Ruthenium-Catalyzed Cycloisomerization of 1,6-Diynes with Styryl Terminals Leading to Indenylidene Cycloalkanes
Yamamoto, Yoshihiko; Nishimura, Kei-ichiro; Shibuya, Masatoshi; ACS Catalysis 7 (2017) 1101–; doi:10.1021/acscatal.6b03322

data_4516726
_publ_section_title
;
 Ruthenium-Catalyzed Cycloisomerization of 1,6-Diynes with Styryl
 Terminals Leading to Indenylidene Cycloalkanes
;
_journal_issue                   2
_journal_name_full               'ACS Catalysis'
_journal_page_first              1101
_journal_paper_doi               10.1021/acscatal.6b03322
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C28 H21 N3 O3'
_chemical_formula_weight         447.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                86.4189(15)
_cell_angle_beta                 81.6947(13)
_cell_angle_gamma                73.8739(14)
_cell_formula_units_Z            4
_cell_length_a                   8.4814(4)
_cell_length_b                   13.8492(7)
_cell_length_c                   19.5575(10)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    93.0(2)
_cell_measurement_theta_max      28.9023
_cell_measurement_theta_min      2.5698
_cell_volume                     2183.10(19)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v3.0.29'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHELL V6.3.1 (Bruke AXS)'
_computing_publication_material  'Generate Report (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      93.0(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.737
_diffrn_measured_fraction_theta_max 0.737
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16542
_diffrn_reflns_theta_full        28.90
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         2.52
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.376
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         8496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          1.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+2.2813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                7554
_reflns_number_total             8496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b03322_si_002.cif
_cod_data_source_block           I
_cod_database_code               4516726
_shelx_res_checksum              74521
_shelx_hkl_checksum              44058