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_4133015
_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_sum            'C34 H51 K N5 O12 U'
_chemical_formula_weight         998.92
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-05-23 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 107.908(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      32.0020
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_cell_volume                     4382.77(16)
_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 0.924
_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     -8.00  93.00   1.00   12.80    --   19.91  57.00 -30.00  101
  2  \w     -8.00  57.00   1.00   12.80    --   19.91  77.00  60.00   65
  3  \w    -52.00  49.00   1.00   12.80    --   19.91 -19.00 150.00  101
  4  \w    -23.00  11.00   1.00   12.80    --  -20.22 -77.00  90.00   34
  5  \w    -95.00 -66.00   1.00   12.80    --  -20.22 -77.00  90.00   29
  6  \w     34.00  95.00   1.00   12.80    --   19.91-178.00-150.00   61
  7  \w   -100.00 -72.00   1.00   12.80    --  -20.22 178.00  90.00   28
;
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54935
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.948
_diffrn_reflns_theta_min         2.640
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.857
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.512
_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 pale blue'
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       prism
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.129
_refine_diff_density_max         1.808
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         15207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+4.1066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0643
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11915
_reflns_number_total             15207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07885_si_005.cif
_cod_data_source_block           rf291
_cod_original_cell_volume        4382.75(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4133015
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.367
_shelx_estimated_absorpt_t_max   0.636
_shelx_res_checksum              22921
_shelx_hkl_checksum              83598
_shelx_fab_checksum              43884
_publcif_funding_html
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