# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_daifn-6-twin
_database_code_depnum_ccdc_archive 'CCDC 1539224'
_audit_update_record             
;
2017-03-21 deposited with the CCDC.
2017-04-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H25 Cl N O5 Pb1.50'
_chemical_formula_weight         705.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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           tetragonal
_symmetry_space_group_name_H-M   'I 4/m'

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

_cell_length_a                   33.2401(4)
_cell_length_b                   33.2401(4)
_cell_length_c                   5.88940(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6507.22(16)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9823
_cell_measurement_theta_min      3.76
_cell_measurement_theta_max      67.03

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2656
_exptl_absorpt_coefficient_mu    15.914
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.0352
_exptl_absorpt_correction_T_max  0.2510
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Gemini CCD'
_diffrn_measurement_method       'ω & π scans'
_diffrn_detector_area_resol_mean none
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            9614
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.76
_diffrn_reflns_theta_max         67.03
_reflns_number_total             3199
_reflns_number_gt                2893
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.
 During the final refinement, the crystal data were modelled by the PLATON SQUEEZE,Based on the elemental analysis and the TG curve, indicating that there were at least 16 DMA molecules in 8 similar voids of the structure, which were not included in the final molecular formula. 
 During the refinement of complex, the restraint command 'ISOR'and 'DELU' is used to testrain the C atoms with NPD and ADP problems. These atoms are as follows: C10 C11 C10' C11'.
 During the refinement of complex, the -NH2 group on the ligand can not be located due to the symmetry and disorder, but it is included in the final molecular formula, which lead to the calculated and Reported Mol. Weight Differ and  Density Dx Differ. 
;

_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)+(0.1088P)²+455.2567P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.000143(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3199
_refine_ls_number_parameters     185
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0899
_refine_ls_wR_factor_ref         0.2537
_refine_ls_wR_factor_gt          0.2504
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.001
_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
Pb1 Pb 0.474357(12) 0.070772(12) 0.0000 0.03305(12) Uani 1 2 d S . .
Pb2 Pb 0.48168(6) 0.13923(5) 0.5000 0.0846(5) Uani 0.50 2 d SP . .
Cl1 Cl 0.47620(7) 0.05185(8) -0.5000 0.0320(6) Uani 1 2 d S . .
O3 O 0.4866(7) 0.2204(9) 0.5000 0.190(12) Uani 1 2 d S . .
O1 O 0.5265(2) 0.11686(19) 0.1837(15) 0.068(2) Uani 1 1 d . . .
O2 O 0.4366(2) 0.13042(19) 0.1843(12) 0.0595(19) Uani 1 1 d . . .
C1 C 0.5400(4) 0.1290(4) 0.0000 0.045(4) Uani 1 2 d S . .
C2 C 0.5730(3) 0.1588(4) 0.0000 0.036(3) Uani 1 2 d S . .
C5 C 0.6339(5) 0.2184(4) 0.0000 0.052(4) Uani 1 2 d S . .
C6 C 0.6648(5) 0.2500(5) 0.0000 0.072(6) Uani 1 2 d S . .
C7 C 0.4244(3) 0.1445(3) 0.0000 0.035(3) Uani 1 2 d S . .
C8 C 0.3959(4) 0.1791(4) 0.0000 0.044(4) Uani 1 2 d S . .
C11 C 0.3421(5) 0.2411(5) 0.0000 0.063(3) Uani 1 2 d SU . .
C12 C 0.7248(4) 0.3106(5) 0.0000 0.073(6) Uani 1 2 d S . .
