Synthesis of Silver(I) and Gold(I) Complexes Containing Enantiopure Pybox Ligands. First Assays on the Silver(I)-Catalyzed Asymmetric Addition of Alkynes to Imines.
Borrajo-Calleja, Gustavo M; de Julián, Eire; Bayón, Esther; Díez, Josefina; Lastra, Elena; Merino, Isabel; Gamasa, M. Pilar; Inorganic chemistry 55 (2016) 8794–8807; doi:10.1021/acs.inorgchem.6b01323

data_4348542
_publ_section_title
;
 Synthesis of Silver(I) and Gold(I) Complexes Containing Enantiopure Pybox
 Ligands. First Assays on the Silver(I)-Catalyzed Asymmetric Addition of
 Alkynes to Imines.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8794
_journal_page_last               8807
_journal_paper_doi               10.1021/acs.inorgchem.6b01323
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C50 H38 Ag N6 O4, B F4, C H2 Cl2'
_chemical_formula_sum            'C51 H40 Ag B Cl2 F4 N6 O4'
_chemical_formula_weight         1066.47
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 95.998(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   12.818(5)
_cell_length_b                   11.676(5)
_cell_length_c                   14.992(5)
_cell_measurement_reflns_used    9387
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.17
_cell_measurement_theta_min      2.96
_cell_volume                     2231.5(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT  A'
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker CCD Smart 6000'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec Quazar MX multilayer optics'
_diffrn_radiation_source         'Incoatec I\muS microsource'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30650
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         68.302
_diffrn_reflns_theta_min         2.964
_exptl_absorpt_coefficient_mu    5.340
_exptl_absorpt_correction_T_max  0.6063
_exptl_absorpt_correction_T_min  0.4584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       prism
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.151
_refine_diff_density_max         2.067
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 3523 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         7824
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0983P)^2^+2.4337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1414
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.944
_reflns_Friedel_fraction_max     0.927
_reflns_number_gt                7756
_reflns_number_total             7824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01323_si_001.cif
_cod_data_source_block           9
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4348542
_shelxl_version_number           2014-3
_shelx_res_checksum              58519
_shelx_hkl_checksum              93932