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_4133016
_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 D2 N3 O7 U, 4(D2 O)'
_chemical_formula_sum            'C16 H15 D10 N3 O11 U'
_chemical_formula_weight         683.48
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                67.959(7)
_cell_angle_beta                 81.512(10)
_cell_angle_gamma                82.702(10)
_cell_formula_units_Z            2
_cell_length_a                   6.8944(8)
_cell_length_b                   11.1491(12)
_cell_length_c                   14.7213(15)
_cell_measurement_reflns_used    74
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     1034.2(2)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_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_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17879
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.885
_exptl_absorpt_coefficient_mu    7.912
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0990 before and 0.0695 after correction.
The Ratio of minimum to maximum transmission is 0.6814.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.195
_exptl_crystal_description       prism
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.195
_refine_diff_density_max         1.955
_refine_diff_density_min         -2.430
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6005
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0281P)^2^+3.8466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5287
_reflns_number_total             6005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07885_si_003.cif
_cod_data_source_block           rf252
_cod_database_code               4133016
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.274
_shelx_estimated_absorpt_t_max   0.308
_shelx_res_checksum              76975
_shelx_hkl_checksum              61459