C3 C 0.5987(5) 0.1614(6) -0.222(4) 0.053(6) Uani 0.50 1 d P A 1
C4 C 0.6285(6) 0.1930(5) -0.211(3) 0.043(5) Uani 0.50 1 d P A 1
C9 C 0.3930(5) 0.2021(6) 0.162(3) 0.046(5) Uani 0.50 1 d P . 1
C10 C 0.3663(6) 0.2356(6) 0.165(4) 0.054(3) Uani 0.50 1 d PU . 1
C13 C 0.7016(9) 0.3074(9) 0.220(6) 0.097(9) Uiso 0.50 1 d P . 1
C14 C 0.6683(9) 0.2741(7) 0.205(4) 0.104(8) Uani 0.50 1 d P . 1
C3' C 0.5786(7) 0.1828(7) -0.164(5) 0.084(7) Uani 0.50 1 d P . 2
C4' C 0.6064(7) 0.2155(7) -0.157(3) 0.069(6) Uani 0.50 1 d P . 2
C9' C 0.3719(6) 0.1839(6) 0.189(5) 0.062(6) Uani 0.50 1 d P . 2
C10' C 0.3432(6) 0.2150(6) 0.210(4) 0.060(4) Uani 0.50 1 d PU . 2
C13' C 0.7271(9) 0.2799(9) 0.153(6) 0.090(8) Uiso 0.50 1 d P . 2
C14' C 0.6935(9) 0.2485(9) 0.140(6) 0.094(9) Uiso 0.50 1 d P . 2


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 2.554(7) . ?
Pb1 O1 2.554(7) 11 ?
Pb1 O2 2.585(6) . ?
Pb1 O2 2.585(6) 11 ?
Pb1 Cl1 3.0117(6) 1_556 ?
Pb1 Cl1 3.0117(6) . ?
Pb1 Cl1 3.012(3) 14_554 ?
Pb2 O2 2.406(7) . ?
Pb2 O2 2.406(7) 11_556 ?
Pb2 O1 2.499(8) 11_556 ?
Pb2 O1 2.499(8) . ?
Pb2 O3 2.70(3) . ?
Pb2 Cl1 2.910(3) 1_556 ?
Cl1 Pb2 2.910(3) 1_554 ?
Cl1 Pb1 3.0117(6) 1_554 ?
Cl1 Pb1 3.012(3) 6_544 ?
O1 C1 1.239(10) . ?
O2 C7 1.250(9) . ?
C1 O1 1.239(10) 11 ?
C1 C2 1.477(17) . ?
C2 C3' 1.27(3) . ?
C2 C3' 1.27(3) 11 ?
C2 C3 1.56(2) 11 ?
C2 C3 1.56(2) . ?
C5 C4' 1.31(2) . ?
C5 C4' 1.31(2) 11 ?
C5 C6 1.47(2) . ?
C5 C4 1.512(19) 11 ?
C5 C4 1.512(19) . ?
C6 C14' 1.26(3) . ?
C6 C14' 1.26(3) 11 ?
C6 C14 1.46(2) . ?
C6 C14 1.46(2) 11 ?
C7 O2 1.250(9) 11 ?
C7 C8 1.490(16) . ?
C8 C9 1.23(2) . ?
C8 C9 1.23(2) 11 ?
C8 C9' 1.38(3) 11 ?
C8 C9' 1.38(3) . ?
C11 C10 1.27(2) 11 ?
C11 C10 1.27(2) . ?
C11 C10' 1.51(3) 11 ?
C11 C10' 1.51(3) . ?
C11 C12 1.54(2) 10_565 ?
C12 C13' 1.36(3) 11 ?
C12 C13' 1.36(3) . ?
C12 C13 1.51(4) 11 ?
C12 C13 1.51(4) . ?
C12 C11 1.54(2) 2_655 ?
C3 C4 1.45(3) . ?
C9 C10 1.42(3) . ?
C9 C9 1.91(4) 11 ?
C10 C10 1.94(5) 11 ?
C13 C14 1.56(4) . ?
C3' C4' 1.43(3) . ?
C3' C3' 1.94(6) 11 ?
C4' C4' 1.85(4) 11 ?
C9' C10' 1.41(3) . ?
C13' C14' 1.53(4) . ?
C13' C13' 1.81(7) 11 ?
C14' C14' 1.65(7) 11 ?

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
O1 Pb1 O1 50.1(4) . 11 ?
O1 Pb1 O2 72.1(2) . . ?
O1 Pb1 O2 92.7(2) 11 . ?
