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_4105735
_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            'C24 H40 S4 Si2 U'
_chemical_formula_weight         751.01
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 108.5767(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6639(15)
_cell_length_b                   8.7482(7)
_cell_length_c                   17.1940(13)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.50
_cell_volume                     2803.7(4)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15037
_diffrn_reflns_theta_full        28.19
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    6.185
_exptl_absorpt_correction_T_max  0.6375
_exptl_absorpt_correction_T_min  0.5495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.392
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0162
_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^)+(0.0211P)^2^+2.6551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0369
_refine_ls_wR_factor_ref         0.0376
_reflns_number_gt                3111
_reflns_number_total             3250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109491k_si_002.cif
_cod_data_source_block           nas18
_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 
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_cod_database_code               4105735