Ruthenium(II)-Catalyzed Selective Intramolecular [2 + 2 + 2] Alkyne Cyclotrimerizations
Yoshihiko Yamamoto; Takayasu Arakawa; Ryuji Ogawa; Kenji Itoh; Journal of the American Chemical Society 125 (2003) 12143–12160; doi:10.1021/ja0358697

data_4114226
_publ_section_title
;
 Ruthenium(II)-Catalyzed Selective Intramolecular [2 + 2 + 2] Alkyne
 Cyclotrimerizations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12143
_journal_page_last               12160
_journal_paper_doi               10.1021/ja0358697
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C20 H27 Cl O3 Ru'
_chemical_formula_weight         451.94
_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                 98.0280(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3721(6)
_cell_length_b                   16.7911(10)
_cell_length_c                   11.9364(7)
_cell_measurement_temperature    173(2)
_cell_volume                     1860.0(2)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14172
_diffrn_reflns_theta_full        29.16
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.791321
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.631
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0506P)^2^+1.0314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                4567
_reflns_number_total             4955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0358697si20030501_064533_1.cif
_cod_data_source_block           Complex(27)
_cod_database_code               4114226