# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_Pb3(Kemp)2(DMF)3
_database_code_depnum_ccdc_archive 'CCDC 1409438'
_audit_update_record             
;
2015-06-29 deposited with the CCDC.
2015-07-15 downloaded from the CCDC.
;

#----------------------------------------------------------------------------#

#                   CHEMICAL INFORMATION                                     #

#----------------------------------------------------------------------------#



_chemical_formula_moiety         'C11  H17  N  O5  Pb'

_chemical_formula_sum            'C11  H17  N  O5  Pb'

_chemical_formula_weight         450.46



#----------------------------------------------------------------------------#

#                   UNIT CELL INFORMATION                                    #

#----------------------------------------------------------------------------#

loop_

_symmetry_equiv_pos_as_xyz


















'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'



_symmetry_cell_setting           trigonal

_symmetry_space_group_name_H-M   'R -3'

_cell_length_a                   14.4445(6)

_cell_length_b                   14.4445(6)

_cell_length_c                   34.0453(10)

_cell_angle_alpha                90

_cell_angle_beta                 90

_cell_angle_gamma                120

_cell_volume                     6151.7(6)

_cell_formula_units_Z            18

_cell_measurement_temperature    173.0(2)



#----------------------------------------------------------------------------#

#                   CRYSTAL INFORMATION                                      #

#----------------------------------------------------------------------------#



_exptl_crystal_density_diffrn    2.189

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             3816

_exptl_crystal_description       Block

_exptl_crystal_colour            Colorless

_exptl_crystal_size_max          0.075

_exptl_crystal_size_mid          0.027

_exptl_crystal_size_min          0.014

_exptl_special_details           
;

 ?

;

#----------------------------------------------------------------------------#

#                   ABSORPTION CORRECTION                                    #

#----------------------------------------------------------------------------#



_exptl_absorpt_coefficient_mu    12.353

_exptl_absorpt_correction_type   EMPIRICAL

_exptl_absorpt_process_details   
; 

 SADABS(Blessing, 1995) 

;

_exptl_absorpt_correction_T_min  0.67

_exptl_absorpt_correction_T_max  0.84



#----------------------------------------------------------------------------#

#                   DATA COLLECTION                                          #

#----------------------------------------------------------------------------#



_diffrn_measurement_device_type  'Bruker SMART BREEZE'

_diffrn_measurement_method       CCD

_diffrn_ambient_temperature      173.0(2)

_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_type           MoK\a

_diffrn_radiation_monochromator  graphite

_diffrn_reflns_av_R_equivalents  0.1255

_diffrn_reflns_number            23965

_diffrn_reflns_limit_h_min       -18

_diffrn_reflns_limit_h_max       19

_diffrn_reflns_limit_k_min       -19

_diffrn_reflns_limit_k_max       19

_diffrn_reflns_limit_l_min       -43

_diffrn_reflns_limit_l_max       45

_diffrn_reflns_theta_min         1.734

_diffrn_reflns_theta_max         28.35

_diffrn_reflns_theta_full        25.242

_diffrn_measured_fraction_theta_full 
1

_diffrn_measured_fraction_theta_max 
0.996

_diffrn_reflns_Laue_measured_fraction_full 
1

_diffrn_reflns_Laue_measured_fraction_max 
0.996

_diffrn_reflns_point_group_measured_fraction_full 
1

_diffrn_reflns_point_group_measured_fraction_max 
0.996

_reflns_number_total             3412

_reflns_number_gt                1560

_reflns_threshold_expression     'I > 2σ(I)'



#----------------------------------------------------------------------------#

#                   COMPUTER PROGRAMS USED                                   #

#----------------------------------------------------------------------------#



_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'



#----------------------------------------------------------------------------#

#                   STRUCTURE SOLUTION

#----------------------------------------------------------------------------#



_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom



#----------------------------------------------------------------------------#

#                   REFINEMENT INFORMATION                                   #

#----------------------------------------------------------------------------#

_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)+(0.0001P)²] where P=(Fo²+2Fc²)/3'

_refine_ls_extinction_method     SHELXL

_refine_ls_extinction_expression 
Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^

