C(sp3)‒H Alkenylation Catalyzed by Cationic Alkylhafnium Complexes: Stereoselective Synthesis of Trisubstituted Alkenes from 2,6-Dimethylpyridines and Internal Alkynes
Lopez, Michael J.; Kondo, Ai; Nagae, Haruki; Yamamoto, Koji; Tsurugi, Hayato; Mashima, Kazushi; Organometallics 35 (2016) 3816–; doi:10.1021/acs.organomet.6b00655

data_4086797
_publ_section_title
;
 C(sp3)--H Alkenylation Catalyzed by Cationic Alkylhafnium Complexes:
 Stereoselective Synthesis of Trisubstituted Alkenes from
 2,6-Dimethylpyridines and Internal Alkynes
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              3816
_journal_paper_doi               10.1021/acs.organomet.6b00655
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C37 H39 Hf N3'
_chemical_formula_sum            'C37 H39 Hf N3'
_chemical_formula_weight         704.23
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.900(14)
_cell_angle_beta                 100.097(9)
_cell_angle_gamma                101.295(16)
_cell_formula_units_Z            2
_cell_length_a                   9.460(10)
_cell_length_b                   12.221(12)
_cell_length_c                   13.656(13)
_cell_measurement_reflns_used    4252
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.03
_cell_volume                     1522(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13253
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.034
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.451
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             708.00
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.78
_refine_diff_density_min         -1.37
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5893
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                5459
_reflns_number_total             5893
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om6b00655_si_002.cif
_cod_data_source_block           Hf3c
_cod_database_code               4086797