Nonmetathetic Activity of Ruthenium Alkylidene Complexes: 1,4-Hydrovinylative Cyclization of Multiynes with Ethylene
Sang Young Yun; Kung-Pern Wang; Mansuk Kim; Daesung Lee; Journal of the American Chemical Society 134 (2012) 10783–10786; doi:10.1021/ja304255h

data_4118192
_publ_section_title
;
 Nonmetathetic Activity of Ruthenium Alkylidene Complexes:
 1,4-Hydrovinylative Cyclization of Multiynes with Ethylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10783
_journal_page_last               10786
_journal_paper_doi               10.1021/ja304255h
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C35 H56 O4 Si2'
_chemical_formula_weight         596.98
_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                108.260(2)
_cell_angle_beta                 92.017(2)
_cell_angle_gamma                93.497(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1624(13)
_cell_length_b                   13.199(2)
_cell_length_c                   17.708(3)
_cell_measurement_reflns_used    8876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.521
_cell_measurement_theta_min      2.319
_cell_volume                     1805.4(5)
_computing_cell_refinement       'Apex2 v2.1-4 (Bruker, 2007)'
_computing_data_collection       'Apex2 v2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Apex2 v2.1-4 (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows v2.01'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega 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  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20866
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.9742
_exptl_absorpt_correction_T_min  0.9493
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_meas      ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.781
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         8169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.781
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.6665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                6272
_reflns_number_total             8169
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja304255h_si_001.cif
_cod_data_source_block           xray3646_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4118192