 
data_plasilite
 
_audit_creation_method            SHELXL-2013
_chemical_name_mineral            'plasilite' 
_chemical_compound_source         'Blue Lizard mine, Utah'
_chemical_formula_sum
 'H4 Na O9 S U' 
_chemical_formula_weight          441.11

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'U'  'U'  -9.6767   9.6646
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Na'  'Na'   0.0362   0.0249
 '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'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    8.7122(6)
_cell_length_b                    13.8368(4)
_cell_length_c                    7.04650(17)
_cell_angle_alpha                 90
_cell_angle_beta                  112.126(8)
_cell_angle_gamma                 90
_cell_volume                      786.89(7)
_cell_formula_units_Z             4
_exptl_crystal_density_diffrn     3.723          
_exptl_crystal_F_000              780
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.080
_exptl_crystal_size_mid           0.020
_exptl_crystal_size_min           0.005
_exptl_absorpt_coefficient_mu     20.965
_shelx_estimated_absorpt_T_min    0.285
_shelx_estimated_absorpt_T_max    0.902
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    Higashi2001 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71075
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'                       
_diffrn_radiation_monochromator   graphite 
_diffrn_reflns_number             7709
_diffrn_reflns_av_unetI/netI      0.0250
_diffrn_reflns_av_R_equivalents   0.0295
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -7
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_theta_min          3.451
_diffrn_reflns_theta_max          27.477
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.994
_diffrn_measured_fraction_theta_full  0.993
_diffrn_reflns_Laue_measured_fraction_max    0.994
_diffrn_reflns_Laue_measured_fraction_full   0.993
_diffrn_reflns_point_group_measured_fraction_max   0.994
_diffrn_reflns_point_group_measured_fraction_full  0.993
_reflns_number_total              1794
_reflns_number_gt                 1609
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_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)+(0.0260P)²+0.4537P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     refxyz
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          1794
_refine_ls_number_parameters      124
_refine_ls_number_restraints      7
_refine_ls_R_factor_all           0.0231
_refine_ls_R_factor_gt            0.0194
_refine_ls_wR_factor_ref          0.0462
_refine_ls_wR_factor_gt           0.0446
_refine_ls_goodness_of_fit_ref    1.081
_refine_ls_restrained_S_all       1.080
_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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
U U 0.23417(2) 0.46715(2) 0.12219(2) 0.01131(7) Uani 1 1 d . . . . .
S S 0.32042(13) 0.50289(8) 0.66758(15) 0.01204(19) Uani 1 1 d . . . . .
Na Na 0.2793(3) 0.73085(15) 0.6584(3) 0.0305(5) Uani 1 1 d . . . . .
O1 O 0.1796(4) 0.5684(2) 0.6139(5) 0.0187(6) Uani 1 1 d . . . . .
O2 O 0.3124(4) 0.4419(2) 0.4914(4) 0.0205(7) Uani 1 1 d . . . . .
O3 O 0.4736(4) 0.5623(2) 0.7334(5) 0.0186(6) Uani 1 1 d . . . . .
O4 O 0.3242(4) 0.4368(2) 0.8366(4) 0.0173(6) Uani 1 1 d . . . . .
O5 O 0.1933(4) 0.3410(2) 0.1168(4) 0.0229(7) Uani 1 1 d . . . . .
O6 O 0.2856(4) 0.5921(2) 0.1325(5) 0.0225(7) Uani 1 1 d . . . . .
OH7 O -0.0008(4) 0.5113(3) 0.1785(5) 0.0240(7) Uani 1 1 d D . . . .
H7 H -0.002(8) 0.483(4) 0.276(7) 0.029 Uiso 1 1 d D U . . .
OW8 O -0.0797(5) 0.2716(3) 0.6917(6) 0.0326(8) Uani 1 1 d D . . . .
H8A H 0.006(5) 0.242(3) 0.702(9) 0.039 Uiso 1 1 d D U . . .
H8B H -0.044(7) 0.328(2) 0.719(9) 0.039 Uiso 1 1 d D U . . .
OW9 O 0.5186(5) 0.2503(3) 0.0025(6) 0.0319(8) Uani 1 1 d D . . . .
H9A H 0.475(7) 0.296(3) -0.063(8) 0.038 Uiso 1 1 d D U . . .
H9B H 0.448(6) 0.210(3) -0.020(8) 0.038 Uiso 1 1 d D U . . .
 
