# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Scott Oliver'
_publ_contact_author_email       SOLIVER@CHEMISTRY.UCSC.EDU

_publ_section_title              
;
A metal-organic framework via the reaction
of benzoate with a cationic inorganic material
;
loop_
_publ_author_name
'Scott Oliver'
'Steven P. Cummings'
'Martin Grysell'
'Allen Oliver'
'David L. Rogow'
;
C.H.Swanson
;
'Dat T. Tran'

# Attachment 'B912874C-Revised_CIF.cif'

data_xsc07010
_database_code_depnum_ccdc_archive 'CCDC 738466'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H12 O5 Pb'
_chemical_formula_sum            'C14 H12 O5 Pb'
_chemical_formula_weight         467.43

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   15.411(2)
_cell_length_b                   7.4635(12)
_cell_length_c                   11.4497(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.279(2)
_cell_angle_gamma                90.00
_cell_volume                     1316.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3874
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      28.37

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    12.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2492
_exptl_absorpt_correction_T_max  0.5663
_exptl_absorpt_process_details   'Sheldrick, 2007'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II'
_diffrn_measurement_method       \w/2\q-scans
_diffrn_detector_area_resol_mean 83.33
_diffrn_reflns_number            12534
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_av_sigmaI/netI    0.0809
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.64
_diffrn_reflns_theta_max         28.61
_reflns_number_total             3294
_reflns_number_gt                2486
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX-II v2.1-4'
_computing_cell_refinement       'Bruker SAINT v7.34A'
_computing_data_reduction        'Bruker SAINT v7.34A'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

Water hydrogens on O1 were located from a difference Fourier map and held
fixed at that location.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3294
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1288
_refine_ls_wR_factor_gt          0.1203
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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 0.52133(2) 0.02291(5) 0.68865(3) 0.01860(14) Uani 1 1 d . . .
O1 O 0.4954(4) 0.3439(9) 0.6041(6) 0.0230(15) Uani 1 1 d . . .
H1 H 0.5373 0.4138 0.5890 0.028 Uiso 1 1 d . . .
H2 H 0.4547 0.3713 0.5561 0.028 Uiso 1 1 d . . .
O11 O 0.3922(4) -0.1812(9) 0.6905(6) 0.0227(15) Uani 1 1 d . . .
O12 O 0.4049(5) -0.0112(8) 0.5351(6) 0.0221(15) Uani 1 1 d . . .
O21 O 0.3653(5) 0.0428(10) 0.9565(6) 0.0263(17) Uani 1 1 d . . .
O22 O 0.4108(4) 0.1940(9) 0.7997(6) 0.0211(15) Uani 1 1 d . . .
C11 C 0.2668(7) -0.1472(12) 0.5635(8) 0.021(2) Uani 1 1 d . . .
C12 C 0.2145(6) -0.2467(13) 0.6378(8) 0.021(2) Uani 1 1 d . . .
H12A H 0.2393 -0.3045 0.7045 0.025 Uiso 1 1 calc R . .
C13 C 0.1267(7) -0.2600(14) 0.6133(9) 0.025(2) Uani 1 1 d . . .
H13A H 0.0912 -0.3258 0.6649 0.031 Uiso 1 1 calc R . .
C14 C 0.0888(7) -0.1799(14) 0.5154(9) 0.029(2) Uani 1 1 d . . .
H14A H 0.0281 -0.1886 0.5005 0.035 Uiso 1 1 calc R . .
C15 C 0.1421(7) -0.0857(15) 0.4390(9) 0.029(2) Uani 1 1 d . . .
H15A H 0.1177 -0.0324 0.3704 0.035 Uiso 1 1 calc R . .
C16 C 0.2297(7) -0.0704(14) 0.4631(9) 0.026(2) Uani 1 1 d . . .
H16A H 0.2654 -0.0068 0.4107 0.031 Uiso 1 1 calc R . .
C17 C 0.3589(6) -0.1128(13) 0.5963(8) 0.020(2) Uani 1 1 d . . .
C21 C 0.2589(7) 0.1484(13) 0.8169(8) 0.022(2) Uani 1 1 d . . .
C22 C 0.1923(6) 0.0668(14) 0.8788(8) 0.020(2) Uani 1 1 d . . .
H22A H 0.2054 0.0001 0.9477 0.025 Uiso 1 1 calc R . .
C23 C 0.1066(7) 0.0842(15) 0.8385(8) 0.026(2) Uani 1 1 d . . .
H23A H 0.0608 0.0323 0.8811 0.031 Uiso 1 1 calc R . .
C24 C 0.0884(7) 0.1774(14) 0.7361(9) 0.028(2) Uani 1 1 d . . .
H24A H 0.0301 0.1874 0.7080 0.034 Uiso 1 1 calc R . .
C25 C 0.1545(7) 0.2555(15) 0.6749(9) 0.029(3) Uani 1 1 d . . .
H25A H 0.1412 0.3211 0.6057 0.035 Uiso 1 1 calc R . .
C26 C 0.2395(7) 0.2395(13) 0.7129(8) 0.023(2) Uani 1 1 d . . .
H26A H 0.2848 0.2901 0.6687 0.028 Uiso 1 1 calc R . .
C27 C 0.3510(6) 0.1267(12) 0.8612(8) 0.017(2) Uani 1 1 d . . .

