# 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_C4H26Cl4N2Pb
_database_code_depnum_ccdc_archive 'CCDC 1964689'
loop_
_audit_author_name
_audit_author_address
'chen sun'
;Jining University, Qufu, Shandong
China
;
_audit_update_record             
;
2019-11-09 deposited with the CCDC.	2020-01-06 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         C4H26Cl4N2Pb
_chemical_formula_sum            'C4 H26 Cl4 N2 Pb'
_chemical_formula_weight         451.27

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'

_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'
'x, -y, -z'
'-x, y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z'
'x, -y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y, z+1/2'

_cell_length_a                   14.1317(14)
_cell_length_b                   5.8342(6)
_cell_length_c                   14.5513(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1199.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9922
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      24.29

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.498
_exptl_crystal_F_000             856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    14.908
_shelx_estimated_absorpt_T_min   0.317
_shelx_estimated_absorpt_T_max   0.382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3993
_exptl_absorpt_correction_T_max  0.7291
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7086
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.009
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             797
_reflns_number_gt                776
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'APEX2 Software Suite (Bruker,2005)'
_computing_cell_refinement       'APEX2 Software Suite (Bruker,2005)'
_computing_data_reduction        'APEX2 Software Suite (Bruker,2005)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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     
'w=1/[σ²(Fo²)+(0.0258P)²+4.7935P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00316(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         797
_refine_ls_number_parameters     38
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0172
_refine_ls_wR_factor_ref         0.0472
_refine_ls_wR_factor_gt          0.0469
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.000
_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_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 0.250000 0.38620(2) 0.02515(13) Uani 1 4 d S T P . .
Cl1 Cl 0.000000 0.250000 0.20073(15) 0.0474(5) Uani 1 4 d S T P . .
Cl2 Cl 0.000000 -0.250000 0.39481(14) 0.0453(5) Uani 1 4 d S T P . .
Cl3 Cl 0.20317(11) 0.250000 0.40150(11) 0.0427(3) Uani 1 2 d S T P . .
N1 N 0.2157(4) 0.750000 0.1254(3) 0.0438(12) Uani 1 2 d S T P . .
H1A H 0.248709 0.625860 0.112595 0.053 Uiso 0.5 1 d R U P . .
H1B H 0.248709 0.874140 0.112595 0.053 Uiso 0.5 1 d R U P . .
H2A H 0.248539 0.624410 0.103905 0.053 Uiso 0.5 1 d R U P . .
H2B H 0.248539 0.624410 0.103905 0.053 Uiso 0.5 1 d R U P . .
C1 C 0.2029(5) 0.750000 0.2268(5) 0.0542(17) Uani 1 2 d S T P . .
H1C H 0.163722 0.614880 0.241097 0.065 Uiso 0.5 1 d R U P . .
H1D H 0.163722 0.614880 0.241097 0.065 Uiso 0.5 1 d R U P . .
H3A H 0.172162 0.884580 0.250857 0.065 Uiso 0.5 1 d R U P . .
H3B H 0.172162 0.615420 0.250857 0.065 Uiso 0.5 1 d R U P . .
C2 C 0.1238(5) 0.750000 0.0775(6) 0.0549(17) Uani 1 2 d S T P . .
H2C H 0.132842 0.750000 0.012315 0.066 Uiso 1 2 d R U P . .
H2D H 0.082522 0.884350 0.084565 0.066 Uiso 0.5 1 d R U P . .
H2E H 0.082522 0.615650 0.084565 0.066 Uiso 0.5 1 d R U P . .
H4B H 0.095802 0.615650 0.105555 0.066 Uiso 0.5 1 d R U P . .
H4C H 0.095802 0.615650 0.105555 0.066 Uiso 0.5 1 d R U 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 Cl1 2.699(2) . ?
Pb1 Cl3 2.8798(15) 2 ?
Pb1 Cl3 2.8798(15) . ?
Pb1 Cl2 2.9198(3) 1_565 ?
Pb1 Cl2 2.9198(3) . ?
Pb1 Cl2 3.186(2) 9_556 ?
Pb1 Pb1 4.4133(5) 9_566 ?
Pb1 Pb1 4.4133(5) 9_556 ?
N1 C2 1.474(10) . ?
N1 C1 1.486(8) . ?
N1 H1A 0.8816 . ?
N1 H1B 0.8816 . ?
N1 H2A 0.9222 . ?
N1 H2B 0.9222 . ?
N1 H2A 0.9222 12_575 ?
C1 C1 1.494(15) 13_565 ?
C1 H1C 0.9854 . ?
C1 H1D 0.9854 . ?
C1 H3A 0.9632 . ?
C1 H3B 0.9632 . ?
C2 H2C 0.9567 . ?
C2 H2D 0.9825 . ?
C2 H2E 0.9825 . ?
C2 H4B 0.9685 . ?
C2 H4C 0.9685 . ?

