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_4320263
_publ_section_title
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 Oxonium Ions from Aqua Regia: Isolation by Hydrogen Bonding to Crown
 Ethers
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_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            'C12 H27 Au Cl4 O7'
_chemical_formula_weight         622.10
_chemical_name_common            compound_4_II
_chemical_name_systematic
; 
  ? 
;
_space_group_IT_number           10
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2y'
_symmetry_space_group_name_H-M   'P 1 2/m 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                 100.084(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   13.4509(8)
_cell_length_b                   12.0398(7)
_cell_length_c                   20.2750(11)
_cell_measurement_temperature    123(2)
_cell_volume                     3232.7(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    res2ins
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28128
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.38
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    7.349
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.214
_refine_diff_density_min         -4.830
_refine_diff_density_rms         0.299
_refine_ls_extinction_coef       0.00134(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5925
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.1735
_refine_ls_R_factor_gt           0.0871
_refine_ls_shift/su_max          2.230
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+102.7857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2364
_refine_ls_wR_factor_ref         0.2632
_reflns_number_gt                2088
_reflns_number_total             5925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010468i_5.cif
_cod_data_source_block           au18(formII)
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+102.7857P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+102.7857P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4320263