##############################################################################
###                                                                        ###
###           Full Paper (Acta Crystallographica Section C)                ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section C. It conforms to the editorial and technical    #
# requirements of Notes for Authors for Section C, and has been peer         #
# reviewed under the auspices of the IUCr Commission on Journals.            #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
##############################################################################
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
bis(tetraphenylphosphonium)
dioxobis(pyridine-2,6-dicarbothioate-O,N,O')uranium(VI)
;
_chemical_name_common     ?
_chemical_formula_moiety     '2C24 H20 P + , C14 H6 N2 O6 S4 U 2-'
_chemical_formula_sum     'C62 H46 N2 O6 P2 S4 U'
_chemical_formula_iupac     '2C24 H20 P , [U O2 (C7 H3 N O2 S2)2]'
_chemical_formula_weight     1343.22
_chemical_melting_point     ?
_symmetry_cell_setting     triclinic
_symmetry_space_group_name_H-M     'P -1'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, -y, -z'
_cell_length_a     9.2351(7)
_cell_length_b     11.6070(10)
_cell_length_c     13.8070(10)
_cell_angle_alpha     77.8910(10)
_cell_angle_beta     81.460(10)
_cell_angle_gamma     69.140(10)
_cell_volume     1347.7(2)
_cell_formula_units_Z     1
_cell_measurement_reflns_used     4192
_cell_measurement_theta_min     1.51
_cell_measurement_theta_max     23.29
_cell_measurement_temperature     293(2)
_exptl_crystal_description     block
_exptl_crystal_colour     yellow
_exptl_crystal_size_max      .32
_exptl_crystal_size_mid      .25
_exptl_crystal_size_min      .20
_exptl_crystal_density_diffrn     1.655
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     666
_exptl_absorpt_coefficient_mu     3.28
_exptl_absorpt_correction_type     'empirical'
_exptl_absorpt_process_details     '(SADABS in SHELXL97; Sheldrick, 1997)'
_exptl_absorpt_correction_T_min      .31
_exptl_absorpt_correction_T_max      .52
_exptl_special_details
;
 Intensities were measured with a Siemens CCD area detector
;
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength      .71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Siemens P4/PC CCD area-detector'
_diffrn_measurement_method     'ω scans'
_diffrn_detector_area_resol_mean     '8.192 pixels/mm'
_diffrn_reflns_number     9541
_diffrn_reflns_av_R_equivalents      .031
_diffrn_reflns_av_sigmaI/netI      .055
_diffrn_reflns_theta_min     1.51
_diffrn_reflns_theta_max     28.45
_diffrn_reflns_theta_full     25.00
_diffrn_measured_fraction_theta_max      .823
_diffrn_measured_fraction_theta_full      .953
_diffrn_reflns_limit_h_min     -11
_diffrn_reflns_limit_h_max     11
_diffrn_reflns_limit_k_min     -14
_diffrn_reflns_limit_k_max     15
_diffrn_reflns_limit_l_min     -18
_diffrn_reflns_limit_l_max     18
_diffrn_standards_number     0
_diffrn_standards_interval_count     0
_diffrn_standards_interval_time     0
_diffrn_standards_decay_%     <2
_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.
