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_4081626
_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         'C40 H70 O Si2 U'
_chemical_formula_sum            'C40 H70 O Si2 U'
_chemical_formula_weight         861.17
_chemical_name_common            complex_6_tuckin_THF
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2012-03-28T10:14:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.1640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0255(2)
_cell_length_b                   15.0113(3)
_cell_length_c                   22.2071(5)
_cell_measurement_reflns_used    29311
_cell_measurement_temperature    173(2)
_cell_volume                     4007.96(14)
_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 0.996
_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      0.480944E-1
_diffrn_orient_matrix_UB_12      -0.484014E-1
_diffrn_orient_matrix_UB_13      -0.161831E-1
_diffrn_orient_matrix_UB_21      0.449259E-1
_diffrn_orient_matrix_UB_22      0
_diffrn_orient_matrix_UB_23      0.383908E-1
_diffrn_orient_matrix_UB_31      -0.508574E-1
_diffrn_orient_matrix_UB_32      -0.457718E-1
_diffrn_orient_matrix_UB_33      0.171129E-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  0.0721
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26878
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         3.48
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.137
_exptl_absorpt_correction_T_max  0.8128
_exptl_absorpt_correction_T_min  0.7485
_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    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.032
_refine_diff_density_min         -1.871
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         8834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0245P)^2^+11.1568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                6260
_reflns_number_total             8834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400720m_si_002.cif
_cod_data_source_block           6THF
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4081626