Ring-Closing Metathesis of Co2(CO)6-Alkyne Complexes for the Synthesis of 11-Membered Dienediynes: Overcoming Thermodynamic Barriers.
Danilkina, Natalia A.; Lyapunova, Anna G.; Khlebnikov, Alexander F.; Starova, Galina L.; Bräse, Stefan; Balova, Irina A.; The Journal of organic chemistry 80 (2015) 5546–5555; doi:10.1021/acs.joc.5b00409

data_4031007
_publ_section_title
;
 Ring-Closing Metathesis of Co2(CO)6-Alkyne Complexes for the Synthesis of
 11-Membered Dienediynes: Overcoming Thermodynamic Barriers.
;
_journal_issue                   11
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5546
_journal_page_last               5555
_journal_paper_doi               10.1021/acs.joc.5b00409
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C23 H12 Co2 O6 S'
_chemical_formula_sum            'C23 H12 Co2 O6 S'
_chemical_formula_weight         534.25
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-30
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  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.4350(5)
_cell_length_b                   13.7734(4)
_cell_length_c                   27.2118(17)
_cell_measurement_reflns_used    2053
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5914
_cell_measurement_theta_min      2.7514
_cell_volume                     4285.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.9805
_diffrn_measured_fraction_theta_max 0.9805
_diffrn_measurement_details
;
  1 omega  -38.00   87.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       25.3598    0.0000   30.0000 125
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0068232000
_diffrn_orient_matrix_UB_12      -0.0511479000
_diffrn_orient_matrix_UB_13      -0.0009530000
_diffrn_orient_matrix_UB_21      0.0179873000
_diffrn_orient_matrix_UB_22      0.0001520000
_diffrn_orient_matrix_UB_23      -0.0249538000
_diffrn_orient_matrix_UB_31      0.0589464000
_diffrn_orient_matrix_UB_32      -0.0059531000
_diffrn_orient_matrix_UB_33      0.0075126000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            9924
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.30
_diffrn_reflns_theta_min         2.76
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.683
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            dark-bordo
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizms
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                3258
_reflns_number_total             4401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo5b00409_si_003.cif
_cod_data_source_block           ndco
_cod_depositor_comments          'Adding full bibliography for 4031007.cif.'
_cod_database_code               4031007
_chemical_oxdiff_formula         'co1 Cl4 H12 O20'
_reflns_odcompleteness_completeness 88.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.51