ESI-MS, DFT, and Synthetic Studies on the H2-Mediated Coupling of Acetylene: Insertion of C=X Bonds into Rhodacyclopentadienes and Brønsted Acid Cocatalyzed Hydrogenolysis of Organorhodium Intermediates
Vanessa M. Williams; Jong Rock Kong; Byoung Joon Ko; Yogita Mantri; Jennifer S. Brodbelt; Mu-Hyun Baik; Michael J. Krische; Journal of the American Chemical Society 131 (2009) 16054–16062; doi:10.1021/ja906225n

data_4105299
_publ_section_title
;
 ESI-MS, DFT, and Synthetic Studies on the H2-Mediated Coupling of
 Acetylene: Insertion of C=X Bonds into Rhodacyclopentadienes and
 Br\/onsted Acid Cocatalyzed Hydrogenolysis of Organorhodium Intermediates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16054
_journal_page_last               16062
_journal_paper_doi               10.1021/ja906225n
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C16 H21 N O4 S'
_chemical_formula_weight         323.40
_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                75.976(3)
_cell_angle_beta                 82.396(3)
_cell_angle_gamma                74.390(4)
_cell_formula_units_Z            2
_cell_length_a                   8.5116(6)
_cell_length_b                   8.5340(6)
_cell_length_c                   11.9392(10)
_cell_measurement_reflns_used    2708
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     808.26(11)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w-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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3595
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       plates
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       0.29(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   3.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      3.102
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.1255
_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^)+(0.0200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2114
_reflns_number_gt                2969
_reflns_number_total             3596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906225n_si_001.cif
_cod_data_source_block           vw1116
_cod_database_code               4105299