;
_reflns_number_total     5605
_reflns_number_gt     5485
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all      .032
_refine_ls_R_factor_gt      .030
_refine_ls_wR_factor_ref      .073
_refine_ls_goodness_of_fit_ref     1.04
_refine_ls_restrained_S_all     1.042
_refine_ls_number_reflns     5605
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
               'calc w = 1/[σ²(Fo²)+(0.0345P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_shift/su_max      .001
_refine_ls_shift/su_mean      .000
_refine_diff_density_max     1.21
_refine_diff_density_min     -1.95
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C'  .0033  .0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H'  .0000  .0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O'  .0106  .0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'S' 'S'  .1246  .1234
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'U' 'U' -9.6767 9.6646
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N'  .0061  .0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'P' 'P'  .1023  .0942
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'SMART (Siemens, 1996)'
_computing_cell_refinement     'SAINT (Bruker, 1998)'
_computing_data_reduction     'SAINT'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'SHELXTL (Bruker, 1997)'
_computing_publication_material     'SHELXL97'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    U1 1 1/2 1  .01711(6) Uani d S 1 . . U
    P1 1.91206(10) 0.82300(8) 1.31795(6)  .01793(18) Uani d . 1 . . P
    S1 1.22784(13) 0.65734(11)  .66912(7)  .0359(2) Uani d . 1 . . S
    S2 1.46942(13) 0.19370(10) 1.16174(8)  .0384(2) Uani d . 1 . . S
    O1 1.0710(3) 0.5803(3)  .82793(18)  .0287(6) Uani d . 1 . . O
    O2 1.2009(3) 0.3387(2) 1.0960(2)  .0291(6) Uani d . 1 . . O
    O1U 1.0284(3) 0.6208(2) 1.04690(19)  .0260(5) Uani d . 1 . . O
    N1 1.2961(3) 0.4462(3)  .9324(2)  .0188(6) Uani d . 1 . . N
    C1 1.2009(4) 0.5838(3)  .7849(3)  .0218(7) Uani d . 1 . . C
    C2 1.3353(4) 0.5112(3)  .8464(2)  .0206(7) Uani d . 1 . . C
    C3 1.4876(4) 0.5073(3)  .8184(3)  .0242(7) Uani d . 1 . . C
    H3A 1.5115 0.5550  .7593  .029 Uiso calc R 1 . . H
    C4 1.6031(4) 0.4314(3)  .8795(3)  .0252(8) Uani d . 1 . . C
    H4A 1.7055 0.4286  .8629  .030 Uiso calc R 1 . . H
    C5 1.5636(4) 0.3593(3)  .9663(3)  .0232(7) Uani d . 1 . . C
    H5A 1.6399 0.3050 1.0072  .028 Uiso calc R 1 . . H
    C6 1.4086(4) 0.3695(3)  .9911(2)  .0192(7) Uani d . 1 . . C
    C7 1.3475(4) 0.3031(3) 1.0837(3)  .0224(7) Uani d . 1 . . C
    C20 1.8303(4) 0.8952(3) 1.4256(3)  .0219(7) Uani d . 1 . . C
    C21 1.7228(5) 1.0161(4) 1.4126(3)  .0343(9) Uani d . 1 . . C
    H21A 1.7016 1.0602 1.3489  .041 Uiso calc R 1 . . H
    C22 1.6479(6) 1.0703(4) 1.4940(4)  .0470(12) Uani d . 1 . . C
    H22A 1.5783 1.1518 1.4852  .056 Uiso calc R 1 . . H
