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_4348545
_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
'C34 H46 Au3 Cl2 N6 O4, Au Cl2, C3 H6 O, 0.5(C4 H10 O)'
_chemical_formula_sum            'C39 H57 Au4 Cl4 N6 O5.5'
_chemical_formula_weight         1627.57
_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                 95.148(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9624(2)
_cell_length_b                   27.3747(6)
_cell_length_c                   18.1167(3)
_cell_measurement_reflns_used    9490
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      71.9352
_cell_measurement_theta_min      2.9308
_cell_volume                     4920.82(17)
_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    SIR-2004
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19105
_diffrn_reflns_point_group_measured_fraction_full 0.756
_diffrn_reflns_point_group_measured_fraction_max 0.724
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         72.077
_diffrn_reflns_theta_min         2.933
_diffrn_source                   'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.290
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60448
_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    2.197
_exptl_crystal_description       prism
_exptl_crystal_F_000             3044
_exptl_crystal_size_max          0.057
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.018
_refine_diff_density_max         2.209
_refine_diff_density_min         -2.142
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.029(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1066
_refine_ls_number_reflns         14038
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+5.9554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.468
_reflns_Friedel_fraction_full    0.509
_reflns_Friedel_fraction_max     0.472
_reflns_number_gt                13290
_reflns_number_total             14038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01323_si_001.cif
_cod_data_source_block           13
_cod_depositor_comments
;

2020-08-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C78 H114 Au8 Cl8 N12 O11'
_cod_original_formula_weight         3255.14
_cod_original_formula_moiety
'C68 H92 Au6 Cl4 N12 O8, 2(Au Cl2), 2(C3 H6 O), C4 H10 O'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        4920.81(17)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4348545
_shelxl_version_number           2014-3
_shelx_res_checksum              19445
_shelx_hkl_checksum              46742