The influence of pressure on the structure of a 2D uranium(VI) carboxyphosphonoate compound
Spencer, Elinor C.; Ross, Nancy L.; Surbella, Robert G.; Cahill, Christopher L.; Journal of Solid State Chemistry 218 (2014) 1–5; doi:10.1016/j.jssc.2014.05.026

data_1562269
_publ_section_title
;
 The influence of pressure on the structure of a 2D uranium(VI)
 carboxyphosphonoate compound
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              1
_journal_page_last               5
_journal_paper_doi               10.1016/j.jssc.2014.05.026
_journal_volume                  218
_journal_year                    2014
_chemical_formula_moiety         'C2 H3 O7 P U'
_chemical_formula_sum            'C2 H3 O7 P U'
_chemical_formula_weight         408.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 104.783(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6395(4)
_cell_length_b                   7.0346(3)
_cell_length_c                   13.4076(13)
_cell_measurement_reflns_used    2612
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.1090
_cell_measurement_theta_min      3.1600
_cell_volume                     605.49(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)

Absorb Angel (2004) J. Appl. Cryst. 37:486-492

Average v2.2 (Angel, 2003)
;
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.2824
_diffrn_measured_fraction_theta_full 0.160
_diffrn_measured_fraction_theta_max 0.271
_diffrn_measurement_details
;
  1 omega  -40.00    0.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0000    0.0000    0.0000 40

  2 omega  -40.00   20.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000    0.0000    0.0000 60

  3 omega  -20.00   40.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000    0.0000    0.0000 60

  4 omega    0.00   40.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000    0.0000    0.0000 40

  5 omega  -53.00  -13.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0000   39.4600  -12.9000 40

  6 omega  -13.00   27.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000   39.4600  -12.9000 40

  7 omega  -69.00  -19.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0000   81.4000  -28.9000 50

  8 omega  -15.00   11.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000   81.4000  -28.9000 26

  9 omega  -27.00   13.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0000  -39.4600   12.9000 40

 10 omega   13.00   53.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000  -39.4600   12.9000 40

 11 omega  -11.00   15.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0000  -81.4000   28.9000 26

 12 omega   19.00   69.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000  -81.4000   28.9000 50

 13 omega  -97.00  -57.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0000  134.6000  -56.9000 40

 14 omega  -97.00  -37.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  134.6000  -56.9000 60

 15 omega  -58.00  -17.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000  134.6000  -56.9000 41

 16 omega  -38.00  -17.00   1.0000  115.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000  134.6000  -56.9000 21
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0259111000
_diffrn_orient_matrix_UB_12      0.0016377000
_diffrn_orient_matrix_UB_13      -0.0546904000
_diffrn_orient_matrix_UB_21      -0.0139508000
_diffrn_orient_matrix_UB_22      0.0998474000
_diffrn_orient_matrix_UB_23      0.0009223000
_diffrn_orient_matrix_UB_31      0.1060261000
_diffrn_orient_matrix_UB_32      0.0135582000
_diffrn_orient_matrix_UB_33      0.0004102000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.086
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4414
_diffrn_reflns_reduction_process
; 
data averaged using Blessing (1987) criteria 
;
_diffrn_reflns_theta_full        40.00
_diffrn_reflns_theta_max         32.47
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    27.100
_exptl_absorpt_correction_T_max  0.422
_exptl_absorpt_correction_T_min  0.154
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.434     0.997
         range of gasket transmission (min-max)           0.893     1.000
         range of P media transmission (min-max)          1.000     1.000

    DAC transmission function via a table of values

    Gasket shadowing corrections were made based upon
    Gasket thickness = 100.0 microns, radius = 150.0 microns
    Gasket absorption coeff =        30.00 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.20

    Non-absorbing pressure medium
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    4.476
_exptl_crystal_description
;
 crystal was described in terms of coordinates of corners
 now back-transformed to potentially non-integer hkl
;
_exptl_crystal_F_000             712
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.032
_refine_diff_density_max         2.081
_refine_diff_density_min         -1.533
_refine_diff_density_rms         0.415
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         661
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1318
_reflns_number_gt                460
_reflns_number_total             637
_reflns_threshold_expression     'Fsqd > 3.0u(Fsqd)'
_cod_data_source_file            JSSC-2014-218-1.cif
_cod_data_source_block           3.081GPa
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_cell_volume        605.49(7)
_cod_database_code               1562269
_diffrn_reflns_uneti/neti        0.050
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H1A,H1B} of C1
 At 1.5 times of:
  H7 of O7
2. Restrained distances
 C2-O7
 1.3 with sigma of 0.02
 C1-C2
 1.5 with sigma of 0.02
 C2-O6
 1.2 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
3.b Tetrahedral OH refined with riding coordinates:
 O7(H7)
;