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_4085327
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H65 N1 Si2 U1, C5 H12 O1'
_chemical_formula_sum            'C41 H77 N O Si2 U'
_chemical_formula_weight         894.25
_chemical_name_common            complex_2_amide
_chemical_name_systematic
;
amido(eta-5-pentamethylcyclopentadienyl)
(eta-8-(bis{triisopropylsilyl}cyclooctatetraene))uranium(IV)
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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      2.4
_audit_creation_date             2012-09-07T13:02:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.0660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.22460(10)
_cell_length_b                   20.7046(3)
_cell_length_c                   11.5888(2)
_cell_measurement_reflns_used    3338
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     2172.21(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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 Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.200729E-1
_diffrn_orient_matrix_UB_12      0.22958E-2
_diffrn_orient_matrix_UB_13      -0.816875E-1
_diffrn_orient_matrix_UB_21      0.108616
_diffrn_orient_matrix_UB_22      0
_diffrn_orient_matrix_UB_23      0.322932E-1
_diffrn_orient_matrix_UB_31      0.9552E-3
_diffrn_orient_matrix_UB_32      -0.482439E-1
_diffrn_orient_matrix_UB_33      -0.38872E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31233
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         3.45
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.82
_exptl_absorpt_correction_T_max  0.7084
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.036
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+2.1203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0617
_reflns_number_gt                4346
_reflns_number_total             4900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501190x_si_002.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 4085327--4085328.cif.'
_cod_original_formula_sum        'C41 H77 N1 O1 Si2 U1'
_cod_database_code               4085327