Unpredictable cycloisomerization of 1,11-dien-6-ynes by a common cobalt catalyst
Suleymanov, Abdusalom A.; Vasilyev, Dmitry V.; Novikov, Valentin V.; Nelyubina, Yulia V.; Perekalin, Dmitry S.; Beilstein Journal of Organic Chemistry 13 (2017) 639–; doi:10.3762/bjoc.13.62

data_4032426
_publ_section_title
;
 Unpredictable cycloisomerization of 1,11-dien-6-ynes by a common cobalt
 catalyst
;
_journal_name_full               'Beilstein Journal of Organic Chemistry'
_journal_page_first              639
_journal_paper_doi               10.3762/bjoc.13.62
_journal_volume                  13
_journal_year                    2017
_chemical_formula_moiety         'C24 H28 N2 O4 S2'
_chemical_formula_sum            'C24 H28 N2 O4 S2'
_chemical_formula_weight         472.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                65.335(4)
_cell_angle_beta                 79.309(4)
_cell_angle_gamma                86.703(4)
_cell_formula_units_Z            2
_cell_length_a                   7.5018(12)
_cell_length_b                   12.743(2)
_cell_length_c                   13.473(2)
_cell_measurement_reflns_used    2004
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1149.8(3)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1036
_diffrn_reflns_av_unetI/netI     0.1083
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18071
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         1.759
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       prism
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1401
_refine_ls_R_factor_gt           0.0822
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1841
_refine_ls_wR_factor_ref         0.2060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2614
_reflns_number_total             4520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2b.cif
_cod_data_source_block           2b
_cod_original_cell_volume        1149.9(3)
_cod_database_code               4032426
_shelx_estimated_absorpt_t_min   0.925
_shelx_estimated_absorpt_t_max   0.961
_shelxl_version_number           2014/6
_shelx_res_checksum              76658
_shelx_hkl_checksum              13250