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_4105598
_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            'C88 H72 Ce Si4'
_chemical_formula_weight         1381.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 112.23(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3200(10)
_cell_length_b                   17.329(2)
_cell_length_c                   16.4549(10)
_cell_measurement_reflns_used    457
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.35
_cell_volume                     3515.9(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      213(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0665
_diffrn_reflns_av_sigmaI/netI    0.1042
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33993
_diffrn_reflns_theta_full        28.18
_diffrn_reflns_theta_max         28.18
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.698
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         8531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.698
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0639
_reflns_number_gt                4653
_reflns_number_total             8531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109604t_si_005.cif
_cod_data_source_block           ip1_346a
_cod_original_cell_volume        3515.8(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4105598