Cyclometalation Reactions on Rhodium(I). Evidence for a Chelate Effect and Competing C−H and C−O Oxidative Additions
Sjövall, Sven; Andersson, Carlaxel; Wendt, Ola F.; Organometallics 20 (2001) 4919–; doi:10.1021/om010543x

data_4077405
_publ_section_title
;
 Cyclometalation Reactions on Rhodium(I). Evidence for a Chelate Effect
 and Competing C&#x2212;H and C&#x2212;O Oxidative Additions
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              4919
_journal_paper_doi               10.1021/om010543x
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C49 H48 B F4 N O P3 Rh'
_chemical_formula_weight         949.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.4390(10)
_cell_angle_beta                 84.3880(10)
_cell_angle_gamma                71.0460(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4318(6)
_cell_length_b                   13.0682(6)
_cell_length_c                   15.9971(8)
_cell_measurement_reflns_used    3663
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.026
_cell_measurement_theta_min      4.623
_cell_volume                     2246.55(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond (Brandenburg)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_sigmaI/netI    0.1787
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23520
_diffrn_reflns_theta_full        31.82
_diffrn_reflns_theta_max         31.82
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.934552
_exptl_absorpt_correction_T_min  0.780455
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'absorption corrections using SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         13576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.1755
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                5683
_reflns_number_total             13576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010543x.cif
_cod_data_source_block           dppeRh(PNO)-complex3b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077405