Enantioselective Vinylogous Conia-Ene Reaction Catalyzed by a Disilver(I)/Bisdiamine Complex
Zou, Chuncheng; Yang, Lei; Zhang, Lei; Liu, Chengyu; Ma, Yueyue; Song, Gonghua; Liu, Zhen; Cheng, Ruihua; Ye, Jinxing; ACS Catalysis  (2021) 6865–6871; doi:10.1021/acscatal.1c01033

data_4518766
_publ_section_title
;
 Enantioselective Vinylogous Conia-Ene Reaction Catalyzed by a
 Disilver(I)/Bisdiamine Complex
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              6865
_journal_page_last               6871
_journal_paper_doi               10.1021/acscatal.1c01033
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_sum            'C21 H20 O'
_chemical_formula_weight         288.37
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                89.3540(10)
_cell_angle_beta                 84.9290(10)
_cell_angle_gamma                87.9120(10)
_cell_formula_units_Z            2
_cell_length_a                   6.9069(2)
_cell_length_b                   7.5708(2)
_cell_length_c                   15.0339(4)
_cell_measurement_reflns_used    9443
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      139.989
_cell_measurement_theta_min      5.902
_cell_volume                     782.51(4)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25691
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.500
_diffrn_reflns_theta_min         2.951
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.3806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.120
_refine_diff_density_min         -0.108
_refine_diff_density_rms         0.025
_refine_ls_abs_structure_details
; 
 Flack x determined using 2288 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.05(17)
_refine_ls_extinction_coef       0.040(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         5319
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0616P)^2^+0.0465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    0.900
_reflns_Friedel_fraction_max     0.904
_reflns_number_gt                5048
_reflns_number_total             5319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c01033_si_003.cif
_cod_data_source_block           CCDC2027417
_cod_database_code               4518766
_shelx_estimated_absorpt_t_min   0.896
_shelx_estimated_absorpt_t_max   0.930
_shelxl_version_number           2013-4
_shelx_res_checksum              48536
_shelx_hkl_checksum              36573