#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/24/7052475.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_7052475
loop_
_publ_author_name
'Calleja, Maria'
'Mason, Sax A.'
'Paul D. Prince'
'Steed, Jonathan W.'
'Wilkinson, Clive'
_publ_section_title
;
 Single crystal neutron and X-ray diffraction studies of
 (H7O3)[AuCl4]·15-crown-5
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1475
_journal_page_last               1478
_journal_paper_doi               10.1039/B108935H
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C10 H27 Au Cl4 O8'
_chemical_formula_weight         614.10
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.485(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9346(4)
_cell_length_b                   18.6728(9)
_cell_length_c                   13.9672(7)
_cell_measurement_temperature    80(2)
_cell_volume                     2003.62(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.602
_diffrn_measured_fraction_theta_max 0.602
_diffrn_measurement_device_type  'ILL D19'
_diffrn_radiation_monochromator  Ge113
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ILL reactor'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.23160
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8681
_diffrn_reflns_theta_full        66.55
_diffrn_reflns_theta_max         66.55
_diffrn_reflns_theta_min         3.22
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.048
_exptl_absorpt_correction_type   'Face index'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             231
_exptl_crystal_size_max          6.0
_exptl_crystal_size_mid          2.4
_exptl_crystal_size_min          2.0
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    'full anisotropic refinement'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         4176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0287P)²+7.7589P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                3572
_reflns_number_total             4176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108935h.txt
_cod_data_source_block           h7o3(neutron)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7052475
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
H1 H 0.7772(3) 0.25534(13) 0.73544(19) 0.0278(5) Uani 1 1 d . . .
H2 H 0.9217(3) 0.26169(14) 0.65804(19) 0.0273(5) Uani 1 1 d . . .
H3 H 0.9396(3) 0.19259(13) 0.72999(19) 0.0268(5) Uani 1 1 d . . .
H4 H 0.5647(3) 0.26917(14) 0.7859(2) 0.0279(5) Uani 1 1 d . . .
H5 H 0.6804(4) 0.33767(15) 0.7847(3) 0.0417(7) Uani 1 1 d . . .
H6 H 0.3071(4) 0.21796(16) 0.7253(2) 0.0326(6) Uani 1 1 d . . .
H7 H 0.2975(3) 0.24909(16) 0.8256(2) 0.0315(5) Uani 1 1 d . . .
Au1 Au 0.75038(13) 0.50574(5) 0.75035(7) 0.01224(17) Uani 1 1 d . . .
Cl1 Cl 0.81785(12) 0.56212(4) 0.61999(7) 0.02018(17) Uani 1 1 d . . .
O1 O 1.15484(17) 0.17770(7) 0.62273(9) 0.0136(2) Uani 1 1 d . . .
C1 C 1.10964(16) 0.20802(6) 0.52651(8) 0.0153(2) Uani 1 1 d . . .
H1A H 0.9735(4) 0.19452(15) 0.4901(2) 0.0324(6) Uani 1 1 d . . .
H1B H 1.1938(4) 0.18693(15) 0.4813(2) 0.0355(6) Uani 1 1 d . . .
Cl2 Cl 0.55343(11) 0.43510(4) 0.64336(6) 0.01837(16) Uani 1 1 d . . .
O2 O 0.99773(17) 0.31420(7) 0.58193(10) 0.0148(2) Uani 1 1 d . . .
C2 C 1.12892(16) 0.28814(6) 0.53666(9) 0.0159(2) Uani 1 1 d . . .
H2A H 1.2596(3) 0.30210(15) 0.5821(2) 0.0324(6) Uani 1 1 d . . .
H2B H 1.1115(4) 0.31264(15) 0.4634(2) 0.0348(6) Uani 1 1 d . . .
Cl3 Cl 0.68124(12) 0.44983(5) 0.88126(6) 0.02030(17) Uani 1 1 d . . .
O3 O 1.03801(17) 0.37136(7) 0.77545(10) 0.0150(2) Uani 1 1 d . . .
C3 C 1.00819(15) 0.38923(6) 0.60391(8) 0.0156(2) Uani 1 1 d . . .
H3A H 0.8741(3) 0.40729(15) 0.5970(2) 0.0301(5) Uani 1 1 d . . .
H3B H 1.0613(4) 0.41837(14) 0.5488(2) 0.0337(6) Uani 1 1 d . . .
Cl4 Cl 0.94678(11) 0.57527(5) 0.85695(7) 0.02241(18) Uani 1 1 d . . .
O4 O 1.14325(17) 0.25305(7) 0.90139(9) 0.0148(2) Uani 1 1 d . . .
C4 C 1.11795(15) 0.40467(6) 0.70694(9) 0.0150(2) Uani 1 1 d . . .
H4A H 1.2518(3) 0.38455(16) 0.7170(2) 0.0326(6) Uani 1 1 d . . .
