Electronic Supplementary Material for CrystEngComm
This Journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350

_publ_section_title              
;Structure of a lead urate complex and its effect on
the nucleation of monosodium urate monohydrate
;
_publ_contact_author_name        'Jennifer Swift'
_publ_contact_author_email       JAS2@GEORGETOWN.EDU
loop_
_publ_author_name
J.Swift
M.J.Carroll
A.A.Sargeant
S.Sattar

# Attachment 'pbu_final.cif'

data_pbu
_database_code_depnum_ccdc_archive 'CCDC 657248'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H8 N8 O7 Pb'
_chemical_formula_sum            'C10 H8 N8 O7 Pb'
_chemical_formula_weight         559.43

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.7881(14)
_cell_length_b                   8.4503(15)
_cell_length_c                   11.744(2)
_cell_angle_alpha                86.875(14)
_cell_angle_beta                 86.256(15)
_cell_angle_gamma                88.459(15)
_cell_volume                     671.0(2)
_cell_formula_units_Z            2

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.769
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             524

_exptl_special_details           
;
One reference frame every 50 frames.
;

_diffrn_radiation_wavelength     0.71073
_diffrn_standards_number         ?
_diffrn_standards_interval_count 1
_diffrn_standards_interval_time  50
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6176
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0868
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.06
_diffrn_reflns_theta_max         28.55
_diffrn_reflns_resolution_max    0.74
_reflns_number_total             3393
_reflns_number_gt                2809
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Oxford Diffraction CrysAlis CCD'
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_computing_structure_solution    'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_structure_refinement  'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_molecular_graphics    'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_publication_material  'Sheldrick, G.M. (2000). SHELXTL v6.10.'

_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.

We note a large peak in the residual electron density map, and believe
this to be an artifact of a multiple crystal used for data collection. It is
known that urate crystals often grow as twins and while care was taken
to select a single crystal, examination of the final diffraction frames shows
what appears to be a very weakly-diffracting "twin" component. Attempts to
refine the model using both components did not improve the refinement.

Because this sample is a hydrate, TGA experiments were run to assess
the amount of water in the lattice, in case the residual electron density
could be attributable to a fractional water molecule. However, TGA
results show this material is strictly the monohydrate.

The residual electron density represents approximately 2 percent of
a Pb atom.

Hydrogen atoms were all refined using appropriate riding models. In
initial refinements the hydrogen atoms for the water molecule (O1W)
were restrained for O-H distances only; they were allowed to rotate freely.
This led to unusual positions of the hydrogen atoms, despite the availability
of two nearby hydrogen-bond acceptors (O2, O3). We opted to omit the
hydrogen atoms from the final refinements, as the poor data quality would
not allow for appropriate modeling of their behavior. The reported formula
reflects their presence in the lattice.

All non-hydrogen atoms were subjected to soft rigid bond restraints (DELU)
for anisotropic refinement.

;

