Oxidant-Free Direct Coupling of Internal Alkynes and 2-Alkylpyridine via Double C-H Activations by Alkylhafnium Complexes
Hayato Tsurugi; Koji Yamamoto; Kazushi Mashima; Journal of the American Chemical Society 133 (2011) 732–735; doi:10.1021/ja1100118

data_4105546
_publ_contact_author_address
;
                   Department of Chemistry
                   Graduate School of Engineering Science
                   Osaka University
                   Machikaneyama, 1-3
                   Toyonaka
                   Osaka, 560-8531
                   Japan
;
_publ_contact_author_email       mashima@chem.es.osaka-u.ac.jp
_publ_contact_author_fax         ' +81 6 6850 6245'
_publ_contact_author_name        'Kazushi Mashima'
_publ_contact_author_phone       ' +81 6 6850 6245'
_publ_section_title
;
 Oxidant-Free Direct Coupling of Internal Alkynes and 2-Alkylpyridine via
 Double C-H Activations by Alkylhafnium Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              732
_journal_page_last               735
_journal_paper_doi               10.1021/ja1100118
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C52 H53 Hf N3, C6 H14'
_chemical_formula_sum            'C58 H67 Hf N3'
_chemical_formula_weight         984.64
_chemical_melting_point          402(2)
_chemical_name_common            5
_chemical_name_systematic
; 
 ? 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.96(2)
_cell_angle_beta                 88.40(3)
_cell_angle_gamma                69.84(2)
_cell_formula_units_Z            2
_cell_length_a                   11.146(7)
_cell_length_b                   13.285(6)
_cell_length_c                   19.220(11)
_cell_measurement_reflns_used    6780
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      3.1
_cell_volume                     2497(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23323
_diffrn_reflns_theta_full        27.32
_diffrn_reflns_theta_max         27.32
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    2.128
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.209
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         10902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0691P)^2^+4.5490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                9790
_reflns_number_total             10902
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1100118_si_002_3.cif
_cod_data_source_block           complex5
_cod_database_code               4105546