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_4110951
_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
'C78 H64 Au2 O2 P4, 4(C H2 Cl2), H4 O2, 2(N O3), 2(H2 O)'
_chemical_formula_sum            'C82 H80 Au2 Cl8 N2 O12 P4'
_chemical_formula_weight         2086.89
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 121.486(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.183(7)
_cell_length_b                   18.296(4)
_cell_length_c                   18.923(4)
_cell_measurement_reflns_used    42549
_cell_measurement_temperature    134(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.12
_cell_volume                     8321(3)
_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      134(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41413
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    3.917
_exptl_absorpt_correction_T_max  0.297
_exptl_absorpt_correction_T_min  0.168
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         7326
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0192P)^2^+61.9684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                6380
_reflns_number_total             7326
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064609xsi20060816_061828.cif
_cod_data_source_block           complex2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4110951