Visible-Light-Activated Rhodium Complex in Enantioselective Conjugate Addition of α-Amino Radicals with Michael Acceptors
Lin, Shao-Xia; Sun, Gui-Jun; Kang, Qiang; Chem. Commun.  (2017) –; doi:10.1039/C7CC03650G

data_7120286
_publ_section_title
;
 Visible-Light-Activated Rhodium Complex in Enantioselective Conjugate
 Addition of \a-Amino Radicals with Michael Acceptors
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03650G
_journal_year                    2017
_chemical_formula_sum            'C31 H33 N3 O'
_chemical_formula_weight         463.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-06 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.906(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5308(3)
_cell_length_b                   7.8842(2)
_cell_length_c                   12.7592(3)
_cell_measurement_reflns_used    2998
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      73.2520
_cell_measurement_theta_min      4.5870
_cell_volume                     1245.35(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector_area_resol_mean 10.5594
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4859
_diffrn_reflns_point_group_measured_fraction_full 0.697
_diffrn_reflns_point_group_measured_fraction_max 0.667
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.359
_diffrn_reflns_theta_min         3.506
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       prism
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.146
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         3345
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0479P)^2^+0.1026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.281
_reflns_Friedel_fraction_full    0.345
_reflns_Friedel_fraction_max     0.316
_reflns_number_gt                3173
_reflns_number_total             3345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc03650g2.cif
_cod_data_source_block           Compound-1
_cod_database_code               7120286
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.944
_shelx_res_checksum              54431
_shelx_hkl_checksum              51979