#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:33:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179334 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/31/4323125.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_4323125
loop_
_publ_author_name
'Roger E. Cramer'
'David W. Smith'
'William VanDoorne'
_publ_section_title
;
 The Structures of [24-Pyrimidinium crown-6][Au(CN)2]4(NO3)2.2H2O,
 [24-Pyrimidinium crown-6][Au(CN)2]6.5H2O, and [16-Pyrimidinium
 crown-4][Au(CN)2]4.6.5 H2O, in Which Aurophilic Interactions Produce
 Trimers, Tetramers, and Chains of Au(CN)2- Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5895
_journal_page_last               5901
_journal_paper_doi               10.1021/ic980372x
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         (C6H8N3)6[Au(CN)2]6.5H2O
_chemical_formula_sum            'C48 H58 Au6 N30 O5'
_chemical_formula_weight         2317.04
_chemical_name_common            '24PyrC6 hexa-dicyanoaurate'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                102.560(10)
_cell_angle_beta                 112.14
_cell_angle_gamma                101.82
_cell_formula_units_Z            1
_cell_length_a                   11.780(5)
_cell_length_b                   12.064(4)
_cell_length_c                   13.268(4)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      4
_cell_volume                     1616.7(10)
_computing_cell_refinement       SHELXTL
_computing_data_collection       SHELXTL
_computing_data_reduction        SHELXTL
_computing_molecular_graphics    'SHELXL-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3mV'
_diffrn_measurement_method       'Omega scan'
_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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4081
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.629
_exptl_absorpt_correction_T_max  0.058
_exptl_absorpt_correction_T_min  0.035
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            clourless
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_description       Block
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.375
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.908
_refine_diff_density_min         -1.621
_refine_diff_density_rms         0.267
_refine_ls_extinction_coef       0.0016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.991
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         3554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_obs          0.0517
_refine_ls_shift/esd_max         0.074
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0979P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1324
_refine_ls_wR_factor_obs         0.1280
_reflns_number_observed          2879
_reflns_number_total             3691
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980372x_2.cif
_cod_data_source_block           24PyrC6(Au(CN)2)6.5H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323125
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Au1 Au 0.30767(7) 0.74065(6) 0.26436(6) 0.0495(3) Uani 1 d . .
C1O C 0.4558(20) 0.6939(16) 0.3574(15) 0.054(5) Uani 1 d . .
N10 N 0.5428(17) 0.6695(16) 0.4142(14) 0.072(5) Uani 1 d . .
C11 C 0.1586(17) 0.7850(16) 0.1719(14) 0.045(4) Uani 1 d . .
N11 N 0.0705(18) 0.8043(16) 0.1210(17) 0.072(5) Uani 1 d . .
Au2 Au 0.43061(7) 0.80819(6) 0.09652(7) 0.0508(3) Uani 1 d . .
C20 C 0.3798(20) 0.9511(18) 0.0907(15) 0.064(6) Uani 1 d . .
N20 N 0.3465(21) 1.0342(17) 0.0896(14) 0.089(6) Uani 1 d . .
C21 C 0.4818(15) 0.6676(26) 0.1048(16) 0.077(8) Uani 1 d . .
N21 N 0.5064(18) 0.5762(16) 0.1146(15) 0.068(5) Uani 1 d . .
Au3 Au 0.14540(8) 0.72624(7) 0.40822(7) 0.0560(3) Uani 1 d . .
C30 C 0.1069(17) 0.5492(18) 0.3238(15) 0.047(4) Uani 1 d . .
N30 N 0.0818(18) 0.4553(15) 0.2689(16) 0.071(5) Uani 1 d . .
C31 C 0.1783(16) 0.8994(19) 0.4960(14) 0.048(5) Uani 1 d . .
N31 N 0.1887(18) 0.9910(16) 0.5432(14) 0.062(5) Uani 1 d . .
