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