The Pauson-Khand Reaction: A Gas-Phase and Solution-Phase Examination Using Electrospray Ionization Mass Spectrometry
Henderson, Matthew A.; Luo, Jingwei; Oliver, Allen; McIndoe, J. Scott; Organometallics 30 (2011) 5471–; doi:10.1021/om200717r

data_4065325
_publ_section_title
;
 The Pauson-Khand Reaction: A Gas-Phase and Solution-Phase Examination
 Using Electrospray Ionization Mass Spectrometry
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5471
_journal_paper_doi               10.1021/om200717r
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C24 H20 B, C14 H14 Co2 N O6'
_chemical_formula_sum            'C38 H34 B Co2 N O6'
_chemical_formula_weight         729.33
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.705(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.100(2)
_cell_length_b                   10.9572(11)
_cell_length_c                   17.5214(18)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.27
_cell_measurement_theta_min      2.28
_cell_volume                     3357.5(6)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48069
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_T_max  0.9310
_exptl_absorpt_correction_T_min  0.7462
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0454P)^2^+1.6213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                5985
_reflns_number_total             6896
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200717r_si_002.cif
_cod_data_source_block           cmpd1
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4065325