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_4077406
_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            'C46.5 H42 B Cl F4 P3 Rh'
_chemical_formula_weight         918.88
_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                75.61(3)
_cell_angle_beta                 87.31(3)
_cell_angle_gamma                71.07(3)
_cell_formula_units_Z            4
_cell_length_a                   14.804(3)
_cell_length_b                   14.977(3)
_cell_length_c                   20.943(4)
_cell_measurement_reflns_used    3612
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.298
_cell_measurement_theta_min      4.366
_cell_volume                     4251.7(18)
_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 0.878
_diffrn_measured_fraction_theta_max 0.878
_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  0.1161
_diffrn_reflns_av_sigmaI/netI    0.4425
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44146
_diffrn_reflns_theta_full        32.11
_diffrn_reflns_theta_max         32.11
_diffrn_reflns_theta_min         1.00
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  0.931664
_exptl_absorpt_correction_T_min  0.787052
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'absorption corrections using SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.170
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.763
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         26150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.763
_refine_ls_R_factor_all          0.2910
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                6723
_reflns_number_total             26150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010543x.cif
_cod_data_source_block           dpperhstyren-complex6
_cod_original_cell_volume        4251.4(15)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C46.50 H42 B Cl F4 P3 Rh'
_cod_database_code               4077406