Direct observation of key intermediates by negative-ion electrospray ionisation mass spectrometry in palladium-catalysed cross-coupling.
Vikse, Krista L.; Henderson, Matthew A.; Oliver, Allen G.; McIndoe, J. Scott; Chemical communications (Cambridge, England) 46 (2010) 7412–7414; doi:10.1039/c0cc02773a

data_7105661
_publ_section_title
;
 Direct observation of key intermediates by negative-ion electrospray
 ionisation mass spectrometry in palladium-catalysed cross-coupling.
;
_journal_issue                   39
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7412
_journal_page_last               7414
_journal_paper_doi               10.1039/c0cc02773a
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C36 H30 N P2, C18 H14 O3 P S'
_chemical_formula_sum            'C54 H44 N O3 P3 S'
_chemical_formula_weight         879.87
_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                104.5580(10)
_cell_angle_beta                 96.5030(10)
_cell_angle_gamma                99.5370(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2219(12)
_cell_length_b                   15.1177(17)
_cell_length_c                   15.1616(17)
_cell_measurement_reflns_used    9338
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     2206.7(4)
_computing_cell_refinement       'Bruker SAINT v7.53A'
_computing_data_collection       'Bruker APEX-II v2008-6'
_computing_data_reduction        'Bruker SAINT v7.53A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w and \f-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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25164
_diffrn_reflns_theta_full        28.47
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.9599
_exptl_absorpt_correction_T_min  0.9407
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         10846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0470P)^2^+0.8642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                9273
_reflns_number_total             10846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC02773A.TXT
_cod_data_source_block           jsm009
_cod_depositor_comments          'Adding full bibliography for 7105661.cif.'
_cod_database_code               7105661