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_4348540
_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         'C43 H42 Ag2 F3 N6 O7 S, C F3 O3 S'
_chemical_formula_sum            'C44 H42 Ag2 F6 N6 O10 S2'
_chemical_formula_weight         1208.69
_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
_cell_angle_beta                 111.442(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8039(3)
_cell_length_b                   12.5654(1)
_cell_length_c                   21.0568(3)
_cell_measurement_reflns_used    17032
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      74.4532
_cell_measurement_theta_min      3.5145
_cell_volume                     4630.92(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Nova (Cu) X-ray Source'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37484
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.626
_diffrn_reflns_theta_min         3.954
_exptl_absorpt_coefficient_mu    8.412
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_description       prism
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.163
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 6290 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.030(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1269
_refine_ls_number_reflns         18384
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0777P)^2^+3.5145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1416
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                15594
_reflns_number_total             18384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01323_si_001.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4348540
_shelxl_version_number           2014-3
_shelx_res_checksum              82785
_shelx_hkl_checksum              8901