5) 0.0134(5) -0.0002(5)
Br4 0.0487(8) 0.0358(7) 0.0413(6) 0.0111(5) 0.0218(6) 0.0112(5)
N3 0.032(5) 0.029(5) 0.036(5) -0.006(4) 0.017(4) -0.005(4)
N1 0.038(5) 0.035(6) 0.030(5) 0.004(4) 0.022(4) 0.000(4)
N5 0.029(5) 0.044(6) 0.032(5) -0.005(4) 0.018(4) 0.006(4)
N6 0.043(6) 0.026(5) 0.058(6) -0.008(5) 0.030(5) 0.002(4)
N4 0.050(7) 0.041(6) 0.039(5) -0.009(5) 0.023(5) -0.023(5)
C2 0.035(6) 0.020(5) 0.022(5) 0.002(4) 0.001(4) -0.003(4)
C1 0.031(6) 0.029(6) 0.023(5) 0.002(4) 0.016(4) 0.005(5)
C3 0.037(7) 0.043(8) 0.033(6) 0.003(5) 0.013(5) -0.006(5)
N2 0.054(7) 0.045(7) 0.053(6) -0.004(5) 0.041(6) 0.005(5)

_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
Pb Br1 2.8737(12) . ?
Pb Br2 2.9012(11) . ?
Pb Br3 2.9568(12) . ?
Pb Br3 3.1218(12) 1_655 ?
Pb Br4 3.1613(12) . ?
Pb Br4 3.1897(12) 4_576 ?
Br3 Pb 3.1218(12) 1_455 ?
Br4 Pb 3.1897(12) 4_575 ?
N3 C2 1.337(13) . ?
N3 C1 1.339(13) . ?
N3 H3 0.8600 . ?
N1 C3 1.319(14) . ?
N1 C1 1.345(13) . ?
N5 C2 1.351(13) . ?
N5 C3 1.382(15) . ?
N5 H5 0.8600 . ?
N6 C3 1.288(15) . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
N4 C2 1.311(14) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
C1 N2 1.310(12) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?

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 Pb Br2 84.94(3) . . ?
Br1 Pb Br3 86.90(4) . . ?
Br2 Pb Br3 85.13(4) . . ?
Br1 Pb Br3 82.78(4) . 1_655 ?
Br2 Pb Br3 80.72(3) . 1_655 ?
Br3 Pb Br3 163.14(5) . 1_655 ?
Br1 Pb Br4 163.68(3) . . ?
Br2 Pb Br4 84.97(4) . . ?
Br3 Pb Br4 104.98(4) . . ?
Br3 Pb Br4 82.96(4) 1_655 . ?
Br1 Pb Br4 82.53(3) . 4_576 ?
Br2 Pb Br4 164.09(4) . 4_576 ?
Br3 Pb Br4 84.44(3) . 4_576 ?
Br3 Pb Br4 107.26(4) 1_655 4_576 ?
Br4 Pb Br4 109.336(14) . 4_576 ?
Pb Br3 Pb 163.14(5) . 1_455 ?
Pb Br4 Pb 159.81(5) . 4_575 ?
C2 N3 C1 119.5(9) . . ?
C2 N3 H3 120.3 . . ?
C1 N3 H3 120.3 . . ?
C3 N1 C1 116.4(10) . . ?
C2 N5 C3 120.1(9) . . ?
C2 N5 H5 120.0 . . ?
C3 N5 H5 120.0 . . ?
C3 N6 H6A 120.0 . . ?
C3 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C2 N4 H4A 120.0 . . ?
C2 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
N4 C2 N3 121.9(10) . . ?
N4 C2 N5 119.8(10) . . ?
N3 C2 N5 118.3(10) . . ?
N2 C1 N3 117.9(10) . . ?
N2 C1 N1 118.1(10) . . ?
N3 C1 N1 123.8(9) . . ?
N6 C3 N1 120.8(11) . . ?
N6 C3 N5 117.8(11) . . ?
N1 C3 N5 121.4(11) . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?

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
Br1 Pb Br3 Pb 127.80(17) . . . 1_455 ?
Br2 Pb Br3 Pb -147.02(17) . . . 1_455 ?
Br3 Pb Br3 Pb 180.0 1_655 . . 1_455 ?
Br4 Pb Br3 Pb -63.56(17) . . . 1_455 ?
Br4 Pb Br3 Pb 45.01(17) 4_576 . . 1_455 ?
Br1 Pb Br4 Pb 49.7(2) . . . 4_575 ?
Br2 Pb Br4 Pb -2.36(14) . . . 4_575 ?
Br3 Pb Br4 Pb -85.94(14) . . . 4_575 ?
Br3 Pb Br4 Pb 78.89(14) 1_655 . . 4_575 ?
Br4 Pb Br4 Pb -175.23(10) 4_576 . . 4_575 ?
C1 N3 C2 N4 -174.5(10) . . . . ?
C1 N3 C2 N5 6.0(15) . . . . ?
C3 N5 C2 N4 179.9(11) . . . . ?
C3 N5 C2 N3 -0.6(16) . . . . ?
C2 N3 C1 N2 177.2(10) . . . . ?
C2 N3 C1 N1 -6.1(16) . . . . ?
C3 N1 C1 N2 177.0(11) . . . . ?
C3 N1 C1 N3 0.3(17) . . . . ?
C1 N1 C3 N6 -174.9(11) . . . . ?
C1 N1 C3 N5 5.3(17) . . . . ?
C2 N5 C3 N6 174.9(10) . . . . ?
C2 N5 C3 N1 -5.3(18) . . . . ?



_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.91
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.377
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.429
