#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/02/4320261.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320261
loop_
_publ_author_name
'Maria Calleja'
'Karin Johnson'
'Warwick J. Belcher'
'Jonathan W. Steed'
_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            'C28 H45 Au Cl4 O12'
_chemical_formula_weight         420.75
_chemical_name_common            compound_3
_chemical_name_systematic
; 
  ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.7670(10)
_cell_angle_beta                 88.6270(10)
_cell_angle_gamma                66.9940(10)
_cell_formula_units_Z            1
_cell_length_a                   9.2950(6)
_cell_length_b                   10.2293(11)
_cell_length_c                   11.6412(11)
_cell_measurement_temperature    123(2)
_cell_volume                     907.98(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  KappaCCD
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5637
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.82
_exptl_absorpt_coefficient_mu    4.251
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             422
_refine_diff_density_max         0.928
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+0.6137P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0643
_reflns_number_gt                3273
_reflns_number_total             3321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010468i_3.cif
_cod_data_source_block           aubz15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.6137P] 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^)+(0.0000P)^2^+0.6137P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        907.99(14)
_cod_original_formula_sum        'C28 H45 Au1 Cl4 O12'
_cod_database_code               4320261
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.0000 0.0000 0.0000 0.02348(8) Uani 1 d S . .
Cl1 Cl 0.06007(14) 0.13029(15) 0.09555(12) 0.0464(3) Uani 1 d . . .
Cl2 Cl -0.26121(11) 0.12407(12) 0.00686(9) 0.0341(2) Uani 1 d . . .
O1 O 0.3935(4) 0.5241(4) 0.5607(3) 0.0270(6) Uani 1 d . . .
H13 H 0.327(7) 0.562(6) 0.518(5) 0.033(16) Uiso 1 d . . .
H12 H 0.407(7) 0.432(7) 0.622(6) 0.054(16) Uiso 1 d . . .
H11 H 0.5000 0.5000 0.5000 0.11(4) Uiso 1 d S . .
O1A O 0.2149(3) 0.4676(3) 0.3767(2) 0.0261(6) Uani 1 d . . .
O2A O 0.0853(3) 0.7093(3) 0.4455(3) 0.0283(6) Uani 1 d . . .
O3A O 0.1340(3) 0.5394(3) 0.7166(2) 0.0294(6) Uani 1 d . . .
O4A O 0.4196(3) 0.2684(3) 0.7714(2) 0.0269(6) Uani 1 d . . .
O5A O 0.4181(3) 0.2090(3) 0.5610(2) 0.0245(5) Uani 1 d . . .
C1A C 0.1178(5) 0.6261(4) 0.2810(4) 0.0288(8) Uani 1 d . . .
H1A2 H 0.0628 0.6237 0.2107 0.035 Uiso 1 calc R . .
H1A1 H 0.1831 0.6857 0.2439 0.035 Uiso 1 calc R . .
C2A C -0.0010(5) 0.7034(5) 0.3490(4) 0.0301(9) Uani 1 d . . .
H2A2 H -0.0756 0.8124 0.2867 0.036 Uiso 1 calc R . .
H2A1 H -0.0627 0.6407 0.3893 0.036 Uiso 1 calc R . .
C3A C -0.0151(5) 0.7703(5) 0.5232(4) 0.0314(9) Uani 1 d . . .
H3A2 H -0.1029 0.7364 0.5351 0.038 Uiso 1 calc R . .
H3A1 H -0.0617 0.8882 0.4794 0.038 Uiso 1 calc R . .
C4A C 0.0806(5) 0.7086(5) 0.6521(4) 0.0344(9) Uani 1 d . . .
H4A2 H 0.1725 0.7363 0.6405 0.041 Uiso 1 calc R . .
H4A1 H 0.0145 0.7568 0.7037 0.041 Uiso 1 calc R . .
C5A C 0.2469(5) 0.4636(5) 0.8311(4) 0.0341(9) Uani 1 d . . .
H5A2 H 0.1930 0.4805 0.9013 0.041 Uiso 1 calc R . .
H5A1 H 0.3262 0.5089 0.8159 0.041 Uiso 1 calc R . .
C6A C 0.3270(5) 0.2888(5) 0.8681(4) 0.0312(9) Uani 1 d . . .
H6A2 H 0.3963 0.2303 0.9533 0.037 Uiso 1 calc R . .
H6A1 H 0.2466 0.2462 0.8737 0.037 Uiso 1 calc R . .
C7A C 0.4819(5) 0.1097(4) 0.7851(4) 0.0291(8) Uani 1 d . . .
H7A2 H 0.3968 0.0722 0.7969 0.035 Uiso 1 calc R . .
H7A1 H 0.5663 0.0373 0.8621 0.035 Uiso 1 calc R . .
C8A C 0.5485(5) 0.1074(4) 0.6672(3) 0.0269(8) Uani 1 d . . .
H8A2 H 0.6318 0.1475 0.6533 0.032 Uiso 1 calc R . .
H8A1 H 0.5955 -0.0024 0.6764 0.032 Uiso 1 calc R . .
C9A C 0.4516(4) 0.2364(4) 0.4399(3) 0.0231(8) Uani 1 d . . .
C10A C 0.3386(4) 0.3773(4) 0.3383(3) 0.0242(8) Uani 1 d . . .
