# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2018

####################################################################### 
# 
# 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_CAUMOF-19
_database_code_depnum_ccdc_archive 'CCDC 1827791'
_audit_update_record             
;
2018-03-06 deposited with the CCDC.
2018-04-03 downloaded from the CCDC.
;
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C7  H3  N  O4  Pb'
_chemical_formula_sum            'C7  H3  N  O4  Pb'
_chemical_formula_weight         372.29

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.8218(2)
_cell_length_b                   5.5427(10)
_cell_length_c                   14.3601(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.993(10)
_cell_angle_gamma                90
_cell_volume                     755.14(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296.0(2)
_cell_measurement_reflns_used    1928
_cell_measurement_theta_min      2.266
_cell_measurement_theta_max      28.211
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       rod
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.034
_exptl_crystal_density_diffrn    3.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             664
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    22.317
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   
; 
 SADABS(Blessing, 1995) 
;
_exptl_absorpt_correction_T_min  0.5617
_exptl_absorpt_correction_T_max  0.7457

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      296.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       CCD
_diffrn_measurement_device_type  'Bruker SMART BREEZE'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_number            17404
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.266
_diffrn_reflns_theta_max         28.211
_diffrn_reflns_theta_full        28.211
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_reflns_number_total             1842
_reflns_number_gt                1693
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  SHELXL-97

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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)+(0.0352P)²+2.8361P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0117(5)
_refine_ls_number_reflns         1842
_refine_ls_number_parameters     119
_refine_ls_number_restraints     1
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.024
_refine_ls_wR_factor_ref         0.0679
_refine_ls_wR_factor_gt          0.0663
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_restrained_S_all      1.137
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         3.021
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.229

#----------------------------------------------------------------------------#
#                   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
C1 C 0.5266(5) 0.1831(9) 0.8190(4) 0.0183(10) Uani 1 d . .
C2 C 0.3938(6) 0.1051(10) 0.8228(4) 0.0251(11) Uani 1 d . .
H2 H 0.3136 0.1902 0.791 0.03 Uiso 1 calc . .
C3 C 0.3828(6) -0.1014(12) 0.8746(4) 0.0283(13) Uani 1 d . .
H3 H 0.2951 -0.1563 0.879 0.034 Uiso 1 calc . .
C4 C 0.5042(7) -0.2246(10) 0.9197(4) 0.0260(12) Uani 1 d . .
H4 H 0.499 -0.3675 0.9525 0.031 Uiso 1 calc . .
C5 C 0.6332(5) -0.1335(9) 0.9156(4) 0.0200(10) Uani 1 d . .
C6 C 0.5467(5) 0.3939(9) 0.7580(4) 0.0199(10) Uani 1 d . .
C7 C 0.7715(7) -0.2589(9) 0.9628(4) 0.0222(12) Uani 1 d . .
N1 N 0.6444(4) 0.0702(7) 0.8679(3) 0.0163(8) Uani 1 d . .
O1 O 0.6723(4) 0.4592(7) 0.7623(3) 0.0239(8) Uani 1 d . .
O2 O 0.4417(4) 0.4895(8) 0.7036(3) 0.0362(11) Uani 1 d . .
O3 O 0.7653(5) -0.4608(8) 0.9980(3) 0.0355(10) Uani 1 d . .
O4 O 0.8836(4) -0.1482(8) 0.9615(3) 0.0299(9) Uani 1 d . .
Pb1 Pb 0.88436(2) 0.23235(4) 0.88148(2) 0.01793(12) 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
C1 N1 1.343(6) . ?
C1 C2 1.388(7) . ?
C1 C6 1.504(7) . ?
C2 C3 1.385(8) . ?
C3 C4 1.381(9) . ?
C4 C5 1.380(8) . ?
C5 N1 1.340(6) . ?
C5 C7 1.520(8) . ?
C6 O2 1.241(6) . ?
C6 O1 1.272(6) . ?
C7 O3 1.236(6) . ?
C7 O4 1.265(7) . ?
N1 Pb1 2.483(4) . ?
O1 Pb1 2.504(4) 2_656 ?
O1 Pb1 2.646(4) . ?
O2 Pb1 2.702(4) 2_656 ?
O4 Pb1 2.403(4) . ?
Pb1 O1 2.504(4) 2_646 ?
Pb1 O2 2.702(4) 2_646 ?

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
N1 C1 C2 121.7(5) . . ?
N1 C1 C6 116.2(4) . . ?
C2 C1 C6 122.1(5) . . ?
C3 C2 C1 118.9(5) . . ?
C4 C3 C2 118.8(5) . . ?
C5 C4 C3 119.4(5) . . ?
N1 C5 C4 121.8(5) . . ?
N1 C5 C7 115.6(4) . . ?
C4 C5 C7 122.6(5) . . ?
O2 C6 O1 123.1(5) . . ?
O2 C6 C1 119.1(5) . . ?
O1 C6 C1 117.7(4) . . ?
O3 C7 O4 125.5(6) . . ?
O3 C7 C5 117.6(5) . . ?
O4 C7 C5 116.9(4) . . ?
C5 N1 C1 119.1(4) . . ?
C5 N1 Pb1 117.8(3) . . ?
C1 N1 Pb1 123.0(3) . . ?
C6 O1 Pb1 97.3(3) . 2_656 ?
C6 O1 Pb1 119.2(3) . . ?
Pb1 O1 Pb1 142.22(16) 2_656 . ?
C6 O2 Pb1 88.7(3) . 2_656 ?
C7 O4 Pb1 122.9(3) . . ?
O4 Pb1 N1 66.38(14) . . ?
O4 Pb1 O1 80.55(14) . 2_646 ?
N1 Pb1 O1 73.27(13) . 2_646 ?
O4 Pb1 O1 128.82(13) . . ?
N1 Pb1 O1 63.18(13) . . ?
O1 Pb1 O1 77.53(7) 2_646 . ?
O4 Pb1 O2 81.92(15) . 2_646 ?
N1 Pb1 O2 118.86(13) . 2_646 ?
O1 Pb1 O2 50.05(12) 2_646 2_646 ?
O1 Pb1 O2 115.35(13) . 2_646 ?