C51A C 0.2282(14) 0.1096(12) 0.3547(13) 0.030(4) Uani 1 d . .
H51A H 0.2121(14) 0.0257(12) 0.3168(13) 0.021(14) Uiso 1 calc R .
H51B H 0.2781(14) 0.1266(12) 0.4366(13) 0.021(14) Uiso 1 calc R .
N1A N 0.3082(11) 0.1853(10) 0.3120(10) 0.026(3) Uani 1 d . .
C2A C 0.4311(15) 0.1886(14) 0.3401(13) 0.035(4) Uani 1 d . .
C21A C 0.4822(15) 0.1009(15) 0.3962(14) 0.042(4) Uani 1 d . .
H21A H 0.4594(85) 0.0263(33) 0.3379(15) 0.060(18) Uiso 1 calc R .
H21B H 0.4450(77) 0.0878(71) 0.4474(67) 0.060(18) Uiso 1 calc R .
H21C H 0.5745(18) 0.1332(42) 0.4388(72) 0.060(18) Uiso 1 calc R .
N3A N 0.5076(12) 0.2599(11) 0.3145(11) 0.035(3) Uani 1 d . .
C4A C 0.4611(14) 0.3285(13) 0.2532(13) 0.030(4) Uani 1 d . .
N41A N 0.5437(13) 0.3997(12) 0.2308(12) 0.045(4) Uani 1 d . .
H41A H 0.6226(13) 0.4001(12) 0.2554(12) 0.080(29) Uiso 1 calc R .
H41B H 0.5183(13) 0.4455(12) 0.1917(12) 0.080(29) Uiso 1 calc R .
C5A C 0.3305(13) 0.3199(12) 0.2120(12) 0.027(3) Uani 1 d . .
C6A C 0.2590(14) 0.2501(12) 0.2460(11) 0.027(3) Uani 1 d . .
H6A H 0.1729(14) 0.2462(12) 0.2236(11) 0.008(17) Uiso 1 calc R .
C51B C -0.2483(14) -0.0577(12) 0.1734(13) 0.030(4) Uani 1 d . .
H51C H -0.2975(14) -0.0636(12) 0.2176(13) 0.021(14) Uiso 1 calc R .
H51D H -0.3003(14) -0.0431(12) 0.1042(13) 0.021(14) Uiso 1 calc R .
N1B N -0.1264(11) 0.0470(10) 0.2431(10) 0.029(3) Uani 1 d . .
C2B C -0.1356(15) 0.1528(13) 0.2901(13) 0.032(4) Uani 1 d . .
C21B C -0.2651(16) 0.1728(15) 0.2548(16) 0.050(5) Uani 1 d . .
H21D H -0.3261(29) 0.1066(46) 0.2550(84) 0.060(18) Uiso 1 calc R .
H21E H -0.2946(47) 0.1793(89) 0.1789(38) 0.060(18) Uiso 1 calc R .
H21F H -0.2571(26) 0.2454(50) 0.3081(52) 0.060(18) Uiso 1 calc R .
N3B N -0.0309(12) 0.2464(10) 0.3659(11) 0.031(3) Uani 1 d . .
C4B C 0.0890(17) 0.2332(13) 0.3912(14) 0.037(4) Uani 1 d . .
N41B N 0.1858(13) 0.3235(12) 0.4746(11) 0.041(3) Uani 1 d . .
H41C H 0.1712(13) 0.3845(12) 0.5085(11) 0.080(29) Uiso 1 calc R .
H41D H 0.2637(13) 0.3217(12) 0.4952(11) 0.080(29) Uiso 1 calc R .
C5B C 0.1027(14) 0.1301(13) 0.3341(12) 0.027(4) Uani 1 d . .
C6B C -0.0075(15) 0.0372(13) 0.2627(14) 0.034(4) Uani 1 d . .
H6B H -0.0013(15) -0.0349(13) 0.2263(14) 0.008(17) Uiso 1 calc R .