    C23 1.6759(6) 1.0039(4) 1.5890(3)  .0432(11) Uani d . 1 . . C
    H23A 1.6239 1.0406 1.6438  .052 Uiso calc R 1 . . H
    C24 1.7796(6) 0.8847(4) 1.6026(3)  .0379(10) Uani d . 1 . . C
    H24A 1.7967 0.8404 1.6666  .045 Uiso calc R 1 . . H
    C25 1.8599(5) 0.8288(4) 1.5215(3)  .0275(8) Uani d . 1 . . C
    H25A 1.9322 0.7484 1.5311  .033 Uiso calc R 1 . . H
    C30 1.7515(4) 0.8058(3) 1.2705(3)  .0200(7) Uani d . 1 . . C
    C31 1.6867(4) 0.8810(3) 1.1847(3)  .0248(8) Uani d . 1 . . C
    H31A 1.7329 0.9364 1.1460  .030 Uiso calc R 1 . . H
    C32 1.5528(5) 0.8732(4) 1.1570(3)  .0347(9) Uani d . 1 . . C
    H32A 1.5094 0.9232 1.0994  .042 Uiso calc R 1 . . H
    C33 1.4837(5) 0.7917(4) 1.2144(3)  .0341(10) Uani d . 1 . . C
    H33A 1.3929 0.7877 1.1960  .041 Uiso calc R 1 . . H
    C34 1.5484(5) 0.7160(4) 1.2990(3)  .0332(9) Uani d . 1 . . C
    H34A 1.5020 0.6601 1.3367  .040 Uiso calc R 1 . . H
    C35 1.6815(5) 0.7224(3) 1.3281(3)  .0279(8) Uani d . 1 . . C
    H35A 1.7244 0.6716 1.3856  .033 Uiso calc R 1 . . H
    C40 2.0520(4) 0.6700(3) 1.3483(2)  .0211(7) Uani d . 1 . . C
    C41 2.1702(5) 0.6498(4) 1.4103(3)  .0284(8) Uani d . 1 . . C
    H41A 2.1749 0.7154 1.4370  .034 Uiso calc R 1 . . H
    C42 2.2787(5) 0.5319(4) 1.4311(3)  .0348(9) Uani d . 1 . . C
    H42A 2.3554 0.5176 1.4732  .042 Uiso calc R 1 . . H
    C43 2.2739(5) 0.4345(4) 1.3894(3)  .0346(9) Uani d . 1 . . C
    H43A 2.3472 0.3552 1.4040  .042 Uiso calc R 1 . . H
    C44 2.1608(5) 0.4545(4) 1.3261(3)  .0317(9) Uani d . 1 . . C
    H44A 2.1595 0.3893 1.2973  .038 Uiso calc R 1 . . H
    C45 2.0500(5) 0.5717(3) 1.3062(3)  .0259(8) Uani d . 1 . . C
    H45A 1.9734 0.5850 1.2643  .031 Uiso calc R 1 . . H
    C50 2.0018(4) 0.9167(3) 1.2267(2)  .0200(7) Uani d . 1 . . C
    C51 2.0085(5) 1.0293(4) 1.2428(3)  .0297(8) Uani d . 1 . . C
    H51A 1.9637 1.0586 1.3017  .036 Uiso calc R 1 . . H
    C52 2.0818(5) 1.0976(4) 1.1711(3)  .0339(9) Uani d . 1 . . C
    H52A 2.0848 1.1733 1.1814  .041 Uiso calc R 1 . . H
    C53 2.1503(5) 1.0530(4) 1.0844(3)  .0295(8) Uani d . 1 . . C
    H53A 2.2001 1.0987 1.0367  .035 Uiso calc R 1 . . H
    C54 2.1456(5) 0.9406(4) 1.0677(3)  .0282(8) Uani d . 1 . . C
    H54A 2.1927 0.9113 1.0091  .034 Uiso calc R 1 . . H
    C55 2.0711(4) 0.8722(3) 1.1380(3)  .0235(7) Uani d . 1 . . C
    H55A 2.0670 0.7973 1.1266  .028 Uiso calc R 1 . . H
_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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    U1 O1U 2_767 1.774(2) ?
    U1 O1U . 1.774(2) Y
    U1 O2 2_767 2.434(2) ?
    U1 O2 . 2.434(2) Y
    U1 O1 . 2.447(3) Y
    U1 O1 2_767 2.447(3) ?
    U1 N1 . 2.647(3) Y
    U1 N1 2_767 2.647(3) ?
    P1 C30 . 1.795(3) ?
    P1 C40 . 1.793(4) ?
    P1 C50 . 1.792(4) ?
    P1 C20 . 1.795(4) ?
    S1 C1 . 1.675(4) Y
    S2 C7 . 1.676(4) Y
    O1 C1 . 1.268(5) Y
    O2 C7 . 1.263(4) Y
    N1 C2 . 1.342(4) ?
