Aminomethylation Reaction of ortho-Pyridyl C-H Bonds Catalyzed by Group 3 Metal Triamido Complexes.
Nagae, Haruki; Shibata, Yu; Tsurugi, Hayato; Mashima, Kazushi; Journal of the American Chemical Society 137 (2015) 640–643; doi:10.1021/ja511964k

data_4123226
_publ_section_title
;
 Aminomethylation Reaction of ortho-Pyridyl C-H Bonds Catalyzed by Group 3
 Metal Triamido Complexes.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              640
_journal_page_last               643
_journal_paper_doi               10.1021/ja511964k
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C36 H58 N5 Si4 Y'
_chemical_formula_sum            'C36 H58 N5 Si4 Y'
_chemical_formula_weight         762.14
_chemical_melting_point          128
_chemical_name_common            6
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.749(13)
_cell_length_b                   12.001(6)
_cell_length_c                   27.085(14)
_cell_measurement_reflns_used    17529
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.01
_cell_volume                     8370(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'Direct Methods (SIR2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1029
_diffrn_reflns_av_unetI/netI     0.1097
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            79513
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.522
_diffrn_reflns_theta_min         3.013
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 5662 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         19125
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.952
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                15109
_reflns_number_total             19125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja511964k_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4123224--4123226.cif.'
_cod_original_cell_volume        8369(7)
_cod_database_code               4123226
_shelx_estimated_absorpt_t_min   0.682
_shelx_estimated_absorpt_t_max   0.900
_shelxl_version_number           2014-3
_shelx_res_checksum              49713
_shelx_hkl_checksum              90940