_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^)+(0.0612P)^2^+5.3191P] 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         3393
_refine_ls_number_parameters     235
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1349
_refine_ls_wR_factor_gt          0.1245
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.071
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.76960(6) 0.36780(4) 0.08236(3) 0.01579(14) Uani 1 1 d U . .
O1 O 1.0068(11) 0.5908(8) 0.0904(6) 0.0152(14) Uani 1 1 d U . .
O2 O 1.0585(12) 0.9921(9) 0.3329(6) 0.0186(15) Uani 1 1 d U . .
O3 O 0.7040(11) 0.5868(9) 0.6609(6) 0.0184(15) Uani 1 1 d U . .
C1 C 0.9730(14) 0.6361(11) 0.1927(8) 0.0128(17) Uani 1 1 d U . .
C2 C 0.8551(15) 0.6027(11) 0.3751(8) 0.0123(17) Uani 1 1 d U . .
C3 C 0.9172(15) 0.7484(11) 0.4039(8) 0.0124(17) Uani 1 1 d U . .
C4 C 1.0054(15) 0.8536(12) 0.3222(8) 0.0142(18) Uani 1 1 d U . .
C5 C 0.7704(15) 0.6243(12) 0.5622(8) 0.0144(18) Uani 1 1 d U . .
N1 N 1.0287(13) 0.7856(9) 0.2160(7) 0.0133(16) Uani 1 1 d U . .
H1 H 1.0841 0.8438 0.1589 0.016 Uiso 1 1 calc R . .
N2 N 0.8764(13) 0.5392(10) 0.2705(7) 0.0132(16) Uani 1 1 d U . .
N3 N 0.8617(14) 0.7591(10) 0.5211(7) 0.0178(17) Uani 1 1 d U . .
H3 H 0.8829 0.8408 0.5617 0.021 Uiso 1 1 calc R . .
N4 N 0.7656(12) 0.5274(10) 0.4711(7) 0.0130(16) Uani 1 1 d U . .
H4 H 0.7137 0.4328 0.4740 0.016 Uiso 1 1 calc R . .
O1A O 0.8094(11) 0.1095(9) -0.0089(6) 0.0173(14) Uani 1 1 d U . .
O2A O 0.5259(12) -0.3744(9) 0.0646(6) 0.0190(15) Uani 1 1 d U . .
O3A O 0.3789(10) -0.2037(8) 0.4995(6) 0.0157(14) Uani 1 1 d U . .
C1A C 0.7195(16) 0.0131(12) 0.0648(8) 0.0148(18) Uani 1 1 d U . .
C2A C 0.5774(14) -0.0459(12) 0.2409(8) 0.0131(17) Uani 1 1 d U . .
C3A C 0.5228(15) -0.1959(11) 0.2122(8) 0.0131(17) Uani 1 1 d U . .
C4A C 0.5663(16) -0.2439(13) 0.1017(9) 0.0180(19) Uani 1 1 d U . .
C5A C 0.4410(16) -0.1725(12) 0.3983(8) 0.0151(19) Uani 1 1 d U . .
N1A N 0.6746(13) -0.1318(10) 0.0343(7) 0.0134(16) Uani 1 1 d U . .
H1A H 0.7175 -0.1585 -0.0345 0.016 Uiso 1 1 calc R . .
N2A N 0.6731(13) 0.0636(10) 0.1708(7) 0.0135(15) Uani 1 1 d U . .
N3A N 0.4387(13) -0.2717(11) 0.3112(7) 0.0170(17) Uani 1 1 d U . .
H3A H 0.3918 -0.3681 0.3165 0.020 Uiso 1 1 calc R . .
N4A N 0.5231(12) -0.0331(10) 0.3544(7) 0.0122(15) Uani 1 1 d U . .
H4A H 0.5384 0.0513 0.3934 0.015 Uiso 1 1 calc R . .
O1W O 1.1032(11) 0.2396(9) 0.1679(6) 0.0181(14) Uani 1 1 d U . .

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 0.0212(2) 0.0135(2) 0.0127(2) -0.00343(13) -0.00025(14) 0.00173(14)
O1 0.020(4) 0.019(3) 0.007(3) 0.002(2) -0.004(3) -0.003(3)
O2 0.029(4) 0.014(3) 0.013(3) -0.001(3) 0.000(3) -0.004(3)
O3 0.025(4) 0.020(4) 0.010(3) -0.001(3) 0.004(3) -0.001(3)
C1 0.013(4) 0.012(4) 0.014(4) 0.000(3) -0.002(3) -0.003(3)
C2 0.019(5) 0.004(4) 0.013(4) 0.003(3) 0.002(4) 0.004(3)
C3 0.017(5) 0.010(4) 0.011(4) -0.002(3) -0.001(3) 0.006(3)
C4 0.016(5) 0.013(4) 0.015(4) 0.000(3) -0.008(4) 0.000(4)
C5 0.017(5) 0.019(5) 0.008(4) -0.003(3) -0.006(3) 0.001(4)
N1 0.022(4) 0.009(3) 0.010(3) 0.001(3) -0.006(3) -0.001(3)
N2 0.017(4) 0.017(4) 0.006(3) -0.004(3) -0.002(3) 0.003(3)
N3 0.029(5) 0.008(4) 0.016(4) -0.001(3) 0.000(4) -0.002(3)
N4 0.015(4) 0.013(4) 0.011(3) -0.003(3) 0.004(3) 0.003(3)
O1A 0.021(4) 0.017(3) 0.014(3) -0.002(3) 0.002(3) -0.003(3)
O2A 0.030(4) 0.013(3) 0.014(3) -0.001(3) -0.002(3) 0.001(3)
O3A 0.017(4) 0.018(4) 0.011(3) -0.002(3) 0.007(3) -0.002(3)
C1A 0.023(5) 0.013(4) 0.008(4) 0.000(3) 0.001(4) 0.007(4)
C2A 0.009(4) 0.019(4) 0.011(4) -0.001(3) 0.001(3) 0.001(3)
C3A 0.018(5) 0.011(4) 0.011(4) -0.003(3) -0.001(3) 0.003(3)
C4A 0.024(5) 0.019(4) 0.012(4) -0.001(3) -0.004(4) 0.005(4)
C5A 0.020(5) 0.015(4) 0.010(4) -0.003(3) 0.001(4) 0.001(4)
N1A 0.023(4) 0.014(4) 0.004(3) -0.003(3) -0.003(3) 0.002(3)
N2A 0.016(4) 0.017(4) 0.007(3) -0.001(3) 0.002(3) 0.004(3)
N3A 0.022(4) 0.016(4) 0.013(4) -0.001(3) 0.000(3) 0.004(3)
N4A 0.015(4) 0.015(4) 0.007(3) -0.001(3) 0.001(3) 0.000(3)
O1W 0.018(3) 0.020(4) 0.016(3) -0.002(3) -0.002(3) 0.004(3)

