Synthesis of Allylanilines via Scandium-Catalysed Benzylic C(sp3)−H Alkenylation with Alkynes
Zhou, Wei; Cong, Xuefeng; Nishiura, Masayoshi; Hou, Zhaomin; Chemical Communications  (2022) –; doi:10.1039/D2CC02489F

data_7130163
_publ_section_title
;
 Synthesis of Allylanilines via Scandium-Catalysed Benzylic
 C(sp3)&#x2212;H Alkenylation with Alkynes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02489F
_journal_year                    2022
_chemical_formula_sum            'C40 H40 N2'
_chemical_formula_weight         548.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2022-04-27 deposited with the CCDC.	2022-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                70.0360(10)
_cell_angle_beta                 85.2930(10)
_cell_angle_gamma                71.4060(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4940(3)
_cell_length_b                   11.0423(3)
_cell_length_c                   15.0933(5)
_cell_measurement_reflns_used    256
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.47
_cell_volume                     1557.37(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26909
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.057
_diffrn_reflns_theta_max         25.057
_diffrn_reflns_theta_min         1.436
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.500
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.6288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                4944
_reflns_number_total             5512
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           shelx
_cod_database_code               7130163
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              52992