Activation and reduction of diethyl ether by low valent uranium: formation of the trimetallic, mixed valence uranium oxo species [U(CpRR')(μ-I)2]3(μ3-O) (CpRR' = C5Me5, C5Me4H, C5H4SiMe3)
Larch, Christopher P.; Cloke, F. Geoffrey N.; Hitchcock, Peter B.; Chemical Communications (Cambridge, United Kingdom)  (2008) 82–84; doi:10.1039/b714211k

data_7113146
_publ_section_title
;
 Activation and reduction of diethyl ether by low valent uranium:
 formation of the trimetallic, mixed valence uranium oxo species
 [U(CpRR')(\m-I)2]3(\m3-O) (CpRR' = C5Me5, C5Me4H, C5H4SiMe3)
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   1
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              82
_journal_page_last               84
_journal_paper_doi               10.1039/b714211k
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H39 I6 O Si3 U3'
_chemical_formula_sum            'C24 H39 I6 O Si3 U3'
_chemical_formula_weight         1903.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2005-12-13T09:32:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.745(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7070(3)
_cell_length_b                   8.3748(1)
_cell_length_c                   31.3762(4)
_cell_measurement_reflns_used    173999
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     4281.92(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.322147E-1
_diffrn_orient_matrix_UB_12      0.614807E-1
_diffrn_orient_matrix_UB_13      0.253842E-1
_diffrn_orient_matrix_UB_21      0.518921E-1
_diffrn_orient_matrix_UB_22      -0.268517E-1
_diffrn_orient_matrix_UB_23      -0.93344E-2
_diffrn_orient_matrix_UB_31      -0.59446E-2
_diffrn_orient_matrix_UB_32      0.987768E-1
_diffrn_orient_matrix_UB_33      -0.183372E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1254
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            61341
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         3.45
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    15.745
_exptl_absorpt_correction_T_max  0.7279
_exptl_absorpt_correction_T_min  0.0354
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3308
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.959
_refine_diff_density_min         -2.543
_refine_diff_density_rms         0.333
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         8349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+20.2028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.11
_refine_ls_wR_factor_ref         0.1182
_reflns_number_gt                6849
_reflns_number_total             8349
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7102773
_cod_data_source_file            b714211k.txt
_cod_data_source_block           dec705
_cod_database_code               7113146