Rhodium Catalyzed, Carbon‒Hydrogen Bond Directed Hydrodefluorination of Fluoroarenes
Ekkert, Olga; Strudley, Sebastian D. A.; Rozenfeld, Alisa; White, Andrew J. P.; Crimmin, Mark R.; Organometallics 33 (2014) 7027–; doi:10.1021/om501113j

data_4085044
_publ_section_title
;
 Rhodium Catalyzed, Carbon--Hydrogen Bond Directed Hydrodefluorination of
 Fluoroarenes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7027
_journal_paper_doi               10.1021/om501113j
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C33 H47 Al Cl N2 Rh, C7 H8'
_chemical_formula_sum            'C40 H55 Al Cl N2 Rh'
_chemical_formula_weight         729.20
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7070(3)
_cell_length_b                   16.7439(4)
_cell_length_c                   15.6675(3)
_cell_measurement_reflns_used    6497
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.3680
_cell_measurement_theta_min      2.4910
_cell_volume                     3858.16(14)
_computing_cell_refinement       CrysAlisPro,
_computing_data_collection       CrysAlisPro,
_computing_data_reduction        CrysAlisPro,
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18497
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.427
_diffrn_reflns_theta_min         2.600
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            Yellow-brown
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       'blocky needles'
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4176
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+3.8791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3454
_reflns_number_total             4176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501113j_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 4085044.cif.'
_cod_original_cell_volume        3858.17(14)
_cod_database_code               4085044
_shelxl_version_number           2013-4