Insertion, Isomerization, and Cascade Reactivity of the Tethered Silylalkyl Uranium Metallocene (η5-C5Me4SiMe2CH2-κC)2U
Nathan A. Siladke; Joseph W. Ziller; William J. Evans; Journal of the American Chemical Society 133 (2011) 3507–3516; doi:10.1021/ja109491k

data_4105736
_publ_section_title
;
 Insertion, Isomerization, and Cascade Reactivity of the Tethered
 Silylalkyl Uranium Metallocene (\h5-C5Me4SiMe2CH2-\kC)2U
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3507
_journal_page_last               3516
_journal_paper_doi               10.1021/ja109491k
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C66 H108 N4 O4 Si4 U2'
_chemical_formula_weight         1609.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 95.2545(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9569(9)
_cell_length_b                   19.1828(11)
_cell_length_c                   24.7740(15)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    148(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.28
_cell_volume                     7078.2(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  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      148(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40368
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    4.683
_exptl_absorpt_correction_T_max  0.6268
_exptl_absorpt_correction_T_min  0.3994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         8251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+10.7157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0444
_reflns_number_gt                7636
_reflns_number_total             8251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109491k_si_003.cif
_cod_data_source_block           nas22
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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               4105736