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#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/24/7052476.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_7052476
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         614.08
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.347(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9441(7)
_cell_length_b                   18.6964(16)
_cell_length_c                   13.9886(10)
_cell_measurement_temperature    100(2)
_cell_volume                     2012.9(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7727
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    27.3
_exptl_absorpt_correction_T_max  0.5066
_exptl_absorpt_correction_T_min  0.3021
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.775
_refine_diff_density_min         -2.166
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.00149(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+7.4452P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                3759
_reflns_number_total             4598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108935h.txt
_cod_data_source_block           au153(X-ray)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7052476
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
Au1 Au 0.75005(2) 0.505952(9) 0.750363(13) 0.01120(10) Uani 1 1 d . . .
Cl1 Cl 0.81798(17) 0.56227(7) 0.62061(10) 0.0241(3) Uani 1 1 d . . .
O1 O 1.1572(4) 0.17769(16) 0.6235(2) 0.0116(6) Uani 1 1 d . . .
C1 C 1.1107(7) 0.2082(2) 0.5273(3) 0.0155(10) Uani 1 1 d . . .
H1A H 0.9891 0.1958 0.4943 0.019 Uiso 1 1 calc R . .
H1B H 1.1870 0.1892 0.4871 0.019 Uiso 1 1 calc R . .
Cl2 Cl 0.55463(16) 0.43516(6) 0.64355(9) 0.0210(3) Uani 1 1 d . . .
O2 O 0.9995(4) 0.31412(16) 0.5827(2) 0.0125(7) Uani 1 1 d . . .
C2 C 1.1301(6) 0.2877(2) 0.5365(4) 0.0162(10) Uani 1 1 d . . .
H2A H 1.2473 0.3001 0.5770 0.019 Uiso 1 1 calc R . .
H2B H 1.1152 0.3096 0.4705 0.019 Uiso 1 1 calc R . .
Cl3 Cl 0.68019(18) 0.44992(7) 0.88063(9) 0.0239(3) Uani 1 1 d . . .
O3 O 1.0386(4) 0.37079(16) 0.7755(2) 0.0126(7) Uani 1 1 d . . .
C3 C 1.0095(6) 0.3891(2) 0.6043(3) 0.0137(9) Uani 1 1 d . . .
H3A H 0.8908 0.4081 0.5977 0.016 Uiso 1 1 calc R . .
H3B H 1.0603 0.4142 0.5557 0.016 Uiso 1 1 calc R . .
Cl4 Cl 0.94473(17) 0.57534(7) 0.85681(10) 0.0272(3) Uani 1 1 d . . .
O4 O 1.1445(4) 0.25309(16) 0.9013(2) 0.0144(7) Uani 1 1 d . . .
C4 C 1.1177(6) 0.4044(2) 0.7063(3) 0.0140(9) Uani 1 1 d . . .
H4A H 1.2369 0.3857 0.7139 0.017 Uiso 1 1 calc R . .
H4B H 1.1252 0.4567 0.7180 0.017 Uiso 1 1 calc R . .
O5 O 1.0669(4) 0.12795(16) 0.7894(2) 0.0126(7) Uani 1 1 d . . .
C5 C 1.1374(6) 0.3788(2) 0.8755(3) 0.0154(10) Uani 1 1 d . . .
H5A H 1.1117 0.4256 0.9018 0.018 Uiso 1 1 calc R . .
H5B H 1.2632 0.3768 0.8787 0.018 Uiso 1 1 calc R . .
O8 O 0.3771(5) 0.2431(2) 0.7827(3) 0.0236(9) Uani 1 1 d . . .
C6 C 1.0894(6) 0.3193(2) 0.9358(3) 0.0154(10) Uani 1 1 d . . .
H6A H 1.1473 0.3262 1.0064 0.019 Uiso 1 1 calc R . .
H6B H 0.9622 0.3187 0.9283 0.019 Uiso 1 1 calc R . .
O6 O 0.8566(5) 0.2277(2) 0.6904(3) 0.0136(7) Uani 1 1 d . . .
C7 C 1.0776(6) 0.1912(2) 0.9382(3) 0.0157(10) Uani 1 1 d . . .
H7A H 0.9490 0.1927 0.9204 0.019 Uiso 1 1 calc R . .
H7B H 1.1184 0.1896 1.0110 0.019 Uiso 1 1 calc R . .
O7 O 0.6858(5) 0.2861(2) 0.7899(3) 0.0171(8) Uani 1 1 d . . .
C8 C 1.1392(6) 0.1259(3) 0.8942(3) 0.0158(10) Uani 1 1 d . . .
H8A H 1.2677 0.1255 0.9090 0.019 Uiso 1 1 calc R . .
H8B H 1.1006 0.0821 0.9225 0.019 Uiso 1 1 calc R . .
C9 C 1.1588(6) 0.0836(2) 0.7353(3) 0.0122(9) Uani 1 1 d . . .
H9A H 1.1303 0.0327 0.7426 0.015 Uiso 1 1 calc R . .
H9B H 1.2857 0.0900 0.7612 0.015 Uiso 1 1 calc R . .
C10 C 1.1057(6) 0.1049(2) 0.6289(3) 0.0119(9) Uani 1 1 d . . .
H10A H 1.1635 0.0740 0.5891 0.014 Uiso 1 1 calc R . .
