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_4113556
_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            'C42 H56 O5 Si2'
_chemical_formula_weight         697.05
_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                 111.94
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.89360(10)
_cell_length_b                   19.11160(10)
_cell_length_c                   16.22800(10)
_cell_measurement_temperature    293(2)
_cell_volume                     4284.61(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 0.957
_diffrn_measured_fraction_theta_max 0.957
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22538
_diffrn_reflns_theta_full        25.15
_diffrn_reflns_theta_max         25.15
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_F_000             1504
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.087(3)
_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   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         7343
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.366
_refine_ls_shift/su_mean         0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1170P)^2^+0.9789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.1911
_reflns_number_gt                6848
_reflns_number_total             7343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0211592B_2.cif
_cod_data_source_block           9c
_cod_original_cell_volume        4284.67(5)
_cod_database_code               4113556