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_4071840
_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            'C56 H100 Cl3 Li O9 Si2 U2'
_chemical_formula_weight         1562.89
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.896(7)
_cell_length_b                   9.601(2)
_cell_length_c                   39.433(8)
_cell_measurement_reflns_used    29898
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.12
_cell_volume                     12854(5)
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 1999)'
_computing_data_reduction        'DENZO HKL2000 (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      220(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       phi-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_sigmaI/netI    0.1061
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            28640
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.244
_exptl_absorpt_correction_T_max  0.81426
_exptl_absorpt_correction_T_min  0.40118
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6192
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.525
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         11222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.819
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0006P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                3388
_reflns_number_total             11222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800418u_si_001.cif
_cod_data_source_block           aswini
_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      ' C 2/c'
_cod_database_code               4071840