_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 O1 2.468(7) 2_765 ?
Pb1 O1A 2.484(7) . ?
Pb1 O1 2.521(7) . ?
Pb1 O2A 2.707(7) 1_565 ?
Pb1 O1W 2.713(7) . ?
Pb1 O2A 2.728(8) 2_655 ?
Pb1 N2A 2.798(9) . ?
O1 C1 1.286(12) . ?
O1 Pb1 2.468(7) 2_765 ?
O2 C4 1.249(12) . ?
O3 C5 1.244(12) . ?
C1 N2 1.344(13) . ?
C1 N1 1.375(12) . ?
C2 N2 1.364(12) . ?
C2 N4 1.378(12) . ?
C2 C3 1.379(13) . ?
C3 C4 1.389(14) . ?
C3 N3 1.410(12) . ?
C4 N1 1.399(12) . ?
C5 N3 1.361(13) . ?
C5 N4 1.385(12) . ?
N1 H1 0.8800 . ?
N3 H3 0.8800 . ?
N4 H4 0.8800 . ?
O1A C1A 1.290(12) . ?
O2A C4A 1.251(13) . ?
O2A Pb1 2.707(7) 1_545 ?
O2A Pb1 2.728(8) 2_655 ?
O3A C5A 1.251(12) . ?
C1A N1A 1.342(13) . ?
C1A N2A 1.353(12) . ?
C2A N2A 1.355(13) . ?
C2A N4A 1.369(12) . ?
C2A C3A 1.395(14) . ?
C3A C4A 1.392(13) . ?
C3A N3A 1.393(13) . ?
C4A N1A 1.394(14) . ?
C5A N3A 1.358(13) . ?
C5A N4A 1.377(13) . ?
N1A H1A 0.8800 . ?
N3A H3A 0.8800 . ?
N4A H4A 0.8800 . ?

