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_4110994
_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                   10.973(2)
_cell_length_b                   10.973(2)
_cell_length_c                   5.2300(19)
_cell_measurement_reflns_used    1468
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.7
_cell_volume                     545.4(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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.12
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            4631
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         3.71
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS v2.05'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_description       needle
_exptl_crystal_F_000             337
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.880
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.56(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1250
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+9.9454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1734
_reflns_number_gt                1202
_reflns_number_total             1250
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja0636439rom20060524_072008.cif
_cod_data_source_block           AgIIS6_150K
_cod_database_code               4110994