Identification of the +2 Oxidation State for Uranium in a Crystalline Molecular Complex, [K(2.2.2-Cryptand)][(C5H4SiMe3)3U]
Matthew R. MacDonald; Megan E. Fieser; Jefferson E. Bates; Joseph W. Ziller; Filipp Furche; William J. Evans; Journal of the American Chemical Society 135 (2013) 13310–13313; doi:10.1021/ja406791t

data_4120775
_publ_section_title
;
 Identification of the +2 Oxidation State for Uranium in a Crystalline
 Molecular Complex, [K(2.2.2-Cryptand)][(C5H4SiMe3)3U]
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13310
_journal_page_last               13313
_journal_paper_doi               10.1021/ja406791t
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C46 H83 K N2 O7 Si3 U'
_chemical_formula_weight         1137.54
_chemical_name_systematic
; 
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.7714(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9554(14)
_cell_length_b                   24.433(2)
_cell_length_c                   13.7743(12)
_cell_measurement_reflns_used    9748
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.68
_cell_measurement_theta_min      2.56
_cell_volume                     5369.3(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10983
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.697
_exptl_absorpt_coefficient_mu    3.213
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker TWINABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.556
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         10983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0171P)^2^+6.5163P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10019
_reflns_number_total             10983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja406791t_si_003.cif
_cod_data_source_block           mrm45
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4120775
_shelx_estimated_absorpt_t_min   0.495
_shelx_estimated_absorpt_t_max   0.752
_shelxl_version_number           2013-2
_shelx_res_checksum              1055