H4B H 1.1239(4) 0.46308(13) 0.7177(2) 0.0325(5) Uani 1 1 d . . .
O5 O 1.06555(17) 0.12720(7) 0.78939(10) 0.0142(2) Uani 1 1 d . . .
C5 C 1.13672(15) 0.37891(6) 0.87545(9) 0.0159(2) Uani 1 1 d . . .
H5A H 1.1092(4) 0.43065(14) 0.9059(2) 0.0332(6) Uani 1 1 d . . .
H5B H 1.2769(3) 0.37706(16) 0.8777(2) 0.0315(5) Uani 1 1 d . . .
O8 O 0.37415(18) 0.24306(8) 0.78274(11) 0.0212(3) Uani 1 1 d . . .
C6 C 1.08921(15) 0.31902(6) 0.93603(8) 0.0154(2) Uani 1 1 d . . .
H6A H 1.1540(4) 0.32677(15) 1.01442(19) 0.0332(6) Uani 1 1 d . . .
H6B H 0.9475(3) 0.31829(15) 0.9277(2) 0.0302(5) Uani 1 1 d . . .
O6 O 0.85599(17) 0.22772(7) 0.69017(10) 0.0144(2) Uani 1 1 d . . .
C7 C 1.07670(15) 0.19116(6) 0.93913(8) 0.0153(2) Uani 1 1 d . . .
H7A H 0.9330(3) 0.19305(15) 0.9202(2) 0.0310(5) Uani 1 1 d . . .
H7B H 1.1245(4) 0.18849(15) 1.02015(19) 0.0326(6) Uani 1 1 d . . .
O7 O 0.68521(18) 0.28641(7) 0.79030(11) 0.0172(3) Uani 1 1 d . . .
C8 C 1.13853(15) 0.12581(6) 0.89427(8) 0.0153(2) Uani 1 1 d . . .
H8A H 1.2812(3) 0.12642(15) 0.9089(2) 0.0299(5) Uani 1 1 d . . .
H8B H 1.0976(4) 0.07705(14) 0.9263(2) 0.0330(6) Uani 1 1 d . . .
C9 C 1.15673(15) 0.08304(6) 0.73509(8) 0.0140(2) Uani 1 1 d . . .
H9A H 1.1250(4) 0.02656(13) 0.7429(2) 0.0300(5) Uani 1 1 d . . .
H9B H 1.2979(3) 0.09073(15) 0.7642(2) 0.0281(5) Uani 1 1 d . . .
C10 C 1.10345(15) 0.10476(6) 0.62772(8) 0.0140(2) Uani 1 1 d . . .
H10A H 1.1684(4) 0.07003(14) 0.5846(2) 0.0307(5) Uani 1 1 d . . .
H10B H 0.9609(3) 0.10008(14) 0.5982(2) 0.0286(5) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au 0.0000 0.0000 '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
Cl4 Au1 Cl1 89.99(5) . . ?
Cl4 Au1 Cl3 89.96(5) . . ?
Cl1 Au1 Cl3 179.57(6) . . ?
Cl4 Au1 Cl2 179.66(6) . . ?
Cl1 Au1 Cl2 90.18(5) . . ?
Cl3 Au1 Cl2 89.87(5) . . ?
C1 O1 C10 114.78(11) . . ?
O1 C1 C2 108.14(10) . . ?
O1 C1 H1A 109.42(18) . . ?
C2 C1 H1A 109.59(17) . . ?
O1 C1 H1B 110.78(19) . . ?
C2 C1 H1B 110.34(18) . . ?
H1A C1 H1B 108.6(3) . . ?
C2 O2 C3 114.68(11) . . ?
O2 C2 C1 108.12(10) . . ?
O2 C2 H2A 110.38(18) . . ?
C1 C2 H2A 110.33(18) . . ?
O2 C2 H2B 109.52(19) . . ?
C1 C2 H2B 109.86(18) . . ?
H2A C2 H2B 108.6(3) . . ?
C4 O3 C5 112.87(11) . . ?
O2 C3 C4 112.30(10) . . ?
O2 C3 H3A 106.20(18) . . ?
C4 C3 H3A 109.87(17) . . ?
O2 C3 H3B 110.07(17) . . ?
C4 C3 H3B 109.79(18) . . ?
H3A C3 H3B 108.5(2) . . ?
C7 O4 C6 113.81(11) . . ?
O3 C4 C3 108.08(10) . . ?
O3 C4 H4A 110.14(19) . . ?
C3 C4 H4A 111.30(18) . . ?
O3 C4 H4B 110.73(19) . . ?
C3 C4 H4B 108.29(18) . . ?
H4A C4 H4B 108.3(2) . . ?
C9 O5 C8 113.69(11) . . ?
O3 C5 C6 108.87(10) . . ?
O3 C5 H5A 110.61(17) . . ?
C6 C5 H5A 109.5(2) . . ?
O3 C5 H5B 109.09(18) . . ?
C6 C5 H5B 110.62(18) . . ?