C51C C -0.2633(16) -0.3872(13) -0.1336(12) 0.033(4) Uani 1 d . .
H51E H -0.3175(16) -0.4701(13) -0.1624(12) 0.021(14) Uiso 1 calc R .
H51F H -0.1822(16) -0.3864(13) -0.1369(12) 0.021(14) Uiso 1 calc R .
N1C N -0.2372(11) -0.3334(10) -0.0110(10) 0.029(3) Uani 1 d . .
C2C C -0.1903(14) -0.3891(13) 0.0672(13) 0.033(4) Uani 1 d . .
C21C C -0.1609(17) -0.5031(14) 0.0296(14) 0.044(4) Uani 1 d . .
H21G H -0.1021(77) -0.4890(27) -0.0037(79) 0.060(18) Uiso 1 calc R .
H21H H -0.2396(21) -0.5647(28) -0.0263(65) 0.060(18) Uiso 1 calc R .
H21I H -0.1225(90) -0.5280(51) 0.0951(20) 0.060(18) Uiso 1 calc R .
N3C N -0.1705(12) -0.3473(11) 0.1743(11) 0.037(3) Uani 1 d . .
C4C C -0.1903(14) -0.2447(13) 0.2112(13) 0.030(4) Uani 1 d . .
N41C N -0.1666(15) -0.2068(12) 0.3214(12) 0.053(4) Uani 1 d . .
H41E H -0.1398(15) -0.2483(12) 0.3651(12) 0.080(29) Uiso 1 calc R .
H41F H -0.1781(15) -0.1408(12) 0.3489(12) 0.080(29) Uiso 1 calc R .
C5C C -0.2246(14) -0.1740(13) 0.1402(12) 0.027(3) Uani 1 d . .
C6C C -0.2514(13) -0.2255(12) 0.0273(13) 0.029(4) Uani 1 d . .
H6C H -0.2801(13) -0.1851(12) -0.0247(13) 0.008(17) Uiso 1 calc R .
O1 O 0.0385(83) 0.0366(47) 0.0339(31) 0.183(30) Uani 0.50 d P .
O2A O 0.1661(21) 0.5105(22) 0.6704(36) 0.062(12) Uani 0.79(10) d P .
O2B O 0.1443(68) 0.5376(67) 0.6169(96) 0.041(25) Uiso 0.21(10) d P .
O3 O 0.0610(19) 0.7777(17) 0.8814(16) 0.115(6) Uani 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'
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'
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
C11 Au1 C1O 179.1(7) . . ?
C11 Au1 Au3 79.2(5) . . ?
C1O Au1 Au3 100.2(5) . . ?
C11 Au1 Au2 86.2(5) . . ?
C1O Au1 Au2 94.5(5) . . ?
Au3 Au1 Au2 163.73(3) . . ?
N10 C1O Au1 178.0(15) . . ?
N11 C11 Au1 175.7(18) . . ?
C21 Au2 C20 179.1(8) . . ?
C21 Au2 Au1 83.1(6) . . ?
C20 Au2 Au1 96.3(7) . . ?
N20 C20 Au2 177.0(23) . . ?
N21 C21 Au2 173.9(19) . . ?
C31 Au3 C30 177.2(7) . . ?
C31 Au3 Au1 105.1(5) . . ?
C30 Au3 Au1 77.7(5) . . ?
N30 C30 Au3 173.6(18) . . ?
N31 C31 Au3 175.6(18) . . ?
C5B C51A N1A 114.0(11) . . ?
C2A N1A C6A 118.4(12) . . ?
C2A N1A C51A 119.9(12) . . ?
C6A N1A C51A 121.7(11) . . ?
N3A C2A N1A 122.5(14) . . ?
N3A C2A C21A 117.8(13) . . ?
N1A C2A C21A 119.6(14) . . ?
C2A N3A C4A 119.4(13) . . ?
