Aliphatic and Aromatic Carbon-Fluorine Bond Activation with Cp*2ZrH2: Mechanisms of Hydrodefluorination
Bradley M. Kraft; Rene J. Lachicotte; William D. Jones; Journal of the American Chemical Society 123 (2001) 10973–10979; doi:10.1021/ja016087l

data_4115766
_publ_section_title
;
 Aliphatic and Aromatic Carbon-Fluorine Bond Activation with Cp*2ZrH2:
 Mechanisms of Hydrodefluorination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10973
_journal_page_last               10979
_journal_paper_doi               10.1021/ja016087l
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C26 H35 F Zr'
_chemical_formula_weight         457.76
_chemical_name_common            Cp*2Zr(o-C6H4F)H
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6842(7)
_cell_length_b                   9.4119(4)
_cell_length_c                   14.7948(6)
_cell_measurement_reflns_used    6626
_cell_measurement_temperature    193(2)
_cell_volume                     2323.23(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10030
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  0.927999
_exptl_absorpt_correction_T_min  0.763861
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          .14
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .30
_refine_diff_density_max         2.499
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3241
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.365
_refine_ls_shift/su_mean         0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1335P)^2^+15.2887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1978
_refine_ls_wR_factor_ref         0.2013
_reflns_number_gt                3074
_reflns_number_total             3241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja016087l_s2_4.cif
_cod_data_source_block           sad1_jonbk19
_cod_database_code               4115766