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 O1A 72.8(2) 2_765 . ?
O1 Pb1 O1 65.4(3) 2_765 . ?
O1A Pb1 O1 130.8(2) . . ?
O1 Pb1 O2A 101.2(2) 2_765 1_565 ?
O1A Pb1 O2A 136.2(2) . 1_565 ?
O1 Pb1 O2A 78.2(2) . 1_565 ?
O1 Pb1 O1W 82.0(2) 2_765 . ?
O1A Pb1 O1W 76.6(2) . . ?
O1 Pb1 O1W 73.1(2) . . ?
O2A Pb1 O1W 146.8(2) 1_565 . ?
O1 Pb1 O2A 85.6(2) 2_765 2_655 ?
O1A Pb1 O2A 76.2(2) . 2_655 ?
O1 Pb1 O2A 123.1(2) . 2_655 ?
O2A Pb1 O2A 60.0(3) 1_565 2_655 ?
O1W Pb1 O2A 152.4(2) . 2_655 ?
O1 Pb1 N2A 121.6(2) 2_765 . ?
O1A Pb1 N2A 50.4(2) . . ?
O1 Pb1 N2A 144.6(2) . . ?
O2A Pb1 N2A 127.5(2) 1_565 . ?
O1W Pb1 N2A 73.8(2) . . ?
O2A Pb1 N2A 92.3(2) 2_655 . ?
C1 O1 Pb1 142.3(6) . 2_765 ?
C1 O1 Pb1 102.8(6) . . ?
Pb1 O1 Pb1 114.6(3) 2_765 . ?
O1 C1 N2 118.8(9) . . ?
O1 C1 N1 118.2(9) . . ?
N2 C1 N1 122.9(9) . . ?
N2 C2 N4 124.1(9) . . ?
N2 C2 C3 127.3(9) . . ?
N4 C2 C3 108.5(9) . . ?
C2 C3 C4 121.1(9) . . ?
C2 C3 N3 105.9(8) . . ?
C4 C3 N3 132.9(9) . . ?
O2 C4 C3 128.9(9) . . ?
O2 C4 N1 120.4(9) . . ?
C3 C4 N1 110.7(8) . . ?
O3 C5 N3 129.5(9) . . ?
O3 C5 N4 123.9(10) . . ?
N3 C5 N4 106.6(8) . . ?
C1 N1 C4 126.0(9) . . ?
C1 N1 H1 117.0 . . ?
C4 N1 H1 117.0 . . ?
C1 N2 C2 111.8(8) . . ?
C5 N3 C3 109.9(8) . . ?
C5 N3 H3 125.0 . . ?
C3 N3 H3 125.0 . . ?
C2 N4 C5 109.1(8) . . ?
C2 N4 H4 125.4 . . ?
C5 N4 H4 125.4 . . ?
C1A O1A Pb1 103.0(6) . . ?
C4A O2A Pb1 122.4(7) . 1_545 ?
C4A O2A Pb1 115.9(6) . 2_655 ?
Pb1 O2A Pb1 120.0(3) 1_545 2_655 ?
O1A C1A N1A 119.6(8) . . ?
O1A C1A N2A 118.0(9) . . ?
N1A C1A N2A 122.4(9) . . ?
N2A C2A N4A 126.6(9) . . ?
N2A C2A C3A 126.4(9) . . ?
N4A C2A C3A 107.0(9) . . ?
C4A C3A N3A 133.1(9) . . ?
C4A C3A C2A 119.6(9) . . ?
N3A C3A C2A 107.1(8) . . ?
O2A C4A C3A 126.2(10) . . ?
O2A C4A N1A 121.5(9) . . ?
C3A C4A N1A 112.1(9) . . ?
O3A C5A N3A 125.7(10) . . ?
O3A C5A N4A 126.9(9) . . ?
N3A C5A N4A 107.4(8) . . ?
C1A N1A C4A 126.0(8) . . ?
C1A N1A H1A 117.0 . . ?
C4A N1A H1A 117.0 . . ?
C1A N2A C2A 113.2(9) . . ?
C1A N2A Pb1 87.1(6) . . ?
C2A N2A Pb1 156.4(6) . . ?
C5A N3A C3A 108.8(9) . . ?
C5A N3A H3A 125.6 . . ?
C3A N3A H3A 125.6 . . ?
C2A N4A C5A 109.6(8) . . ?
C2A N4A H4A 125.2 . . ?
C5A N4A H4A 125.2 . . ?

