Dirhodium(ii)-catalyzed ortho C-H amination of sterically congested N,N-dialkylanilines.
Ito, Motoki; Nakagawa, Tomoya; Higuchi, Kazuhiro; Sugiyama, Shigeo; Organic & biomolecular chemistry 16 (2018) 6876–6881; doi:10.1039/c8ob01974f

data_7156421
_publ_section_title
;
 Dirhodium(ii)-catalyzed ortho C-H amination of sterically congested
 N,N-dialkylanilines.
;
_journal_issue                   38
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6876
_journal_page_last               6881
_journal_paper_doi               10.1039/c8ob01974f
_journal_volume                  16
_journal_year                    2018
_chemical_formula_moiety         'C40 H56 N4 O6 S2'
_chemical_formula_sum            'C40 H56 N4 O6 S2'
_chemical_formula_weight         753.03
_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
_audit_update_record
;
2018-03-07 deposited with the CCDC.
2018-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                80.876(6)
_cell_angle_beta                 87.787(6)
_cell_angle_gamma                86.969(6)
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_cell_length_b                   12.3118(3)
_cell_length_c                   19.8734(5)
_cell_measurement_reflns_used    16072
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.16
_cell_measurement_theta_min      3.64
_cell_volume                     1986.55(9)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.000
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_diffrn_reflns_limit_k_min       -14
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_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23052
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_diffrn_reflns_theta_max         68.160
_diffrn_reflns_theta_min         3.640
_diffrn_standards_number         0
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_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            colorless
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_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
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_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0516P)^2^+0.9794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                6591
_reflns_number_total             7080
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c8ob01974f3.cif
_cod_data_source_block           Ito001
_cod_depositor_comments          'Adding full bibliography for 7156421.cif.'
_cod_original_cell_volume        1986.54(9)
_cod_database_code               7156421