Selective C-H Activation of Haloalkanes using a Rhodiumtrispyrazolylborate Complex
Andrew J. Vetter; Ryan D. Rieth; William W. Brennessel; William D. Jones; Journal of the American Chemical Society 131 (2009) 10742–10752; doi:10.1021/ja9002316

data_4104734
_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
;
 Selective C-H Activation of Haloalkanes using a
 Rhodiumtrispyrazolylborate Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10742
_journal_page_last               10752
_journal_paper_doi               10.1021/ja9002316
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C22 H34 B Cl3 N7 Rh'
_chemical_formula_sum            'C22 H34 B Cl3 N7 Rh'
_chemical_formula_weight         616.63
_chemical_name_common            JONAV12
_chemical_name_systematic        Tp*Rh(CNneopentyl)(CHCl2)Cl
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.9000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0905(6)
_cell_length_b                   29.6972(17)
_cell_length_c                   10.6304(6)
_cell_measurement_reflns_used    7500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.72
_cell_measurement_theta_min      2.46
_cell_volume                     2698.4(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0158
_diffrn_reflns_av_sigmaI/netI    0.0111
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            40947
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         31.06
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.955
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, Acta Cryst. (1995) 33'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         8111
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+2.2525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                7747
_reflns_number_total             8111
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9002316_si_002_3.cif
_cod_data_source_block           asd_jonav12
_cod_database_code               4104734