H10B H 0.9783 0.1001 0.6032 0.014 Uiso 1 1 calc R . .
H2 H 0.907(8) 0.259(3) 0.670(4) 0.015(15) Uiso 1 1 d . . .
H5 H 0.683(6) 0.324(3) 0.783(4) 0.002(13) Uiso 1 1 d . . .
H1 H 0.758(10) 0.259(5) 0.744(6) 0.07(3) Uiso 1 1 d . . .
H3 H 0.906(9) 0.200(4) 0.717(5) 0.03(2) Uiso 1 1 d . . .
H4 H 0.588(10) 0.270(4) 0.790(5) 0.033(18) Uiso 1 1 d . . .
H7 H 0.323(10) 0.247(3) 0.813(5) 0.03(2) Uiso 1 1 d . . .
H6 H 0.315(11) 0.224(4) 0.738(6) 0.05(2) Uiso 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 0.0033 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'
Cl Cl 0.1484 0.1585 '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'
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 90.06(5) . . ?
Cl4 Au1 Cl3 89.97(5) . . ?
Cl1 Au1 Cl3 179.59(4) . . ?
Cl4 Au1 Cl2 179.56(5) . . ?
Cl1 Au1 Cl2 90.20(5) . . ?
Cl3 Au1 Cl2 89.77(5) . . ?
C1 O1 C10 114.9(3) . . ?
O1 C1 C2 108.6(4) . . ?
O1 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
O1 C1 H1B 110.0 . . ?
C2 C1 H1B 110.0 . . ?
H1A C1 H1B 108.3 . . ?
C3 O2 C2 115.0(3) . . ?
O2 C2 C1 108.0(4) . . ?
O2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
O2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
C4 O3 C5 113.0(3) . . ?
O2 C3 C4 112.1(4) . . ?
O2 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
O2 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C7 O4 C6 114.0(4) . . ?
O3 C4 C3 108.5(4) . . ?
O3 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
O3 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
C8 O5 C9 113.3(3) . . ?
O3 C5 C6 108.5(4) . . ?
O3 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
O3 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
H7 O8 H6 100(8) . . ?
O4 C6 C5 108.0(4) . . ?
O4 C6 H6A 110.1 . . ?
C5 C6 H6A 110.1 . . ?
O4 C6 H6B 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
H2 O6 H1 107(5) . . ?
H2 O6 H3 117(7) . . ?
H1 O6 H3 111(7) . . ?
O4 C7 C8 108.8(4) . . ?
O4 C7 H7A 109.9 . . ?
C8 C7 H7A 109.9 . . ?
O4 C7 H7B 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
H5 O7 H1 112(6) . . ?
H5 O7 H4 111(6) . . ?
H1 O7 H4 118(6) . . ?
O5 C8 C7 107.9(4) . . ?
O5 C8 H8A 110.1 . . ?
C7 C8 H8A 110.1 . . ?
O5 C8 H8B 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
O5 C9 C10 108.4(3) . . ?
O5 C9 H9A 110.0 . . ?
C10 C9 H9A 110.0 . . ?
O5 C9 H9B 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
O1 C10 C9 106.9(4) . . ?
O1 C10 H10A 110.3 . . ?
C9 C10 H10A 110.3 . . ?
O1 C10 H10B 110.3 . . ?
C9 C10 H10B 110.3 . . ?
H10A C10 H10B 108.6 . . ?
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 2.2695(13) . ?
Au1 Cl1 2.2759(12) . ?
Au1 Cl3 2.2863(12) . ?
Au1 Cl2 2.2902(12) . ?
O1 C1 1.424(5) . ?
O1 C10 1.429(5) . ?
C1 C2 1.497(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
O2 C3 1.432(5) . ?
O2 C2 1.438(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O3 C4 1.424(5) . ?
O3 C5 1.433(5) . ?
C3 C4 1.499(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O4 C7 1.424(5) . ?
O4 C6 1.436(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O5 C8 1.437(5) . ?
O5 C9 1.437(5) . ?
C5 C6 1.501(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
O8 H7 0.68(7) . ?
O8 H6 0.78(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
O6 H2 0.80(6) . ?
O6 H1 1.35(9) . ?
O6 H3 0.69(7) . ?
C7 C8 1.502(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
O7 H5 0.72(5) . ?
O7 H1 1.08(9) . ?
O7 H4 0.84(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.497(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
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
C10 O1 C1 C2 165.4(4) . . . . ?
C3 O2 C2 C1 175.1(4) . . . . ?
O1 C1 C2 O2 -67.9(5) . . . . ?
C2 O2 C3 C4 -91.8(5) . . . . ?
C5 O3 C4 C3 176.7(4) . . . . ?
O2 C3 C4 O3 -61.5(5) . . . . ?
C4 O3 C5 C6 -156.6(4) . . . . ?
C7 O4 C6 C5 -168.3(4) . . . . ?
O3 C5 C6 O4 65.3(5) . . . . ?
C6 O4 C7 C8 178.1(4) . . . . ?
C9 O5 C8 C7 160.1(4) . . . . ?
O4 C7 C8 O5 -63.6(5) . . . . ?
C8 O5 C9 C10 -164.6(4) . . . . ?
C1 O1 C10 C9 -177.7(4) . . . . ?
O5 C9 C10 O1 62.1(4) . . . . ?
