Mechanism of Formation of [(PMe3)3Rh(-C≡C-R)2(H)] via C-H Oxidative Addition: Isomerization, Alkyne Exchange, and Hydride Replacement
Jonathan P. Rourke; Graham Stringer; Pauline Chow; Robert J. Deeth; Dmitri S. Yufit; Judith A. K. Howard; Todd B. Marder; Organometallics 21 (2002) 429–437; doi:10.1021/om010685r

data_4063219
_publ_section_title
;
 Mechanism of Formation of [(PMe3)3Rh(-C\\tb C-R)2(H)] via C-H
 Oxidative Addition: Isomerization, Alkyne Exchange, and Hydride
 Replacement
;
_journal_name_full               Organometallics
_journal_page_first              429
_journal_page_last               437
_journal_paper_doi               10.1021/om010685r
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C27 H41 Cl O2 P3 Rh'
_chemical_formula_weight         628.87
_chemical_name_systematic
;
mer-trans-tris(rimethylphosphine)-bis-
-(4-methoxyphenylethynyl)rhodium chloride
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.708(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5752(6)
_cell_length_b                   11.7546(4)
_cell_length_c                   13.8703(5)
_cell_measurement_reflns_used    6850
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      59.81
_cell_measurement_theta_min      4.55
_cell_volume                     3013.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120.0(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker SMART CCD 1K'
_diffrn_measurement_method       \w-scan
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34012
_diffrn_reflns_theta_full        30.36
_diffrn_reflns_theta_max         30.36
_diffrn_reflns_theta_min         1.10
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.7860
_exptl_absorpt_correction_T_min  0.5832
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker XPREP'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+1.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                7768
_reflns_number_total             8280
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4060832
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               4063219