    N1 C6 . 1.347(4) ?
    C1 C2 . 1.497(5) ?
    C2 C3 . 1.390(5) ?
    C3 C4 . 1.383(5) ?
    C4 C5 . 1.391(5) ?
    C5 C6 . 1.389(5) ?
    C6 C7 . 1.493(5) ?
    C20 C21 . 1.394(5) ?
    C20 C25 . 1.396(5) ?
    C21 C22 . 1.376(6) ?
    C22 C23 . 1.384(7) ?
    C23 C24 . 1.367(7) ?
    C24 C25 . 1.392(6) ?
    C30 C31 . 1.388(5) ?
    C30 C35 . 1.400(5) ?
    C31 C32 . 1.385(5) ?
    C32 C33 . 1.377(6) ?
    C33 C34 . 1.377(6) ?
    C34 C35 . 1.379(5) ?
    C40 C45 . 1.392(5) ?
    C40 C41 . 1.411(5) ?
    C41 C42 . 1.380(6) ?
    C42 C43 . 1.389(6) ?
    C43 C44 . 1.386(6) ?
    C44 C45 . 1.382(5) ?
    C50 C51 . 1.396(5) ?
    C50 C55 . 1.404(5) ?
    C51 C52 . 1.385(5) ?
    C52 C53 . 1.379(6) ?
    C53 C54 . 1.387(5) ?
    C54 C55 . 1.383(5) ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O1U U1 O1U 2_767 . 180.00(7) Y
    O1U U1 O2 2_767 2_767 92.16(11) ?
    O1U U1 O2 . 2_767 87.84(10) ?
    O1U U1 O2 2_767 . 87.84(10) ?
    O1U U1 O2 . . 92.16(11) Y
    O2 U1 O2 2_767 . 180.00(11) ?
    O1U U1 O1 2_767 . 86.74(10) ?
    O1U U1 O1 . . 93.26(10) Y
    O2 U1 O1 2_767 . 61.58(9) ?
    O2 U1 O1 . . 118.42(9) Y
    O1U U1 O1 2_767 2_767 93.26(10) ?
    O1U U1 O1 . 2_767 86.74(10) ?
    O2 U1 O1 2_767 2_767 118.42(9) ?
    O2 U1 O1 . 2_767 61.58(9) ?
    O1 U1 O1 . 2_767 180.0 ?
    O1U U1 N1 2_767 . 95.04(10) ?
    O1U U1 N1 . . 84.96(10) Y
    O2 U1 N1 2_767 . 120.25(9) ?
    O2 U1 N1 . . 59.75(9) Y
    O1 U1 N1 . . 59.77(9) Y
    O1 U1 N1 2_767 . 120.23(9) ?
    O1U U1 N1 2_767 2_767 84.96(10) ?
    O1U U1 N1 . 2_767 95.04(10) ?
    O2 U1 N1 2_767 2_767 59.75(9) ?
    O2 U1 N1 . 2_767 120.25(9) ?
    O1 U1 N1 . 2_767 120.23(9) ?
    O1 U1 N1 2_767 2_767 59.77(9) ?
    N1 U1 N1 . 2_767 180.0 ?
    C30 P1 C40 . . 107.77(16) ?
    C30 P1 C50 . . 110.97(16) ?
    C40 P1 C50 . . 108.83(17) ?
    C30 P1 C20 . . 105.17(16) ?
    C40 P1 C20 . . 112.27(16) ?
    C50 P1 C20 . . 111.73(16) ?
    C1 O1 U1 . . 130.8(2) ?
    C7 O2 U1 . . 132.0(2) ?
    C2 N1 C6 . . 119.2(3) ?
    C2 N1 U1 . . 119.6(2) ?
    C6 N1 U1 . . 120.3(2) ?
    O1 C1 C2 . . 113.7(3) ?
    O1 C1 S1 . . 125.2(3) ?
    C2 C1 S1 . . 121.1(3) ?
