Iron-Catalyzed Directed C(sp(2))-H and C(sp(3))-H Functionalization with Trimethylaluminum.
Shang, Rui; Ilies, Laurean; Nakamura, Eiichi; Journal of the American Chemical Society 137 (2015) 7660–7663; doi:10.1021/jacs.5b04818

data_4123928
_publ_section_title
;
 Iron-Catalyzed Directed C(sp(2))-H and C(sp(3))-H Functionalization with
 Trimethylaluminum.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7660
_journal_page_last               7663
_journal_paper_doi               10.1021/jacs.5b04818
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C16 H13 N3 O'
_chemical_formula_weight         263.29
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 97.865(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.7323(3)
_cell_length_b                   26.7612(7)
_cell_length_c                   10.8183(3)
_cell_measurement_reflns_used    4557
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      68.13
_cell_measurement_theta_min      3.30
_cell_volume                     2504.31(13)
_computing_cell_refinement       'Rapid Auto (Rigaku)'
_computing_data_collection       'Rapid Auto (Rigaku)'
_computing_data_reduction        'Rapid Auto (Rigaku)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       IP
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1155
_diffrn_reflns_av_sigmaI/netI    0.1478
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25247
_diffrn_reflns_theta_full        68.13
_diffrn_reflns_theta_max         68.13
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  0.9716
_exptl_absorpt_correction_T_min  0.8990
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'Empirical Absorption Correction March 2001 T Higashi'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.00015(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.759
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         4557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.759
_refine_ls_R_factor_all          0.1730
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1955
_reflns_number_gt                1360
_reflns_number_total             4557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b04818_si_002.cif
_cod_data_source_block           MeQNHPA
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4123928