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
Pb1 0.0247(2) 0.0147(2) 0.01647(19) -0.00065(14) 0.00059(13) -0.00082(15)
O1 0.029(4) 0.022(4) 0.018(3) 0.002(3) -0.008(3) -0.003(3)
O11 0.024(4) 0.024(4) 0.020(4) 0.001(3) -0.005(3) -0.001(3)
O12 0.032(4) 0.016(3) 0.018(3) -0.001(3) -0.004(3) -0.005(3)
O21 0.033(4) 0.030(4) 0.015(3) 0.002(3) 0.002(3) -0.013(3)
O22 0.014(3) 0.021(4) 0.029(4) -0.005(3) 0.006(3) -0.002(3)
C11 0.035(6) 0.009(4) 0.017(5) -0.003(4) 0.000(4) 0.003(4)
C12 0.021(5) 0.025(5) 0.016(5) -0.005(4) 0.000(4) -0.003(4)
C13 0.022(6) 0.030(6) 0.024(5) 0.001(4) 0.001(4) 0.002(5)
C14 0.025(6) 0.033(6) 0.029(6) -0.010(5) -0.004(5) 0.003(5)
C15 0.038(7) 0.030(6) 0.019(5) 0.001(4) -0.013(5) 0.002(5)
C16 0.036(6) 0.022(5) 0.021(5) -0.002(4) 0.001(4) -0.002(5)
C17 0.017(5) 0.021(5) 0.023(5) -0.011(4) -0.003(4) 0.004(4)
C21 0.028(6) 0.023(5) 0.015(5) -0.001(4) 0.004(4) 0.001(4)
C22 0.022(5) 0.023(5) 0.017(5) 0.003(4) 0.002(4) 0.002(4)
C23 0.025(6) 0.034(6) 0.018(5) -0.002(4) 0.003(4) -0.002(5)
C24 0.027(6) 0.032(6) 0.026(5) 0.000(5) 0.004(5) 0.004(5)
C25 0.037(7) 0.037(6) 0.013(5) -0.001(4) -0.008(4) 0.005(5)
C26 0.034(6) 0.021(5) 0.014(5) -0.003(4) 0.008(4) -0.004(4)
C27 0.026(5) 0.012(4) 0.014(4) -0.003(3) 0.002(4) -0.004(4)

_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 O12 2.497(7) . ?
Pb1 O22 2.499(6) . ?
Pb1 O11 2.507(7) . ?
Pb1 O1 2.611(7) . ?
Pb1 O22 2.671(6) 2_646 ?
Pb1 O1 2.740(7) 2_646 ?
O1 Pb1 2.740(7) 2_656 ?
O1 H1 0.8494 . ?
O1 H2 0.8505 . ?
O11 C17 1.289(11) . ?
O12 C17 1.260(12) . ?
O21 C27 1.273(11) . ?
O22 C27 1.275(11) . ?
O22 Pb1 2.671(6) 2_656 ?
C11 C16 1.395(14) . ?
C11 C12 1.398(13) . ?
C11 C17 1.483(14) . ?
C12 C13 1.380(14) . ?
C12 H12A 0.9500 . ?
C13 C14 1.389(14) . ?
C13 H13A 0.9500 . ?
C14 C15 1.402(15) . ?
C14 H14A 0.9500 . ?
C15 C16 1.377(15) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C21 C26 1.398(13) . ?
C21 C22 1.400(13) . ?
C21 C27 1.505(14) . ?
C22 C23 1.396(14) . ?
C22 H22A 0.9500 . ?
C23 C24 1.386(14) . ?
C23 H23A 0.9500 . ?
C24 C25 1.379(15) . ?
C24 H24A 0.9500 . ?
C25 C26 1.377(14) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?

