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_4032427
_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         'C28 H36 N2 O4 S2'
_chemical_formula_sum            'C28 H36 N2 O4 S2'
_chemical_formula_weight         528.71
_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                61.5480(10)
_cell_angle_beta                 71.9710(10)
_cell_angle_gamma                72.6980(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1158(6)
_cell_length_b                   9.4944(7)
_cell_length_c                   9.9154(7)
_cell_measurement_reflns_used    2442
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     705.83(9)
_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 0.999
_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  0.0244
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8566
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.996
_diffrn_reflns_theta_min         2.384
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       prism
_exptl_crystal_F_000             282
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.4736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                3283
_reflns_number_total             3755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1h.cif
_cod_data_source_block           1d
_cod_database_code               4032427
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.967
_shelxl_version_number           2014/6
_shelx_res_checksum              74700
_shelx_hkl_checksum              56265