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_4086796
_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         'C36 H38 Hf N2 O'
_chemical_formula_sum            'C36 H38 Hf N2 O'
_chemical_formula_weight         693.20
_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                91.855(14)
_cell_angle_beta                 100.13(3)
_cell_angle_gamma                100.99(2)
_cell_formula_units_Z            2
_cell_length_a                   9.601(13)
_cell_length_b                   11.974(14)
_cell_length_c                   13.526(16)
_cell_measurement_reflns_used    4345
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.06
_cell_volume                     1499(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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0520
_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       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11712
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.181
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.504
_exptl_absorpt_correction_T_max  0.479
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696.00
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.210
_refine_diff_density_max         3.64
_refine_diff_density_min         -1.36
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0531P)^2^+7.4701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                4764
_reflns_number_total             5183
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om6b00655_si_002.cif
_cod_data_source_block           Hf3b
_cod_database_code               4086796