Scandium-catalyzed C(sp3)‒H alkylation of N,N-dimethyl anilines with alkenes
Gao, Hongjie; Su, Jianhong; Xu, Pengfei; Xu, Xin; Organic Chemistry Frontiers 5 (2018) 59–; doi:10.1039/C7QO00718C

data_1553883
_publ_section_title
;
 Scandium-catalyzed C(sp3)--H alkylation of N,N-dimethyl anilines with
 alkenes
;
_journal_issue                   1
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              59
_journal_paper_doi               10.1039/C7QO00718C
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C43 H60 N2 P Sc Si2'
_chemical_formula_sum            'C43 H60 N2 P Sc Si2'
_chemical_formula_weight         737.04
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-08-11 deposited with the CCDC.
2017-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                75.984(2)
_cell_angle_beta                 74.865(2)
_cell_angle_gamma                66.722(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8597(7)
_cell_length_b                   13.0923(8)
_cell_length_c                   18.0508(12)
_cell_measurement_reflns_used    9677
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.37
_cell_volume                     2247.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19540
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  0.9204
_exptl_absorpt_correction_T_min  0.8607
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear dark colourless'
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         10127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0783P)^2^+0.2938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1448
_reflns_number_gt                6939
_reflns_number_total             10127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7qo00718c2.cif
_cod_data_source_block           t
_cod_original_cell_volume        2247.6(2)
_cod_database_code               1553883