Synthesis and CO2Insertion Chemistry of Uranium(IV) Mixed-Sandwich Alkyl and Hydride Complexes
Higgins, Jessica A.; Cloke, F. Geoffrey N.; Roe, S. Mark; Organometallics 32 (2013) 5244–; doi:10.1021/om400720m

data_4081622
_publ_section_title
;
 Synthesis and CO2Insertion Chemistry of Uranium(IV) Mixed-Sandwich Alkyl
 and Hydride Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5244
_journal_paper_doi               10.1021/om400720m
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C43 H70 Si2 U'
_chemical_formula_sum            'C43 H70 Si2 U'
_chemical_formula_weight         881.2
_chemical_name_common            complex_3_benzyl
_chemical_name_systematic
;
 ?
;
_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      2.4
_audit_creation_date             2011-11-30T16:15:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                82.5670(10)
_cell_angle_beta                 75.3250(10)
_cell_angle_gamma                69.3610(10)
_cell_formula_units_Z            4
_cell_length_a                   12.9743(2)
_cell_length_b                   17.3522(3)
_cell_length_c                   20.0913(4)
_cell_measurement_reflns_used    62514
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     4090.81(13)
_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_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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      0.540793E-1
_diffrn_orient_matrix_UB_12      -0.93059E-2
_diffrn_orient_matrix_UB_13      -0.459121E-1
_diffrn_orient_matrix_UB_21      0.458497E-1
_diffrn_orient_matrix_UB_22      -0.544084E-1
_diffrn_orient_matrix_UB_23      0.179528E-1
_diffrn_orient_matrix_UB_31      -0.459838E-1
_diffrn_orient_matrix_UB_32      -0.274389E-1
_diffrn_orient_matrix_UB_33      -0.149064E-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  0.0632
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59024
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.054
_exptl_absorpt_correction_T_max  0.8827
_exptl_absorpt_correction_T_min  0.6794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.631
_refine_diff_density_min         -1.79
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         18674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.048
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0396P)^2^+5.0333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                15295
_reflns_number_total             18674
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400720m_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        4090.81(12)
_cod_database_code               4081622