Single crystal neutron and X-ray diffraction studies of (H7O3)[AuCl4]·15-crown-5
Calleja, Maria; Mason, Sax A.; Paul D. Prince; Steed, Jonathan W.; Wilkinson, Clive; New Journal of Chemistry 25 (2001) 1475–1478; doi:10.1039/B108935H

data_7052476
_publ_section_title
;
 Single crystal neutron and X-ray diffraction studies of
 (H7O3)[AuCl4]&#x00B7;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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0000P)^2^+7.4452P] where P=(Fo^2^+2Fc^2^)/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