Intermolecular Alkyne Hydroacylation. Mechanistic Insight from the Isolation of the Vinyl Intermediate That Precedes Reductive Elimination
Pawley, Rebekah J.; Huertos, Miguel A.; Lloyd-Jones, Guy C.; Weller, Andrew S.; Willis, Michael C.; Organometallics 31 (2012) 5650–; doi:10.1021/om300647n

data_4078972
_publ_section_title
;
 Intermolecular Alkyne Hydroacylation. Mechanistic Insight from the
 Isolation of the Vinyl Intermediate That Precedes Reductive Elimination
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              5650
_journal_paper_doi               10.1021/om300647n
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C54 H40 F6 O2 P2 Rh S, B12 H12, 2(C H2 Cl2)'
_chemical_formula_sum            'C56 H56 B12 Cl4 F6 O2 P2 Rh S'
_chemical_formula_weight         1343.44
_chemical_melting_point          ?
_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                104.2065(7)
_cell_angle_beta                 113.9716(6)
_cell_angle_gamma                105.7943(7)
_cell_formula_units_Z            2
_cell_length_a                   14.31300(20)
_cell_length_b                   15.74190(20)
_cell_length_c                   16.96970(29)
_cell_measurement_reflns_used    12642
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     3073.92(9)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23797
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         5.10
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1362
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         14009
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+3.4499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                11362
_reflns_number_total             14009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300647n_si_004.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3073.922(87)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4078972