The Synthesis of a Dicyclopenta[a,e]pentalene via a Molybdenum Hexacarbonyl-Mediated Tandem Allenic Pauson-Khand Reaction1
Hui Cao; Judith Flippen-Anderson; James M. Cook; Journal of the American Chemical Society 125 (2003) 3230–3231; doi:10.1021/ja021159+

data_4113555
_publ_section_title
;
 The Synthesis of a Dicyclopenta[a,e]pentalene via a Molybdenum
 Hexacarbonyl-Mediated Tandem Allenic Pauson-Khand Reaction1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3230
_journal_page_last               3231
_journal_paper_doi               10.1021/ja021159+
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C39 H56 O4 Si2'
_chemical_formula_weight         645.02
_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                105.0370(10)
_cell_angle_beta                 102.0660(10)
_cell_angle_gamma                95.0260(10)
_cell_formula_units_Z            4
_cell_length_a                   14.43580(10)
_cell_length_b                   16.47100(10)
_cell_length_c                   17.15210(10)
_cell_measurement_temperature    293(2)
_cell_volume                     3807.94(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23416
_diffrn_reflns_theta_full        67.14
_diffrn_reflns_theta_max         67.14
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_F_000             1400
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0069(5)
_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   0.892
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         12291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.169
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1825P)^2^+0.2589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1948
_refine_ls_wR_factor_ref         0.2078
_reflns_number_gt                9867
_reflns_number_total             12291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0211592B_1.cif
_cod_data_source_block           8c
_cod_original_cell_volume        3807.94(4)
_cod_database_code               4113555