Energetics of C-H Bond Activation of Fluorinated Aromatic Hydrocarbons Using a [Tp'Rh(CNneopentyl)] Complex
Meagan E. Evans; Catherine L. Burke; Sornanong Yaibuathes; Eric Clot; Odile Eisenstein; William D. Jones; Journal of the American Chemical Society 131 (2009) 13464–13473; doi:10.1021/ja905057w

data_4105030
_publ_contact_author_address
'Department of Chemistry, University of Rochester, Rochester, New York 14627'
_publ_contact_author_email       jones@chem.rochester.edu
_publ_contact_author_name        'William D. Jones'
_publ_section_title
;
 Energetics of C-H Bond Activation of Fluorinated Aromatic Hydrocarbons
 Using a [Tp'Rh(CNneopentyl)] Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13464
_journal_page_last               13473
_journal_paper_doi               10.1021/ja905057w
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C27 H33 B Cl F5 N7 Rh'
_chemical_formula_sum            'C27 H33 B Cl F5 N7 Rh'
_chemical_formula_weight         699.77
_chemical_name_common            'jonme05, 2-Cl'
_chemical_name_systematic
;
 Tp'Rh(CNR)(C6F5)Cl
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 98.717(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0818(7)
_cell_length_b                   17.0067(14)
_cell_length_c                   21.3708(18)
_cell_measurement_reflns_used    4049
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      2.27
_cell_volume                     2903.4(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.1006
_diffrn_reflns_av_sigmaI/netI    0.0882
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33549
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.9429
_exptl_absorpt_correction_T_min  0.8416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       needle
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         8135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+0.3114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1649
_reflns_number_gt                5096
_reflns_number_total             8135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905057w_si_002.cif
_cod_data_source_block           jonme05
_cod_database_code               4105030