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_1562266
_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                 103.071(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.69750(14)
_cell_length_b                   7.13226(14)
_cell_length_c                   14.3094(3)
_cell_measurement_reflns_used    3984
_cell_measurement_temperature    297.8(5)
_cell_measurement_theta_max      31.9350
_cell_measurement_theta_min      4.2220
_cell_volume                     665.83(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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      297.8(5)
_diffrn_detector_area_resol_mean 16.0122
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.9508
_diffrn_measurement_details
;
  1 omega -107.00  -68.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753 -178.0000    0.0000 39

  2 omega -100.00   16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -19.0000   60.0000 116

  3 omega  -84.00    1.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -77.0000  -30.0000 85

  4 omega -109.00  -35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753 -178.0000   90.0000 74

  5 omega -109.00  -35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753 -178.0000 -120.0000 74

  6 omega  -50.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753   38.0000  120.0000 94

  7 omega -102.00    4.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -77.0000   60.0000 106

  8 omega -112.00  -71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  178.0000 -180.0000 41

  9 omega -100.00   -6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -57.0000 -150.0000 94
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1036213000
_diffrn_orient_matrix_UB_12      0.0121865000
_diffrn_orient_matrix_UB_13      -0.0027305000
_diffrn_orient_matrix_UB_21      -0.0032366000
_diffrn_orient_matrix_UB_22      0.0943048000
_diffrn_orient_matrix_UB_23      0.0153450000
_diffrn_orient_matrix_UB_31      0.0327744000
_diffrn_orient_matrix_UB_32      -0.0291696000
_diffrn_orient_matrix_UB_33      0.0484397000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0434
_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       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11003
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         32.41
_diffrn_reflns_theta_min         3.76
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.608
_exptl_absorpt_correction_T_max  0.464
_exptl_absorpt_correction_T_min  0.069
_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_density_diffrn    4.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.1417
_exptl_crystal_size_mid          0.1326
_exptl_crystal_size_min          0.0316
_refine_diff_density_max         1.478
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.276
_refine_ls_extinction_coef       0.00366(19)
_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   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0110P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0501
_reflns_number_gt                1923
_reflns_number_total             2276
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2014-218-1.cif
_cod_data_source_block           Ambient_conditions
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_hydrogen_treatment' value 'Constr' was changed
to 'constr' 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_database_code               1562266
_chemical_oxdiff_formula         'U P C2 H2 O7'
_chemical_oxdiff_usercomment     'GW R652-2'
_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)
;