Synthesis and Reactivity of a Mixed-Sandwich Uranium(IV) Primary Amido Complex
Higgins Frey, Jessica A.; Cloke, F. Geoffrey N.; Roe, S. Mark; Organometallics 34 (2015) 2102–; doi:10.1021/om501190x

data_4085328
_publ_section_title
;
 Synthesis and Reactivity of a Mixed-Sandwich Uranium(IV) Primary Amido
 Complex
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2102
_journal_paper_doi               10.1021/om501190x
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C37 H65 N O2 Si2 U'
_chemical_formula_sum            'C37 H65 N O2 Si2 U'
_chemical_formula_weight         850.11
_chemical_name_common            complex_3_carbamate
_chemical_name_systematic
;
(kappa-2-carbamato)(eta-5-pentamethylcyclopentadienyl)
(eta-8-(bis{triisopropylsilyl}cyclooctatetraene))uranium(IV)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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             2012-08-30T11:35:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                101.496(7)
_cell_angle_beta                 93.003(7)
_cell_angle_gamma                104.307(7)
_cell_formula_units_Z            2
_cell_length_a                   8.8461(2)
_cell_length_b                   11.9688(3)
_cell_length_c                   19.1218(13)
_cell_measurement_reflns_used    38113
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1911.37(17)
_computing_cell_refinement
;
        CrystalClear-SM Expert 3.1 b10 (Rigaku, 20112)
;
_computing_data_collection
;
        CrystalClear-SM Expert 3.1 b10 (Rigaku, 20112)
;
_computing_data_reduction
;
        CrystalClear-SM Expert 3.1 b10 (Rigaku, 20112)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device
;
        AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
        Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.073232
_diffrn_orient_matrix_UB_12      -0.091122
_diffrn_orient_matrix_UB_13      -0.007938
_diffrn_orient_matrix_UB_21      -0.078524
_diffrn_orient_matrix_UB_22      0.034996
_diffrn_orient_matrix_UB_23      -0.02018
_diffrn_orient_matrix_UB_31      -0.000449
_diffrn_orient_matrix_UB_32      -0.002294
_diffrn_orient_matrix_UB_33      -0.053522
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41797
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    4.339
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Semi-empirical from equivalents
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.737
_refine_diff_density_min         -2.109
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+3.1426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                8243
_reflns_number_total             8721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501190x_si_002.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 4085327--4085328.cif.'
_cod_original_cell_volume        1911.37(15)
_cod_database_code               4085328