Nickel-Catalyzed {[}4+2] Cycloaddition of Enones with Alkynes
Koyama, Ichiro; Kurahashi, Takuya; Matsubara, Seijiro; JOURNAL OF THE AMERICAN CHEMICAL SOCIETY 131 (2009) 1350–; doi:10.1021/ja807952r

data_4101596
_publ_section_title
;
 Nickel-Catalyzed {[}4+2] Cycloaddition of Enones with Alkynes
;
_journal_issue                   4
_journal_name_full               'JOURNAL OF THE AMERICAN CHEMICAL SOCIETY'
_journal_page_first              1350
_journal_paper_doi               10.1021/ja807952r
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C22.50 H30 N2 Ni O3 '
_chemical_formula_sum            'C22.5 H30 N2 Ni O3'
_chemical_formula_weight         435.20
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                66.224(8)
_cell_angle_beta                 67.551(8)
_cell_angle_gamma                76.882(9)
_cell_formula_units_Z            2
_cell_length_a                   10.5195(18)
_cell_length_b                   10.9929(17)
_cell_length_c                   11.5575(15)
_cell_measurement_reflns_used    2923
_cell_measurement_temperature    153.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     1126.2(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SAPI91
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8219
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             462.00
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.04
_refine_diff_density_min         -0.91
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4785
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0020Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                3512
_reflns_number_total             4785
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            reformated.cif
_cod_data_source_block           '__koyama02'
_cod_original_formula_sum        'C22.50 H30 N2 Ni O3 '
_cod_database_code               4101596