Redox Non-innocence of Thioether Macrocycles: Elucidation of the Electronic Structures of Mononuclear Complexes of Gold(II) and Silver(II)
Jennifer L. Shaw; Joanna Wolowska; David Collison; Judith A. K. Howard; Eric J. L. McInnes; Jonathan McMaster; Alexander J. Blake; Claire Wilson; Martin Schröder; Journal of the American Chemical Society 128 (2006) 13827–13839; doi:10.1021/ja0636439

data_4110995
_publ_section_title
;
 Redox Non-innocence of Thioether Macrocycles: Elucidation of the
 Electronic Structures of Mononuclear Complexes of Gold(II) and Silver(II)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13827
_journal_page_last               13839
_journal_paper_doi               10.1021/ja0636439
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C12 H24 Ag S6 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C12 H24 Ag Cl2 O8 S6'
_chemical_formula_weight         667.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           143
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3'
_symmetry_space_group_name_H-M   'P 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   10.851(2)
_cell_length_b                   10.851(2)
_cell_length_c                   5.186(2)
_cell_measurement_reflns_used    673
_cell_measurement_temperature    30(2)
_cell_measurement_theta_max      26.65
_cell_measurement_theta_min      3.75
_cell_volume                     528.8(2)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_publication_material  'enCIFer (CCDC, 2003); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      30(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker APEX with Bede Microsource'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         Microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            1895
_diffrn_reflns_theta_full        24.93
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         3.76
_exptl_absorpt_coefficient_mu    1.838
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SHELXTL v6.12'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.096
_exptl_crystal_description       needle
_exptl_crystal_F_000             337
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.174
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1113
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                876
_reflns_number_total             1113
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja0636439rom20060524_072020.cif
_cod_data_source_block           AgIIS6_30K
_cod_database_code               4110995