Strain-Induced Cleavage of Carbon-Carbon Bonds: Bridge Rupture Reactions of Group 8 Dicarba[2]metallocenophanes
David E. Herbert; Joe B. Gilroy; Anne Staubitz; Mairi F. Haddow; Jeremy N. Harvey; Ian Manners; Journal of the American Chemical Society 132 (2010) 1988–1998; doi:10.1021/ja9087049

data_4101878
_publ_section_title
;
 Strain-Induced Cleavage of Carbon-Carbon Bonds: Bridge Rupture Reactions
 of Group 8 Dicarba[2]metallocenophanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1988
_journal_page_last               1998
_journal_paper_doi               10.1021/ja9087049
_journal_volume                  132
_journal_year                    2010
_chemical_absolute_configuration uk
_chemical_formula_moiety         'C20 H28 Fe'
_chemical_formula_sum            'C20 H28 Fe'
_chemical_formula_weight         324.27
_chemical_name_common            rac-1,1'-ditertbutylethylenylferrocene
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 97.722(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   31.1903(13)
_cell_length_b                   9.7393(4)
_cell_length_c                   8.3897(3)
_cell_measurement_reflns_used    3828
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.19
_cell_volume                     2525.44(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.809
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4409
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         33.81
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS v2 (Bruker AXS, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4409
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+6.2880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1507
_reflns_number_gt                3699
_reflns_number_total             4409
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9087049_si_003.cif
_cod_data_source_block           Fe-tBu_rac_twin5
_cod_database_code               4101878