O1 Pb1 O2 92.7(2) . 11 ?
O1 Pb1 O2 72.1(2) 11 11 ?
O2 Pb1 O2 49.7(3) . 11 ?
O1 Pb1 Cl1 72.4(2) . 1_556 ?
O1 Pb1 Cl1 121.70(19) 11 1_556 ?
O2 Pb1 Cl1 76.08(16) . 1_556 ?
O2 Pb1 Cl1 125.49(16) 11 1_556 ?
O1 Pb1 Cl1 121.70(19) . . ?
O1 Pb1 Cl1 72.4(2) 11 . ?
O2 Pb1 Cl1 125.49(16) . . ?
O2 Pb1 Cl1 76.08(16) 11 . ?
Cl1 Pb1 Cl1 155.78(10) 1_556 . ?
O1 Pb1 Cl1 74.35(16) . 14_554 ?
O1 Pb1 Cl1 74.35(16) 11 14_554 ?
O2 Pb1 Cl1 144.35(16) . 14_554 ?
O2 Pb1 Cl1 144.35(16) 11 14_554 ?
Cl1 Pb1 Cl1 82.78(6) 1_556 14_554 ?
Cl1 Pb1 Cl1 82.78(6) . 14_554 ?
O2 Pb2 O2 101.2(3) . 11_556 ?
O2 Pb2 O1 155.7(2) . 11_556 ?
O2 Pb2 O1 76.1(2) 11_556 11_556 ?
O2 Pb2 O1 76.1(2) . . ?
O2 Pb2 O1 155.7(2) 11_556 . ?
O1 Pb2 O1 96.4(4) 11_556 . ?
O2 Pb2 O3 99.2(3) . . ?
O2 Pb2 O3 99.2(3) 11_556 . ?
O1 Pb2 O3 105.1(3) 11_556 . ?
O1 Pb2 O3 105.1(3) . . ?
O2 Pb2 Cl1 80.77(16) . 1_556 ?
O2 Pb2 Cl1 80.77(16) 11_556 1_556 ?
O1 Pb2 Cl1 74.95(16) 11_556 1_556 ?
O1 Pb2 Cl1 74.95(16) . 1_556 ?
O3 Pb2 Cl1 179.9(5) . 1_556 ?
Pb2 Cl1 Pb1 78.05(5) 1_554 . ?
Pb2 Cl1 Pb1 78.05(5) 1_554 1_554 ?
Pb1 Cl1 Pb1 155.78(10) . 1_554 ?
Pb2 Cl1 Pb1 152.36(10) 1_554 6_544 ?
Pb1 Cl1 Pb1 99.67(5) . 6_544 ?
Pb1 Cl1 Pb1 99.67(5) 1_554 6_544 ?
C1 O1 Pb2 140.4(7) . . ?
C1 O1 Pb1 94.1(6) . . ?
Pb2 O1 Pb1 95.1(2) . . ?
C7 O2 Pb2 145.8(7) . . ?
C7 O2 Pb1 94.6(6) . . ?
Pb2 O2 Pb1 96.6(2) . . ?
O1 C1 O1 121.7(12) 11 . ?
O1 C1 C2 119.2(6) 11 . ?
O1 C1 C2 119.2(6) . . ?
C3' C2 C3' 100(2) . 11 ?
C3' C2 C1 121.9(12) . . ?
C3' C2 C1 121.9(12) 11 . ?
C3' C2 C3 121.6(15) . 11 ?
C3' C2 C3 41.2(13) 11 11 ?
C1 C2 C3 116.3(9) . 11 ?
C3' C2 C3 41.2(13) . . ?
C3' C2 C3 121.6(15) 11 . ?
C1 C2 C3 116.3(9) . . ?
C3 C2 C3 113.3(16) 11 . ?
C4' C5 C4' 90(2) . 11 ?
C4' C5 C6 122.8(12) . . ?
C4' C5 C6 122.8(12) 11 . ?
C4' C5 C4 117.3(15) . 11 ?
C4' C5 C4 45.0(12) 11 11 ?