C11A C 0.3601(5) 0.4143(5) 0.2116(4) 0.0286(8) Uani 1 d . . .
H11A H 0.2838 0.5078 0.1429 0.034 Uiso 1 calc R . .
C12A C 0.4945(5) 0.3133(5) 0.1853(4) 0.0334(9) Uani 1 d . . .
H12A H 0.5097 0.3396 0.0986 0.040 Uiso 1 calc R . .
C13A C 0.6042(5) 0.1766(5) 0.2840(4) 0.0317(9) Uani 1 d . . .
H13A H 0.6946 0.1085 0.2653 0.038 Uiso 1 calc R . .
C14A C 0.5833(5) 0.1374(4) 0.4121(4) 0.0281(8) Uani 1 d . . .
H14A H 0.6595 0.0429 0.4801 0.034 Uiso 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Au1 Cl2 180.0 2 . ?
Cl2 Au1 Cl1 90.23(4) 2 . ?
Cl2 Au1 Cl1 89.77(4) . . ?
Cl2 Au1 Cl1 89.77(4) 2 2 ?
Cl2 Au1 Cl1 90.23(4) . 2 ?
Cl1 Au1 Cl1 180.0 . 2 ?
C10A O1A C1A 116.6(3) . . ?
C2A O2A C3A 112.7(3) . . ?
C5A O3A C4A 113.3(3) . . ?
C7A O4A C6A 113.4(3) . . ?
C9A O5A C8A 117.5(3) . . ?
O1A C1A C2A 106.2(3) . . ?
O2A C2A C1A 107.7(3) . . ?
O2A C3A C4A 109.5(3) . . ?
O3A C4A C3A 107.9(3) . . ?
O3A C5A C6A 107.9(3) . . ?
O4A C6A C5A 108.2(3) . . ?
O4A C7A C8A 109.4(3) . . ?
O5A C8A C7A 106.5(3) . . ?
O5A C9A C14A 125.1(3) . . ?
O5A C9A C10A 115.1(3) . . ?
C14A C9A C10A 119.7(3) . . ?
O1A C10A C11A 125.5(3) . . ?
O1A C10A C9A 114.9(3) . . ?
C11A C10A C9A 119.7(3) . . ?
C10A C11A C12A 119.9(4) . . ?
C13A C12A C11A 120.4(4) . . ?
C12A C13A C14A 120.2(4) . . ?
C9A C14A C13A 120.1(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 Cl2 2.2760(9) 2 ?
Au1 Cl2 2.2760(9) . ?
Au1 Cl1 2.2805(11) . ?
Au1 Cl1 2.2805(11) 2 ?
O1A C10A 1.369(4) . ?
O1A C1A 1.431(4) . ?
O2A C2A 1.431(5) . ?
O2A C3A 1.437(5) . ?
O3A C5A 1.425(5) . ?
O3A C4A 1.429(5) . ?
O4A C7A 1.430(5) . ?
O4A C6A 1.437(4) . ?
O5A C9A 1.369(4) . ?
O5A C8A 1.438(4) . ?
C1A C2A 1.509(5) . ?
C3A C4A 1.503(6) . ?
C5A C6A 1.502(6) . ?
C7A C8A 1.498(5) . ?
C9A C14A 1.385(5) . ?
C9A C10A 1.415(5) . ?
C10A C11A 1.387(5) . ?
C11A C12A 1.402(6) . ?
C12A C13A 1.374(6) . ?
C13A C14A 1.400(6) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10A O1A C1A C2A -176.1(3) . . . . ?
C3A O2A C2A C1A -175.7(3) . . . . ?
O1A C1A C2A O2A 62.6(4) . . . . ?
C2A O2A C3A C4A 155.1(3) . . . . ?
C5A O3A C4A C3A 170.6(3) . . . . ?
O2A C3A C4A O3A -64.4(4) . . . . ?
C4A O3A C5A C6A -164.1(3) . . . . ?
C7A O4A C6A C5A -170.8(3) . . . . ?
O3A C5A C6A O4A 66.9(4) . . . . ?
C6A O4A C7A C8A 169.0(3) . . . . ?
C9A O5A C8A C7A 175.0(3) . . . . ?
O4A C7A C8A O5A -62.0(4) . . . . ?
C8A O5A C9A C14A 23.5(5) . . . . ?
C8A O5A C9A C10A -157.2(3) . . . . ?
C1A O1A C10A C11A -12.7(5) . . . . ?
C1A O1A C10A C9A 166.7(3) . . . . ?
O5A C9A C10A O1A 1.8(5) . . . . ?
C14A C9A C10A O1A -178.8(3) . . . . ?
O5A C9A C10A C11A -178.8(3) . . . . ?
C14A C9A C10A C11A 0.6(5) . . . . ?
O1A C10A C11A C12A 178.4(4) . . . . ?
C9A C10A C11A C12A -1.0(6) . . . . ?
C10A C11A C12A C13A 0.9(6) . . . . ?
C11A C12A C13A C14A -0.4(6) . . . . ?
O5A C9A C14A C13A 179.2(3) . . . . ?
C10A C9A C14A C13A -0.1(6) . . . . ?
C12A C13A C14A C9A 0.0(6) . . . . ?