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
O12 Pb1 O22 85.6(2) . . ?
O12 Pb1 O11 52.1(2) . . ?
O22 Pb1 O11 75.9(2) . . ?
O12 Pb1 O1 74.4(2) . . ?
O22 Pb1 O1 67.6(2) . . ?
O11 Pb1 O1 116.5(2) . . ?
O12 Pb1 O22 102.5(2) . 2_646 ?
O22 Pb1 O22 135.63(16) . 2_646 ?
O11 Pb1 O22 75.6(2) . 2_646 ?
O1 Pb1 O22 156.7(2) . 2_646 ?
O12 Pb1 O1 118.7(2) . 2_646 ?
O22 Pb1 O1 74.3(2) . 2_646 ?
O11 Pb1 O1 66.8(2) . 2_646 ?
O1 Pb1 O1 138.73(18) . 2_646 ?
O22 Pb1 O1 63.4(2) 2_646 2_646 ?
Pb1 O1 Pb1 98.2(2) . 2_656 ?
Pb1 O1 H1 121.9 . . ?
Pb1 O1 H1 87.9 2_656 . ?
Pb1 O1 H2 124.4 . . ?
Pb1 O1 H2 111.1 2_656 . ?
H1 O1 H2 105.9 . . ?
C17 O11 Pb1 93.0(6) . . ?
C17 O12 Pb1 94.3(6) . . ?
C27 O22 Pb1 126.1(6) . . ?
C27 O22 Pb1 128.4(6) . 2_656 ?
Pb1 O22 Pb1 103.0(2) . 2_656 ?
C16 C11 C12 119.3(10) . . ?
C16 C11 C17 120.6(9) . . ?
C12 C11 C17 119.9(9) . . ?
C13 C12 C11 119.4(9) . . ?
C13 C12 H12A 120.3 . . ?
C11 C12 H12A 120.3 . . ?
C12 C13 C14 121.7(10) . . ?
C12 C13 H13A 119.1 . . ?
C14 C13 H13A 119.1 . . ?
C13 C14 C15 118.6(10) . . ?
C13 C14 H14A 120.7 . . ?
C15 C14 H14A 120.7 . . ?
C16 C15 C14 120.1(10) . . ?
C16 C15 H15A 120.0 . . ?
C14 C15 H15A 120.0 . . ?
C15 C16 C11 120.8(10) . . ?
C15 C16 H16A 119.6 . . ?
C11 C16 H16A 119.6 . . ?
O12 C17 O11 119.0(9) . . ?
O12 C17 C11 120.7(9) . . ?
O11 C17 C11 120.2(9) . . ?
C26 C21 C22 119.8(10) . . ?
C26 C21 C27 121.5(9) . . ?
C22 C21 C27 118.6(8) . . ?
C23 C22 C21 119.4(9) . . ?
C23 C22 H22A 120.3 . . ?
C21 C22 H22A 120.3 . . ?
C24 C23 C22 119.9(10) . . ?
C24 C23 H23A 120.0 . . ?
C22 C23 H23A 120.0 . . ?
C25 C24 C23 120.3(10) . . ?
C25 C24 H24A 119.9 . . ?
C23 C24 H24A 119.9 . . ?
C26 C25 C24 120.7(10) . . ?
C26 C25 H25A 119.6 . . ?
C24 C25 H25A 119.6 . . ?
C25 C26 C21 119.8(10) . . ?
C25 C26 H26A 120.1 . . ?
C21 C26 H26A 120.1 . . ?
O21 C27 O22 123.7(9) . . ?
O21 C27 C21 119.0(8) . . ?
O22 C27 C21 117.3(8) . . ?

