Potassium tetracyanidoaurate(III) monohydrate: a redetermination
Matsushita, Nobuyuki; Noguchi, Wataru; Tanaka, Rikako; IUCrData 2 (2017) x170382–; doi:10.1107/S2414314617003820

data_1545566
_publ_section_title
;
 Potassium tetracyanidoaurate(III) monohydrate: a redetermination
;
_journal_coeditor_code           WM4042
_journal_issue                   3
_journal_name_full               IUCrData
_journal_page_first              x170382
_journal_paper_doi               10.1107/S2414314617003820
_journal_volume                  2
_journal_year                    2017
_chemical_formula_iupac          'K [Au (C N)4], H2 O'
_chemical_formula_moiety         'K +, C4 Au N4 -, H2 O'
_chemical_formula_sum            'C4 H2 Au K N4 O'
_chemical_formula_weight         358.16
_chemical_name_systematic
;
Potassium tetracyanidoaurate(III) monohydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6460(7)
_cell_length_b                   7.0733(8)
_cell_length_c                   17.4356(19)
_cell_measurement_reflns_used    8740
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.93
_cell_measurement_theta_min      3.07
_cell_volume                     819.63(15)
_computing_cell_refinement
;
<i>RAPID-AUTO</i> (Rigaku, 2006)
;
_computing_data_collection
;
<i>RAPID-AUTO</i> (Rigaku, 2006)
;
_computing_data_reduction
;
<i>RAPID-AUTO</i> (Rigaku, 2006)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg, 2017)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015<i>b</i>) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging-plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17391
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.981
_diffrn_reflns_theta_min         3.108
_exptl_absorpt_coefficient_mu    18.402
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>ABSCOR</i>; Higashi, 1995)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.439
_refine_diff_density_min         -1.085
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1076 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.006(6)
_refine_ls_extinction_coef       0.0093(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0151
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0069P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0317
_refine_ls_wR_factor_ref         0.0335
_reflns_number_gt                2666
_reflns_number_total             2828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4042sup1.cif
_cod_data_source_block           I
_cod_database_code               1545566
_cod_database_fobs_code          1545566
_shelx_estimated_absorpt_t_min   0.073
_shelx_estimated_absorpt_t_max   0.120
_shelx_hkl_checksum              50095
_shelx_res_checksum              42442