_refine_ls_number_reflns         3412

_refine_ls_number_parameters     168

_refine_ls_number_restraints     0

_refine_ls_number_constraints    0

_refine_ls_R_factor_all          0.1398

_refine_ls_R_factor_gt           0.0465

_refine_ls_wR_factor_ref         0.0778

_refine_ls_wR_factor_gt          0.0625

_refine_ls_goodness_of_fit_ref   0.771

_refine_ls_restrained_S_all      0.771

_refine_ls_shift/su_max          0.001

_refine_ls_shift/su_mean         0

_refine_diff_density_max         2.013

_refine_diff_density_min         -1.604

_refine_diff_density_rms         0.253



#----------------------------------------------------------------------------#

#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #

#----------------------------------------------------------------------------#



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 0 '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 0.006 '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'



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_calc_flag

_atom_site_disorder_assembly

_atom_site_disorder_group



































Pb1 Pb 0.07562(3) 0.40049(3) 0.15531(2) 0.02740(13) Uani 1 d . .
O1 O 0.1179(6) 0.2560(5) 0.1740(2) 0.037(2) Uani 1 d . .
O2 O -0.0152(7) 0.2517(6) 0.2063(2) 0.054(2) Uani 1 d . .
O3 O 0.0993(5) 0.5324(5) 0.2169(2) 0.0279(18) Uani 1 d . .
O4 O 0.1614(6) 0.5996(6) 0.1280(2) 0.041(2) Uani 1 d . .
C1 C 0.0475(8) 0.2156(8) 0.2002(3) 0.026(3) Uani 1 d . .
C2 C 0.0287(8) 0.1156(8) 0.2238(3) 0.023(2) Uani 1 d . .
C3 C -0.0864(8) 0.0253(7) 0.2123(3) 0.028(3) Uani 1 d . .
H3A H -0.1376 0.0416 0.2242 0.033 Uiso 1 calc . .
H3B H -0.0941 0.0272 0.184 0.033 Uiso 1 calc . .
C4 C 0.0386(9) 0.1491(8) 0.2653(3) 0.041(3) Uani 1 d . .
H4A H -0.0157 0.1669 0.2713 0.061 Uiso 1 calc . .
H4B H 0.0299 0.0917 0.282 0.061 Uiso 1 calc . .
H4C H 0.1078 0.2105 0.2696 0.061 Uiso 1 calc . .
C5 C 0.1842(9) 0.5330(7) 0.2273(3) 0.028(3) Uani 1 d . .
C6 C 0.2236(8) 0.5665(8) 0.2690(3) 0.025(3) Uani 1 d . .
C7 C 0.1297(8) 0.4803(8) 0.2944(3) 0.039(3) Uani 1 d . .
H7A H 0.1472 0.4946 0.3217 0.059 Uiso 1 calc . .
H7B H 0.0657 0.4826 0.289 0.059 Uiso 1 calc . .
H7C H 0.1186 0.4107 0.288 0.059 Uiso 1 calc . .
C8 C 0.2359(8) 0.6762(8) 0.2799(3) 0.030(3) Uani 1 d . .
H8A H 0.1787 0.6817 0.2671 0.036 Uiso 1 calc . .
H8B H 0.2256 0.6772 0.308 0.036 Uiso 1 calc . .
C11 C -0.0774(11) 0.1707(13) 0.1030(5) 0.059(4) Uani 1 d . .
N1 N -0.1228(8) 0.0971(8) 0.0749(3) 0.043(3) Uani 1 d . .
C9 C -0.1262(11) 0.1245(10) 0.0351(4) 0.075(5) Uani 1 d . .
H9A H -0.162 0.0606 0.0196 0.113 Uiso 1 calc . .
H9B H -0.1642 0.1631 0.0333 0.113 Uiso 1 calc . .
H9C H -0.0546 0.1685 0.0255 0.113 Uiso 1 calc . .
C10 C -0.1829(10) -0.0138(10) 0.0863(5) 0.077(5) Uani 1 d . .
H10A H -0.2108 -0.0575 0.0632 0.115 Uiso 1 calc . .
H10B H -0.137 -0.033 0.1001 0.115 Uiso 1 calc . .
H10C H -0.2409 -0.0247 0.1031 0.115 Uiso 1 calc . .
H11 H -0.076(11) 0.162(11) 0.137(5) 0.11(6) Uiso 1 d . .
O5 O -0.0267(7) 0.2694(8) 0.0958(3) 0.071(3) Uani 1 d . .








