Formation of a Cyclobutylidene Ring: Intramolecular [2 + 2] Cycloaddition of Allyl and Vinylidene CC Bonds under Mild Conditions
Patricia Álvarez; Elena Lastra; José Gimeno; Mauro Bassetti; Larry R. Falvello; Journal of the American Chemical Society 125 (2003) 2386–2387; doi:10.1021/ja027209s

data_4113504
_publ_section_title
;
 Formation of a Cyclobutylidene Ring: Intramolecular [2 + 2] Cycloaddition
 of Allyl and Vinylidene CC Bonds under Mild Conditions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2386
_journal_page_last               2387
_journal_paper_doi               10.1021/ja027209s
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C51 H45 Cl2 F6 P3 Ru'
_chemical_formula_weight         1036.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.21(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.073(3)
_cell_length_b                   25.216(6)
_cell_length_c                   16.324(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      11.0
_cell_volume                     4499(2)
_computing_cell_refinement       'CAD4/PC V2.0 (Nonius, 1996)'
_computing_data_collection       'CAD4/PC V2.0 (Nonius, 1996)'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_molecular_graphics    'SHELXTL Rel. 5.05/V (Siemens, 1996)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
  SIR92 - A program for crystal structure solution. 
  Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. 
  (1993) J. Appl. Cryst. 26, 343-350.
;
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       'omega-theta scan'
_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  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0930
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8326
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.03
_diffrn_standards_interval_time  30
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         7901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+7.1874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1517
_reflns_number_gt                5615
_reflns_number_total             7901
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja027209s-8_s2.cif
_cod_data_source_block           complex3
_cod_database_code               4113504