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_4115764
_publ_section_title
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 Aliphatic and Aromatic Carbon-Fluorine Bond Activation with Cp*2ZrH2:
 Mechanisms of Hydrodefluorination
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_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            'C20 H30 F Zr'
_chemical_formula_weight         380.66
_chemical_name_common            Cp*2ZrHF
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.4715(7)
_cell_length_b                   15.6123(7)
_cell_length_c                   15.7459(7)
_cell_measurement_reflns_used    7814
_cell_measurement_temperature    193(2)
_cell_volume                     3803.4(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens SMART CCD area detector'
_diffrn_measurement_method       'w 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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16660
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.9279
_exptl_absorpt_correction_T_min  0.8018
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    NA
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.290
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.13(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.004
_refine_ls_goodness_of_fit_obs   1.032
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_restrained_S_obs      1.032
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_obs          0.0491
_refine_ls_shift/esd_max         0.017
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+5.3642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1231
_refine_ls_wR_factor_obs         0.1174
_reflns_number_observed          4723
_reflns_number_total             5442
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja016087l_s2_2.cif
_cod_data_source_block           sad1_jonbk03
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NA' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+5.3642P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+5.3642P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4115764