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_4081629
_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         'C74 H124 O4 Si4 U2, C6 H6'
_chemical_formula_sum            'C80 H130 O4 Si4 U2'
_chemical_formula_weight         1744.26
_chemical_name_common            complex_10_tuckin_CO2
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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             2011-11-18T14:04:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 115.5660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.69590(10)
_cell_length_b                   27.3298(3)
_cell_length_c                   13.4179(2)
_cell_measurement_reflns_used    117685
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      3.395
_cell_volume                     3869.05(9)
_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 0.971
_diffrn_measured_fraction_theta_max 0.971
_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      0.310268E-1
_diffrn_orient_matrix_UB_12      -0.82544E-2
_diffrn_orient_matrix_UB_13      -0.567134E-1
_diffrn_orient_matrix_UB_21      -0.661037E-1
_diffrn_orient_matrix_UB_22      -0.260834E-1
_diffrn_orient_matrix_UB_23      -0.303483E-1
_diffrn_orient_matrix_UB_31      -0.604223E-1
_diffrn_orient_matrix_UB_32      0.242973E-1
_diffrn_orient_matrix_UB_33      -0.51846E-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  0.0792
_diffrn_reflns_av_unetI/netI     0.066
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29297
_diffrn_reflns_theta_full        27.08
_diffrn_reflns_theta_max         27.08
_diffrn_reflns_theta_min         3.4
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.289
_exptl_absorpt_correction_T_max  0.607
_exptl_absorpt_correction_T_min  0.5261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.507
_refine_diff_density_min         -1.928
_refine_diff_density_rms         0.143
_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     406
_refine_ls_number_reflns         8254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+8.4428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.085
_reflns_number_gt                6432
_reflns_number_total             8254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400720m_si_002.cif
_cod_data_source_block           10
_cod_original_cell_volume        3869.05(8)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4081629