Solvent-Assisted Spontaneous Resolution of a 16-Membered Ring Containing Gold(I) Showing Short Au...Au Aurophilic Interaction and a Figure-Eight Conformation
Tünde Tunyogi; Andrea Deák; Gábor Tárkányi; Péter Király; Gábor Pálinkás; Inorganic Chemistry 47 (2008) 2049–2055; doi:10.1021/ic702059v

data_4304545
_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         00-36-1-438-1143
_publ_contact_author_name        'Andrea De\'ak'
_publ_contact_author_phone       00-36-1-438-1161/327
_publ_section_title
;
Solvent-Assisted Spontaneous Resolution of a 16-Membered Ring Containing
Gold(I) Showing Short Au...Au Aurophilic Interaction and a Figure-Eight
Conformation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2049
_journal_page_last               2055
_journal_paper_doi               10.1021/ic702059v
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety
'C72 H54 Au2 N2 O2 P4, 3(C H4 O), 2(N O3), H2 O'
_chemical_formula_sum            'C75 H68 Au2 N4 O12 P4'
_chemical_formula_weight         1735.15
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7471(17)
_cell_length_b                   18.000(2)
_cell_length_c                   25.977(3)
_cell_measurement_reflns_used    88536
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.08
_cell_volume                     6895.5(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      103(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            83193
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    4.409
_exptl_absorpt_correction_T_max  0.5186
_exptl_absorpt_correction_T_min  0.3267
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trapezoidal
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.714
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         12066
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+31.0827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                11143
_reflns_number_total             12066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702059v-file003_1.cif
_cod_data_source_block           complex1
_cod_database_code               4304545