    N1 C2 C3 . . 122.0(3) ?
    N1 C2 C1 . . 113.5(3) ?
    C3 C2 C1 . . 124.5(3) ?
    C4 C3 C2 . . 119.1(4) ?
    C3 C4 C5 . . 118.9(3) ?
    C6 C5 C4 . . 119.1(3) ?
    N1 C6 C5 . . 121.6(3) ?
    N1 C6 C7 . . 113.0(3) ?
    C5 C6 C7 . . 125.3(3) ?
    O2 C7 C6 . . 113.9(3) ?
    O2 C7 S2 . . 125.4(3) ?
    C6 C7 S2 . . 120.6(3) ?
    C21 C20 C25 . . 119.7(4) ?
    C21 C20 P1 . . 118.4(3) ?
    C25 C20 P1 . . 121.5(3) ?
    C22 C21 C20 . . 120.0(4) ?
    C21 C22 C23 . . 120.2(4) ?
    C24 C23 C22 . . 120.2(4) ?
    C23 C24 C25 . . 120.7(4) ?
    C20 C25 C24 . . 119.1(4) ?
    C31 C30 C35 . . 119.8(3) ?
    C31 C30 P1 . . 122.0(3) ?
    C35 C30 P1 . . 117.9(3) ?
    C30 C31 C32 . . 119.7(4) ?
    C33 C32 C31 . . 120.3(4) ?
    C34 C33 C32 . . 120.2(4) ?
    C33 C34 C35 . . 120.5(4) ?
    C34 C35 C30 . . 119.5(3) ?
    C45 C40 C41 . . 119.4(3) ?
    C45 C40 P1 . . 120.1(3) ?
    C41 C40 P1 . . 120.4(3) ?
    C42 C41 C40 . . 119.5(4) ?
    C41 C42 C43 . . 120.2(4) ?
    C44 C43 C42 . . 120.6(4) ?
    C43 C44 C45 . . 119.6(4) ?
    C40 C45 C44 . . 120.5(3) ?
    C51 C50 C55 . . 119.7(3) ?
    C51 C50 P1 . . 122.0(3) ?
    C55 C50 P1 . . 118.4(3) ?
    C52 C51 C50 . . 120.1(4) ?
    C53 C52 C51 . . 119.8(4) ?
    C52 C53 C54 . . 120.7(4) ?
    C55 C54 C53 . . 120.1(4) ?
    C54 C55 C50 . . 119.6(3) ?
data_global
_journal_date_recd_electronic     2000-07-20
_journal_date_accepted     2000-11-13
_journal_name_full     'Acta Crystallographica, Section C'
_journal_year     2001
_journal_volume     57
_journal_issue      3
_journal_page_first     240
_journal_page_last     242
_journal_paper_category     FM
_publ_contact_author_name     'Dr Mary P. Neu'
_publ_contact_author_address
;
MS G739
Los Alamos National Laboratory
Los Alamos
NM 87545
USA
;
_publ_contact_author_email     'mneu@lanl.gov'
_publ_contact_author_fax     '505 665 4624'
_publ_contact_author_phone     '505 667 9313'
_publ_section_title
;
Actinide interactions with microbial chelators: the
bis[pyridine-2,6-bis(monothiocarboxylate)] dioxo uranium(VI) ion
;
loop_
    _publ_author_name
    _publ_author_address
    'Neu, Mary P.'
;
MS G739
Los Alamos National Laboratory
Los Alamos
NM 87545
USA
;
    'Johnson, Mitchell T.'
;
MS J514
Los Alamos National Laboratory
Los Alamos
NM 87545
USA
;
    'Matonic, John H.'
;
MS G739
Los Alamos National Laboratory
Los Alamos
NM 87545
USA
;
    'Scott, Brian L.'
;
MS J514
Los Alamos National Laboratory
Los Alamos
NM 87545
USA
;