 
_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
U O5 1.779(3) . ?
U O6 1.781(3) . ?
U OH7 2.310(3) . ?
U OH7 2.338(3) 3_565 ?
U O3 2.394(3) 3_666 ?
U O2 2.454(3) . ?
U O4 2.456(3) 1_554 ?
U U 3.8920(4) 3_565 ?
S O1 1.456(3) . ?
S O2 1.481(3) . ?
S O3 1.485(3) . ?
S O4 1.492(3) . ?
S Na 3.172(2) . ?
Na O1 2.387(4) . ?
Na OW9 2.389(4) 3_666 ?
Na OW8 2.417(4) 2_556 ?
Na OW8 2.425(4) 3_566 ?
Na OW9 2.442(4) 2_655 ?
Na O6 2.459(4) 4_576 ?
Na O3 2.813(4) . ?
Na Na 3.5629(6) 4_575 ?
Na Na 3.5629(6) 4_576 ?
O3 U 2.394(3) 3_666 ?
O4 U 2.456(3) 1_556 ?
O6 Na 2.459(4) 4_575 ?
OH7 U 2.338(3) 3_565 ?
OW8 Na 2.417(4) 2_546 ?
OW8 Na 2.425(4) 3_566 ?
OW9 Na 2.389(4) 3_666 ?
OW9 Na 2.442(4) 2_645 ?
 
