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_4133014
_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         'C16 H15 N3 O6 U, C20 H30 Co, 4(C5 H5 N)'
_chemical_formula_sum            'C56 H65 Co N7 O6 U'
_chemical_formula_weight         1229.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-06-05 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3320(5)
_cell_length_b                   20.4637(7)
_cell_length_c                   18.2836(5)
_cell_measurement_reflns_used    14710
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.3500
_cell_measurement_theta_min      3.8980
_cell_volume                     5362.3(3)
_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 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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    -62.00  31.00   1.00    5.00    --  -40.41  57.00  90.00   93
  2  \w     12.00  39.00   1.00    5.00    --   40.41 -99.00 150.00   27
  3  \w     51.00  85.00   1.00    5.00    --   40.41-125.00  30.00   34
  4  \w     79.00 117.00   1.00   20.00    --  107.03-125.00  30.00   38
  5  \w     63.00 108.00   1.00   20.00    --  107.03 -94.00-120.00   45
  6  \w     75.00 121.00   1.00   20.00    --  107.03-125.00-180.00   46
  7  \w     36.00 126.00   1.00   20.00    --  107.03 -61.00-120.00   90
  8  \w     79.00 149.00   1.00   20.00    --  107.03  30.00-150.00   70
  9  \w    132.00 159.00   1.00   20.00    --  107.03 125.00  60.00   27
 10  \w    139.00 168.00   1.00   20.00    --  107.03  45.00 150.00   29
 11  \w     81.00 126.00   1.00   20.00    --  107.03  45.00 150.00   45
 12  \w     41.00 134.00   1.00   20.00    --  107.03 -61.00 120.00   93
 13  \w     32.00 132.00   1.00   20.00    --  107.03 -30.00 -30.00  100
 14  \w     34.00 140.00   1.00   20.00    --  107.03 -77.00   0.00  106
 15  \w     25.00 153.00   1.00   20.00    --  107.03 -15.00-180.00  128
 16  \w      1.00  81.00   1.00    5.00    --   40.41 -99.00-180.00   80
 17  \w   -115.00 -21.00   1.00    5.00    --  -40.41 -38.00 -60.00   94
 18  \w   -113.00 -22.00   1.00    5.00    --  -40.41 -38.00-150.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_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_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9930
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.792
_diffrn_reflns_theta_min         3.241
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.302
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.107
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense green'
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       prism
_exptl_crystal_F_000             2468
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.111
_refine_diff_density_max         7.794
_refine_diff_density_min         -3.065
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         9930
_refine_ls_number_restraints     586
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0856
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1176P)^2^+68.6276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9024
_reflns_number_total             9930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07885_si_004.cif
_cod_data_source_block           RF191
_cod_database_code               4133014
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.076
_shelx_estimated_absorpt_t_max   0.367
_shelx_res_checksum              1477
_shelx_hkl_checksum              62441
_publcif_funding_html
;
;