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_1562270
_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                 103.136(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.70402(15)
_cell_length_b                   7.13304(15)
_cell_length_c                   14.33410(9)
_cell_measurement_reflns_used    2667
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      32.0130
_cell_measurement_theta_min      4.2230
_cell_volume                     667.52(2)
_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
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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)
;
_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      298(2)
_diffrn_detector_area_resol_mean 16.0122
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.9240
_diffrn_measurement_details
;
  1 omega -104.00  -41.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753 -178.0000  120.0000 63

  2 omega -101.00   -1.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -38.0000    0.0000 100

  3 omega  -53.00   23.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753   57.0000 -180.0000 76

  4 omega -109.00  -35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753 -178.0000  -60.0000 74

  5 omega -100.00  -75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -57.0000  -90.0000 25

  6 omega -102.00    4.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -77.0000 -180.0000 106
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0968253000
_diffrn_orient_matrix_UB_12      -0.0280681000
_diffrn_orient_matrix_UB_13      -0.0070440000
_diffrn_orient_matrix_UB_21      -0.0472080000
_diffrn_orient_matrix_UB_22      -0.0770811000
_diffrn_orient_matrix_UB_23      -0.0279404000
_diffrn_orient_matrix_UB_31      -0.0164744000
_diffrn_orient_matrix_UB_32      0.0561705000
_diffrn_orient_matrix_UB_33      -0.0418652000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6696
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         32.45
_diffrn_reflns_theta_min         3.76
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.546
_exptl_absorpt_correction_T_max  0.487
_exptl_absorpt_correction_T_min  0.090
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.060
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.1409
_exptl_crystal_size_mid          0.1327
_exptl_crystal_size_min          0.0292
_refine_diff_density_max         2.068
_refine_diff_density_min         -1.677
_refine_diff_density_rms         0.290
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0148P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0593
_reflns_number_gt                1907
_reflns_number_total             2220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2014-218-1.cif
_cod_data_source_block           Post-HP_expt
_cod_database_code               1562270
_chemical_oxdiff_formula         'C2 H3 O7 P U'
_chemical_oxdiff_usercomment     'UPA post HP-XRD expt'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H1A,H1B} of C1
 At 1.5 times of:
  H7 of O7
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;