#------------------------------------------------------------------------------
#$Date: 2025-07-05 13:10:14 +0300 (Sat, 05 Jul 2025) $
#$Revision: 300370 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/55/1545566.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1545566
loop_
_publ_author_name
'Matsushita, Nobuyuki'
'Noguchi, Wataru'
'Tanaka, Rikako'
_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
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2017)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_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       ω
_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
;
(ABSCOR; 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 x determined using 1076 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons et al.,  2013)
;
_refine_ls_abs_structure_Flack   -0.006(6)
_refine_ls_extinction_coef       0.0093(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_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/[σ²(Fo²)+(0.0069P)²] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_data_source_file            wm4042sup1.cif
_cod_data_source_block           I
_cod_database_code               1545566
_cod_database_fobs_code          1545566
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.073
_shelx_estimated_absorpt_t_max   0.120
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Au Au 0.75839(2) 0.57191(2) 0.26080(2) 0.01211(5) Uani d 1
C C1 0.6473(6) 0.4715(7) 0.3595(2) 0.0172(9) Uani d 1
C C2 1.0114(6) 0.6470(7) 0.3147(2) 0.0177(8) Uani d 1
C C3 0.8687(6) 0.6664(6) 0.1607(2) 0.0163(8) Uani d 1
C C4 0.5035(6) 0.4994(6) 0.2069(2) 0.0165(8) Uani d 1
N N1 0.5844(5) 0.4150(6) 0.4160(2) 0.0214(8) Uani d 1
N N2 1.1526(6) 0.6928(7) 0.3475(2) 0.0255(9) Uani d 1
N N3 0.9262(6) 0.7151(6) 0.1027(2) 0.0220(8) Uani d 1
N N4 0.3604(5) 0.4584(6) 0.1752(2) 0.0228(8) Uani d 1
K K 0.23731(16) 0.46003(12) 0.51708(4) 0.02024(17) Uani d 1
O O 0.6252(5) 0.3372(5) 0.01812(17) 0.0252(7) Uani d 1
H H1 0.6663 0.3529 0.0632 0.038 Uiso calc 1
H H2 0.7007 0.4050 -0.0090 0.038 Uiso calc 1
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'
N N 0.0061 0.0033 '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'
K K 0.2009 0.2494 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C2 Au C1 . . 90.01(16)
C2 Au C4 . . 179.39(17)
C1 Au C4 . . 90.03(17)
C2 Au C3 . . 90.75(17)
C1 Au C3 . . 178.63(18)
C4 Au C3 . . 89.22(16)
N1 C1 Au . . 179.7(4)
N2 C2 Au . . 177.7(4)
N3 C3 Au . . 177.3(4)
N4 C4 Au . . 178.9(4)
C1 N1 K . . 140.5(3)
C1 N1 K . 4_556 120.6(3)
K N1 K . 4_556 97.27(11)
C2 N2 K . 1_655 115.4(3)
C3 N3 K . 3_655 133.8(3)
C3 N3 K . 2_664 125.2(3)
K N3 K 3_655 2_664 99.69(11)
C4 N4 K . 2_564 126.9(3)
O K O 2_565 3_655 78.50(5)
O K N4 2_565 2_565 72.47(10)
O K N4 3_655 2_565 95.14(11)
O K N1 2_565 . 137.61(11)
O K N1 3_655 . 73.89(11)
N4 K N1 2_565 . 140.78(11)
O K N3 2_565 3_645 89.34(10)
O K N3 3_655 3_645 120.90(10)
N4 K N3 2_565 3_645 135.75(11)
N1 K N3 . 3_645 78.33(10)
O K N3 2_565 2_665 149.29(10)
O K N3 3_655 2_665 104.76(11)
N4 K N3 2_565 2_665 76.83(10)
N1 K N3 . 2_665 70.24(11)
N3 K N3 3_645 2_665 113.15(8)
O K N1 2_565 4_456 98.92(11)
O K N1 3_655 4_456 169.76(10)
N4 K N1 2_565 4_456 74.67(11)
N1 K N1 . 4_456 113.35(8)
N3 K N1 3_645 4_456 68.68(11)
N3 K N1 2_665 4_456 72.36(10)
O K N2 2_565 1_455 67.62(9)
O K N2 3_655 1_455 54.90(9)
N4 K N2 2_565 1_455 133.59(12)
N1 K N2 . 1_455 70.24(10)
N3 K N2 3_645 1_455 66.90(11)
N3 K N2 2_665 1_455 139.40(10)
N1 K N2 4_456 1_455 133.45(10)
O K K 2_565 4_556 166.83(8)
O K K 3_655 4_556 110.40(7)
N4 K K 2_565 4_556 115.09(9)
N1 K K . 4_556 42.63(8)
N3 K K 3_645 4_556 77.79(8)
N3 K K 2_665 4_556 39.84(7)
N1 K K 4_456 4_556 73.99(8)
N2 K K 1_455 4_556 108.91(7)
O K K 2_565 4_456 72.78(7)
O K K 3_655 4_456 144.74(7)
N4 K K 2_565 4_456 95.29(8)
N1 K K . 4_456 115.57(9)
N3 K K 3_645 4_456 40.46(8)
N3 K K 2_665 4_456 110.40(9)
N1 K K 4_456 4_456 40.10(7)
N2 K K 1_455 4_456 94.69(7)
K K K 4_556 4_456 95.28(3)
K O K 2_564 3_645 138.03(13)
K O H1 2_564 . 102.6
K O H1 3_645 . 102.6
K O H2 2_564 . 102.6
K O H2 3_645 . 102.6
H1 O H2 . . 105.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Au C2 . 1.998(4)
Au C1 . 2.002(4)
Au C4 . 2.003(4)
Au C3 . 2.007(4)
C1 N1 . 1.143(5)
C2 N2 . 1.146(5)
C3 N3 . 1.135(5)
C4 N4 . 1.138(5)
N1 K . 2.920(4)
N1 K 4_556 3.071(4)
N2 K 1_655 3.431(4)
N3 K 3_655 2.923(4)
N3 K 2_664 2.961(4)
N4 K 2_564 2.891(4)
K O 2_565 2.804(3)
K O 3_655 2.886(4)
K N4 2_565 2.891(4)
K N3 3_645 2.923(4)
K N3 2_665 2.961(4)
K N1 4_456 3.071(4)
K N2 1_455 3.431(4)
K K 4_556 4.4972(12)
K K 4_456 4.4972(12)
O K 2_564 2.804(3)
O K 3_645 2.886(3)
O H1 . 0.8400
O H2 . 0.8400
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O H2 N1 2_664 0.84 2.32 3.157(5) 178.4 y
O H1 N2 3_745 0.84 2.27 2.952(5) 138.5 y
