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_4105408
_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            'C56 H82 O2 U2'
_chemical_formula_weight         1263.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.3839(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.0169(17)
_cell_length_b                   17.007(3)
_cell_length_c                   13.543(2)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.20
_cell_volume                     2537.4(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26811
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    6.413
_exptl_absorpt_correction_T_max  0.6054
_exptl_absorpt_correction_T_min  0.3461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.305
_refine_diff_density_min         -4.523
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         5199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+69.1063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                4590
_reflns_number_total             5199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9075259_si_002_2.cif
_cod_data_source_block           cat11
_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_original_cell_volume        2537.3(7)
_cod_database_code               4105408