Oxidative Addition of a Strained C-C Bond onto Electron-Rich Rhodium(I) at Room Temperature
Yusuke Masuda; Maki Hasegawa; Makoto Yamashita; Kyoko Nozaki; Naoki Ishida; Masahiro Murakami; Journal of the American Chemical Society 135 (2013) 7142–7145; doi:10.1021/ja403461f

data_4119754
_publ_section_title
;
 Oxidative Addition of a Strained C-C Bond onto Electron-Rich Rhodium(I)
 at Room Temperature
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7142
_journal_page_last               7145
_journal_paper_doi               10.1021/ja403461f
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C32 H50 B N2 O P2 Rh'
_chemical_formula_weight         654.40
_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                84.987(7)
_cell_angle_beta                 89.233(7)
_cell_angle_gamma                80.471(6)
_cell_formula_units_Z            4
_cell_length_a                   12.139(3)
_cell_length_b                   12.768(3)
_cell_length_c                   21.324(6)
_cell_measurement_reflns_used    12260
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      31.4
_cell_measurement_theta_min      1.9
_cell_volume                     3247.0(14)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'RIGAKU/MSCIO Saturn CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22309
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.9377
_exptl_absorpt_correction_T_min  0.8808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       Block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         11221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0654P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1086
_reflns_number_gt                9843
_reflns_number_total             11221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja403461f_si_002.cif
_cod_data_source_block           pbprh
_cod_database_code               4119754