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
O1 Pb1 O1 C1 -175.4(8) 2_765 . . . ?
O1A Pb1 O1 C1 -141.0(6) . . . . ?
O2A Pb1 O1 C1 76.3(6) 1_565 . . . ?
O1W Pb1 O1 C1 -86.6(6) . . . . ?
O2A Pb1 O1 C1 118.2(6) 2_655 . . . ?
N2A Pb1 O1 C1 -64.9(7) . . . . ?
O1 Pb1 O1 Pb1 0.0 2_765 . . 2_765 ?
O1A Pb1 O1 Pb1 34.3(4) . . . 2_765 ?
O2A Pb1 O1 Pb1 -108.3(3) 1_565 . . 2_765 ?
O1W Pb1 O1 Pb1 88.8(3) . . . 2_765 ?
O2A Pb1 O1 Pb1 -66.5(4) 2_655 . . 2_765 ?
N2A Pb1 O1 Pb1 110.5(4) . . . 2_765 ?
Pb1 O1 C1 N2 -156.0(7) 2_765 . . . ?
Pb1 O1 C1 N2 17.1(10) . . . . ?
Pb1 O1 C1 N1 27.3(15) 2_765 . . . ?
Pb1 O1 C1 N1 -159.6(7) . . . . ?
N2 C2 C3 C4 3.0(16) . . . . ?
N4 C2 C3 C4 -177.2(8) . . . . ?
N2 C2 C3 N3 -179.9(9) . . . . ?
N4 C2 C3 N3 -0.1(11) . . . . ?
C2 C3 C4 O2 175.3(10) . . . . ?
N3 C3 C4 O2 -0.9(19) . . . . ?
C2 C3 C4 N1 -3.5(13) . . . . ?
N3 C3 C4 N1 -179.6(10) . . . . ?
O1 C1 N1 C4 -179.3(9) . . . . ?
N2 C1 N1 C4 4.1(15) . . . . ?
O2 C4 N1 C1 -178.6(9) . . . . ?
C3 C4 N1 C1 0.2(14) . . . . ?
O1 C1 N2 C2 179.0(9) . . . . ?
N1 C1 N2 C2 -4.5(13) . . . . ?
N4 C2 N2 C1 -178.5(9) . . . . ?
C3 C2 N2 C1 1.2(14) . . . . ?
O3 C5 N3 C3 178.4(10) . . . . ?
N4 C5 N3 C3 -0.5(11) . . . . ?
C2 C3 N3 C5 0.4(11) . . . . ?
C4 C3 N3 C5 177.0(10) . . . . ?
N2 C2 N4 C5 179.6(9) . . . . ?
C3 C2 N4 C5 -0.2(11) . . . . ?
O3 C5 N4 C2 -178.5(9) . . . . ?
N3 C5 N4 C2 0.4(11) . . . . ?
O1 Pb1 O1A C1A 173.1(7) 2_765 . . . ?
O1 Pb1 O1A C1A 140.6(6) . . . . ?
O2A Pb1 O1A C1A -98.6(7) 1_565 . . . ?
O1W Pb1 O1A C1A 87.5(6) . . . . ?
O2A Pb1 O1A C1A -97.3(6) 2_655 . . . ?
N2A Pb1 O1A C1A 7.5(6) . . . . ?
Pb1 O1A C1A N1A 166.1(8) . . . . ?
Pb1 O1A C1A N2A -13.7(10) . . . . ?
N2A C2A C3A C4A -0.3(16) . . . . ?
N4A C2A C3A C4A -177.9(9) . . . . ?
N2A C2A C3A N3A 176.6(9) . . . . ?
N4A C2A C3A N3A -1.0(11) . . . . ?
Pb1 O2A C4A C3A -87.5(12) 1_545 . . . ?
Pb1 O2A C4A C3A 107.7(10) 2_655 . . . ?
Pb1 O2A C4A N1A 88.5(10) 1_545 . . . ?
Pb1 O2A C4A N1A -76.3(11) 2_655 . . . ?
N3A C3A C4A O2A 4.1(19) . . . . ?
C2A C3A C4A O2A -180.0(10) . . . . ?
N3A C3A C4A N1A -172.2(10) . . . . ?
C2A C3A C4A N1A 3.7(14) . . . . ?
O1A C1A N1A C4A -175.3(9) . . . . ?
N2A C1A N1A C4A 4.5(16) . . . . ?
O2A C4A N1A C1A 177.5(10) . . . . ?
C3A C4A N1A C1A -5.9(14) . . . . ?
O1A C1A N2A C2A 179.4(9) . . . . ?
N1A C1A N2A C2A -0.4(14) . . . . ?
O1A C1A N2A Pb1 11.8(9) . . . . ?
N1A C1A N2A Pb1 -167.9(9) . . . . ?
N4A C2A N2A C1A 175.6(9) . . . . ?
C3A C2A N2A C1A -1.6(14) . . . . ?
N4A C2A N2A Pb1 -37(2) . . . . ?
C3A C2A N2A Pb1 145.9(13) . . . . ?
O1 Pb1 N2A C1A -23.3(7) 2_765 . . . ?
O1A Pb1 N2A C1A -7.0(5) . . . . ?
O1 Pb1 N2A C1A -114.5(6) . . . . ?
O2A Pb1 N2A C1A 116.1(6) 1_565 . . . ?
O1W Pb1 N2A C1A -92.8(6) . . . . ?
O2A Pb1 N2A C1A 63.0(6) 2_655 . . . ?
O1 Pb1 N2A C2A -173.6(16) 2_765 . . . ?
O1A Pb1 N2A C2A -157.3(18) . . . . ?
O1 Pb1 N2A C2A 95.2(17) . . . . ?
O2A Pb1 N2A C2A -34.2(17) 1_565 . . . ?
O1W Pb1 N2A C2A 116.9(17) . . . . ?
O2A Pb1 N2A C2A -87.4(16) 2_655 . . . ?
O3A C5A N3A C3A -179.1(10) . . . . ?
N4A C5A N3A C3A 1.0(11) . . . . ?
C4A C3A N3A C5A 176.3(11) . . . . ?
C2A C3A N3A C5A 0.0(11) . . . . ?
N2A C2A N4A C5A -176.0(9) . . . . ?
C3A C2A N4A C5A 1.7(11) . . . . ?
O3A C5A N4A C2A 178.4(10) . . . . ?
N3A C5A N4A C2A -1.7(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.55
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         5.908
_refine_diff_density_min         -2.973
_refine_diff_density_rms         0.373

