Synthesis of Heteroleptic Uranium (μ-η6:η6-C6H6)2- Sandwich Complexes via Facile Displacement of (η5-C5Me5)1- by Ligands of Lower Hapticity and Their Conversion to Heteroleptic Bis(imido) Compounds
William J. Evans; Christopher A. Traina; Joseph W. Ziller; Journal of the American Chemical Society 131 (2009) 17473–17481; doi:10.1021/ja9075259

data_4105407
_publ_section_title
;
 Synthesis of Heteroleptic Uranium (\m-\h6:\h6-C6H6)2- Sandwich Complexes
 via Facile Displacement of (\h5-C5Me5)1- by Ligands of Lower Hapticity
 and Their Conversion to Heteroleptic Bis(imido) Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17473
_journal_page_last               17481
_journal_paper_doi               10.1021/ja9075259
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C40 H74 Si4 U2'
_chemical_formula_weight         1143.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                99.8602(3)
_cell_angle_beta                 104.2888(3)
_cell_angle_gamma                99.0500(3)
_cell_formula_units_Z            1
_cell_length_a                   8.6310(3)
_cell_length_b                   11.2450(3)
_cell_length_c                   12.1742(4)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.28
_cell_volume                     1103.19(6)
_computing_cell_refinement       'Bruker SMART APEX2/SAINT'
_computing_data_collection       'Bruker SMART APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'phi and omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0133
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12615
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    7.464
_exptl_absorpt_correction_T_max  0.5695
_exptl_absorpt_correction_T_min  0.2674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.247
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0138
_refine_ls_R_factor_gt           0.0132
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+0.4257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0327
_refine_ls_wR_factor_ref         0.0329
_reflns_number_gt                4855
_reflns_number_total             4998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9075259_si_002_1.cif
_cod_data_source_block           cat10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4105407