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
O12 Pb1 O1 Pb1 130.4(3) . . . 2_656 ?
O22 Pb1 O1 Pb1 38.8(2) . . . 2_656 ?
O11 Pb1 O1 Pb1 98.8(2) . . . 2_656 ?
O22 Pb1 O1 Pb1 -144.3(4) 2_646 . . 2_656 ?
O1 Pb1 O1 Pb1 14.46(17) 2_646 . . 2_656 ?
O12 Pb1 O11 C17 -7.0(5) . . . . ?
O22 Pb1 O11 C17 88.4(5) . . . . ?
O1 Pb1 O11 C17 32.7(6) . . . . ?
O22 Pb1 O11 C17 -125.9(6) 2_646 . . . ?
O1 Pb1 O11 C17 167.2(6) 2_646 . . . ?
O22 Pb1 O12 C17 -68.3(6) . . . . ?
O11 Pb1 O12 C17 7.2(5) . . . . ?
O1 Pb1 O12 C17 -136.3(6) . . . . ?
O22 Pb1 O12 C17 67.5(6) 2_646 . . . ?
O1 Pb1 O12 C17 1.2(6) 2_646 . . . ?
O12 Pb1 O22 C27 81.3(7) . . . . ?
O11 Pb1 O22 C27 29.3(7) . . . . ?
O1 Pb1 O22 C27 156.2(8) . . . . ?
O22 Pb1 O22 C27 -22.1(7) 2_646 . . . ?
O1 Pb1 O22 C27 -40.2(7) 2_646 . . . ?
O12 Pb1 O22 Pb1 -115.7(2) . . . 2_656 ?
O11 Pb1 O22 Pb1 -167.6(3) . . . 2_656 ?
O1 Pb1 O22 Pb1 -40.7(2) . . . 2_656 ?
O22 Pb1 O22 Pb1 141.0(3) 2_646 . . 2_656 ?
O1 Pb1 O22 Pb1 122.9(3) 2_646 . . 2_656 ?
C16 C11 C12 C13 -3.0(14) . . . . ?
C17 C11 C12 C13 172.4(9) . . . . ?
C11 C12 C13 C14 1.2(15) . . . . ?
C12 C13 C14 C15 1.1(16) . . . . ?
C13 C14 C15 C16 -1.6(16) . . . . ?
C14 C15 C16 C11 -0.2(16) . . . . ?
C12 C11 C16 C15 2.5(15) . . . . ?
C17 C11 C16 C15 -172.9(9) . . . . ?
Pb1 O12 C17 O11 -12.7(9) . . . . ?
Pb1 O12 C17 C11 164.7(8) . . . . ?
Pb1 O11 C17 O12 12.7(9) . . . . ?
Pb1 O11 C17 C11 -164.7(7) . . . . ?
C16 C11 C17 O12 1.2(14) . . . . ?
C12 C11 C17 O12 -174.1(9) . . . . ?
C16 C11 C17 O11 178.6(9) . . . . ?
C12 C11 C17 O11 3.2(14) . . . . ?
C26 C21 C22 C23 -2.8(15) . . . . ?
C27 C21 C22 C23 -179.5(9) . . . . ?
C21 C22 C23 C24 1.8(15) . . . . ?
C22 C23 C24 C25 -1.1(16) . . . . ?
C23 C24 C25 C26 1.3(16) . . . . ?
C24 C25 C26 C21 -2.2(16) . . . . ?
C22 C21 C26 C25 3.0(15) . . . . ?
C27 C21 C26 C25 179.6(9) . . . . ?
Pb1 O22 C27 O21 68.4(11) . . . . ?
Pb1 O22 C27 O21 -90.4(10) 2_656 . . . ?
Pb1 O22 C27 C21 -111.4(8) . . . . ?
Pb1 O22 C27 C21 89.9(9) 2_656 . . . ?
C26 C21 C27 O21 179.9(9) . . . . ?
C22 C21 C27 O21 -3.5(13) . . . . ?
C26 C21 C27 O22 -0.4(13) . . . . ?
C22 C21 C27 O22 176.2(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O21 0.85 1.87 2.713(10) 172.4 2_656
O1 H1 O22 0.85 2.57 3.171(9) 128.9 2_656
O1 H2 O21 0.85 1.88 2.728(10) 173.8 4_565

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        28.61
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         2.514
_refine_diff_density_min         -4.286
_refine_diff_density_rms         0.348