N41A C4A N3A 116.6(13) . . ?
N41A C4A C5A 123.0(15) . . ?
N3A C4A C5A 120.4(14) . . ?
C6A C5A C4A 117.2(14) . . ?
C6A C5A C51C 117.4(13) . 2 ?
C4A C5A C51C 125.4(14) . 2 ?
C5A C6A N1A 121.7(14) . . ?
C5C C51B N1B 113.4(11) . . ?
C2B N1B C6B 119.1(13) . . ?
C2B N1B C51B 118.4(12) . . ?
C6B N1B C51B 122.5(11) . . ?
N1B C2B N3B 122.1(13) . . ?
N1B C2B C21B 120.5(14) . . ?
N3B C2B C21B 117.3(13) . . ?
C2B N3B C4B 118.2(12) . . ?
N41B C4B N3B 114.7(13) . . ?
N41B C4B C5B 124.1(16) . . ?
N3B C4B C5B 121.2(15) . . ?
C6B C5B C4B 117.0(13) . . ?
C6B C5B C51A 118.1(13) . . ?
C4B C5B C51A 124.6(15) . . ?
N1B C6B C5B 121.8(13) . . ?
N1C C51C C5A 112.6(11) . 2 ?
C6C N1C C2C 118.0(13) . . ?
C6C N1C C51C 121.7(12) . . ?
C2C N1C C51C 120.1(12) . . ?
N3C C2C N1C 122.1(14) . . ?
N3C C2C C21C 118.7(13) . . ?
N1C C2C C21C 119.2(14) . . ?
C2C N3C C4C 120.1(13) . . ?
N3C C4C N41C 116.9(14) . . ?
N3C C4C C5C 121.8(13) . . ?
N41C C4C C5C 121.1(14) . . ?
C6C C5C C4C 115.2(13) . . ?
C6C C5C C51B 118.4(13) . . ?
C4C C5C C51B 125.9(13) . . ?
N1C C6C C5C 122.2(14) . . ?
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 C11 1.98(2) . ?
Au1 C1O 1.99(2) . ?
Au1 Au3 3.1758(13) . ?
Au1 Au2 3.2337(12) . ?
C1O N10 1.16(2) . ?
C11 N11 1.11(2) . ?
Au2 C21 1.92(3) . ?
Au2 C20 1.94(2) . ?
C20 N20 1.15(2) . ?
C21 N21 1.22(3) . ?
Au3 C31 2.03(2) . ?
Au3 C30 2.05(2) . ?
C30 N30 1.11(2) . ?
C31 N31 1.10(2) . ?
C51A C5B 1.48(2) . ?
C51A N1A 1.52(2) . ?
N1A C2A 1.34(2) . ?
N1A C6A 1.35(2) . ?
C2A N3A 1.31(2) . ?
C2A C21A 1.52(2) . ?
N3A C4A 1.34(2) . ?
C4A N41A 1.33(2) . ?
C4A C5A 1.40(2) . ?
C5A C6A 1.34(2) . ?
C5A C51C 1.54(2) 2 ?
C51B C5C 1.49(2) . ?
C51B N1B 1.50(2) . ?
N1B C2B 1.34(2) . ?
N1B C6B 1.36(2) . ?
C2B N3B 1.34(2) . ?
C2B C21B 1.51(2) . ?
N3B C4B 1.38(2) . ?
C4B N41B 1.31(2) . ?
C4B C5B 1.38(2) . ?
C5B C6B 1.36(2) . ?
C51C N1C 1.50(2) . ?
C51C C5A 1.54(2) 2 ?
N1C C6C 1.36(2) . ?
N1C C2C 1.36(2) . ?
C2C N3C 1.31(2) . ?
C2C C21C 1.51(2) . ?
N3C C4C 1.33(2) . ?
C4C N41C 1.33(2) . ?
C4C C5C 1.41(2) . ?
C5C C6C 1.37(2) . ?
