Oxonium Ions from Aqua Regia: Isolation by Hydrogen Bonding to Crown Ethers
Maria Calleja; Karin Johnson; Warwick J. Belcher; Jonathan W. Steed; Inorganic Chemistry 40 (2001) 4978–4985; doi:10.1021/ic010468i

data_4320266
_publ_section_title
;
 Oxonium Ions from Aqua Regia: Isolation by Hydrogen Bonding to Crown
 Ethers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4978
_journal_page_last               4985
_journal_paper_doi               10.1021/ic010468i
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C40 H51 Au Cl12 O17'
_chemical_formula_weight         1426.17
_chemical_name_common            compound_8
_chemical_name_systematic
; 
  ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 91.536(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.490(2)
_cell_length_b                   12.3900(10)
_cell_length_c                   21.171(2)
_cell_measurement_temperature    100(2)
_cell_volume                     5372.8(8)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'XSeed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '2o phi+omega frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1207
_diffrn_reflns_av_sigmaI/netI    0.1537
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14884
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.70
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.401
_exptl_absorpt_correction_T_max  0.4285
_exptl_absorpt_correction_T_min  0.1717
_exptl_absorpt_correction_type   Scalepack
_exptl_absorpt_process_details   'Otwinowski & Minor, 1996'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.824
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.452(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         8864
_refine_ls_number_restraints     344
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.160
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+74.6191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                5333
_reflns_number_total             8864
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010468i_8.cif
_cod_data_source_block           ccdib18
_cod_original_cell_volume        5372.6(9)
_cod_database_code               4320266