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 Pb1 Cl3 94.43(3) . 2 ?
Cl1 Pb1 Cl3 94.43(3) . . ?
Cl3 Pb1 Cl3 171.14(7) 2 . ?
Cl1 Pb1 Cl2 92.46(4) . 1_565 ?
Cl3 Pb1 Cl2 89.810(4) 2 1_565 ?
Cl3 Pb1 Cl2 89.810(4) . 1_565 ?
Cl1 Pb1 Cl2 92.46(4) . . ?
Cl3 Pb1 Cl2 89.810(4) 2 . ?
Cl3 Pb1 Cl2 89.810(4) . . ?
Cl2 Pb1 Cl2 175.08(8) 1_565 . ?
Cl1 Pb1 Cl2 180.0 . 9_556 ?
Cl3 Pb1 Cl2 85.57(3) 2 9_556 ?
Cl3 Pb1 Cl2 85.57(3) . 9_556 ?
Cl2 Pb1 Cl2 87.54(4) 1_565 9_556 ?
Cl2 Pb1 Cl2 87.54(4) . 9_556 ?
Cl1 Pb1 Pb1 138.625(6) . 9_566 ?
Cl3 Pb1 Pb1 86.68(3) 2 9_566 ?
Cl3 Pb1 Pb1 86.68(3) . 9_566 ?
Cl2 Pb1 Pb1 46.17(4) 1_565 9_566 ?
Cl2 Pb1 Pb1 128.92(4) . 9_566 ?
Cl2 Pb1 Pb1 41.375(6) 9_556 9_566 ?
Cl1 Pb1 Pb1 138.625(6) . 9_556 ?
Cl3 Pb1 Pb1 86.68(3) 2 9_556 ?
Cl3 Pb1 Pb1 86.68(3) . 9_556 ?
Cl2 Pb1 Pb1 128.92(4) 1_565 9_556 ?
Cl2 Pb1 Pb1 46.17(4) . 9_556 ?
Cl2 Pb1 Pb1 41.375(6) 9_556 9_556 ?
Pb1 Pb1 Pb1 82.750(12) 9_566 9_556 ?
Pb1 Cl2 Pb1 175.08(8) 1_545 . ?
Pb1 Cl2 Pb1 92.46(4) 1_545 9_556 ?
Pb1 Cl2 Pb1 92.46(4) . 9_556 ?
C2 N1 C1 111.2(6) . . ?
C2 N1 H1A 111.5 . . ?
C1 N1 H1A 105.9 . . ?
C2 N1 H1B 111.5 . . ?
C1 N1 H1B 105.9 . . ?
H1A N1 H1B 110.5 . . ?
C2 N1 H2A 106.4 . . ?
C1 N1 H2A 113.5 . . ?
H1A N1 H2A 7.6 . . ?
H1B N1 H2A 108.3 . . ?
C2 N1 H2B 106.4 . . ?
C1 N1 H2B 113.5 . . ?
H1A N1 H2B 7.6 . . ?
H1B N1 H2B 108.3 . . ?
H2A N1 H2B 0.0 . . ?
C2 N1 H2A 106.4(2) . 12_575 ?
C1 N1 H2A 113.48(19) . 12_575 ?
H1A N1 H2A 108.3 . 12_575 ?
H1B N1 H2A 7.6 . 12_575 ?
H2A N1 H2A 105.2 . 12_575 ?
H2B N1 H2A 105.2 . 12_575 ?
N1 C1 C1 109.9(7) . 13_565 ?
N1 C1 H1C 106.2 . . ?
C1 C1 H1C 113.9 13_565 . ?
N1 C1 H1D 106.2 . . ?
C1 C1 H1D 113.9 13_565 . ?
H1C C1 H1D 0.0 . . ?
N1 C1 H3A 114.6 . . ?
C1 C1 H3A 103.7 13_565 . ?
H1C C1 H3A 108.8 . . ?
H1D C1 H3A 108.8 . . ?
N1 C1 H3B 114.6 . . ?
C1 C1 H3B 103.7 13_565 . ?
H1C C1 H3B 10.8 . . ?
H1D C1 H3B 10.8 . . ?
H3A C1 H3B 109.2 . . ?
N1 C2 H2C 110.6 . . ?
N1 C2 H2D 118.2 . . ?
H2C C2 H2D 100.6 . . ?
N1 C2 H2E 118.2 . . ?
H2C C2 H2E 100.6 . . ?
H2D C2 H2E 105.8 . . ?
N1 C2 H4B 99.2 . . ?
H2C C2 H4B 118.2 . . ?
H2D C2 H4B 111.0 . . ?
H2E C2 H4B 21.2 . . ?
N1 C2 H4C 99.2 . . ?
H2C C2 H4C 118.2 . . ?
H2D C2 H4C 111.0 . . ?
H2E C2 H4C 21.2 . . ?
H4B C2 H4C 0.0 . . ?

_refine_diff_density_max         0.907
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.280

