Coordinative Unsaturation versus Oxophilicity:ansaDimethylsilyl Oxo-Bridged Uranium Metallocenes. Synthesis, Structures, and Unexpected Catalytic Activity with Alkynes and Silanes
Wang, Jiaxi; Gurevich, Ylia; Botoshansky, Mark; Eisen, Moris S.; Organometallics 27 (2008) 4494–; doi:10.1021/om800418u

data_4071841
_publ_section_title
;
 Coordinative Unsaturation versus Oxophilicity:ansaDimethylsilyl
 Oxo-Bridged Uranium Metallocenes. Synthesis, Structures, and Unexpected
 Catalytic Activity with Alkynes and Silanes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4494
_journal_paper_doi               10.1021/om800418u
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C42 H65 Cl3 Li O2 Si2 U2'
_chemical_formula_weight         1247.47
_chemical_name_common            Uran-lithium
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.33(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.052(3)
_cell_length_b                   10.636(2)
_cell_length_c                   28.982(6)
_cell_measurement_reflns_used    37581
_cell_measurement_temperature    230(1)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      1.36
_cell_volume                     4601.9(16)
_computing_cell_refinement       'DENZO SMN (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 1999)'
_computing_data_reduction        'DENZO SMN (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'TEXSAN  (MSC, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      230(1)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Nonius kappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_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  0.1020
_diffrn_reflns_av_sigmaI/netI    0.1819
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            22823
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.36
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.288
_exptl_absorpt_correction_T_max  0.558
_exptl_absorpt_correction_T_min  0.329
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
  'PLATON (Spek, A.L. 1995)'
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2396
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.399
_refine_diff_density_min         -1.938
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1677
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1513
_reflns_number_gt                3809
_reflns_number_total             7888
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800418u_si_002.cif
_cod_data_source_block           complex31
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4071841