H5A C5 H5B 108.2(2) . . ?
H6 O8 H7 105.8(3) . . ?
O4 C6 C5 108.16(10) . . ?
O4 C6 H6A 110.27(18) . . ?
C5 C6 H6A 110.02(19) . . ?
O4 C6 H6B 109.78(18) . . ?
C5 C6 H6B 110.00(18) . . ?
H6A C6 H6B 108.6(2) . . ?
H1 O6 H2 112.9(2) . . ?
H1 O6 H3 112.1(2) . . ?
H2 O6 H3 108.7(2) . . ?
O4 C7 C8 108.25(10) . . ?
O4 C7 H7A 109.94(18) . . ?
C8 C7 H7A 110.47(17) . . ?
O4 C7 H7B 110.65(18) . . ?
C8 C7 H7B 109.03(18) . . ?
H7A C7 H7B 108.5(2) . . ?
H1 O7 H4 119.0(2) . . ?
H1 O7 H5 114.1(3) . . ?
H4 O7 H5 107.4(3) . . ?
O5 C8 C7 108.62(10) . . ?
O5 C8 H8A 108.90(17) . . ?
C7 C8 H8A 109.94(17) . . ?
O5 C8 H8B 110.26(18) . . ?
C7 C8 H8B 109.93(18) . . ?
H8A C8 H8B 109.2(2) . . ?
O5 C9 C10 108.57(10) . . ?
O5 C9 H9A 110.02(18) . . ?
C10 C9 H9A 110.07(18) . . ?
O5 C9 H9B 109.36(17) . . ?
C10 C9 H9B 109.74(17) . . ?
H9A C9 H9B 109.1(2) . . ?
O1 C10 C9 107.01(9) . . ?
O1 C10 H10A 110.96(18) . . ?
C9 C10 H10A 109.49(17) . . ?
O1 C10 H10B 109.57(17) . . ?
C9 C10 H10B 110.79(18) . . ?
H10A C10 H10B 109.0(2) . . ?
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 Cl4 2.2739(13) . ?
Au1 Cl1 2.2797(12) . ?
Au1 Cl3 2.2883(12) . ?
Au1 Cl2 2.2906(12) . ?
O1 C1 1.4192(16) . ?
O1 C10 1.4284(16) . ?
C1 C2 1.5069(15) . ?
C1 H1A 1.102(3) . ?
C1 H1B 1.100(3) . ?
O2 C2 1.4316(17) . ?
O2 C3 1.4322(16) . ?
C2 H2A 1.103(3) . ?
C2 H2B 1.098(3) . ?
O3 C4 1.4171(17) . ?
O3 C5 1.4272(17) . ?
C3 C4 1.5118(16) . ?
C3 H3A 1.097(3) . ?
C3 H3B 1.108(3) . ?
O4 C7 1.4252(17) . ?
O4 C6 1.4281(17) . ?
C4 H4A 1.102(3) . ?
C4 H4B 1.100(3) . ?
O5 C9 1.4328(17) . ?
O5 C8 1.4343(17) . ?
C5 C6 1.5060(17) . ?
C5 H5A 1.100(3) . ?
C5 H5B 1.105(3) . ?
O8 H6 0.966(3) . ?
O8 H7 0.960(3) . ?
C6 H6A 1.096(3) . ?
C6 H6B 1.101(3) . ?
O6 H1 1.120(3) . ?
O6 H2 0.996(3) . ?
O6 H3 0.998(3) . ?
C7 C8 1.5087(16) . ?
C7 H7A 1.104(3) . ?
C7 H7B 1.101(3) . ?
O7 H1 1.317(3) . ?
O7 H4 0.996(3) . ?
O7 H5 0.960(3) . ?
C8 H8A 1.099(3) . ?
C8 H8B 1.099(3) . ?
C9 C10 1.5083(16) . ?
C9 H9A 1.096(3) . ?
C9 H9B 1.101(3) . ?
C10 H10A 1.097(3) . ?
C10 H10B 1.106(3) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H2 O2 0.996(3) 1.666(3) 2.6475(18) 167.4(3) .
O6 H2 O3 0.996(3) 2.641(3) 3.1366(18) 110.8(2) .
O8 H7 O4 0.960(3) 1.809(3) 2.7670(19) 174.8(3) 1_455
O6 H3 O5 0.998(3) 1.662(3) 2.6562(18) 173.8(3) .
O7 H4 O8 0.996(3) 1.579(3) 2.574(2) 177.9(3) .
O8 H6 O1 0.966(3) 1.792(3) 2.7509(19) 171.4(3) 1_455
O7 H5 Cl3 0.960(3) 2.490(3) 3.3087(16) 143.1(3) .
O7 H5 Cl2 0.960(3) 2.688(4) 3.4555(16) 137.2(3) .
O6 H1 O7 1.120(3) 1.317(3) 2.4374(19) 178.5(3) .
