Synthesis and Characterization of a Water Stable Uranyl(V) Complex.
Faizova, Radmila; Scopelliti, Rosario; Chauvin, Anne-Sophie; Mazzanti, Marinella; Journal of the American Chemical Society 140 (2018) 13554–13557; doi:10.1021/jacs.8b07885

data_4133017
_publ_section_title
;
 Synthesis and Characterization of a Water Stable Uranyl(V) Complex.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13554
_journal_page_last               13557
_journal_paper_doi               10.1021/jacs.8b07885
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C32 H30 N6 O8 U'
_chemical_formula_sum            'C32 H30 N6 O8 U'
_chemical_formula_weight         864.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-05-28 # Formatted by publCIF

;
_cell_angle_alpha                84.793(2)
_cell_angle_beta                 78.643(2)
_cell_angle_gamma                77.371(2)
_cell_formula_units_Z            4
_cell_length_a                   10.3525(3)
_cell_length_b                   19.8443(5)
_cell_length_c                   19.8538(5)
_cell_measurement_reflns_used    16235
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.1300
_cell_measurement_theta_min      4.4110
_cell_volume                     3897.26(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury 3.10.1 (CCDC, 2018)'
_computing_publication_material  'CIFTab (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.968
_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    -53.00 -27.00   1.00    1.00    --  -42.88 -37.00 -90.00   26
  2  \w    -69.00  29.00   1.00    1.00    --  -42.88  57.00  60.00   98
  3  \w      2.00  84.00   1.00    1.00    --   42.88 -99.00-180.00   82
  4  \w     28.00  53.00   1.00    1.00    --   42.88-125.00-180.00   25
  5  \w     81.00 107.00   1.00    4.00    --  109.26-111.00 -90.00   26
  6  \w    111.00 141.00   1.00    4.00    --  109.26 -72.00 -13.00   30
  7  \w     52.00 115.00   1.00    4.00    --  109.26-111.00-180.00   63
  8  \w     39.00 116.00   1.00    4.00    --  109.26-111.00 -30.00   77
  9  \w     51.00  91.00   1.00    4.00    --  109.26 -72.00 -13.00   40
 10  \w     39.00 136.00   1.00    4.00    --  109.26 -30.00  60.00   97
 11  \w     78.00 151.00   1.00    4.00    --  109.26  77.00  60.00   73
 12  \w    147.00 173.00   1.00    4.00    --  109.26  45.00-120.00   26
 13  \w     86.00 140.00   1.00    4.00    --  109.26  45.00-120.00   54
 14  \w     31.00  67.00   1.00    4.00    --  109.26 -94.00   0.00   36
 15  \w     28.00 105.00   1.00    4.00    --  109.26 -94.00  60.00   77
 16  \w     49.00 133.00   1.00    4.00    --  109.26 -61.00 150.00   84
 17  \w     28.00 162.00   1.00    4.00    --  109.26 -15.00-120.00  134
 18  \w   -110.00 -28.00   1.00    1.00    --  -42.88 -57.00 -90.00   82
 19  \w   -116.00 -89.00   1.00    1.00    --  -42.88 -99.00  60.00   27
 20  \w   -117.00 -86.00   1.00    1.00    --  -42.88 -99.00   0.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28537
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.288
_diffrn_reflns_theta_min         4.451
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.149
_exptl_absorpt_correction_T_max  0.182
_exptl_absorpt_correction_T_min  0.014
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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_colour            green
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       prism
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.693
_exptl_crystal_size_mid          0.407
_exptl_crystal_size_min          0.278
_refine_diff_density_max         4.201
_refine_diff_density_min         -5.287
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         15609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1158P)^2^+13.9827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14724
_reflns_number_total             15609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07885_si_006.cif
_cod_data_source_block           rf298
_cod_database_code               4133017
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.043
_shelx_estimated_absorpt_t_max   0.133
_shelx_res_checksum              54693
_shelx_hkl_checksum              34225
_shelx_fab_checksum              56202
_publcif_funding_html
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