X-ray Crystallographic and NMR Spectroscopic Study of (η2-Alkene)(μ-alkyne)pentacarbonyldicobalt Complexes: Arrested Pauson−Khand Reaction Intermediates
Brusey, Sarah A.; Banide, Emilie V.; Dörrich, Steffen; O’Donohue, Paul; Ortin, Yannick; Müller-Bunz, Helge; Long, Conor; Evans, Paul; McGlinchey, Michael J.; Organometallics 28 (2009) 6308–; doi:10.1021/om900615m

data_4070113
_publ_section_title
;
 X-ray Crystallographic and NMR Spectroscopic Study of
 (\h2-Alkene)(\m-alkyne)pentacarbonyldicobalt Complexes: Arrested
 Pauson&#x2212;Khand Reaction Intermediates
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6308
_journal_paper_doi               10.1021/om900615m
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C18 H14 O'
_chemical_formula_sum            'C18 H14 O'
_chemical_formula_weight         246.29
_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                 101.579(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5912(14)
_cell_length_b                   13.8714(16)
_cell_length_c                   8.0454(9)
_cell_measurement_reflns_used    5427
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.96
_cell_measurement_theta_min      2.32
_cell_volume                     1267.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            30199
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         32.02
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9619
_exptl_absorpt_correction_T_min  0.9134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS v.2.10 (Bruker,2003) was used for absorption correction. 
 R(int) for selected reflections was 0.066 before and 0.027 after 
 correction. The Ratio of minimum to maximum transmission is 0.949619. 
 The \l/2 correction factor is 0.0015 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0851P)^2^+0.2850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                3763
_reflns_number_total             4213
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900615m_si_002.cif
_cod_data_source_block           mjm258
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4070113