New crystallographic data and formula revision of phuralumite, Al2[(UO2)3(PO4)2O(OH)](OH)3(H2O)9
Fabrice Dal Bo; Frederic Hatert; Simon Philippo; Journal of GeoSciences 62 (2017) 87–95; doi:10.3190/jgeosci.233

data_1566258
_publ_section_title
;
 New crystallographic data and formula revision of phuralumite,
 Al2[(UO2)3(PO4)2O(OH)](OH)3(H2O)9
;
_journal_name_full               'Journal of GeoSciences'
_journal_page_first              87
_journal_page_last               95
_journal_paper_doi               10.3190/jgeosci.233
_journal_volume                  62
_journal_year                    2017
_chemical_formula_moiety         'Al2 O21 P2 U3, 6.5(O)'
_chemical_formula_sum            'Al2 H20 O27 P2 U3'
_chemical_formula_weight         1282.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 107.862(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4423(5)
_cell_length_b                   20.8723(9)
_cell_length_c                   13.4307(6)
_cell_measurement_reflns_used    3002
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2110
_cell_measurement_theta_min      2.3410
_cell_volume                     2519.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 32.0175
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9089
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -61.00  38.00   1.00   85.17    --  -17.07  19.00 -30.00   99
  2  \w    -89.00 -57.00   1.00   85.17    --  -17.07 -37.00 120.00   32
  3  \w    -23.00   2.00   1.00   85.17    --  -17.07 -99.00 150.00   25
  4  \w    -24.00  16.00   1.00   85.17    --  -17.07 -99.00 -90.00   40
  5  \w    -24.00  23.00   1.00   85.17    --  -17.07 -99.00  60.00   47
  6  \w    -80.00 -50.00   1.00   85.17    --  -17.07-178.00 -30.00   30
  7  \w    -92.00 -41.00   1.00   85.17    --  -17.07-178.00 -90.00   51
  8  \w    -54.00 -28.00   1.00   85.17    --  -17.07 -37.00 120.00   26
  9  \w    -90.00 -20.00   1.00   85.17    --  -17.07 -37.00 150.00   70
 10  \w     67.00  92.00   1.00   85.17    --   19.10 178.00 -60.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0589795000
_diffrn_orient_matrix_UB_12      -0.0219438000
_diffrn_orient_matrix_UB_13      -0.0208800000
_diffrn_orient_matrix_UB_21      -0.0438082000
_diffrn_orient_matrix_UB_22      0.0163989000
_diffrn_orient_matrix_UB_23      0.0263431000
_diffrn_orient_matrix_UB_31      -0.0287303000
_diffrn_orient_matrix_UB_32      0.0201087000
_diffrn_orient_matrix_UB_33      -0.0441988000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_unetI/netI     0.1266
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22883
_diffrn_reflns_theta_full        28.86
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         1.95
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.540
_exptl_absorpt_correction_T_max  0.438
_exptl_absorpt_correction_T_min  0.176
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    3.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.397
_refine_diff_density_min         -3.942
_refine_diff_density_rms         0.523
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                3937
_reflns_number_total             6007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jgeosci.233_VC2054-Phuralumite.cif
_cod_data_source_block           vc2054-phuralumite-4
_cod_original_cell_volume        2519.3(2)
_cod_original_formula_sum        'H20 Al2 O27 P2 U3'
_cod_database_code               1566258
_chemical_oxdiff_formula         'Al2 H20 O27 P2 U3'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.522
_oxdiff_exptl_absorpt_empirical_full_min 0.784