Unprecedented Bending and Rearrangement of f-Element Sandwich Complexes Induced by Superbulky Cyclooctatetraenide Ligands
Volker Lorenz; Benjamin M. Schmiege; Cristian G. Hrib; Joseph W. Ziller; Anja Edelmann; Steffen Blaurock; William J. Evans; Frank T. Edelmann; Journal of the American Chemical Society 133 (2011) 1257–1259; doi:10.1021/ja109604t

data_4105595
_publ_section_title
;
 Unprecedented Bending and Rearrangement of f-Element Sandwich Complexes
 Induced by Superbulky Cyclooctatetraenide Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1257
_journal_page_last               1259
_journal_paper_doi               10.1021/ja109604t
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C44 H38 Si2'
_chemical_formula_weight         622.92
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.83(3)
_cell_angle_beta                 69.82(3)
_cell_angle_gamma                89.81(3)
_cell_formula_units_Z            2
_cell_length_a                   10.125(2)
_cell_length_b                   13.433(3)
_cell_length_c                   13.925(3)
_cell_measurement_reflns_used    1278
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.66
_cell_volume                     1777.3(7)
_computing_cell_refinement       'Stoe CELL'
_computing_data_collection       'Stoe EXPOSE'
_computing_data_reduction        'Stoe INTEGRATE'
_computing_molecular_graphics    'Bruker SHELXTL PLUS'
_computing_publication_material  'Bruker SHELXTL PLUS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Stoe IPDS 1'
_diffrn_measurement_method       Phi-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
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_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
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_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       platelet
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.870
_refine_ls_hydrogen_treatment    refall
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_refine_ls_number_reflns         5885
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                3970
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109604t_si_002.cif
_cod_data_source_block           ip1_164a
_cod_original_cell_volume        1777.4(6)
_cod_database_code               4105595