Synthesis and Solution- and Solid-State Characterization of Gold(I) Rings with Short Au...Au Interactions. Spontaneous Resolution of a Gold(I) Complex
Andrea Deák; Tünde Megyes; Gábor Tárkányi; Péter Király; László Biczók; Gábor Pálinkás; Peter J. Stang; Journal of the American Chemical Society 128 (2006) 12668–12670; doi:10.1021/ja064609x

data_4110950
_publ_contact_author_address
; Institute of Structural Chemistry,
  Chemical Research Center of the Hungarian Academy of Sciences,
  H-1525 Budapest,
  P.O.Box 17,
  Hungary
;
_publ_contact_author_email       deak@chemres.hu
_publ_contact_author_fax         00-36-1-438-4141/201
_publ_contact_author_name        'Andrea De\'ak'
_publ_contact_author_phone       00-36-1-438-1161/327
_publ_section_title
;
 Synthesis and Solution- and Solid-State Characterization of Gold(I) Rings
 with Short Au...Au Interactions. Spontaneous Resolution of a Gold(I)
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12668
_journal_page_last               12670
_journal_paper_doi               10.1021/ja064609x
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C39 H32 Au2 N2 O7 P2, 2(C4 H10 O)'
_chemical_formula_sum            'C47 H52 Au2 N2 O9 P2'
_chemical_formula_weight         1244.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 107.416(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.553(5)
_cell_length_b                   16.745(6)
_cell_length_c                   12.475(4)
_cell_measurement_reflns_used    19070
_cell_measurement_temperature    136(2)
_cell_measurement_theta_max      27.66
_cell_measurement_theta_min      3.015
_cell_volume                     2103.4(14)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'WinGX (Farrugia, 1999), PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      136(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'R Axis Rapid'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16583
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    7.105
_exptl_absorpt_correction_T_max  0.1026
_exptl_absorpt_correction_T_min  0.0392
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.534
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.018(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         7133
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+23.6489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                6684
_reflns_number_total             7133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064609xsi20060816_061809.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        2103.4(15)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4110950