C6 C5 C4 118.8(9) . 11 ?
C4' C5 C4 45.0(12) . . ?
C4' C5 C4 117.3(15) 11 . ?
C6 C5 C4 118.8(9) . . ?
C4 C5 C4 110.4(16) 11 . ?
C14' C6 C14' 82(3) . 11 ?
C14' C6 C14 54.4(18) . . ?
C14' C6 C14 120(2) 11 . ?
C14' C6 C14 120(2) . 11 ?
C14' C6 C14 54.4(18) 11 11 ?
C14 C6 C14 112(2) . 11 ?
C14' C6 C5 120.0(18) . . ?
C14' C6 C5 120.0(18) 11 . ?
C14 C6 C5 116.8(12) . . ?
C14 C6 C5 116.8(12) 11 . ?
O2 C7 O2 120.5(10) 11 . ?
O2 C7 C8 119.7(5) 11 . ?
O2 C7 C8 119.7(5) . . ?
C9 C8 C9 102(2) . 11 ?
C9 C8 C9' 120.8(15) . 11 ?
C9 C8 C9' 41.8(12) 11 11 ?
C9 C8 C9' 41.8(12) . . ?
C9 C8 C9' 120.8(15) 11 . ?
C9' C8 C9' 108(2) 11 . ?
C9 C8 C7 122.1(10) . . ?
C9 C8 C7 122.1(10) 11 . ?
C9' C8 C7 117.1(11) 11 . ?
C9' C8 C7 117.1(11) . . ?
C10 C11 C10 99(2) 11 . ?
C10 C11 C10' 43.7(12) 11 11 ?
C10 C11 C10' 121.5(17) . 11 ?
C10 C11 C10' 121.5(17) 11 . ?
C10 C11 C10' 43.7(12) . . ?
C10' C11 C10' 110(2) 11 . ?
C10 C11 C12 122.4(12) 11 10_565 ?
C10 C11 C12 122.4(12) . 10_565 ?
C10' C11 C12 116.1(11) 11 10_565 ?
C10' C11 C12 116.1(11) . 10_565 ?
C13' C12 C13' 83(3) 11 . ?
C13' C12 C13 53.7(17) 11 11 ?
C13' C12 C13 123(2) . 11 ?
C13' C12 C13 123(2) 11 . ?
C13' C12 C13 53.7(17) . . ?
C13 C12 C13 118(3) 11 . ?
C13' C12 C11 117.9(16) 11 2_655 ?
C13' C12 C11 117.9(16) . 2_655 ?
C13 C12 C11 115.1(14) 11 2_655 ?
C13 C12 C11 115.1(14) . 2_655 ?
C4 C3 C2 112.2(17) . . ?
C3 C4 C5 121.5(16) . . ?
C8 C9 C10 123.0(18) . . ?
C8 C9 C9 38.9(10) . 11 ?
C10 C9 C9 90.6(12) . 11 ?
C11 C10 C9 120.0(19) . . ?
C11 C10 C10 40.5(11) . 11 ?
C9 C10 C10 89.4(12) . 11 ?
C12 C13 C14 111(2) . . ?
C6 C14 C13 120(2) . . ?
C2 C3' C4' 123(2) . . ?
C2 C3' C3' 40.2(12) . 11 ?
C4' C3' C3' 88.3(14) . 11 ?
C5 C4' C3' 122(2) . . ?
C5 C4' C4' 44.8(10) . 11 ?
C3' C4' C4' 91.7(14) . 11 ?
C8 C9' C10' 123(2) . . ?
C9' C10' C11 112(2) . . ?
C12 C13' C14' 116(3) . . ?
C12 C13' C13' 48.6(14) . 11 ?
C14' C13' C13' 87.0(18) . 11 ?
C6 C14' C13' 124(3) . . ?
C6 C14' C14' 49.2(16) . 11 ?
C13' C14' C14' 93.0(18) . 11 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        67.03
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         3.167
_refine_diff_density_min         -4.187
_refine_diff_density_rms         0.311
