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_4114227
_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            'C28 H29 Cl O Ru'
_chemical_formula_weight         518.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.559(2)
_cell_length_b                   7.3310(9)
_cell_length_c                   38.161(5)
_cell_measurement_temperature    173(2)
_cell_volume                     4632.5(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0855
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            33668
_diffrn_reflns_theta_full        29.12
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.462469
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    0.743
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.6
_refine_diff_density_max         1.173
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         6194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+5.2344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                5805
_reflns_number_total             6194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0358697si20030501_064533_2.cif
_cod_data_source_block           complex(28)
_cod_original_cell_volume        4632.6(10)
_cod_database_code               4114227