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
O5 U O6 177.21(15) . . ?
O5 U OH7 94.58(15) . . ?
O6 U OH7 87.81(15) . . ?
O5 U OH7 90.38(14) . 3_565 ?
O6 U OH7 91.89(14) . 3_565 ?
OH7 U OH7 66.26(13) . 3_565 ?
O5 U O3 90.84(13) . 3_666 ?
O6 U O3 86.37(13) . 3_666 ?
OH7 U O3 147.31(11) . 3_666 ?
OH7 U O3 146.03(11) 3_565 3_666 ?
O5 U O2 81.73(12) . . ?
O6 U O2 97.47(13) . . ?
OH7 U O2 76.46(11) . . ?
OH7 U O2 141.13(11) 3_565 . ?
O3 U O2 72.47(11) 3_666 . ?
O5 U O4 86.44(12) . 1_554 ?
O6 U O4 92.66(13) . 1_554 ?
OH7 U O4 139.77(10) . 1_554 ?
OH7 U O4 73.52(10) 3_565 1_554 ?
O3 U O4 72.68(10) 3_666 1_554 ?
O2 U O4 142.90(10) . 1_554 ?
O5 U U 92.95(11) . 3_565 ?
O6 U U 89.84(11) . 3_565 ?
OH7 U U 33.36(8) . 3_565 ?
OH7 U U 32.91(8) 3_565 3_565 ?
O3 U U 176.05(8) 3_666 3_565 ?
O2 U U 109.19(8) . 3_565 ?
O4 U U 106.42(7) 1_554 3_565 ?
O1 S O2 111.59(19) . . ?
O1 S O3 107.9(2) . . ?
O2 S O3 109.29(19) . . ?
O1 S O4 110.65(18) . . ?
O2 S O4 107.40(18) . . ?
O3 S O4 110.05(18) . . ?
O1 S Na 45.41(14) . . ?
O2 S Na 125.48(14) . . ?
O3 S Na 62.45(13) . . ?
O4 S Na 126.47(13) . . ?
O1 Na OW9 109.20(14) . 3_666 ?
O1 Na OW8 89.48(13) . 2_556 ?
OW9 Na OW8 85.30(14) 3_666 2_556 ?
O1 Na OW8 76.55(13) . 3_566 ?
OW9 Na OW8 174.24(16) 3_666 3_566 ?
OW8 Na OW8 95.14(15) 2_556 3_566 ?
O1 Na OW9 109.44(14) . 2_655 ?
OW9 Na OW9 93.63(14) 3_666 2_655 ?
OW8 Na OW9 160.17(15) 2_556 2_655 ?
OW8 Na OW9 84.00(13) 3_566 2_655 ?
O1 Na O6 161.02(14) . 4_576 ?
OW9 Na O6 86.36(13) 3_666 4_576 ?
OW8 Na O6 80.81(13) 2_556 4_576 ?
OW8 Na O6 88.04(14) 3_566 4_576 ?
OW9 Na O6 79.37(13) 2_655 4_576 ?
O1 Na O3 53.65(10) . . ?
OW9 Na O3 74.80(12) 3_666 . ?
OW8 Na O3 126.32(13) 2_556 . ?
OW8 Na O3 109.27(13) 3_566 . ?
OW9 Na O3 71.96(12) 2_655 . ?
O6 Na O3 144.23(13) 4_576 . ?
O1 Na S 25.74(8) . . ?
OW9 Na S 93.04(11) 3_666 . ?
OW8 Na S 108.49(11) 2_556 . ?
OW8 Na S 92.26(11) 3_566 . ?
OW9 Na S 91.33(11) 2_655 . ?
O6 Na S 170.62(11) 4_576 . ?
O3 Na S 27.91(7) . . ?
O1 Na Na 98.37(10) . 4_575 ?
OW9 Na Na 134.27(11) 3_666 4_575 ?
OW8 Na Na 131.73(12) 2_556 4_575 ?
OW8 Na Na 42.53(10) 3_566 4_575 ?
OW9 Na Na 41.92(9) 2_655 4_575 ?
O6 Na Na 76.70(11) 4_576 4_575 ?
O3 Na Na 94.88(9) . 4_575 ?
S Na Na 97.24(7) . 4_575 ?
O1 Na Na 97.73(10) . 4_576 ?
OW9 Na Na 43.07(10) 3_666 4_576 ?
OW8 Na Na 42.70(10) 2_556 4_576 ?
OW8 Na Na 137.82(10) 3_566 4_576 ?
OW9 Na Na 135.34(10) 2_655 4_576 ?
O6 Na Na 86.19(11) 4_576 4_576 ?
O3 Na Na 99.30(9) . 4_576 ?
S Na Na 99.77(8) . 4_576 ?
Na Na Na 162.89(13) 4_575 4_576 ?
S O1 Na 108.85(18) . . ?
S O2 U 135.58(19) . . ?
S O3 U 136.49(19) . 3_666 ?
S O3 Na 89.65(14) . . ?
U O3 Na 133.58(13) 3_666 . ?
S O4 U 129.11(17) . 1_556 ?
U O6 Na 163.3(2) . 4_575 ?
U OH7 U 113.74(12) . 3_565 ?
Na OW8 Na 94.77(15) 2_546 3_566 ?
Na OW9 Na 95.01(15) 3_666 2_645 ?
 
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 
OH7 H7 O1  0.80(3) 2.10(5) 2.739(5) 137(6) 3_566
OW8 H8A O5  0.82(3) 2.26(3) 3.050(5) 161(5) 4_566
OW8 H8B OH7  0.84(3) 2.32(3) 3.141(5) 166(5) 3_566
OW9 H9A O4  0.79(3) 2.31(3) 3.066(5) 162(6) 1_554
OW9 H9B O2  0.80(3) 2.43(3) 3.193(5) 161(5) 4_565
 
_refine_diff_density_max    3.067
_refine_diff_density_min   -0.696
_refine_diff_density_rms    0.195

_shelxl_version_number 2013-4



