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_4105409
_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            'C41 H69 N4 U'
_chemical_formula_weight         856.03
_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                92.8200(10)
_cell_angle_beta                 91.4350(10)
_cell_angle_gamma                116.5340(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9380(7)
_cell_length_b                   10.8469(8)
_cell_length_c                   20.2681(19)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    148(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.27
_cell_volume                     1949.6(3)
_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  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      148(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22088
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    4.195
_exptl_absorpt_correction_T_max  0.6554
_exptl_absorpt_correction_T_min  0.3759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.175
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         8483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0169
_refine_ls_R_factor_gt           0.0159
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+0.7469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0389
_refine_ls_wR_factor_ref         0.0393
_reflns_number_gt                8174
_reflns_number_total             8483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9075259_si_002_3.cif
_cod_data_source_block           cat19
_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               4105409