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_4348538
_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         'C35 H46 Ag2 F3 N6 O7 S, C F3 O3 S'
_chemical_formula_sum            'C36 H46 Ag2 F6 N6 O10 S2'
_chemical_formula_weight         1116.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.5986(1)
_cell_length_b                   21.2402(2)
_cell_length_c                   31.0125(3)
_cell_measurement_reflns_used    19753
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.9592
_cell_measurement_theta_min      2.8474
_cell_volume                     8957.56(14)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'DIRDIF-2008( Beurskens, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            28254
_diffrn_reflns_point_group_measured_fraction_full 0.877
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         74.126
_diffrn_reflns_theta_min         2.850
_diffrn_source                   'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39472
_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    1.656
_exptl_crystal_description       prism
_exptl_crystal_F_000             4512
_exptl_crystal_size_max          0.2547
_exptl_crystal_size_mid          0.1200
_exptl_crystal_size_min          0.0724
_refine_diff_density_max         1.239
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 4870 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1121
_refine_ls_number_reflns         14770
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+6.9205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1218
_reflns_Friedel_coverage         0.575
_reflns_Friedel_fraction_full    0.734
_reflns_Friedel_fraction_max     0.650
_reflns_number_gt                13874
_reflns_number_total             14770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01323_si_001.cif
_cod_data_source_block           1
_cod_database_code               4348538
_shelxl_version_number           2014-3
_shelx_res_checksum              17395
_shelx_hkl_checksum              30689