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1 '
_symmetry_space_group_name_Hall  '-P 1'

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2.00 9.00 11.00 0.0185
-6.00 8.00 5.00 0.0287
5.00 0.00 -14.00 0.0209
-6.00 -7.00 7.00 0.0154
3.00 -6.00 13.00 0.0403
8.00 0.00 9.00 0.0428
-2.00 7.00 -13.00 0.0400
-2.00 11.00 4.00 0.0255
7.00 -8.00 2.00 0.0461
0.00 -10.00 -10.00 0.0200
5.00 7.00 -8.00 0.0163
_audit_creation_date             
;
'Fri Dec 02 10:52:10 2005'
;
_audit_creation_method_reference 
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle7 beta (release 01-12-2005 CrysAlis171 .NET)
(compiled Dec 1 2005,15:12:38)
;
_computing_data_collection_reference 
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.28cycle7 beta (release 01-12-2005 CrysAlis171 .NET)
(compiled Dec 1 2005,15:12:38)
;
_computing_cell_refinment_reference 
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle7 beta (release 01-12-2005 CrysAlis171 .NET)
(compiled Dec 1 2005,15:12:38)
;
_computing_data_reduction_reference 
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle7 beta (release 01-12-2005 CrysAlis171 .NET)
(compiled Dec 1 2005,15:12:38)
;
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      4.0505
_cell_measurement_theta_max      28.4896
_cell_measurement_resolution_max 0.75
_cell_measurement_temperature    110
_exptl_crystal_size_max          0.04615
_exptl_crystal_size_mid          0.02860
_exptl_crystal_size_min          0.01538
_exptl_absorpt_coefficient_mu    12.64518
_exptl_absorpt_correction_T_min  0.45658
_exptl_absorpt_correction_T_max  0.68995
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle7 beta (release 01-12-2005 CrysAlis171 .NET)
(compiled Dec 1 2005,15:12:38)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 15.9890
_diffrn_orient_matrix_UB_11      0.0269798487
_diffrn_orient_matrix_UB_12      0.0678870103
_diffrn_orient_matrix_UB_13      0.0278096933
_diffrn_orient_matrix_UB_21      -0.0993822797
_diffrn_orient_matrix_UB_22      0.0111373791
_diffrn_orient_matrix_UB_23      0.0212163688
_diffrn_orient_matrix_UB_31      0.0192179135
_diffrn_orient_matrix_UB_32      -0.0483755717
_diffrn_orient_matrix_UB_33      0.0495259628
_diffrn_measurement_details      'see scan set'

loop_
_diffrn_scan_number
_diffrn_scan_type
_diffrn_scan_start
_diffrn_scan_end
_diffrn_scan_width
_diffrn_scan_exptime
_diffrn_scan_omega
_diffrn_scan_theta
_diffrn_scan_kappa
_diffrn_scan_phi
_diffrn_scan_omega1
_diffrn_scan_theta1
_diffrn_scan_frames

1 omega -70.80 37.20 1.00 60.00 - -35.00 81.00 350.00 0.00 0.00 108
2 omega -5.50 96.50 1.00 60.00 - 25.00 71.00 120.00 0.00 0.00 102
3 omega -5.50 96.50 1.00 60.00 - 25.00 71.00 230.00 0.00 0.00 102
4 omega -111.38 31.62 1.00 60.00 - -35.00 -19.00 0.00 0.00 0.00 143

_diffrn_measurement_method       ' omega scans'

_JHU_your_name_here              'Dr. Amy A Sarjeant'
_JHU_your_lab_here               'NCB 240'
_JHU_your_phone_number_here      x6-8569
_JHU_your_email_here             xray@jhu.edu

_JHU_Institutional_Source        'Swift Lab'
_JHU_Submitting_Scientist        'Rupa Hiremath'

_JHU_identifying_number          pbu

_diffrn_source_power             2
_diffrn_source_voltage           50
_diffrn_source_current           40
_diffrn_measurement_device       Kappa
_diffrn_measurement_device_type  Xcalibur3
_diffrn_ambient_temperature      110

_JHU_diffraction_detector_distance 50
_JHU_quality_factor              3


