Stereodefined Synthesis of a New Type of 1,3-Dienes by Ligand-Controlled Carbon−Carbon and Carbon−Heteroatom Bond Formation in Nickel-Catalyzed Reaction of Diaryldichalcogenides with Alkynes
Ananikov, Valentine P.; Orlov, Nikolay V.; Kabeshov, Mikhail A.; Beletskaya, Irina P.; Starikova, Zoya A.; Organometallics 27 (2008) 4056–; doi:10.1021/om800282h

data_4071634
_publ_section_title
;
 Stereodefined Synthesis of a New Type of 1,3-Dienes by Ligand-Controlled
 Carbon&#x2212;Carbon and Carbon&#x2212;Heteroatom Bond Formation in
 Nickel-Catalyzed Reaction of Diaryldichalcogenides with Alkynes
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4056
_journal_paper_doi               10.1021/om800282h
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C20 H22 O2 S2'
_chemical_formula_weight         358.50
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   24.993(4)
_cell_length_b                   24.993(4)
_cell_length_c                   7.3862(18)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.89
_cell_measurement_theta_min      3.72
_cell_volume                     3995.7(13)
_computing_cell_refinement       'SAINTPlus (Bruker, 1998a)'
_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10992
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1710
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+3.5270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                1864
_reflns_number_total             2327
_reflns_threshold_expression     I>2u(I)
_cod_data_source_file            om800282h-file002.cif
_cod_data_source_block           bel
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3995.7(14)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4071634