#----------------------------------------------------------------------------#

#                   MOLECULAR GEOMETRY                                       #

#----------------------------------------------------------------------------#



_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 O3 2.473(7) 15 ?
Pb1 O1 2.532(7) . ?
Pb1 O2 2.556(7) . ?
Pb1 O4 2.573(7) 15 ?
Pb1 O5 2.659(9) . ?
Pb1 O4 2.666(7) . ?
Pb1 O3 2.738(7) . ?
O1 C1 1.256(12) . ?
O2 C1 1.266(12) . ?
O3 C5 1.272(11) . ?
O3 Pb1 2.473(7) 14_455 ?
O4 C5 1.277(12) 14_455 ?
O4 Pb1 2.573(7) 14_455 ?
C1 C2 1.553(14) . ?
C2 C4 1.479(14) . ?
C2 C3 1.509(13) 3 ?
C2 C3 1.566(13) . ?
C3 C2 1.509(13) 2 ?
C5 O4 1.276(12) 15 ?
C5 C6 1.516(15) . ?
C6 C8 1.544(13) 2_665 ?
C6 C8 1.548(13) . ?
C6 C7 1.564(13) . ?
C8 C6 1.544(13) 3_565 ?
C11 O5 1.260(16) . ?
C11 N1 1.332(16) . ?
N1 C9 1.419(15) . ?
N1 C10 1.442(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






















































O3 Pb1 O1 73.1(2) 15 . ?
O3 Pb1 O2 124.0(2) 15 . ?
O1 Pb1 O2 50.9(2) . . ?
O3 Pb1 O4 77.8(2) 15 15 ?
O1 Pb1 O4 76.9(2) . 15 ?
O2 Pb1 O4 86.5(3) . 15 ?
O3 Pb1 O5 81.8(3) 15 . ?
O1 Pb1 O5 83.2(3) . . ?
O2 Pb1 O5 92.8(3) . . ?
O4 Pb1 O5 154.8(2) 15 . ?
O3 Pb1 O4 73.9(2) 15 . ?
O1 Pb1 O4 143.5(2) . . ?
O2 Pb1 O4 155.6(3) . . ?
O4 Pb1 O4 81.2(4) 15 . ?
O5 Pb1 O4 107.2(3) . . ?
O3 Pb1 O3 119.8(3) 15 . ?
O1 Pb1 O3 112.6(2) . . ?
O2 Pb1 O3 84.2(2) . . ?
O4 Pb1 O3 49.4(2) 15 . ?
O5 Pb1 O3 155.6(2) . . ?
O4 Pb1 O3 71.8(2) . . ?
C1 O1 Pb1 95.0(6) . . ?
C1 O2 Pb1 93.6(6) . . ?
C5 O3 Pb1 132.7(6) . 14_455 ?
C5 O3 Pb1 90.1(6) . . ?
Pb1 O3 Pb1 95.6(2) 14_455 . ?
C5 O4 Pb1 97.7(6) 14_455 14_455 ?
C5 O4 Pb1 164.4(8) 14_455 . ?
Pb1 O4 Pb1 95.0(2) 14_455 . ?
O1 C1 O2 120.3(10) . . ?
O1 C1 C2 121.5(9) . . ?
O2 C1 C2 118.0(9) . . ?
C4 C2 C3 112.4(9) . 3 ?
C4 C2 C1 104.2(8) . . ?
C3 C2 C1 109.4(9) 3 . ?
C4 C2 C3 113.6(9) . . ?
C3 C2 C3 111.3(10) 3 . ?
C1 C2 C3 105.3(8) . . ?
C2 C3 C2 116.1(10) 2 . ?
O3 C5 O4 121.6(11) . 15 ?
O3 C5 C6 118.1(10) . . ?
O4 C5 C6 119.8(10) 15 . ?
C5 C6 C8 114.7(9) . 2_665 ?
C5 C6 C8 112.4(9) . . ?
C8 C6 C8 112.1(10) 2_665 . ?
C5 C6 C7 103.0(8) . . ?
C8 C6 C7 106.6(8) 2_665 . ?
C8 C6 C7 107.1(8) . . ?
C6 C8 C6 116.8(10) 3_565 . ?
O5 C11 N1 122.6(16) . . ?
C11 N1 C9 122.3(13) . . ?
C11 N1 C10 118.5(13) . . ?
C9 N1 C10 118.7(11) . . ?
C11 O5 Pb1 117.4(10) . . ?

#===END









